#------------------------------------------------------------------------------
#$Date: 2016-03-24 17:09:42 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179679 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/01/7000127.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_7000127
loop_
_publ_author_name
'Sproules, Stephen A.'
'Morgan, Hugh T.'
'Doonan, Christian J.'
'White, Jonathan M.'
'Young, Charles G.'
_publ_section_title
;
 Synthesis and characterisation of second-generation metallodithiolene
 complexes of the type [Tp*ME(dithiolene)](M=Mo, W; E=O, S) and a novel
 'organoscorpionate' complex of tungsten.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3552
_journal_page_last               3557
_journal_paper_doi               10.1039/b506050h
_journal_year                    2005
_chemical_formula_sum            'C27 H34 B N6 O8 S3 W'
_chemical_formula_weight         861.44
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                76.7550(10)
_cell_angle_beta                 86.9340(10)
_cell_angle_gamma                70.7050(10)
_cell_formula_units_Z            2
_cell_length_a                   9.7848(6)
_cell_length_b                   12.0313(7)
_cell_length_c                   15.8803(9)
_cell_measurement_reflns_used    7335
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.21
_cell_volume                     1717.04(18)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0215
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9082
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    3.601
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red-black
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             858
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.582
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         5972
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0456P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0716
_reflns_number_gt                5725
_reflns_number_total             5972
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b506050h.txt
_cod_data_source_block           jmwspr5
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'multiscan' changed to
'multi-scan' 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 
;
_cod_original_cell_volume        1717.04(17)
_cod_original_sg_symbol_H-M      'P-1 '
_cod_database_code               7000127
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
H1 H 0.390(4) -0.006(3) 0.318(2) 0.022(9) Uiso 1 1 d . . .
C1 C 0.7745(4) 0.1481(3) 0.1238(2) 0.0197(7) Uani 1 1 d . . .
C2 C 0.8084(4) 0.3648(3) 0.3519(2) 0.0223(8) Uani 1 1 d . . .
C3 C 0.8054(4) 0.4235(3) 0.2677(2) 0.0198(7) Uani 1 1 d . . .
C4 C 0.6307(4) 0.1357(3) 0.1399(2) 0.0187(7) Uani 1 1 d . . .
C5 C 0.8464(4) 0.4055(3) 0.4276(2) 0.0255(8) Uani 1 1 d . . .
C6 C 0.7572(6) 0.5258(5) 0.5285(3) 0.0528(13) Uani 1 1 d . . .
H6A H 0.8226 0.5732 0.5114 0.079 Uiso 1 1 calc R . .
H6B H 0.8021 0.4567 0.5760 0.079 Uiso 1 1 calc R . .
H6C H 0.6657 0.5766 0.5474 0.079 Uiso 1 1 calc R . .
C7 C 0.8421(4) 0.5347(3) 0.2358(2) 0.0247(8) Uani 1 1 d . . .
C8 C 0.9070(6) 0.6886(4) 0.2796(3) 0.0427(11) Uani 1 1 d . . .
H8A H 0.9235 0.7111 0.3328 0.064 Uiso 1 1 calc R . .
H8B H 0.8266 0.7533 0.2459 0.064 Uiso 1 1 calc R . .
H8C H 0.9948 0.6765 0.2453 0.064 Uiso 1 1 calc R . .
C9 C 0.8144(4) 0.2207(3) 0.0420(3) 0.0268(8) Uani 1 1 d . . .
C10 C 0.9923(5) 0.3047(4) -0.0224(3) 0.0489(13) Uani 1 1 d . . .
H10A H 1.0929 0.2984 -0.0126 0.073 Uiso 1 1 calc R . .
H10B H 0.9297 0.3887 -0.0275 0.073 Uiso 1 1 calc R . .
H10C H 0.9848 0.2793 -0.0758 0.073 Uiso 1 1 calc R . .
C11 C 0.7359(4) -0.0253(3) 0.0126(3) 0.0306(9) Uani 1 1 d . . .
H11A H 0.6938 0.0599 -0.0168 0.046 Uiso 1 1 calc R . .
H11B H 0.7331 -0.0764 -0.0269 0.046 Uiso 1 1 calc R . .
H11C H 0.8366 -0.0417 0.0299 0.046 Uiso 1 1 calc R . .
C12 C 0.6510(4) -0.0523(3) 0.0908(2) 0.0239(8) Uani 1 1 d . . .
C13 C 0.5922(4) -0.1436(3) 0.1180(3) 0.0292(9) Uani 1 1 d . . .
H13 H 0.6017 -0.2083 0.0908 0.035 Uiso 1 1 calc R . .
C14 C 0.5164(5) -0.1234(3) 0.1924(3) 0.0307(9) Uani 1 1 d . . .
C15 C 0.4314(7) -0.1970(5) 0.2451(3) 0.0582(15) Uani 1 1 d . . .
H15A H 0.4119 -0.2487 0.2111 0.087 Uiso 1 1 calc R . .
H15B H 0.3396 -0.1430 0.2612 0.087 Uiso 1 1 calc R . .
H15C H 0.4873 -0.2475 0.2976 0.087 Uiso 1 1 calc R . .
C16 C 0.4976(4) 0.2288(3) 0.0927(2) 0.0226(8) Uani 1 1 d . . .
C17 C 0.3667(5) 0.4346(3) 0.0417(3) 0.0370(10) Uani 1 1 d . . .
H17A H 0.3639 0.4267 -0.0182 0.055 Uiso 1 1 calc R . .
H17B H 0.3704 0.5149 0.0420 0.055 Uiso 1 1 calc R . .
H17C H 0.2797 0.4240 0.0710 0.055 Uiso 1 1 calc R . .
C21 C 0.4368(4) 0.4621(3) 0.2760(3) 0.0305(9) Uani 1 1 d . . .
H21A H 0.4770 0.4863 0.2196 0.046 Uiso 1 1 calc R . .
H21B H 0.5096 0.4435 0.3217 0.046 Uiso 1 1 calc R . .
H21C H 0.3510 0.5282 0.2855 0.046 Uiso 1 1 calc R . .
C22 C 0.3953(4) 0.3528(3) 0.2779(2) 0.0240(8) Uani 1 1 d . . .
C23 C 0.2547(4) 0.3496(4) 0.2732(3) 0.0326(9) Uani 1 1 d . . .
H23 H 0.1675 0.4155 0.2714 0.039 Uiso 1 1 calc R . .
C24 C 0.2659(4) 0.2337(4) 0.2717(3) 0.0302(9) Uani 1 1 d . . .
C25 C 0.1499(5) 0.1804(4) 0.2642(4) 0.0509(14) Uani 1 1 d . . .
H25A H 0.1746 0.1340 0.2190 0.076 Uiso 1 1 calc R . .
H25B H 0.0572 0.2454 0.2492 0.076 Uiso 1 1 calc R . .
H25C H 0.1421 0.1268 0.3196 0.076 Uiso 1 1 calc R . .
C31 C 0.9714(4) -0.0662(3) 0.4080(3) 0.0294(9) Uani 1 1 d . . .
H31A H 0.9763 0.0155 0.4008 0.044 Uiso 1 1 calc R . .
H31B H 1.0208 -0.1014 0.3602 0.044 Uiso 1 1 calc R . .
H31C H 1.0188 -0.1166 0.4630 0.044 Uiso 1 1 calc R . .
C32 C 0.8158(4) -0.0605(3) 0.4079(2) 0.0229(8) Uani 1 1 d . . .
C33 C 0.7526(4) -0.1353(3) 0.4657(2) 0.0282(8) Uani 1 1 d . . .
H33 H 0.7977 -0.1950 0.5155 0.034 Uiso 1 1 calc R . .
C34 C 0.6127(4) -0.1059(3) 0.4365(2) 0.0253(8) Uani 1 1 d . . .
C35 C 0.4963(5) -0.1560(4) 0.4749(3) 0.0345(10) Uani 1 1 d . . .
H35A H 0.5202 -0.1951 0.5360 0.052 Uiso 1 1 calc R . .
H35B H 0.4889 -0.2154 0.4437 0.052 Uiso 1 1 calc R . .
H35C H 0.4036 -0.0902 0.4701 0.052 Uiso 1 1 calc R . .
B1 B 0.4717(5) 0.0285(4) 0.2947(3) 0.0240(9) Uani 1 1 d . . .
N11 N 0.6169(3) 0.0171(3) 0.1496(2) 0.0211(6) Uani 1 1 d . . .
N12 N 0.5304(3) -0.0238(3) 0.2122(2) 0.0226(6) Uani 1 1 d . . .
N21 N 0.4901(3) 0.2403(3) 0.28065(19) 0.0200(6) Uani 1 1 d . . .
N22 N 0.4083(3) 0.1675(3) 0.2756(2) 0.0222(6) Uani 1 1 d . . .
N31 N 0.7168(3) 0.0146(3) 0.34724(19) 0.0207(6) Uani 1 1 d . . .
N32 N 0.5914(3) -0.0151(3) 0.36409(19) 0.0215(6) Uani 1 1 d . . .
O5 O 0.9634(3) 0.3686(3) 0.4619(2) 0.0425(8) Uani 1 1 d . . .
O6 O 0.7292(3) 0.4821(3) 0.45453(18) 0.0349(7) Uani 1 1 d . . .
O7 O 0.8461(5) 0.5838(3) 0.1624(2) 0.0547(10) Uani 1 1 d . . .
O8 O 0.8717(4) 0.5778(3) 0.30151(19) 0.0461(8) Uani 1 1 d . . .
O9 O 0.7377(3) 0.2655(2) -0.02207(18) 0.0345(7) Uani 1 1 d . . .
O10 O 0.9472(3) 0.2277(2) 0.04969(18) 0.0321(6) Uani 1 1 d . . .
O16 O 0.4002(3) 0.2033(2) 0.06648(18) 0.0299(6) Uani 1 1 d . . .
O17 O 0.4951(3) 0.3423(2) 0.08663(17) 0.0250(6) Uani 1 1 d . . .
S1 S 0.91081(9) 0.03660(8) 0.19493(6) 0.02249(19) Uani 1 1 d . . .
S2 S 0.77109(10) 0.23074(8) 0.38183(6) 0.0223(2) Uani 1 1 d . . .
S3 S 0.75893(9) 0.36328(8) 0.18614(6) 0.01996(19) Uani 1 1 d . . .
W W 0.719992(13) 0.180276(11) 0.249878(8) 0.01611(7) Uani 1 1 d . . .
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'
W W -0.8490 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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C4 C1 C9 124.2(3) . . ?
C4 C1 S1 112.9(2) . . ?
C9 C1 S1 120.5(3) . . ?
C4 C1 W 74.24(19) . . ?
C9 C1 W 133.7(2) . . ?
S1 C1 W 74.13(13) . . ?
C3 C2 C5 125.1(3) . . ?
C3 C2 S2 121.8(3) . . ?
C5 C2 S2 113.1(3) . . ?
C2 C3 C7 125.7(3) . . ?
C2 C3 S3 119.5(3) . . ?
C7 C3 S3 114.8(3) . . ?
N11 C4 C1 118.3(3) . . ?
N11 C4 C16 108.5(3) . . ?
C1 C4 C16 121.3(3) . . ?
N11 C4 W 119.7(2) . . ?
C1 C4 W 66.62(19) . . ?
C16 C4 W 117.5(2) . . ?
O5 C5 O6 124.9(4) . . ?
O5 C5 C2 124.5(4) . . ?
O6 C5 C2 110.5(3) . . ?
O7 C7 O8 122.1(3) . . ?
O7 C7 C3 126.3(4) . . ?
O8 C7 C3 111.6(3) . . ?
O9 C9 O10 124.8(3) . . ?
O9 C9 C1 124.3(4) . . ?
O10 C9 C1 110.9(3) . . ?
N11 C12 C13 107.2(3) . . ?
N11 C12 C11 122.4(3) . . ?
C13 C12 C11 130.5(3) . . ?
C12 C13 C14 107.3(3) . . ?
N12 C14 C13 109.1(3) . . ?
N12 C14 C15 123.6(4) . . ?
C13 C14 C15 127.4(4) . . ?
O16 C16 O17 123.7(3) . . ?
O16 C16 C4 123.3(3) . . ?
O17 C16 C4 112.9(3) . . ?
N21 C22 C23 108.8(3) . . ?
N21 C22 C21 124.9(3) . . ?
C23 C22 C21 126.3(3) . . ?
C24 C23 C22 107.1(3) . . ?
N22 C24 C23 108.1(3) . . ?
N22 C24 C25 122.0(3) . . ?
C23 C24 C25 129.9(4) . . ?
N31 C32 C33 109.2(3) . . ?
N31 C32 C31 123.9(3) . . ?
C33 C32 C31 126.7(3) . . ?
C34 C33 C32 106.8(3) . . ?
N32 C34 C33 107.7(3) . . ?
N32 C34 C35 123.1(4) . . ?
C33 C34 C35 129.2(4) . . ?
N32 B1 N22 109.4(3) . . ?
N32 B1 N12 110.2(3) . . ?
N22 B1 N12 113.9(3) . . ?
C12 N11 N12 110.2(3) . . ?
C12 N11 C4 126.7(3) . . ?
N12 N11 C4 121.0(3) . . ?
C14 N12 N11 106.1(3) . . ?
C14 N12 B1 127.0(3) . . ?
N11 N12 B1 126.6(3) . . ?
C22 N21 N22 106.6(3) . . ?
C22 N21 W 130.8(2) . . ?
N22 N21 W 118.9(2) . . ?
C24 N22 N21 109.4(3) . . ?
C24 N22 B1 126.1(3) . . ?
N21 N22 B1 123.0(3) . . ?
C32 N31 N32 106.9(3) . . ?
C32 N31 W 130.5(2) . . ?
N32 N31 W 121.7(2) . . ?
C34 N32 N31 109.4(3) . . ?
C34 N32 B1 128.6(3) . . ?
N31 N32 B1 120.0(3) . . ?
C5 O6 C6 113.9(3) . . ?
C7 O8 C8 117.6(3) . . ?
C9 O10 C10 115.9(3) . . ?
C16 O17 C17 114.2(3) . . ?
C1 S1 W 59.92(11) . . ?
C2 S2 W 107.23(13) . . ?
C3 S3 W 109.25(12) . . ?
C1 W N21 117.61(12) . . ?
C1 W N31 113.04(12) . . ?
N21 W N31 81.69(11) . . ?
C1 W C4 39.15(13) . . ?
N21 W C4 81.15(12) . . ?
N31 W C4 95.57(11) . . ?
C1 W S3 81.64(9) . . ?
N21 W S3 102.32(8) . . ?
N31 W S3 161.24(8) . . ?
C4 W S3 103.14(9) . . ?
C1 W S1 45.96(9) . . ?
N21 W S1 146.54(8) . . ?
N31 W S1 81.66(8) . . ?
C4 W S1 71.84(9) . . ?
S3 W S1 102.76(3) . . ?
C1 W S2 152.07(10) . . ?
N21 W S2 88.04(8) . . ?
N31 W S2 79.66(8) . . ?
C4 W S2 168.74(9) . . ?
S3 W S2 82.15(3) . . ?
S1 W S2 117.06(3) . . ?
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
C1 C4 1.467(5) . ?
C1 C9 1.501(5) . ?
C1 S1 1.772(4) . ?
C1 W 2.133(3) . ?
C2 C3 1.359(5) . ?
C2 C5 1.504(5) . ?
C2 S2 1.726(4) . ?
C3 C7 1.471(5) . ?
C3 S3 1.766(4) . ?
C4 N11 1.450(4) . ?
C4 C16 1.506(5) . ?
C4 W 2.236(3) . ?
C5 O5 1.193(5) . ?
C5 O6 1.333(5) . ?
C6 O6 1.464(5) . ?
C7 O7 1.185(5) . ?
C7 O8 1.349(5) . ?
C8 O8 1.448(5) . ?
C9 O9 1.205(5) . ?
C9 O10 1.344(5) . ?
C10 O10 1.447(5) . ?
C11 C12 1.491(5) . ?
C12 N11 1.349(5) . ?
C12 C13 1.378(5) . ?
C13 C14 1.387(6) . ?
C14 N12 1.357(5) . ?
C14 C15 1.500(6) . ?
C16 O16 1.213(4) . ?
C16 O17 1.339(4) . ?
C17 O17 1.460(4) . ?
C21 C22 1.493(5) . ?
C22 N21 1.357(4) . ?
C22 C23 1.395(5) . ?
C23 C24 1.367(5) . ?
C24 N22 1.354(5) . ?
C24 C25 1.498(5) . ?
C31 C32 1.501(5) . ?
C32 N31 1.344(5) . ?
C32 C33 1.402(5) . ?
C33 C34 1.373(6) . ?
C34 N32 1.363(4) . ?
C34 C35 1.498(5) . ?
B1 N32 1.526(5) . ?
B1 N22 1.541(5) . ?
B1 N12 1.580(5) . ?
N11 N12 1.381(4) . ?
N21 N22 1.385(4) . ?
N21 W 2.189(3) . ?
N31 N32 1.384(4) . ?
N31 W 2.234(3) . ?
S1 W 2.3705(9) . ?
S2 W 2.4301(9) . ?
S3 W 2.3472(8) . ?
