# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2012


data_global
_journal_name_full               Chem.Commun.
_journal_coden_cambridge         0182
_journal_year                    ?

_publ_section_title              
;
Four-Coordinate Quadruply Bonded Dimolybdenum Complexes with Carboxylate and
Terphenyl Ligands
;
#
# Mario Carrasco, Michelle Faust, Riccardo Peloso, Amor Rodr\'iguez,
# Joaqu\'in L\'opez-Serrano, Eleuterio \'Alvarez, Celia Maya, Philip P. Power
# and Ernesto Carmona
#
# To be submitted to Chem. Commun.
# Manuscript number ...........
#=============================================================================80
#
# Person for contact
_publ_contact_author_name        "Dr. Eleuterio \'Alvarez"
_publ_contact_author_address     
;
Instituto de Investigaciones Qu\'imicas, C.S.I.C-Universidad de Sevilla,
Avd. Am\'erico Vespucio, 49., Isla de la Cartuja, 41092 Sevilla, Spain
;
_publ_contact_author_phone       '+34 954 489560'
_publ_contact_author_fax         '+34 954 460565'
_publ_contact_author_email       ealvarez@iiq.csic.es
#=============================================================================80

# Publication details

loop_
_publ_author_name
_publ_author_address

'Mario Carrasco'
;
Instituto de Investigaciones Qu\'imicas, C.S.I.C-Universidad de Sevilla,
Avd. Am\'erico Vespucio, 49., Isla de la Cartuja, 41092 Sevilla, Spain
;
'Michelle Faust'
;
Department of Chemistry, University of California, One Shields Avenue,
Davis, Califonia 95616, United States
;
'Riccardo Peloso'
;
Instituto de Investigaciones Qu\'imicas, C.S.I.C-Universidad de Sevilla,
Avd. Am\'erico Vespucio, 49., Isla de la Cartuja, 41092 Sevilla, Spain
;
A.Rodriguez
;
Instituto de Investigaciones Qu\'imicas, C.S.I.C-Universidad de Sevilla,
Avd. Am\'erico Vespucio, 49., Isla de la Cartuja, 41092 Sevilla, Spain
;
J.Lopez-Serrano
;
Instituto de Investigaciones Qu\'imicas, C.S.I.C-Universidad de Sevilla,
Avd. Am\'erico Vespucio, 49., Isla de la Cartuja, 41092 Sevilla, Spain
;
;
E.Alvarez
;
;
Instituto de Investigaciones Qu\'imicas, C.S.I.C-Universidad de Sevilla,
Avd. Am\'erico Vespucio, 49., Isla de la Cartuja, 41092 Sevilla, Spain
;
'Celia Maya'
;
Instituto de Investigaciones Qu\'imicas, C.S.I.C-Universidad de Sevilla,
Avd. Am\'erico Vespucio, 49., Isla de la Cartuja, 41092 Sevilla, Spain
;
'Philip P. Power'
;
Department of Chemistry, University of California, One Shields Avenue,
Davis, Califonia 95616, United States
;
'Ernesto Carmona'
;
Instituto de Investigaciones Qu\'imicas, C.S.I.C-Universidad de Sevilla,
Avd. Am\'erico Vespucio, 49., Isla de la Cartuja, 41092 Sevilla, Spain
;

_journal_volume                  ?
_journal_page_first              ?
_journal_page_last               ?

#======================================# 
#data for compound 2 (local labelling cm01907c)

data_2
_database_code_depnum_ccdc_archive 'CCDC 862529'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H30 Mo2 O6'
_chemical_formula_sum            'C28 H30 Mo2 O6'
_chemical_formula_weight         654.40

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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.3595(4)
_cell_length_b                   9.8309(4)
_cell_length_c                   16.4231(7)
_cell_angle_alpha                104.220(2)
_cell_angle_beta                 96.024(2)
_cell_angle_gamma                91.870(1)
_cell_volume                     1298.70(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9929
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      30.50

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             660
_exptl_absorpt_coefficient_mu    1.006
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.795
_exptl_absorpt_correction_T_max  0.834
_exptl_absorpt_process_details   
;
SADABS, Bruker (2006). APEX 2. Version 2.1. Bruker Analytical
X-ray Solutions, Madison, Wisconsin, USA.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            33792
_diffrn_reflns_av_R_equivalents  0.0180
_diffrn_reflns_av_sigmaI/netI    0.0176
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         33.14
_reflns_number_total             9722
_reflns_number_gt                8791
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0257P)^2^+0.5784P] 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         9722
_refine_ls_number_parameters     332
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0195
_refine_ls_wR_factor_ref         0.0519
_refine_ls_wR_factor_gt          0.0504
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.850679(10) 0.081239(9) 0.311721(6) 0.01299(2) Uani 1 1 d . . .
Mo2 Mo 1.001992(10) 0.238098(9) 0.289694(6) 0.01202(2) Uani 1 1 d . . .
O1 O 0.75421(10) 0.22290(9) 0.40973(6) 0.01766(15) Uani 1 1 d . . .
O2 O 0.91424(10) 0.39063(9) 0.38537(5) 0.01695(15) Uani 1 1 d . . .
O3 O 1.02097(10) 0.04051(9) 0.40385(5) 0.01700(15) Uani 1 1 d . . .
O4 O 1.18943(10) 0.20535(9) 0.38282(5) 0.01657(15) Uani 1 1 d . . .
O5 O 0.95312(10) -0.07640(8) 0.22620(5) 0.01552(14) Uani 1 1 d . . .
O6 O 1.11381(10) 0.08932(9) 0.20030(5) 0.01559(14) Uani 1 1 d . . .
C1 C 0.80587(14) 0.35125(12) 0.42541(7) 0.0175(2) Uani 1 1 d . . .
C2 C 0.73483(17) 0.45950(14) 0.48989(9) 0.0258(2) Uani 1 1 d . . .
H2A H 0.6466 0.4168 0.5096 0.039 Uiso 1 1 calc R . .
H2B H 0.6967 0.5328 0.4650 0.039 Uiso 1 1 calc R . .
H2C H 0.8155 0.4986 0.5366 0.039 Uiso 1 1 calc R . .
C3 C 1.15681(13) 0.11032(12) 0.41949(7) 0.01603(19) Uani 1 1 d . . .
C4 C 1.28234(15) 0.07696(14) 0.48280(8) 0.0226(2) Uani 1 1 d . . .
H4A H 1.3591 0.0188 0.4537 0.034 Uiso 1 1 calc R . .
H4B H 1.2317 0.0280 0.5181 0.034 Uiso 1 1 calc R . .
H4C H 1.3365 0.1627 0.5171 0.034 Uiso 1 1 calc R . .
C5 C 1.06814(13) -0.03950(12) 0.18955(7) 0.01507(18) Uani 1 1 d . . .
C6 C 1.14815(15) -0.15263(13) 0.13210(8) 0.0215(2) Uani 1 1 d . . .
H6A H 1.1702 -0.2271 0.1593 0.032 Uiso 1 1 calc R . .
H6B H 1.2473 -0.1145 0.1197 0.032 Uiso 1 1 calc R . .
H6C H 1.0782 -0.1888 0.0805 0.032 Uiso 1 1 calc R . .
C7 C 0.85795(12) 0.31093(11) 0.19099(7) 0.01297(17) Uani 1 1 d . . .
C8 C 0.72183(12) 0.23458(11) 0.13999(7) 0.01366(17) Uani 1 1 d . . .
C9 C 0.64198(13) 0.27908(12) 0.07319(7) 0.0172(2) Uani 1 1 d . . .
H9 H 0.5539 0.2254 0.0402 0.021 Uiso 1 1 calc R . .
C10 C 0.69397(14) 0.40400(13) 0.05578(8) 0.0209(2) Uani 1 1 d . . .
H10 H 0.6415 0.4336 0.0110 0.025 Uiso 1 1 calc R . .
C11 C 0.82502(14) 0.48394(13) 0.10599(8) 0.0194(2) Uani 1 1 d . . .
H11 H 0.8589 0.5684 0.0954 0.023 Uiso 1 1 calc R . .
C12 C 0.90624(13) 0.43786(11) 0.17240(7) 0.01437(18) Uani 1 1 d . . .
C13 C 1.05024(13) 0.52311(11) 0.22396(7) 0.01472(18) Uani 1 1 d . . .
C14 C 1.03223(15) 0.63163(12) 0.29514(8) 0.0191(2) Uani 1 1 d . . .
C15 C 1.16970(18) 0.70580(13) 0.34352(9) 0.0253(2) Uani 1 1 d . . .
H15 H 1.1589 0.7780 0.3909 0.030 Uiso 1 1 calc R . .
C16 C 1.32179(17) 0.67295(14) 0.32166(9) 0.0268(3) Uani 1 1 d . . .
H16 H 1.4124 0.7220 0.3549 0.032 Uiso 1 1 calc R . .
C17 C 1.33975(14) 0.56727(13) 0.25039(9) 0.0220(2) Uani 1 1 d . . .
H17 H 1.4424 0.5463 0.2359 0.026 Uiso 1 1 calc R . .
C18 C 1.20479(13) 0.49201(11) 0.20015(8) 0.01607(19) Uani 1 1 d . . .
C19 C 0.86757(17) 0.67027(14) 0.31946(10) 0.0266(3) Uani 1 1 d . . .
H19A H 0.8785 0.7346 0.3744 0.040 Uiso 1 1 calc R . .
H19B H 0.8056 0.5870 0.3206 0.040 Uiso 1 1 calc R . .
H19C H 0.8138 0.7139 0.2788 0.040 Uiso 1 1 calc R . .
C20 C 1.22355(15) 0.38121(13) 0.12084(8) 0.0204(2) Uani 1 1 d . . .
H20A H 1.3355 0.3767 0.1128 0.031 Uiso 1 1 calc R . .
H20B H 1.1646 0.4046 0.0732 0.031 Uiso 1 1 calc R . .
H20C H 1.1825 0.2917 0.1259 0.031 Uiso 1 1 calc R . .
C21 C 0.66390(13) 0.10213(12) 0.15941(7) 0.01502(18) Uani 1 1 d . . .
C22 C 0.68600(14) -0.02993(12) 0.10553(8) 0.0183(2) Uani 1 1 d . . .
C23 C 0.63068(15) -0.15190(13) 0.12548(9) 0.0235(2) Uani 1 1 d . . .
H23 H 0.6417 -0.2390 0.0890 0.028 Uiso 1 1 calc R . .
C24 C 0.55980(15) -0.14523(14) 0.19855(9) 0.0264(3) Uani 1 1 d . . .
H24 H 0.5294 -0.2276 0.2126 0.032 Uiso 1 1 calc R . .
C25 C 0.53387(15) -0.01579(14) 0.25103(9) 0.0233(2) Uani 1 1 d . . .
H25 H 0.4863 -0.0124 0.3001 0.028 Uiso 1 1 calc R . .
C26 C 0.57871(13) 0.11074(12) 0.23097(8) 0.0172(2) Uani 1 1 d . . .
C27 C 0.77111(17) -0.03986(14) 0.02830(9) 0.0253(2) Uani 1 1 d . . .
H27A H 0.8086 -0.1325 0.0104 0.038 Uiso 1 1 calc R . .
H27B H 0.8612 0.0280 0.0415 0.038 Uiso 1 1 calc R . .
H27C H 0.6979 -0.0214 -0.0163 0.038 Uiso 1 1 calc R . .
C28 C 0.51100(14) 0.24640(14) 0.27376(8) 0.0209(2) Uani 1 1 d . . .
H28A H 0.4178 0.2634 0.2390 0.031 Uiso 1 1 calc R . .
H28B H 0.5910 0.3223 0.2819 0.031 Uiso 1 1 calc R . .
H28C H 0.4810 0.2400 0.3276 0.031 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.01185(4) 0.01230(4) 0.01589(5) 0.00579(3) 0.00137(3) -0.00041(3)
Mo2 0.01166(4) 0.01119(4) 0.01381(4) 0.00499(3) 0.00020(3) -0.00055(3)
O1 0.0169(4) 0.0187(4) 0.0186(4) 0.0063(3) 0.0036(3) 0.0015(3)
O2 0.0185(4) 0.0146(3) 0.0176(4) 0.0043(3) 0.0014(3) 0.0008(3)
O3 0.0180(4) 0.0174(4) 0.0172(4) 0.0078(3) 0.0007(3) 0.0014(3)
O4 0.0147(3) 0.0179(4) 0.0171(4) 0.0056(3) -0.0007(3) 0.0006(3)
O5 0.0148(3) 0.0137(3) 0.0185(4) 0.0052(3) 0.0011(3) -0.0001(3)
O6 0.0158(3) 0.0143(3) 0.0176(4) 0.0057(3) 0.0024(3) 0.0003(3)
C1 0.0177(5) 0.0188(5) 0.0158(5) 0.0047(4) 0.0005(4) 0.0030(4)
C2 0.0293(6) 0.0234(6) 0.0241(6) 0.0022(5) 0.0081(5) 0.0055(5)
C3 0.0173(5) 0.0166(5) 0.0139(4) 0.0034(4) 0.0002(4) 0.0037(4)
C4 0.0228(5) 0.0257(6) 0.0197(5) 0.0080(5) -0.0033(4) 0.0059(4)
C5 0.0147(4) 0.0152(4) 0.0155(5) 0.0050(4) -0.0001(3) 0.0016(3)
C6 0.0229(5) 0.0182(5) 0.0232(6) 0.0036(4) 0.0051(4) 0.0041(4)
C7 0.0126(4) 0.0122(4) 0.0150(4) 0.0051(3) 0.0018(3) 0.0011(3)
C8 0.0129(4) 0.0132(4) 0.0158(5) 0.0054(4) 0.0018(3) 0.0007(3)
C9 0.0143(4) 0.0197(5) 0.0186(5) 0.0080(4) -0.0013(4) 0.0003(4)
C10 0.0188(5) 0.0234(5) 0.0237(6) 0.0140(5) -0.0022(4) 0.0017(4)
C11 0.0183(5) 0.0179(5) 0.0258(6) 0.0133(4) 0.0012(4) 0.0011(4)
C12 0.0140(4) 0.0125(4) 0.0181(5) 0.0063(4) 0.0030(3) 0.0017(3)
C13 0.0159(4) 0.0106(4) 0.0191(5) 0.0067(4) 0.0017(4) 0.0002(3)
C14 0.0246(5) 0.0123(4) 0.0216(5) 0.0058(4) 0.0041(4) 0.0011(4)
C15 0.0360(7) 0.0144(5) 0.0234(6) 0.0030(4) -0.0012(5) -0.0025(5)
C16 0.0279(6) 0.0190(5) 0.0313(7) 0.0083(5) -0.0081(5) -0.0082(5)
C17 0.0164(5) 0.0176(5) 0.0337(7) 0.0121(5) -0.0014(4) -0.0027(4)
C18 0.0158(4) 0.0122(4) 0.0217(5) 0.0075(4) 0.0019(4) 0.0001(3)
C19 0.0317(7) 0.0182(5) 0.0321(7) 0.0055(5) 0.0133(5) 0.0072(5)
C20 0.0198(5) 0.0199(5) 0.0236(6) 0.0070(4) 0.0070(4) 0.0026(4)
C21 0.0120(4) 0.0149(4) 0.0185(5) 0.0063(4) -0.0016(3) -0.0015(3)
C22 0.0165(5) 0.0154(5) 0.0212(5) 0.0042(4) -0.0047(4) -0.0014(4)
C23 0.0213(5) 0.0145(5) 0.0315(7) 0.0057(4) -0.0098(5) -0.0039(4)
C24 0.0226(6) 0.0207(6) 0.0380(7) 0.0170(5) -0.0071(5) -0.0081(4)
C25 0.0173(5) 0.0275(6) 0.0290(6) 0.0163(5) 0.0003(4) -0.0051(4)
C26 0.0124(4) 0.0196(5) 0.0212(5) 0.0094(4) 0.0000(4) -0.0019(4)
C27 0.0303(6) 0.0215(6) 0.0219(6) 0.0013(5) 0.0017(5) 0.0034(5)
C28 0.0145(5) 0.0267(6) 0.0241(6) 0.0104(5) 0.0039(4) 0.0040(4)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 Mo2 2.08605(14) . ?
Mo1 O3 2.0878(8) . ?
Mo1 O5 2.0922(9) . ?
Mo1 O1 2.1036(9) . ?
Mo1 C26 2.5712(11) . ?
Mo2 O2 2.1004(9) . ?
Mo2 O6 2.1192(9) . ?
Mo2 O4 2.1609(8) . ?
Mo2 C7 2.1925(10) . ?
O1 C1 1.2753(14) . ?
O2 C1 1.2769(14) . ?
O3 C3 1.2759(14) . ?
O4 C3 1.2665(14) . ?
O5 C5 1.2745(13) . ?
O6 C5 1.2747(13) . ?
C1 C2 1.4920(18) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C4 1.5003(16) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 C6 1.4967(17) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 C12 1.4119(14) . ?
C7 C8 1.4124(15) . ?
C8 C9 1.3934(15) . ?
C8 C21 1.4923(15) . ?
C9 C10 1.3937(16) . ?
C9 H9 0.9300 . ?
C10 C11 1.3904(17) . ?
C10 H10 0.9300 . ?
C11 C12 1.4012(15) . ?
C11 H11 0.9300 . ?
C12 C13 1.4967(15) . ?
C13 C14 1.4007(17) . ?
C13 C18 1.4102(15) . ?
C14 C15 1.3974(18) . ?
C14 C19 1.5078(18) . ?
C15 C16 1.384(2) . ?
C15 H15 0.9300 . ?
C16 C17 1.386(2) . ?
C16 H16 0.9300 . ?
C17 C18 1.3969(16) . ?
C17 H17 0.9300 . ?
C18 C20 1.5049(17) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.4101(16) . ?
C21 C26 1.4234(16) . ?
C22 C23 1.3956(17) . ?
C22 C27 1.5024(19) . ?
C23 C24 1.382(2) . ?
C23 H23 0.9300 . ?
C24 C25 1.388(2) . ?
C24 H24 0.9300 . ?
C25 C26 1.4118(16) . ?
C25 H25 0.9300 . ?
C26 C28 1.5051(18) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 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
Mo2 Mo1 O3 92.30(2) . . ?
Mo2 Mo1 O5 92.16(2) . . ?
O3 Mo1 O5 85.94(3) . . ?
Mo2 Mo1 O1 92.64(2) . . ?
O3 Mo1 O1 87.61(3) . . ?
O5 Mo1 O1 172.11(3) . . ?
Mo2 Mo1 C26 103.24(2) . . ?
O3 Mo1 C26 161.19(3) . . ?
O5 Mo1 C26 103.74(4) . . ?
O1 Mo1 C26 81.23(4) . . ?
Mo1 Mo2 O2 91.21(2) . . ?
Mo1 Mo2 O6 91.66(2) . . ?
O2 Mo2 O6 174.21(3) . . ?
Mo1 Mo2 O4 91.47(2) . . ?
O2 Mo2 O4 88.65(3) . . ?
O6 Mo2 O4 86.25(3) . . ?
Mo1 Mo2 C7 103.21(3) . . ?
O2 Mo2 C7 91.49(4) . . ?
O6 Mo2 C7 92.75(4) . . ?
O4 Mo2 C7 165.31(4) . . ?
C1 O1 Mo1 116.55(8) . . ?
C1 O2 Mo2 118.01(8) . . ?
C3 O3 Mo1 118.35(7) . . ?
C3 O4 Mo2 115.61(7) . . ?
C5 O5 Mo1 117.64(7) . . ?
C5 O6 Mo2 116.69(7) . . ?
O1 C1 O2 121.56(11) . . ?
O1 C1 C2 119.64(11) . . ?
O2 C1 C2 118.77(11) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O4 C3 O3 122.26(10) . . ?
O4 C3 C4 119.17(10) . . ?
O3 C3 C4 118.57(10) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O5 C5 O6 121.70(11) . . ?
O5 C5 C6 117.87(10) . . ?
O6 C5 C6 120.43(10) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C12 C7 C8 116.33(9) . . ?
C12 C7 Mo2 119.46(8) . . ?
C8 C7 Mo2 124.11(7) . . ?
C9 C8 C7 122.17(10) . . ?
C9 C8 C21 119.89(10) . . ?
C7 C8 C21 117.93(9) . . ?
C8 C9 C10 120.07(10) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
C11 C10 C9 119.43(10) . . ?
C11 C10 H10 120.3 . . ?
C9 C10 H10 120.3 . . ?
C10 C11 C12 120.30(10) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C11 C12 C7 121.67(10) . . ?
C11 C12 C13 119.48(9) . . ?
C7 C12 C13 118.84(9) . . ?
C14 C13 C18 120.37(10) . . ?
C14 C13 C12 120.63(10) . . ?
C18 C13 C12 119.00(10) . . ?
C15 C14 C13 119.08(12) . . ?
C15 C14 C19 119.83(12) . . ?
C13 C14 C19 121.09(11) . . ?
C16 C15 C14 120.68(13) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C15 C16 C17 120.33(12) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 H16 119.8 . . ?
C16 C17 C18 120.46(12) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C17 C18 C13 119.04(11) . . ?
C17 C18 C20 120.57(11) . . ?
C13 C18 C20 120.38(10) . . ?
C14 C19 H19A 109.5 . . ?
C14 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C14 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C26 120.14(10) . . ?
C22 C21 C8 120.68(10) . . ?
C26 C21 C8 119.11(10) . . ?
C23 C22 C21 119.32(12) . . ?
C23 C22 C27 120.14(12) . . ?
C21 C22 C27 120.53(11) . . ?
C24 C23 C22 121.01(12) . . ?
C24 C23 H23 119.5 . . ?
C22 C23 H23 119.5 . . ?
C23 C24 C25 120.14(11) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C24 C25 C26 120.99(12) . . ?
C24 C25 H25 119.5 . . ?
C26 C25 H25 119.5 . . ?
C25 C26 C21 118.02(11) . . ?
C25 C26 C28 120.17(11) . . ?
C21 C26 C28 120.81(10) . . ?
C25 C26 Mo1 83.09(7) . . ?
C21 C26 Mo1 86.50(6) . . ?
C28 C26 Mo1 109.93(8) . . ?
C22 C27 H27A 109.5 . . ?
C22 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C22 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 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
O3 Mo1 Mo2 O2 -88.22(3) . . . . ?
O5 Mo1 Mo2 O2 -174.24(3) . . . . ?
O1 Mo1 Mo2 O2 -0.50(3) . . . . ?
C26 Mo1 Mo2 O2 81.11(4) . . . . ?
O3 Mo1 Mo2 O6 86.75(3) . . . . ?
O5 Mo1 Mo2 O6 0.73(3) . . . . ?
O1 Mo1 Mo2 O6 174.47(3) . . . . ?
C26 Mo1 Mo2 O6 -103.92(4) . . . . ?
O3 Mo1 Mo2 O4 0.46(3) . . . . ?
O5 Mo1 Mo2 O4 -85.56(3) . . . . ?
O1 Mo1 Mo2 O4 88.18(3) . . . . ?
C26 Mo1 Mo2 O4 169.79(4) . . . . ?
O3 Mo1 Mo2 C7 179.97(4) . . . . ?
O5 Mo1 Mo2 C7 93.95(4) . . . . ?
O1 Mo1 Mo2 C7 -92.32(4) . . . . ?
C26 Mo1 Mo2 C7 -10.71(4) . . . . ?
Mo2 Mo1 O1 C1 1.52(8) . . . . ?
O3 Mo1 O1 C1 93.71(8) . . . . ?
C26 Mo1 O1 C1 -101.48(8) . . . . ?
Mo1 Mo2 O2 C1 -0.32(8) . . . . ?
O4 Mo2 O2 C1 -91.76(8) . . . . ?
C7 Mo2 O2 C1 102.94(8) . . . . ?
Mo2 Mo1 O3 C3 -1.40(8) . . . . ?
O5 Mo1 O3 C3 90.60(9) . . . . ?
O1 Mo1 O3 C3 -93.95(9) . . . . ?
C26 Mo1 O3 C3 -147.39(11) . . . . ?
Mo1 Mo2 O4 C3 0.27(8) . . . . ?
O2 Mo2 O4 C3 91.44(8) . . . . ?
O6 Mo2 O4 C3 -91.30(8) . . . . ?
C7 Mo2 O4 C3 -177.83(13) . . . . ?
Mo2 Mo1 O5 C5 1.29(8) . . . . ?
O3 Mo1 O5 C5 -90.87(8) . . . . ?
C26 Mo1 O5 C5 105.48(8) . . . . ?
Mo1 Mo2 O6 C5 -3.03(7) . . . . ?
O4 Mo2 O6 C5 88.33(8) . . . . ?
C7 Mo2 O6 C5 -106.34(8) . . . . ?
Mo1 O1 C1 O2 -2.13(14) . . . . ?
Mo1 O1 C1 C2 175.76(9) . . . . ?
Mo2 O2 C1 O1 1.63(14) . . . . ?
Mo2 O2 C1 C2 -176.28(8) . . . . ?
Mo2 O4 C3 O3 -1.44(15) . . . . ?
Mo2 O4 C3 C4 177.80(8) . . . . ?
Mo1 O3 C3 O4 1.98(15) . . . . ?
Mo1 O3 C3 C4 -177.28(8) . . . . ?
Mo1 O5 C5 O6 -4.07(14) . . . . ?
Mo1 O5 C5 C6 176.57(8) . . . . ?
Mo2 O6 C5 O5 4.80(14) . . . . ?
Mo2 O6 C5 C6 -175.85(8) . . . . ?
Mo1 Mo2 C7 C12 166.23(8) . . . . ?
O2 Mo2 C7 C12 74.63(9) . . . . ?
O6 Mo2 C7 C12 -101.42(9) . . . . ?
O4 Mo2 C7 C12 -15.7(2) . . . . ?
Mo1 Mo2 C7 C8 -17.53(9) . . . . ?
O2 Mo2 C7 C8 -109.13(9) . . . . ?
O6 Mo2 C7 C8 74.82(9) . . . . ?
O4 Mo2 C7 C8 160.51(12) . . . . ?
C12 C7 C8 C9 1.96(16) . . . . ?
Mo2 C7 C8 C9 -174.39(9) . . . . ?
C12 C7 C8 C21 -178.11(10) . . . . ?
Mo2 C7 C8 C21 5.54(14) . . . . ?
C7 C8 C9 C10 -1.20(18) . . . . ?
C21 C8 C9 C10 178.87(11) . . . . ?
C8 C9 C10 C11 -0.50(19) . . . . ?
C9 C10 C11 C12 1.33(19) . . . . ?
C10 C11 C12 C7 -0.51(18) . . . . ?
C10 C11 C12 C13 178.06(11) . . . . ?
C8 C7 C12 C11 -1.10(16) . . . . ?
Mo2 C7 C12 C11 175.43(9) . . . . ?
C8 C7 C12 C13 -179.67(10) . . . . ?
Mo2 C7 C12 C13 -3.15(14) . . . . ?
C11 C12 C13 C14 88.05(14) . . . . ?
C7 C12 C13 C14 -93.35(13) . . . . ?
C11 C12 C13 C18 -92.36(13) . . . . ?
C7 C12 C13 C18 86.25(13) . . . . ?
C18 C13 C14 C15 -1.82(17) . . . . ?
C12 C13 C14 C15 177.77(10) . . . . ?
C18 C13 C14 C19 177.45(11) . . . . ?
C12 C13 C14 C19 -2.96(16) . . . . ?
C13 C14 C15 C16 0.02(18) . . . . ?
C19 C14 C15 C16 -179.26(12) . . . . ?
C14 C15 C16 C17 1.1(2) . . . . ?
C15 C16 C17 C18 -0.47(19) . . . . ?
C16 C17 C18 C13 -1.30(17) . . . . ?
C16 C17 C18 C20 177.54(11) . . . . ?
C14 C13 C18 C17 2.45(16) . . . . ?
C12 C13 C18 C17 -177.14(10) . . . . ?
C14 C13 C18 C20 -176.39(10) . . . . ?
C12 C13 C18 C20 4.02(15) . . . . ?
C9 C8 C21 C22 72.00(14) . . . . ?
C7 C8 C21 C22 -107.94(12) . . . . ?
C9 C8 C21 C26 -104.93(13) . . . . ?
C7 C8 C21 C26 75.13(13) . . . . ?
C26 C21 C22 C23 -3.19(16) . . . . ?
C8 C21 C22 C23 179.91(10) . . . . ?
C26 C21 C22 C27 178.03(10) . . . . ?
C8 C21 C22 C27 1.13(16) . . . . ?
C21 C22 C23 C24 -2.25(17) . . . . ?
C27 C22 C23 C24 176.54(11) . . . . ?
C22 C23 C24 C25 3.82(18) . . . . ?
C23 C24 C25 C26 0.11(18) . . . . ?
C24 C25 C26 C21 -5.39(17) . . . . ?
C24 C25 C26 C28 163.25(11) . . . . ?
C24 C25 C26 Mo1 -87.68(11) . . . . ?
C22 C21 C26 C25 6.89(16) . . . . ?
C8 C21 C26 C25 -176.17(10) . . . . ?
C22 C21 C26 C28 -161.67(10) . . . . ?
C8 C21 C26 C28 15.28(15) . . . . ?
C22 C21 C26 Mo1 87.16(10) . . . . ?
C8 C21 C26 Mo1 -95.90(9) . . . . ?
Mo2 Mo1 C26 C25 171.63(7) . . . . ?
O3 Mo1 C26 C25 -43.41(15) . . . . ?
O5 Mo1 C26 C25 76.05(8) . . . . ?
O1 Mo1 C26 C25 -97.71(8) . . . . ?
Mo2 Mo1 C26 C21 52.85(7) . . . . ?
O3 Mo1 C26 C21 -162.19(10) . . . . ?
O5 Mo1 C26 C21 -42.73(7) . . . . ?
O1 Mo1 C26 C21 143.51(7) . . . . ?
Mo2 Mo1 C26 C28 -68.73(8) . . . . ?
O3 Mo1 C26 C28 76.23(14) . . . . ?
O5 Mo1 C26 C28 -164.31(7) . . . . ?
O1 Mo1 C26 C28 21.94(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        33.14
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         0.742
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.071


###END

#========================================================================# 
#data for compound 3 (local labelling ea15508a)
#========================================================================
data_3
_database_code_depnum_ccdc_archive 'CCDC 862530'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H44 Mo2 O4'
_chemical_formula_sum            'C46 H44 Mo2 O4'
_chemical_formula_weight         852.69

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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.3268(4)
_cell_length_b                   20.3348(9)
_cell_length_c                   11.1270(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.516(2)
_cell_angle_gamma                90.00
_cell_volume                     1863.29(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    7428
_cell_measurement_theta_min      2.67
_cell_measurement_theta_max      28.21

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             872
_exptl_absorpt_coefficient_mu    0.718
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9018
_exptl_absorpt_correction_T_max  0.9650
_exptl_absorpt_process_details   
;
SADABS, Bruker (2006). APEX 2. Version 2.1. Bruker Analytical
X-ray Solutions, Madison, Wisconsin, USA.
;

_diffrn_ambient_temperature      173(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-Nonius X8kappa APEX II CCD area detector'
;
_diffrn_measurement_method       'phi and omega scans with narrow frames'
_diffrn_detector_area_resol_mean 8.26
_diffrn_standards_decay_%        0
_diffrn_reflns_number            32923
_diffrn_reflns_av_R_equivalents  0.0756
_diffrn_reflns_av_sigmaI/netI    0.0621
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.00
_diffrn_reflns_theta_max         30.66
_reflns_number_total             5654
_reflns_number_gt                3648
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker (2006). APEX 2. Version 2.1.'
_computing_cell_refinement       'Bruker (2006). APEX 2. Version 2.1.'
_computing_data_reduction        'Bruker (2006). APEX 2. Version 2.1.'
_computing_structure_solution    'Bruker (2006). APEX 2. Version 2.1.'
_computing_structure_refinement  'XL, SHELXTL v. 6.14 (Bruker, 2003)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.14 (Bruker, 2003)'
_computing_publication_material  'XCIF, SHELXTL v. 6.14 (Bruker, 2003)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0587P)^2^+1.6241P] 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         5654
_refine_ls_number_parameters     239
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0437
_refine_ls_wR_factor_ref         0.1281
_refine_ls_wR_factor_gt          0.0972
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.04077(4) 0.451991(15) 0.48860(3) 0.01959(10) Uani 1 1 d . . .
O1 O -0.1975(3) 0.41472(14) 0.4729(2) 0.0300(6) Uani 1 1 d . . .
O2 O 0.2852(3) 0.48279(16) 0.5075(3) 0.0330(7) Uani 1 1 d . . .
C1 C 0.0876(4) 0.42159(18) 0.6791(3) 0.0182(7) Uani 1 1 d . . .
C2 C 0.1454(4) 0.35720(19) 0.7058(3) 0.0206(7) Uani 1 1 d . . .
C3 C 0.1770(5) 0.3347(2) 0.8252(3) 0.0273(8) Uani 1 1 d . . .
H3 H 0.2132 0.2908 0.8406 0.033 Uiso 1 1 calc R . .
C4 C 0.1566(5) 0.3752(2) 0.9217(3) 0.0320(9) Uani 1 1 d . . .
H4 H 0.1788 0.3593 1.0027 0.038 Uiso 1 1 calc R . .
C5 C 0.1040(5) 0.4385(2) 0.8990(3) 0.0270(9) Uani 1 1 d . . .
H5 H 0.0909 0.4668 0.9647 0.032 Uiso 1 1 calc R . .
C6 C 0.0695(4) 0.46166(18) 0.7795(3) 0.0220(8) Uani 1 1 d . . .
C7 C 0.1784(4) 0.30859(18) 0.6101(3) 0.0208(7) Uani 1 1 d . . .
C8 C 0.3356(5) 0.3039(2) 0.5788(3) 0.0256(8) Uani 1 1 d . . .
C9 C 0.3698(5) 0.2563(2) 0.4985(4) 0.0310(9) Uani 1 1 d . . .
H9 H 0.4747 0.2543 0.4750 0.037 Uiso 1 1 calc R . .
C10 C 0.2515(6) 0.2111(2) 0.4516(4) 0.0353(10) Uani 1 1 d . . .
H10 H 0.2762 0.1777 0.3975 0.042 Uiso 1 1 calc R . .
C11 C 0.0997(5) 0.2149(2) 0.4836(4) 0.0328(9) Uani 1 1 d . . .
H11 H 0.0199 0.1836 0.4516 0.039 Uiso 1 1 calc R . .
C12 C 0.0588(5) 0.26351(19) 0.5620(3) 0.0248(8) Uani 1 1 d . . .
C13 C 0.4729(4) 0.34954(18) 0.6410(3) 0.0202(7) Uani 1 1 d . . .
H13A H 0.5039 0.3360 0.7258 0.030 Uiso 1 1 calc R . .
H13B H 0.4341 0.3951 0.6383 0.030 Uiso 1 1 calc R . .
H13C H 0.5673 0.3463 0.5981 0.030 Uiso 1 1 calc R . .
C14 C -0.1131(4) 0.26506(19) 0.5994(3) 0.0245(8) Uani 1 1 d . . .
H14A H -0.1039 0.2658 0.6883 0.037 Uiso 1 1 calc R . .
H14B H -0.1736 0.2258 0.5680 0.037 Uiso 1 1 calc R . .
H14C H -0.1708 0.3045 0.5658 0.037 Uiso 1 1 calc R . .
C15 C 0.0121(5) 0.53061(19) 0.7617(3) 0.0243(8) Uani 1 1 d . . .
C16 C -0.1565(5) 0.5441(2) 0.7469(4) 0.0340(9) Uani 1 1 d . . .
C17 C -0.2071(6) 0.6097(3) 0.7329(4) 0.0441(12) Uani 1 1 d . . .
H17 H -0.3200 0.6193 0.7189 0.053 Uiso 1 1 calc R . .
C18 C -0.0982(7) 0.6602(2) 0.7391(4) 0.0446(13) Uani 1 1 d . . .
H18 H -0.1356 0.7042 0.7289 0.053 Uiso 1 1 calc R . .
C19 C 0.0651(7) 0.6473(2) 0.7599(4) 0.0450(12) Uani 1 1 d . . .
H19 H 0.1398 0.6828 0.7654 0.054 Uiso 1 1 calc R . .
C20 C 0.1236(6) 0.5836(2) 0.7730(4) 0.0338(10) Uani 1 1 d . . .
C21 C -0.2789(5) 0.4896(2) 0.7588(4) 0.0307(9) Uani 1 1 d . . .
H21A H -0.2877 0.4829 0.8448 0.046 Uiso 1 1 calc R . .
H21B H -0.2424 0.4487 0.7248 0.046 Uiso 1 1 calc R . .
H21C H -0.3851 0.5020 0.7146 0.046 Uiso 1 1 calc R . .
C22 C -0.3094(5) 0.4559(3) 0.4762(4) 0.0367(10) Uani 1 1 d . . .
H22 H -0.4181 0.4403 0.4661 0.044 Uiso 1 1 calc R . .
C29 C 0.3060(6) 0.5698(2) 0.8069(5) 0.0418(11) Uani 1 1 d . . .
H29A H 0.3680 0.6075 0.7839 0.063 Uiso 1 1 calc R . .
H29B H 0.3347 0.5305 0.7637 0.063 Uiso 1 1 calc R . .
H29C H 0.3316 0.5625 0.8947 0.063 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.02635(16) 0.01482(15) 0.01779(14) 0.00040(15) 0.00390(10) 0.00258(14)
O1 0.0313(15) 0.0268(15) 0.0297(14) 0.0076(13) -0.0031(12) -0.0082(12)
O2 0.0265(14) 0.0378(18) 0.0359(16) 0.0129(15) 0.0088(12) 0.0066(13)
C1 0.0191(16) 0.0153(17) 0.0200(16) -0.0015(15) 0.0022(13) -0.0033(13)
C2 0.0246(18) 0.0188(18) 0.0182(15) 0.0020(15) 0.0028(13) -0.0009(14)
C3 0.037(2) 0.022(2) 0.0233(18) 0.0051(17) 0.0049(16) 0.0050(17)
C4 0.045(2) 0.032(2) 0.0193(17) 0.0033(18) 0.0049(17) 0.0080(19)
C5 0.036(2) 0.026(2) 0.0192(16) -0.0019(16) 0.0061(15) 0.0091(16)
C6 0.0260(18) 0.018(2) 0.0214(16) -0.0015(16) 0.0035(14) 0.0023(14)
C7 0.0296(19) 0.0140(17) 0.0185(16) 0.0014(15) 0.0031(14) 0.0028(14)
C8 0.030(2) 0.0201(19) 0.0266(18) 0.0045(17) 0.0054(15) 0.0064(15)
C9 0.035(2) 0.027(2) 0.033(2) 0.0033(19) 0.0111(17) 0.0141(18)
C10 0.053(3) 0.026(2) 0.028(2) -0.0077(19) 0.0062(19) 0.011(2)
C11 0.043(2) 0.021(2) 0.032(2) -0.0055(19) -0.0021(18) 0.0023(18)
C12 0.031(2) 0.0171(18) 0.0258(18) 0.0008(16) 0.0025(15) -0.0001(15)
C13 0.0143(15) 0.0193(18) 0.0285(18) 0.0040(16) 0.0077(13) 0.0032(13)
C14 0.0283(19) 0.0162(18) 0.0290(18) -0.0056(16) 0.0046(15) -0.0048(15)
C15 0.038(2) 0.0198(19) 0.0157(15) -0.0004(15) 0.0060(15) 0.0058(15)
C16 0.040(2) 0.032(2) 0.0265(18) -0.005(2) -0.0066(16) 0.010(2)
C17 0.048(3) 0.039(3) 0.042(3) -0.009(2) -0.004(2) 0.022(2)
C18 0.083(4) 0.021(2) 0.029(2) 0.000(2) 0.005(2) 0.020(2)
C19 0.075(4) 0.021(2) 0.045(3) -0.006(2) 0.029(3) -0.002(2)
C20 0.049(3) 0.024(2) 0.032(2) -0.0058(19) 0.0169(19) -0.0033(19)
C21 0.027(2) 0.029(2) 0.034(2) -0.0056(19) -0.0024(16) 0.0034(17)
C22 0.029(2) 0.047(3) 0.033(2) 0.016(2) -0.0001(16) -0.011(2)
C29 0.044(3) 0.029(2) 0.056(3) -0.008(2) 0.021(2) -0.012(2)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 Mo1 2.0949(6) 3_566 ?
Mo1 O1 2.106(3) . ?
Mo1 O2 2.110(3) . ?
Mo1 C1 2.187(3) . ?
O1 C22 1.257(5) . ?
O2 C22 1.272(6) 3_566 ?
C1 C6 1.409(5) . ?
C1 C2 1.412(5) . ?
C2 C3 1.392(5) . ?
C2 C7 1.508(5) . ?
C3 C4 1.383(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.371(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.399(5) . ?
C5 H5 0.9500 . ?
C6 C15 1.485(5) . ?
C7 C12 1.400(5) . ?
C7 C8 1.406(5) . ?
C8 C9 1.375(5) . ?
C8 C13 1.553(5) . ?
C9 C10 1.392(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.365(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.393(5) . ?
C11 H11 0.9500 . ?
C12 C14 1.550(5) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C20 1.415(6) . ?
C15 C16 1.416(6) . ?
C16 C17 1.401(6) . ?
C16 C21 1.525(6) . ?
C17 C18 1.364(7) . ?
C17 H17 0.9500 . ?
C18 C19 1.370(7) . ?
C18 H18 0.9500 . ?
C19 C20 1.384(6) . ?
C19 H19 0.9500 . ?
C20 C29 1.535(7) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 O2 1.272(6) 3_566 ?
C22 H22 0.9500 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 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
Mo1 Mo1 O1 91.56(9) 3_566 . ?
Mo1 Mo1 O2 92.09(9) 3_566 . ?
O1 Mo1 O2 176.09(11) . . ?
Mo1 Mo1 C1 99.24(10) 3_566 . ?
O1 Mo1 C1 90.53(11) . . ?
O2 Mo1 C1 87.50(12) . . ?
C22 O1 Mo1 116.8(3) . . ?
C22 O2 Mo1 115.8(3) 3_566 . ?
C6 C1 C2 116.2(3) . . ?
C6 C1 Mo1 125.5(3) . . ?
C2 C1 Mo1 118.2(2) . . ?
C3 C2 C1 121.1(3) . . ?
C3 C2 C7 115.5(3) . . ?
C1 C2 C7 123.4(3) . . ?
C4 C3 C2 121.2(4) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C5 C4 C3 119.2(4) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C4 C5 C6 120.4(4) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C5 C6 C1 121.9(3) . . ?
C5 C6 C15 117.5(3) . . ?
C1 C6 C15 120.7(3) . . ?
C12 C7 C8 119.8(3) . . ?
C12 C7 C2 120.3(3) . . ?
C8 C7 C2 119.5(3) . . ?
C9 C8 C7 119.9(4) . . ?
C9 C8 C13 120.0(3) . . ?
C7 C8 C13 120.0(3) . . ?
C8 C9 C10 120.4(4) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
C11 C10 C9 119.7(4) . . ?
C11 C10 H10 120.1 . . ?
C9 C10 H10 120.1 . . ?
C10 C11 C12 121.7(4) . . ?
C10 C11 H11 119.2 . . ?
C12 C11 H11 119.2 . . ?
C11 C12 C7 118.5(4) . . ?
C11 C12 C14 120.2(3) . . ?
C7 C12 C14 121.1(3) . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C20 C15 C16 119.3(4) . . ?
C20 C15 C6 120.9(4) . . ?
C16 C15 C6 119.5(4) . . ?
C17 C16 C15 118.3(4) . . ?
C17 C16 C21 120.6(4) . . ?
C15 C16 C21 120.8(4) . . ?
C18 C17 C16 121.6(5) . . ?
C18 C17 H17 119.2 . . ?
C16 C17 H17 119.2 . . ?
C17 C18 C19 120.0(4) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
C18 C19 C20 121.5(5) . . ?
C18 C19 H19 119.3 . . ?
C20 C19 H19 119.3 . . ?
C19 C20 C15 119.1(4) . . ?
C19 C20 C29 121.1(4) . . ?
C15 C20 C29 119.6(4) . . ?
C16 C21 H21A 109.5 . . ?
C16 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C16 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O1 C22 O2 123.7(4) . 3_566 ?
O1 C22 H22 118.2 . . ?
O2 C22 H22 118.2 3_566 . ?
C20 C29 H29A 109.5 . . ?
C20 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C20 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 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
Mo1 Mo1 O1 C22 2.5(3) 3_566 . . . ?
C1 Mo1 O1 C22 101.7(3) . . . . ?
Mo1 Mo1 O2 C22 -0.9(3) 3_566 . . 3_566 ?
C1 Mo1 O2 C22 -100.0(3) . . . 3_566 ?
Mo1 Mo1 C1 C6 -2.5(3) 3_566 . . . ?
O1 Mo1 C1 C6 -94.1(3) . . . . ?
O2 Mo1 C1 C6 89.3(3) . . . . ?
Mo1 Mo1 C1 C2 179.5(3) 3_566 . . . ?
O1 Mo1 C1 C2 87.9(3) . . . . ?
O2 Mo1 C1 C2 -88.8(3) . . . . ?
C6 C1 C2 C3 2.0(5) . . . . ?
Mo1 C1 C2 C3 -179.8(3) . . . . ?
C6 C1 C2 C7 -177.4(3) . . . . ?
Mo1 C1 C2 C7 0.8(5) . . . . ?
C1 C2 C3 C4 -1.6(6) . . . . ?
C7 C2 C3 C4 177.9(4) . . . . ?
C2 C3 C4 C5 0.1(6) . . . . ?
C3 C4 C5 C6 0.7(6) . . . . ?
C4 C5 C6 C1 -0.2(6) . . . . ?
C4 C5 C6 C15 179.7(4) . . . . ?
C2 C1 C6 C5 -1.2(5) . . . . ?
Mo1 C1 C6 C5 -179.2(3) . . . . ?
C2 C1 C6 C15 179.0(3) . . . . ?
Mo1 C1 C6 C15 0.9(5) . . . . ?
C3 C2 C7 C12 86.7(4) . . . . ?
C1 C2 C7 C12 -93.8(5) . . . . ?
C3 C2 C7 C8 -86.4(4) . . . . ?
C1 C2 C7 C8 93.1(4) . . . . ?
C12 C7 C8 C9 1.8(5) . . . . ?
C2 C7 C8 C9 175.0(4) . . . . ?
C12 C7 C8 C13 -174.3(3) . . . . ?
C2 C7 C8 C13 -1.1(5) . . . . ?
C7 C8 C9 C10 -2.4(6) . . . . ?
C13 C8 C9 C10 173.6(4) . . . . ?
C8 C9 C10 C11 1.3(6) . . . . ?
C9 C10 C11 C12 0.5(6) . . . . ?
C10 C11 C12 C7 -1.1(6) . . . . ?
C10 C11 C12 C14 -178.1(4) . . . . ?
C8 C7 C12 C11 0.0(5) . . . . ?
C2 C7 C12 C11 -173.2(4) . . . . ?
C8 C7 C12 C14 177.0(3) . . . . ?
C2 C7 C12 C14 3.8(5) . . . . ?
C5 C6 C15 C20 82.1(5) . . . . ?
C1 C6 C15 C20 -98.0(4) . . . . ?
C5 C6 C15 C16 -90.7(5) . . . . ?
C1 C6 C15 C16 89.2(5) . . . . ?
C20 C15 C16 C17 5.7(6) . . . . ?
C6 C15 C16 C17 178.6(4) . . . . ?
C20 C15 C16 C21 -168.1(4) . . . . ?
C6 C15 C16 C21 4.8(5) . . . . ?
C15 C16 C17 C18 -3.1(7) . . . . ?
C21 C16 C17 C18 170.7(4) . . . . ?
C16 C17 C18 C19 -0.3(7) . . . . ?
C17 C18 C19 C20 1.1(7) . . . . ?
C18 C19 C20 C15 1.6(7) . . . . ?
C18 C19 C20 C29 -174.8(4) . . . . ?
C16 C15 C20 C19 -5.0(6) . . . . ?
C6 C15 C20 C19 -177.8(4) . . . . ?
C16 C15 C20 C29 171.5(4) . . . . ?
C6 C15 C20 C29 -1.3(6) . . . . ?
Mo1 O1 C22 O2 -2.5(5) . . . 3_566 ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        30.66
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.927
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.134

_iucr_refine_instructions_details 
;
TITL ea15508a in P2(1)/n
CELL 0.71073 8.3268 20.3348 11.1270 90.000 98.516 90.000
ZERR 2.00 0.0004 0.0009 0.0004 0.000 0.002 0.000
LATT 1
SYMM 0.5-X, 0.5+Y, 0.5-Z
SFAC C H O Mo
UNIT 92 88 8 4
OMIT -1 6 3
OMIT 4 7 1
L.S. 12
ACTA
BOND $H
FMAP 2
PLAN 10
CONF
SIZE 0.250 0.120 0.050
TEMP -100
WGHT 0.058700 1.624100
FVAR 0.37160
MOLE 1
MO1 4 0.040768 0.451991 0.488604 11.00000 0.02635
0.01482 0.01779 0.00040 0.00390 0.00258
O1 3 -0.197460 0.414724 0.472890 11.00000 0.03133
0.02676 0.02974 0.00757 -0.00311 -0.00825
O2 3 0.285234 0.482789 0.507505 11.00000 0.02651
0.03784 0.03590 0.01293 0.00881 0.00660
C1 1 0.087570 0.421593 0.679073 11.00000 0.01906
0.01526 0.01998 -0.00152 0.00223 -0.00327
C2 1 0.145381 0.357201 0.705841 11.00000 0.02457
0.01884 0.01816 0.00199 0.00282 -0.00086
C3 1 0.177007 0.334739 0.825191 11.00000 0.03672
0.02217 0.02329 0.00508 0.00492 0.00500
AFIX 43
H3 2 0.213238 0.290829 0.840641 11.00000 -1.20000
AFIX 0
C4 1 0.156617 0.375213 0.921656 11.00000 0.04494
0.03188 0.01928 0.00333 0.00494 0.00803
AFIX 43
H4 2 0.178825 0.359343 1.002717 11.00000 -1.20000
AFIX 0
C5 1 0.103986 0.438506 0.898965 11.00000 0.03630
0.02602 0.01918 -0.00191 0.00613 0.00907
AFIX 43
H5 2 0.090871 0.466813 0.964736 11.00000 -1.20000
AFIX 0
C6 1 0.069472 0.461659 0.779518 11.00000 0.02604
0.01847 0.02141 -0.00152 0.00346 0.00229
C7 1 0.178448 0.308594 0.610087 11.00000 0.02963
0.01404 0.01848 0.00136 0.00311 0.00284
C8 1 0.335574 0.303949 0.578772 11.00000 0.03029
0.02014 0.02660 0.00448 0.00538 0.00640
C9 1 0.369752 0.256348 0.498543 11.00000 0.03484
0.02702 0.03311 0.00329 0.01112 0.01410
AFIX 43
H9 2 0.474746 0.254325 0.474999 11.00000 -1.20000
AFIX 0
C10 1 0.251456 0.211110 0.451613 11.00000 0.05282
0.02575 0.02753 -0.00773 0.00616 0.01150
AFIX 43
H10 2 0.276238 0.177721 0.397528 11.00000 -1.20000
AFIX 0
C11 1 0.099680 0.214908 0.483609 11.00000 0.04294
0.02090 0.03234 -0.00547 -0.00209 0.00231
AFIX 43
H11 2 0.019903 0.183628 0.451628 11.00000 -1.20000
AFIX 0
C12 1 0.058831 0.263508 0.561989 11.00000 0.03107
0.01712 0.02580 0.00078 0.00245 -0.00014
C13 1 0.472870 0.349542 0.640969 11.00000 0.01425
0.01928 0.02854 0.00400 0.00767 0.00320
AFIX 137
H13A 2 0.503876 0.336031 0.725773 11.00000 -1.50000
H13B 2 0.434114 0.395100 0.638253 11.00000 -1.50000
H13C 2 0.567269 0.346272 0.598135 11.00000 -1.50000
AFIX 0
C14 1 -0.113146 0.265062 0.599435 11.00000 0.02827
0.01624 0.02896 -0.00559 0.00459 -0.00476
AFIX 137
H14A 2 -0.103851 0.265846 0.688258 11.00000 -1.50000
H14B 2 -0.173581 0.225822 0.567960 11.00000 -1.50000
H14C 2 -0.170752 0.304501 0.565764 11.00000 -1.50000
AFIX 0
C15 1 0.012147 0.530615 0.761705 11.00000 0.03799
0.01981 0.01572 -0.00042 0.00596 0.00579
C16 1 -0.156471 0.544112 0.746855 11.00000 0.03976
0.03218 0.02652 -0.00515 -0.00658 0.00955
C17 1 -0.207084 0.609744 0.732931 11.00000 0.04780
0.03931 0.04183 -0.00936 -0.00434 0.02222
AFIX 43
H17 2 -0.319963 0.619345 0.718873 11.00000 -1.20000
AFIX 0
C18 1 -0.098213 0.660160 0.739073 11.00000 0.08279
0.02092 0.02912 0.00031 0.00531 0.02037
AFIX 43
H18 2 -0.135560 0.704239 0.728922 11.00000 -1.20000
AFIX 0
C19 1 0.065081 0.647251 0.759889 11.00000 0.07482
0.02107 0.04516 -0.00600 0.02931 -0.00172
AFIX 43
H19 2 0.139778 0.682821 0.765421 11.00000 -1.20000
AFIX 0
C20 1 0.123591 0.583567 0.773030 11.00000 0.04868
0.02380 0.03220 -0.00576 0.01693 -0.00332
C21 1 -0.278870 0.489567 0.758832 11.00000 0.02697
0.02907 0.03387 -0.00555 -0.00241 0.00340
AFIX 137
H21A 2 -0.287736 0.482933 0.844837 11.00000 -1.50000
H21B 2 -0.242385 0.448705 0.724779 11.00000 -1.50000
H21C 2 -0.385123 0.502023 0.714573 11.00000 -1.50000
AFIX 0
C22 1 -0.309408 0.455862 0.476243 11.00000 0.02900
0.04704 0.03259 0.01622 -0.00015 -0.01109
AFIX 43
H22 2 -0.418126 0.440270 0.466076 11.00000 -1.20000
AFIX 0
C29 1 0.305972 0.569767 0.806871 11.00000 0.04428
0.02949 0.05587 -0.00799 0.02146 -0.01230
AFIX 137
H29A 2 0.368013 0.607501 0.783861 11.00000 -1.50000
H29B 2 0.334733 0.530492 0.763665 11.00000 -1.50000
H29C 2 0.331576 0.562498 0.894688 11.00000 -1.50000
HKLF 4
END
;

###END