# Electronic Supplementary Material (ESI) for Catalysis Science & Technology.
# 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. 
# 
#######################################################################

data_Compound3
_database_code_depnum_ccdc_archive 'CCDC 1030682'
_audit_update_record             
;
2014-10-23 deposited with the CCDC.
2015-01-16 downloaded from the CCDC.
;

#===============================================================================

# 5. CHEMICAL DATA

_chemical_formula_moiety         'C9 H5 F3 Mo O3'
_chemical_formula_sum            'C9 H5 F3 Mo O3'
_chemical_formula_weight         314.07
_chemical_compound_source        'see text'

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'
F F 0.0171 0.0103 ' 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 0.0060 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#===============================================================================

# 6. CRYSTAL DATA

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

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z

_cell_length_a                   6.4530(2)
_cell_length_b                   6.5440(2)
_cell_length_c                   6.7851(2)
_cell_angle_alpha                107.752(1)
_cell_angle_beta                 97.132(1)
_cell_angle_gamma                107.192(1)
_cell_volume                     253.356(14)
_cell_formula_units_Z            1
_cell_measurement_temperature    123
_cell_measurement_reflns_used    8174
_cell_measurement_theta_min      3.2434
_cell_measurement_theta_max      25.3472

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow

_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.070
_exptl_crystal_density_diffrn    2.059
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_F_000             152
_exptl_absorpt_coefficient_mu    1.326
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS, Bruker, 2012'
_exptl_absorpt_correction_T_min  0.529
_exptl_absorpt_correction_T_max  0.913

#===============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
;
Diffractometer operator             A. Poethig
scanspeed                           20 s per frame
dx                                  35
2853 frames measured in 9 data sets
phi-scan with delta_phi         = 0.5
omega-scans with delta_omega    = 0.5
;
_diffrn_ambient_temperature      123
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine focus sealed tube'
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device       ' κ-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker APEX-II CCD '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 16

# number of measured reflections (redundant set)
_diffrn_reflns_number            910
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0158
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         3.24
_diffrn_reflns_theta_max         25.37
_diffrn_reflns_theta_full        25.37
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measured_fraction_theta_full 0.978
_diffrn_reflns_reduction_process 
;
;

# number of unique reflections
_reflns_number_total             910
# number of observed reflections (> n sig(I))
_reflns_number_gt                905
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'APEX II Control Software (Bruker, 2008a)'
_computing_cell_refinement       'SAINT (Bruker, 2008b)'
_computing_data_reduction        'SAINT (Bruker, 2008b)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  
'SHELXL97 (Sheldrick, 1997), SHELXLE (Huebschle, 2011)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2004)'

#===============================================================================

# 8. REFINEMENT DATA

_refine_special_details          Twin
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0147P)²+0.3456P] where P=(Fo²+2Fc²)/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_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881'


_refine_ls_number_reflns         910
_refine_ls_number_parameters     145
_refine_ls_number_restraints     3
_refine_ls_number_constraints    ?
_refine_ls_R_factor_all          0.0147
_refine_ls_R_factor_gt           0.0147
_refine_ls_wR_factor_ref         0.0381
_refine_ls_wR_factor_gt          0.0381
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_restrained_S_all      1.109
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.069

#===============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_calc_flag
_atom_site_refinement_flags

_atom_site_disorder_assembly
_atom_site_disorder_group

Mo1 Mo Uani 0.17440 0.20990 0.41780 1.000 0.0114(1) d . . .
F1 F Uani -0.1556(5) -0.1268(5) 0.5734(4) 1.000 0.0295(9) d . . .
F2 F Uani -0.3145(4) -0.1048(5) 0.2872(4) 1.000 0.0261(8) d . . .
F3 F Uani -0.0983(5) -0.3014(5) 0.2734(5) 1.000 0.0301(9) d . . .
O1 O Uani -0.1304(6) 0.4224(7) 0.6792(6) 1.000 0.0315(12) d . . .
O2 O Uani 0.5099(6) 0.6142(6) 0.8239(5) 1.000 0.0260(10) d . . .
O3 O Uani 0.3972(6) -0.0428(6) 0.6578(5) 1.000 0.0284(11) d . . .
C1 C Uani 0.2836(9) 0.0576(9) 0.1059(7) 1.000 0.0217(16) d . . .
C2 C Uani 0.4088(8) 0.2940(9) 0.2030(7) 1.000 0.0251(16) d . . .
C3 C Uani 0.2598(9) 0.4152(8) 0.1997(7) 1.000 0.0254(14) d . . .
C4 C Uani 0.0432(9) 0.2533(9) 0.1021(7) 1.000 0.0245(16) d . . .
C5 C Uani 0.0589(8) 0.0330(9) 0.0449(7) 1.000 0.0218(16) d . . .
C6 C Uani -0.1140(8) -0.0959(8) 0.3896(7) 1.000 0.0182(12) d . . .
C7 C Uani -0.0189(8) 0.3435(8) 0.5863(8) 1.000 0.0195(12) d . . .
C8 C Uani 0.3919(8) 0.4693(8) 0.6748(7) 1.000 0.0172(12) d . . .
C9 C Uani 0.3116(8) 0.0493(8) 0.5763(7) 1.000 0.0188(12) d . . .
H1 H Uiso 0.34550 -0.06900 0.07430 1.000 0.0260 c R . .
H2 H Uiso 0.57530 0.36420 0.24820 1.000 0.0300 c R . .
H3 H Uiso 0.30330 0.58530 0.24240 1.000 0.0300 c R . .
H4 H Uiso -0.09440 0.28830 0.06660 1.000 0.0290 c R . .
H5 H Uiso -0.06710 -0.11520 -0.03550 1.000 0.0260 c R . .


#===============================================================================

# 10. MOLECULAR GEOMETRY

_geom_special_details            
;
 Bond distances, angles etc. have been calculated using the
 rounded fractional coordinates. All su's are estimated
 from the variances of the (full) variance-covariance matrix.
 The cell esds are taken into account in the estimation of
 distances, angles and torsion angles
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 C1 2.3383 . . yes
Mo1 C2 2.2933 . . yes
Mo1 C3 2.2969 . . yes
Mo1 C4 2.3342 . . yes
Mo1 C5 2.3522 . . yes
Mo1 C6 2.2319 . . yes
Mo1 C7 2.0042 . . yes
Mo1 C8 2.0177 . . yes
Mo1 C9 2.0119 . . yes
F1 C6 1.369(5) . . yes
F2 C6 1.367(6) . . yes
F3 C6 1.376(6) . . yes
O1 C7 1.147(7) . . yes
O2 C8 1.140(6) . . yes
O3 C9 1.140(6) . . yes
C1 C2 1.410(8) . . no
C1 C5 1.404(8) . . no
C2 C3 1.418(8) . . no
C3 C4 1.408(8) . . no
C4 C5 1.412(8) . . no
C1 H1 1.0000 . . no
C2 H2 1.0000 . . no
C3 H3 1.0000 . . no
C4 H4 1.0000 . . no
C5 H5 1.0000 . . no

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Mo1 C2 35.42 . . . yes
C1 Mo1 C3 59.14 . . . yes
C1 Mo1 C4 58.62 . . . yes
C1 Mo1 C5 34.84 . . . yes
C1 Mo1 C6 99.54 . . . yes
C1 Mo1 C7 154.66 . . . yes
C1 Mo1 C8 121.88 . . . yes
C1 Mo1 C9 94.12 . . . yes
C2 Mo1 C3 35.98 . . . yes
C2 Mo1 C4 59.17 . . . yes
C2 Mo1 C5 58.58 . . . yes
C2 Mo1 C6 134.66 . . . yes
C2 Mo1 C7 139.67 . . . yes
C2 Mo1 C8 91.03 . . . yes
C2 Mo1 C9 104.69 . . . yes
C3 Mo1 C4 35.38 . . . yes
C3 Mo1 C5 58.62 . . . yes
C3 Mo1 C6 133.36 . . . yes
C3 Mo1 C7 105.54 . . . yes
C3 Mo1 C8 92.10 . . . yes
C3 Mo1 C9 139.65 . . . yes
C4 Mo1 C5 35.07 . . . yes
C4 Mo1 C6 98.09 . . . yes
C4 Mo1 C7 96.88 . . . yes
C4 Mo1 C8 123.80 . . . yes
C4 Mo1 C9 151.32 . . . yes
C5 Mo1 C6 80.17 . . . yes
C5 Mo1 C7 120.85 . . . yes
C5 Mo1 C8 148.39 . . . yes
C5 Mo1 C9 116.97 . . . yes
C6 Mo1 C7 76.04 . . . yes
C6 Mo1 C8 131.43 . . . yes
C6 Mo1 C9 76.35 . . . yes
C7 Mo1 C8 75.62 . . . yes
C7 Mo1 C9 108.65 . . . yes
C8 Mo1 C9 76.48 . . . yes
Mo1 C1 C2 70.55 . . . yes
Mo1 C1 C5 73.12 . . . yes
C2 C1 C5 107.8(5) . . . no
Mo1 C2 C1 74.03 . . . yes
Mo1 C2 C3 72.15 . . . yes
C1 C2 C3 108.0(5) . . . no
Mo1 C3 C2 71.87 . . . yes
Mo1 C3 C4 73.76 . . . yes
C2 C3 C4 108.0(5) . . . no
Mo1 C4 C3 70.86 . . . yes
Mo1 C4 C5 73.16 . . . yes
C3 C4 C5 107.7(5) . . . no
Mo1 C5 C1 72.04 . . . yes
Mo1 C5 C4 71.77 . . . yes
C1 C5 C4 108.6(5) . . . no
Mo1 C6 F1 117.84 . . . yes
Mo1 C6 F2 114.02 . . . yes
Mo1 C6 F3 113.69 . . . yes
F1 C6 F2 103.4(4) . . . yes
F1 C6 F3 102.8(4) . . . yes
F2 C6 F3 103.4(4) . . . yes
Mo1 C7 O1 178.33 . . . yes
Mo1 C8 O2 177.76 . . . yes
Mo1 C9 O3 175.95 . . . yes
Mo1 C1 H1 126.00 . . . no
C2 C1 H1 126.00 . . . no
C5 C1 H1 126.00 . . . no
Mo1 C2 H2 126.00 . . . no
C1 C2 H2 126.00 . . . no
C3 C2 H2 126.00 . . . no
Mo1 C3 H3 126.00 . . . no
C2 C3 H3 126.00 . . . no
C4 C3 H3 126.00 . . . no
Mo1 C4 H4 126.00 . . . no
C3 C4 H4 126.00 . . . no
C5 C4 H4 126.00 . . . no
Mo1 C5 H5 126.00 . . . no
C1 C5 H5 126.00 . . . no
C4 C5 H5 126.00 . . . no

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
C2 Mo1 C1 C5 -116.45 . . . . no
C3 Mo1 C1 C2 38.17 . . . . no
C3 Mo1 C1 C5 -78.28 . . . . no
C4 Mo1 C1 C2 79.75 . . . . no
C4 Mo1 C1 C5 -36.70 . . . . no
C5 Mo1 C1 C2 116.45 . . . . no
C6 Mo1 C1 C2 173.45 . . . . no
C6 Mo1 C1 C5 57.00 . . . . no
C7 Mo1 C1 C2 95.97 . . . . no
C7 Mo1 C1 C5 -20.48 . . . . no
C8 Mo1 C1 C2 -33.09 . . . . no
C8 Mo1 C1 C5 -149.53 . . . . no
C9 Mo1 C1 C2 -109.72 . . . . no
C9 Mo1 C1 C5 133.83 . . . . no
C1 Mo1 C2 C3 115.46 . . . . no
C3 Mo1 C2 C1 -115.46 . . . . no
C4 Mo1 C2 C1 -78.04 . . . . no
C4 Mo1 C2 C3 37.43 . . . . no
C5 Mo1 C2 C1 -36.83 . . . . no
C5 Mo1 C2 C3 78.64 . . . . no
C6 Mo1 C2 C1 -9.10 . . . . no
C6 Mo1 C2 C3 106.36 . . . . no
C7 Mo1 C2 C1 -138.89 . . . . no
C7 Mo1 C2 C3 -23.42 . . . . no
C8 Mo1 C2 C1 152.38 . . . . no
C8 Mo1 C2 C3 -92.16 . . . . no
C9 Mo1 C2 C1 76.08 . . . . no
C9 Mo1 C2 C3 -168.45 . . . . no
C1 Mo1 C3 C2 -37.56 . . . . no
C1 Mo1 C3 C4 78.10 . . . . no
C2 Mo1 C3 C4 115.66 . . . . no
C4 Mo1 C3 C2 -115.66 . . . . no
C5 Mo1 C3 C2 -78.50 . . . . no
C5 Mo1 C3 C4 37.17 . . . . no
C6 Mo1 C3 C2 -110.19 . . . . no
C6 Mo1 C3 C4 5.47 . . . . no
C7 Mo1 C3 C2 164.51 . . . . no
C7 Mo1 C3 C4 -79.83 . . . . no
C8 Mo1 C3 C2 88.86 . . . . no
C8 Mo1 C3 C4 -155.48 . . . . no
C9 Mo1 C3 C2 17.40 . . . . no
C9 Mo1 C3 C4 133.06 . . . . no
C1 Mo1 C4 C3 -79.70 . . . . no
C1 Mo1 C4 C5 36.45 . . . . no
C2 Mo1 C4 C3 -38.08 . . . . no
C2 Mo1 C4 C5 78.08 . . . . no
C3 Mo1 C4 C5 116.15 . . . . no
C5 Mo1 C4 C3 -116.15 . . . . no
C6 Mo1 C4 C3 -175.98 . . . . no
C6 Mo1 C4 C5 -59.83 . . . . no
C7 Mo1 C4 C3 107.22 . . . . no
C7 Mo1 C4 C5 -136.63 . . . . no
C8 Mo1 C4 C3 29.94 . . . . no
C8 Mo1 C4 C5 146.09 . . . . no
C9 Mo1 C4 C3 -99.69 . . . . no
C9 Mo1 C4 C5 16.47 . . . . no
C1 Mo1 C5 C4 -117.39 . . . . no
C2 Mo1 C5 C1 37.46 . . . . no
C2 Mo1 C5 C4 -79.93 . . . . no
C3 Mo1 C5 C1 79.89 . . . . no
C3 Mo1 C5 C4 -37.50 . . . . no
C4 Mo1 C5 C1 117.39 . . . . no
C6 Mo1 C5 C1 -122.92 . . . . no
C6 Mo1 C5 C4 119.69 . . . . no
C7 Mo1 C5 C1 169.96 . . . . no
C7 Mo1 C5 C4 52.57 . . . . no
C8 Mo1 C5 C1 55.22 . . . . no
C8 Mo1 C5 C4 -62.16 . . . . no
C9 Mo1 C5 C1 -53.83 . . . . no
C9 Mo1 C5 C4 -171.22 . . . . no
C1 Mo1 C6 F1 147.26 . . . . no
C1 Mo1 C6 F2 -91.29 . . . . no
C1 Mo1 C6 F3 26.85 . . . . no
C2 Mo1 C6 F1 152.59 . . . . no
C2 Mo1 C6 F2 -85.95 . . . . no
C2 Mo1 C6 F3 32.19 . . . . no
C3 Mo1 C6 F1 -156.57 . . . . no
C3 Mo1 C6 F2 -35.11 . . . . no
C3 Mo1 C6 F3 83.03 . . . . no
C4 Mo1 C6 F1 -153.37 . . . . no
C4 Mo1 C6 F2 -31.91 . . . . no
C4 Mo1 C6 F3 86.22 . . . . no
C5 Mo1 C6 F1 176.35 . . . . no
C5 Mo1 C6 F2 -62.19 . . . . no
C5 Mo1 C6 F3 55.95 . . . . no
C7 Mo1 C6 F1 -58.24 . . . . no
C7 Mo1 C6 F2 63.22 . . . . no
C7 Mo1 C6 F3 -178.65 . . . . no
C8 Mo1 C6 F1 -2.35 . . . . no
C8 Mo1 C6 F2 119.11 . . . . no
C8 Mo1 C6 F3 -122.75 . . . . no
C9 Mo1 C6 F1 55.30 . . . . no
C9 Mo1 C6 F2 176.76 . . . . no
C9 Mo1 C6 F3 -65.10 . . . . no
Mo1 C1 C2 C3 -64.64 . . . . no
C5 C1 C2 Mo1 64.12 . . . . no
C5 C1 C2 C3 -0.5(5) . . . . no
Mo1 C1 C5 C4 62.86 . . . . no
C2 C1 C5 Mo1 -62.44 . . . . no
C2 C1 C5 C4 0.4(5) . . . . no
Mo1 C2 C3 C4 -65.46 . . . . no
C1 C2 C3 Mo1 65.88 . . . . no
C1 C2 C3 C4 0.4(5) . . . . no
Mo1 C3 C4 C5 -64.38 . . . . no
C2 C3 C4 Mo1 64.21 . . . . no
C2 C3 C4 C5 -0.2(5) . . . . no
Mo1 C4 C5 C1 -63.03 . . . . no
C3 C4 C5 Mo1 62.87 . . . . no
C3 C4 C5 C1 -0.2(5) . . . . no

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
#
#D   H   A   D - H  H...A   D...A    D - H...A  symm(A)
#
C2 H2 F3 1.0000 2.4900 3.351(7) 144.00 1_665 yes


#===END
####################################################################### 
# 
# 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_Compound6
_database_code_depnum_ccdc_archive 'CCDC 1030683'
_audit_update_record             
;
2014-10-23 deposited with the CCDC.
2015-01-16 downloaded from the CCDC.
;

#===============================================================================

# 5. CHEMICAL DATA

_chemical_formula_moiety         'C6 H5 F3 Mo O3'
_chemical_formula_sum            'C6 H5 F3 Mo O3'
_chemical_formula_weight         278.04

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'
F F 0.0171 0.0103 ' 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 0.0060 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#===============================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_Int_Tables_number      15

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,y,1/2-z
3 -x,-y,-z
4 x,-y,1/2+z
5 1/2+x,1/2+y,z
6 1/2-x,1/2+y,1/2-z
7 1/2-x,1/2-y,-z
8 1/2+x,1/2-y,1/2+z

_cell_length_a                   20.5911(3)
_cell_length_b                   6.9325(1)
_cell_length_c                   12.3919(2)
_cell_angle_alpha                90
_cell_angle_beta                 117.372(1)
_cell_angle_gamma                90
_cell_volume                     1570.87(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    123
_cell_measurement_reflns_used    3206
_cell_measurement_theta_min      3.1426
_cell_measurement_theta_max      25.3817

_exptl_crystal_description       fragment
_exptl_crystal_colour            'clear intense yellow'

_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.080
_exptl_crystal_density_diffrn    2.351
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_F_000             1072
_exptl_absorpt_coefficient_mu    1.693
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2008b'
_exptl_absorpt_correction_T_min  0.594
_exptl_absorpt_correction_T_max  0.881

#===============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
;
Diffractometer operator             A. Poethig
scanspeed                           5 s per frame
dx                                  50
2194 frames measured in 3 data sets
phi-scan with delta_phi         = 0.5
omega-scans with delta_omega    = 0.5
;
_diffrn_ambient_temperature      123
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed-tube'
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device       ' κ-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker APEX-II CCD '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 16

# number of measured reflections (redundant set)
_diffrn_reflns_number            8754
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0238
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.23
_diffrn_reflns_theta_max         25.40
_diffrn_reflns_theta_full        25.40
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_reduction_process 
;
;

# number of unique reflections
_reflns_number_total             1447
# number of observed reflections (> n sig(I))
_reflns_number_gt                1266
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'APEX II Control Software (Bruker, 2008a)'
_computing_cell_refinement       'SAINT (Bruker, 2008b)'
_computing_data_reduction        'SAINT (Bruker, 2008b)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXLE (Huebschle, 2011)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2004)'

#===============================================================================

# 8. REFINEMENT DATA

_refine_special_details          
;
 Refinement on F² for ALL reflections except those
 flagged by the user for potential systematic errors.
 Weighted R-factors wR and all goodnesses of fit S
 are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The
 observed criterion of F² > 2sigma(F²) is used only
 for calculating -R-factor-obs etc. and is not
 relevant to the choice of reflections for refinement.
 R-factors based on F² 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/[σ²(Fo²)+(0.0193P)²+2.5435P] where P=(Fo²+2Fc²)/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_abs_structure_details ?
_refine_ls_abs_structure_Flack   .
_refine_ls_number_reflns         1447
_refine_ls_number_parameters     118
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0194
_refine_ls_wR_factor_ref         0.0448
_refine_ls_wR_factor_gt          0.0431
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.077

#===============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_calc_flag
_atom_site_refinement_flags

_atom_site_disorder_assembly
_atom_site_disorder_group

Mo1 Mo Uani 0.59771(1) 0.83059(3) 0.62032(2) 1.000 0.0141(1) d . . .
F1 F Uani 0.74344(9) 0.7402(3) 0.83610(15) 1.000 0.0316(6) d . . .
F2 F Uani 0.67206(10) 0.4929(2) 0.78816(15) 1.000 0.0316(6) d . . .
F3 F Uani 0.65333(10) 0.7343(3) 0.87876(15) 1.000 0.0308(6) d . . .
O1 O Uani 0.63889(11) 1.0427(3) 0.73106(18) 1.000 0.0248(7) d . . .
O2 O Uani 0.59205(11) 1.1087(3) 0.60946(18) 1.000 0.0286(7) d . . .
O3 O Uani 0.52179(11) 0.7485(3) 0.62483(19) 1.000 0.0285(7) d . . .
C1 C Uani 0.55951(16) 0.6614(4) 0.4318(2) 1.000 0.0222(9) d . . .
C2 C Uani 0.61659(16) 0.5579(4) 0.5217(3) 1.000 0.0225(10) d . . .
C3 C Uani 0.68184(15) 0.6739(4) 0.5652(2) 1.000 0.0207(9) d . . .
C4 C Uani 0.66337(15) 0.8471(4) 0.5016(2) 1.000 0.0185(9) d . . .
C5 C Uani 0.58701(15) 0.8440(4) 0.4226(2) 1.000 0.0199(9) d . . .
C6 C Uani 0.67258(17) 0.6881(4) 0.7910(3) 1.000 0.0231(9) d . . .
H1 H Uiso 0.51080 0.61720 0.38490 1.000 0.0270 c R . .
H2 H Uiso 0.61320 0.43250 0.54960 1.000 0.0270 c R . .
H3 H Uiso 0.72900 0.63830 0.62640 1.000 0.0250 c R . .
H4 H Uiso 0.69600 0.94940 0.50970 1.000 0.0220 c R . .
H5 H Uiso 0.55910 0.94720 0.37210 1.000 0.0240 c R . .


#===============================================================================

# 10. MOLECULAR GEOMETRY

_geom_special_details            
;
 Bond distances, angles etc. have been calculated using the
 rounded fractional coordinates. All su's are estimated
 from the variances of the (full) variance-covariance matrix.
 The cell esds are taken into account in the estimation of
 distances, angles and torsion angles
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 O1 1.922(2) . . yes
Mo1 O2 1.933(2) . . yes
Mo1 O3 1.689(2) . . yes
Mo1 C1 2.401(2) . . yes
Mo1 C2 2.378(3) . . yes
Mo1 C3 2.395(3) . . yes
Mo1 C4 2.415(3) . . yes
Mo1 C5 2.359(2) . . yes
Mo1 C6 2.197(3) . . yes
F1 C6 1.350(4) . . yes
F2 C6 1.354(3) . . yes
F3 C6 1.356(4) . . yes
O1 O2 1.440(3) . . yes
C1 C2 1.390(4) . . no
C1 C5 1.413(4) . . no
C2 C3 1.441(5) . . no
C3 C4 1.390(4) . . no
C4 C5 1.420(4) . . no
C1 H1 0.9500 . . no
C2 H2 0.9500 . . no
C3 H3 0.9500 . . no
C4 H4 0.9500 . . no
C5 H5 0.9500 . . no

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mo1 O2 43.88(9) . . . yes
O1 Mo1 O3 110.21(10) . . . yes
O1 Mo1 C1 155.26(10) . . . yes
O1 Mo1 C2 148.47(11) . . . yes
O1 Mo1 C3 114.28(10) . . . yes
O1 Mo1 C4 102.23(10) . . . yes
O1 Mo1 C5 120.75(9) . . . yes
O1 Mo1 C6 76.86(10) . . . yes
O2 Mo1 O3 108.15(10) . . . yes
O2 Mo1 C1 115.94(9) . . . yes
O2 Mo1 C2 140.91(10) . . . yes
O2 Mo1 C3 117.46(10) . . . yes
O2 Mo1 C4 86.74(10) . . . yes
O2 Mo1 C5 85.10(9) . . . yes
O2 Mo1 C6 120.58(10) . . . yes
O3 Mo1 C1 88.48(11) . . . yes
O3 Mo1 C2 96.99(11) . . . yes
O3 Mo1 C3 131.20(10) . . . yes
O3 Mo1 C4 145.30(9) . . . yes
O3 Mo1 C5 113.70(10) . . . yes
O3 Mo1 C6 93.85(12) . . . yes
C1 Mo1 C2 33.83(11) . . . yes
C1 Mo1 C3 57.12(10) . . . yes
C1 Mo1 C4 56.99(10) . . . yes
C1 Mo1 C5 34.52(10) . . . yes
C1 Mo1 C6 119.22(10) . . . yes
C2 Mo1 C3 35.14(11) . . . yes
C2 Mo1 C4 56.99(10) . . . yes
C2 Mo1 C5 57.10(10) . . . yes
C2 Mo1 C6 85.94(11) . . . yes
C3 Mo1 C4 33.59(9) . . . yes
C3 Mo1 C5 57.04(9) . . . yes
C3 Mo1 C6 77.95(11) . . . yes
C4 Mo1 C5 34.58(10) . . . yes
C4 Mo1 C6 105.43(12) . . . yes
C5 Mo1 C6 134.97(12) . . . yes
Mo1 O1 O2 68.45(12) . . . yes
Mo1 O2 O1 67.68(12) . . . yes
Mo1 C1 C2 72.20(16) . . . yes
Mo1 C1 C5 71.13(14) . . . yes
C2 C1 C5 107.7(3) . . . no
Mo1 C2 C1 73.97(17) . . . yes
Mo1 C2 C3 73.07(17) . . . yes
C1 C2 C3 108.1(3) . . . no
Mo1 C3 C2 71.79(18) . . . yes
Mo1 C3 C4 74.02(18) . . . yes
C2 C3 C4 107.8(3) . . . no
Mo1 C4 C3 72.40(17) . . . yes
Mo1 C4 C5 70.53(17) . . . yes
C3 C4 C5 107.8(3) . . . no
Mo1 C5 C1 74.36(14) . . . yes
Mo1 C5 C4 74.90(14) . . . yes
C1 C5 C4 108.4(2) . . . no
Mo1 C6 F1 115.1(2) . . . yes
Mo1 C6 F2 115.5(2) . . . yes
Mo1 C6 F3 109.4(2) . . . yes
F1 C6 F2 105.8(3) . . . yes
F1 C6 F3 105.3(2) . . . yes
F2 C6 F3 104.8(3) . . . yes
Mo1 C1 H1 122.00 . . . no
C2 C1 H1 126.00 . . . no
C5 C1 H1 126.00 . . . no
Mo1 C2 H2 119.00 . . . no
C1 C2 H2 126.00 . . . no
C3 C2 H2 126.00 . . . no
Mo1 C3 H3 120.00 . . . no
C2 C3 H3 126.00 . . . no
C4 C3 H3 126.00 . . . no
Mo1 C4 H4 123.00 . . . no
C3 C4 H4 126.00 . . . no
C5 C4 H4 126.00 . . . no
Mo1 C5 H5 117.00 . . . no
C1 C5 H5 126.00 . . . no
C4 C5 H5 126.00 . . . no

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 O1 O2 -95.51(15) . . . . no
C1 Mo1 O1 O2 41.5(3) . . . . no
C2 Mo1 O1 O2 116.5(2) . . . . no
C3 Mo1 O1 O2 105.11(14) . . . . no
C4 Mo1 O1 O2 71.97(15) . . . . no
C5 Mo1 O1 O2 40.33(18) . . . . no
C6 Mo1 O1 O2 175.21(18) . . . . no
O3 Mo1 O2 O1 100.58(15) . . . . no
C1 Mo1 O2 O1 -162.05(15) . . . . no
C2 Mo1 O2 O1 -132.08(18) . . . . no
C3 Mo1 O2 O1 -97.36(14) . . . . no
C4 Mo1 O2 O1 -111.44(15) . . . . no
C5 Mo1 O2 O1 -146.07(15) . . . . no
C6 Mo1 O2 O1 -5.4(2) . . . . no
O1 Mo1 C1 C2 114.9(3) . . . . no
O1 Mo1 C1 C5 -1.8(4) . . . . no
O2 Mo1 C1 C2 145.55(19) . . . . no
O2 Mo1 C1 C5 29.0(2) . . . . no
O3 Mo1 C1 C2 -105.0(2) . . . . no
O3 Mo1 C1 C5 138.43(19) . . . . no
C2 Mo1 C1 C5 -116.6(3) . . . . no
C3 Mo1 C1 C2 38.33(19) . . . . no
C3 Mo1 C1 C5 -78.3(2) . . . . no
C4 Mo1 C1 C2 78.6(2) . . . . no
C4 Mo1 C1 C5 -38.00(18) . . . . no
C5 Mo1 C1 C2 116.6(3) . . . . no
C6 Mo1 C1 C2 -11.4(2) . . . . no
C6 Mo1 C1 C5 -128.01(19) . . . . no
O1 Mo1 C2 C1 -133.4(2) . . . . no
O1 Mo1 C2 C3 -18.2(3) . . . . no
O2 Mo1 C2 C1 -53.8(3) . . . . no
O2 Mo1 C2 C3 61.4(2) . . . . no
O3 Mo1 C2 C1 76.6(2) . . . . no
O3 Mo1 C2 C3 -168.16(16) . . . . no
C1 Mo1 C2 C3 115.2(3) . . . . no
C3 Mo1 C2 C1 -115.2(3) . . . . no
C4 Mo1 C2 C1 -78.6(2) . . . . no
C4 Mo1 C2 C3 36.60(14) . . . . no
C5 Mo1 C2 C1 -37.12(19) . . . . no
C5 Mo1 C2 C3 78.08(17) . . . . no
C6 Mo1 C2 C1 170.0(2) . . . . no
C6 Mo1 C2 C3 -74.77(17) . . . . no
O1 Mo1 C3 C2 169.66(16) . . . . no
O1 Mo1 C3 C4 -74.99(16) . . . . no
O2 Mo1 C3 C2 -141.40(16) . . . . no
O2 Mo1 C3 C4 -26.05(18) . . . . no
O3 Mo1 C3 C2 15.7(2) . . . . no
O3 Mo1 C3 C4 131.06(17) . . . . no
C1 Mo1 C3 C2 -36.86(16) . . . . no
C1 Mo1 C3 C4 78.50(16) . . . . no
C2 Mo1 C3 C4 115.4(2) . . . . no
C4 Mo1 C3 C2 -115.4(2) . . . . no
C5 Mo1 C3 C2 -78.25(18) . . . . no
C5 Mo1 C3 C4 37.10(15) . . . . no
C6 Mo1 C3 C2 100.22(18) . . . . no
C6 Mo1 C3 C4 -144.43(18) . . . . no
O1 Mo1 C4 C3 115.72(16) . . . . no
O1 Mo1 C4 C5 -127.40(16) . . . . no
O2 Mo1 C4 C3 157.03(16) . . . . no
O2 Mo1 C4 C5 -86.09(17) . . . . no
O3 Mo1 C4 C3 -85.2(2) . . . . no
O3 Mo1 C4 C5 31.7(3) . . . . no
C1 Mo1 C4 C3 -78.95(17) . . . . no
C1 Mo1 C4 C5 37.93(16) . . . . no
C2 Mo1 C4 C3 -38.34(16) . . . . no
C2 Mo1 C4 C5 78.54(18) . . . . no
C3 Mo1 C4 C5 116.9(2) . . . . no
C5 Mo1 C4 C3 -116.9(2) . . . . no
C6 Mo1 C4 C3 36.17(17) . . . . no
C6 Mo1 C4 C5 153.05(16) . . . . no
O1 Mo1 C5 C1 179.15(17) . . . . no
O1 Mo1 C5 C4 64.61(19) . . . . no
O2 Mo1 C5 C1 -154.10(19) . . . . no
O2 Mo1 C5 C4 91.36(17) . . . . no
O3 Mo1 C5 C1 -46.4(2) . . . . no
O3 Mo1 C5 C4 -160.96(16) . . . . no
C1 Mo1 C5 C4 -114.5(2) . . . . no
C2 Mo1 C5 C1 36.36(19) . . . . no
C2 Mo1 C5 C4 -78.18(19) . . . . no
C3 Mo1 C5 C1 78.52(19) . . . . no
C3 Mo1 C5 C4 -36.02(16) . . . . no
C4 Mo1 C5 C1 114.5(2) . . . . no
C6 Mo1 C5 C1 76.4(2) . . . . no
C6 Mo1 C5 C4 -38.1(2) . . . . no
O1 Mo1 C6 F1 -59.9(2) . . . . no
O1 Mo1 C6 F2 176.2(3) . . . . no
O1 Mo1 C6 F3 58.3(2) . . . . no
O2 Mo1 C6 F1 -56.1(3) . . . . no
O2 Mo1 C6 F2 -179.9(2) . . . . no
O2 Mo1 C6 F3 62.2(2) . . . . no
O3 Mo1 C6 F1 -169.8(2) . . . . no
O3 Mo1 C6 F2 66.3(3) . . . . no
O3 Mo1 C6 F3 -51.5(2) . . . . no
C1 Mo1 C6 F1 99.8(2) . . . . no
C1 Mo1 C6 F2 -24.1(3) . . . . no
C1 Mo1 C6 F3 -141.94(19) . . . . no
C2 Mo1 C6 F1 93.5(2) . . . . no
C2 Mo1 C6 F2 -30.4(3) . . . . no
C2 Mo1 C6 F3 -148.3(2) . . . . no
C3 Mo1 C6 F1 58.9(2) . . . . no
C3 Mo1 C6 F2 -65.0(3) . . . . no
C3 Mo1 C6 F3 177.1(2) . . . . no
C4 Mo1 C6 F1 39.4(2) . . . . no
C4 Mo1 C6 F2 -84.5(3) . . . . no
C4 Mo1 C6 F3 157.62(19) . . . . no
C5 Mo1 C6 F1 60.7(3) . . . . no
C5 Mo1 C6 F2 -63.2(3) . . . . no
C5 Mo1 C6 F3 178.94(16) . . . . no
Mo1 C1 C2 C3 -65.6(2) . . . . no
C5 C1 C2 Mo1 62.7(2) . . . . no
C5 C1 C2 C3 -3.0(3) . . . . no
Mo1 C1 C5 C4 67.76(18) . . . . no
C2 C1 C5 Mo1 -63.4(2) . . . . no
C2 C1 C5 C4 4.4(3) . . . . no
Mo1 C2 C3 C4 -65.8(2) . . . . no
C1 C2 C3 Mo1 66.2(2) . . . . no
C1 C2 C3 C4 0.4(3) . . . . no
Mo1 C3 C4 C5 -62.03(19) . . . . no
C2 C3 C4 Mo1 64.3(2) . . . . no
C2 C3 C4 C5 2.3(3) . . . . no
Mo1 C4 C5 C1 -67.40(19) . . . . no
C3 C4 C5 Mo1 63.24(19) . . . . no
C3 C4 C5 C1 -4.2(3) . . . . no

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
#
#D   H   A   D - H  H...A   D...A    D - H...A  symm(A)
#
C2 H2 O2 0.9500 2.4600 3.412(4) 175.00 1_545 yes
C3 H3 O1 0.9500 2.5600 3.501(4) 172.00 6_646 yes

#===END
