# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_global

#------------------ AUDIT DETAILS -------------------------------------------#

_audit_creation_date             2013-06-06
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_update_record             ?


#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_name_common            chisholm1939
_chemical_formula_moiety         'C50 H64 Mo2 O9, C4 H8 O'
_chemical_formula_sum            'C54 H72 Mo2 O10'
_chemical_formula_weight         1072.99
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
_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, -z'

_cell_length_a                   10.2136(2)
_cell_length_b                   10.3526(2)
_cell_length_c                   12.6092(2)
_cell_angle_alpha                83.0670(10)
_cell_angle_beta                 80.8170(10)
_cell_angle_gamma                84.8880(10)
_cell_volume                     1303.23(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5934
_cell_measurement_theta_min      0.74
_cell_measurement_theta_max      27.485
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             560
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.739
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_ub_11      0.0448338
_diffrn_orient_matrix_ub_12      -0.0853352
_diffrn_orient_matrix_ub_13      -0.020196
_diffrn_orient_matrix_ub_21      -0.0315445
_diffrn_orient_matrix_ub_22      -0.0419214
_diffrn_orient_matrix_ub_23      0.074286
_diffrn_orient_matrix_ub_31      -0.0829561
_diffrn_orient_matrix_ub_32      -0.0218449
_diffrn_orient_matrix_ub_33      -0.0245824
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_reflns_av_R_equivalents  0.059
_diffrn_reflns_number            11602
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.646
_diffrn_reflns_theta_max         27.519
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_ful 1
_diffrn_reflns_point_group_measured_fraction_max 0.997
_reflns_number_total             5984
_reflns_number_gt                4445
_reflns_threshold_expression     'I > 2\s(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 The TiPB ligand was severely disordered over two positions. The central
 carbon of the carboxylate (C1A/C1B) was the pivot point for the disorder
 and was restrained using the EXYZ and EADP commands. The two disordered parts
 (C1A > C16A/C1B > C16B) were modeled using the SAME command.
 The THF moiety coordinated axially was also disordered and was modeled in the 
 same manner as the TiPB, using the SAME command. The thermal ellipsoids were
 further restrained using the SIMU command. 
;
_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^)+(0.0764P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5984
_refine_ls_number_parameters     462
_refine_ls_number_restraints     103
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0426
_refine_ls_wR_factor_ref         0.1363
_refine_ls_wR_factor_gt          0.1005
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_restrained_S_all      1.117
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.647
_refine_diff_density_min         -1.192
_refine_diff_density_rms         0.257

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
C1A C 0.3960(3) 1.1686(3) 0.6467(3) 0.0322(8) Uani 0.362(6) d A 1
C2A C 0.346(4) 1.252(5) 0.737(4) 0.031(4) Uani 0.362(6) d A 1
C3A C 0.217(3) 1.240(3) 0.796(3) 0.034(8) Uani 0.362(6) d A 1
C4A C 0.168(2) 1.333(2) 0.866(2) 0.033(5) Uani 0.362(6) d A 1
H4A H 0.0825 1.3253 0.9077 0.039 Uiso 0.362(6) calc A 1
C5A C 0.2400(13) 1.4384(16) 0.8766(13) 0.030(4) Uani 0.362(6) d A 1
C6A C 0.3627(18) 1.451(2) 0.812(2) 0.034(5) Uani 0.362(6) d A 1
H6A H 0.4043 1.5307 0.8057 0.041 Uiso 0.362(6) calc A 1
C7A C 0.4272(17) 1.3470(15) 0.7547(13) 0.025(4) Uani 0.362(6) d A 1
C8A C 0.5629(16) 1.3657(17) 0.6855(11) 0.029(4) Uani 0.362(6) d A 1
H8A H 0.565 1.3172 0.6212 0.034 Uiso 0.362(6) calc A 1
C9A C 0.673(2) 1.298(3) 0.7474(16) 0.073(7) Uani 0.362(6) d A 1
H9A1 H 0.7595 1.3074 0.7022 0.11 Uiso 0.362(6) calc A 1
H9A2 H 0.6577 1.2054 0.7655 0.11 Uiso 0.362(6) calc A 1
H9A3 H 0.671 1.3387 0.814 0.11 Uiso 0.362(6) calc A 1
C10A C 0.589(3) 1.505(2) 0.642(2) 0.044(5) Uani 0.362(6) d A 1
H10A H 0.5172 1.5433 0.603 0.066 Uiso 0.362(6) calc A 1
H10B H 0.6738 1.5059 0.5925 0.066 Uiso 0.362(6) calc A 1
H10C H 0.5944 1.5551 0.702 0.066 Uiso 0.362(6) calc A 1
C11A C 0.132(2) 1.132(2) 0.782(3) 0.043(10) Uani 0.362(6) d A 1
H11A H 0.1551 1.1114 0.7058 0.052 Uiso 0.362(6) calc A 1
C12A C 0.164(2) 1.0072(19) 0.8543(19) 0.040(4) Uani 0.362(6) d A 1
H12A H 0.1098 0.9384 0.8421 0.06 Uiso 0.362(6) calc A 1
H12B H 0.1444 1.0239 0.9303 0.06 Uiso 0.362(6) calc A 1
H12C H 0.2584 0.9792 0.8367 0.06 Uiso 0.362(6) calc A 1
C13A C -0.016(2) 1.167(3) 0.803(3) 0.059(6) Uani 0.362(6) d A 1
H13A H -0.0636 1.0941 0.7883 0.088 Uiso 0.362(6) calc A 1
H13B H -0.0377 1.2448 0.7545 0.088 Uiso 0.362(6) calc A 1
H13C H -0.0428 1.1843 0.8779 0.088 Uiso 0.362(6) calc A 1
C14A C 0.1886(14) 1.5383(14) 0.9554(11) 0.038(4) Uani 0.362(6) d A 1
H14A H 0.1096 1.5038 1.0044 0.046 Uiso 0.362(6) calc A 1
C15A C 0.145(2) 1.6631(14) 0.8977(14) 0.098(5) Uani 0.362(6) d A 1
H15A H 0.1005 1.7215 0.9502 0.146 Uiso 0.362(6) calc A 1
H15B H 0.0825 1.6472 0.8499 0.146 Uiso 0.362(6) calc A 1
H15C H 0.222 1.7036 0.8547 0.146 Uiso 0.362(6) calc A 1
C16A C 0.2942(14) 1.5604(14) 1.0270(10) 0.068(2) Uani 0.362(6) d A 1
H16A H 0.3087 1.4812 1.0759 0.102 Uiso 0.362(6) calc A 1
H16B H 0.2621 1.6333 1.0694 0.102 Uiso 0.362(6) calc A 1
H16C H 0.378 1.5805 0.9806 0.102 Uiso 0.362(6) calc A 1
C1B C 0.3960(3) 1.1686(3) 0.6467(3) 0.0322(8) Uani 0.638(6) d A 2
C2B C 0.349(2) 1.269(3) 0.723(2) 0.031(4) Uani 0.638(6) d A 2
C3B C 0.2328(16) 1.2491(16) 0.7974(16) 0.036(5) Uani 0.638(6) d A 2
C4B C 0.2016(12) 1.3312(15) 0.8781(12) 0.044(4) Uani 0.638(6) d A 2
H4B H 0.1211 1.3219 0.9269 0.053 Uiso 0.638(6) calc A 2
C5B C 0.2842(11) 1.4272(9) 0.8904(8) 0.045(3) Uani 0.638(6) d A 2
C6B C 0.4000(12) 1.4411(14) 0.8171(13) 0.048(4) Uani 0.638(6) d A 2
H6B H 0.4619 1.4992 0.8289 0.057 Uiso 0.638(6) calc A 2
C7B C 0.4288(10) 1.3713(9) 0.7254(8) 0.033(3) Uani 0.638(6) d A 2
C8B C 0.5591(9) 1.3859(10) 0.6469(7) 0.031(2) Uani 0.638(6) d A 2
H8B H 0.553 1.3398 0.5828 0.037 Uiso 0.638(6) calc A 2
C9B C 0.6760(12) 1.3181(13) 0.7010(9) 0.059(3) Uani 0.638(6) d A 2
H9B1 H 0.759 1.3266 0.6504 0.088 Uiso 0.638(6) calc A 2
H9B2 H 0.6613 1.2255 0.721 0.088 Uiso 0.638(6) calc A 2
H9B3 H 0.682 1.3591 0.766 0.088 Uiso 0.638(6) calc A 2
C10B C 0.5811(17) 1.5280(13) 0.6068(15) 0.056(4) Uani 0.638(6) d A 2
H10D H 0.5044 1.568 0.574 0.084 Uiso 0.638(6) calc A 2
H10E H 0.6615 1.5329 0.5528 0.084 Uiso 0.638(6) calc A 2
H10F H 0.5916 1.5748 0.6677 0.084 Uiso 0.638(6) calc A 2
C11B C 0.1448(14) 1.1427(12) 0.7850(12) 0.034(4) Uani 0.638(6) d A 2
H11B H 0.1846 1.1013 0.7185 0.041 Uiso 0.638(6) calc A 2
C12B C 0.1421(17) 1.0372(13) 0.8808(12) 0.074(5) Uani 0.638(6) d A 2
H12D H 0.0852 0.9694 0.8713 0.112 Uiso 0.638(6) calc A 2
H12E H 0.1069 1.0759 0.9477 0.112 Uiso 0.638(6) calc A 2
H12F H 0.2325 0.9985 0.885 0.112 Uiso 0.638(6) calc A 2
C13B C 0.0045(14) 1.1941(17) 0.7718(16) 0.070(5) Uani 0.638(6) d A 2
H13D H -0.0484 1.1211 0.7668 0.105 Uiso 0.638(6) calc A 2
H13E H 0.0061 1.2549 0.7058 0.105 Uiso 0.638(6) calc A 2
H13F H -0.0353 1.2395 0.8343 0.105 Uiso 0.638(6) calc A 2
C14B C 0.2450(15) 1.5177(8) 0.9772(8) 0.083(4) Uani 0.638(6) d A 2
H14B H 0.335 1.52 0.9984 0.099 Uiso 0.638(6) calc A 2
C15B C 0.2253(14) 1.6529(8) 0.9415(8) 0.098(5) Uani 0.638(6) d A 2
H15D H 0.2089 1.7029 1.0041 0.146 Uiso 0.638(6) calc A 2
H15E H 0.1486 1.6671 0.9026 0.146 Uiso 0.638(6) calc A 2
H15F H 0.3048 1.6817 0.8933 0.146 Uiso 0.638(6) calc A 2
C16B C 0.1766(9) 1.4646(7) 1.0827(5) 0.068(2) Uani 0.638(6) d A 2
H16D H 0.2149 1.3763 1.1017 0.102 Uiso 0.638(6) calc A 2
H16E H 0.0818 1.4617 1.0791 0.102 Uiso 0.638(6) calc A 2
H16F H 0.1875 1.5204 1.1377 0.102 Uiso 0.638(6) calc A 2
C17 C 0.2818(3) 0.8568(3) 0.5473(3) 0.0336(8) Uani 1 d . .
C18 C 0.1691(4) 0.7735(4) 0.5676(3) 0.0416(9) Uani 1 d . .
C19 C 0.1760(4) 0.6551(4) 0.6316(4) 0.0551(12) Uani 1 d . .
H19 H 0.2528 0.6288 0.6646 0.066 Uiso 1 calc . .
C20 C 0.0721(5) 0.5755(5) 0.6476(5) 0.0817(18) Uani 1 d . .
H20 H 0.0786 0.4938 0.6904 0.098 Uiso 1 calc . .
C21 C -0.0415(5) 0.6129(5) 0.6021(5) 0.090(2) Uani 1 d . .
H21 H -0.1135 0.5581 0.6143 0.108 Uiso 1 calc . .
C22 C -0.0492(5) 0.7314(5) 0.5383(5) 0.0813(18) Uani 1 d . .
H22 H -0.1269 0.7581 0.5066 0.098 Uiso 1 calc . .
C23 C 0.0549(4) 0.8100(4) 0.5207(4) 0.0578(12) Uani 1 d . .
H23 H 0.0492 0.8904 0.476 0.069 Uiso 1 calc . .
Mo1 Mo 0.54553(3) 0.93956(3) 0.55886(2) 0.02861(13) Uani 1 d . .
O1 O 0.4665(2) 1.0664(2) 0.67658(18) 0.0293(5) Uani 1 d . .
O2 O 0.7178(2) 1.0444(2) 0.52356(19) 0.0315(5) Uani 1 d . .
O3 O 0.3796(2) 0.8268(2) 0.60034(18) 0.0299(5) Uani 1 d . .
O5 O 0.6309(2) 0.8070(2) 0.44888(18) 0.0289(5) Uani 1 d . .
O4A O 0.6611(17) 0.8350(12) 0.7098(15) 0.047(3) Uani 0.50(3) d B 3
C24A C 0.776(2) 0.885(3) 0.7445(19) 0.093(7) Uani 0.50(3) d B 3
H24A H 0.7946 0.9718 0.7045 0.111 Uiso 0.50(3) calc B 3
H24B H 0.8561 0.825 0.73 0.111 Uiso 0.50(3) calc B 3
C25A C 0.741(3) 0.897(3) 0.8661(15) 0.116(8) Uani 0.50(3) d B 3
H25A H 0.7967 0.8324 0.9072 0.14 Uiso 0.50(3) calc B 3
H25B H 0.7562 0.9855 0.8819 0.14 Uiso 0.50(3) calc B 3
C26A C 0.602(3) 0.872(2) 0.8949(14) 0.098(7) Uani 0.50(3) d B 3
H26A H 0.5446 0.9546 0.8957 0.117 Uiso 0.50(3) calc B 3
H26B H 0.5844 0.8207 0.9665 0.117 Uiso 0.50(3) calc B 3
C27A C 0.578(3) 0.796(3) 0.8068(18) 0.073(7) Uani 0.50(3) d B 3
H27A H 0.5965 0.7014 0.8279 0.087 Uiso 0.50(3) calc B 3
H27B H 0.4836 0.8104 0.7958 0.087 Uiso 0.50(3) calc B 3
O4B O 0.6374(13) 0.8291(13) 0.7434(11) 0.033(3) Uani 0.50(3) d B 4
C24B C 0.7314(19) 0.9057(17) 0.7799(14) 0.059(5) Uani 0.50(3) d B 4
H24C H 0.7527 0.9827 0.7273 0.071 Uiso 0.50(3) calc B 4
H24D H 0.8148 0.8524 0.79 0.071 Uiso 0.50(3) calc B 4
C25B C 0.659(3) 0.947(3) 0.8873(13) 0.124(8) Uani 0.50(3) d B 4
H25C H 0.7166 0.9246 0.944 0.149 Uiso 0.50(3) calc B 4
H25D H 0.6382 1.0427 0.8804 0.149 Uiso 0.50(3) calc B 4
C26B C 0.5381(18) 0.8816(19) 0.9174(14) 0.069(4) Uani 0.50(3) d B 4
H26C H 0.4598 0.9454 0.9236 0.083 Uiso 0.50(3) calc B 4
H26D H 0.5385 0.8268 0.9874 0.083 Uiso 0.50(3) calc B 4
C27B C 0.535(2) 0.799(3) 0.8287(15) 0.051(5) Uani 0.50(3) d B 4
H27C H 0.5463 0.706 0.8564 0.061 Uiso 0.50(3) calc B 4
H27D H 0.4483 0.8151 0.8025 0.061 Uiso 0.50(3) calc B 4

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
C1A 0.0244(18) 0.0238(18) 0.052(2) -0.0134(16) -0.0086(16) -0.0036(14)
C2A 0.034(2) 0.022(7) 0.040(8) -0.006(7) -0.013(3) 0.003(3)
C3A 0.035(12) 0.040(17) 0.028(12) -0.016(10) -0.003(8) 0.007(9)
C4A 0.031(9) 0.019(7) 0.052(10) -0.009(6) -0.017(8) 0.003(6)
C5A 0.028(7) 0.033(7) 0.040(7) -0.017(5) -0.030(6) 0.011(6)
C6A 0.027(10) 0.017(6) 0.064(11) -0.012(6) -0.021(9) 0.001(7)
C7A 0.036(7) 0.015(7) 0.024(8) 0.012(6) -0.014(5) -0.002(5)
C8A 0.046(8) 0.026(7) 0.018(8) 0.006(6) -0.021(6) -0.008(5)
C9A 0.063(11) 0.094(15) 0.072(15) -0.015(12) -0.051(12) 0.019(9)
C10A 0.027(7) 0.040(12) 0.063(14) -0.003(8) -0.004(8) -0.001(7)
C11A 0.045(16) 0.032(13) 0.056(17) -0.023(11) -0.001(11) -0.014(11)
C12A 0.042(8) 0.021(8) 0.061(11) -0.015(6) -0.009(7) -0.002(6)
C13A 0.031(9) 0.033(12) 0.100(16) 0.013(9) 0.009(8) -0.002(8)
C14A 0.041(7) 0.043(8) 0.035(7) -0.012(5) -0.028(5) 0.024(6)
C15A 0.178(15) 0.035(4) 0.068(7) -0.022(4) 0.025(6) -0.001(6)
C16A 0.111(6) 0.053(4) 0.047(4) -0.025(3) -0.022(4) 0.004(4)
C1B 0.0244(18) 0.0238(18) 0.052(2) -0.0134(16) -0.0086(16) -0.0036(14)
C2B 0.034(2) 0.022(7) 0.040(8) -0.006(7) -0.013(3) 0.003(3)
C3B 0.046(8) 0.015(6) 0.050(9) -0.004(5) -0.015(6) -0.006(5)
C4B 0.044(7) 0.045(6) 0.043(6) -0.013(4) -0.004(6) 0.002(5)
C5B 0.060(7) 0.030(5) 0.052(5) -0.016(4) -0.022(6) -0.004(5)
C6B 0.042(7) 0.043(6) 0.068(7) -0.028(5) -0.019(6) -0.006(5)
C7B 0.047(5) 0.015(4) 0.039(6) 0.003(4) -0.021(4) -0.001(3)
C8B 0.025(3) 0.033(5) 0.037(6) -0.005(4) -0.013(4) 0.002(3)
C9B 0.050(5) 0.060(6) 0.079(9) -0.014(6) -0.042(6) -0.001(4)
C10B 0.052(6) 0.027(5) 0.089(13) -0.008(5) -0.005(6) -0.006(4)
C11B 0.036(7) 0.029(7) 0.036(8) -0.006(5) 0.004(5) -0.004(5)
C12B 0.111(12) 0.042(8) 0.076(9) 0.008(6) -0.029(8) -0.032(7)
C13B 0.055(8) 0.045(8) 0.114(13) 0.000(7) -0.019(8) -0.021(5)
C14B 0.151(12) 0.037(5) 0.061(6) -0.032(5) 0.007(7) -0.017(7)
C15B 0.178(15) 0.035(4) 0.068(7) -0.022(4) 0.025(6) -0.001(6)
C16B 0.111(6) 0.053(4) 0.047(4) -0.025(3) -0.022(4) 0.004(4)
C17 0.0261(18) 0.0221(18) 0.054(2) -0.0092(16) -0.0090(16) 0.0018(14)
C18 0.0265(19) 0.028(2) 0.072(3) -0.0057(18) -0.0140(18) -0.0002(15)
C19 0.035(2) 0.039(2) 0.093(3) 0.008(2) -0.022(2) -0.0095(19)
C20 0.056(3) 0.047(3) 0.146(5) 0.030(3) -0.040(3) -0.028(2)
C21 0.044(3) 0.063(3) 0.167(6) 0.023(4) -0.041(3) -0.025(3)
C22 0.034(3) 0.055(3) 0.160(5) 0.012(3) -0.041(3) -0.012(2)
C23 0.030(2) 0.033(2) 0.113(4) 0.007(2) -0.028(2) -0.0045(18)
Mo1 0.02375(19) 0.02007(18) 0.0448(2) -0.00817(12) -0.01147(13) 0.00107(11)
O1 0.0257(12) 0.0230(12) 0.0428(13) -0.0111(10) -0.0120(10) 0.0009(10)
O2 0.0229(12) 0.0217(12) 0.0527(14) -0.0066(11) -0.0128(10) 0.0006(9)
O3 0.0234(12) 0.0212(12) 0.0467(14) -0.0056(10) -0.0099(10) 0.0001(9)
O5 0.0246(12) 0.0208(12) 0.0453(14) -0.0104(10) -0.0137(10) 0.0019(9)
O4A 0.059(6) 0.024(4) 0.049(8) 0.018(4) 0.004(6) 0.004(4)
C24A 0.088(13) 0.138(16) 0.063(11) 0.007(9) -0.038(9) -0.046(11)
C25A 0.149(18) 0.146(16) 0.073(11) 0.004(9) -0.048(11) -0.085(13)
C26A 0.149(19) 0.081(11) 0.057(9) -0.001(7) 0.002(11) -0.015(14)
C27A 0.085(18) 0.049(10) 0.10(2) -0.010(13) -0.051(13) 0.005(11)
O4B 0.039(6) 0.046(5) 0.017(6) 0.003(4) -0.007(5) -0.026(4)
C24B 0.074(10) 0.055(7) 0.061(10) 0.019(6) -0.048(7) -0.036(7)
C25B 0.159(18) 0.143(15) 0.091(10) -0.052(11) -0.009(12) -0.094(14)
C26B 0.066(9) 0.084(9) 0.061(8) -0.036(7) -0.006(7) -0.003(7)
C27B 0.062(10) 0.062(11) 0.034(6) 0.003(5) -0.015(6) -0.022(9)


#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
C1A O5 1.269(4) 2_676 ?
C1A O1 1.279(4) . ?
C1A C2A 1.509(13) . ?
C2A C7A 1.406(13) . ?
C2A C3A 1.409(14) . ?
C3A C4A 1.396(14) . ?
C3A C11A 1.515(15) . ?
C4A C5A 1.398(14) . ?
C4A H4A 0.95 . ?
C5A C6A 1.390(14) . ?
C5A C14A 1.522(12) . ?
C6A C7A 1.422(14) . ?
C6A H6A 0.95 . ?
C7A C8A 1.530(13) . ?
C8A C10A 1.509(14) . ?
C8A C9A 1.537(13) . ?
C8A H8A 1 . ?
C9A H9A1 0.98 . ?
C9A H9A2 0.98 . ?
C9A H9A3 0.98 . ?
C10A H10A 0.98 . ?
C10A H10B 0.98 . ?
C10A H10C 0.98 . ?
C11A C13A 1.513(15) . ?
C11A C12A 1.525(15) . ?
C11A H11A 1 . ?
C12A H12A 0.98 . ?
C12A H12B 0.98 . ?
C12A H12C 0.98 . ?
C13A H13A 0.98 . ?
C13A H13B 0.98 . ?
C13A H13C 0.98 . ?
C14A C15A 1.474(14) . ?
C14A C16A 1.560(14) . ?
C14A H14A 1 . ?
C15A H15A 0.98 . ?
C15A H15B 0.98 . ?
C15A H15C 0.98 . ?
C16A H16A 0.98 . ?
C16A H16B 0.98 . ?
C16A H16C 0.98 . ?
C2B C7B 1.398(9) . ?
C2B C3B 1.406(11) . ?
C3B C4B 1.385(10) . ?
C3B C11B 1.519(11) . ?
C4B C5B 1.397(10) . ?
C4B H4B 0.95 . ?
C5B C6B 1.387(10) . ?
C5B C14B 1.509(9) . ?
C6B C7B 1.414(11) . ?
C6B H6B 0.95 . ?
C7B C8B 1.535(9) . ?
C8B C10B 1.521(10) . ?
C8B C9B 1.543(9) . ?
C8B H8B 1 . ?
C9B H9B1 0.98 . ?
C9B H9B2 0.98 . ?
C9B H9B3 0.98 . ?
C10B H10D 0.98 . ?
C10B H10E 0.98 . ?
C10B H10F 0.98 . ?
C11B C13B 1.512(10) . ?
C11B C12B 1.526(10) . ?
C11B H11B 1 . ?
C12B H12D 0.98 . ?
C12B H12E 0.98 . ?
C12B H12F 0.98 . ?
C13B H13D 0.98 . ?
C13B H13E 0.98 . ?
C13B H13F 0.98 . ?
C14B C15B 1.424(10) . ?
C14B C16B 1.468(11) . ?
C14B H14B 1 . ?
C15B H15D 0.98 . ?
C15B H15E 0.98 . ?
C15B H15F 0.98 . ?
C16B H16D 0.98 . ?
C16B H16E 0.98 . ?
C16B H16F 0.98 . ?
C17 O2 1.274(4) 2_676 ?
C17 O3 1.285(4) . ?
C17 C18 1.471(5) . ?
C18 C19 1.387(5) . ?
C18 C23 1.393(5) . ?
C19 C20 1.376(6) . ?
C19 H19 0.95 . ?
C20 C21 1.379(7) . ?
C20 H20 0.95 . ?
C21 C22 1.387(7) . ?
C21 H21 0.95 . ?
C22 C23 1.370(6) . ?
C22 H22 0.95 . ?
C23 H23 0.95 . ?
Mo1 Mo1 2.1022(6) 2_676 ?
Mo1 O5 2.104(2) . ?
Mo1 O3 2.105(2) . ?
Mo1 O2 2.108(2) . ?
Mo1 O1 2.116(2) . ?
Mo1 O4A 2.486(15) . ?
O2 C17 1.274(4) 2_676 ?
O5 C1B 1.269(4) 2_676 ?
O5 C1A 1.269(4) 2_676 ?
O4A C27A 1.412(13) . ?
O4A C24A 1.474(13) . ?
C24A C25A 1.535(16) . ?
C24A H24A 0.99 . ?
C24A H24B 0.99 . ?
C25A C26A 1.453(16) . ?
C25A H25A 0.99 . ?
C25A H25B 0.99 . ?
C26A C27A 1.499(14) . ?
C26A H26A 0.99 . ?
C26A H26B 0.99 . ?
C27A H27A 0.99 . ?
C27A H27B 0.99 . ?
O4B C27B 1.400(13) . ?
O4B C24B 1.459(10) . ?
C24B C25B 1.526(16) . ?
C24B H24C 0.99 . ?
C24B H24D 0.99 . ?
C25B C26B 1.438(16) . ?
C25B H25C 0.99 . ?
C25B H25D 0.99 . ?
C26B C27B 1.490(13) . ?
C26B H26C 0.99 . ?
C26B H26D 0.99 . ?
C27B H27C 0.99 . ?
C27B H27D 0.99 . ?

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
O5 C1A O1 122.3(3) 2_676 . ?
O5 C1A C2A 125(3) 2_676 . ?
O1 C1A C2A 113(3) . . ?
C7A C2A C3A 121.8(11) . . ?
C7A C2A C1A 117.7(12) . . ?
C3A C2A C1A 120.4(13) . . ?
C4A C3A C2A 117.6(14) . . ?
C4A C3A C11A 120.4(15) . . ?
C2A C3A C11A 122.0(14) . . ?
C3A C4A C5A 122.4(15) . . ?
C3A C4A H4A 118.8 . . ?
C5A C4A H4A 118.8 . . ?
C6A C5A C4A 117.9(12) . . ?
C6A C5A C14A 119.5(12) . . ?
C4A C5A C14A 122.5(13) . . ?
C5A C6A C7A 121.3(13) . . ?
C5A C6A H6A 119.4 . . ?
C7A C6A H6A 119.4 . . ?
C2A C7A C6A 116.2(16) . . ?
C2A C7A C8A 121.4(13) . . ?
C6A C7A C8A 119.1(12) . . ?
C10A C8A C7A 115.4(14) . . ?
C10A C8A C9A 112.5(14) . . ?
C7A C8A C9A 109.4(13) . . ?
C10A C8A H8A 106.3 . . ?
C7A C8A H8A 106.3 . . ?
C9A C8A H8A 106.3 . . ?
C8A C9A H9A1 109.5 . . ?
C8A C9A H9A2 109.5 . . ?
H9A1 C9A H9A2 109.5 . . ?
C8A C9A H9A3 109.5 . . ?
H9A1 C9A H9A3 109.5 . . ?
H9A2 C9A H9A3 109.5 . . ?
C8A C10A H10A 109.5 . . ?
C8A C10A H10B 109.5 . . ?
H10A C10A H10B 109.5 . . ?
C8A C10A H10C 109.5 . . ?
H10A C10A H10C 109.5 . . ?
H10B C10A H10C 109.5 . . ?
C13A C11A C3A 114.5(18) . . ?
C13A C11A C12A 109.1(16) . . ?
C3A C11A C12A 111.4(18) . . ?
C13A C11A H11A 107.2 . . ?
C3A C11A H11A 107.2 . . ?
C12A C11A H11A 107.2 . . ?
C11A C12A H12A 109.5 . . ?
C11A C12A H12B 109.5 . . ?
H12A C12A H12B 109.5 . . ?
C11A C12A H12C 109.5 . . ?
H12A C12A H12C 109.5 . . ?
H12B C12A H12C 109.5 . . ?
C11A C13A H13A 109.5 . . ?
C11A C13A H13B 109.5 . . ?
H13A C13A H13B 109.5 . . ?
C11A C13A H13C 109.5 . . ?
H13A C13A H13C 109.5 . . ?
H13B C13A H13C 109.5 . . ?
C15A C14A C5A 110.9(11) . . ?
C15A C14A C16A 110.3(14) . . ?
C5A C14A C16A 112.1(10) . . ?
C15A C14A H14A 107.8 . . ?
C5A C14A H14A 107.8 . . ?
C16A C14A H14A 107.8 . . ?
C14A C15A H15A 109.5 . . ?
C14A C15A H15B 109.5 . . ?
H15A C15A H15B 109.5 . . ?
C14A C15A H15C 109.5 . . ?
H15A C15A H15C 109.5 . . ?
H15B C15A H15C 109.5 . . ?
C14A C16A H16A 109.5 . . ?
C14A C16A H16B 109.5 . . ?
H16A C16A H16B 109.5 . . ?
C14A C16A H16C 109.5 . . ?
H16A C16A H16C 109.5 . . ?
H16B C16A H16C 109.5 . . ?
C7B C2B C3B 122.1(7) . . ?
C4B C3B C2B 117.7(10) . . ?
C4B C3B C11B 122.6(10) . . ?
C2B C3B C11B 119.6(9) . . ?
C3B C4B C5B 122.4(10) . . ?
C3B C4B H4B 118.8 . . ?
C5B C4B H4B 118.8 . . ?
C6B C5B C4B 118.0(8) . . ?
C6B C5B C14B 120.9(8) . . ?
C4B C5B C14B 121.0(9) . . ?
C5B C6B C7B 121.9(9) . . ?
C5B C6B H6B 119 . . ?
C7B C6B H6B 119 . . ?
C2B C7B C6B 116.7(9) . . ?
C2B C7B C8B 120.9(7) . . ?
C6B C7B C8B 121.0(8) . . ?
C10B C8B C7B 112.0(9) . . ?
C10B C8B C9B 111.9(8) . . ?
C7B C8B C9B 109.6(8) . . ?
C10B C8B H8B 107.7 . . ?
C7B C8B H8B 107.7 . . ?
C9B C8B H8B 107.7 . . ?
C8B C9B H9B1 109.5 . . ?
C8B C9B H9B2 109.5 . . ?
H9B1 C9B H9B2 109.5 . . ?
C8B C9B H9B3 109.5 . . ?
H9B1 C9B H9B3 109.5 . . ?
H9B2 C9B H9B3 109.5 . . ?
C8B C10B H10D 109.5 . . ?
C8B C10B H10E 109.5 . . ?
H10D C10B H10E 109.5 . . ?
C8B C10B H10F 109.5 . . ?
H10D C10B H10F 109.5 . . ?
H10E C10B H10F 109.5 . . ?
C13B C11B C3B 113.0(10) . . ?
C13B C11B C12B 109.8(11) . . ?
C3B C11B C12B 110.7(11) . . ?
C13B C11B H11B 107.7 . . ?
C3B C11B H11B 107.7 . . ?
C12B C11B H11B 107.7 . . ?
C11B C12B H12D 109.5 . . ?
C11B C12B H12E 109.5 . . ?
H12D C12B H12E 109.5 . . ?
C11B C12B H12F 109.5 . . ?
H12D C12B H12F 109.5 . . ?
H12E C12B H12F 109.5 . . ?
C11B C13B H13D 109.5 . . ?
C11B C13B H13E 109.5 . . ?
H13D C13B H13E 109.5 . . ?
C11B C13B H13F 109.5 . . ?
H13D C13B H13F 109.5 . . ?
H13E C13B H13F 109.5 . . ?
C15B C14B C16B 119.9(8) . . ?
C15B C14B C5B 116.5(8) . . ?
C16B C14B C5B 118.4(7) . . ?
C15B C14B H14B 97.6 . . ?
C16B C14B H14B 97.6 . . ?
C5B C14B H14B 97.6 . . ?
C14B C15B H15D 109.5 . . ?
C14B C15B H15E 109.5 . . ?
H15D C15B H15E 109.5 . . ?
C14B C15B H15F 109.5 . . ?
H15D C15B H15F 109.5 . . ?
H15E C15B H15F 109.5 . . ?
C14B C16B H16D 109.5 . . ?
C14B C16B H16E 109.5 . . ?
H16D C16B H16E 109.5 . . ?
C14B C16B H16F 109.5 . . ?
H16D C16B H16F 109.5 . . ?
H16E C16B H16F 109.5 . . ?
O2 C17 O3 121.1(3) 2_676 . ?
O2 C17 C18 119.8(3) 2_676 . ?
O3 C17 C18 119.0(3) . . ?
C19 C18 C23 118.6(4) . . ?
C19 C18 C17 120.6(3) . . ?
C23 C18 C17 120.8(3) . . ?
C20 C19 C18 120.4(4) . . ?
C20 C19 H19 119.8 . . ?
C18 C19 H19 119.8 . . ?
C19 C20 C21 120.8(5) . . ?
C19 C20 H20 119.6 . . ?
C21 C20 H20 119.6 . . ?
C20 C21 C22 119.1(5) . . ?
C20 C21 H21 120.4 . . ?
C22 C21 H21 120.4 . . ?
C23 C22 C21 120.3(4) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C22 C23 C18 120.8(4) . . ?
C22 C23 H23 119.6 . . ?
C18 C23 H23 119.6 . . ?
Mo1 Mo1 O5 92.90(6) 2_676 . ?
Mo1 Mo1 O3 91.83(6) 2_676 . ?
O5 Mo1 O3 89.05(9) . . ?
Mo1 Mo1 O2 91.60(6) 2_676 . ?
O5 Mo1 O2 90.36(9) . . ?
O3 Mo1 O2 176.54(8) . . ?
Mo1 Mo1 O1 90.63(6) 2_676 . ?
O5 Mo1 O1 176.45(8) . . ?
O3 Mo1 O1 91.28(8) . . ?
O2 Mo1 O1 89.09(9) . . ?
Mo1 Mo1 O4A 169.4(3) 2_676 . ?
O5 Mo1 O4A 95.3(4) . . ?
O3 Mo1 O4A 95.0(4) . . ?
O2 Mo1 O4A 81.7(4) . . ?
O1 Mo1 O4A 81.2(4) . . ?
C1A O1 Mo1 117.7(2) . . ?
C17 O2 Mo1 117.8(2) 2_676 . ?
C17 O3 Mo1 117.5(2) . . ?
C1B O5 Mo1 116.4(2) 2_676 . ?
C1A O5 Mo1 116.4(2) 2_676 . ?
C27A O4A C24A 104.8(12) . . ?
C27A O4A Mo1 115.7(14) . . ?
C24A O4A Mo1 124.9(13) . . ?
O4A C24A C25A 107.4(11) . . ?
O4A C24A H24A 110.2 . . ?
C25A C24A H24A 110.2 . . ?
O4A C24A H24B 110.2 . . ?
C25A C24A H24B 110.2 . . ?
H24A C24A H24B 108.5 . . ?
C26A C25A C24A 106.0(11) . . ?
C26A C25A H25A 110.5 . . ?
C24A C25A H25A 110.5 . . ?
C26A C25A H25B 110.5 . . ?
C24A C25A H25B 110.5 . . ?
H25A C25A H25B 108.7 . . ?
C25A C26A C27A 103.1(12) . . ?
C25A C26A H26A 111.2 . . ?
C27A C26A H26A 111.2 . . ?
C25A C26A H26B 111.2 . . ?
C27A C26A H26B 111.2 . . ?
H26A C26A H26B 109.1 . . ?
O4A C27A C26A 109.9(12) . . ?
O4A C27A H27A 109.7 . . ?
C26A C27A H27A 109.7 . . ?
O4A C27A H27B 109.7 . . ?
C26A C27A H27B 109.7 . . ?
H27A C27A H27B 108.2 . . ?
C27B O4B C24B 109.3(10) . . ?
O4B C24B C25B 104.2(10) . . ?
O4B C24B H24C 110.9 . . ?
C25B C24B H24C 110.9 . . ?
O4B C24B H24D 110.9 . . ?
C25B C24B H24D 110.9 . . ?
H24C C24B H24D 108.9 . . ?
C26B C25B C24B 109.5(9) . . ?
C26B C25B H25C 109.8 . . ?
C24B C25B H25C 109.8 . . ?
C26B C25B H25D 109.8 . . ?
C24B C25B H25D 109.8 . . ?
H25C C25B H25D 108.2 . . ?
C25B C26B C27B 105.0(10) . . ?
C25B C26B H26C 110.7 . . ?
C27B C26B H26C 110.7 . . ?
C25B C26B H26D 110.7 . . ?
C27B C26B H26D 110.7 . . ?
H26C C26B H26D 108.8 . . ?
O4B C27B C26B 110.2(12) . . ?
O4B C27B H27C 109.6 . . ?
C26B C27B H27C 109.6 . . ?
O4B C27B H27D 109.6 . . ?
C26B C27B H27D 109.6 . . ?
H27C C27B H27D 108.1 . . ?

# END of CIF
_database_code_depnum_ccdc_archive 'CCDC 943288'