#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:19:29 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179322 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/19/4321947.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_4321947
loop_
_publ_author_name
'Hing W. Yim'
'Linh M. Tran'
'Ebern D. Dobbin'
'Daniel Rabinovich'
'Louise M. Liable-Sands'
'Christopher D. Incarvito'
'Kin-Chung Lam'
'Arnold L. Rheingold'
_publ_contact_author
;
     Dr. Daniel Rabinovich
     Department of Chemistry
     University of North Carolina at Charlotte
     9201 University City Blvd.
     Charlotte, NC  28223
     USA
;
_publ_contact_author_email       DRabinov@email.uncc.edu
_publ_contact_author_fax         '+704 547 3151'
_publ_contact_author_phone       '+704 547 4442'
_publ_section_title
;
 Tris[(alkylthio)methyl]silanes: Syntheses and Structures of Chromium,
 Molybdenum, and Tungsten Complexes with a Tripodal Thioether Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2211
_journal_page_last               2215
_journal_paper_doi               10.1021/ic981001j
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C10 H18 Mo O3 S3 Si'
_chemical_formula_weight         406.45
_chemical_name_systematic
; 
 ? 
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.8987(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   8.34630(6)
_cell_length_b                   15.2747(2)
_cell_length_c                   27.1865(4)
_cell_measurement_reflns_used    7801
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     3465.51(7)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    XP
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-5.03 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXS-5.03 (Sheldrick, 1994)'
_diffrn_ambient_temperature      198(2)
_diffrn_measurement_device       'Siemens P4/CCD'
_diffrn_measurement_method       'phi, omega'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0359
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            19659
_diffrn_reflns_theta_max         27.91
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    1.184
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_description       rod
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.064
_refine_ls_goodness_of_fit_obs   1.103
_refine_ls_hydrogen_treatment    'idealized contributions'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         7789
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_restrained_S_obs      1.103
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_obs          0.0260
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0300P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0634
_refine_ls_wR_factor_obs         0.0603
_reflns_number_observed          6722
_reflns_number_total             7793
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981001j_2.cif
_cod_data_source_block           drab03
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3465.44(10)
_cod_database_code               4321947
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_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Mo1A Mo 0.41359(2) 0.903196(10) 0.258558(6) 0.02198(5) Uani 1 d . .
S11A S 0.61305(7) 1.01163(3) 0.30229(2) 0.02763(11) Uani 1 d . .
S21A S 0.40573(6) 1.01019(3) 0.18310(2) 0.02672(11) Uani 1 d . .
S31A S 0.66465(6) 0.83605(3) 0.21552(2) 0.02421(11) Uani 1 d . .
Si1A Si 0.77412(7) 1.02934(3) 0.19965(2) 0.02647(12) Uani 1 d . .
O1A O 0.1095(2) 0.99226(12) 0.30419(7) 0.0505(5) Uani 1 d . .
O2A O 0.4027(2) 0.76567(11) 0.34477(6) 0.0463(4) Uani 1 d . .
O3A O 0.1665(2) 0.77725(10) 0.20542(7) 0.0453(4) Uani 1 d . .
C1A C 0.2234(3) 0.95934(14) 0.28713(8) 0.0313(5) Uani 1 d . .
C2A C 0.4107(2) 0.81866(14) 0.31366(8) 0.0294(5) Uani 1 d . .
C3A C 0.2623(2) 0.82284(12) 0.22479(8) 0.0287(4) Uani 1 d . .
C4A C 0.9472(3) 1.09429(15) 0.17452(9) 0.0385(5) Uani 1 d . .
H4AA H 1.0350(3) 1.09544(15) 0.19887(9) 0.058 Uiso 1 calc R .
H4AB H 0.9120(3) 1.15427(15) 0.16749(9) 0.058 Uiso 1 calc R .
H4AC H 0.9843(3) 1.06684(15) 0.14418(9) 0.058 Uiso 1 calc R .
C11A C 0.7047(3) 1.08597(13) 0.25811(8) 0.0322(5) Uani 1 d . .
H11A H 0.7978(3) 1.11500(13) 0.27413(8) 0.039 Uiso 1 calc R .
H11B H 0.6262(3) 1.13201(13) 0.24903(8) 0.039 Uiso 1 calc R .
C12A C 0.5064(3) 1.09104(15) 0.34004(9) 0.0429(6) Uani 1 d . .
H12A H 0.4497(3) 1.06025(15) 0.36617(9) 0.064 Uiso 1 calc R .
H12B H 0.4290(3) 1.12315(15) 0.31943(9) 0.064 Uiso 1 calc R .
H12C H 0.5833(3) 1.13226(15) 0.35474(9) 0.064 Uiso 1 calc R .
C21A C 0.6005(2) 1.02575(14) 0.15326(8) 0.0295(4) Uani 1 d . .
H21A H 0.5981(2) 1.08112(14) 0.13433(8) 0.035 Uiso 1 calc R .
H21B H 0.6182(2) 0.97723(14) 0.12981(8) 0.035 Uiso 1 calc R .
C22A C 0.2958(3) 0.9542(2) 0.13363(9) 0.0460(6) Uani 1 d . .
H22A H 0.1867(3) 0.9413(2) 0.14433(9) 0.069 Uiso 1 calc R .
H22B H 0.3505(3) 0.8994(2) 0.12558(9) 0.069 Uiso 1 calc R .
H22C H 0.2912(3) 0.9919(2) 0.10447(9) 0.069 Uiso 1 calc R .
C31A C 0.8352(2) 0.91244(13) 0.21615(8) 0.0287(4) Uani 1 d . .
H31A H 0.9159(2) 0.89186(13) 0.19246(8) 0.034 Uiso 1 calc R .
H31B H 0.8860(2) 0.91222(13) 0.24931(8) 0.034 Uiso 1 calc R .
C32A C 0.7523(3) 0.74595(14) 0.25160(9) 0.0374(5) Uani 1 d . .
H32A H 0.6734(3) 0.69880(14) 0.25462(9) 0.056 Uiso 1 calc R .
H32B H 0.7828(3) 0.76726(14) 0.28442(9) 0.056 Uiso 1 calc R .
H32C H 0.8474(3) 0.72367(14) 0.23501(9) 0.056 Uiso 1 calc R .
Mo1B Mo 1.09005(2) 1.271848(10) 0.488992(6) 0.02125(5) Uani 1 d . .
S11B S 0.84167(6) 1.33174(3) 0.53656(2) 0.02398(10) Uani 1 d . .
S21B S 1.08846(6) 1.14852(3) 0.55571(2) 0.02841(11) Uani 1 d . .
S31B S 0.88035(6) 1.18689(3) 0.43582(2) 0.02568(11) Uani 1 d . .
Si1B Si 0.72118(7) 1.13941(4) 0.53358(2) 0.02853(13) Uani 1 d . .
O1B O 1.3402(2) 1.38663(10) 0.54863(7) 0.0481(5) Uani 1 d . .
O2B O 1.1039(2) 1.41511(12) 0.40576(7) 0.0513(5) Uani 1 d . .
O3B O 1.3905(2) 1.18494(13) 0.43996(7) 0.0542(5) Uani 1 d . .
C1B C 1.2436(3) 1.34419(13) 0.52744(8) 0.0296(5) Uani 1 d . .
C2B C 1.0967(3) 1.36169(14) 0.43704(8) 0.0310(5) Uani 1 d . .
C3B C 1.2772(3) 1.21762(14) 0.45819(8) 0.0312(5) Uani 1 d . .
C4B C 0.5452(3) 1.07256(14) 0.55421(10) 0.0396(6) Uani 1 d . .
H4BA H 0.5768(3) 1.01093(14) 0.55688(10) 0.059 Uiso 1 calc R .
H4BB H 0.4572(3) 1.07831(14) 0.53016(10) 0.059 Uiso 1 calc R .
H4BC H 0.5101(3) 1.09363(14) 0.58633(10) 0.059 Uiso 1 calc R .
C11B C 0.6670(2) 1.25994(13) 0.52775(8) 0.0285(4) Uani 1 d . .
H11C H 0.6191(2) 1.27067(13) 0.49476(8) 0.034 Uiso 1 calc R .
H11D H 0.5855(2) 1.27464(13) 0.55252(8) 0.034 Uiso 1 calc R .
C12B C 0.7644(3) 1.43185(13) 0.50822(10) 0.0430(6) Uani 1 d . .
H12D H 0.8465(3) 1.47763(13) 0.51012(10) 0.065 Uiso 1 calc R .
H12E H 0.6688(3) 1.45120(13) 0.52567(10) 0.065 Uiso 1 calc R .
H12F H 0.7363(3) 1.42046(13) 0.47367(10) 0.065 Uiso 1 calc R .
C21B C 0.8895(3) 1.12958(15) 0.58152(9) 0.0358(5) Uani 1 d . .
H21C H 0.8712(3) 1.17253(15) 0.60811(9) 0.043 Uiso 1 calc R .
H21D H 0.8867(3) 1.07033(15) 0.59624(9) 0.043 Uiso 1 calc R .
C22B C 1.1949(3) 1.1873(2) 0.61085(9) 0.0469(6) Uani 1 d . .
H22D H 1.3063(3) 1.2005(2) 0.60277(9) 0.070 Uiso 1 calc R .
H22E H 1.1925(3) 1.1418(2) 0.63626(9) 0.070 Uiso 1 calc R .
H22F H 1.1429(3) 1.2403(2) 0.62306(9) 0.070 Uiso 1 calc R .
C31B C 0.7923(3) 1.09779(13) 0.47138(9) 0.0338(5) Uani 1 d . .
H31C H 0.8729(3) 1.05102(13) 0.47657(9) 0.041 Uiso 1 calc R .
H31D H 0.7005(3) 1.07251(13) 0.45276(9) 0.041 Uiso 1 calc R .
C32B C 0.9816(3) 1.1267(2) 0.38730(9) 0.0416(6) Uani 1 d . .
H32D H 1.0346(3) 1.1681(2) 0.36535(9) 0.062 Uiso 1 calc R .
H32E H 0.9028(3) 1.0923(2) 0.36846(9) 0.062 Uiso 1 calc R .
H32F H 1.0617(3) 1.0874(2) 0.40206(9) 0.062 Uiso 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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_
_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
C1A Mo1A C2A 88.07(9) . . ?
C1A Mo1A C3A 86.60(9) . . ?
C2A Mo1A C3A 86.05(8) . . ?
C1A Mo1A S11A 93.21(6) . . ?
C2A Mo1A S11A 94.82(6) . . ?
C3A Mo1A S11A 179.10(6) . . ?
C1A Mo1A S21A 91.53(7) . . ?
C2A Mo1A S21A 176.94(6) . . ?
C3A Mo1A S21A 90.90(6) . . ?
S11A Mo1A S21A 88.22(2) . . ?
C1A Mo1A S31A 176.09(7) . . ?
C2A Mo1A S31A 95.84(6) . . ?
C3A Mo1A S31A 93.39(6) . . ?
S11A Mo1A S31A 86.75(2) . . ?
S21A Mo1A S31A 84.56(2) . . ?
C12A S11A C11A 99.73(11) . . ?
C12A S11A Mo1A 111.25(9) . . ?
C11A S11A Mo1A 111.32(7) . . ?
C22A S21A C21A 99.93(11) . . ?
C22A S21A Mo1A 106.86(8) . . ?
C21A S21A Mo1A 114.40(7) . . ?
C32A S31A C31A 99.71(10) . . ?
C32A S31A Mo1A 111.66(8) . . ?
C31A S31A Mo1A 111.78(7) . . ?
C4A Si1A C21A 110.70(11) . . ?
C4A Si1A C11A 107.89(10) . . ?
C21A Si1A C11A 109.06(10) . . ?
C4A Si1A C31A 111.92(10) . . ?
C21A Si1A C31A 109.03(9) . . ?
C11A Si1A C31A 108.18(10) . . ?
O1A C1A Mo1A 179.5(2) . . ?
O2A C2A Mo1A 176.1(2) . . ?
O3A C3A Mo1A 177.0(2) . . ?
S11A C11A Si1A 113.65(10) . . ?
S21A C21A Si1A 112.26(11) . . ?
S31A C31A Si1A 112.77(11) . . ?
C3B Mo1B C2B 87.52(9) . . ?
C3B Mo1B C1B 87.02(9) . . ?
C2B Mo1B C1B 87.97(9) . . ?
C3B Mo1B S31B 94.89(6) . . ?
C2B Mo1B S31B 88.58(6) . . ?
C1B Mo1B S31B 175.98(6) . . ?
C3B Mo1B S21B 90.26(7) . . ?
C2B Mo1B S21B 177.67(7) . . ?
C1B Mo1B S21B 92.65(6) . . ?
S31B Mo1B S21B 90.88(2) . . ?
C3B Mo1B S11B 174.33(7) . . ?
C2B Mo1B S11B 98.14(7) . . ?
C1B Mo1B S11B 93.16(6) . . ?
S31B Mo1B S11B 85.29(2) . . ?
S21B Mo1B S11B 84.07(2) . . ?
C12B S11B C11B 99.82(10) . . ?
C12B S11B Mo1B 111.14(9) . . ?
C11B S11B Mo1B 111.04(7) . . ?
C22B S21B C21B 99.69(12) . . ?
C22B S21B Mo1B 109.12(9) . . ?
C21B S21B Mo1B 113.15(7) . . ?
C32B S31B C31B 101.62(11) . . ?
C32B S31B Mo1B 109.75(8) . . ?
C31B S31B Mo1B 110.49(8) . . ?
C4B Si1B C11B 111.38(10) . . ?
C4B Si1B C21B 108.89(11) . . ?
C11B Si1B C21B 107.74(10) . . ?
C4B Si1B C31B 109.76(10) . . ?
C11B Si1B C31B 108.98(10) . . ?
C21B Si1B C31B 110.06(11) . . ?
O1B C1B Mo1B 176.9(2) . . ?
O2B C2B Mo1B 178.6(2) . . ?
O3B C3B Mo1B 179.5(2) . . ?
S11B C11B Si1B 112.32(11) . . ?
S21B C21B Si1B 112.80(12) . . ?
S31B C31B Si1B 110.68(10) . . ?
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
Mo1A C1A 1.974(2) . ?
Mo1A C2A 1.978(2) . ?
Mo1A C3A 1.977(2) . ?
Mo1A S11A 2.6204(5) . ?
Mo1A S21A 2.6229(5) . ?
Mo1A S31A 2.6246(5) . ?
S11A C12A 1.829(2) . ?
S11A C11A 1.829(2) . ?
S21A C22A 1.828(2) . ?
S21A C21A 1.844(2) . ?
S31A C32A 1.835(2) . ?
S31A C31A 1.841(2) . ?
Si1A C4A 1.889(2) . ?
Si1A C21A 1.907(2) . ?
Si1A C11A 1.908(2) . ?
Si1A C31A 1.909(2) . ?
O1A C1A 1.177(3) . ?
O2A C2A 1.173(3) . ?
O3A C3A 1.178(2) . ?
Mo1B C3B 1.966(2) . ?
Mo1B C2B 1.971(2) . ?
Mo1B C1B 1.978(2) . ?
Mo1B S31B 2.5996(5) . ?
Mo1B S21B 2.6154(5) . ?
Mo1B S11B 2.6251(5) . ?
S11B C12B 1.826(2) . ?
S11B C11B 1.837(2) . ?
S21B C22B 1.829(2) . ?
S21B C21B 1.835(2) . ?
S31B C32B 1.826(2) . ?
S31B C31B 1.830(2) . ?
Si1B C4B 1.881(2) . ?
Si1B C11B 1.902(2) . ?
Si1B C21B 1.908(2) . ?
Si1B C31B 1.910(2) . ?
O1B C1B 1.178(3) . ?
O2B C2B 1.181(3) . ?
O3B C3B 1.185(3) . ?
