# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
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data_mo_ZL215F2_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1401809'
_audit_update_record
;
2015-05-19 deposited with the CCDC.
2015-10-09 downloaded from the CCDC.
;
_audit_creation_method SHELXL-2013
_chemical_name_systematic
;
Thienyl[2,3-b]thiophenene-2,5-di[(ethoxycarbene)pentacarbonyltungsten(0)
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C22 H12 O12 S2 W2'
_chemical_formula_sum 'C22 H12 O12 S2 W2'
_chemical_formula_weight 900.14
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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 21/c'
_space_group_name_Hall '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 13.1323(5)
_cell_length_b 14.6364(6)
_cell_length_c 13.8925(6)
_cell_angle_alpha 90
_cell_angle_beta 95.4568(11)
_cell_angle_gamma 90
_cell_volume 2658.17(19)
_cell_formula_units_Z 4
_cell_measurement_temperature 150(2)
_cell_measurement_reflns_used 9718
_cell_measurement_theta_min 2.469
_cell_measurement_theta_max 34.985
_exptl_crystal_description parallelopipped
_exptl_crystal_colour red
_exptl_crystal_density_meas .
_exptl_crystal_density_method 'not measured'
_exptl_crystal_density_diffrn 2.249
_exptl_crystal_F_000 1680
_exptl_crystal_size_max 0.218
_exptl_crystal_size_mid 0.063
_exptl_crystal_size_min 0.042
_exptl_absorpt_coefficient_mu 8.865
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.1464
_exptl_absorpt_correction_T_max 0.2720
_exptl_absorpt_process_details SADABS
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 150(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_source ' I\mS micro focus'
_diffrn_radiation_monochromator 'Focusing Montel optics'
_diffrn_measurement_device_type 'Bruker kappa Photon CMOS'
_diffrn_measurement_method '\f and \w scans'
_diffrn_detector_area_resol_mean 10.24
_diffrn_reflns_number 122480
_diffrn_reflns_av_unetI/netI 0.0234
_diffrn_reflns_av_R_equivalents 0.0439
_diffrn_reflns_limit_h_min -21
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_k_max 23
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_theta_min 2.469
_diffrn_reflns_theta_max 35.060
_diffrn_reflns_theta_full 25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total 11750
_reflns_number_gt 9579
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
;
_computing_data_collection 'Bruker APEX2'
_computing_cell_refinement 'Bruker SAINT'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'Bruker SHELXTS (Sheldrick, 2014)'
_computing_structure_refinement Bruker
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 1997), POV-RAY (Cason, 2004),
Mercury (Macrae et al., 2008)
;
_computing_publication_material 'SHELXL-2014, PLATON (Spek, 2009)'
_refine_special_details
;
?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0219P)^2^+4.4584P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary intrinsic-phasing
_atom_sites_solution_secondary .
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_number_reflns 11750
_refine_ls_number_parameters 345
_refine_ls_number_restraints 315
_refine_ls_R_factor_all 0.0407
_refine_ls_R_factor_gt 0.0252
_refine_ls_wR_factor_ref 0.0556
_refine_ls_wR_factor_gt 0.0503
_refine_ls_goodness_of_fit_ref 1.040
_refine_ls_restrained_S_all 1.028
_refine_ls_shift/su_max 0.004
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 2.470
_refine_diff_density_min -0.972
_refine_diff_density_rms 0.169
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 1.07619(2) 0.49418(2) 0.30777(2) 0.01784(2) Uani 1 1 d . U . . .
C1 C 1.12028(19) 0.56534(18) 0.4289(2) 0.0222(5) Uani 1 1 d . U . . .
O1 O 1.14349(17) 0.60185(15) 0.50110(15) 0.0295(4) Uani 1 1 d . U . . .
C2 C 1.2275(2) 0.4737(2) 0.2898(2) 0.0259(5) Uani 1 1 d . U . . .
O2 O 1.31307(16) 0.4678(2) 0.28291(17) 0.0405(6) Uani 1 1 d . U . . .
C3 C 1.0752(2) 0.37997(19) 0.3938(2) 0.0256(5) Uani 1 1 d . U . . .
O3 O 1.0763(2) 0.31775(16) 0.44249(19) 0.0414(6) Uani 1 1 d . U . . .
C4 C 0.9307(2) 0.5316(2) 0.3293(2) 0.0268(5) Uani 1 1 d . U . . .
O4 O 0.85107(17) 0.55682(18) 0.3417(2) 0.0433(6) Uani 1 1 d . U . . .
C5 C 1.0756(2) 0.60439(19) 0.2177(2) 0.0260(5) Uani 1 1 d . U . . .
O5 O 1.0719(2) 0.66362(16) 0.16462(17) 0.0407(6) Uani 1 1 d . U . . .
C6 C 1.01487(18) 0.40991(17) 0.18486(18) 0.0189(4) Uani 1 1 d . U . . .
O6 O 1.04952(14) 0.39779(14) 0.09921(14) 0.0253(4) Uani 1 1 d . U . . .
W2 W 0.45622(2) 0.16447(2) 0.35752(2) 0.02049(3) Uani 1 1 d . U . . .
C7 C 0.4121(2) 0.1670(2) 0.4933(2) 0.0327(6) Uani 1 1 d . U . . .
O7 O 0.3894(2) 0.1691(2) 0.57086(19) 0.0540(8) Uani 1 1 d . U . . .
C8 C 0.4070(2) 0.0322(2) 0.3454(2) 0.0315(6) Uani 1 1 d . U . . .
O8 O 0.3789(2) -0.04148(18) 0.3433(2) 0.0531(7) Uani 1 1 d . U . . .
C9 C 0.5947(2) 0.1137(2) 0.4113(2) 0.0269(5) Uani 1 1 d . U . . .
O9 O 0.67141(18) 0.08330(18) 0.43970(18) 0.0406(5) Uani 1 1 d . U . . .
C10 C 0.4998(2) 0.2983(2) 0.3703(2) 0.0252(5) Uani 1 1 d . U . . .
O10 O 0.52340(18) 0.37295(16) 0.37551(18) 0.0374(5) Uani 1 1 d . U . . .
C11 C 0.3141(2) 0.2106(2) 0.3058(2) 0.0314(6) Uani 1 1 d . U . . .
O11 O 0.23450(18) 0.2370(2) 0.2810(2) 0.0504(7) Uani 1 1 d . U . . .
C12 C 0.51977(18) 0.16682(17) 0.21685(18) 0.0189(4) Uani 1 1 d . U . . .
O12 O 0.48215(13) 0.13319(14) 0.13293(13) 0.0229(4) Uani 1 1 d . U . . .
S1 S 0.86859(5) 0.31059(5) 0.07111(5) 0.02373(12) Uani 1 1 d . U . . .
S2 S 0.65991(5) 0.20860(5) 0.08461(5) 0.02214(12) Uani 1 1 d . U . . .
C13 C 0.91898(17) 0.35910(17) 0.18187(17) 0.0180(4) Uani 1 1 d . U . . .
C14 C 0.85839(18) 0.34210(17) 0.25456(18) 0.0200(4) Uani 1 1 d . U . . .
H14 H 0.8735 0.3629 0.3191 0.024 Uiso 1 1 calc R U . . .
C15 C 0.77074(17) 0.29003(17) 0.22309(17) 0.0175(4) Uani 1 1 d . U . . .
C16 C 0.76620(18) 0.26964(17) 0.12511(18) 0.0191(4) Uani 1 1 d . U . . .
C17 C 0.68615(18) 0.25402(18) 0.26613(18) 0.0198(4) Uani 1 1 d . U . . .
H17 H 0.6774 0.2601 0.3329 0.024 Uiso 1 1 calc R U . . .
C18 C 0.61754(18) 0.20915(17) 0.20131(17) 0.0182(4) Uani 1 1 d . U . . .
C19 C 1.1453(2) 0.4365(2) 0.0745(2) 0.0303(6) Uani 1 1 d . U . . .
H19A H 1.2037 0.4070 0.1128 0.036 Uiso 1 1 calc R U . . .
H19B H 1.1474 0.5029 0.0884 0.036 Uiso 1 1 calc R U . . .
C20 C 1.1513(2) 0.4200(2) -0.0312(2) 0.0280(6) Uani 1 1 d . U . . .
H20A H 1.0947 0.4516 -0.0684 0.042 Uiso 1 1 calc R U . . .
H20B H 1.1467 0.3543 -0.0444 0.042 Uiso 1 1 calc R U . . .
H20C H 1.2165 0.4434 -0.0499 0.042 Uiso 1 1 calc R U . . .
C21 C 0.3823(2) 0.0885(2) 0.1234(2) 0.0294(6) Uani 1 1 d . U . . .
H21A H 0.3304 0.1289 0.1484 0.035 Uiso 1 1 calc R U . . .
H21B H 0.3853 0.0310 0.1611 0.035 Uiso 1 1 calc R U . . .
C22 C 0.3539(2) 0.0686(3) 0.0189(2) 0.0368(7) Uani 1 1 d . U . . .
H22A H 0.3454 0.1262 -0.0170 0.055 Uiso 1 1 calc R U . . .
H22B H 0.2896 0.0343 0.0117 0.055 Uiso 1 1 calc R U . . .
H22C H 0.4081 0.0323 -0.0065 0.055 Uiso 1 1 calc R U . . .
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
W1 0.01343(4) 0.01821(4) 0.02177(5) -0.00011(3) 0.00112(3) -0.00156(3)
C1 0.0190(11) 0.0222(11) 0.0256(12) 0.0032(9) 0.0040(9) -0.0004(9)
O1 0.0354(11) 0.0298(10) 0.0237(9) -0.0028(8) 0.0039(8) -0.0030(9)
C2 0.0213(11) 0.0333(14) 0.0226(12) -0.0008(10) -0.0007(9) -0.0013(10)
O2 0.0180(9) 0.0681(17) 0.0353(12) -0.0028(12) 0.0025(8) 0.0022(10)
C3 0.0222(12) 0.0249(12) 0.0294(13) -0.0011(10) 0.0014(10) -0.0009(9)
O3 0.0473(14) 0.0291(11) 0.0475(14) 0.0126(10) 0.0030(11) 0.0010(10)
C4 0.0219(11) 0.0246(12) 0.0341(14) 0.0014(11) 0.0034(10) 0.0011(10)
O4 0.0258(11) 0.0433(14) 0.0627(17) 0.0068(12) 0.0134(10) 0.0102(10)
C5 0.0277(13) 0.0236(12) 0.0260(12) -0.0036(10) -0.0016(10) -0.0052(10)
O5 0.0586(16) 0.0277(11) 0.0338(12) 0.0042(9) -0.0054(11) -0.0089(10)
C6 0.0147(9) 0.0182(10) 0.0240(11) 0.0010(8) 0.0028(8) -0.0014(8)
O6 0.0184(8) 0.0327(10) 0.0260(9) -0.0061(8) 0.0079(7) -0.0100(7)
W2 0.01675(4) 0.02447(5) 0.02094(5) -0.00188(4) 0.00538(3) -0.00482(3)
C7 0.0283(13) 0.0411(17) 0.0299(13) -0.0061(12) 0.0093(11) -0.0125(12)
O7 0.0554(16) 0.078(2) 0.0318(12) -0.0131(13) 0.0197(11) -0.0263(15)
C8 0.0359(15) 0.0345(14) 0.0250(13) 0.0010(11) 0.0070(11) -0.0119(12)
O8 0.078(2) 0.0381(14) 0.0441(15) -0.0003(11) 0.0104(14) -0.0308(14)
C9 0.0285(13) 0.0270(13) 0.0257(13) 0.0004(10) 0.0045(10) -0.0025(10)
O9 0.0341(12) 0.0450(14) 0.0414(13) 0.0033(11) -0.0028(10) 0.0090(10)
C10 0.0189(11) 0.0288(13) 0.0285(13) -0.0039(10) 0.0054(9) -0.0010(9)
O10 0.0363(12) 0.0274(11) 0.0492(14) -0.0056(10) 0.0078(10) -0.0032(9)
C11 0.0220(12) 0.0362(15) 0.0367(15) -0.0110(12) 0.0074(11) -0.0029(11)
O11 0.0247(11) 0.0607(18) 0.0651(18) -0.0138(14) 0.0008(11) 0.0088(11)
C12 0.0151(9) 0.0189(10) 0.0226(10) -0.0011(8) 0.0010(8) -0.0014(8)
O12 0.0155(8) 0.0309(10) 0.0223(8) -0.0038(7) 0.0025(6) -0.0073(7)
S1 0.0196(3) 0.0318(3) 0.0206(3) -0.0035(2) 0.0062(2) -0.0098(2)
S2 0.0173(3) 0.0305(3) 0.0187(3) -0.0030(2) 0.0024(2) -0.0083(2)
C13 0.0127(9) 0.0215(11) 0.0196(10) -0.0025(8) 0.0006(7) -0.0031(8)
C14 0.0164(10) 0.0218(11) 0.0217(11) -0.0010(9) 0.0006(8) -0.0039(8)
C15 0.0130(9) 0.0211(10) 0.0186(10) 0.0010(8) 0.0021(7) -0.0023(8)
C16 0.0155(9) 0.0226(11) 0.0192(10) 0.0003(8) 0.0020(8) -0.0041(8)
C17 0.0156(10) 0.0256(12) 0.0184(10) 0.0008(9) 0.0022(8) -0.0042(8)
C18 0.0148(9) 0.0207(10) 0.0192(10) 0.0009(8) 0.0018(8) -0.0026(8)
C19 0.0205(12) 0.0410(16) 0.0307(14) -0.0087(12) 0.0099(10) -0.0140(11)
C20 0.0231(12) 0.0339(14) 0.0282(13) -0.0030(11) 0.0082(10) -0.0056(11)
C21 0.0205(12) 0.0405(16) 0.0273(13) -0.0064(11) 0.0035(10) -0.0151(11)
C22 0.0268(14) 0.055(2) 0.0277(14) -0.0044(13) -0.0007(11) -0.0187(14)
_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
W1 C1 2.017(3) . ?
W1 C4 2.036(3) . ?
W1 C5 2.041(3) . ?
W1 C2 2.049(3) . ?
W1 C3 2.055(3) . ?
W1 C6 2.196(3) . ?
C1 O1 1.151(3) . ?
C2 O2 1.140(3) . ?
C3 O3 1.134(4) . ?
C4 O4 1.138(3) . ?
C5 O5 1.136(4) . ?
C6 O6 1.326(3) . ?
C6 C13 1.460(3) . ?
O6 C19 1.451(3) . ?
W2 C7 2.026(3) . ?
W2 C9 2.040(3) . ?
W2 C10 2.043(3) . ?
W2 C8 2.043(3) . ?
W2 C11 2.050(3) . ?
W2 C12 2.197(2) . ?
C7 O7 1.145(4) . ?
C8 O8 1.139(4) . ?
C9 O9 1.137(4) . ?
C10 O10 1.136(4) . ?
C11 O11 1.137(4) . ?
C12 O12 1.318(3) . ?
C12 C18 1.460(3) . ?
O12 C21 1.460(3) . ?
S1 C16 1.709(2) . ?
S1 C13 1.765(2) . ?
S2 C16 1.707(2) . ?
S2 C18 1.763(2) . ?
C13 C14 1.367(3) . ?
C14 C15 1.415(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.389(3) . ?
C15 C17 1.413(3) . ?
C17 C18 1.378(3) . ?
C17 H17 0.9500 . ?
C19 C20 1.497(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.492(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
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
C1 W1 C4 86.40(11) . . ?
C1 W1 C5 95.02(10) . . ?
C4 W1 C5 85.92(12) . . ?
C1 W1 C2 88.43(11) . . ?
C4 W1 C2 172.63(12) . . ?
C5 W1 C2 89.31(12) . . ?
C1 W1 C3 87.25(11) . . ?
C4 W1 C3 94.33(11) . . ?
C5 W1 C3 177.72(11) . . ?
C2 W1 C3 90.66(11) . . ?
C1 W1 C6 173.59(9) . . ?
C4 W1 C6 89.18(11) . . ?
C5 W1 C6 89.28(10) . . ?
C2 W1 C6 96.38(10) . . ?
C3 W1 C6 88.46(10) . . ?
O1 C1 W1 176.1(2) . . ?
O2 C2 W1 175.4(3) . . ?
O3 C3 W1 178.5(3) . . ?
O4 C4 W1 176.7(3) . . ?
O5 C5 W1 176.7(2) . . ?
O6 C6 C13 106.0(2) . . ?
O6 C6 W1 129.88(17) . . ?
C13 C6 W1 124.04(17) . . ?
C6 O6 C19 122.7(2) . . ?
C7 W2 C9 89.37(12) . . ?
C7 W2 C10 90.25(12) . . ?
C9 W2 C10 94.87(11) . . ?
C7 W2 C8 88.70(12) . . ?
C9 W2 C8 87.08(13) . . ?
C10 W2 C8 177.78(12) . . ?
C7 W2 C11 89.39(13) . . ?
C9 W2 C11 177.51(12) . . ?
C10 W2 C11 87.30(12) . . ?
C8 W2 C11 90.73(13) . . ?
C7 W2 C12 173.99(10) . . ?
C9 W2 C12 86.04(10) . . ?
C10 W2 C12 86.29(10) . . ?
C8 W2 C12 94.92(10) . . ?
C11 W2 C12 95.34(11) . . ?
O7 C7 W2 178.4(3) . . ?
O8 C8 W2 176.8(3) . . ?
O9 C9 W2 178.1(3) . . ?
O10 C10 W2 178.6(3) . . ?
O11 C11 W2 177.1(3) . . ?
O12 C12 C18 106.8(2) . . ?
O12 C12 W2 129.72(17) . . ?
C18 C12 W2 123.50(17) . . ?
C12 O12 C21 120.4(2) . . ?
C16 S1 C13 90.22(12) . . ?
C16 S2 C18 90.82(11) . . ?
C14 C13 C6 129.3(2) . . ?
C14 C13 S1 111.99(17) . . ?
C6 C13 S1 118.73(18) . . ?
C13 C14 C15 112.5(2) . . ?
C13 C14 H14 123.7 . . ?
C15 C14 H14 123.7 . . ?
C16 C15 C17 111.9(2) . . ?
C16 C15 C14 112.1(2) . . ?
C17 C15 C14 136.0(2) . . ?
C15 C16 S2 113.14(18) . . ?
C15 C16 S1 113.10(18) . . ?
S2 C16 S1 133.76(15) . . ?
C18 C17 C15 113.1(2) . . ?
C18 C17 H17 123.4 . . ?
C15 C17 H17 123.4 . . ?
C17 C18 C12 129.4(2) . . ?
C17 C18 S2 111.04(17) . . ?
C12 C18 S2 119.53(18) . . ?
O6 C19 C20 107.3(2) . . ?
O6 C19 H19A 110.3 . . ?
C20 C19 H19A 110.3 . . ?
O6 C19 H19B 110.3 . . ?
C20 C19 H19B 110.3 . . ?
H19A C19 H19B 108.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O12 C21 C22 108.4(2) . . ?
O12 C21 H21A 110.0 . . ?
C22 C21 H21A 110.0 . . ?
O12 C21 H21B 110.0 . . ?
C22 C21 H21B 110.0 . . ?
H21A C21 H21B 108.4 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C13 C6 O6 C19 -178.7(2) . . . . ?
W1 C6 O6 C19 5.0(4) . . . . ?
C18 C12 O12 C21 -178.0(2) . . . . ?
W2 C12 O12 C21 2.0(4) . . . . ?
O6 C6 C13 C14 172.8(3) . . . . ?
W1 C6 C13 C14 -10.6(4) . . . . ?
O6 C6 C13 S1 -7.3(3) . . . . ?
W1 C6 C13 S1 169.24(13) . . . . ?
C16 S1 C13 C14 0.7(2) . . . . ?
C16 S1 C13 C6 -179.2(2) . . . . ?
C6 C13 C14 C15 179.9(2) . . . . ?
S1 C13 C14 C15 0.0(3) . . . . ?
C13 C14 C15 C16 -0.9(3) . . . . ?
C13 C14 C15 C17 179.6(3) . . . . ?
C17 C15 C16 S2 0.7(3) . . . . ?
C14 C15 C16 S2 -178.86(18) . . . . ?
C17 C15 C16 S1 -178.96(18) . . . . ?
C14 C15 C16 S1 1.4(3) . . . . ?
C18 S2 C16 C15 0.1(2) . . . . ?
C18 S2 C16 S1 179.7(2) . . . . ?
C13 S1 C16 C15 -1.2(2) . . . . ?
C13 S1 C16 S2 179.2(2) . . . . ?
C16 C15 C17 C18 -1.5(3) . . . . ?
C14 C15 C17 C18 177.9(3) . . . . ?
C15 C17 C18 C12 -177.0(2) . . . . ?
C15 C17 C18 S2 1.6(3) . . . . ?
O12 C12 C18 C17 179.6(3) . . . . ?
W2 C12 C18 C17 -0.4(4) . . . . ?
O12 C12 C18 S2 1.1(3) . . . . ?
W2 C12 C18 S2 -178.91(12) . . . . ?
C16 S2 C18 C17 -1.0(2) . . . . ?
C16 S2 C18 C12 177.8(2) . . . . ?
C6 O6 C19 C20 -172.0(2) . . . . ?
C12 O12 C21 C22 172.7(3) . . . . ?
_shelxl_version_number 2013-4
_shelx_res_file
;
REM Solution 1 R1 0.071 Rweak 0.003, Alpha = 0.0267 in P2(1)/c
REM Formula: C22 O12 S2 W2
TITL mo_ZL215F2_0m in P2(1)/c
CELL 0.71073 13.1323 14.6364 13.8925 90.0000 95.4568 90.0000
ZERR 4.00 0.0005 0.0006 0.0006 0.0000 0.0011 0.0000
LATT 1
SYMM -X, 1/2+Y, 1/2-Z
SFAC C H O S W
UNIT 88 48 48 8 8
TEMP -123.00
SIZE 0.042 0.063 0.218
L.S. 16
BOND $H
CONF
ACTA
FMAP 2
PLAN 20
RIGU
WGHT 0.021900 4.458400
FVAR 0.05962
W1 5 1.076186 0.494178 0.307773 11.00000 0.01343 0.01821 =
0.02177 -0.00011 0.00112 -0.00156
C1 1 1.120280 0.565336 0.428934 11.00000 0.01904 0.02225 =
0.02564 0.00320 0.00400 -0.00035
O1 3 1.143487 0.601853 0.501098 11.00000 0.03540 0.02976 =
0.02369 -0.00277 0.00389 -0.00296
C2 1 1.227532 0.473672 0.289793 11.00000 0.02127 0.03329 =
0.02256 -0.00077 -0.00067 -0.00132
O2 3 1.313065 0.467761 0.282910 11.00000 0.01802 0.06813 =
0.03533 -0.00276 0.00252 0.00223
C3 1 1.075197 0.379971 0.393769 11.00000 0.02217 0.02490 =
0.02945 -0.00113 0.00141 -0.00091
O3 3 1.076279 0.317753 0.442495 11.00000 0.04735 0.02907 =
0.04749 0.01260 0.00302 0.00101
C4 1 0.930746 0.531605 0.329316 11.00000 0.02187 0.02464 =
0.03407 0.00143 0.00336 0.00112
O4 3 0.851074 0.556825 0.341715 11.00000 0.02576 0.04328 =
0.06274 0.00679 0.01342 0.01016
C5 1 1.075630 0.604386 0.217703 11.00000 0.02774 0.02355 =
0.02597 -0.00359 -0.00160 -0.00520
O5 3 1.071943 0.663620 0.164617 11.00000 0.05857 0.02769 =
0.03383 0.00416 -0.00540 -0.00889
C6 1 1.014869 0.409911 0.184856 11.00000 0.01472 0.01815 =
0.02397 0.00104 0.00281 -0.00137
O6 3 1.049520 0.397795 0.099205 11.00000 0.01840 0.03268 =
0.02595 -0.00614 0.00793 -0.00995
W2 5 0.456219 0.164473 0.357524 11.00000 0.01675 0.02447 =
0.02094 -0.00188 0.00538 -0.00482
C7 1 0.412126 0.166971 0.493325 11.00000 0.02829 0.04107 =
0.02987 -0.00608 0.00933 -0.01247
O7 3 0.389395 0.169080 0.570865 11.00000 0.05539 0.07782 =
0.03178 -0.01311 0.01968 -0.02626
C8 1 0.406962 0.032183 0.345436 11.00000 0.03588 0.03448 =
0.02502 0.00100 0.00701 -0.01194
O8 3 0.378935 -0.041475 0.343254 11.00000 0.07807 0.03810 =
0.04412 -0.00034 0.01037 -0.03076
C9 1 0.594723 0.113680 0.411348 11.00000 0.02852 0.02697 =
0.02566 0.00039 0.00451 -0.00250
O9 3 0.671411 0.083298 0.439700 11.00000 0.03407 0.04496 =
0.04141 0.00329 -0.00281 0.00900
C10 1 0.499800 0.298283 0.370299 11.00000 0.01892 0.02883 =
0.02850 -0.00390 0.00545 -0.00102
O10 3 0.523398 0.372953 0.375509 11.00000 0.03626 0.02739 =
0.04923 -0.00560 0.00779 -0.00320
C11 1 0.314110 0.210610 0.305771 11.00000 0.02201 0.03624 =
0.03675 -0.01095 0.00741 -0.00293
O11 3 0.234501 0.237038 0.281042 11.00000 0.02471 0.06070 =
0.06512 -0.01375 0.00084 0.00877
C12 1 0.519772 0.166821 0.216852 11.00000 0.01513 0.01888 =
0.02263 -0.00113 0.00098 -0.00136
O12 3 0.482150 0.133191 0.132930 11.00000 0.01550 0.03092 =
0.02229 -0.00377 0.00254 -0.00730
S1 4 0.868590 0.310586 0.071114 11.00000 0.01961 0.03183 =
0.02059 -0.00352 0.00622 -0.00977
S2 4 0.659914 0.208602 0.084612 11.00000 0.01731 0.03047 =
0.01875 -0.00297 0.00237 -0.00828
C13 1 0.918981 0.359105 0.181866 11.00000 0.01265 0.02147 =
0.01962 -0.00252 0.00063 -0.00314
C14 1 0.858393 0.342100 0.254562 11.00000 0.01641 0.02178 =
0.02172 -0.00103 0.00059 -0.00391
AFIX 43
H14 2 0.873474 0.362946 0.319103 11.00000 -1.20000
AFIX 0
C15 1 0.770745 0.290033 0.223091 11.00000 0.01298 0.02107 =
0.01857 0.00100 0.00209 -0.00235
C16 1 0.766197 0.269639 0.125111 11.00000 0.01551 0.02258 =
0.01917 0.00028 0.00200 -0.00414
C17 1 0.686151 0.254017 0.266132 11.00000 0.01563 0.02560 =
0.01843 0.00080 0.00222 -0.00418
AFIX 43
H17 2 0.677446 0.260102 0.332936 11.00000 -1.20000
AFIX 0
C18 1 0.617535 0.209149 0.201311 11.00000 0.01485 0.02075 =
0.01916 0.00093 0.00180 -0.00257
C19 1 1.145320 0.436537 0.074490 11.00000 0.02050 0.04102 =
0.03068 -0.00873 0.00987 -0.01401
AFIX 23
H19A 2 1.203674 0.406978 0.112799 11.00000 -1.20000
H19B 2 1.147450 0.502887 0.088387 11.00000 -1.20000
AFIX 0
C20 1 1.151325 0.420034 -0.031174 11.00000 0.02312 0.03391 =
0.02817 -0.00295 0.00820 -0.00565
AFIX 137
H20A 2 1.094716 0.451596 -0.068401 11.00000 -1.50000
H20B 2 1.146664 0.354313 -0.044351 11.00000 -1.50000
H20C 2 1.216527 0.443390 -0.049937 11.00000 -1.50000
AFIX 0
C21 1 0.382281 0.088490 0.123360 11.00000 0.02050 0.04054 =
0.02726 -0.00637 0.00351 -0.01510
AFIX 23
H21A 2 0.330413 0.128881 0.148449 11.00000 -1.20000
H21B 2 0.385281 0.030998 0.161065 11.00000 -1.20000
AFIX 0
C22 1 0.353930 0.068608 0.018943 11.00000 0.02676 0.05522 =
0.02772 -0.00439 -0.00071 -0.01872
AFIX 137
H22A 2 0.345448 0.126157 -0.016980 11.00000 -1.50000
H22B 2 0.289602 0.034257 0.011671 11.00000 -1.50000
H22C 2 0.408115 0.032345 -0.006467 11.00000 -1.50000
AFIX 0
HKLF 4
REM mo_ZL215F2_0m in P2(1)/c
REM R1 = 0.0252 for 9579 Fo > 4sig(Fo) and 0.0407 for all 11750 data
REM 345 parameters refined using 315 restraints
END
WGHT 0.0214 4.4944
REM Highest difference peak 2.470, deepest hole -0.972, 1-sigma level 0.169
Q1 1 0.4817 0.1206 0.3370 11.00000 0.05 2.47
Q2 1 0.4545 -0.1695 0.3596 11.00000 0.05 1.86
Q3 1 0.8358 0.4912 0.4089 11.00000 0.05 1.79
Q4 1 0.9245 0.6791 0.1911 11.00000 0.05 1.74
Q5 1 0.6957 0.1649 0.2589 11.00000 0.05 1.69
Q6 1 1.0780 0.5234 0.3075 11.00000 0.05 1.64
Q7 1 1.0510 0.4991 0.3436 11.00000 0.05 1.47
Q8 1 1.0109 0.4885 -0.0215 11.00000 0.05 1.35
Q9 1 0.4360 0.1930 0.3157 11.00000 0.05 1.33
Q10 1 0.3911 0.1615 0.0316 11.00000 0.05 1.27
Q11 1 1.0624 0.4896 0.2768 11.00000 0.05 1.25
Q12 1 1.0970 0.4843 0.3249 11.00000 0.05 1.08
Q13 1 1.1466 0.4532 0.3180 11.00000 0.05 1.07
Q14 1 1.1079 0.5390 0.3628 11.00000 0.05 1.07
Q15 1 0.4896 0.1269 0.4055 11.00000 0.05 1.06
Q16 1 0.6084 0.1666 -0.0265 11.00000 0.05 1.06
Q17 1 0.4366 0.1205 0.3048 11.00000 0.05 1.02
Q18 1 0.4348 0.2230 0.3648 11.00000 0.05 0.95
Q19 1 1.1623 0.6808 0.0884 11.00000 0.05 0.93
Q20 1 0.5115 0.2217 0.3726 11.00000 0.05 0.92
;
_shelx_res_checksum 84962
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane, DCM'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_mo_ZL220F22_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1401810'
_audit_update_record
;
2015-05-19 deposited with the CCDC.
2015-10-09 downloaded from the CCDC.
;
_audit_creation_method SHELXL-2014
_chemical_name_systematic
'Thienyl[2,3-b]thiophenene-2,5-di[(ethoxycarbene)pentacarbonylchromium(0)], Thienyl[2,3-b]thiophenene-2-[(ethoxycarbene)pentacarbonylchromium(0)]-5-[(ethoxycarbene)pentacarbonyltungsten(0)] co-crystal'
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety
'0.38(C22 H12 Cr2 O12 S2), 0.62(C22 H12 Cr O12 S2 W)'
_chemical_formula_sum 'C22 H12 Cr1.38 O12 S2 W0.62'
_chemical_formula_weight 717.85
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'
Cr Cr 0.3209 0.6236 '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'
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 21/c'
_space_group_name_Hall '-P 2ybc'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 13.0556(8)
_cell_length_b 14.5145(10)
_cell_length_c 13.8325(9)
_cell_angle_alpha 90
_cell_angle_beta 95.3950(18)
_cell_angle_gamma 90
_cell_volume 2609.6(3)
_cell_formula_units_Z 4
_cell_measurement_temperature 150(2)
_cell_measurement_reflns_used 9529
_cell_measurement_theta_min 2.485
_cell_measurement_theta_max 28.357
_exptl_crystal_description needle
_exptl_crystal_colour purple
_exptl_crystal_density_meas .
_exptl_crystal_density_method 'not measured'
_exptl_crystal_density_diffrn 1.827
_exptl_crystal_F_000 1404
_exptl_crystal_size_max 0.298
_exptl_crystal_size_mid 0.081
_exptl_crystal_size_min 0.057
_exptl_absorpt_coefficient_mu 3.517
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.5058
_exptl_absorpt_correction_T_max 0.7457
_exptl_absorpt_process_details SADABS
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 150(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_source ' I\mS micro focus'
_diffrn_radiation_monochromator 'Focusing Montel optics'
_diffrn_measurement_device_type 'Bruker kappa Photon CMOS'
_diffrn_measurement_method '\f and \w scans'
_diffrn_detector_area_resol_mean 10.24
_diffrn_reflns_number 98242
_diffrn_reflns_av_unetI/netI 0.0200
_diffrn_reflns_av_R_equivalents 0.0498
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_theta_min 2.485
_diffrn_reflns_theta_max 28.363
_diffrn_reflns_theta_full 25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total 6523
_reflns_number_gt 5789
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
;
_computing_data_collection 'Bruker APEX2'
_computing_cell_refinement 'Bruker SAINT'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'Bruker SHELXTS (Sheldrick, 2014)'
_computing_structure_refinement Bruker
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 1997), POV-RAY (Cason, 2004),
Mercury (Macrae et al., 2008)
;
_computing_publication_material 'SHELXL-2014, PLATON (Spek, 2009)'
_refine_special_details
;
?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0206P)^2^+4.0832P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary intrinsic-phasing
_atom_sites_solution_secondary .
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_number_reflns 6523
_refine_ls_number_parameters 347
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0344
_refine_ls_R_factor_gt 0.0271
_refine_ls_wR_factor_ref 0.0659
_refine_ls_wR_factor_gt 0.0626
_refine_ls_goodness_of_fit_ref 1.152
_refine_ls_restrained_S_all 1.152
_refine_ls_shift/su_max 0.004
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.606
_refine_diff_density_min -0.491
_refine_diff_density_rms 0.096
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 1.07717(2) 0.49381(2) 0.30742(2) 0.01723(7) Uani 0.6799(13) 1 d . . P .
.
W1 W 1.07717(2) 0.49381(2) 0.30742(2) 0.01723(7) Uani 0.3201(13) 1 d . . P . .
C1 C 1.1186(2) 0.56209(18) 0.4227(2) 0.0254(5) Uani 1 1 d . . . . .
O1 O 1.14058(16) 0.59903(14) 0.49475(15) 0.0339(5) Uani 1 1 d . . . . .
C2 C 1.2216(2) 0.4734(2) 0.2904(2) 0.0284(6) Uani 1 1 d . . . . .
O2 O 1.30767(16) 0.46759(18) 0.28530(16) 0.0439(6) Uani 1 1 d . . . . .
C3 C 1.0747(2) 0.38253(19) 0.3888(2) 0.0270(6) Uani 1 1 d . . . . .
O3 O 1.07629(18) 0.31970(15) 0.43717(18) 0.0420(5) Uani 1 1 d . . . . .
C4 C 0.9363(2) 0.53008(19) 0.3283(2) 0.0282(6) Uani 1 1 d . . . . .
O4 O 0.85801(16) 0.55777(16) 0.34188(19) 0.0443(6) Uani 1 1 d . . . . .
C5 C 1.0757(2) 0.59874(19) 0.2198(2) 0.0278(6) Uani 1 1 d . . . . .
O5 O 1.07247(19) 0.65891(15) 0.16680(17) 0.0417(5) Uani 1 1 d . . . . .
C6 C 1.01666(18) 0.41155(17) 0.18874(18) 0.0200(5) Uani 1 1 d . . . . .
O6 O 1.05113(13) 0.39813(13) 0.10275(14) 0.0266(4) Uani 1 1 d . . . . .
Cr2 Cr 0.45611(2) 0.16382(2) 0.35822(2) 0.01916(8) Uani 0.7027(13) 1 d . . P .
.
W2 W 0.45611(2) 0.16382(2) 0.35822(2) 0.01916(8) Uani 0.2973(13) 1 d . . P . .
C7 C 0.4157(2) 0.1653(2) 0.4879(2) 0.0370(7) Uani 1 1 d . . . . .
O7 O 0.3924(2) 0.1671(2) 0.56567(18) 0.0554(7) Uani 1 1 d . . . . .
C8 C 0.4106(2) 0.0354(2) 0.3463(2) 0.0331(6) Uani 1 1 d . . . . .
O8 O 0.3829(2) -0.03872(17) 0.34573(18) 0.0531(7) Uani 1 1 d . . . . .
C9 C 0.5904(2) 0.11507(19) 0.4095(2) 0.0265(5) Uani 1 1 d . . . . .
O9 O 0.66709(17) 0.08432(16) 0.43881(16) 0.0396(5) Uani 1 1 d . . . . .
C10 C 0.4970(2) 0.2919(2) 0.3705(2) 0.0279(6) Uani 1 1 d . . . . .
O10 O 0.51820(17) 0.36795(15) 0.37693(17) 0.0399(5) Uani 1 1 d . . . . .
C11 C 0.3216(2) 0.2077(2) 0.3074(2) 0.0340(6) Uani 1 1 d . . . . .
O11 O 0.24204(18) 0.23514(19) 0.2832(2) 0.0531(7) Uani 1 1 d . . . . .
C12 C 0.51828(18) 0.16595(16) 0.22205(18) 0.0193(5) Uani 1 1 d . . . . .
S1 S 0.86850(5) 0.31202(5) 0.07415(5) 0.02501(15) Uani 1 1 d . . . . .
S2 S 0.65834(5) 0.20934(5) 0.08817(5) 0.02340(15) Uani 1 1 d . . . . .
O12 O 0.48084(13) 0.13229(13) 0.13745(13) 0.0247(4) Uani 1 1 d . . . . .
C13 C 0.91969(18) 0.36082(17) 0.18567(18) 0.0200(5) Uani 1 1 d . . . . .
C14 C 0.85840(18) 0.34353(17) 0.25847(18) 0.0201(5) Uani 1 1 d . . . . .
H14 H 0.8733 0.3644 0.3233 0.024 Uiso 1 1 calc R U . . .
C15 C 0.77027(18) 0.29107(16) 0.22660(18) 0.0191(5) Uani 1 1 d . . . . .
C16 C 0.76554(18) 0.27103(17) 0.12848(18) 0.0198(5) Uani 1 1 d . . . . .
C17 C 0.68505(18) 0.25464(17) 0.27035(18) 0.0210(5) Uani 1 1 d . . . . .
H17 H 0.6764 0.2610 0.3375 0.025 Uiso 1 1 calc R U . . .
C18 C 0.61661(18) 0.20956(16) 0.20623(18) 0.0189(5) Uani 1 1 d . . . . .
C19 C 1.1485(2) 0.4356(2) 0.0767(2) 0.0318(6) Uani 1 1 d . . . . .
H19A H 1.2069 0.4041 0.1135 0.038 Uiso 1 1 calc R U . . .
H19B H 1.1528 0.5023 0.0916 0.038 Uiso 1 1 calc R U . . .
C20 C 1.1514(2) 0.4201(2) -0.0298(2) 0.0292(6) Uani 1 1 d . . . . .
H20A H 1.2176 0.4414 -0.0497 0.044 Uiso 1 1 calc R U . . .
H20B H 1.0954 0.4545 -0.0656 0.044 Uiso 1 1 calc R U . . .
H20C H 1.1433 0.3542 -0.0441 0.044 Uiso 1 1 calc R U . . .
C21 C 0.3822(2) 0.0845(2) 0.1271(2) 0.0334(7) Uani 1 1 d . . . . .
H21A H 0.3290 0.1226 0.1544 0.040 Uiso 1 1 calc R U . . .
H21B H 0.3878 0.0253 0.1628 0.040 Uiso 1 1 calc R U . . .
C22 C 0.3531(2) 0.0673(3) 0.0222(2) 0.0429(8) Uani 1 1 d . . . . .
H22A H 0.2898 0.0306 0.0145 0.064 Uiso 1 1 calc R U . . .
H22B H 0.4086 0.0338 -0.0054 0.064 Uiso 1 1 calc R U . . .
H22C H 0.3415 0.1263 -0.0116 0.064 Uiso 1 1 calc R U . . .
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
Cr1 0.01228(10) 0.01745(11) 0.02196(12) 0.00035(7) 0.00158(7) -0.00085(7)
W1 0.01228(10) 0.01745(11) 0.02196(12) 0.00035(7) 0.00158(7) -0.00085(7)
C1 0.0209(12) 0.0254(13) 0.0310(14) 0.0074(11) 0.0080(10) 0.0020(10)
O1 0.0389(12) 0.0343(11) 0.0291(11) 0.0007(9) 0.0069(9) 0.0000(9)
C2 0.0284(14) 0.0330(14) 0.0228(13) -0.0010(11) -0.0025(11) -0.0013(11)
O2 0.0243(11) 0.0692(16) 0.0374(12) -0.0021(11) -0.0010(9) 0.0023(10)
C3 0.0197(12) 0.0267(13) 0.0347(15) -0.0052(11) 0.0035(11) -0.0004(10)
O3 0.0465(13) 0.0304(11) 0.0489(14) 0.0117(10) 0.0039(11) 0.0017(10)
C4 0.0235(13) 0.0244(13) 0.0365(15) 0.0019(11) 0.0012(11) -0.0001(10)
O4 0.0268(11) 0.0413(13) 0.0660(16) 0.0025(11) 0.0107(10) 0.0079(9)
C5 0.0258(13) 0.0272(13) 0.0293(14) -0.0054(11) -0.0034(11) -0.0045(10)
O5 0.0540(14) 0.0303(11) 0.0388(12) 0.0036(9) -0.0059(10) -0.0079(10)
C6 0.0157(11) 0.0197(11) 0.0248(12) 0.0023(9) 0.0027(9) -0.0003(9)
O6 0.0180(9) 0.0324(10) 0.0307(10) -0.0053(8) 0.0096(7) -0.0097(7)
Cr2 0.01509(11) 0.02298(12) 0.01998(12) -0.00103(8) 0.00468(7) -0.00477(7)
W2 0.01509(11) 0.02298(12) 0.01998(12) -0.00103(8) 0.00468(7) -0.00477(7)
C7 0.0312(15) 0.0411(17) 0.0390(17) -0.0046(14) 0.0039(13) -0.0122(13)
O7 0.0522(15) 0.081(2) 0.0351(13) -0.0079(12) 0.0155(11) -0.0239(14)
C8 0.0378(16) 0.0378(16) 0.0243(14) 0.0008(12) 0.0066(12) -0.0081(13)
O8 0.0760(18) 0.0387(13) 0.0446(14) 0.0040(11) 0.0062(13) -0.0245(13)
C9 0.0283(14) 0.0269(13) 0.0249(13) -0.0005(10) 0.0056(11) -0.0041(11)
O9 0.0332(12) 0.0451(13) 0.0396(12) 0.0047(10) -0.0018(9) 0.0074(10)
C10 0.0209(13) 0.0350(15) 0.0286(14) -0.0014(11) 0.0062(10) -0.0001(11)
O10 0.0365(12) 0.0332(12) 0.0510(14) -0.0078(10) 0.0088(10) -0.0006(9)
C11 0.0330(16) 0.0362(16) 0.0340(16) -0.0082(12) 0.0098(12) -0.0055(12)
O11 0.0319(13) 0.0608(16) 0.0655(17) -0.0156(13) -0.0013(11) 0.0090(11)
C12 0.0160(11) 0.0186(11) 0.0231(12) -0.0004(9) 0.0009(9) -0.0010(9)
S1 0.0207(3) 0.0326(3) 0.0227(3) -0.0030(3) 0.0069(2) -0.0100(3)
S2 0.0178(3) 0.0322(3) 0.0203(3) -0.0027(2) 0.0022(2) -0.0084(2)
O12 0.0167(8) 0.0348(10) 0.0227(9) -0.0032(8) 0.0026(7) -0.0092(7)
C13 0.0150(11) 0.0218(11) 0.0228(12) -0.0006(9) -0.0001(9) -0.0031(9)
C14 0.0157(11) 0.0230(12) 0.0214(12) -0.0001(9) 0.0005(9) -0.0043(9)
C15 0.0150(11) 0.0199(11) 0.0222(12) 0.0013(9) 0.0000(9) -0.0012(9)
C16 0.0155(11) 0.0220(11) 0.0222(12) 0.0000(9) 0.0028(9) -0.0025(9)
C17 0.0166(11) 0.0255(12) 0.0211(12) 0.0014(10) 0.0029(9) -0.0027(9)
C18 0.0149(11) 0.0212(11) 0.0208(12) -0.0002(9) 0.0023(9) -0.0008(9)
C19 0.0196(13) 0.0422(16) 0.0355(15) -0.0066(13) 0.0125(11) -0.0123(11)
C20 0.0240(13) 0.0340(14) 0.0305(14) -0.0018(12) 0.0076(11) -0.0073(11)
C21 0.0222(13) 0.0472(17) 0.0313(15) -0.0063(13) 0.0044(11) -0.0189(12)
C22 0.0321(16) 0.063(2) 0.0334(16) -0.0064(15) 0.0022(13) -0.0223(15)
_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
Cr1 C1 1.911(3) . ?
Cr1 C5 1.945(3) . ?
Cr1 C2 1.945(3) . ?
Cr1 C4 1.960(3) . ?
Cr1 C3 1.971(3) . ?
Cr1 C6 2.122(2) . ?
C1 O1 1.145(3) . ?
C2 O2 1.135(3) . ?
C3 O3 1.130(3) . ?
C4 O4 1.130(3) . ?
C5 O5 1.139(3) . ?
C6 O6 1.325(3) . ?
C6 C13 1.462(3) . ?
O6 C19 1.459(3) . ?
Cr2 C7 1.917(3) . ?
Cr2 C11 1.937(3) . ?
Cr2 C10 1.937(3) . ?
Cr2 C8 1.959(3) . ?
Cr2 C9 1.961(3) . ?
Cr2 C12 2.120(2) . ?
C7 O7 1.145(4) . ?
C8 O8 1.135(4) . ?
C9 O9 1.135(3) . ?
C10 O10 1.139(4) . ?
C11 O11 1.134(4) . ?
C12 O12 1.319(3) . ?
C12 C18 1.466(3) . ?
S1 C16 1.707(2) . ?
S1 C13 1.770(3) . ?
S2 C16 1.710(2) . ?
S2 C18 1.769(2) . ?
O12 C21 1.458(3) . ?
C13 C14 1.367(3) . ?
C14 C15 1.415(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.384(3) . ?
C15 C17 1.418(3) . ?
C17 C18 1.365(3) . ?
C17 H17 0.9500 . ?
C19 C20 1.495(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.485(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
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
C1 Cr1 C5 95.68(11) . . ?
C1 Cr1 C2 88.78(11) . . ?
C5 Cr1 C2 89.78(12) . . ?
C1 Cr1 C4 86.20(11) . . ?
C5 Cr1 C4 85.83(12) . . ?
C2 Cr1 C4 172.97(12) . . ?
C1 Cr1 C3 88.12(11) . . ?
C5 Cr1 C3 176.17(11) . . ?
C2 Cr1 C3 90.74(11) . . ?
C4 Cr1 C3 94.01(11) . . ?
C1 Cr1 C6 173.07(10) . . ?
C5 Cr1 C6 88.71(10) . . ?
C2 Cr1 C6 96.62(10) . . ?
C4 Cr1 C6 88.78(11) . . ?
C3 Cr1 C6 87.46(10) . . ?
O1 C1 Cr1 175.9(2) . . ?
O2 C2 Cr1 174.3(3) . . ?
O3 C3 Cr1 177.6(3) . . ?
O4 C4 Cr1 174.6(3) . . ?
O5 C5 Cr1 177.9(2) . . ?
O6 C6 C13 105.4(2) . . ?
O6 C6 Cr1 130.10(17) . . ?
C13 C6 Cr1 124.37(17) . . ?
C6 O6 C19 123.0(2) . . ?
C7 Cr2 C11 90.94(13) . . ?
C7 Cr2 C10 90.29(12) . . ?
C11 Cr2 C10 87.09(12) . . ?
C7 Cr2 C8 88.93(12) . . ?
C11 Cr2 C8 91.44(13) . . ?
C10 Cr2 C8 178.33(12) . . ?
C7 Cr2 C9 88.89(13) . . ?
C11 Cr2 C9 178.04(12) . . ?
C10 Cr2 C9 94.86(11) . . ?
C8 Cr2 C9 86.60(12) . . ?
C7 Cr2 C12 173.32(11) . . ?
C11 Cr2 C12 94.73(11) . . ?
C10 Cr2 C12 86.47(10) . . ?
C8 Cr2 C12 94.45(10) . . ?
C9 Cr2 C12 85.58(10) . . ?
O7 C7 Cr2 179.2(3) . . ?
O8 C8 Cr2 175.4(3) . . ?
O9 C9 Cr2 178.0(2) . . ?
O10 C10 Cr2 178.0(3) . . ?
O11 C11 Cr2 175.8(3) . . ?
O12 C12 C18 106.5(2) . . ?
O12 C12 Cr2 129.94(17) . . ?
C18 C12 Cr2 123.55(17) . . ?
C16 S1 C13 90.24(12) . . ?
C16 S2 C18 90.67(12) . . ?
C12 O12 C21 120.9(2) . . ?
C14 C13 C6 129.5(2) . . ?
C14 C13 S1 111.67(18) . . ?
C6 C13 S1 118.81(18) . . ?
C13 C14 C15 112.6(2) . . ?
C13 C14 H14 123.7 . . ?
C15 C14 H14 123.7 . . ?
C16 C15 C14 112.3(2) . . ?
C16 C15 C17 112.1(2) . . ?
C14 C15 C17 135.7(2) . . ?
C15 C16 S1 113.20(18) . . ?
C15 C16 S2 112.92(18) . . ?
S1 C16 S2 133.87(16) . . ?
C18 C17 C15 113.2(2) . . ?
C18 C17 H17 123.4 . . ?
C15 C17 H17 123.4 . . ?
C17 C18 C12 129.7(2) . . ?
C17 C18 S2 111.16(18) . . ?
C12 C18 S2 119.14(18) . . ?
O6 C19 C20 107.0(2) . . ?
O6 C19 H19A 110.3 . . ?
C20 C19 H19A 110.3 . . ?
O6 C19 H19B 110.3 . . ?
C20 C19 H19B 110.3 . . ?
H19A C19 H19B 108.6 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O12 C21 C22 108.6(2) . . ?
O12 C21 H21A 110.0 . . ?
C22 C21 H21A 110.0 . . ?
O12 C21 H21B 110.0 . . ?
C22 C21 H21B 110.0 . . ?
H21A C21 H21B 108.3 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C13 C6 O6 C19 -178.4(2) . . . . ?
Cr1 C6 O6 C19 5.1(4) . . . . ?
C18 C12 O12 C21 -179.5(2) . . . . ?
Cr2 C12 O12 C21 -0.3(4) . . . . ?
O6 C6 C13 C14 172.1(3) . . . . ?
Cr1 C6 C13 C14 -11.1(4) . . . . ?
O6 C6 C13 S1 -7.7(3) . . . . ?
Cr1 C6 C13 S1 169.02(12) . . . . ?
C16 S1 C13 C14 0.7(2) . . . . ?
C16 S1 C13 C6 -179.5(2) . . . . ?
C6 C13 C14 C15 -179.7(2) . . . . ?
S1 C13 C14 C15 0.2(3) . . . . ?
C13 C14 C15 C16 -1.2(3) . . . . ?
C13 C14 C15 C17 179.5(3) . . . . ?
C14 C15 C16 S1 1.8(3) . . . . ?
C17 C15 C16 S1 -178.76(18) . . . . ?
C14 C15 C16 S2 -178.94(18) . . . . ?
C17 C15 C16 S2 0.6(3) . . . . ?
C13 S1 C16 C15 -1.4(2) . . . . ?
C13 S1 C16 S2 179.5(2) . . . . ?
C18 S2 C16 C15 0.1(2) . . . . ?
C18 S2 C16 S1 179.2(2) . . . . ?
C16 C15 C17 C18 -1.1(3) . . . . ?
C14 C15 C17 C18 178.2(3) . . . . ?
C15 C17 C18 C12 -177.5(2) . . . . ?
C15 C17 C18 S2 1.1(3) . . . . ?
O12 C12 C18 C17 179.6(2) . . . . ?
Cr2 C12 C18 C17 0.3(4) . . . . ?
O12 C12 C18 S2 1.0(3) . . . . ?
Cr2 C12 C18 S2 -178.27(12) . . . . ?
C16 S2 C18 C17 -0.7(2) . . . . ?
C16 S2 C18 C12 178.1(2) . . . . ?
C6 O6 C19 C20 -170.3(2) . . . . ?
C12 O12 C21 C22 171.5(3) . . . . ?
_shelxl_version_number 2013-4
_shelx_res_file
;
TITL mo_ZL220F22_0m in P2(1)/c
CELL 0.71073 13.0556 14.5145 13.8325 90.000 95.395 90.000
ZERR 4.00 0.00080 0.00100 0.00090 0.0000 0.0018 0.0000
LATT 1
SYMM -X, 1/2+Y, 1/2-Z
SFAC C H O S Cr W
UNIT 88 48 48 8 5.53 2.47
REM Solution 1 R1 0.162 Rweak 0.007, Alpha= 0.0395 in P2(1)/c
REM Formula: C22 O12 S2 Cr2
L.S. 10
BOND $H
CONF
ACTA
FMAP 2
PLAN 20
EADP Cr2 W2
EADP Cr1 W1
EXYZ Cr2 W2
EXYZ Cr1 W1
SIZE 0.057 0.081 0.298
TEMP -123.000
WGHT 0.020600 4.083200
FVAR 0.26138 0.67991 0.70271
CR1 5 1.077174 0.493812 0.307421 21.00000 0.01228 0.01745 =
0.02196 0.00035 0.00158 -0.00085
W1 6 1.077174 0.493812 0.307421 -21.00000 0.01228 0.01745 =
0.02196 0.00035 0.00158 -0.00085
C1 1 1.118579 0.562092 0.422671 11.00000 0.02088 0.02537 =
0.03101 0.00738 0.00798 0.00199
O1 3 1.140579 0.599033 0.494749 11.00000 0.03891 0.03429 =
0.02910 0.00066 0.00689 -0.00003
C2 1 1.221638 0.473423 0.290354 11.00000 0.02845 0.03295 =
0.02279 -0.00102 -0.00247 -0.00134
O2 3 1.307669 0.467586 0.285297 11.00000 0.02426 0.06920 =
0.03741 -0.00210 -0.00104 0.00225
C3 1 1.074675 0.382530 0.388781 11.00000 0.01974 0.02672 =
0.03468 -0.00516 0.00354 -0.00039
O3 3 1.076287 0.319698 0.437166 11.00000 0.04649 0.03042 =
0.04889 0.01170 0.00389 0.00173
C4 1 0.936294 0.530084 0.328286 11.00000 0.02345 0.02442 =
0.03647 0.00194 0.00122 -0.00009
O4 3 0.858006 0.557772 0.341882 11.00000 0.02684 0.04135 =
0.06601 0.00246 0.01069 0.00793
C5 1 1.075746 0.598738 0.219812 11.00000 0.02579 0.02717 =
0.02928 -0.00540 -0.00339 -0.00446
O5 3 1.072466 0.658909 0.166802 11.00000 0.05400 0.03028 =
0.03879 0.00362 -0.00587 -0.00791
C6 1 1.016658 0.411548 0.188740 11.00000 0.01567 0.01967 =
0.02476 0.00229 0.00265 -0.00032
O6 3 1.051127 0.398130 0.102754 11.00000 0.01802 0.03242 =
0.03071 -0.00526 0.00957 -0.00968
CR2 5 0.456106 0.163824 0.358217 31.00000 0.01509 0.02298 =
0.01998 -0.00103 0.00468 -0.00477
W2 6 0.456106 0.163824 0.358217 -31.00000 0.01509 0.02298 =
0.01998 -0.00103 0.00468 -0.00477
C7 1 0.415714 0.165309 0.487922 11.00000 0.03116 0.04111 =
0.03898 -0.00460 0.00389 -0.01218
O7 3 0.392424 0.167062 0.565667 11.00000 0.05221 0.08104 =
0.03509 -0.00790 0.01552 -0.02392
C8 1 0.410609 0.035398 0.346322 11.00000 0.03783 0.03782 =
0.02429 0.00078 0.00663 -0.00808
O8 3 0.382850 -0.038724 0.345731 11.00000 0.07600 0.03875 =
0.04457 0.00404 0.00618 -0.02453
C9 1 0.590408 0.115066 0.409535 11.00000 0.02833 0.02692 =
0.02487 -0.00052 0.00565 -0.00410
O9 3 0.667091 0.084322 0.438806 11.00000 0.03323 0.04507 =
0.03963 0.00466 -0.00176 0.00742
C10 1 0.497028 0.291906 0.370490 11.00000 0.02091 0.03498 =
0.02863 -0.00137 0.00622 -0.00010
O10 3 0.518204 0.367955 0.376928 11.00000 0.03655 0.03315 =
0.05097 -0.00777 0.00877 -0.00062
C11 1 0.321637 0.207716 0.307387 11.00000 0.03299 0.03625 =
0.03399 -0.00825 0.00980 -0.00546
O11 3 0.242043 0.235140 0.283156 11.00000 0.03188 0.06085 =
0.06547 -0.01556 -0.00128 0.00898
C12 1 0.518278 0.165952 0.222052 11.00000 0.01600 0.01857 =
0.02313 -0.00044 0.00093 -0.00104
S1 4 0.868502 0.312021 0.074155 11.00000 0.02066 0.03258 =
0.02270 -0.00304 0.00686 -0.01000
S2 4 0.658337 0.209338 0.088173 11.00000 0.01778 0.03216 =
0.02032 -0.00274 0.00221 -0.00835
O12 3 0.480844 0.132291 0.137454 11.00000 0.01667 0.03480 =
0.02274 -0.00320 0.00260 -0.00919
C13 1 0.919688 0.360821 0.185668 11.00000 0.01505 0.02184 =
0.02283 -0.00063 -0.00009 -0.00311
C14 1 0.858396 0.343526 0.258471 11.00000 0.01574 0.02298 =
0.02144 -0.00012 0.00050 -0.00433
AFIX 43
H14 2 0.873331 0.364430 0.323347 11.00000 -1.20000
AFIX 0
C15 1 0.770274 0.291074 0.226599 11.00000 0.01497 0.01991 =
0.02222 0.00133 0.00001 -0.00123
C16 1 0.765543 0.271031 0.128479 11.00000 0.01550 0.02198 =
0.02221 -0.00002 0.00284 -0.00254
C17 1 0.685053 0.254639 0.270351 11.00000 0.01655 0.02553 =
0.02108 0.00136 0.00288 -0.00273
AFIX 43
H17 2 0.676449 0.260953 0.337467 11.00000 -1.20000
AFIX 0
C18 1 0.616609 0.209557 0.206229 11.00000 0.01486 0.02115 =
0.02085 -0.00018 0.00229 -0.00075
C19 1 1.148457 0.435645 0.076664 11.00000 0.01958 0.04218 =
0.03555 -0.00656 0.01245 -0.01228
AFIX 23
H19A 2 1.206948 0.404052 0.113520 11.00000 -1.20000
H19B 2 1.152824 0.502305 0.091642 11.00000 -1.20000
AFIX 0
C20 1 1.151443 0.420110 -0.029846 11.00000 0.02403 0.03403 =
0.03047 -0.00176 0.00762 -0.00733
AFIX 137
H20A 2 1.217566 0.441412 -0.049655 11.00000 -1.50000
H20B 2 1.095433 0.454492 -0.065604 11.00000 -1.50000
H20C 2 1.143289 0.354241 -0.044117 11.00000 -1.50000
AFIX 0
C21 1 0.382227 0.084475 0.127062 11.00000 0.02216 0.04716 =
0.03130 -0.00626 0.00438 -0.01891
AFIX 23
H21A 2 0.329015 0.122554 0.154367 11.00000 -1.20000
H21B 2 0.387754 0.025304 0.162771 11.00000 -1.20000
AFIX 0
C22 1 0.353068 0.067304 0.022216 11.00000 0.03210 0.06294 =
0.03338 -0.00638 0.00218 -0.02228
AFIX 137
H22A 2 0.289850 0.030564 0.014515 11.00000 -1.50000
H22B 2 0.408569 0.033764 -0.005431 11.00000 -1.50000
H22C 2 0.341549 0.126255 -0.011606 11.00000 -1.50000
AFIX 0
HKLF 4
REM mo_ZL220F22_0m in P2(1)/c
REM R1 = 0.0271 for 5789 Fo > 4sig(Fo) and 0.0344 for all 6523 data
REM 347 parameters refined using 0 restraints
END
WGHT 0.0206 4.0774
REM Highest difference peak 0.606, deepest hole -0.491, 1-sigma level 0.096
Q1 1 0.4604 0.2469 0.3600 11.00000 0.05 0.61
Q2 1 1.0773 0.4978 0.3850 11.00000 0.05 0.57
Q3 1 1.0318 0.4358 0.2378 11.00000 0.05 0.54
Q4 1 0.4619 0.1682 0.2811 11.00000 0.05 0.52
Q5 1 1.0807 0.4253 0.3057 11.00000 0.05 0.51
Q6 1 1.0809 0.4902 0.2438 11.00000 0.05 0.51
Q7 1 0.5021 0.1382 0.3369 11.00000 0.05 0.50
Q8 1 0.4594 0.0939 0.3515 11.00000 0.05 0.48
Q9 1 1.0367 0.4386 0.3212 11.00000 0.05 0.45
Q10 1 0.4622 0.1684 0.4384 11.00000 0.05 0.44
Q11 1 1.0815 0.5738 0.2990 11.00000 0.05 0.44
Q12 1 0.9203 0.6787 0.1874 11.00000 0.05 0.43
Q13 1 0.3085 0.1291 0.0397 11.00000 0.05 0.42
Q14 1 0.5183 0.1301 0.4185 11.00000 0.05 0.42
Q15 1 0.8998 0.3529 0.1424 11.00000 0.05 0.42
Q16 1 0.4579 -0.1574 0.3695 11.00000 0.05 0.40
Q17 1 0.9948 0.4968 0.3224 11.00000 0.05 0.40
Q18 1 1.1152 0.5581 0.3616 11.00000 0.05 0.40
Q19 1 0.4015 0.1970 0.2946 11.00000 0.05 0.39
Q20 1 0.7617 0.2846 0.1811 11.00000 0.05 0.39
;
_shelx_res_checksum 73229
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_mo_ZL228F5_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1401811'
_audit_update_record
;
2015-05-19 deposited with the CCDC.
2015-10-09 downloaded from the CCDC.
;
_audit_creation_method SHELXL-2014/5
_chemical_name_systematic
'2-(Ethoxy-(pentacarbonyl-tungsten)-carbene)-4,6-diethoxy-5,5,5,5-tetracarbonyl-5-tungsta-cyclopenta[b]thieno[3,2-d]thiophene hemidichloromethane'
_chemical_name_common .
_chemical_melting_point ?
_chemical_formula_moiety 'C24 H16 O12 S2 W2, 0.5(C1 H2 Cl2)'
_chemical_formula_sum 'C24.50 H17 Cl O12 S2 W2'
_chemical_formula_weight 970.65
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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system tetragonal
_space_group_IT_number 88
_space_group_name_H-M_alt 'I 41/a'
_space_group_name_Hall '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
_cell_length_a 26.7813(12)
_cell_length_b 26.7813(12)
_cell_length_c 17.3239(8)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 12425.4(13)
_cell_formula_units_Z 16
_cell_measurement_temperature 150(2)
_cell_measurement_reflns_used 9322
_cell_measurement_theta_min 2.567
_cell_measurement_theta_max 33.054
_exptl_crystal_description prism
_exptl_crystal_colour purple
_exptl_crystal_density_meas .
_exptl_crystal_density_method 'not measured'
_exptl_crystal_density_diffrn 2.076
_exptl_crystal_F_000 7312
_exptl_crystal_size_max 0.259
_exptl_crystal_size_mid 0.069
_exptl_crystal_size_min 0.058
_exptl_absorpt_coefficient_mu 7.678
_shelx_estimated_absorpt_T_min 0.241
_shelx_estimated_absorpt_T_max 0.664
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.4610
_exptl_absorpt_correction_T_max 0.7465
_exptl_absorpt_process_details 'SADABS (Bruker, 2014)'
_diffrn_ambient_temperature 150(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'I\ms micro focus'
_diffrn_measurement_device_type 'Bruker kappa, Photon 100 CMOS'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean 10.24
_diffrn_reflns_number 270658
_diffrn_reflns_av_unetI/netI 0.0164
_diffrn_reflns_av_R_equivalents 0.0489
_diffrn_reflns_limit_h_min -41
_diffrn_reflns_limit_h_max 41
_diffrn_reflns_limit_k_min -41
_diffrn_reflns_limit_k_max 41
_diffrn_reflns_limit_l_min -26
_diffrn_reflns_limit_l_max 26
_diffrn_reflns_theta_min 2.067
_diffrn_reflns_theta_max 33.240
_diffrn_reflns_theta_full 25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total 11904
_reflns_number_gt 10088
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
;
_computing_data_collection 'APEX2 (Bruker, 2014)'
_computing_cell_refinement 'SAINT (Bruker, 2014)'
_computing_data_reduction 'SAINT (Bruker, 2014)'
_computing_structure_solution 'SHELXTS (Sheldrick, 2014)'
_computing_structure_refinement 'SHELXTL, SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 1997), POV-RAY (Cason, 2004),
Mercury (Macrae et al., 2008)
;
_computing_publication_material 'SHELXL-2014, PLATON (Spek, 2009)'
_refine_special_details ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0188P)^2^+19.9755P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary intrinsic-phasing
_atom_sites_solution_secondary .
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_number_reflns 11904
_refine_ls_number_parameters 415
_refine_ls_number_restraints 2
_refine_ls_R_factor_all 0.0302
_refine_ls_R_factor_gt 0.0200
_refine_ls_wR_factor_ref 0.0446
_refine_ls_wR_factor_gt 0.0416
_refine_ls_goodness_of_fit_ref 1.091
_refine_ls_restrained_S_all 1.092
_refine_ls_shift/su_max 0.010
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.967
_refine_diff_density_min -0.563
_refine_diff_density_rms 0.124
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.56510(2) 0.40289(2) 0.56786(2) 0.02085(2) Uani 1 1 d . . . . .
C1 C 0.50550(8) 0.44685(8) 0.58364(12) 0.0261(4) Uani 1 1 d . . . . .
O1 O 0.47029(6) 0.47061(7) 0.59419(10) 0.0366(4) Uani 1 1 d . . . . .
C2 C 0.51691(9) 0.34489(9) 0.56882(14) 0.0318(5) Uani 1 1 d . . . . .
O2 O 0.48819(7) 0.31317(7) 0.56740(13) 0.0506(5) Uani 1 1 d . . . . .
C3 C 0.55618(8) 0.40747(9) 0.44971(14) 0.0305(5) Uani 1 1 d . . . . .
O3 O 0.54974(8) 0.40998(9) 0.38521(11) 0.0500(5) Uani 1 1 d . . . . .
C4 C 0.57244(10) 0.39949(9) 0.68506(14) 0.0325(5) Uani 1 1 d . . . . .
O4 O 0.57523(10) 0.39806(8) 0.75041(12) 0.0584(6) Uani 1 1 d . . . . .
C5 C 0.63341(8) 0.36003(7) 0.55541(12) 0.0237(4) Uani 1 1 d . . . . .
O5 O 0.64695(6) 0.31283(6) 0.55873(11) 0.0345(4) Uani 1 1 d . . . . .
C6 C 0.62128(7) 0.46076(7) 0.55713(11) 0.0200(3) Uani 1 1 d . . . . .
O6 O 0.62306(5) 0.50977(5) 0.56182(8) 0.0233(3) Uani 1 1 d . . . . .
W2 W 0.78842(2) 0.63935(2) 0.46955(2) 0.01871(2) Uani 1 1 d . . . . .
C7 C 0.76256(8) 0.71029(8) 0.47804(13) 0.0267(4) Uani 1 1 d . . . . .
O7 O 0.74890(8) 0.75035(6) 0.48435(12) 0.0422(4) Uani 1 1 d . . . . .
C8 C 0.72421(8) 0.62023(8) 0.41372(12) 0.0238(4) Uani 1 1 d . . . . .
O8 O 0.68709(7) 0.61150(7) 0.38483(10) 0.0374(4) Uani 1 1 d . . . . .
C9 C 0.82129(9) 0.65769(8) 0.36699(14) 0.0297(4) Uani 1 1 d . . . . .
O9 O 0.83892(8) 0.67069(7) 0.31030(11) 0.0458(5) Uani 1 1 d . . . . .
C10 C 0.84928(9) 0.66611(9) 0.52739(15) 0.0351(5) Uani 1 1 d . . . . .
O10 O 0.88115(8) 0.68445(9) 0.55956(16) 0.0652(7) Uani 1 1 d . . . . .
C11 C 0.75624(9) 0.62292(8) 0.57371(12) 0.0256(4) Uani 1 1 d . . . . .
O11 O 0.73862(8) 0.61307(7) 0.63115(10) 0.0420(4) Uani 1 1 d . . . . .
C12 C 0.81439(7) 0.56204(7) 0.46895(10) 0.0192(3) Uani 1 1 d . . . . .
O12 O 0.85971(5) 0.54379(6) 0.45710(9) 0.0253(3) Uani 1 1 d . . . . .
S1 S 0.73739(2) 0.37137(2) 0.52229(3) 0.02322(9) Uani 1 1 d . . . . .
S2 S 0.81094(2) 0.45900(2) 0.48463(3) 0.02149(9) Uani 1 1 d . . . . .
C13 C 0.67654(7) 0.39093(7) 0.54001(11) 0.0209(4) Uani 1 1 d . . . . .
C14 C 0.67119(7) 0.44229(7) 0.53837(11) 0.0192(3) Uani 1 1 d . . . . .
C15 C 0.71688(7) 0.46685(7) 0.51952(11) 0.0183(3) Uani 1 1 d . . . . .
C16 C 0.75534(7) 0.43236(7) 0.50943(11) 0.0197(3) Uani 1 1 d . . . . .
C17 C 0.78292(7) 0.51877(7) 0.48590(11) 0.0193(3) Uani 1 1 d . . . . .
C18 C 0.73316(7) 0.51623(7) 0.50562(11) 0.0198(3) Uani 1 1 d . . . . .
H18 H 0.7121 0.5446 0.5095 0.024 Uiso 1 1 calc R U . . .
C19 C 0.60931(10) 0.27493(9) 0.5752(2) 0.0499(8) Uani 1 1 d . . . . .
H19A H 0.5848 0.2733 0.5325 0.060 Uiso 1 1 calc R U . . .
H19B H 0.5912 0.2834 0.6233 0.060 Uiso 1 1 calc R U . . .
C20 C 0.63507(12) 0.22631(12) 0.5837(3) 0.0745(13) Uani 1 1 d . . . . .
H20A H 0.6523 0.2180 0.5355 0.112 Uiso 1 1 calc R U . . .
H20B H 0.6105 0.2003 0.5956 0.112 Uiso 1 1 calc R U . . .
H20C H 0.6595 0.2285 0.6258 0.112 Uiso 1 1 calc R U . . .
C21 C 0.57789(8) 0.53746(8) 0.58029(14) 0.0283(4) Uani 1 1 d . . . . .
H21A H 0.5655 0.5281 0.6322 0.034 Uiso 1 1 calc R U . . .
H21B H 0.5514 0.5302 0.5420 0.034 Uiso 1 1 calc R U . . .
C22 C 0.59153(11) 0.59162(10) 0.5782(2) 0.0541(8) Uani 1 1 d . . . . .
H22A H 0.6199 0.5976 0.6127 0.081 Uiso 1 1 calc R U . . .
H22B H 0.5630 0.6117 0.5952 0.081 Uiso 1 1 calc R U . . .
H22C H 0.6006 0.6011 0.5254 0.081 Uiso 1 1 calc R U . . .
C23 C 0.90266(8) 0.57509(9) 0.44184(16) 0.0342(5) Uani 1 1 d . . . . .
H23A H 0.9047 0.6023 0.4804 0.041 Uiso 1 1 calc R U . . .
H23B H 0.9001 0.5902 0.3898 0.041 Uiso 1 1 calc R U . . .
C24 C 0.94785(9) 0.54227(11) 0.44683(19) 0.0431(6) Uani 1 1 d . . . . .
H24A H 0.9497 0.5273 0.4983 0.065 Uiso 1 1 calc R U . . .
H24B H 0.9779 0.5623 0.4375 0.065 Uiso 1 1 calc R U . . .
H24C H 0.9455 0.5158 0.4079 0.065 Uiso 1 1 calc R U . . .
Cl1 Cl 0.5462(3) 0.7210(3) 0.6142(2) 0.090(4) Uani 0.388(16) 1 d . . P A 1
Cl1A Cl 0.4932(17) 0.8025(6) 0.6391(8) 0.107(19) Uani 0.112(16) 1 d . . P A 2
C25 C 0.5052(14) 0.7667(6) 0.6456(12) 0.087(8) Uani 0.25 1 d . . P . .
Cl2A Cl 0.5553(4) 0.2562(4) 0.7844(5) 0.250(6) Uani 0.35 1 d D . P B 1
Cl2B Cl 0.4891(16) 0.2669(9) 0.7539(10) 0.241(12) Uani 0.15 1 d D . P B 2
C26 C 0.5000 0.2500 0.8482(11) 0.48(5) Uani 0.5 2 d DS T P . .
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
W1 0.01894(4) 0.02072(4) 0.02289(4) -0.00054(3) 0.00084(3) -0.00134(3)
C1 0.0263(10) 0.0303(10) 0.0217(9) 0.0003(8) 0.0018(8) -0.0008(8)
O1 0.0304(9) 0.0459(10) 0.0336(9) 0.0006(8) 0.0049(7) 0.0119(7)
C2 0.0263(10) 0.0311(11) 0.0380(12) -0.0102(9) 0.0074(9) -0.0032(9)
O2 0.0374(10) 0.0398(10) 0.0745(15) -0.0205(10) 0.0175(10) -0.0159(8)
C3 0.0208(9) 0.0400(13) 0.0307(11) -0.0031(9) -0.0002(8) 0.0033(9)
O3 0.0527(12) 0.0707(15) 0.0265(9) -0.0050(9) -0.0024(8) 0.0041(11)
C4 0.0414(13) 0.0251(10) 0.0311(11) 0.0006(9) -0.0033(9) 0.0008(9)
O4 0.0967(19) 0.0494(12) 0.0290(9) 0.0010(9) -0.0117(11) 0.0130(12)
C5 0.0249(10) 0.0196(9) 0.0265(9) -0.0001(7) -0.0020(8) -0.0008(7)
O5 0.0254(8) 0.0173(7) 0.0608(11) 0.0039(7) -0.0013(7) -0.0017(6)
C6 0.0216(9) 0.0195(8) 0.0189(8) 0.0010(7) -0.0021(7) 0.0015(7)
O6 0.0231(7) 0.0186(6) 0.0282(7) -0.0011(5) 0.0012(6) 0.0025(5)
W2 0.02119(4) 0.01632(3) 0.01863(3) -0.00004(3) 0.00011(3) -0.00145(3)
C7 0.0298(10) 0.0222(9) 0.0282(10) 0.0008(8) -0.0030(8) -0.0029(8)
O7 0.0524(11) 0.0215(8) 0.0526(11) 0.0012(8) -0.0069(9) 0.0059(7)
C8 0.0299(10) 0.0199(9) 0.0218(9) 0.0013(7) -0.0006(8) -0.0004(8)
O8 0.0343(9) 0.0403(10) 0.0376(9) -0.0037(8) -0.0124(7) -0.0036(7)
C9 0.0354(12) 0.0220(10) 0.0318(11) 0.0006(8) 0.0049(9) -0.0020(8)
O9 0.0625(13) 0.0364(10) 0.0386(10) 0.0084(8) 0.0217(9) -0.0033(9)
C10 0.0282(11) 0.0319(12) 0.0452(14) -0.0138(10) -0.0045(10) 0.0037(9)
O10 0.0360(11) 0.0650(15) 0.0946(18) -0.0472(14) -0.0212(11) 0.0046(10)
C11 0.0344(11) 0.0182(9) 0.0241(9) -0.0028(7) 0.0018(8) -0.0004(8)
O11 0.0650(13) 0.0327(9) 0.0281(8) -0.0015(7) 0.0163(8) -0.0070(8)
C12 0.0188(8) 0.0226(9) 0.0161(8) -0.0015(7) 0.0005(6) 0.0001(7)
O12 0.0200(7) 0.0233(7) 0.0325(8) -0.0018(6) 0.0067(6) -0.0005(5)
S1 0.0221(2) 0.0151(2) 0.0324(2) -0.00122(18) -0.00176(19) 0.00180(17)
S2 0.0183(2) 0.0185(2) 0.0277(2) -0.00241(18) 0.00038(17) 0.00176(16)
C13 0.0194(8) 0.0204(9) 0.0229(9) 0.0007(7) -0.0018(7) 0.0008(7)
C14 0.0205(8) 0.0173(8) 0.0197(8) 0.0001(6) -0.0016(7) -0.0003(7)
C15 0.0180(8) 0.0172(8) 0.0197(8) -0.0005(6) -0.0009(6) 0.0013(6)
C16 0.0204(8) 0.0156(8) 0.0232(8) -0.0018(7) -0.0022(7) 0.0001(6)
C17 0.0200(8) 0.0179(8) 0.0201(8) -0.0018(7) 0.0000(7) 0.0017(7)
C18 0.0208(8) 0.0168(8) 0.0218(8) -0.0006(7) 0.0001(7) 0.0015(6)
C19 0.0298(12) 0.0223(11) 0.098(3) 0.0100(13) 0.0028(14) -0.0067(9)
C20 0.0403(17) 0.0331(15) 0.150(4) 0.026(2) 0.013(2) -0.0035(13)
C21 0.0264(10) 0.0221(9) 0.0363(11) -0.0029(8) -0.0019(9) 0.0080(8)
C22 0.0429(15) 0.0222(12) 0.097(3) -0.0055(14) 0.0036(16) 0.0073(11)
C23 0.0215(10) 0.0338(12) 0.0472(14) 0.0030(10) 0.0108(9) -0.0033(9)
C24 0.0211(11) 0.0498(16) 0.0585(17) -0.0119(13) 0.0035(11) 0.0002(10)
Cl1 0.082(5) 0.118(6) 0.069(2) -0.022(3) -0.009(3) 0.061(5)
Cl1A 0.21(5) 0.041(8) 0.075(8) 0.024(6) 0.015(17) 0.038(16)
C25 0.12(2) 0.044(8) 0.100(18) -0.017(8) 0.02(2) 0.026(13)
Cl2A 0.248(10) 0.343(12) 0.159(7) -0.069(7) 0.051(6) -0.179(10)
Cl2B 0.33(4) 0.20(3) 0.194(18) 0.063(16) 0.03(2) 0.01(3)
C26 1.14(13) 0.19(3) 0.10(2) 0.000 0.000 -0.32(6)
_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
W1 C1 2.002(2) . ?
W1 C2 2.019(2) . ?
W1 C4 2.042(2) . ?
W1 C3 2.064(2) . ?
W1 C6 2.168(2) . ?
W1 C5 2.170(2) . ?
C1 O1 1.152(3) . ?
C2 O2 1.146(3) . ?
C3 O3 1.133(3) . ?
C4 O4 1.135(3) . ?
C5 O5 1.317(2) . ?
C5 C13 1.446(3) . ?
O5 C19 1.459(3) . ?
C6 O6 1.316(2) . ?
C6 C14 1.462(3) . ?
O6 C21 1.455(2) . ?
W2 C7 2.027(2) . ?
W2 C8 2.038(2) . ?
W2 C9 2.043(2) . ?
W2 C10 2.043(2) . ?
W2 C11 2.048(2) . ?
W2 C12 2.184(2) . ?
C7 O7 1.139(3) . ?
C8 O8 1.137(3) . ?
C9 O9 1.144(3) . ?
C10 O10 1.132(3) . ?
C11 O11 1.132(3) . ?
C12 O12 1.325(2) . ?
C12 C17 1.463(3) . ?
O12 C23 1.448(3) . ?
S1 C16 1.7170(19) . ?
S1 C13 1.739(2) . ?
S2 C16 1.706(2) . ?
S2 C17 1.7681(19) . ?
C13 C14 1.383(3) . ?
C14 C15 1.427(3) . ?
C15 C16 1.394(3) . ?
C15 C18 1.413(3) . ?
C17 C18 1.377(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.481(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.496(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.498(3) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
Cl1 C25 1.73(2) . ?
Cl1A C25 1.77(4) 15_566 ?
Cl2A C26 1.855(12) . ?
Cl2B C26 1.720(17) . ?
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
C1 W1 C2 86.66(9) . . ?
C1 W1 C4 88.12(9) . . ?
C2 W1 C4 91.09(10) . . ?
C1 W1 C3 90.46(9) . . ?
C2 W1 C3 88.85(10) . . ?
C4 W1 C3 178.58(10) . . ?
C1 W1 C6 98.31(8) . . ?
C2 W1 C6 173.73(8) . . ?
C4 W1 C6 92.88(9) . . ?
C3 W1 C6 87.29(8) . . ?
C1 W1 C5 175.21(8) . . ?
C2 W1 C5 97.63(8) . . ?
C4 W1 C5 89.67(9) . . ?
C3 W1 C5 91.75(8) . . ?
C6 W1 C5 77.56(7) . . ?
O1 C1 W1 177.3(2) . . ?
O2 C2 W1 177.0(2) . . ?
O3 C3 W1 177.9(2) . . ?
O4 C4 W1 178.2(3) . . ?
O5 C5 C13 109.73(18) . . ?
O5 C5 W1 137.36(15) . . ?
C13 C5 W1 112.91(14) . . ?
C5 O5 C19 119.10(19) . . ?
O6 C6 C14 108.54(16) . . ?
O6 C6 W1 137.13(14) . . ?
C14 C6 W1 114.32(13) . . ?
C6 O6 C21 119.47(16) . . ?
C7 W2 C8 88.95(9) . . ?
C7 W2 C9 89.14(9) . . ?
C8 W2 C9 90.65(9) . . ?
C7 W2 C10 84.74(9) . . ?
C8 W2 C10 173.65(9) . . ?
C9 W2 C10 89.91(10) . . ?
C7 W2 C11 89.64(9) . . ?
C8 W2 C11 90.52(9) . . ?
C9 W2 C11 178.30(9) . . ?
C10 W2 C11 88.79(10) . . ?
C7 W2 C12 175.85(8) . . ?
C8 W2 C12 91.62(8) . . ?
C9 W2 C12 94.96(8) . . ?
C10 W2 C12 94.63(8) . . ?
C11 W2 C12 86.24(8) . . ?
O7 C7 W2 178.2(2) . . ?
O8 C8 W2 176.28(19) . . ?
O9 C9 W2 176.1(2) . . ?
O10 C10 W2 174.6(2) . . ?
O11 C11 W2 178.9(2) . . ?
O12 C12 C17 105.47(16) . . ?
O12 C12 W2 129.97(14) . . ?
C17 C12 W2 124.51(13) . . ?
C12 O12 C23 122.87(17) . . ?
C16 S1 C13 89.93(9) . . ?
C16 S2 C17 90.28(9) . . ?
C14 C13 C5 119.35(18) . . ?
C14 C13 S1 113.13(15) . . ?
C5 C13 S1 127.52(15) . . ?
C13 C14 C15 111.97(17) . . ?
C13 C14 C6 115.25(17) . . ?
C15 C14 C6 132.78(17) . . ?
C16 C15 C18 111.76(17) . . ?
C16 C15 C14 110.91(17) . . ?
C18 C15 C14 137.28(18) . . ?
C15 C16 S2 113.53(14) . . ?
C15 C16 S1 114.02(15) . . ?
S2 C16 S1 132.43(12) . . ?
C18 C17 C12 130.26(17) . . ?
C18 C17 S2 111.67(14) . . ?
C12 C17 S2 118.04(14) . . ?
C17 C18 C15 112.76(17) . . ?
C17 C18 H18 123.6 . . ?
C15 C18 H18 123.6 . . ?
O5 C19 C20 108.0(2) . . ?
O5 C19 H19A 110.1 . . ?
C20 C19 H19A 110.1 . . ?
O5 C19 H19B 110.1 . . ?
C20 C19 H19B 110.1 . . ?
H19A C19 H19B 108.4 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O6 C21 C22 106.6(2) . . ?
O6 C21 H21A 110.4 . . ?
C22 C21 H21A 110.4 . . ?
O6 C21 H21B 110.4 . . ?
C22 C21 H21B 110.4 . . ?
H21A C21 H21B 108.6 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O12 C23 C24 107.0(2) . . ?
O12 C23 H23A 110.3 . . ?
C24 C23 H23A 110.3 . . ?
O12 C23 H23B 110.3 . . ?
C24 C23 H23B 110.3 . . ?
H23A C23 H23B 108.6 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Cl1 C25 Cl1 96(2) 12_767 . ?
Cl1A C25 Cl1A 91(2) . 12_767 ?
Cl2A C26 Cl2A 106.8(11) 6_554 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C13 C5 O5 C19 178.9(2) . . . . ?
W1 C5 O5 C19 -0.3(4) . . . . ?
C14 C6 O6 C21 -179.76(17) . . . . ?
W1 C6 O6 C21 1.5(3) . . . . ?
C17 C12 O12 C23 -177.18(19) . . . . ?
W2 C12 O12 C23 0.4(3) . . . . ?
O5 C5 C13 C14 -176.46(19) . . . . ?
W1 C5 C13 C14 2.9(2) . . . . ?
O5 C5 C13 S1 3.6(3) . . . . ?
W1 C5 C13 S1 -177.03(12) . . . . ?
C16 S1 C13 C14 -1.90(16) . . . . ?
C16 S1 C13 C5 178.08(19) . . . . ?
C5 C13 C14 C15 -177.75(17) . . . . ?
S1 C13 C14 C15 2.2(2) . . . . ?
C5 C13 C14 C6 3.2(3) . . . . ?
S1 C13 C14 C6 -176.77(14) . . . . ?
O6 C6 C14 C13 173.05(17) . . . . ?
W1 C6 C14 C13 -7.9(2) . . . . ?
O6 C6 C14 C15 -5.7(3) . . . . ?
W1 C6 C14 C15 173.38(17) . . . . ?
C13 C14 C15 C16 -1.4(2) . . . . ?
C6 C14 C15 C16 177.4(2) . . . . ?
C13 C14 C15 C18 175.7(2) . . . . ?
C6 C14 C15 C18 -5.6(4) . . . . ?
C18 C15 C16 S2 0.8(2) . . . . ?
C14 C15 C16 S2 178.64(13) . . . . ?
C18 C15 C16 S1 -177.90(14) . . . . ?
C14 C15 C16 S1 0.0(2) . . . . ?
C17 S2 C16 C15 -0.79(16) . . . . ?
C17 S2 C16 S1 177.58(16) . . . . ?
C13 S1 C16 C15 1.08(16) . . . . ?
C13 S1 C16 S2 -177.29(16) . . . . ?
O12 C12 C17 C18 177.1(2) . . . . ?
W2 C12 C17 C18 -0.7(3) . . . . ?
O12 C12 C17 S2 -0.9(2) . . . . ?
W2 C12 C17 S2 -178.65(9) . . . . ?
C16 S2 C17 C18 0.60(15) . . . . ?
C16 S2 C17 C12 178.94(16) . . . . ?
C12 C17 C18 C15 -178.36(19) . . . . ?
S2 C17 C18 C15 -0.3(2) . . . . ?
C16 C15 C18 C17 -0.3(2) . . . . ?
C14 C15 C18 C17 -177.4(2) . . . . ?
C5 O5 C19 C20 -174.1(3) . . . . ?
C6 O6 C21 C22 -177.8(2) . . . . ?
C12 O12 C23 C24 169.4(2) . . . . ?
_shelxl_version_number 2014/5
_shelx_res_file
;
TITL mo_ZL228F5_0m in I4(1)/a
CELL 0.71073 26.7813 26.7813 17.3239 90.000 90.000 90.000
ZERR 16.00 0.0012 0.0012 0.0008 0.0000 0.0000 0.0000
LATT 2
SYMM 1/2-X, -Y, 1/2+Z
SYMM 3/4-Y, 1/4+X, 1/4+Z
SYMM 3/4+Y, 3/4-X, 3/4+Z
SFAC C H O S W Cl
UNIT 392 272 192 32 32 16
REM Solution 1 R1 0.094 Rweak 0.003, Alpha= 0.0287 in I4(1)/a
REM Formula: C27 O10 S2 W2
L.S. 16
BOND $H
CONF
ACTA
FMAP 2
PLAN 20
SIZE 0.058 0.069 0.259
TEMP -123.00
DFIX 1.79 Cl2A C26
DFIX 1.79 Cl2B C26
WGHT 0.018800 19.975498
FVAR 0.04049 0.77591
W1 5 0.565101 0.402886 0.567862 11.00000 0.01894 0.02072 =
0.02289 -0.00054 0.00084 -0.00134
C1 1 0.505503 0.446853 0.583637 11.00000 0.02633 0.03030 =
0.02167 0.00033 0.00184 -0.00076
O1 3 0.470293 0.470609 0.594192 11.00000 0.03040 0.04589 =
0.03364 0.00059 0.00487 0.01187
C2 1 0.516913 0.344891 0.568819 11.00000 0.02631 0.03105 =
0.03797 -0.01016 0.00737 -0.00317
O2 3 0.488192 0.313168 0.567396 11.00000 0.03737 0.03984 =
0.07450 -0.02052 0.01752 -0.01587
C3 1 0.556181 0.407474 0.449709 11.00000 0.02082 0.04005 =
0.03068 -0.00313 -0.00023 0.00327
O3 3 0.549739 0.409982 0.385215 11.00000 0.05269 0.07072 =
0.02653 -0.00505 -0.00239 0.00407
C4 1 0.572437 0.399492 0.685056 11.00000 0.04143 0.02513 =
0.03107 0.00061 -0.00334 0.00079
O4 3 0.575235 0.398064 0.750408 11.00000 0.09666 0.04941 =
0.02902 0.00097 -0.01170 0.01295
C5 1 0.633407 0.360035 0.555409 11.00000 0.02488 0.01957 =
0.02651 -0.00010 -0.00198 -0.00078
O5 3 0.646950 0.312827 0.558733 11.00000 0.02542 0.01734 =
0.06083 0.00385 -0.00129 -0.00174
C6 1 0.621279 0.460759 0.557133 11.00000 0.02163 0.01952 =
0.01892 0.00103 -0.00213 0.00146
O6 3 0.623058 0.509765 0.561818 11.00000 0.02309 0.01863 =
0.02822 -0.00109 0.00121 0.00249
W2 5 0.788416 0.639354 0.469551 11.00000 0.02119 0.01632 =
0.01863 -0.00004 0.00011 -0.00145
C7 1 0.762558 0.710291 0.478042 11.00000 0.02981 0.02219 =
0.02818 0.00081 -0.00297 -0.00295
O7 3 0.748904 0.750346 0.484348 11.00000 0.05237 0.02152 =
0.05260 0.00119 -0.00694 0.00590
C8 1 0.724207 0.620231 0.413716 11.00000 0.02987 0.01986 =
0.02177 0.00127 -0.00063 -0.00039
O8 3 0.687088 0.611503 0.384834 11.00000 0.03426 0.04030 =
0.03765 -0.00368 -0.01238 -0.00358
C9 1 0.821293 0.657692 0.366991 11.00000 0.03545 0.02201 =
0.03175 0.00057 0.00490 -0.00201
O9 3 0.838917 0.670685 0.310297 11.00000 0.06255 0.03637 =
0.03858 0.00838 0.02170 -0.00332
C10 1 0.849276 0.666112 0.527385 11.00000 0.02822 0.03193 =
0.04521 -0.01378 -0.00449 0.00367
O10 3 0.881153 0.684447 0.559561 11.00000 0.03601 0.06499 =
0.09461 -0.04723 -0.02120 0.00456
C11 1 0.756240 0.622920 0.573711 11.00000 0.03439 0.01824 =
0.02410 -0.00279 0.00183 -0.00035
O11 3 0.738619 0.613074 0.631151 11.00000 0.06503 0.03271 =
0.02812 -0.00154 0.01631 -0.00703
C12 1 0.814389 0.562038 0.468948 11.00000 0.01883 0.02262 =
0.01610 -0.00154 0.00047 0.00013
O12 3 0.859712 0.543786 0.457101 11.00000 0.01997 0.02328 =
0.03251 -0.00185 0.00673 -0.00052
S1 4 0.737395 0.371374 0.522289 11.00000 0.02213 0.01509 =
0.03245 -0.00122 -0.00176 0.00180
S2 4 0.810945 0.458995 0.484629 11.00000 0.01827 0.01851 =
0.02770 -0.00241 0.00038 0.00176
C13 1 0.676537 0.390925 0.540006 11.00000 0.01936 0.02037 =
0.02286 0.00069 -0.00179 0.00080
C14 1 0.671189 0.442294 0.538374 11.00000 0.02052 0.01730 =
0.01974 0.00011 -0.00162 -0.00032
C15 1 0.716884 0.466846 0.519518 11.00000 0.01796 0.01724 =
0.01971 -0.00048 -0.00092 0.00134
C16 1 0.755343 0.432358 0.509431 11.00000 0.02041 0.01563 =
0.02320 -0.00182 -0.00215 0.00011
C17 1 0.782918 0.518765 0.485896 11.00000 0.02003 0.01787 =
0.02012 -0.00175 -0.00003 0.00173
C18 1 0.733163 0.516232 0.505623 11.00000 0.02078 0.01677 =
0.02178 -0.00064 0.00009 0.00148
AFIX 43
H18 2 0.712055 0.544631 0.509477 11.00000 -1.20000
AFIX 0
C19 1 0.609308 0.274932 0.575176 11.00000 0.02984 0.02225 =
0.09772 0.01001 0.00285 -0.00666
AFIX 23
H19A 2 0.584809 0.273255 0.532460 11.00000 -1.20000
H19B 2 0.591247 0.283355 0.623308 11.00000 -1.20000
AFIX 0
C20 1 0.635072 0.226310 0.583732 11.00000 0.04030 0.03307 =
0.15001 0.02626 0.01252 -0.00350
AFIX 137
H20A 2 0.652303 0.218015 0.535502 11.00000 -1.50000
H20B 2 0.610507 0.200291 0.595568 11.00000 -1.50000
H20C 2 0.659453 0.228451 0.625786 11.00000 -1.50000
AFIX 0
C21 1 0.577887 0.537456 0.580294 11.00000 0.02644 0.02208 =
0.03633 -0.00288 -0.00185 0.00797
AFIX 23
H21A 2 0.565537 0.528101 0.632178 11.00000 -1.20000
H21B 2 0.551407 0.530223 0.542021 11.00000 -1.20000
AFIX 0
C22 1 0.591532 0.591620 0.578229 11.00000 0.04287 0.02224 =
0.09717 -0.00552 0.00362 0.00726
AFIX 137
H22A 2 0.619923 0.597600 0.612701 11.00000 -1.50000
H22B 2 0.562960 0.611671 0.595209 11.00000 -1.50000
H22C 2 0.600650 0.601063 0.525425 11.00000 -1.50000
AFIX 0
C23 1 0.902659 0.575088 0.441842 11.00000 0.02146 0.03381 =
0.04724 0.00297 0.01084 -0.00331
AFIX 23
H23A 2 0.904732 0.602288 0.480408 11.00000 -1.20000
H23B 2 0.900105 0.590156 0.389808 11.00000 -1.20000
AFIX 0
C24 1 0.947850 0.542272 0.446827 11.00000 0.02110 0.04982 =
0.05851 -0.01191 0.00354 0.00025
AFIX 137
H24A 2 0.949674 0.527266 0.498344 11.00000 -1.50000
H24B 2 0.977898 0.562265 0.437495 11.00000 -1.50000
H24C 2 0.945537 0.515820 0.407903 11.00000 -1.50000
AFIX 0
PART 1
CL1 6 0.546157 0.720994 0.614180 20.50000 0.08237 0.11802 =
0.06920 -0.02220 -0.00921 0.06117
PART 2
CL1A 6 0.493152 0.802477 0.639084 -20.50000 0.20521 0.04074 =
0.07515 0.02359 0.01454 0.03796
PART 0
C25 1 0.505235 0.766696 0.645557 10.25000 0.11699 0.04375 =
0.09968 -0.01744 0.02089 0.02635
PART 1
CL2A 6 0.555284 0.256172 0.784380 10.35000 0.24767 0.34282 =
0.15850 -0.06918 0.05092 -0.17895
PART 2
CL2B 6 0.489080 0.266890 0.753909 10.15000 0.33158 0.19608 =
0.19449 0.06327 0.03253 0.00906
PART 0
C26 1 0.500000 0.250000 0.848193 10.25000 1.13960 0.19215 =
0.10100 0.00000 0.00000 -0.32420
HKLF 4
REM mo_ZL228F5_0m in I4(1)/a
REM R1 = 0.0200 for 10088 Fo > 4sig(Fo) and 0.0302 for all 11904 data
REM 415 parameters refined using 2 restraints
END
WGHT 0.0188 20.0000
REM Highest difference peak 0.967, deepest hole -0.563, 1-sigma level 0.124
Q1 1 0.7954 0.6414 0.4129 11.00000 0.05 0.94
Q2 1 0.5625 0.4012 0.4993 11.00000 0.05 0.88
Q3 1 0.5699 0.4029 0.6199 11.00000 0.05 0.80
Q4 1 0.5443 0.4188 0.3789 11.00000 0.05 0.70
Q5 1 0.5691 0.2478 0.7775 11.00000 0.05 0.69
Q6 1 0.7487 0.4987 0.5699 11.00000 0.05 0.68
Q7 1 0.7992 0.6585 0.4624 11.00000 0.05 0.68
Q8 1 0.5714 0.3821 0.5713 11.00000 0.05 0.66
Q9 1 0.6712 0.2111 0.5688 11.00000 0.05 0.64
Q10 1 0.6108 0.2599 0.6391 11.00000 0.05 0.63
Q11 1 0.7906 0.6372 0.6585 11.00000 0.05 0.62
Q12 1 0.5408 0.3876 0.3950 11.00000 0.05 0.61
Q13 1 0.7613 0.6215 0.5225 11.00000 0.05 0.60
Q14 1 0.5620 0.4106 0.3726 11.00000 0.05 0.58
Q15 1 0.5701 0.2397 0.8383 11.00000 0.05 0.58
Q16 1 0.5295 0.2889 0.7801 11.00000 0.05 0.57
Q17 1 0.5523 0.3667 0.6222 11.00000 0.05 0.57
Q18 1 0.5289 0.4189 0.4278 11.00000 0.05 0.56
Q19 1 0.5368 0.7614 0.6560 11.00000 0.05 0.56
Q20 1 0.8077 0.6713 0.2823 11.00000 0.05 0.55
;
_shelx_res_checksum 90597
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_mo_ZL228F7_2_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1401812'
_audit_update_record
;
2015-05-19 deposited with the CCDC.
2015-10-09 downloaded from the CCDC.
;
_audit_creation_method SHELXL-2014/5
_chemical_name_systematic
2,2,2,2,5,5,5,5-Octacarbonyl-1,3,4,6-tetraethoxy-2,5-ditungsta-dicyclopenta[b,e]thieno[3,2-d]thiophene
_chemical_name_common .
_chemical_melting_point ?
_chemical_formula_moiety 'C26 H20 O12 S2 W2'
_chemical_formula_sum 'C26 H20 O12 S2 W2'
_chemical_formula_weight 956.24
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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 21/c'
_space_group_name_Hall '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 7.2013(3)
_cell_length_b 34.2589(15)
_cell_length_c 12.5924(5)
_cell_angle_alpha 90
_cell_angle_beta 101.9948(12)
_cell_angle_gamma 90
_cell_volume 3038.8(2)
_cell_formula_units_Z 4
_cell_measurement_temperature 150(2)
_cell_measurement_reflns_used 9009
_cell_measurement_theta_min 2.378
_cell_measurement_theta_max 38.750
_exptl_crystal_description block
_exptl_crystal_colour purple
_exptl_crystal_density_meas .
_exptl_crystal_density_method 'not measured'
_exptl_crystal_density_diffrn 2.090
_exptl_crystal_F_000 1808
_exptl_crystal_size_max 0.296
_exptl_crystal_size_mid 0.166
_exptl_crystal_size_min 0.086
_exptl_absorpt_coefficient_mu 7.762
_shelx_estimated_absorpt_T_min 0.207
_shelx_estimated_absorpt_T_max 0.555
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.4197
_exptl_absorpt_correction_T_max 0.7479
_exptl_absorpt_process_details 'SADABS (Bruker, 2014)'
_diffrn_ambient_temperature 150(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'I\ms micro focus'
_diffrn_measurement_device_type 'Bruker kappa, Photon 100 CMOS'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean 10.24
_diffrn_reflns_number 223788
_diffrn_reflns_av_unetI/netI 0.0236
_diffrn_reflns_av_R_equivalents 0.0635
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_k_min -57
_diffrn_reflns_limit_k_max 57
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_theta_min 2.036
_diffrn_reflns_theta_max 36.318
_diffrn_reflns_theta_full 25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total 14696
_reflns_number_gt 12986
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
;
_computing_data_collection 'APEX2 (Bruker, 2014)'
_computing_cell_refinement 'SAINT (Bruker, 2014)'
_computing_data_reduction 'SAINT (Bruker, 2014)'
_computing_structure_solution 'SHELXTS (Sheldrick, 2014)'
_computing_structure_refinement 'SHELXTL, SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 1997), POV-RAY (Cason, 2004),
Mercury (Macrae et al., 2008)
;
_computing_publication_material 'SHELXL-2014, PLATON (Spek, 2009)'
_refine_special_details ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0195P)^2^+2.5989P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary intrinsic-phasing
_atom_sites_solution_secondary .
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_number_reflns 14696
_refine_ls_number_parameters 383
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0329
_refine_ls_R_factor_gt 0.0252
_refine_ls_wR_factor_ref 0.0538
_refine_ls_wR_factor_gt 0.0522
_refine_ls_goodness_of_fit_ref 1.157
_refine_ls_restrained_S_all 1.157
_refine_ls_shift/su_max 0.006
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 1.843
_refine_diff_density_min -1.595
_refine_diff_density_rms 0.137
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.13788(2) 0.27640(2) 0.38855(2) 0.01640(2) Uani 1 1 d . . . . .
C1 C -0.0324(3) 0.30713(8) 0.2687(2) 0.0287(5) Uani 1 1 d . . . . .
O1 O -0.1253(3) 0.32369(7) 0.19868(19) 0.0497(6) Uani 1 1 d . . . . .
C2 C 0.1028(3) 0.23115(7) 0.28333(19) 0.0236(4) Uani 1 1 d . . . . .
O2 O 0.0724(3) 0.20583(6) 0.22199(16) 0.0358(4) Uani 1 1 d . . . . .
C3 C 0.3714(3) 0.30069(7) 0.34289(18) 0.0229(4) Uani 1 1 d . . . . .
O3 O 0.5006(3) 0.31630(6) 0.32498(17) 0.0356(4) Uani 1 1 d . . . . .
C4 C -0.0888(3) 0.25777(7) 0.45036(18) 0.0228(4) Uani 1 1 d . . . . .
O4 O -0.2143(3) 0.24747(6) 0.48474(18) 0.0382(4) Uani 1 1 d . . . . .
C5 C 0.3307(3) 0.24863(6) 0.52003(17) 0.0173(3) Uani 1 1 d . . . . .
O5 O 0.3855(2) 0.21288(4) 0.55155(14) 0.0233(3) Uani 1 1 d . . . . .
C6 C 0.1926(3) 0.32105(5) 0.51176(16) 0.0157(3) Uani 1 1 d . . . . .
O6 O 0.1029(2) 0.35149(4) 0.53894(13) 0.0206(3) Uani 1 1 d . . . . .
W2 W 0.49370(2) 0.46634(2) 0.75757(2) 0.01644(2) Uani 1 1 d . . . . .
C7 C 0.3322(3) 0.50522(7) 0.65847(19) 0.0250(4) Uani 1 1 d . . . . .
O7 O 0.2427(3) 0.52896(6) 0.60698(18) 0.0414(5) Uani 1 1 d . . . . .
C8 C 0.5689(4) 0.51284(7) 0.85536(19) 0.0265(4) Uani 1 1 d . . . . .
O8 O 0.6083(3) 0.54065(6) 0.90575(18) 0.0426(5) Uani 1 1 d . . . . .
C9 C 0.7264(3) 0.47526(6) 0.69051(18) 0.0219(4) Uani 1 1 d . . . . .
O9 O 0.8577(3) 0.47999(6) 0.65467(16) 0.0355(4) Uani 1 1 d . . . . .
C10 C 0.2653(3) 0.45162(7) 0.82447(19) 0.0254(4) Uani 1 1 d . . . . .
O10 O 0.1394(3) 0.44235(7) 0.85966(18) 0.0442(5) Uani 1 1 d . . . . .
C11 C 0.6514(3) 0.42130(6) 0.85805(16) 0.0175(3) Uani 1 1 d . . . . .
O11 O 0.7683(2) 0.41860(5) 0.95364(12) 0.0217(3) Uani 1 1 d . . . . .
C12 C 0.4314(3) 0.41499(6) 0.65700(15) 0.0159(3) Uani 1 1 d . . . . .
O12 O 0.3680(2) 0.40775(4) 0.55311(11) 0.0187(3) Uani 1 1 d . . . . .
S1 S 0.60400(7) 0.26663(2) 0.71295(4) 0.02037(9) Uani 1 1 d . . . . .
S2 S 0.73034(8) 0.33957(2) 0.86130(4) 0.02161(10) Uani 1 1 d . . . . .
C13 C 0.4286(3) 0.27664(5) 0.59949(16) 0.0165(3) Uani 1 1 d . . . . .
C14 C 0.3697(2) 0.31499(5) 0.59259(15) 0.0146(3) Uani 1 1 d . . . . .
C15 C 0.4758(3) 0.33816(5) 0.67859(15) 0.0154(3) Uani 1 1 d . . . . .
C16 C 0.6026(3) 0.31482(6) 0.75074(16) 0.0186(3) Uani 1 1 d . . . . .
C17 C 0.6190(3) 0.38272(6) 0.81068(16) 0.0172(3) Uani 1 1 d . . . . .
C18 C 0.4930(3) 0.37800(6) 0.71233(15) 0.0154(3) Uani 1 1 d . . . . .
C19 C 0.2997(4) 0.18021(7) 0.4855(2) 0.0307(5) Uani 1 1 d . . . . .
H19A H 0.3415 0.1799 0.4155 0.037 Uiso 1 1 calc R U . . .
H19B H 0.1596 0.1824 0.4706 0.037 Uiso 1 1 calc R U . . .
C20 C 0.3628(6) 0.14343(8) 0.5487(3) 0.0500(8) Uani 1 1 d . . . . .
H20A H 0.5016 0.1415 0.5624 0.075 Uiso 1 1 calc R U . . .
H20B H 0.3067 0.1207 0.5066 0.075 Uiso 1 1 calc R U . . .
H20C H 0.3213 0.1442 0.6180 0.075 Uiso 1 1 calc R U . . .
C21 C -0.0869(3) 0.36020(8) 0.4781(2) 0.0326(5) Uani 1 1 d . . . . .
H21A H -0.1639 0.3361 0.4651 0.039 Uiso 1 1 calc R U . . .
H21B H -0.0811 0.3720 0.4072 0.039 Uiso 1 1 calc R U . . .
C22 C -0.1707(5) 0.38782(12) 0.5446(3) 0.0516(9) Uani 1 1 d . . . . .
H22A H -0.1693 0.3762 0.6159 0.077 Uiso 1 1 calc R U . . .
H22B H -0.3019 0.3936 0.5083 0.077 Uiso 1 1 calc R U . . .
H22C H -0.0967 0.4120 0.5537 0.077 Uiso 1 1 calc R U . . .
C23 C 0.8203(3) 0.45352(7) 1.01733(19) 0.0274(4) Uani 1 1 d . . . . .
H23A H 0.7056 0.4688 1.0217 0.033 Uiso 1 1 calc R U . . .
H23B H 0.9050 0.4700 0.9836 0.033 Uiso 1 1 calc R U . . .
C24 C 0.9205(5) 0.44091(10) 1.1285(2) 0.0487(8) Uani 1 1 d . . . . .
H24A H 0.8318 0.4266 1.1636 0.073 Uiso 1 1 calc R U . . .
H24B H 0.9677 0.4639 1.1720 0.073 Uiso 1 1 calc R U . . .
H24C H 1.0274 0.4239 1.1226 0.073 Uiso 1 1 calc R U . . .
C25 C 0.3125(3) 0.43924(6) 0.47674(17) 0.0243(4) Uani 1 1 d . . . . .
H25A H 0.4095 0.4602 0.4887 0.029 Uiso 1 1 calc R U . . .
H25B H 0.1897 0.4505 0.4850 0.029 Uiso 1 1 calc R U . . .
C26 C 0.2951(4) 0.42175(8) 0.36574(19) 0.0348(6) Uani 1 1 d . . . . .
H26A H 0.4187 0.4115 0.3580 0.052 Uiso 1 1 calc R U . . .
H26B H 0.2534 0.4419 0.3106 0.052 Uiso 1 1 calc R U . . .
H26C H 0.2020 0.4005 0.3562 0.052 Uiso 1 1 calc R U . . .
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
W1 0.01449(3) 0.01763(4) 0.01611(3) -0.00442(2) 0.00093(2) -0.00074(2)
C1 0.0259(10) 0.0302(12) 0.0268(11) -0.0021(9) -0.0021(8) -0.0009(8)
O1 0.0486(13) 0.0526(14) 0.0393(12) 0.0113(10) -0.0109(10) 0.0086(10)
C2 0.0196(9) 0.0284(11) 0.0234(10) -0.0088(8) 0.0064(7) -0.0027(7)
O2 0.0352(9) 0.0377(10) 0.0365(10) -0.0214(8) 0.0125(8) -0.0057(8)
C3 0.0241(9) 0.0223(10) 0.0220(9) -0.0048(7) 0.0043(7) -0.0005(7)
O3 0.0341(9) 0.0346(10) 0.0421(11) -0.0054(8) 0.0170(8) -0.0098(7)
C4 0.0202(9) 0.0237(10) 0.0235(9) -0.0078(8) 0.0024(7) -0.0024(7)
O4 0.0320(9) 0.0415(11) 0.0446(11) -0.0064(9) 0.0165(8) -0.0098(8)
C5 0.0153(7) 0.0154(8) 0.0213(9) -0.0028(6) 0.0046(6) -0.0009(6)
O5 0.0258(7) 0.0131(6) 0.0289(8) -0.0026(5) 0.0005(6) -0.0009(5)
C6 0.0141(7) 0.0144(8) 0.0176(8) -0.0013(6) 0.0011(6) -0.0006(6)
O6 0.0158(6) 0.0191(7) 0.0251(7) -0.0052(5) -0.0002(5) 0.0046(5)
W2 0.02032(4) 0.01349(3) 0.01519(3) -0.00187(2) 0.00293(2) -0.00012(3)
C7 0.0297(10) 0.0212(10) 0.0244(10) 0.0012(8) 0.0063(8) 0.0019(8)
O7 0.0491(12) 0.0321(10) 0.0408(11) 0.0111(8) 0.0042(9) 0.0132(9)
C8 0.0364(12) 0.0203(10) 0.0238(10) -0.0054(8) 0.0085(9) -0.0020(8)
O8 0.0605(13) 0.0290(10) 0.0394(11) -0.0174(8) 0.0131(10) -0.0103(9)
C9 0.0263(10) 0.0178(9) 0.0204(9) -0.0013(7) 0.0024(7) 0.0002(7)
O9 0.0311(9) 0.0396(11) 0.0381(10) 0.0038(8) 0.0125(8) -0.0008(8)
C10 0.0263(10) 0.0277(11) 0.0217(10) 0.0013(8) 0.0041(8) 0.0043(8)
O10 0.0310(10) 0.0630(15) 0.0422(11) 0.0100(10) 0.0157(8) 0.0004(9)
C11 0.0177(8) 0.0198(9) 0.0145(8) -0.0022(6) 0.0019(6) -0.0025(6)
O11 0.0237(7) 0.0229(7) 0.0155(6) -0.0045(5) -0.0029(5) -0.0023(5)
C12 0.0152(7) 0.0165(8) 0.0156(8) -0.0002(6) 0.0022(6) 0.0000(6)
O12 0.0235(7) 0.0160(6) 0.0144(6) 0.0003(5) -0.0014(5) -0.0001(5)
S1 0.0213(2) 0.01345(19) 0.0229(2) 0.00091(17) -0.00344(17) 0.00217(16)
S2 0.0240(2) 0.0175(2) 0.0185(2) 0.00021(17) -0.00682(17) 0.00127(17)
C13 0.0161(7) 0.0133(7) 0.0192(8) -0.0010(6) 0.0012(6) 0.0007(6)
C14 0.0140(7) 0.0140(7) 0.0151(7) -0.0011(6) 0.0014(6) 0.0002(6)
C15 0.0158(7) 0.0137(7) 0.0151(8) -0.0002(6) -0.0004(6) 0.0001(6)
C16 0.0195(8) 0.0158(8) 0.0179(8) -0.0002(6) -0.0022(6) 0.0000(6)
C17 0.0186(8) 0.0164(8) 0.0149(8) 0.0007(6) -0.0004(6) -0.0009(6)
C18 0.0165(7) 0.0144(7) 0.0145(7) 0.0002(6) 0.0012(6) 0.0002(6)
C19 0.0378(12) 0.0171(9) 0.0350(13) -0.0080(9) 0.0024(10) -0.0042(9)
C20 0.082(2) 0.0156(11) 0.0479(18) -0.0014(11) 0.0018(16) -0.0041(13)
C21 0.0158(9) 0.0354(13) 0.0417(14) -0.0094(10) -0.0050(9) 0.0101(8)
C22 0.0396(16) 0.067(2) 0.0502(19) 0.0020(16) 0.0130(14) 0.0269(15)
C23 0.0291(10) 0.0286(11) 0.0219(10) -0.0116(8) -0.0009(8) -0.0027(8)
C24 0.0549(18) 0.0505(18) 0.0287(13) -0.0161(12) -0.0191(12) 0.0129(14)
C25 0.0317(11) 0.0194(9) 0.0189(9) 0.0044(7) -0.0015(8) 0.0006(8)
C26 0.0546(16) 0.0275(12) 0.0173(10) 0.0017(8) -0.0045(10) -0.0036(11)
_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
W1 C2 2.021(2) . ?
W1 C1 2.030(2) . ?
W1 C4 2.051(2) . ?
W1 C3 2.062(2) . ?
W1 C5 2.149(2) . ?
W1 C6 2.1561(19) . ?
C1 O1 1.141(3) . ?
C2 O2 1.152(3) . ?
C3 O3 1.135(3) . ?
C4 O4 1.136(3) . ?
C5 O5 1.322(2) . ?
C5 C13 1.458(3) . ?
O5 C19 1.453(3) . ?
C6 O6 1.309(2) . ?
C6 C14 1.472(3) . ?
O6 C21 1.452(3) . ?
W2 C8 2.018(2) . ?
W2 C7 2.020(2) . ?
W2 C9 2.050(2) . ?
W2 C10 2.060(2) . ?
W2 C12 2.1597(19) . ?
W2 C11 2.162(2) . ?
C7 O7 1.150(3) . ?
C8 O8 1.147(3) . ?
C9 O9 1.141(3) . ?
C10 O10 1.134(3) . ?
C11 O11 1.321(2) . ?
C11 C17 1.449(3) . ?
O11 C23 1.446(3) . ?
C12 O12 1.317(2) . ?
C12 C18 1.469(3) . ?
O12 C25 1.445(2) . ?
S1 C16 1.719(2) . ?
S1 C13 1.733(2) . ?
S2 C16 1.724(2) . ?
S2 C17 1.738(2) . ?
C13 C14 1.378(3) . ?
C14 C15 1.429(3) . ?
C15 C16 1.398(3) . ?
C15 C18 1.427(3) . ?
C17 C18 1.384(3) . ?
C19 C20 1.508(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.473(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.499(4) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.502(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
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
C2 W1 C1 86.36(10) . . ?
C2 W1 C4 90.53(9) . . ?
C1 W1 C4 92.18(10) . . ?
C2 W1 C3 97.17(9) . . ?
C1 W1 C3 89.14(10) . . ?
C4 W1 C3 172.26(8) . . ?
C2 W1 C5 97.96(9) . . ?
C1 W1 C5 174.94(9) . . ?
C4 W1 C5 90.43(8) . . ?
C3 W1 C5 87.70(8) . . ?
C2 W1 C6 174.51(9) . . ?
C1 W1 C6 99.13(9) . . ?
C4 W1 C6 89.35(8) . . ?
C3 W1 C6 82.91(8) . . ?
C5 W1 C6 76.55(7) . . ?
O1 C1 W1 177.5(3) . . ?
O2 C2 W1 176.3(2) . . ?
O3 C3 W1 174.0(2) . . ?
O4 C4 W1 179.9(3) . . ?
O5 C5 C13 109.38(17) . . ?
O5 C5 W1 138.25(14) . . ?
C13 C5 W1 112.36(13) . . ?
C5 O5 C19 118.48(18) . . ?
O6 C6 C14 109.60(16) . . ?
O6 C6 W1 136.62(13) . . ?
C14 C6 W1 113.58(13) . . ?
C6 O6 C21 119.18(17) . . ?
C8 W2 C7 84.47(10) . . ?
C8 W2 C9 89.70(9) . . ?
C7 W2 C9 93.57(9) . . ?
C8 W2 C10 94.57(10) . . ?
C7 W2 C10 90.45(9) . . ?
C9 W2 C10 174.40(9) . . ?
C8 W2 C12 176.24(9) . . ?
C7 W2 C12 98.75(8) . . ?
C9 W2 C12 88.16(8) . . ?
C10 W2 C12 87.38(8) . . ?
C8 W2 C11 99.47(9) . . ?
C7 W2 C11 175.60(8) . . ?
C9 W2 C11 88.43(8) . . ?
C10 W2 C11 87.31(8) . . ?
C12 W2 C11 77.38(7) . . ?
O7 C7 W2 175.9(2) . . ?
O8 C8 W2 176.0(2) . . ?
O9 C9 W2 178.9(2) . . ?
O10 C10 W2 177.7(2) . . ?
O11 C11 C17 109.21(17) . . ?
O11 C11 W2 137.81(15) . . ?
C17 C11 W2 112.96(13) . . ?
C11 O11 C23 119.37(18) . . ?
O12 C12 C18 108.47(16) . . ?
O12 C12 W2 136.31(14) . . ?
C18 C12 W2 114.76(13) . . ?
C12 O12 C25 120.75(16) . . ?
C16 S1 C13 89.61(9) . . ?
C16 S2 C17 89.67(9) . . ?
C14 C13 C5 119.05(17) . . ?
C14 C13 S1 113.73(14) . . ?
C5 C13 S1 126.97(15) . . ?
C13 C14 C15 111.90(16) . . ?
C13 C14 C6 112.90(16) . . ?
C15 C14 C6 134.06(17) . . ?
C16 C15 C18 110.41(16) . . ?
C16 C15 C14 110.41(16) . . ?
C18 C15 C14 139.17(17) . . ?
C15 C16 S1 114.21(14) . . ?
C15 C16 S2 114.23(15) . . ?
S1 C16 S2 131.56(12) . . ?
C18 C17 C11 119.63(17) . . ?
C18 C17 S2 113.28(15) . . ?
C11 C17 S2 127.04(14) . . ?
C17 C18 C15 112.24(17) . . ?
C17 C18 C12 113.62(17) . . ?
C15 C18 C12 133.19(17) . . ?
O5 C19 C20 107.2(2) . . ?
O5 C19 H19A 110.3 . . ?
C20 C19 H19A 110.3 . . ?
O5 C19 H19B 110.3 . . ?
C20 C19 H19B 110.3 . . ?
H19A C19 H19B 108.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O6 C21 C22 106.5(2) . . ?
O6 C21 H21A 110.4 . . ?
C22 C21 H21A 110.4 . . ?
O6 C21 H21B 110.4 . . ?
C22 C21 H21B 110.4 . . ?
H21A C21 H21B 108.6 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O11 C23 C24 107.4(2) . . ?
O11 C23 H23A 110.2 . . ?
C24 C23 H23A 110.2 . . ?
O11 C23 H23B 110.2 . . ?
C24 C23 H23B 110.2 . . ?
H23A C23 H23B 108.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O12 C25 C26 106.22(18) . . ?
O12 C25 H25A 110.5 . . ?
C26 C25 H25A 110.5 . . ?
O12 C25 H25B 110.5 . . ?
C26 C25 H25B 110.5 . . ?
H25A C25 H25B 108.7 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C13 C5 O5 C19 177.87(19) . . . . ?
W1 C5 O5 C19 -0.8(3) . . . . ?
C14 C6 O6 C21 -172.5(2) . . . . ?
W1 C6 O6 C21 1.9(3) . . . . ?
C17 C11 O11 C23 -179.33(18) . . . . ?
W2 C11 O11 C23 -1.3(3) . . . . ?
C18 C12 O12 C25 -174.73(17) . . . . ?
W2 C12 O12 C25 -3.2(3) . . . . ?
O5 C5 C13 C14 -169.15(18) . . . . ?
W1 C5 C13 C14 9.9(2) . . . . ?
O5 C5 C13 S1 4.8(3) . . . . ?
W1 C5 C13 S1 -176.20(12) . . . . ?
C16 S1 C13 C14 -1.19(17) . . . . ?
C16 S1 C13 C5 -175.38(19) . . . . ?
C5 C13 C14 C15 177.88(18) . . . . ?
S1 C13 C14 C15 3.2(2) . . . . ?
C5 C13 C14 C6 8.3(3) . . . . ?
S1 C13 C14 C6 -166.42(14) . . . . ?
O6 C6 C14 C13 153.20(18) . . . . ?
W1 C6 C14 C13 -22.6(2) . . . . ?
O6 C6 C14 C15 -13.3(3) . . . . ?
W1 C6 C14 C15 170.84(18) . . . . ?
C13 C14 C15 C16 -4.0(2) . . . . ?
C6 C14 C15 C16 162.7(2) . . . . ?
C13 C14 C15 C18 175.0(2) . . . . ?
C6 C14 C15 C18 -18.4(4) . . . . ?
C18 C15 C16 S1 -176.13(14) . . . . ?
C14 C15 C16 S1 3.1(2) . . . . ?
C18 C15 C16 S2 3.6(2) . . . . ?
C14 C15 C16 S2 -177.15(14) . . . . ?
C13 S1 C16 C15 -1.18(17) . . . . ?
C13 S1 C16 S2 179.16(17) . . . . ?
C17 S2 C16 C15 -1.44(17) . . . . ?
C17 S2 C16 S1 178.23(17) . . . . ?
O11 C11 C17 C18 176.76(18) . . . . ?
W2 C11 C17 C18 -1.8(2) . . . . ?
O11 C11 C17 S2 -6.0(3) . . . . ?
W2 C11 C17 S2 175.43(12) . . . . ?
C16 S2 C17 C18 -1.20(17) . . . . ?
C16 S2 C17 C11 -178.55(19) . . . . ?
C11 C17 C18 C15 -178.96(18) . . . . ?
S2 C17 C18 C15 3.5(2) . . . . ?
C11 C17 C18 C12 10.7(3) . . . . ?
S2 C17 C18 C12 -166.86(14) . . . . ?
C16 C15 C18 C17 -4.4(2) . . . . ?
C14 C15 C18 C17 176.6(2) . . . . ?
C16 C15 C18 C12 163.4(2) . . . . ?
C14 C15 C18 C12 -15.6(4) . . . . ?
O12 C12 C18 C17 159.05(17) . . . . ?
W2 C12 C18 C17 -14.5(2) . . . . ?
O12 C12 C18 C15 -8.6(3) . . . . ?
W2 C12 C18 C15 177.77(18) . . . . ?
C5 O5 C19 C20 -170.9(2) . . . . ?
C6 O6 C21 C22 163.9(2) . . . . ?
C11 O11 C23 C24 169.1(2) . . . . ?
C12 O12 C25 C26 166.3(2) . . . . ?
_shelxl_version_number 2014/5
_shelx_res_file
;
TITL mo_ZL228F7_2_0m in P2(1)/c
CELL 0.71073 7.2013 34.2589 12.5924 90.0000 101.9948 90.0000
ZERR 4.00 0.0003 0.0015 0.0005 0.0000 0.0012 0.0000
LATT 1
SYMM -X, 1/2+Y, 1/2-Z
SFAC C H O S W
UNIT 104 80 48 8 8
REM Solution 1 R1 0.101 Rweak 0.005, Alpha= 0.0464 in P2(1)/c
REM Formula: C26 O12 S2 W2
SHEL 999 0.60
L.S. 16
BOND $H
CONF
ACTA
FMAP 2
PLAN 20
SIZE 0.086 0.166 0.296
TEMP -123.00
WGHT 0.019500 2.598900
FVAR 0.11793
W1 5 0.137884 0.276396 0.388555 11.00000 0.01449 0.01763 =
0.01611 -0.00442 0.00093 -0.00074
C1 1 -0.032386 0.307129 0.268717 11.00000 0.02586 0.03020 =
0.02676 -0.00215 -0.00205 -0.00091
O1 3 -0.125340 0.323691 0.198682 11.00000 0.04856 0.05261 =
0.03934 0.01130 -0.01085 0.00865
C2 1 0.102796 0.231148 0.283326 11.00000 0.01961 0.02845 =
0.02343 -0.00876 0.00636 -0.00268
O2 3 0.072380 0.205826 0.221986 11.00000 0.03524 0.03773 =
0.03649 -0.02137 0.01249 -0.00573
C3 1 0.371399 0.300692 0.342887 11.00000 0.02406 0.02226 =
0.02204 -0.00485 0.00432 -0.00052
O3 3 0.500581 0.316295 0.324980 11.00000 0.03409 0.03459 =
0.04206 -0.00539 0.01703 -0.00975
C4 1 -0.088802 0.257768 0.450364 11.00000 0.02025 0.02375 =
0.02347 -0.00776 0.00237 -0.00238
O4 3 -0.214304 0.247467 0.484740 11.00000 0.03204 0.04150 =
0.04461 -0.00642 0.01651 -0.00979
C5 1 0.330651 0.248633 0.520035 11.00000 0.01534 0.01545 =
0.02134 -0.00284 0.00456 -0.00090
O5 3 0.385500 0.212876 0.551548 11.00000 0.02577 0.01310 =
0.02888 -0.00261 0.00048 -0.00093
C6 1 0.192624 0.321055 0.511759 11.00000 0.01409 0.01442 =
0.01762 -0.00131 0.00109 -0.00065
O6 3 0.102860 0.351486 0.538944 11.00000 0.01585 0.01907 =
0.02506 -0.00522 -0.00018 0.00460
W2 5 0.493696 0.466339 0.757574 11.00000 0.02032 0.01349 =
0.01519 -0.00187 0.00293 -0.00012
C7 1 0.332169 0.505215 0.658472 11.00000 0.02972 0.02122 =
0.02442 0.00118 0.00627 0.00193
O7 3 0.242728 0.528959 0.606980 11.00000 0.04911 0.03213 =
0.04081 0.01108 0.00421 0.01319
C8 1 0.568936 0.512838 0.855364 11.00000 0.03641 0.02031 =
0.02383 -0.00541 0.00847 -0.00202
O8 3 0.608312 0.540650 0.905750 11.00000 0.06049 0.02904 =
0.03943 -0.01741 0.01312 -0.01027
C9 1 0.726388 0.475264 0.690513 11.00000 0.02633 0.01781 =
0.02037 -0.00132 0.00236 0.00016
O9 3 0.857743 0.479987 0.654671 11.00000 0.03110 0.03964 =
0.03812 0.00382 0.01248 -0.00079
C10 1 0.265292 0.451620 0.824465 11.00000 0.02634 0.02772 =
0.02171 0.00130 0.00414 0.00429
O10 3 0.139440 0.442350 0.859658 11.00000 0.03105 0.06299 =
0.04215 0.01001 0.01567 0.00044
C11 1 0.651424 0.421295 0.858046 11.00000 0.01767 0.01980 =
0.01445 -0.00221 0.00193 -0.00251
O11 3 0.768270 0.418601 0.953643 11.00000 0.02372 0.02289 =
0.01547 -0.00451 -0.00292 -0.00227
C12 1 0.431411 0.414987 0.656996 11.00000 0.01519 0.01648 =
0.01560 -0.00020 0.00215 0.00001
O12 3 0.368008 0.407746 0.553106 11.00000 0.02346 0.01604 =
0.01439 0.00027 -0.00138 -0.00010
S1 4 0.603998 0.266632 0.712950 11.00000 0.02125 0.01345 =
0.02293 0.00091 -0.00344 0.00217
S2 4 0.730339 0.339569 0.861303 11.00000 0.02400 0.01745 =
0.01851 0.00021 -0.00682 0.00127
C13 1 0.428585 0.276635 0.599490 11.00000 0.01607 0.01331 =
0.01917 -0.00103 0.00119 0.00068
C14 1 0.369713 0.314992 0.592591 11.00000 0.01400 0.01402 =
0.01513 -0.00112 0.00143 0.00025
C15 1 0.475761 0.338164 0.678586 11.00000 0.01578 0.01366 =
0.01508 -0.00016 -0.00039 0.00012
C16 1 0.602626 0.314821 0.750743 11.00000 0.01955 0.01580 =
0.01788 -0.00022 -0.00221 0.00004
C17 1 0.619048 0.382721 0.810680 11.00000 0.01863 0.01636 =
0.01491 0.00069 -0.00038 -0.00086
C18 1 0.493036 0.378001 0.712327 11.00000 0.01650 0.01437 =
0.01448 0.00018 0.00118 0.00017
C19 1 0.299726 0.180205 0.485532 11.00000 0.03780 0.01708 =
0.03500 -0.00803 0.00240 -0.00416
AFIX 23
H19A 2 0.341547 0.179889 0.415450 11.00000 -1.20000
H19B 2 0.159610 0.182370 0.470559 11.00000 -1.20000
AFIX 0
C20 1 0.362845 0.143432 0.548665 11.00000 0.08155 0.01560 =
0.04793 -0.00140 0.00181 -0.00410
AFIX 137
H20A 2 0.501569 0.141517 0.562392 11.00000 -1.50000
H20B 2 0.306669 0.120714 0.506644 11.00000 -1.50000
H20C 2 0.321301 0.144175 0.617974 11.00000 -1.50000
AFIX 0
C21 1 -0.086893 0.360200 0.478126 11.00000 0.01582 0.03544 =
0.04169 -0.00935 -0.00503 0.01012
AFIX 23
H21A 2 -0.163887 0.336066 0.465107 11.00000 -1.20000
H21B 2 -0.081136 0.372027 0.407151 11.00000 -1.20000
AFIX 0
C22 1 -0.170731 0.387820 0.544587 11.00000 0.03963 0.06671 =
0.05018 0.00202 0.01301 0.02689
AFIX 137
H22A 2 -0.169324 0.376243 0.615916 11.00000 -1.50000
H22B 2 -0.301936 0.393551 0.508336 11.00000 -1.50000
H22C 2 -0.096703 0.412039 0.553720 11.00000 -1.50000
AFIX 0
C23 1 0.820328 0.453521 1.017333 11.00000 0.02906 0.02861 =
0.02192 -0.01164 -0.00092 -0.00267
AFIX 23
H23A 2 0.705553 0.468827 1.021717 11.00000 -1.20000
H23B 2 0.905015 0.470019 0.983557 11.00000 -1.20000
AFIX 0
C24 1 0.920479 0.440906 1.128475 11.00000 0.05493 0.05048 =
0.02870 -0.01615 -0.01914 0.01294
AFIX 137
H24A 2 0.831843 0.426597 1.163579 11.00000 -1.50000
H24B 2 0.967664 0.463934 1.171962 11.00000 -1.50000
H24C 2 1.027418 0.423937 1.122559 11.00000 -1.50000
AFIX 0
C25 1 0.312519 0.439245 0.476743 11.00000 0.03174 0.01935 =
0.01886 0.00443 -0.00153 0.00063
AFIX 23
H25A 2 0.409546 0.460150 0.488718 11.00000 -1.20000
H25B 2 0.189696 0.450494 0.485034 11.00000 -1.20000
AFIX 0
C26 1 0.295146 0.421755 0.365739 11.00000 0.05460 0.02747 =
0.01729 0.00171 -0.00446 -0.00361
AFIX 137
H26A 2 0.418699 0.411494 0.358048 11.00000 -1.50000
H26B 2 0.253357 0.441854 0.310571 11.00000 -1.50000
H26C 2 0.202047 0.400505 0.356169 11.00000 -1.50000
AFIX 0
HKLF 4
REM mo_ZL228F7_2_0m in P2(1)/c
REM R1 = 0.0252 for 12986 Fo > 4sig(Fo) and 0.0329 for all 14696 data
REM 383 parameters refined using 0 restraints
END
WGHT 0.0195 2.5987
REM Highest difference peak 1.843, deepest hole -1.595, 1-sigma level 0.137
Q1 1 0.1186 0.2928 0.3637 11.00000 0.05 1.84
Q2 1 0.1461 0.2760 0.3300 11.00000 0.05 1.50
Q3 1 0.5032 0.4652 0.8170 11.00000 0.05 1.44
Q4 1 0.4707 0.4524 0.7206 11.00000 0.05 1.39
Q5 1 0.5261 0.4826 0.7941 11.00000 0.05 1.37
Q6 1 0.1732 0.2941 0.4256 11.00000 0.05 1.36
Q7 1 0.4879 0.4658 0.6999 11.00000 0.05 1.36
Q8 1 -0.2173 0.3608 0.5397 11.00000 0.05 1.36
Q9 1 0.1345 0.2766 0.4454 11.00000 0.05 1.35
Q10 1 0.2380 0.2754 0.3954 11.00000 0.05 1.34
Q11 1 0.0428 0.2762 0.3840 11.00000 0.05 1.33
Q12 1 0.4630 0.4817 0.7188 11.00000 0.05 1.27
Q13 1 0.1036 0.2605 0.3577 11.00000 0.05 1.23
Q14 1 0.5245 0.4476 0.7827 11.00000 0.05 1.22
Q15 1 0.5853 0.4669 0.7589 11.00000 0.05 1.18
Q16 1 0.1765 0.2562 0.4219 11.00000 0.05 1.18
Q17 1 0.3959 0.4641 0.7605 11.00000 0.05 1.15
Q18 1 0.5313 0.4883 0.7453 11.00000 0.05 0.92
Q19 1 0.1019 0.2523 0.4030 11.00000 0.05 0.92
Q20 1 0.4530 0.3952 0.6874 11.00000 0.05 0.82
;
_shelx_res_checksum 79843
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_nvj14_p21c
_database_code_depnum_ccdc_archive 'CCDC 1422363'
_audit_update_record
;
2015-09-04 deposited with the CCDC.
2015-10-09 downloaded from the CCDC.
;
_audit_creation_method SHELXL-2014/7
_shelx_SHELXL_version_number 2014/7
_chemical_name_systematic
5,5,5,5-Tetracarbonyl-4,6-diethoxy-5-tungsta(0)cyclopentatrieno[b]thiophene
_chemical_name_common .
_chemical_melting_point ?
_chemical_formula_moiety 'C14 H12 O6 S W'
_chemical_formula_sum 'C14 H12 O6 S W'
_chemical_formula_weight 492.15
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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 21/c'
_space_group_name_Hall '-P 2ybc'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 7.3338(4)
_cell_length_b 21.4603(12)
_cell_length_c 10.6447(6)
_cell_angle_alpha 90
_cell_angle_beta 108.0170(10)
_cell_angle_gamma 90
_cell_volume 1593.17(15)
_cell_formula_units_Z 4
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 6702
_cell_measurement_theta_min 2.766
_cell_measurement_theta_max 26.589
_exptl_crystal_description prism
_exptl_crystal_colour dark-blue-black
_exptl_crystal_size_min 0.11
_exptl_crystal_size_mid 0.14
_exptl_crystal_size_max 0.38
_exptl_crystal_density_meas .
_exptl_crystal_density_method 'not measured'
_exptl_crystal_density_diffrn 2.052
_exptl_crystal_F_000 936
_exptl_absorpt_coefficient_mu 7.405
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.278
_exptl_absorpt_correction_T_max 0.443
_exptl_absorpt_process_details 'SADABS (Bruker, 2001)'
_exptl_special_details ?
_diffrn_ambient_temperature 293(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 'Bruker (Seimens) P4'
_diffrn_measurement_method '\f and \w scans'
_diffrn_detector 'SMART 1000 CCD'
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number 8550
_diffrn_reflns_av_unetI/netI 0.0264
_diffrn_reflns_av_R_equivalents 0.0260
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_k_max 25
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_limit_l_max 5
_diffrn_reflns_theta_min 2.766
_diffrn_reflns_theta_max 26.589
_diffrn_reflns_theta_full 25.242
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total 3039
_reflns_number_gt 2844
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
;
_computing_data_collection 'SMART (Bruker, 2001)'
_computing_cell_refinement 'SAINT (Bruker, 2001)'
_computing_data_reduction 'SAINT (Bruker, 2001)'
_computing_structure_solution 'SHELXTL (Sheldrick, 1997)'
_computing_structure_refinement
;
SHELXTL and SHELXL-2014 (Sheldrick, 2015)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 1997), POV-RAY (Cason, 2004),
Mercury (Macrae et al., 2008)
;
_computing_publication_material 'SHELXL-2014, PLATON (Spek, 2009)'
_refine_special_details ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0337P)^2^+0.8706P] 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 none
_refine_ls_extinction_coef .
_refine_ls_number_reflns 3039
_refine_ls_number_parameters 224
_refine_ls_number_restraints 10
_refine_ls_R_factor_all 0.0259
_refine_ls_R_factor_gt 0.0240
_refine_ls_wR_factor_ref 0.0637
_refine_ls_wR_factor_gt 0.0624
_refine_ls_goodness_of_fit_ref 1.138
_refine_ls_restrained_S_all 1.144
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 1.404
_refine_diff_density_min -0.526
_refine_diff_density_rms 0.107
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.43483(2) 0.34548(2) 0.70073(2) 0.03871(8) Uani 1 1 d . . . . .
C1 C 0.2549(7) 0.3030(2) 0.5414(4) 0.0563(10) Uani 1 1 d . . . . .
O1 O 0.1577(6) 0.27439(18) 0.4572(3) 0.0866(11) Uani 1 1 d . . . . .
C2 C 0.4914(8) 0.25735(19) 0.7644(4) 0.0573(11) Uani 1 1 d . . . . .
O2 O 0.5135(7) 0.20542(17) 0.7930(4) 0.0884(12) Uani 1 1 d . . . . .
C3 C 0.2230(7) 0.35363(17) 0.7889(4) 0.0470(9) Uani 1 1 d . . . . .
O3 O 0.1071(6) 0.36171(19) 0.8370(4) 0.0739(9) Uani 1 1 d . . . . .
C4 C 0.6517(7) 0.34765(16) 0.6147(5) 0.0490(10) Uani 1 1 d . . . . .
O4 O 0.7701(7) 0.35121(17) 0.5672(5) 0.0794(12) Uani 1 1 d . . . . .
C5 C 0.6217(5) 0.39473(16) 0.8690(3) 0.0389(7) Uani 1 1 d . . . . .
O5 O 0.7461(4) 0.37989(12) 0.9836(2) 0.0454(6) Uani 1 1 d . . . . .
C6 C 0.3786(5) 0.44213(16) 0.6393(3) 0.0346(7) Uani 1 1 d . . . . .
O6 O 0.2734(4) 0.47156(12) 0.5347(2) 0.0434(6) Uani 1 1 d . . . . .
C7 C 0.6074(5) 0.46196(16) 0.8556(3) 0.0373(7) Uani 1 1 d D . . . .
C8 C 0.4819(5) 0.48590(15) 0.7403(4) 0.0375(7) Uani 1 1 d D . . . .
S1 S 0.7257(5) 0.51691(9) 0.9664(3) 0.0457(6) Uani 0.636(6) 1 d D . P A 1
C9 C 0.491(2) 0.5507(4) 0.7515(12) 0.061(5) Uani 0.636(6) 1 d D . P A 1
H9 H 0.4148 0.5755 0.6838 0.073 Uiso 0.636(6) 1 calc R U P A 1
C10 C 0.614(4) 0.5779(5) 0.8645(15) 0.034(3) Uani 0.636(6) 1 d D . P A 1
H10 H 0.6336 0.6202 0.8819 0.041 Uiso 0.636(6) 1 calc R U P A 1
S1A S 0.4612(10) 0.5634(2) 0.7267(6) 0.0449(13) Uani 0.364(6) 1 d D . P A 2
C9A C 0.684(3) 0.5127(6) 0.9372(15) 0.063(9) Uiso 0.364(6) 1 d D . P A 2
H9A H 0.7722 0.5080 1.0210 0.076 Uiso 0.364(6) 1 calc R U P A 2
C10A C 0.620(7) 0.5703(8) 0.884(3) 0.037(5) Uani 0.364(6) 1 d D . P A 2
H10A H 0.6578 0.6080 0.9277 0.045 Uiso 0.364(6) 1 calc R U P A 2
C11 C 0.7825(7) 0.31474(19) 1.0192(4) 0.0564(11) Uani 1 1 d . . . . .
H11A H 0.8329 0.2937 0.9563 0.068 Uiso 1 1 calc R U . . .
H11B H 0.6646 0.2942 1.0190 0.068 Uiso 1 1 calc R U . . .
C12 C 0.9243(8) 0.3125(2) 1.1535(5) 0.0753(15) Uani 1 1 d . . . . .
H12A H 1.0423 0.3312 1.1515 0.113 Uiso 1 1 calc R U . . .
H12B H 0.9471 0.2699 1.1815 0.113 Uiso 1 1 calc R U . . .
H12C H 0.8752 0.3349 1.2141 0.113 Uiso 1 1 calc R U . . .
C13 C 0.1514(6) 0.4363(2) 0.4244(4) 0.0486(9) Uani 1 1 d . . . . .
H13A H 0.0552 0.4137 0.4515 0.058 Uiso 1 1 calc R U . . .
H13B H 0.2273 0.4065 0.3936 0.058 Uiso 1 1 calc R U . . .
C14 C 0.0565(6) 0.4815(2) 0.3160(4) 0.0550(11) Uani 1 1 d . . . . .
H14A H -0.0233 0.5095 0.3460 0.083 Uiso 1 1 calc R U . . .
H14B H -0.0207 0.4590 0.2402 0.083 Uiso 1 1 calc R U . . .
H14C H 0.1528 0.5049 0.2925 0.083 Uiso 1 1 calc R U . . .
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
W1 0.04663(12) 0.03074(11) 0.03288(12) -0.00115(4) 0.00373(8) -0.00200(5)
C1 0.069(3) 0.048(2) 0.043(2) -0.0031(18) 0.005(2) -0.013(2)
O1 0.108(3) 0.077(2) 0.056(2) -0.0211(18) -0.0024(19) -0.030(2)
C2 0.080(3) 0.036(2) 0.047(2) -0.0038(17) 0.007(2) -0.003(2)
O2 0.130(3) 0.043(2) 0.077(3) 0.0034(15) 0.009(2) 0.003(2)
C3 0.050(2) 0.040(2) 0.044(2) -0.0001(15) 0.0060(19) -0.0073(16)
O3 0.072(2) 0.081(2) 0.076(2) -0.003(2) 0.032(2) -0.006(2)
C4 0.053(3) 0.048(2) 0.044(2) -0.0037(15) 0.010(2) 0.0032(16)
O4 0.071(3) 0.099(3) 0.074(3) -0.0090(18) 0.030(2) 0.0003(18)
C5 0.0394(18) 0.0422(19) 0.0343(17) -0.0017(14) 0.0103(14) 0.0001(14)
O5 0.0505(15) 0.0398(14) 0.0363(13) 0.0041(11) -0.0007(11) 0.0011(11)
C6 0.0308(16) 0.0408(17) 0.0312(17) 0.0010(13) 0.0081(13) -0.0006(13)
O6 0.0450(14) 0.0416(14) 0.0390(13) 0.0059(10) 0.0061(11) 0.0029(11)
C7 0.0403(18) 0.0390(18) 0.0312(18) -0.0031(15) 0.0090(14) -0.0070(15)
C8 0.0385(18) 0.0328(18) 0.0400(18) 0.0057(15) 0.0103(15) 0.0010(14)
S1 0.0508(12) 0.0387(10) 0.0446(12) -0.0053(7) 0.0103(11) -0.0051(7)
C9 0.061(7) 0.047(7) 0.079(9) 0.031(5) 0.027(6) 0.018(5)
C10 0.042(5) 0.021(4) 0.039(7) 0.008(3) 0.013(5) 0.003(3)
S1A 0.054(2) 0.0269(19) 0.050(2) -0.005(2) 0.0109(18) -0.0037(18)
C10A 0.057(11) 0.034(9) 0.020(7) -0.002(7) 0.012(7) -0.009(9)
C11 0.065(3) 0.042(2) 0.049(2) 0.0032(17) -0.001(2) 0.0051(18)
C12 0.088(4) 0.050(3) 0.060(3) 0.011(2) -0.017(2) -0.002(2)
C13 0.047(2) 0.054(2) 0.038(2) 0.0028(16) 0.0041(17) -0.0006(17)
C14 0.051(2) 0.070(3) 0.040(2) 0.0094(18) 0.0083(18) 0.0118(18)
_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
W1 C2 2.009(4) . ?
W1 C1 2.017(4) . ?
W1 C3 2.056(5) . ?
W1 C4 2.067(5) . ?
W1 C5 2.164(4) . ?
W1 C6 2.176(3) . ?
C1 O1 1.136(5) . ?
C2 O2 1.153(5) . ?
C3 O3 1.133(6) . ?
C4 O4 1.135(6) . ?
C5 O5 1.317(4) . ?
C5 C7 1.450(5) . ?
O5 C11 1.452(5) . ?
C6 O6 1.304(4) . ?
C6 C8 1.452(5) . ?
O6 C13 1.450(5) . ?
C7 C8 1.385(5) . ?
C7 C9A 1.399(10) . ?
C7 S1 1.703(4) . ?
C8 C9 1.395(9) . ?
C8 S1A 1.673(6) . ?
S1 C10 1.734(8) . ?
C9 C10 1.391(9) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
S1A C10A 1.728(10) . ?
C9A C10A 1.379(10) . ?
C9A H9A 0.9300 . ?
C10A H10A 0.9300 . ?
C11 C12 1.486(6) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.504(5) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
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
C2 W1 C1 82.60(18) . . ?
C2 W1 C3 91.85(18) . . ?
C1 W1 C3 91.84(18) . . ?
C2 W1 C4 93.65(18) . . ?
C1 W1 C4 91.76(18) . . ?
C3 W1 C4 173.77(15) . . ?
C2 W1 C5 99.71(16) . . ?
C1 W1 C5 177.60(16) . . ?
C3 W1 C5 87.43(15) . . ?
C4 W1 C5 88.77(15) . . ?
C2 W1 C6 177.85(15) . . ?
C1 W1 C6 99.47(15) . . ?
C3 W1 C6 87.50(13) . . ?
C4 W1 C6 86.89(13) . . ?
C5 W1 C6 78.22(13) . . ?
O1 C1 W1 174.2(4) . . ?
O2 C2 W1 175.0(4) . . ?
O3 C3 W1 176.1(4) . . ?
O4 C4 W1 177.4(3) . . ?
O5 C5 C7 109.9(3) . . ?
O5 C5 W1 136.8(2) . . ?
C7 C5 W1 113.4(2) . . ?
C5 O5 C11 119.6(3) . . ?
O6 C6 C8 110.7(3) . . ?
O6 C6 W1 136.5(2) . . ?
C8 C6 W1 112.8(2) . . ?
C6 O6 C13 119.5(3) . . ?
C8 C7 C9A 106.9(7) . . ?
C8 C7 C5 117.6(3) . . ?
C9A C7 C5 135.3(7) . . ?
C8 C7 S1 114.4(3) . . ?
C5 C7 S1 128.0(3) . . ?
C7 C8 C9 107.1(5) . . ?
C7 C8 C6 117.9(3) . . ?
C9 C8 C6 135.0(6) . . ?
C7 C8 S1A 117.6(4) . . ?
C6 C8 S1A 124.5(3) . . ?
C7 S1 C10 92.8(4) . . ?
C10 C9 C8 119.5(9) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
C9 C10 S1 106.2(8) . . ?
C9 C10 H10 126.9 . . ?
S1 C10 H10 126.9 . . ?
C8 S1A C10A 89.1(6) . . ?
C10A C9A C7 115.0(12) . . ?
C10A C9A H9A 122.5 . . ?
C7 C9A H9A 122.5 . . ?
C9A C10A S1A 111.3(11) . . ?
C9A C10A H10A 124.4 . . ?
S1A C10A H10A 124.4 . . ?
O5 C11 C12 107.5(4) . . ?
O5 C11 H11A 110.2 . . ?
C12 C11 H11A 110.2 . . ?
O5 C11 H11B 110.2 . . ?
C12 C11 H11B 110.2 . . ?
H11A C11 H11B 108.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O6 C13 C14 108.0(3) . . ?
O6 C13 H13A 110.1 . . ?
C14 C13 H13A 110.1 . . ?
O6 C13 H13B 110.1 . . ?
C14 C13 H13B 110.1 . . ?
H13A C13 H13B 108.4 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 C5 O5 C11 179.4(3) . . . . ?
W1 C5 O5 C11 0.4(5) . . . . ?
C8 C6 O6 C13 -177.1(3) . . . . ?
W1 C6 O6 C13 2.0(5) . . . . ?
O5 C5 C7 C8 -179.9(3) . . . . ?
W1 C5 C7 C8 -0.6(4) . . . . ?
O5 C5 C7 C9A -4.6(15) . . . . ?
W1 C5 C7 C9A 174.6(14) . . . . ?
O5 C5 C7 S1 -0.6(5) . . . . ?
W1 C5 C7 S1 178.6(2) . . . . ?
C5 C7 C8 C9 179.0(8) . . . . ?
S1 C7 C8 C9 -0.3(8) . . . . ?
C9A C7 C8 C6 -178.6(11) . . . . ?
C5 C7 C8 C6 -2.1(5) . . . . ?
S1 C7 C8 C6 178.6(3) . . . . ?
C9A C7 C8 S1A 1.9(11) . . . . ?
C5 C7 C8 S1A 178.4(4) . . . . ?
O6 C6 C8 C7 -177.0(3) . . . . ?
W1 C6 C8 C7 3.7(4) . . . . ?
O6 C6 C8 C9 1.5(11) . . . . ?
W1 C6 C8 C9 -177.8(10) . . . . ?
O6 C6 C8 S1A 2.5(5) . . . . ?
W1 C6 C8 S1A -176.8(4) . . . . ?
C8 C7 S1 C10 -0.2(11) . . . . ?
C5 C7 S1 C10 -179.5(11) . . . . ?
C7 C8 C9 C10 1(2) . . . . ?
C6 C8 C9 C10 -177.7(16) . . . . ?
C8 C9 C10 S1 -1(3) . . . . ?
C7 S1 C10 C9 0.7(19) . . . . ?
C7 C8 S1A C10A -2(2) . . . . ?
C6 C8 S1A C10A 178(2) . . . . ?
C8 C7 C9A C10A -1(3) . . . . ?
C5 C7 C9A C10A -176(3) . . . . ?
C7 C9A C10A S1A -1(5) . . . . ?
C8 S1A C10A C9A 2(4) . . . . ?
C5 O5 C11 C12 -178.8(4) . . . . ?
C6 O6 C13 C14 -176.9(3) . . . . ?
_shelx_res_file
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nvj14_p21c.res created by SHELXL-2014/7
TITL NvJ14_P21c in P21/c
CELL 0.71073 7.3338 21.4603 10.6447 90.000 108.017 90.000
ZERR 4.00 0.0004 0.0012 0.0006 0.000 0.001 0.000
LATT 1
SYMM -X, 0.5+Y, 0.5-Z
SFAC C H O S W
UNIT 56 48 24 4 4
L.S. 16
ACTA
BOND $H
CONF
MPLA 5 C7 C8 C9 C10 S1 C10A C5 C6
MPLA 5 W1 C5 C6 C7 C8 S1 S1A C9 C9A
MPLA 5 C7 C8 C9A C10A S1A C10 C5 C6
FMAP 2
PLAN 10
DFIX 2.564 0.02 S1 C9 S1a C9a
DFIX 1.375 0.01 C9 C10 C9a C10a
DFIX 1.390 0.01 C8 C9 C7 C9a
DFIX 1.721 0.01 C7 S1 S1 C10 C8 S1a S1a C10a
TEMP 20
WGHT 0.033700 0.870600
FVAR 0.16544 0.63608
MOLE 1
W1 5 0.434831 0.345485 0.700734 11.00000 0.04663 0.03074 =
0.03288 -0.00115 0.00373 -0.00200
C1 1 0.254856 0.302967 0.541365 11.00000 0.06911 0.04832 =
0.04306 -0.00310 0.00483 -0.01254
O1 3 0.157717 0.274393 0.457205 11.00000 0.10818 0.07689 =
0.05562 -0.02109 -0.00240 -0.03019
C2 1 0.491438 0.257349 0.764442 11.00000 0.08030 0.03621 =
0.04698 -0.00376 0.00747 -0.00271
O2 3 0.513457 0.205421 0.792986 11.00000 0.13001 0.04330 =
0.07659 0.00342 0.00948 0.00337
C3 1 0.222981 0.353627 0.788915 11.00000 0.05037 0.04050 =
0.04420 -0.00011 0.00601 -0.00731
O3 3 0.107125 0.361706 0.836998 11.00000 0.07195 0.08063 =
0.07557 -0.00345 0.03211 -0.00605
C4 1 0.651704 0.347650 0.614722 11.00000 0.05277 0.04765 =
0.04361 -0.00368 0.01041 0.00316
O4 3 0.770097 0.351207 0.567186 11.00000 0.07100 0.09860 =
0.07386 -0.00900 0.03024 0.00032
C5 1 0.621687 0.394731 0.868966 11.00000 0.03940 0.04219 =
0.03432 -0.00169 0.01034 0.00006
O5 3 0.746057 0.379888 0.983588 11.00000 0.05048 0.03982 =
0.03628 0.00409 -0.00072 0.00105
C6 1 0.378563 0.442133 0.639290 11.00000 0.03081 0.04078 =
0.03116 0.00100 0.00813 -0.00063
O6 3 0.273416 0.471559 0.534726 11.00000 0.04503 0.04156 =
0.03899 0.00589 0.00611 0.00294
C7 1 0.607439 0.461956 0.855628 11.00000 0.04030 0.03896 =
0.03118 -0.00305 0.00899 -0.00704
C8 1 0.481891 0.485898 0.740313 11.00000 0.03845 0.03279 =
0.03999 0.00569 0.01025 0.00100
PART 1
S1 4 0.725665 0.516909 0.966396 21.00000 0.05085 0.03867 =
0.04465 -0.00533 0.01034 -0.00507
C9 1 0.490884 0.550688 0.751457 21.00000 0.06100 0.04711 =
0.07860 0.03068 0.02694 0.01778
AFIX 43
H9 2 0.414820 0.575512 0.683821 21.00000 -1.20000
AFIX 0
C10 1 0.614439 0.577863 0.864460 21.00000 0.04169 0.02104 =
0.03927 0.00761 0.01327 0.00265
AFIX 43
H10 2 0.633574 0.620238 0.881867 21.00000 -1.20000
PART 2
AFIX 0
S1A 4 0.461158 0.563424 0.726652 -21.00000 0.05400 0.02689 =
0.05015 -0.00467 0.01092 -0.00367
C9A 1 0.684345 0.512723 0.937247 -21.00000 0.06316
AFIX 43
H9A 2 0.772176 0.508000 1.021009 -21.00000 -1.20000
AFIX 0
C10A 1 0.620222 0.570300 0.884254 -21.00000 0.05706 0.03426 =
0.02047 -0.00181 0.01237 -0.00903
AFIX 43
H10A 2 0.657752 0.607976 0.927734 -21.00000 -1.20000
PART 0
AFIX 0
C11 1 0.782458 0.314742 1.019215 11.00000 0.06536 0.04226 =
0.04878 0.00320 -0.00109 0.00513
AFIX 23
H11A 2 0.832878 0.293750 0.956328 11.00000 -1.20000
H11B 2 0.664573 0.294193 1.019038 11.00000 -1.20000
AFIX 0
C12 1 0.924312 0.312475 1.153451 11.00000 0.08794 0.05045 =
0.06017 0.01072 -0.01691 -0.00209
AFIX 137
H12A 2 1.042330 0.331167 1.151498 11.00000 -1.50000
H12B 2 0.947087 0.269889 1.181535 11.00000 -1.50000
H12C 2 0.875188 0.334904 1.214066 11.00000 -1.50000
AFIX 0
C13 1 0.151396 0.436321 0.424428 11.00000 0.04722 0.05409 =
0.03821 0.00279 0.00409 -0.00056
AFIX 23
H13A 2 0.055221 0.413731 0.451464 11.00000 -1.20000
H13B 2 0.227254 0.406468 0.393568 11.00000 -1.20000
AFIX 0
C14 1 0.056477 0.481526 0.315959 11.00000 0.05143 0.07002 =
0.03964 0.00938 0.00827 0.01180
AFIX 137
H14A 2 -0.023283 0.509543 0.345996 11.00000 -1.50000
H14B 2 -0.020675 0.459032 0.240174 11.00000 -1.50000
H14C 2 0.152800 0.504861 0.292464 11.00000 -1.50000
AFIX 0
HKLF 4
REM NvJ14_P21c in P21/c
REM R1 = 0.0240 for 2844 Fo > 4sig(Fo) and 0.0259 for all 3039 data
REM 224 parameters refined using 10 restraints
END
WGHT 0.0336 0.9237
REM Highest difference peak 1.404, deepest hole -0.526, 1-sigma level 0.107
Q1 1 0.5610 0.3449 0.7248 11.00000 0.05 1.40
Q2 1 0.2923 0.3455 0.6611 11.00000 0.05 1.05
Q3 1 0.4411 0.3806 0.7174 11.00000 0.05 0.70
Q4 1 0.4155 0.3117 0.6802 11.00000 0.05 0.53
Q5 1 0.4778 0.3199 0.7526 11.00000 0.05 0.52
Q6 1 0.6394 0.5899 0.8628 11.00000 0.05 0.39
Q7 1 0.2130 0.2926 0.4232 11.00000 0.05 0.37
Q8 1 0.5046 0.4697 0.7986 11.00000 0.05 0.37
Q9 1 0.5494 0.4790 0.7917 11.00000 0.05 0.36
Q10 1 0.9332 0.2891 1.1795 11.00000 0.05 0.34
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_shelx_res_checksum 45386