Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2008
data_global
_journal_name_full 'Dalton Trans.'
_journal_coden_cambridge 0222
#===================================================================
# 0. AUDIT DETAILS
_audit_creation_date 17-Aug-07
_audit_creation_method 'PLATON
option'
_audit_update_record
;
20-Aug-07 Updated by the Author E.H.
Text writing by E.H.
Checkcif OK
20-Aug-07 Updated by the Author E.H.
;
#===================================================================
# 1. SUBMISSION DETAILS
#===================================================================
# Name and address of author for X-ray correspondence
_publ_contact_author_name
;
Dr. Eberhardt Herdtweck
;
_publ_contact_author_address
;
Department Chemie,
Lehrstuhl f\"ur Anorganische Chemie,
Technische Universit\"at M\"unchen,
Lichtenbergstrasse 4,
D-85747 Garching bei M\"unchen,
Germany.
;
_publ_contact_author_email eberhardt.herdtweck@ch.tum.de
_publ_contact_author_fax '+49(0)89 289 13473'
_publ_contact_author_phone '+49(0)89 289 13143'
# Publication choise FI FM FO CI CM CO
_publ_requested_category ?
_publ_requested_coeditor_name ?
_publ_contact_letter # Include date of submission
;
Date of submission: November 2007
;
#===================================================================
# 2. PROCESSING SUMMARY (JOURNAL OFFICE ONLY)
#===================================================================
#===================================================================
# 3. TITLE AND AUTHOR LIST
#===================================================================
_publ_section_title
;
O,S-Donor Ligands as Inhibitors of Xantine Oxidase. Synthesis,
molybdenum complexation and enzyme inhibition
;
# The loop structure below should contain the names and addresses of all
# authors, in the required order of publication. Repeat as necessary.
loop_
_publ_author_name
_publ_author_address
'Sousa, C.'
;
Centro de Quimica Estrutural,
Complexo I,
Instituto Superior Tecnico,
Av. Rovisco Pais,
1049-001 Lisboa,
Portugal.
;
M.Gil
;
Centro de Quimica Estrutural,
Complexo I,
Instituto Superior Tecnico,
Av. Rovisco Pais,
1049-001 Lisboa,
Portugal.
;
R.Jelic
;
Centro de Quimica Estrutural,
Complexo I,
Instituto Superior Tecnico,
Av. Rovisco Pais,
1049-001 Lisboa,
Portugal.
;
M.J.Romao
;
Faculty of Science,
Chemistry Department,
Kragujevac,
Serbia and Montenegro.
;
J.Trincao
;
REQUIMTE-CQFB, Departamento de Qu\'imica,
Faculdade de Ciencias e Tecnologia,
Universidade Nova de Lisboa,
Portugal.
;
E.Herdtweck
;
REQUIMTE-CQFB, Departamento de Qu\'imica,
Faculdade de Ciencias e Tecnologia,
Universidade Nova de Lisboa,
Portugal.
;
C.Pereira
;
Department Chemie,
Lehrstuhl f\"ur Anorganische Chemie,
Technische Universit\"at M\"unchen,
Lichtenbergstrasse 4,
D-85747 Garching bei M\"unchen,
Germany.
;
P.Fresco
;
Laboratorio de Farmacologia,
REQUIMTE-FARMA,
Faculdade de Farm\'acia,
Universidade do Porto,
Rua Anibal Cunha, 164,
4050-123 Porto,
Portugal.
;
M.A.Santos
;
Laboratorio de Farmacologia,
REQUIMTE-FARMA,
Faculdade de Farm\'acia,
Universidade do Porto,
Rua Anibal Cunha, 164,
4050-123 Porto,
Portugal.
;
#===================================================================
# 4. TEXT
#===================================================================
# Insert blank lines between references
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C.,
Polidori, G. & Camalli, M. (1994). SIR92, J. Appl. Cryst. 27, 435-436.
Farrugia, L. J. (1999). WinGX (Version 1.70.01 January 2005),
J. Appl. Cryst. 32, 837-838.
Nonius (2001a). Data Collection Software for Nonius Kappa-CCD devices.
Nonius BV, Delft, The Netherlands.
Nonius (2001b). DENZO Processing Software for Nonius Kappa-CCD devices,
Nonius BV, Delft, The Netherlands.
Sheldrick, G. M. (1998). SHELXL97, University of G\"ottingen, G\"ottingen,
Germany.
Spek, A. L. (2007). PLATON, A Multipurpose Crystallographic Tool, Utrecht
University, Utrecht, The Netherlands.
;
data_a
_database_code_depnum_ccdc_archive 'CCDC 656367'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C12 H11 Mo O6.50 S2'
_chemical_formula_sum 'C12 H11 Mo O6.50 S2'
_chemical_formula_weight 419.27
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'
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'
_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M P-1
_symmetry_space_group_name_Hall 'P -1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 9.8133(2)
_cell_length_b 10.9684(2)
_cell_length_c 14.5117(3)
_cell_angle_alpha 103.8730(10)
_cell_angle_beta 106.2010(10)
_cell_angle_gamma 90.0260(10)
_cell_volume 1452.40(5)
_cell_formula_units_Z 4
_cell_measurement_temperature 273(2)
_cell_measurement_reflns_used 9209
_cell_measurement_theta_min 2.72
_cell_measurement_theta_max 29.74
_exptl_crystal_description plate
_exptl_crystal_colour yellow
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.02
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.917
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 836
_exptl_absorpt_coefficient_mu 1.217
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.7928
_exptl_absorpt_correction_T_max 0.9761
_exptl_absorpt_process_details
'SADABS-Bruker Nonius area detector scaling and absorption correction - V2.10'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 273(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 81371
_diffrn_reflns_av_R_equivalents 0.0564
_diffrn_reflns_av_sigmaI/netI 0.0237
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_theta_min 1.51
_diffrn_reflns_theta_max 25.00
_reflns_number_total 5108
_reflns_number_gt 4450
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'Bruker SMART'
_computing_cell_refinement 'Bruker SMART'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'Ortep-3 for Windows/Platon'
_computing_publication_material 'Bruker SHELXTL'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0539P)^2^+4.2233P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 5108
_refine_ls_number_parameters 400
_refine_ls_number_restraints 2
_refine_ls_R_factor_all 0.0386
_refine_ls_R_factor_gt 0.0316
_refine_ls_wR_factor_ref 0.0884
_refine_ls_wR_factor_gt 0.0837
_refine_ls_goodness_of_fit_ref 0.956
_refine_ls_restrained_S_all 0.955
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
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
Mo1 Mo 0.11473(3) 0.42933(3) 0.28806(2) 0.01634(10) Uani 1 1 d . . .
S1 S -0.03116(10) 0.60071(9) 0.23897(7) 0.0199(2) Uani 1 1 d . . .
S2 S 0.31955(10) 0.29525(9) 0.32241(7) 0.0194(2) Uani 1 1 d . . .
O11 O 0.0253(3) 0.2886(3) 0.2166(2) 0.0253(6) Uani 1 1 d . . .
O12 O 0.0452(3) 0.4603(3) 0.3866(2) 0.0252(6) Uani 1 1 d . . .
O18 O 0.1813(3) 0.4576(2) 0.16679(18) 0.0177(5) Uani 1 1 d . . .
O28 O 0.2870(3) 0.5619(2) 0.36562(18) 0.0171(5) Uani 1 1 d . . .
O24 O 0.6666(3) 0.6016(2) 0.42758(18) 0.0175(5) Uani 1 1 d . . .
014 O 0.1657(3) 0.6699(2) 0.01284(18) 0.0187(6) Uani 1 1 d . . .
C11 C 0.0408(4) 0.6311(3) 0.1520(3) 0.0167(7) Uani 1 1 d . . .
C12 C 0.0054(4) 0.7314(4) 0.1062(3) 0.0207(8) Uani 1 1 d . . .
H12 H -0.0604 0.7866 0.1234 0.025 Uiso 1 1 calc R . .
C13 C 0.0673(4) 0.7464(4) 0.0374(3) 0.0213(8) Uani 1 1 d . . .
H13 H 0.0417 0.8112 0.0062 0.026 Uiso 1 1 calc R . .
C16 C 0.1467(4) 0.5518(3) 0.1264(3) 0.0152(7) Uani 1 1 d . . .
C15 C 0.2106(4) 0.5781(3) 0.0588(3) 0.0162(7) Uani 1 1 d . . .
C17 C 0.3310(4) 0.5141(4) 0.0305(3) 0.0241(9) Uani 1 1 d . . .
H17A H 0.2969 0.4588 -0.0346 0.036 Uiso 1 1 calc R . .
H17B H 0.3736 0.4661 0.0771 0.036 Uiso 1 1 calc R . .
H17C H 0.4005 0.5758 0.0307 0.036 Uiso 1 1 calc R . .
C21 C 0.4565(4) 0.4086(3) 0.3615(3) 0.0170(8) Uani 1 1 d . . .
C22 C 0.6017(4) 0.3842(4) 0.3795(3) 0.0190(8) Uani 1 1 d . . .
H22 H 0.6284 0.3018 0.3697 0.023 Uiso 1 1 calc R . .
C23 C 0.7008(4) 0.4812(4) 0.4108(3) 0.0197(8) Uani 1 1 d . . .
H23 H 0.7961 0.4646 0.4213 0.024 Uiso 1 1 calc R . .
C25 C 0.5286(4) 0.6304(3) 0.4118(3) 0.0168(8) Uani 1 1 d . . .
C26 C 0.4207(4) 0.5352(3) 0.3785(3) 0.0152(7) Uani 1 1 d . . .
C27 C 0.5058(4) 0.7659(3) 0.4365(3) 0.0203(8) Uani 1 1 d . . .
H27A H 0.4702 0.7858 0.4932 0.030 Uiso 1 1 calc R . .
H27B H 0.4380 0.7860 0.3812 0.030 Uiso 1 1 calc R . .
H27C H 0.5943 0.8141 0.4512 0.030 Uiso 1 1 calc R . .
Mo2 Mo 0.67047(3) -0.15010(3) 0.21585(2) 0.01580(10) Uani 1 1 d . . .
S4 S 0.65863(10) 0.03042(8) 0.37987(7) 0.0195(2) Uani 1 1 d . . .
S3 S 0.41237(10) -0.12763(9) 0.16455(8) 0.0230(2) Uani 1 1 d . . .
O22 O 0.6285(3) -0.2655(2) 0.2668(2) 0.0227(6) Uani 1 1 d . . .
O21 O 0.6991(3) -0.2317(2) 0.10771(19) 0.0228(6) Uani 1 1 d . . .
O44 O 1.1182(3) 0.1560(2) 0.45876(19) 0.0223(6) Uani 1 1 d . . .
O34 O 0.4218(3) 0.2524(3) 0.10705(19) 0.0246(6) Uani 1 1 d . . .
O48 O 0.8706(3) -0.0893(2) 0.28659(18) 0.0167(5) Uani 1 1 d . . .
O38 O 0.6600(3) 0.0194(2) 0.16770(19) 0.0195(6) Uani 1 1 d . . .
C31 C 0.4098(4) 0.0140(4) 0.1337(3) 0.0203(8) Uani 1 1 d . . .
C32 C 0.2850(4) 0.0738(4) 0.1019(3) 0.0244(9) Uani 1 1 d . . .
H32 H 0.1961 0.0330 0.0891 0.029 Uiso 1 1 calc R . .
C33 C 0.2962(5) 0.1912(4) 0.0902(3) 0.0285(10) Uani 1 1 d . . .
H33 H 0.2136 0.2309 0.0696 0.034 Uiso 1 1 calc R . .
C35 C 0.5448(4) 0.1968(4) 0.1337(3) 0.0220(8) Uani 1 1 d . . .
C36 C 0.5421(4) 0.0755(4) 0.1445(3) 0.0198(8) Uani 1 1 d . . .
C37 C 0.6738(5) 0.2763(4) 0.1496(3) 0.0287(10) Uani 1 1 d . . .
H37A H 0.7045 0.2567 0.0908 0.043 Uiso 1 1 calc R . .
H37B H 0.7475 0.2608 0.2040 0.043 Uiso 1 1 calc R . .
H37C H 0.6536 0.3633 0.1645 0.043 Uiso 1 1 calc R . .
C41 C 0.8304(4) 0.0830(3) 0.4112(3) 0.0169(8) Uani 1 1 d . . .
C42 C 0.8947(4) 0.1919(3) 0.4877(3) 0.0197(8) Uani 1 1 d . . .
H42 H 0.8404 0.2410 0.5236 0.024 Uiso 1 1 calc R . .
C43 C 1.0337(5) 0.2230(4) 0.5076(3) 0.0251(9) Uani 1 1 d . . .
H43 H 1.0738 0.2944 0.5577 0.030 Uiso 1 1 calc R . .
C45 C 1.0630(4) 0.0517(3) 0.3847(3) 0.0186(8) Uani 1 1 d . . .
C46 C 0.9220(4) 0.0142(3) 0.3595(2) 0.0145(7) Uani 1 1 d . . .
C47 C 1.1692(4) -0.0133(4) 0.3387(3) 0.0239(9) Uani 1 1 d . . .
H47A H 1.1639 0.0112 0.2787 0.036 Uiso 1 1 calc R . .
H47B H 1.1495 -0.1027 0.3239 0.036 Uiso 1 1 calc R . .
H47C H 1.2628 0.0096 0.3838 0.036 Uiso 1 1 calc R . .
O5 O 0.9300(3) 0.0405(3) 0.1105(2) 0.0278(6) Uani 1 1 d D . .
H51 H 0.964(5) 0.121(3) 0.153(3) 0.043(14) Uiso 1 1 d D . .
H52 H 0.840(4) 0.021(6) 0.117(5) 0.08(2) Uiso 1 1 d D . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.01274(18) 0.01916(18) 0.01781(17) 0.00513(13) 0.00503(13) -0.00011(13)
S1 0.0167(5) 0.0251(5) 0.0204(5) 0.0060(4) 0.0092(4) 0.0066(4)
S2 0.0184(5) 0.0167(4) 0.0229(5) 0.0070(4) 0.0039(4) 0.0001(4)
O11 0.0196(15) 0.0225(14) 0.0304(15) 0.0058(12) 0.0025(12) -0.0025(11)
O12 0.0188(15) 0.0386(17) 0.0243(14) 0.0127(12) 0.0121(12) 0.0041(12)
O18 0.0185(14) 0.0170(13) 0.0201(13) 0.0058(10) 0.0088(11) 0.0058(10)
O28 0.0147(14) 0.0163(13) 0.0204(13) 0.0028(10) 0.0067(10) 0.0026(10)
O24 0.0135(13) 0.0170(13) 0.0222(13) 0.0034(10) 0.0065(11) 0.0012(10)
014 0.0176(14) 0.0187(13) 0.0220(13) 0.0064(11) 0.0080(11) 0.0039(11)
C11 0.0120(18) 0.0193(18) 0.0160(17) 0.0011(14) 0.0023(14) 0.0005(14)
C12 0.016(2) 0.0186(19) 0.025(2) 0.0041(15) 0.0041(16) 0.0066(15)
C13 0.019(2) 0.0175(19) 0.028(2) 0.0062(16) 0.0079(16) 0.0056(16)
C16 0.0131(18) 0.0144(17) 0.0151(17) 0.0008(14) 0.0017(14) 0.0003(14)
C15 0.0164(19) 0.0126(17) 0.0162(17) -0.0007(14) 0.0031(15) -0.0012(14)
C17 0.026(2) 0.0193(19) 0.032(2) 0.0058(16) 0.0174(18) 0.0077(17)
C21 0.019(2) 0.0194(19) 0.0142(17) 0.0053(14) 0.0055(15) -0.0013(15)
C22 0.021(2) 0.0182(19) 0.0195(18) 0.0062(15) 0.0070(15) 0.0075(15)
C23 0.015(2) 0.023(2) 0.0218(19) 0.0074(16) 0.0057(15) 0.0068(16)
C25 0.0142(19) 0.0230(19) 0.0144(17) 0.0041(14) 0.0062(14) 0.0044(15)
C26 0.0149(19) 0.0201(18) 0.0127(17) 0.0050(14) 0.0066(14) 0.0046(15)
C27 0.020(2) 0.0162(19) 0.025(2) 0.0003(15) 0.0110(16) 0.0019(15)
Mo2 0.01456(18) 0.01351(17) 0.01913(18) 0.00174(12) 0.00650(13) 0.00231(12)
S4 0.0173(5) 0.0160(4) 0.0244(5) 0.0002(4) 0.0092(4) 0.0018(4)
S3 0.0141(5) 0.0194(5) 0.0338(5) 0.0029(4) 0.0075(4) 0.0010(4)
O22 0.0250(15) 0.0155(13) 0.0286(15) 0.0027(11) 0.0118(12) 0.0023(11)
O21 0.0240(15) 0.0220(14) 0.0215(14) 0.0020(11) 0.0081(11) 0.0049(11)
O44 0.0179(14) 0.0193(14) 0.0256(14) -0.0023(11) 0.0064(11) -0.0016(11)
O34 0.0244(16) 0.0283(15) 0.0247(14) 0.0117(12) 0.0083(12) 0.0122(12)
O48 0.0175(14) 0.0128(12) 0.0185(13) 0.0011(10) 0.0053(10) 0.0040(10)
O38 0.0176(14) 0.0171(13) 0.0255(14) 0.0081(11) 0.0066(11) 0.0027(11)
C31 0.018(2) 0.0221(19) 0.0174(18) -0.0005(15) 0.0039(15) 0.0024(16)
C32 0.016(2) 0.026(2) 0.024(2) -0.0003(16) 0.0010(16) 0.0069(16)
C33 0.022(2) 0.035(2) 0.023(2) 0.0041(18) 0.0014(17) 0.0109(19)
C35 0.028(2) 0.023(2) 0.0171(19) 0.0053(15) 0.0090(16) 0.0086(17)
C36 0.021(2) 0.0221(19) 0.0164(18) 0.0047(15) 0.0052(15) 0.0041(16)
C37 0.033(2) 0.025(2) 0.041(3) 0.0182(19) 0.022(2) 0.0100(18)
C41 0.018(2) 0.0154(18) 0.0196(18) 0.0064(14) 0.0071(15) 0.0031(15)
C42 0.022(2) 0.0163(18) 0.0207(19) 0.0008(15) 0.0092(16) 0.0006(15)
C43 0.033(2) 0.0149(19) 0.023(2) -0.0041(15) 0.0080(18) -0.0015(17)
C45 0.021(2) 0.0166(18) 0.0178(18) 0.0039(15) 0.0046(15) 0.0026(15)
C46 0.018(2) 0.0127(17) 0.0120(17) 0.0026(13) 0.0042(14) 0.0042(14)
C47 0.018(2) 0.024(2) 0.028(2) 0.0015(17) 0.0092(17) 0.0013(16)
O5 0.0262(17) 0.0270(16) 0.0311(16) 0.0024(13) 0.0138(13) -0.0004(13)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Mo1 O12 1.714(3) . ?
Mo1 O11 1.718(3) . ?
Mo1 O28 2.095(3) . ?
Mo1 O18 2.127(2) . ?
Mo1 S1 2.4832(10) . ?
Mo1 S2 2.4993(10) . ?
S1 C11 1.703(4) . ?
S2 C21 1.705(4) . ?
O18 C16 1.306(4) . ?
O28 C26 1.316(4) . ?
O24 C23 1.344(4) . ?
O24 C25 1.359(4) . ?
014 C13 1.346(5) . ?
014 C15 1.346(4) . ?
C11 C12 1.412(5) . ?
C11 C16 1.427(5) . ?
C12 C13 1.346(6) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C16 C15 1.384(5) . ?
C15 C17 1.480(5) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C21 C22 1.413(5) . ?
C21 C26 1.413(5) . ?
C22 C23 1.344(6) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C25 C26 1.385(5) . ?
C25 C27 1.476(5) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
Mo2 O21 1.708(3) . ?
Mo2 O22 1.714(3) . ?
Mo2 O48 1.975(3) . ?
Mo2 O38 2.130(2) . ?
Mo2 S3 2.4630(10) . ?
Mo2 S4 2.7376(9) . ?
S4 C41 1.682(4) . ?
S3 C31 1.716(4) . ?
O44 C43 1.345(5) . ?
O44 C45 1.357(4) . ?
O34 C33 1.335(5) . ?
O34 C35 1.353(5) . ?
O48 C46 1.337(4) . ?
O38 C36 1.308(5) . ?
C31 C32 1.404(5) . ?
C31 C36 1.414(6) . ?
C32 C33 1.347(6) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
C35 C36 1.379(5) . ?
C35 C37 1.467(6) . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C41 C42 1.424(5) . ?
C41 C46 1.430(5) . ?
C42 C43 1.339(6) . ?
C42 H42 0.9300 . ?
C43 H43 0.9300 . ?
C45 C46 1.365(5) . ?
C45 C47 1.483(5) . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
O5 H51 0.95(2) . ?
O5 H52 0.94(2) . ?
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
O12 Mo1 O11 102.62(14) . . ?
O12 Mo1 O28 91.60(12) . . ?
O11 Mo1 O28 158.55(12) . . ?
O12 Mo1 O18 159.57(12) . . ?
O11 Mo1 O18 90.65(12) . . ?
O28 Mo1 O18 80.58(10) . . ?
O12 Mo1 S1 84.00(10) . . ?
O11 Mo1 S1 107.61(9) . . ?
O28 Mo1 S1 89.59(7) . . ?
O18 Mo1 S1 77.14(7) . . ?
O12 Mo1 S2 109.08(9) . . ?
O11 Mo1 S2 83.15(9) . . ?
O28 Mo1 S2 77.01(7) . . ?
O18 Mo1 S2 87.66(7) . . ?
S1 Mo1 S2 161.26(3) . . ?
C11 S1 Mo1 100.58(13) . . ?
C21 S2 Mo1 99.46(13) . . ?
C16 O18 Mo1 123.9(2) . . ?
C26 O28 Mo1 123.3(2) . . ?
C23 O24 C25 121.0(3) . . ?
C13 014 C15 121.4(3) . . ?
C12 C11 C16 118.3(3) . . ?
C12 C11 S1 124.3(3) . . ?
C16 C11 S1 117.4(3) . . ?
C13 C12 C11 119.6(4) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
014 C13 C12 121.5(3) . . ?
014 C13 H13 119.2 . . ?
C12 C13 H13 119.2 . . ?
O18 C16 C15 121.8(3) . . ?
O18 C16 C11 119.9(3) . . ?
C15 C16 C11 118.3(3) . . ?
014 C15 C16 120.6(3) . . ?
014 C15 C17 113.6(3) . . ?
C16 C15 C17 125.8(3) . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C22 C21 C26 118.5(3) . . ?
C22 C21 S2 124.5(3) . . ?
C26 C21 S2 117.0(3) . . ?
C23 C22 C21 119.3(3) . . ?
C23 C22 H22 120.3 . . ?
C21 C22 H22 120.3 . . ?
C22 C23 O24 122.0(3) . . ?
C22 C23 H23 119.0 . . ?
O24 C23 H23 119.0 . . ?
O24 C25 C26 120.1(3) . . ?
O24 C25 C27 115.6(3) . . ?
C26 C25 C27 124.3(3) . . ?
O28 C26 C25 120.6(3) . . ?
O28 C26 C21 120.3(3) . . ?
C25 C26 C21 119.0(3) . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O21 Mo2 O22 103.82(12) . . ?
O21 Mo2 O48 96.88(12) . . ?
O22 Mo2 O48 106.95(12) . . ?
O21 Mo2 O38 90.59(11) . . ?
O22 Mo2 O38 159.87(12) . . ?
O48 Mo2 O38 84.75(10) . . ?
O21 Mo2 S3 102.12(9) . . ?
O22 Mo2 S3 85.28(10) . . ?
O48 Mo2 S3 154.26(7) . . ?
O38 Mo2 S3 77.90(7) . . ?
O21 Mo2 S4 165.34(9) . . ?
O22 Mo2 S4 90.36(9) . . ?
O48 Mo2 S4 75.05(7) . . ?
O38 Mo2 S4 76.65(7) . . ?
S3 Mo2 S4 82.47(3) . . ?
C41 S4 Mo2 94.71(13) . . ?
C31 S3 Mo2 100.42(14) . . ?
C43 O44 C45 120.0(3) . . ?
C33 O34 C35 121.0(3) . . ?
C46 O48 Mo2 128.9(2) . . ?
C36 O38 Mo2 123.0(2) . . ?
C32 C31 C36 118.6(4) . . ?
C32 C31 S3 123.9(3) . . ?
C36 C31 S3 117.5(3) . . ?
C33 C32 C31 118.9(4) . . ?
C33 C32 H32 120.6 . . ?
C31 C32 H32 120.6 . . ?
O34 C33 C32 122.3(4) . . ?
O34 C33 H33 118.8 . . ?
C32 C33 H33 118.8 . . ?
O34 C35 C36 120.2(4) . . ?
O34 C35 C37 114.5(3) . . ?
C36 C35 C37 125.3(4) . . ?
O38 C36 C35 120.8(4) . . ?
O38 C36 C31 120.4(3) . . ?
C35 C36 C31 118.7(4) . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C42 C41 C46 116.2(3) . . ?
C42 C41 S4 124.9(3) . . ?
C46 C41 S4 118.9(3) . . ?
C43 C42 C41 119.5(4) . . ?
C43 C42 H42 120.2 . . ?
C41 C42 H42 120.2 . . ?
C42 C43 O44 123.3(3) . . ?
C42 C43 H43 118.4 . . ?
O44 C43 H43 118.4 . . ?
O44 C45 C46 120.3(3) . . ?
O44 C45 C47 113.8(3) . . ?
C46 C45 C47 125.8(3) . . ?
O48 C46 C45 119.1(3) . . ?
O48 C46 C41 120.2(3) . . ?
C45 C46 C41 120.7(3) . . ?
C45 C47 H47A 109.5 . . ?
C45 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C45 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
H51 O5 H52 108(5) . . ?
_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max 2.376
_refine_diff_density_min -0.904
_refine_diff_density_rms 0.094
#===================================================================
data_LISA-4419-173
_database_code_depnum_ccdc_archive 'CCDC 656368'
#===================================================================
#===================================================================
# 5. CHEMICAL DATA
#===================================================================
_chemical_name_systematic
;
;
_chemical_name_common ?
_chemical_formula_moiety 'C12 H10 Mo2 O9 S2'
_chemical_formula_structural ?
_chemical_formula_analytical ?
_chemical_formula_sum 'C12 H10 Mo2 O9 S2'
_chemical_formula_weight 554.22
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
S S 0.1246 0.1234 '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'
Mo Mo -1.6832 0.6857 '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'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
#===================================================================
# 6. CRYSTAL DATA
#===================================================================
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 21/n'
_symmetry_Int_Tables_number 14
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,1/2+y,1/2-z
-x,-y,-z
1/2+x,1/2-y,1/2+z
_cell_length_a 8.2509(1)
_cell_length_b 13.9940(2)
_cell_length_c 14.6426(2)
_cell_angle_alpha 90
_cell_angle_beta 105.8518(6)
_cell_angle_gamma 90
_cell_volume 1626.39(4)
_cell_formula_units_Z 4
_cell_measurement_temperature 173(1)
_cell_measurement_reflns_used 3102
_cell_measurement_theta_min 2.05
_cell_measurement_theta_max 25.32
_exptl_crystal_description prism
_exptl_crystal_colour yellow
_exptl_crystal_size_max 0.23
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.10
_exptl_crystal_density_meas none
_exptl_crystal_density_diffrn 2.263
_exptl_crystal_density_method none
_exptl_crystal_F_000 1080
_exptl_absorpt_coefficient_mu 1.845
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.639
_exptl_absorpt_correction_T_max 0.833
_exptl_absorpt_process_details
'(applied during the scaling procedure; Nonius, 2001b)'
_exptl_special_details
;
Diffractometer operator E. Herdtweck
scanspeed 2 x 40 s per film
repetition 1
dx 40
565 films measured in 10 data sets
set 1: phi-scan with delta_phi = 2.0
set 2 to 10: omega-scans with delta_omega = 2.0
;
_publ_section_exptl_prep
;
The crystal was fixed in a capillary with perfluorinated ether and
transferred to the diffractometer.
;
_publ_section_exptl_refinement
;
Solution and refinements with the program WinGX;
Farrugia (1999).
Hydrogen atoms could not be located in the difference Fourier maps
and were calculated in ideal positions (riding model).
;
#===================================================================
# 7. EXPERIMENTAL DATA
#===================================================================
_diffrn_ambient_temperature 173(1)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_source 'NONIUS FR 591 rotating anode'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device ' \k-geometry diffractometer '
_diffrn_measurement_device_type ' Nonius \k-CCD diffractometer'
_diffrn_measurement_method ' phi- and omega-rotation '
_diffrn_detector ' CCD plate '
_diffrn_detector_area_resol_mean 18 # 9 for binned mode
_diffrn_standards_decay_% 0
# number of measured reflections (redundant set)
_diffrn_reflns_number 40422
_diffrn_reflns_av_R_equivalents 0.034
_diffrn_reflns_av_sigmaI/netI 0.0165
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_theta_min 2.05
_diffrn_reflns_theta_max 25.32
_reflns_number_total 2963
_reflns_number_gt 2826
# number of observed reflections (> n sig(I))
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'Kappa-CCD Control Software (Nonius, 2001a)'
_computing_cell_refinement 'DENZO (Nonius, 2001b)'
_computing_data_reduction 'DENZO (Nonius, 2001b)'
_computing_structure_solution 'SIR92 (Altomare, 1994)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)'
_computing_molecular_graphics 'PLATON (Spek, 2007)'
_computing_publication_material 'PLATON (Spek, 2007)'
#===================================================================
# 8. REFINEMENT DATA
#===================================================================
_refine_special_details
;
Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^
or flagged by the user for potential systematic errors. Weighted R-factors
wR and all goodnesses of fit S are based on F^2^, conventional R-factors R
are based on F, with F set to zero for negative F^2^. The observed criterion
of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme sigma
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0116P)^2^+1.7030P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method SHELXL
_refine_ls_extinction_coef 0.00071(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns 2963
_refine_ls_number_parameters 229
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0181
_refine_ls_R_factor_gt 0.0164
_refine_ls_wR_factor_ref 0.0407
_refine_ls_wR_factor_gt 0.0401
_refine_ls_goodness_of_fit_ref 1.139
_refine_ls_restrained_S_all 1.139
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full 25.32
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max 0.300
_refine_diff_density_min -0.308
_refine_diff_density_rms 0.060
#===================================================================
# 9. ATOMIC COORDINATES AND THERMAL PARAMETERS
#===================================================================
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_calc_flag
_atom_site_refinement_flags
Mo1 Mo Uani 0.58082(2) 0.32020(1) 0.29920(1) 1.000 0.0164(1) . .
Mo2 Mo Uani 0.25841(2) 0.25148(1) 0.36184(1) 1.000 0.0165(1) . .
S1 S Uani 0.72983(7) 0.18810(4) 0.24391(4) 1.000 0.0212(2) . .
S2 S Uani 0.19903(7) 0.07933(4) 0.33218(4) 1.000 0.0205(2) . .
O1 O Uani 0.5932(2) 0.40730(11) 0.22107(11) 1.000 0.0253(5) . .
O2 O Uani 0.75375(19) 0.33840(11) 0.39312(11) 1.000 0.0227(5) . .
O3 O Uani 0.39587(18) 0.35688(10) 0.34687(10) 1.000 0.0186(4) . .
O4 O Uani 0.06913(19) 0.27569(11) 0.28297(11) 1.000 0.0248(5) . .
O5 O Uani 0.2246(2) 0.26660(12) 0.46999(11) 1.000 0.0262(5) . .
O14 O Uani 0.2884(2) 0.01975(11) 0.07784(11) 1.000 0.0230(5) . .
O18 O Uani 0.37428(18) 0.23756(10) 0.21313(10) 1.000 0.0179(5) . .
O24 O Uani 0.7244(2) -0.03367(11) 0.42720(11) 1.000 0.0235(5) . .
O28 O Uani 0.50561(18) 0.19066(10) 0.40342(10) 1.000 0.0179(4) . .
C11 C Uani 0.5617(3) 0.12177(15) 0.18137(14) 1.000 0.0176(6) . .
C12 C Uani 0.5824(3) 0.03204(16) 0.14290(16) 1.000 0.0232(7) . .
C13 C Uani 0.4452(3) -0.01644(17) 0.09393(16) 1.000 0.0249(7) . .
C15 C Uani 0.2626(3) 0.10502(16) 0.11531(15) 1.000 0.0199(6) . .
C16 C Uani 0.3970(3) 0.15632(15) 0.17044(14) 1.000 0.0165(6) . .
C17 C Uani 0.0834(3) 0.13430(19) 0.08916(17) 1.000 0.0298(8) . .
C21 C Uani 0.3998(3) 0.03373(15) 0.36681(14) 1.000 0.0179(6) . .
C22 C Uani 0.4356(3) -0.06426(16) 0.36036(15) 1.000 0.0230(7) . .
C23 C Uani 0.5968(3) -0.09379(17) 0.38902(16) 1.000 0.0272(7) . .
C25 C Uani 0.6973(3) 0.06145(16) 0.43455(15) 1.000 0.0198(6) . .
C26 C Uani 0.5353(3) 0.09718(15) 0.40144(14) 1.000 0.0164(6) . .
C27 C Uani 0.8506(3) 0.11567(18) 0.48184(17) 1.000 0.0275(8) . .
H121 H Uiso 0.69180 0.00590 0.15130 1.000 0.0280 calc R
H131 H Uiso 0.45930 -0.07810 0.07000 1.000 0.0300 calc R
H171 H Uiso 0.01790 0.09180 0.03940 0.500 0.0450 calc R
H172 H Uiso 0.07350 0.20020 0.06570 0.500 0.0450 calc R
H173 H Uiso 0.04020 0.13020 0.14510 0.500 0.0450 calc R
H174 H Uiso 0.06980 0.18970 0.12740 0.500 0.0450 calc R
H175 H Uiso 0.01430 0.08130 0.10110 0.500 0.0450 calc R
H176 H Uiso 0.04750 0.15130 0.02170 0.500 0.0450 calc R
H221 H Uiso 0.34730 -0.10870 0.33610 1.000 0.0280 calc R
H231 H Uiso 0.62120 -0.15930 0.38210 1.000 0.0330 calc R
H271 H Uiso 0.93620 0.10580 0.44770 1.000 0.0410 calc R
H272 H Uiso 0.89400 0.09340 0.54740 1.000 0.0410 calc R
H273 H Uiso 0.82340 0.18380 0.48170 1.000 0.0410 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.0151(1) 0.0139(1) 0.0198(1) 0.0003(1) 0.0039(1) -0.0023(1)
Mo2 0.0139(1) 0.0152(1) 0.0202(1) 0.0019(1) 0.0043(1) 0.0008(1)
S1 0.0144(3) 0.0229(3) 0.0261(3) -0.0020(2) 0.0051(2) -0.0001(2)
S2 0.0181(3) 0.0186(3) 0.0239(3) 0.0014(2) 0.0043(2) -0.0044(2)
O1 0.0261(9) 0.0224(9) 0.0276(9) 0.0052(7) 0.0079(7) -0.0013(7)
O2 0.0203(8) 0.0206(8) 0.0256(8) -0.0015(7) 0.0034(7) -0.0054(7)
O3 0.0196(8) 0.0128(7) 0.0241(8) -0.0017(6) 0.0069(6) -0.0003(6)
O4 0.0170(8) 0.0234(9) 0.0320(9) 0.0057(7) 0.0034(7) 0.0004(7)
O5 0.0280(9) 0.0266(9) 0.0263(9) 0.0015(7) 0.0113(7) 0.0031(7)
O14 0.0291(9) 0.0191(8) 0.0216(8) -0.0026(6) 0.0085(7) -0.0059(7)
O18 0.0158(8) 0.0169(8) 0.0199(8) -0.0017(6) 0.0029(6) 0.0003(6)
O24 0.0273(9) 0.0222(8) 0.0206(8) 0.0027(6) 0.0061(7) 0.0094(7)
O28 0.0164(8) 0.0137(7) 0.0222(8) 0.0005(6) 0.0027(6) 0.0006(6)
C11 0.0200(11) 0.0184(11) 0.0152(10) 0.0027(8) 0.0063(9) -0.0011(9)
C12 0.0259(13) 0.0202(12) 0.0251(12) 0.0019(9) 0.0097(10) 0.0042(10)
C13 0.0375(14) 0.0168(11) 0.0234(12) -0.0006(9) 0.0136(10) -0.0008(10)
C15 0.0230(12) 0.0206(11) 0.0158(10) 0.0016(9) 0.0048(9) -0.0026(9)
C16 0.0195(11) 0.0157(10) 0.0144(10) 0.0019(8) 0.0049(8) -0.0001(9)
C17 0.0197(12) 0.0396(15) 0.0260(12) -0.0041(11) -0.0008(10) -0.0035(11)
C21 0.0260(12) 0.0180(11) 0.0111(10) 0.0020(8) 0.0076(9) 0.0005(9)
C22 0.0357(14) 0.0166(11) 0.0175(11) -0.0005(9) 0.0088(10) -0.0024(10)
C23 0.0439(15) 0.0164(11) 0.0223(12) 0.0009(9) 0.0109(11) 0.0058(11)
C25 0.0246(12) 0.0200(11) 0.0154(10) 0.0032(9) 0.0067(9) 0.0052(9)
C26 0.0204(11) 0.0170(11) 0.0125(10) 0.0021(8) 0.0058(8) 0.0015(9)
C27 0.0196(12) 0.0313(14) 0.0279(13) 0.0041(10) 0.0002(10) 0.0035(10)
#==================================================================
# 10. MOLECULAR GEOMETRY
#===================================================================
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 S1 2.4755(6) . . yes
Mo1 O1 1.6937(16) . . yes
Mo1 O2 1.7088(16) . . yes
Mo1 O3 1.9135(15) . . yes
Mo1 O18 2.1579(15) . . yes
Mo2 S2 2.4731(6) . . yes
Mo2 O3 1.9094(15) . . yes
Mo2 O4 1.7036(16) . . yes
Mo2 O5 1.6946(16) . . yes
Mo2 O28 2.1393(15) . . yes
S1 C11 1.712(2) . . yes
S2 C21 1.717(3) . . yes
O14 C13 1.349(3) . . yes
O14 C15 1.354(3) . . yes
O18 C16 1.335(3) . . yes
O24 C23 1.344(3) . . yes
O24 C25 1.359(3) . . yes
O28 C26 1.333(3) . . yes
C11 C12 1.406(3) . . no
C11 C16 1.410(4) . . no
C12 C13 1.346(3) . . no
C15 C16 1.381(3) . . no
C15 C17 1.480(4) . . no
C21 C22 1.411(3) . . no
C21 C26 1.409(3) . . no
C22 C23 1.346(4) . . no
C25 C26 1.385(3) . . no
C25 C27 1.475(3) . . no
C12 H121 0.9503 . . no
C13 H131 0.9503 . . no
C17 H171 0.9806 . . no
C17 H172 0.9797 . . no
C17 H173 0.9802 . . no
C17 H174 0.9806 . . no
C17 H175 0.9799 . . no
C17 H176 0.9799 . . no
C22 H221 0.9499 . . no
C23 H231 0.9499 . . no
C27 H271 0.9801 . . no
C27 H272 0.9793 . . no
C27 H273 0.9793 . . no
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1 Mo1 O1 100.93(6) . . . yes
S1 Mo1 O2 89.68(5) . . . yes
S1 Mo1 O3 146.77(5) . . . yes
S1 Mo1 O18 78.01(4) . . . yes
O1 Mo1 O2 104.19(8) . . . yes
O1 Mo1 O3 104.75(7) . . . yes
O1 Mo1 O18 100.07(7) . . . yes
O2 Mo1 O3 103.90(7) . . . yes
O2 Mo1 O18 154.49(6) . . . yes
O3 Mo1 O18 77.03(6) . . . yes
S2 Mo2 O3 145.87(5) . . . yes
S2 Mo2 O4 88.49(5) . . . yes
S2 Mo2 O5 102.15(6) . . . yes
S2 Mo2 O28 77.89(4) . . . yes
O3 Mo2 O4 103.41(7) . . . yes
O3 Mo2 O5 105.39(7) . . . yes
O3 Mo2 O28 77.88(6) . . . yes
O4 Mo2 O5 104.73(8) . . . yes
O4 Mo2 O28 153.93(7) . . . yes
O5 Mo2 O28 99.86(7) . . . yes
Mo1 S1 C11 100.23(8) . . . yes
Mo2 S2 C21 100.44(8) . . . yes
Mo1 O3 Mo2 113.11(7) . . . yes
C13 O14 C15 120.63(19) . . . yes
Mo1 O18 C16 122.71(14) . . . yes
C23 O24 C25 121.26(19) . . . yes
Mo2 O28 C26 123.43(14) . . . yes
S1 C11 C12 121.96(19) . . . yes
S1 C11 C16 119.34(16) . . . yes
C12 C11 C16 118.7(2) . . . no
C11 C12 C13 119.1(2) . . . no
O14 C13 C12 122.1(2) . . . yes
O14 C15 C16 120.3(2) . . . yes
O14 C15 C17 113.3(2) . . . yes
C16 C15 C17 126.4(2) . . . no
O18 C16 C11 119.6(2) . . . yes
O18 C16 C15 121.6(2) . . . yes
C11 C16 C15 118.9(2) . . . no
S2 C21 C22 122.95(18) . . . yes
S2 C21 C26 118.59(17) . . . yes
C22 C21 C26 118.4(2) . . . no
C21 C22 C23 119.0(2) . . . no
O24 C23 C22 122.2(2) . . . yes
O24 C25 C26 119.3(2) . . . yes
O24 C25 C27 113.7(2) . . . yes
C26 C25 C27 126.9(2) . . . no
O28 C26 C21 119.6(2) . . . yes
O28 C26 C25 120.8(2) . . . yes
C21 C26 C25 119.6(2) . . . no
C11 C12 H121 120.47 . . . no
C13 C12 H121 120.38 . . . no
O14 C13 H131 118.99 . . . no
C12 C13 H131 118.95 . . . no
C15 C17 H171 109.46 . . . no
C15 C17 H172 109.45 . . . no
C15 C17 H173 109.46 . . . no
C15 C17 H174 109.46 . . . no
C15 C17 H175 109.45 . . . no
C15 C17 H176 109.48 . . . no
H171 C17 H172 109.52 . . . no
H171 C17 H173 109.45 . . . no
H171 C17 H174 141.08 . . . no
H171 C17 H175 56.22 . . . no
H171 C17 H176 56.27 . . . no
H172 C17 H173 109.49 . . . no
H172 C17 H174 56.25 . . . no
H172 C17 H175 141.10 . . . no
H172 C17 H176 56.27 . . . no
H173 C17 H174 56.26 . . . no
H173 C17 H175 56.25 . . . no
H173 C17 H176 141.06 . . . no
H174 C17 H175 109.49 . . . no
H174 C17 H176 109.48 . . . no
H175 C17 H176 109.46 . . . no
C21 C22 H221 120.53 . . . no
C23 C22 H221 120.49 . . . no
O24 C23 H231 118.92 . . . no
C22 C23 H231 118.90 . . . no
C25 C27 H271 109.45 . . . no
C25 C27 H272 109.48 . . . no
C25 C27 H273 109.46 . . . no
H271 C27 H272 109.49 . . . no
H271 C27 H273 109.44 . . . no
H272 C27 H273 109.52 . . . no
# End of Crystallographic Information File
#===================================================================
data_LISB-4420-173
_database_code_depnum_ccdc_archive 'CCDC 664272'
#===================================================================
#===================================================================
# 5. CHEMICAL DATA
#===================================================================
_chemical_name_systematic
;
;
_chemical_name_common ?
_chemical_formula_moiety 'C12 H10 Mo2 O9 S2'
_chemical_formula_structural ?
_chemical_formula_analytical ?
_chemical_formula_sum 'C12 H10 Mo2 O9 S2'
_chemical_formula_weight 554.22
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
S S 0.1246 0.1234 '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'
Mo Mo -1.6832 0.6857 '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'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
#===================================================================
# 6. CRYSTAL DATA
#===================================================================
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_Hall '-C 2yc'
_symmetry_space_group_name_H-M 'C 2/c'
_symmetry_Int_Tables_number 15
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,y,1/2-z
3 -x,-y,-z
4 x,-y,1/2+z
5 1/2+x,1/2+y,z
6 1/2-x,1/2+y,1/2-z
7 1/2-x,1/2-y,-z
8 1/2+x,1/2-y,1/2+z
_cell_length_a 31.3625(3)
_cell_length_b 8.8600(1)
_cell_length_c 12.3099(1)
_cell_angle_alpha 90
_cell_angle_beta 108.7833(6)
_cell_angle_gamma 90
_cell_volume 3238.40(6)
_cell_formula_units_Z 8
_cell_measurement_temperature 173(1)
_cell_measurement_reflns_used 3170
_cell_measurement_theta_min 1.37
_cell_measurement_theta_max 25.33
_exptl_crystal_description fragment
_exptl_crystal_colour yellow
_exptl_crystal_size_max 0.13
_exptl_crystal_size_mid 0.13
_exptl_crystal_size_min 0.05
_exptl_crystal_density_meas none
_exptl_crystal_density_diffrn 2.273
_exptl_crystal_density_method none
_exptl_crystal_F_000 2160
_exptl_absorpt_coefficient_mu 1.853
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.823
_exptl_absorpt_correction_T_max 0.913
_exptl_absorpt_process_details
'(applied during the scaling procedure; Nonius, 2001b)'
_exptl_special_details
;
Diffractometer operator E. Herdtweck
scanspeed 2 x 30 s per film
repetition 1
dx 40
530 films measured in 9 data sets
set 1: phi-scan with delta_phi = 2.0
set 2 to 9: omega-scans with delta_omega = 2.0
;
_publ_section_exptl_prep
;
The crystal was fixed in a capillary with perfluorinated ether and
transferred to the diffractometer.
;
_publ_section_exptl_refinement
;
Solution and refinements with the program WinGX;
Farrugia (1999).
Hydrogen atoms could be located in the difference Fourier maps
and were allowed to refine freely.
;
#===================================================================
# 7. EXPERIMENTAL DATA
#===================================================================
_diffrn_ambient_temperature 173(1)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_source 'NONIUS FR 591 rotating anode'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device ' \k-geometry diffractometer '
_diffrn_measurement_device_type ' Nonius \k-CCD diffractometer'
_diffrn_measurement_method ' phi- and omega-rotation '
_diffrn_detector ' CCD plate '
_diffrn_detector_area_resol_mean 18 # 9 for binned mode
_diffrn_standards_decay_% 0
# number of measured reflections (redundant set)
_diffrn_reflns_number 37862
_diffrn_reflns_av_R_equivalents 0.044
_diffrn_reflns_av_sigmaI/netI 0.0234
_diffrn_reflns_limit_h_min -37
_diffrn_reflns_limit_h_max 37
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_theta_min 1.37
_diffrn_reflns_theta_max 25.33
_reflns_number_total 2966
_reflns_number_gt 2682
# number of observed reflections (> n sig(I))
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'Kappa-CCD Control Software (Nonius, 2001a)'
_computing_cell_refinement 'DENZO (Nonius, 2001b)'
_computing_data_reduction 'DENZO (Nonius, 2001b)'
_computing_structure_solution 'SIR92 (Altomare, 1994)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)'
_computing_molecular_graphics 'PLATON (Spek, 2007)'
_computing_publication_material 'PLATON (Spek, 2007)'
#===================================================================
# 8. REFINEMENT DATA
#===================================================================
_refine_special_details
;
Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^
or flagged by the user for potential systematic errors. Weighted R-factors
wR and all goodnesses of fit S are based on F^2^, conventional R-factors R
are based on F, with F set to zero for negative F^2^. The observed criterion
of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme sigma
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0167P)^2^+7.8083P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_ls_hydrogen_treatment refall
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 2966
_refine_ls_number_parameters 266
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0255
_refine_ls_R_factor_gt 0.0204
_refine_ls_wR_factor_ref 0.0476
_refine_ls_wR_factor_gt 0.0457
_refine_ls_goodness_of_fit_ref 1.060
_refine_ls_restrained_S_all 1.060
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full 25.33
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max 0.349
_refine_diff_density_min -0.420
_refine_diff_density_rms 0.074
#===================================================================
# 9. ATOMIC COORDINATES AND THERMAL PARAMETERS
#===================================================================
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_calc_flag
_atom_site_refinement_flags
Mo1 Mo Uani 0.08994(1) 0.63263(2) 0.09450(2) 1.000 0.0173(1) . .
Mo2 Mo Uani 0.16212(1) 0.89080(3) 0.17615(2) 1.000 0.0179(1) . .
S1 S Uani 0.06601(2) 0.53501(7) 0.25437(6) 1.000 0.0205(2) . .
S2 S Uani 0.17941(2) 0.94526(7) 0.38286(6) 1.000 0.0206(2) . .
O1 O Uani 0.03943(6) 0.6439(2) -0.01127(16) 1.000 0.0228(6) . .
O2 O Uani 0.10929(6) 0.4571(2) 0.07957(16) 1.000 0.0242(6) . .
O3 O Uani 0.12756(6) 0.7715(2) 0.04878(14) 1.000 0.0201(6) . .
O4 O Uani 0.14268(7) 1.0706(2) 0.14749(16) 1.000 0.0250(6) . .
O5 O Uani 0.21477(6) 0.8975(2) 0.16546(16) 1.000 0.0258(6) . .
O14 O Uani 0.04148(6) 0.9726(2) 0.40490(15) 1.000 0.0212(6) . .
O18 O Uani 0.08452(6) 0.83573(19) 0.18546(14) 1.000 0.0170(5) . .
O24 O Uani 0.19926(6) 0.4754(2) 0.52065(15) 1.000 0.0214(6) . .
O28 O Uani 0.16385(6) 0.6684(2) 0.24900(15) 1.000 0.0192(5) . .
C11 C Uani 0.05681(8) 0.7005(3) 0.3150(2) 1.000 0.0168(8) . .
C12 C Uani 0.03803(9) 0.7067(3) 0.4044(2) 1.000 0.0185(8) . .
C13 C Uani 0.03155(10) 0.8410(3) 0.4464(2) 1.000 0.0230(9) . .
C15 C Uani 0.05928(9) 0.9726(3) 0.3175(2) 1.000 0.0178(8) . .
C16 C Uani 0.06766(8) 0.8382(3) 0.2718(2) 1.000 0.0159(8) . .
C17 C Uani 0.06631(11) 1.1261(3) 0.2795(3) 1.000 0.0222(9) . .
C21 C Uani 0.18762(9) 0.7655(3) 0.4386(2) 1.000 0.0177(8) . .
C22 C Uani 0.20387(9) 0.7361(3) 0.5571(2) 1.000 0.0211(9) . .
C23 C Uani 0.20876(10) 0.5921(3) 0.5932(3) 1.000 0.0239(9) . .
C25 C Uani 0.18371(9) 0.4970(3) 0.4054(2) 1.000 0.0183(8) . .
C26 C Uani 0.17773(9) 0.6419(3) 0.3619(2) 1.000 0.0170(8) . .
C27 C Uani 0.17633(11) 0.3531(3) 0.3417(3) 1.000 0.0232(9) . .
H121 H Uiso 0.0306(9) 0.624(3) 0.430(2) 1.000 0.008(7) . .
H131 H Uiso 0.0186(10) 0.855(3) 0.504(3) 1.000 0.026(8) . .
H171 H Uiso 0.0834(11) 1.127(3) 0.227(3) 1.000 0.039(9) . .
H172 H Uiso 0.0801(11) 1.179(4) 0.338(3) 1.000 0.034(9) . .
H173 H Uiso 0.0373(12) 1.174(4) 0.241(3) 1.000 0.045(10) . .
H221 H Uiso 0.2108(9) 0.806(3) 0.607(2) 1.000 0.012(7) . .
H231 H Uiso 0.2188(9) 0.563(3) 0.666(3) 1.000 0.018(7) . .
H271 H Uiso 0.1617(10) 0.287(3) 0.376(2) 1.000 0.027(8) . .
H272 H Uiso 0.2063(12) 0.314(4) 0.343(3) 1.000 0.041(9) . .
H273 H Uiso 0.1579(11) 0.370(3) 0.262(3) 1.000 0.034(9) . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.0184(1) 0.0173(1) 0.0167(1) -0.0039(1) 0.0063(1) -0.0010(1)
Mo2 0.0194(1) 0.0186(1) 0.0167(1) 0.0008(1) 0.0071(1) -0.0027(1)
S1 0.0250(4) 0.0136(3) 0.0253(4) 0.0001(3) 0.0114(3) -0.0010(3)
S2 0.0254(4) 0.0169(3) 0.0197(3) -0.0027(3) 0.0074(3) -0.0012(3)
O1 0.0203(10) 0.0247(10) 0.0236(10) -0.0043(8) 0.0072(9) 0.0004(8)
O2 0.0227(10) 0.0222(10) 0.0271(10) -0.0075(8) 0.0072(9) 0.0006(8)
O3 0.0214(10) 0.0249(10) 0.0151(9) -0.0009(8) 0.0075(8) -0.0005(8)
O4 0.0283(11) 0.0199(10) 0.0284(11) 0.0035(8) 0.0113(9) -0.0027(8)
O5 0.0221(11) 0.0337(12) 0.0221(10) -0.0004(8) 0.0077(9) -0.0036(9)
O14 0.0259(11) 0.0203(10) 0.0199(10) -0.0002(8) 0.0108(8) 0.0012(8)
O18 0.0202(10) 0.0160(9) 0.0170(9) -0.0019(7) 0.0091(8) -0.0009(8)
O24 0.0221(10) 0.0220(10) 0.0208(10) 0.0020(8) 0.0079(8) -0.0009(8)
O28 0.0240(10) 0.0174(9) 0.0157(9) -0.0002(7) 0.0059(8) -0.0009(8)
C11 0.0142(14) 0.0179(13) 0.0156(13) 0.0015(10) 0.0011(11) 0.0001(11)
C12 0.0169(14) 0.0192(14) 0.0184(14) 0.0068(11) 0.0042(11) 0.0010(11)
C13 0.0234(16) 0.0302(16) 0.0177(14) 0.0027(12) 0.0100(13) 0.0013(12)
C15 0.0168(13) 0.0207(14) 0.0164(13) -0.0003(11) 0.0059(11) -0.0005(11)
C16 0.0151(14) 0.0166(13) 0.0142(13) -0.0004(10) 0.0024(11) -0.0001(10)
C17 0.0295(18) 0.0146(14) 0.0239(16) -0.0025(12) 0.0105(14) -0.0022(13)
C21 0.0152(14) 0.0198(14) 0.0203(13) -0.0005(11) 0.0090(11) -0.0008(11)
C22 0.0195(15) 0.0264(16) 0.0186(14) -0.0059(13) 0.0079(12) -0.0010(12)
C23 0.0196(15) 0.0351(17) 0.0163(15) 0.0026(13) 0.0049(12) 0.0017(13)
C25 0.0172(14) 0.0214(14) 0.0182(14) -0.0007(11) 0.0084(11) -0.0001(11)
C26 0.0133(13) 0.0224(14) 0.0168(14) -0.0007(11) 0.0069(11) -0.0016(11)
C27 0.0253(17) 0.0185(14) 0.0274(17) 0.0027(12) 0.0107(14) -0.0009(12)
#==================================================================
# 10. MOLECULAR GEOMETRY
#===================================================================
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 S1 2.4770(7) . . yes
Mo1 O1 1.6990(19) . . yes
Mo1 O2 1.7007(18) . . yes
Mo1 O3 1.9106(19) . . yes
Mo1 O18 2.1548(17) . . yes
Mo1 O28 2.5003(19) . . yes
Mo2 S2 2.4725(7) . . yes
Mo2 O3 1.9121(17) . . yes
Mo2 O4 1.7016(18) . . yes
Mo2 O5 1.699(2) . . yes
Mo2 O18 2.521(2) . . yes
Mo2 O28 2.1584(18) . . yes
S1 C11 1.711(3) . . yes
S2 C21 1.720(3) . . yes
O14 C13 1.349(3) . . yes
O14 C15 1.362(3) . . yes
O18 C16 1.331(3) . . yes
O24 C23 1.336(4) . . yes
O24 C25 1.357(3) . . yes
O28 C26 1.337(3) . . yes
C11 C12 1.407(4) . . no
C11 C16 1.416(4) . . no
C12 C13 1.339(4) . . no
C15 C16 1.378(4) . . no
C15 C17 1.478(4) . . no
C21 C22 1.406(3) . . no
C21 C26 1.414(4) . . no
C22 C23 1.344(4) . . no
C25 C26 1.380(4) . . no
C25 C27 1.476(4) . . no
C12 H121 0.86(3) . . no
C13 H131 0.93(3) . . no
C17 H171 0.96(4) . . no
C17 H172 0.85(4) . . no
C17 H173 0.98(4) . . no
C22 H221 0.85(3) . . no
C23 H231 0.89(3) . . no
C27 H271 0.93(3) . . no
C27 H272 1.00(4) . . no
C27 H273 0.98(3) . . no
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1 Mo1 O1 100.55(7) . . . yes
S1 Mo1 O2 88.65(7) . . . yes
S1 Mo1 O3 146.38(5) . . . yes
S1 Mo1 O18 77.52(5) . . . yes
S1 Mo1 O28 83.33(5) . . . yes
O1 Mo1 O2 104.36(9) . . . yes
O1 Mo1 O3 104.37(8) . . . yes
O1 Mo1 O18 97.99(8) . . . yes
O1 Mo1 O28 169.35(7) . . . yes
O2 Mo1 O3 106.34(9) . . . yes
O2 Mo1 O18 155.56(8) . . . yes
O2 Mo1 O28 85.55(8) . . . yes
O3 Mo1 O18 76.99(7) . . . yes
O3 Mo1 O28 68.49(7) . . . yes
O18 Mo1 O28 73.01(6) . . . yes
S2 Mo2 O3 146.14(6) . . . yes
S2 Mo2 O4 88.62(7) . . . yes
S2 Mo2 O5 100.16(7) . . . yes
S2 Mo2 O18 83.45(4) . . . yes
S2 Mo2 O28 77.45(5) . . . yes
O3 Mo2 O4 106.07(9) . . . yes
O3 Mo2 O5 105.32(9) . . . yes
O3 Mo2 O18 68.26(7) . . . yes
O3 Mo2 O28 76.57(7) . . . yes
O4 Mo2 O5 104.09(10) . . . yes
O4 Mo2 O18 84.49(9) . . . yes
O4 Mo2 O28 154.19(9) . . . yes
O5 Mo2 O18 170.69(7) . . . yes
O5 Mo2 O28 99.73(8) . . . yes
O18 Mo2 O28 72.53(7) . . . yes
Mo1 S1 C11 100.61(9) . . . yes
Mo2 S2 C21 100.65(8) . . . yes
Mo1 O3 Mo2 110.81(8) . . . yes
C13 O14 C15 120.2(2) . . . yes
Mo1 O18 Mo2 84.21(6) . . . yes
Mo1 O18 C16 123.14(16) . . . yes
Mo2 O18 C16 132.13(15) . . . yes
C23 O24 C25 121.2(2) . . . yes
Mo1 O28 Mo2 84.64(6) . . . yes
Mo1 O28 C26 132.88(17) . . . yes
Mo2 O28 C26 123.27(16) . . . yes
S1 C11 C12 123.1(2) . . . yes
S1 C11 C16 118.68(19) . . . yes
C12 C11 C16 118.2(2) . . . no
C11 C12 C13 119.4(3) . . . no
O14 C13 C12 122.7(2) . . . yes
O14 C15 C16 120.2(2) . . . yes
O14 C15 C17 113.0(2) . . . yes
C16 C15 C17 126.8(3) . . . no
O18 C16 C11 119.4(2) . . . yes
O18 C16 C15 121.2(2) . . . yes
C11 C16 C15 119.4(2) . . . no
S2 C21 C22 122.9(2) . . . yes
S2 C21 C26 118.57(18) . . . yes
C22 C21 C26 118.5(2) . . . no
C21 C22 C23 118.9(3) . . . no
O24 C23 C22 122.5(3) . . . yes
O24 C25 C26 119.7(2) . . . yes
O24 C25 C27 112.1(2) . . . yes
C26 C25 C27 128.2(2) . . . no
O28 C26 C21 119.1(2) . . . yes
O28 C26 C25 121.7(2) . . . yes
C21 C26 C25 119.2(2) . . . no
C11 C12 H121 119.0(18) . . . no
C13 C12 H121 121.6(18) . . . no
O14 C13 H131 112.5(17) . . . no
C12 C13 H131 124.7(17) . . . no
C15 C17 H171 113.1(16) . . . no
C15 C17 H172 109(2) . . . no
C15 C17 H173 110(2) . . . no
H171 C17 H172 109(3) . . . no
H171 C17 H173 108(3) . . . no
H172 C17 H173 108(3) . . . no
C21 C22 H221 122.5(17) . . . no
C23 C22 H221 118.5(17) . . . no
O24 C23 H231 112.4(18) . . . no
C22 C23 H231 125.2(18) . . . no
C25 C27 H271 108.7(16) . . . no
C25 C27 H272 108(2) . . . no
C25 C27 H273 110.0(16) . . . no
H271 C27 H272 112(3) . . . no
H271 C27 H273 110(3) . . . no
H272 C27 H273 109(3) . . . no
# End of Crystallographic Information File