# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2a
_database_code_depnum_ccdc_archive 'CCDC 1042920'
_audit_update_record             
;
2015-01-12 deposited with the CCDC.
2015-06-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H20 Cl3.08 Mo O2.92'
_chemical_formula_weight         392.03

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'
Cl Cl 0.1484 0.1585 '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           orthorhombic
_symmetry_space_group_name_H-M   Fdd2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   34.442(5)
_cell_length_b                   7.3616(10)
_cell_length_c                   12.1624(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3083.7(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8278
_cell_measurement_theta_min      2.3655
_cell_measurement_theta_max      28.629

_exptl_crystal_description       prism
_exptl_crystal_colour            bright-green
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1581
_exptl_absorpt_coefficient_mu    1.377
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7334
_exptl_absorpt_correction_T_max  0.8097
_exptl_absorpt_process_details   
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1304 (selected reflections only, before parameter refinement)
 R(int) =  0.0492 (selected reflections only, after parameter refinement)
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8046
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.29
_diffrn_reflns_theta_max         27.00
_reflns_number_total             1681
_reflns_number_gt                1681
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1996)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) 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)+(0.0098P)²+6.2803P] 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_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.92(4)
_refine_ls_number_reflns         1681
_refine_ls_number_parameters     89
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0168
_refine_ls_R_factor_gt           0.0168
_refine_ls_wR_factor_ref         0.0425
_refine_ls_wR_factor_gt          0.0425
_refine_ls_goodness_of_fit_ref   1.209
_refine_ls_restrained_S_all      1.209
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.0000 1.0000 1.011999(9) 0.02504(8) Uani 1 2 d S . .
Cl1 Cl 0.045376(15) 1.23691(6) 0.99067(4) 0.02246(12) Uani 1 1 d . A .
Cl2 Cl 0.03814(8) 0.8593(3) 1.12969(19) 0.0256(5) Uani 0.539(7) 1 d P A 1
O2 O 0.0281(2) 0.8671(10) 1.1002(8) 0.0299(15) Uani 0.461(7) 1 d P A 2
O1 O 0.03050(4) 0.87201(19) 0.87164(13) 0.0207(3) Uani 1 1 d . A .
C3 C 0.10324(6) 0.7537(3) 0.7777(3) 0.0294(6) Uani 1 1 d . . .
H3A H 0.0963 0.6895 0.7089 0.035 Uiso 1 1 calc R . .
H3B H 0.1318 0.7501 0.7857 0.035 Uiso 1 1 calc R . .
C2 C 0.08439(6) 0.6580(3) 0.8753(2) 0.0273(5) Uani 1 1 d . A .
H2A H 0.0912 0.5274 0.8738 0.033 Uiso 1 1 calc R . .
H2B H 0.0945 0.7103 0.9446 0.033 Uiso 1 1 calc R . .
C1 C 0.04068(6) 0.6788(3) 0.8719(2) 0.0253(4) Uani 1 1 d . . .
H1A H 0.0303 0.6197 0.8050 0.030 Uiso 1 1 calc R A .
H1B H 0.0290 0.6188 0.9369 0.030 Uiso 1 1 calc R . .
C4 C 0.08970(6) 0.9507(3) 0.7710(2) 0.0261(4) Uani 1 1 d . A .
H4A H 0.1006 1.0200 0.8336 0.031 Uiso 1 1 calc R . .
H4B H 0.0994 1.0061 0.7022 0.031 Uiso 1 1 calc R . .
C5 C 0.04580(6) 0.9624(3) 0.77368(18) 0.0230(4) Uani 1 1 d . . .
H5A H 0.0377 1.0915 0.7738 0.028 Uiso 1 1 calc R A .
H5B H 0.0350 0.9042 0.7070 0.028 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 0.02451(12) 0.03786(15) 0.01276(11) 0.000 0.000 -0.01290(12)
Cl1 0.0248(3) 0.0178(2) 0.0248(3) -0.00033(19) -0.00425(19) -0.00158(17)
Cl2 0.0318(11) 0.0223(6) 0.0226(9) 0.0043(6) -0.0022(6) 0.0004(6)
O2 0.030(3) 0.023(2) 0.037(4) 0.004(3) -0.006(2) 0.004(2)
O1 0.0205(7) 0.0215(7) 0.0202(7) -0.0026(6) 0.0047(6) 0.0002(5)
C3 0.0184(9) 0.0348(11) 0.0349(18) -0.0068(10) 0.0049(10) -0.0007(9)
C2 0.0217(10) 0.0209(10) 0.0395(12) -0.0040(9) 0.0022(10) 0.0018(8)
C1 0.0220(10) 0.0197(10) 0.0343(12) -0.0075(9) 0.0056(9) -0.0017(8)
C4 0.0225(10) 0.0310(10) 0.0249(11) -0.0017(9) 0.0048(10) -0.0038(8)
C5 0.0230(10) 0.0303(10) 0.0157(10) 0.0005(8) 0.0028(9) -0.0014(8)

_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 O2 1.744(9) 2_575 ?
Mo1 O2 1.744(9) . ?
Mo1 Cl2 2.201(3) . ?
Mo1 Cl2 2.201(3) 2_575 ?
Mo1 O1 2.2148(15) . ?
Mo1 O1 2.2148(15) 2_575 ?
Mo1 Cl1 2.3562(5) . ?
Mo1 Cl1 2.3562(5) 2_575 ?
O1 C5 1.463(3) . ?
O1 C1 1.465(2) . ?
C3 C2 1.525(4) . ?
C3 C4 1.526(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C2 C1 1.514(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C4 C5 1.515(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?

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
O2 Mo1 O2 104.1(6) 2_575 . ?
O2 Mo1 Cl2 101.2(2) 2_575 . ?
O2 Mo1 Cl2 6.1(3) . . ?
O2 Mo1 Cl2 6.1(3) 2_575 2_575 ?
O2 Mo1 Cl2 101.2(3) . 2_575 ?
Cl2 Mo1 Cl2 98.89(12) . 2_575 ?
O2 Mo1 O1 167.3(3) 2_575 . ?
O2 Mo1 O1 88.4(3) . . ?
Cl2 Mo1 O1 91.04(7) . . ?
Cl2 Mo1 O1 169.81(7) 2_575 . ?
O2 Mo1 O1 88.4(3) 2_575 2_575 ?
O2 Mo1 O1 167.3(3) . 2_575 ?
Cl2 Mo1 O1 169.81(7) . 2_575 ?
Cl2 Mo1 O1 91.04(7) 2_575 2_575 ?
O1 Mo1 O1 79.15(8) . 2_575 ?
O2 Mo1 Cl1 91.2(3) 2_575 . ?
O2 Mo1 Cl1 96.6(3) . . ?
Cl2 Mo1 Cl1 91.38(6) . . ?
Cl2 Mo1 Cl1 96.84(6) 2_575 . ?
O1 Mo1 Cl1 85.15(4) . . ?
O1 Mo1 Cl1 85.11(4) 2_575 . ?
O2 Mo1 Cl1 96.6(3) 2_575 2_575 ?
O2 Mo1 Cl1 91.2(3) . 2_575 ?
Cl2 Mo1 Cl1 96.84(6) . 2_575 ?
Cl2 Mo1 Cl1 91.38(6) 2_575 2_575 ?
O1 Mo1 Cl1 85.11(4) . 2_575 ?
O1 Mo1 Cl1 85.15(4) 2_575 2_575 ?
Cl1 Mo1 Cl1 167.36(3) . 2_575 ?
C5 O1 C1 110.94(17) . . ?
C5 O1 Mo1 127.24(12) . . ?
C1 O1 Mo1 121.64(14) . . ?
C2 C3 C4 110.5(2) . . ?
C2 C3 H3A 109.6 . . ?
C4 C3 H3A 109.6 . . ?
C2 C3 H3B 109.6 . . ?
C4 C3 H3B 109.6 . . ?
H3A C3 H3B 108.1 . . ?
C1 C2 C3 110.9(2) . . ?
C1 C2 H2A 109.5 . . ?
C3 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C3 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
O1 C1 C2 109.63(17) . . ?
O1 C1 H1A 109.7 . . ?
C2 C1 H1A 109.7 . . ?
O1 C1 H1B 109.7 . . ?
C2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
C5 C4 C3 110.98(18) . . ?
C5 C4 H4A 109.4 . . ?
C3 C4 H4A 109.4 . . ?
C5 C4 H4B 109.4 . . ?
C3 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
O1 C5 C4 110.55(18) . . ?
O1 C5 H5A 109.5 . . ?
C4 C5 H5A 109.5 . . ?
O1 C5 H5B 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.221
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.058
####################################################################### 
# 
# 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_2c
_database_code_depnum_ccdc_archive 'CCDC 1042921'
_audit_update_record             
;
2015-01-12 deposited with the CCDC.
2015-06-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H20 Cl3.10 Mo O2.90'
_chemical_formula_weight         392.47

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'
Cl Cl 0.1484 0.1585 '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           orthorhombic
_symmetry_space_group_name_H-M   Fdd2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   34.417(6)
_cell_length_b                   7.3606(13)
_cell_length_c                   12.169(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3082.7(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3762
_cell_measurement_theta_min      2.367
_cell_measurement_theta_max      27.861

_exptl_crystal_description       needle
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1583
_exptl_absorpt_coefficient_mu    1.381
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7602
_exptl_absorpt_correction_T_max  0.8629
_exptl_absorpt_process_details   
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1016 (selected reflections only, before parameter refinement)
 R(int) =  0.0483 (selected reflections only, after parameter refinement)
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8563
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.37
_diffrn_reflns_theta_max         27.91
_reflns_number_total             1843
_reflns_number_gt                1742
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1996)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) 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)+(0.0287P)²+0.3221P] 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_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(4)
_refine_ls_number_reflns         1843
_refine_ls_number_parameters     88
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0220
_refine_ls_wR_factor_ref         0.0540
_refine_ls_wR_factor_gt          0.0530
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.95428(7) 0.0380(4) 0.7665(2) 0.0223(5) Uani 1 1 d . . .
H1A H 0.9624 -0.0910 0.7668 0.027 Uiso 1 1 calc R . .
H1B H 0.9652 0.0962 0.7000 0.027 Uiso 1 1 calc R . .
C2 C 0.91021(7) 0.0492(4) 0.7632(2) 0.0252(5) Uani 1 1 d . . .
H2A H 0.8992 -0.0196 0.8257 0.030 Uiso 1 1 calc R . .
H2B H 0.9006 -0.0065 0.6943 0.030 Uiso 1 1 calc R . .
C3 C 0.89684(7) 0.2459(4) 0.7692(3) 0.0289(7) Uani 1 1 d . . .
H3A H 0.8682 0.2500 0.7769 0.035 Uiso 1 1 calc R . .
H3B H 0.9039 0.3094 0.7003 0.035 Uiso 1 1 calc R . .
C4 C 0.91567(7) 0.3422(4) 0.8668(3) 0.0263(5) Uani 1 1 d . . .
H4A H 0.9090 0.4729 0.8647 0.032 Uiso 1 1 calc R . .
H4B H 0.9053 0.2908 0.9361 0.032 Uiso 1 1 calc R . .
C5 C 0.95922(7) 0.3208(3) 0.8648(3) 0.0244(5) Uani 1 1 d . . .
H5A H 0.9699 0.3802 0.7984 0.029 Uiso 1 1 calc R . .
H5B H 0.9707 0.3803 0.9301 0.029 Uiso 1 1 calc R . .
Cl2 Cl 0.96197(9) 0.1405(3) 1.1218(2) 0.0245(6) Uani 0.549(8) 1 d P A 1
O2 O 0.9721(3) 0.1335(11) 1.0915(10) 0.032(2) Uani 0.451(8) 1 d P A 2
Cl1 Cl 0.954626(18) -0.23710(7) 0.98315(5) 0.02152(14) Uani 1 1 d . A .
Mo1 Mo 1.0000 0.0000 1.004273(13) 0.02466(10) Uani 1 2 d S . .
O1 O 0.96937(5) 0.1284(2) 0.86433(16) 0.0200(4) Uani 1 1 d . A .

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
C1 0.0199(12) 0.0307(12) 0.0164(12) 0.0003(10) -0.0012(11) -0.0012(9)
C2 0.0191(12) 0.0334(12) 0.0233(13) 0.0002(11) -0.0045(11) -0.0030(10)
C3 0.0159(11) 0.0335(13) 0.037(2) 0.0079(12) -0.0040(13) -0.0007(11)
C4 0.0193(12) 0.0228(12) 0.0367(15) 0.0037(12) -0.0009(12) 0.0023(10)
C5 0.0212(12) 0.0195(12) 0.0323(14) 0.0075(11) -0.0038(12) -0.0029(10)
Cl2 0.0294(12) 0.0227(7) 0.0214(11) -0.0037(6) 0.0032(8) -0.0006(7)
O2 0.026(4) 0.035(4) 0.035(5) -0.003(3) 0.018(3) 0.000(3)
Cl1 0.0226(3) 0.0182(3) 0.0238(3) 0.0002(2) 0.0044(2) -0.0018(2)
Mo1 0.02360(16) 0.03738(18) 0.01301(13) 0.000 0.000 -0.01235(15)
O1 0.0189(8) 0.0209(9) 0.0201(9) 0.0009(7) -0.0041(7) 0.0009(6)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.459(3) . ?
C1 C2 1.520(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.521(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.528(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.507(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 O1 1.459(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
Cl2 Mo1 2.197(3) . ?
O2 Mo1 1.737(10) . ?
Cl1 Mo1 2.3560(6) . ?
Mo1 O2 1.737(10) 2_755 ?
Mo1 Cl2 2.197(3) 2_755 ?
Mo1 O1 2.2145(18) 2_755 ?
Mo1 O1 2.2145(18) . ?
Mo1 Cl1 2.3559(6) 2_755 ?

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
O1 C1 C2 110.6(2) . . ?
O1 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
C1 C2 C3 110.6(2) . . ?
C1 C2 H2A 109.5 . . ?
C3 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C3 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
C2 C3 C4 110.5(2) . . ?
C2 C3 H3A 109.5 . . ?
C4 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 108.1 . . ?
C5 C4 C3 111.1(2) . . ?
C5 C4 H4A 109.4 . . ?
C3 C4 H4A 109.4 . . ?
C5 C4 H4B 109.4 . . ?
C3 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
O1 C5 C4 109.9(2) . . ?
O1 C5 H5A 109.7 . . ?
C4 C5 H5A 109.7 . . ?
O1 C5 H5B 109.7 . . ?
C4 C5 H5B 109.7 . . ?
H5A C5 H5B 108.2 . . ?
O2 Mo1 O2 104.6(7) . 2_755 ?
O2 Mo1 Cl2 6.4(3) . . ?
O2 Mo1 Cl2 101.4(3) 2_755 . ?
O2 Mo1 Cl2 101.4(3) . 2_755 ?
O2 Mo1 Cl2 6.4(3) 2_755 2_755 ?
Cl2 Mo1 Cl2 98.80(12) . 2_755 ?
O2 Mo1 O1 167.1(3) . 2_755 ?
O2 Mo1 O1 88.0(3) 2_755 2_755 ?
Cl2 Mo1 O1 170.02(8) . 2_755 ?
Cl2 Mo1 O1 90.92(8) 2_755 2_755 ?
O2 Mo1 O1 88.0(3) . . ?
O2 Mo1 O1 167.1(3) 2_755 . ?
Cl2 Mo1 O1 90.92(8) . . ?
Cl2 Mo1 O1 170.02(8) 2_755 . ?
O1 Mo1 O1 79.47(9) 2_755 . ?
O2 Mo1 Cl1 96.8(3) . . ?
O2 Mo1 Cl1 90.8(3) 2_755 . ?
Cl2 Mo1 Cl1 91.42(7) . . ?
Cl2 Mo1 Cl1 96.73(7) 2_755 . ?
O1 Mo1 Cl1 85.16(4) 2_755 . ?
O1 Mo1 Cl1 85.22(4) . . ?
O2 Mo1 Cl1 90.8(3) . 2_755 ?
O2 Mo1 Cl1 96.8(3) 2_755 2_755 ?
Cl2 Mo1 Cl1 96.73(7) . 2_755 ?
Cl2 Mo1 Cl1 91.42(7) 2_755 2_755 ?
O1 Mo1 Cl1 85.22(4) 2_755 2_755 ?
O1 Mo1 Cl1 85.16(4) . 2_755 ?
Cl1 Mo1 Cl1 167.47(3) . 2_755 ?
C5 O1 C1 111.1(2) . . ?
C5 O1 Mo1 121.69(16) . . ?
C1 O1 Mo1 127.02(14) . . ?

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
O1 C1 C2 C3 56.0(3) . . . . ?
C1 C2 C3 C4 -51.7(3) . . . . ?
C2 C3 C4 C5 52.9(3) . . . . ?
C3 C4 C5 O1 -57.3(3) . . . . ?
C4 C5 O1 C1 61.8(3) . . . . ?
C4 C5 O1 Mo1 -114.1(2) . . . . ?
C2 C1 O1 C5 -61.3(3) . . . . ?
C2 C1 O1 Mo1 114.24(19) . . . . ?
O2 Mo1 O1 C5 38.5(3) . . . . ?
O2 Mo1 O1 C5 -152.0(13) 2_755 . . . ?
Cl2 Mo1 O1 C5 44.14(17) . . . . ?
Cl2 Mo1 O1 C5 -122.8(5) 2_755 . . . ?
O1 Mo1 O1 C5 -138.56(19) 2_755 . . . ?
Cl1 Mo1 O1 C5 135.49(16) . . . . ?
Cl1 Mo1 O1 C5 -52.54(16) 2_755 . . . ?
O2 Mo1 O1 C1 -136.7(3) . . . . ?
O2 Mo1 O1 C1 32.8(13) 2_755 . . . ?
Cl2 Mo1 O1 C1 -131.00(18) . . . . ?
Cl2 Mo1 O1 C1 62.1(5) 2_755 . . . ?
O1 Mo1 O1 C1 46.30(15) 2_755 . . . ?
Cl1 Mo1 O1 C1 -39.65(17) . . . . ?
Cl1 Mo1 O1 C1 132.32(18) 2_755 . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.91
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.067
####################################################################### 
# 
# 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_2d
_database_code_depnum_ccdc_archive 'CCDC 1042922'
_audit_update_record             
;
2015-01-12 deposited with the CCDC.
2015-06-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H20 Cl3.08 Mo O2.92'
_chemical_formula_weight         392.01

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'
Cl Cl 0.1484 0.1585 '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           orthorhombic
_symmetry_space_group_name_H-M   Fdd2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   34.424(5)
_cell_length_b                   7.3591(10)
_cell_length_c                   12.1582(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3080.1(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5316
_cell_measurement_theta_min      2.3665
_cell_measurement_theta_max      28.570

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1581
_exptl_absorpt_coefficient_mu    1.379
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7895
_exptl_absorpt_correction_T_max  0.8745
_exptl_absorpt_process_details   
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.0939 (selected reflections only, before parameter refinement)
 R(int) =  0.0404 (selected reflections only, after parameter refinement)
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(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  "'phi and omega scans"
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8150
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.37
_diffrn_reflns_theta_max         26.97
_reflns_number_total             1679
_reflns_number_gt                1633
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1996)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) 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)+(0.0097P)²+4.9752P] 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_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.98(3)
_refine_ls_number_reflns         1679
_refine_ls_number_parameters     89
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0168
_refine_ls_R_factor_gt           0.0159
_refine_ls_wR_factor_ref         0.0348
_refine_ls_wR_factor_gt          0.0345
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.95420(5) 0.0371(3) 0.77475(17) 0.0224(4) Uani 1 1 d . . .
H1A H 0.9622 -0.0920 0.7753 0.027 Uiso 1 1 calc R . .
H1B H 0.9651 0.0947 0.7079 0.027 Uiso 1 1 calc R . .
C2 C 0.91024(5) 0.0490(3) 0.77192(19) 0.0254(4) Uani 1 1 d . . .
H2A H 0.8993 -0.0198 0.8346 0.031 Uiso 1 1 calc R . .
H2B H 0.9005 -0.0066 0.7031 0.031 Uiso 1 1 calc R . .
C3 C 0.89684(5) 0.2464(3) 0.7782(2) 0.0283(5) Uani 1 1 d . . .
H3A H 0.9039 0.3101 0.7093 0.034 Uiso 1 1 calc R . .
H3B H 0.8682 0.2505 0.7859 0.034 Uiso 1 1 calc R . .
C4 C 0.91564(5) 0.3419(3) 0.8757(2) 0.0263(4) Uani 1 1 d . . .
H4A H 0.9089 0.4726 0.8740 0.032 Uiso 1 1 calc R . .
H4B H 0.9054 0.2899 0.9450 0.032 Uiso 1 1 calc R . .
C5 C 0.95923(6) 0.3206(3) 0.8729(2) 0.0247(4) Uani 1 1 d . . .
H5A H 0.9697 0.3798 0.8061 0.030 Uiso 1 1 calc R . .
H5B H 0.9708 0.3805 0.9380 0.030 Uiso 1 1 calc R . .
Cl2 Cl 0.96186(7) 0.1405(3) 1.13020(17) 0.0246(5) Uani 0.538(6) 1 d P A 1
O2 O 0.9720(2) 0.1328(9) 1.1004(8) 0.0323(16) Uani 0.462(6) 1 d P A 2
Cl1 Cl 0.954637(14) -0.23713(6) 0.99149(4) 0.02163(11) Uani 1 1 d . A .
Mo1 Mo 1.0000 0.0000 1.012753(11) 0.02452(7) Uani 1 2 d S . .
O1 O 0.96950(4) 0.12838(17) 0.87260(12) 0.0201(3) Uani 1 1 d . A .

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
C1 0.0224(10) 0.0294(10) 0.0153(9) 0.0002(8) -0.0039(8) -0.0017(8)
C2 0.0209(9) 0.0322(10) 0.0232(10) -0.0003(9) -0.0037(9) -0.0037(8)
C3 0.0169(8) 0.0339(10) 0.0341(16) 0.0078(10) -0.0034(9) 0.0010(9)
C4 0.0201(9) 0.0209(10) 0.0378(12) 0.0041(9) -0.0018(9) 0.0014(8)
C5 0.0224(9) 0.0190(9) 0.0327(11) 0.0067(9) -0.0058(9) -0.0015(8)
Cl2 0.0304(10) 0.0221(6) 0.0213(9) -0.0041(5) 0.0021(6) -0.0005(6)
O2 0.029(3) 0.029(3) 0.039(4) -0.003(3) 0.010(2) 0.001(2)
Cl1 0.0235(2) 0.0179(2) 0.0235(3) 0.00050(19) 0.00420(18) -0.00143(17)
Mo1 0.02390(12) 0.03760(14) 0.01206(10) 0.000 0.000 -0.01260(12)
O1 0.0199(7) 0.0205(7) 0.0200(7) 0.0022(6) -0.0039(6) 0.0001(5)

_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
C1 O1 1.464(2) . ?
C1 C2 1.516(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.525(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.523(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.509(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 O1 1.458(2) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
Cl2 Mo1 2.198(2) . ?
O2 Mo1 1.738(8) . ?
Cl1 Mo1 2.3560(5) . ?
Mo1 O2 1.738(8) 2_755 ?
Mo1 Cl2 2.198(2) 2_755 ?
Mo1 O1 2.2133(13) 2_755 ?
Mo1 O1 2.2133(13) . ?
Mo1 Cl1 2.3560(5) 2_755 ?

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
O1 C1 C2 110.55(16) . . ?
O1 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
C1 C2 C3 110.82(17) . . ?
C1 C2 H2A 109.5 . . ?
C3 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C3 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
C4 C3 C2 110.47(18) . . ?
C4 C3 H3A 109.6 . . ?
C2 C3 H3A 109.6 . . ?
C4 C3 H3B 109.6 . . ?
C2 C3 H3B 109.6 . . ?
H3A C3 H3B 108.1 . . ?
C5 C4 C3 110.91(19) . . ?
C5 C4 H4A 109.5 . . ?
C3 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 108.0 . . ?
O1 C5 C4 109.99(16) . . ?
O1 C5 H5A 109.7 . . ?
C4 C5 H5A 109.7 . . ?
O1 C5 H5B 109.7 . . ?
C4 C5 H5B 109.7 . . ?
H5A C5 H5B 108.2 . . ?
O2 Mo1 O2 104.4(6) 2_755 . ?
O2 Mo1 Cl2 6.2(3) 2_755 2_755 ?
O2 Mo1 Cl2 101.4(2) . 2_755 ?
O2 Mo1 Cl2 101.4(2) 2_755 . ?
O2 Mo1 Cl2 6.2(3) . . ?
Cl2 Mo1 Cl2 98.97(11) 2_755 . ?
O2 Mo1 O1 88.2(3) 2_755 2_755 ?
O2 Mo1 O1 167.2(3) . 2_755 ?
Cl2 Mo1 O1 90.92(7) 2_755 2_755 ?
Cl2 Mo1 O1 169.82(7) . 2_755 ?
O2 Mo1 O1 167.2(3) 2_755 . ?
O2 Mo1 O1 88.2(3) . . ?
Cl2 Mo1 O1 169.82(7) 2_755 . ?
Cl2 Mo1 O1 90.92(7) . . ?
O1 Mo1 O1 79.31(7) 2_755 . ?
O2 Mo1 Cl1 96.7(2) 2_755 2_755 ?
O2 Mo1 Cl1 91.1(2) . 2_755 ?
Cl2 Mo1 Cl1 91.36(6) 2_755 2_755 ?
Cl2 Mo1 Cl1 96.82(6) . 2_755 ?
O1 Mo1 Cl1 85.25(4) 2_755 2_755 ?
O1 Mo1 Cl1 85.05(4) . 2_755 ?
O2 Mo1 Cl1 91.1(2) 2_755 . ?
O2 Mo1 Cl1 96.7(2) . . ?
Cl2 Mo1 Cl1 96.82(6) 2_755 . ?
Cl2 Mo1 Cl1 91.36(6) . . ?
O1 Mo1 Cl1 85.05(4) 2_755 . ?
O1 Mo1 Cl1 85.25(4) . . ?
Cl1 Mo1 Cl1 167.40(2) 2_755 . ?
C5 O1 C1 111.08(15) . . ?
C5 O1 Mo1 121.82(13) . . ?
C1 O1 Mo1 126.91(11) . . ?

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
O1 C1 C2 C3 55.7(2) . . . . ?
C1 C2 C3 C4 -52.0(2) . . . . ?
C2 C3 C4 C5 53.1(2) . . . . ?
C3 C4 C5 O1 -57.7(2) . . . . ?
C4 C5 O1 C1 61.8(2) . . . . ?
C4 C5 O1 Mo1 -113.48(17) . . . . ?
C2 C1 O1 C5 -60.9(2) . . . . ?
C2 C1 O1 Mo1 114.02(15) . . . . ?
O2 Mo1 O1 C5 -151.1(11) 2_755 . . . ?
O2 Mo1 O1 C5 38.4(3) . . . . ?
Cl2 Mo1 O1 C5 -122.5(4) 2_755 . . . ?
Cl2 Mo1 O1 C5 43.99(14) . . . . ?
O1 Mo1 O1 C5 -138.87(15) 2_755 . . . ?
Cl1 Mo1 O1 C5 -52.78(13) 2_755 . . . ?
Cl1 Mo1 O1 C5 135.28(13) . . . . ?
O2 Mo1 O1 C1 34.4(11) 2_755 . . . ?
O2 Mo1 O1 C1 -136.0(3) . . . . ?
Cl2 Mo1 O1 C1 63.1(4) 2_755 . . . ?
Cl2 Mo1 O1 C1 -130.48(14) . . . . ?
O1 Mo1 O1 C1 46.66(12) 2_755 . . . ?
Cl1 Mo1 O1 C1 132.75(13) 2_755 . . . ?
Cl1 Mo1 O1 C1 -39.19(13) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.97
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.267
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.044
####################################################################### 
# 
# 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_2b
_database_code_depnum_ccdc_archive 'CCDC 1042923'
_audit_update_record             
;
2015-01-12 deposited with the CCDC.
2015-06-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H20 Cl3.08 Mo O2.92'
_chemical_formula_weight         392.18

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'
Cl Cl 0.1484 0.1585 '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           orthorhombic
_symmetry_space_group_name_H-M   Fdd2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   34.434(3)
_cell_length_b                   7.3641(7)
_cell_length_c                   12.1545(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3082.1(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5126
_cell_measurement_theta_min      2.366
_cell_measurement_theta_max      28.561

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1582
_exptl_absorpt_coefficient_mu    1.379
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7894
_exptl_absorpt_correction_T_max  0.8304
_exptl_absorpt_process_details   
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.0897 (selected reflections only, before parameter refinement)
 R(int) =  0.0440 (selected reflections only, after parameter refinement)
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7422
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.37
_diffrn_reflns_theta_max         27.00
_reflns_number_total             1677
_reflns_number_gt                1649
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1996)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) 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)+(0.0142P)²+4.2941P] 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_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_number_reflns         1677
_refine_ls_number_parameters     88
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0176
_refine_ls_R_factor_gt           0.0171
_refine_ls_wR_factor_ref         0.0398
_refine_ls_wR_factor_gt          0.0396
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.066
_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
C1 C 0.04066(6) 0.3210(3) 0.1346(2) 0.0252(4) Uani 1 1 d . . .
H1A H 0.0301 0.3800 0.2014 0.030 Uiso 1 1 calc R . .
H1B H 0.0291 0.3809 0.0695 0.030 Uiso 1 1 calc R . .
C2 C 0.08439(6) 0.3422(3) 0.1319(2) 0.0268(4) Uani 1 1 d . . .
H2A H 0.0911 0.4728 0.1337 0.032 Uiso 1 1 calc R . .
H2B H 0.0946 0.2903 0.0626 0.032 Uiso 1 1 calc R . .
C3 C 0.10317(5) 0.2463(3) 0.2297(3) 0.0294(5) Uani 1 1 d . . .
H3A H 0.1318 0.2504 0.2220 0.035 Uiso 1 1 calc R . .
H3B H 0.0961 0.3098 0.2985 0.035 Uiso 1 1 calc R . .
C4 C 0.08979(5) 0.0496(3) 0.2356(2) 0.0260(4) Uani 1 1 d . . .
H4A H 0.1008 -0.0190 0.1729 0.031 Uiso 1 1 calc R . .
H4B H 0.0995 -0.0062 0.3044 0.031 Uiso 1 1 calc R . .
C5 C 0.04582(5) 0.0374(3) 0.23267(17) 0.0239(4) Uani 1 1 d . . .
H5A H 0.0378 -0.0917 0.2322 0.029 Uiso 1 1 calc R . .
H5B H 0.0349 0.0950 0.2994 0.029 Uiso 1 1 calc R . .
Cl2 Cl 0.03803(7) 0.1405(3) -0.12307(18) 0.0252(5) Uani 0.543(7) 1 d P A 1
O2 O 0.0282(2) 0.1328(10) -0.0927(8) 0.0319(16) Uani 0.457(7) 1 d P A 2
Cl1 Cl 0.045394(14) -0.23709(6) 0.01592(4) 0.02217(11) Uani 1 1 d . A .
Mo1 Mo 0.0000 0.0000 -0.005223(9) 0.02520(8) Uani 1 2 d S . .
O1 O 0.03055(4) 0.12826(18) 0.13477(12) 0.0206(3) Uani 1 1 d . A .

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
C1 0.0236(9) 0.0194(10) 0.0325(11) -0.0065(9) -0.0051(9) 0.0012(8)
C2 0.0227(9) 0.0207(10) 0.0370(11) -0.0034(9) -0.0017(10) -0.0008(8)
C3 0.0160(8) 0.0356(11) 0.0367(17) -0.0078(10) -0.0042(10) -0.0001(9)
C4 0.0207(9) 0.0330(10) 0.0243(10) -0.0007(9) -0.0054(9) 0.0034(8)
C5 0.0228(10) 0.0333(11) 0.0155(9) 0.0003(8) -0.0045(8) 0.0015(8)
Cl2 0.0314(9) 0.0234(6) 0.0209(9) 0.0035(6) 0.0023(6) 0.0006(5)
O2 0.035(4) 0.030(3) 0.030(4) 0.001(2) 0.006(2) 0.001(2)
Cl1 0.0240(2) 0.0189(2) 0.0236(3) -0.00044(19) 0.00425(18) 0.00151(16)
Mo1 0.02429(12) 0.03825(15) 0.01305(10) 0.000 0.000 0.01243(11)
O1 0.0208(6) 0.0205(7) 0.0205(7) -0.0024(6) -0.0043(6) -0.0006(5)

_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
C1 O1 1.462(2) . ?
C1 C2 1.514(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.526(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.522(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.517(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 O1 1.463(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
Cl2 Mo1 2.199(2) . ?
O2 Mo1 1.740(9) . ?
Cl1 Mo1 2.3575(5) . ?
Mo1 O2 1.740(9) 2 ?
Mo1 Cl2 2.199(2) 2 ?
Mo1 O1 2.2122(14) . ?
Mo1 O1 2.2122(14) 2 ?
Mo1 Cl1 2.3575(5) 2 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 109.68(16) . . ?
O1 C1 H1A 109.7 . . ?
C2 C1 H1A 109.7 . . ?
O1 C1 H1B 109.7 . . ?
C2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
C1 C2 C3 110.92(19) . . ?
C1 C2 H2A 109.5 . . ?
C3 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C3 C2 H2B 109.5 . . ?
H2A C2 H2B 108.0 . . ?
C4 C3 C2 110.46(19) . . ?
C4 C3 H3A 109.6 . . ?
C2 C3 H3A 109.6 . . ?
C4 C3 H3B 109.6 . . ?
C2 C3 H3B 109.6 . . ?
H3A C3 H3B 108.1 . . ?
C5 C4 C3 110.91(17) . . ?
C5 C4 H4A 109.5 . . ?
C3 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 108.0 . . ?
O1 C5 C4 110.56(17) . . ?
O1 C5 H5A 109.5 . . ?
C4 C5 H5A 109.5 . . ?
O1 C5 H5B 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
O2 Mo1 O2 104.7(5) 2 . ?
O2 Mo1 Cl2 6.1(3) 2 2 ?
O2 Mo1 Cl2 101.4(2) . 2 ?
O2 Mo1 Cl2 101.4(2) 2 . ?
O2 Mo1 Cl2 6.1(3) . . ?
Cl2 Mo1 Cl2 98.72(11) 2 . ?
O2 Mo1 O1 167.2(3) 2 . ?
O2 Mo1 O1 88.0(3) . . ?
Cl2 Mo1 O1 170.04(7) 2 . ?
Cl2 Mo1 O1 90.97(7) . . ?
O2 Mo1 O1 88.0(3) 2 2 ?
O2 Mo1 O1 167.2(3) . 2 ?
Cl2 Mo1 O1 90.97(7) 2 2 ?
Cl2 Mo1 O1 170.04(7) . 2 ?
O1 Mo1 O1 79.44(7) . 2 ?
O2 Mo1 Cl1 96.5(2) 2 2 ?
O2 Mo1 Cl1 91.1(2) . 2 ?
Cl2 Mo1 Cl1 91.41(6) 2 2 ?
Cl2 Mo1 Cl1 96.74(6) . 2 ?
O1 Mo1 Cl1 85.14(4) . 2 ?
O1 Mo1 Cl1 85.24(4) 2 2 ?
O2 Mo1 Cl1 91.1(2) 2 . ?
O2 Mo1 Cl1 96.5(2) . . ?
Cl2 Mo1 Cl1 96.74(6) 2 . ?
Cl2 Mo1 Cl1 91.41(6) . . ?
O1 Mo1 Cl1 85.24(4) . . ?
O1 Mo1 Cl1 85.14(4) 2 . ?
Cl1 Mo1 Cl1 167.48(2) 2 . ?
C1 O1 C5 111.06(16) . . ?
C1 O1 Mo1 121.81(13) . . ?
C5 O1 Mo1 126.97(11) . . ?

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
O1 C1 C2 C3 -57.7(3) . . . . ?
C1 C2 C3 C4 53.2(2) . . . . ?
C2 C3 C4 C5 -52.0(3) . . . . ?
C3 C4 C5 O1 55.9(2) . . . . ?
C2 C1 O1 C5 61.9(2) . . . . ?
C2 C1 O1 Mo1 -113.78(17) . . . . ?
C4 C5 O1 C1 -61.2(2) . . . . ?
C4 C5 O1 Mo1 114.22(16) . . . . ?
O2 Mo1 O1 C1 -150.4(11) 2 . . . ?
O2 Mo1 O1 C1 38.9(3) . . . . ?
Cl2 Mo1 O1 C1 -122.5(4) 2 . . . ?
Cl2 Mo1 O1 C1 44.28(14) . . . . ?
O1 Mo1 O1 C1 -138.46(15) 2 . . . ?
Cl1 Mo1 O1 C1 -52.41(13) 2 . . . ?
Cl1 Mo1 O1 C1 135.61(13) . . . . ?
O2 Mo1 O1 C5 34.6(11) 2 . . . ?
O2 Mo1 O1 C5 -136.1(3) . . . . ?
Cl2 Mo1 O1 C5 62.6(4) 2 . . . ?
Cl2 Mo1 O1 C5 -130.68(15) . . . . ?
O1 Mo1 O1 C5 46.58(12) 2 . . . ?
Cl1 Mo1 O1 C5 132.64(14) 2 . . . ?
Cl1 Mo1 O1 C5 -39.34(14) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.047
####################################################################### 
# 
# 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_2e
_database_code_depnum_ccdc_archive 'CCDC 1042924'
_audit_update_record             
;
2015-01-12 deposited with the CCDC.
2015-06-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H20 Cl3.05 Mo O2.95'
_chemical_formula_weight         391.60

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'
Cl Cl 0.1484 0.1585 '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           Orthorhombic
_symmetry_space_group_name_H-M   Fdd2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   34.402(7)
_cell_length_b                   7.3748(15)
_cell_length_c                   12.165(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3086.2(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5711
_cell_measurement_theta_min      2.368
_cell_measurement_theta_max      28.7145

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1580
_exptl_absorpt_coefficient_mu    1.372
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7522
_exptl_absorpt_correction_T_max  0.8418
_exptl_absorpt_process_details   
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1528 (selected reflections only, before parameter refinement)
 R(int) =  0.0648 (selected reflections only, after parameter refinement)
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6806
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.28
_diffrn_reflns_theta_max         26.00
_reflns_number_total             1521
_reflns_number_gt                1506
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1996)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) 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)+(0.0229P)²+3.0532P] 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_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.93(4)
_refine_ls_number_reflns         1521
_refine_ls_number_parameters     89
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0210
_refine_ls_R_factor_gt           0.0207
_refine_ls_wR_factor_ref         0.0522
_refine_ls_wR_factor_gt          0.0520
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.075
_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
C1 C 0.95410(7) 0.0379(4) 0.5903(2) 0.0236(5) Uani 1 1 d . . .
H1A H 0.9622 -0.0909 0.5902 0.028 Uiso 1 1 calc R . .
H1B H 0.9649 0.0963 0.5237 0.028 Uiso 1 1 calc R . .
C2 C 0.91027(7) 0.0490(4) 0.5878(2) 0.0268(5) Uani 1 1 d . . .
H2A H 0.8994 -0.0199 0.6505 0.032 Uiso 1 1 calc R . .
H2B H 0.9005 -0.0064 0.5190 0.032 Uiso 1 1 calc R . .
C3 C 0.89690(7) 0.2456(4) 0.5943(3) 0.0296(7) Uani 1 1 d . . .
H3A H 0.8683 0.2496 0.6021 0.036 Uiso 1 1 calc R . .
H3B H 0.9039 0.3092 0.5255 0.036 Uiso 1 1 calc R . .
C4 C 0.91565(7) 0.3417(4) 0.6917(3) 0.0281(5) Uani 1 1 d . . .
H4A H 0.9088 0.4721 0.6898 0.034 Uiso 1 1 calc R . .
H4B H 0.9055 0.2900 0.7610 0.034 Uiso 1 1 calc R . .
C5 C 0.95923(8) 0.3208(4) 0.6884(3) 0.0264(5) Uani 1 1 d . . .
H5A H 0.9697 0.3796 0.6215 0.032 Uiso 1 1 calc R . .
H5B H 0.9709 0.3808 0.7533 0.032 Uiso 1 1 calc R . .
Cl1 Cl 0.954679(19) -0.23713(7) 0.80712(5) 0.02319(15) Uani 1 1 d . A .
Cl2 Cl 0.96185(10) 0.1399(4) 0.9464(2) 0.0261(7) Uani 0.527(9) 1 d P A 1
O2 O 0.9719(3) 0.1335(12) 0.9174(10) 0.031(2) Uani 0.473(9) 1 d P A 2
Mo1 Mo 1.0000 0.0000 0.828508(7) 0.02599(10) Uani 1 2 d S . .
O1 O 0.96946(5) 0.1278(2) 0.68828(15) 0.0214(4) Uani 1 1 d . A .

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
C1 0.0275(13) 0.0297(13) 0.0137(12) 0.0004(10) -0.0031(11) -0.0012(10)
C2 0.0262(13) 0.0308(13) 0.0236(13) 0.0011(11) -0.0051(11) -0.0032(10)
C3 0.0207(12) 0.0352(14) 0.033(2) 0.0080(12) -0.0041(13) 0.0010(11)
C4 0.0269(12) 0.0195(13) 0.0378(14) 0.0040(11) -0.0033(13) 0.0025(10)
C5 0.0292(13) 0.0191(12) 0.0309(14) 0.0067(11) -0.0043(12) -0.0016(11)
Cl1 0.0266(3) 0.0186(3) 0.0244(3) 0.0002(2) 0.0047(2) -0.0016(2)
Cl2 0.0321(14) 0.0238(8) 0.0224(12) -0.0040(7) 0.0029(8) -0.0012(8)
O2 0.025(4) 0.027(3) 0.040(5) 0.004(3) 0.010(3) 0.002(3)
Mo1 0.02728(16) 0.03797(19) 0.01273(14) 0.000 0.000 -0.01300(14)
O1 0.0233(8) 0.0212(10) 0.0196(8) 0.0025(7) -0.0044(7) 0.0001(6)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.463(3) . ?
C1 C2 1.510(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.523(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.523(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.508(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 O1 1.466(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
Cl1 Mo1 2.3573(7) . ?
Cl2 Mo1 2.201(3) . ?
O2 Mo1 1.754(11) . ?
Mo1 O2 1.754(11) 2_755 ?
Mo1 Cl2 2.201(3) 2_755 ?
Mo1 O1 2.2142(18) . ?
Mo1 O1 2.2142(18) 2_755 ?
Mo1 Cl1 2.3573(7) 2_755 ?

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
O1 C1 C2 110.6(2) . . ?
O1 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
C1 C2 C3 110.6(2) . . ?
C1 C2 H2A 109.5 . . ?
C3 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C3 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
C2 C3 C4 110.8(2) . . ?
C2 C3 H3A 109.5 . . ?
C4 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 108.1 . . ?
C5 C4 C3 110.7(2) . . ?
C5 C4 H4A 109.5 . . ?
C3 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
O1 C5 C4 109.8(2) . . ?
O1 C5 H5A 109.7 . . ?
C4 C5 H5A 109.7 . . ?
O1 C5 H5B 109.7 . . ?
C4 C5 H5B 109.7 . . ?
H5A C5 H5B 108.2 . . ?
O2 Mo1 O2 103.9(7) . 2_755 ?
O2 Mo1 Cl2 6.2(3) . . ?
O2 Mo1 Cl2 101.0(3) 2_755 . ?
O2 Mo1 Cl2 101.0(3) . 2_755 ?
O2 Mo1 Cl2 6.2(3) 2_755 2_755 ?
Cl2 Mo1 Cl2 98.69(16) . 2_755 ?
O2 Mo1 O1 88.5(4) . . ?
O2 Mo1 O1 167.4(4) 2_755 . ?
Cl2 Mo1 O1 91.10(10) . . ?
Cl2 Mo1 O1 169.93(9) 2_755 . ?
O2 Mo1 O1 167.4(4) . 2_755 ?
O2 Mo1 O1 88.5(4) 2_755 2_755 ?
Cl2 Mo1 O1 169.92(9) . 2_755 ?
Cl2 Mo1 O1 91.10(10) 2_755 2_755 ?
O1 Mo1 O1 79.22(9) . 2_755 ?
O2 Mo1 Cl1 96.9(3) . . ?
O2 Mo1 Cl1 91.0(3) 2_755 . ?
Cl2 Mo1 Cl1 91.45(8) . . ?
Cl2 Mo1 Cl1 96.80(8) 2_755 . ?
O1 Mo1 Cl1 85.23(5) . . ?
O1 Mo1 Cl1 85.01(5) 2_755 . ?
O2 Mo1 Cl1 91.0(3) . 2_755 ?
O2 Mo1 Cl1 96.9(3) 2_755 2_755 ?
Cl2 Mo1 Cl1 96.80(8) . 2_755 ?
Cl2 Mo1 Cl1 91.45(8) 2_755 2_755 ?
O1 Mo1 Cl1 85.01(5) . 2_755 ?
O1 Mo1 Cl1 85.23(5) 2_755 2_755 ?
Cl1 Mo1 Cl1 167.32(3) . 2_755 ?
C1 O1 C5 110.76(19) . . ?
C1 O1 Mo1 127.30(14) . . ?
C5 O1 Mo1 121.76(16) . . ?

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
O1 C1 C2 C3 56.0(3) . . . . ?
C1 C2 C3 C4 -52.0(3) . . . . ?
C2 C3 C4 C5 53.1(3) . . . . ?
C3 C4 C5 O1 -57.7(3) . . . . ?
C2 C1 O1 C5 -61.5(3) . . . . ?
C2 C1 O1 Mo1 113.7(2) . . . . ?
C4 C5 O1 C1 62.1(3) . . . . ?
C4 C5 O1 Mo1 -113.4(2) . . . . ?
O2 Mo1 O1 C1 -136.1(3) . . . . ?
O2 Mo1 O1 C1 33.7(14) 2_755 . . . ?
Cl2 Mo1 O1 C1 -130.49(19) . . . . ?
Cl2 Mo1 O1 C1 63.0(6) 2_755 . . . ?
O1 Mo1 O1 C1 46.69(16) 2_755 . . . ?
Cl1 Mo1 O1 C1 -39.12(17) . . . . ?
Cl1 Mo1 O1 C1 132.78(18) 2_755 . . . ?
O2 Mo1 O1 C5 38.6(3) . . . . ?
O2 Mo1 O1 C5 -151.6(14) 2_755 . . . ?
Cl2 Mo1 O1 C5 44.23(18) . . . . ?
Cl2 Mo1 O1 C5 -122.3(5) 2_755 . . . ?
O1 Mo1 O1 C5 -138.59(19) 2_755 . . . ?
Cl1 Mo1 O1 C5 135.59(17) . . . . ?
Cl1 Mo1 O1 C5 -52.51(16) 2_755 . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.053

####################################################################### 
# 
# 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_1b
_database_code_depnum_ccdc_archive 'CCDC 1042925'
_audit_update_record             
;
2015-01-12 deposited with the CCDC.
2015-06-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H20 Cl4 Mo O2'
_chemical_formula_weight         410.00

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'
Cl Cl 0.1484 0.1585 '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           Orthorhombic
_symmetry_space_group_name_H-M   Fdd2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   34.242(5)
_cell_length_b                   7.4150(11)
_cell_length_c                   12.1939(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3096.0(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1120
_cell_measurement_theta_min      2.379
_cell_measurement_theta_max      20.0365

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.759
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1648
_exptl_absorpt_coefficient_mu    1.526
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7603
_exptl_absorpt_correction_T_max  0.8501
_exptl_absorpt_process_details   
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1330 (selected reflections only, before parameter refinement)
 R(int) =  0.0641 (selected reflections only, after parameter refinement)
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8251
_diffrn_reflns_av_R_equivalents  0.0724
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.38
_diffrn_reflns_theta_max         26.98
_reflns_number_total             1691
_reflns_number_gt                1470
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1996)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) 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)+(0.0577P)²+1.8509P] 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_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.98(10)
_refine_ls_number_reflns         1691
_refine_ls_number_parameters     79
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0433
_refine_ls_wR_factor_ref         0.1096
_refine_ls_wR_factor_gt          0.1039
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.085
_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
C1 C 0.54117(16) 0.6790(7) 0.3623(6) 0.0181(12) Uani 1 1 d . . .
H1A H 0.5301 0.6201 0.2964 0.022 Uiso 1 1 calc R . .
H1B H 0.5298 0.6202 0.4278 0.022 Uiso 1 1 calc R . .
C2 C 0.58446(16) 0.6551(8) 0.3632(6) 0.0221(13) Uani 1 1 d . . .
H2A H 0.5908 0.5249 0.3605 0.027 Uiso 1 1 calc R . .
H2B H 0.5952 0.7046 0.4323 0.027 Uiso 1 1 calc R . .
C3 C 0.60323(16) 0.7495(8) 0.2667(5) 0.0230(15) Uani 1 1 d . . .
H3A H 0.5962 0.6857 0.1982 0.028 Uiso 1 1 calc R . .
H3B H 0.6320 0.7451 0.2746 0.028 Uiso 1 1 calc R . .
C4 C 0.59009(17) 0.9453(8) 0.2590(6) 0.0238(13) Uani 1 1 d . . .
H4A H 0.6017 1.0153 0.3200 0.029 Uiso 1 1 calc R . .
H4B H 0.5994 0.9980 0.1891 0.029 Uiso 1 1 calc R . .
C5 C 0.54593(16) 0.9583(8) 0.2647(5) 0.0183(12) Uani 1 1 d . . .
H5A H 0.5381 1.0869 0.2653 0.022 Uiso 1 1 calc R . .
H5B H 0.5345 0.9014 0.1987 0.022 Uiso 1 1 calc R . .
Cl1 Cl 0.53737(5) 0.8572(2) 0.61726(18) 0.0413(5) Uani 1 1 d . . .
Cl2 Cl 0.54576(4) 1.23584(17) 0.47986(11) 0.0200(3) Uani 1 1 d . . .
Mo1 Mo 0.5000 1.0000 0.49590(4) 0.0217(2) Uani 1 2 d S . .
O1 O 0.53085(10) 0.8701(5) 0.3621(3) 0.0162(8) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.018(3) 0.013(3) 0.023(3) -0.003(2) -0.001(3) -0.001(2)
C2 0.024(3) 0.016(3) 0.026(3) 0.003(3) 0.000(3) -0.001(2)
C3 0.017(3) 0.025(3) 0.027(4) -0.006(3) 0.003(2) 0.001(3)
C4 0.022(3) 0.027(3) 0.022(3) 0.003(3) -0.001(3) -0.003(2)
C5 0.019(3) 0.024(3) 0.013(3) 0.000(2) 0.003(2) -0.001(2)
Cl1 0.0480(11) 0.0378(11) 0.0381(10) 0.0038(9) 0.0014(9) -0.0019(9)
Cl2 0.0213(7) 0.0166(7) 0.0220(8) 0.0017(6) -0.0029(5) -0.0029(5)
Mo1 0.0212(4) 0.0254(4) 0.0184(3) 0.000 0.000 -0.0075(4)
O1 0.019(2) 0.017(2) 0.0124(19) -0.0021(17) 0.0032(18) -0.0031(16)

_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
C1 O1 1.461(6) . ?
C1 C2 1.493(7) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.513(9) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.523(9) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.517(8) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 O1 1.451(7) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
Cl1 Mo1 2.224(2) . ?
Cl2 Mo1 2.3562(13) . ?
Mo1 O1 2.169(4) . ?
Mo1 O1 2.169(4) 2_675 ?
Mo1 Cl1 2.224(2) 2_675 ?
Mo1 Cl2 2.3562(13) 2_675 ?

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
O1 C1 C2 110.8(4) . . ?
O1 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
C1 C2 C3 111.2(5) . . ?
C1 C2 H2A 109.4 . . ?
C3 C2 H2A 109.4 . . ?
C1 C2 H2B 109.4 . . ?
C3 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
C2 C3 C4 111.3(5) . . ?
C2 C3 H3A 109.4 . . ?
C4 C3 H3A 109.4 . . ?
C2 C3 H3B 109.4 . . ?
C4 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
C5 C4 C3 110.6(5) . . ?
C5 C4 H4A 109.5 . . ?
C3 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
O1 C5 C4 111.3(5) . . ?
O1 C5 H5A 109.4 . . ?
C4 C5 H5A 109.4 . . ?
O1 C5 H5B 109.4 . . ?
C4 C5 H5B 109.4 . . ?
H5A C5 H5B 108.0 . . ?
O1 Mo1 O1 82.4(2) . 2_675 ?
O1 Mo1 Cl1 172.66(12) . 2_675 ?
O1 Mo1 Cl1 90.52(11) 2_675 2_675 ?
O1 Mo1 Cl1 90.52(11) . . ?
O1 Mo1 Cl1 172.66(12) 2_675 . ?
Cl1 Mo1 Cl1 96.59(11) 2_675 . ?
O1 Mo1 Cl2 86.74(10) . . ?
O1 Mo1 Cl2 86.10(10) 2_675 . ?
Cl1 Mo1 Cl2 94.85(6) 2_675 . ?
Cl1 Mo1 Cl2 91.48(6) . . ?
O1 Mo1 Cl2 86.10(10) . 2_675 ?
O1 Mo1 Cl2 86.74(10) 2_675 2_675 ?
Cl1 Mo1 Cl2 91.48(6) 2_675 2_675 ?
Cl1 Mo1 Cl2 94.85(6) . 2_675 ?
Cl2 Mo1 Cl2 170.48(7) . 2_675 ?
C5 O1 C1 110.7(4) . . ?
C5 O1 Mo1 126.1(3) . . ?
C1 O1 Mo1 123.1(4) . . ?

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
O1 C1 C2 C3 -56.9(7) . . . . ?
C1 C2 C3 C4 51.7(7) . . . . ?
C2 C3 C4 C5 -50.2(7) . . . . ?
C3 C4 C5 O1 54.8(7) . . . . ?
C4 C5 O1 C1 -60.4(6) . . . . ?
C4 C5 O1 Mo1 116.3(4) . . . . ?
C2 C1 O1 C5 61.3(7) . . . . ?
C2 C1 O1 Mo1 -115.5(5) . . . . ?
O1 Mo1 O1 C5 45.2(3) 2_675 . . . ?
Cl1 Mo1 O1 C5 61.4(11) 2_675 . . . ?
Cl1 Mo1 O1 C5 -132.8(4) . . . . ?
Cl2 Mo1 O1 C5 -41.3(4) . . . . ?
Cl2 Mo1 O1 C5 132.4(4) 2_675 . . . ?
O1 Mo1 O1 C1 -138.6(4) 2_675 . . . ?
Cl1 Mo1 O1 C1 -122.3(9) 2_675 . . . ?
Cl1 Mo1 O1 C1 43.5(4) . . . . ?
Cl2 Mo1 O1 C1 135.0(4) . . . . ?
Cl2 Mo1 O1 C1 -51.3(4) 2_675 . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.98
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.124
####################################################################### 
# 
# 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_1c
_database_code_depnum_ccdc_archive 'CCDC 1042926'
_audit_update_record             
;
2015-01-12 deposited with the CCDC.
2015-06-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H20 Cl4 Mo O2'
_chemical_formula_weight         410.00

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'
Cl Cl 0.1484 0.1585 '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           Orthorhombic
_symmetry_space_group_name_H-M   Fdd2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   34.184(6)
_cell_length_b                   7.4247(12)
_cell_length_c                   12.202(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3097.0(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4741
_cell_measurement_theta_min      2.383
_cell_measurement_theta_max      28.4835

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.759
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1648
_exptl_absorpt_coefficient_mu    1.525
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7401
_exptl_absorpt_correction_T_max  0.8381
_exptl_absorpt_process_details   
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1007 (selected reflections only, before parameter refinement)
 R(int) =  0.0439 (selected reflections only, after parameter refinement)
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6075
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.38
_diffrn_reflns_theta_max         27.00
_reflns_number_total             1684
_reflns_number_gt                1668
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1996)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) 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)+(0.0382P)²+19.9289P] 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_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.85(6)
_refine_ls_number_reflns         1684
_refine_ls_number_parameters     79
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0270
_refine_ls_wR_factor_ref         0.0731
_refine_ls_wR_factor_gt          0.0729
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.080
_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
C1 C 0.04089(10) 0.3228(5) 0.1270(4) 0.0196(7) Uani 1 1 d . . .
H1A H 0.0298 0.3816 0.1929 0.024 Uiso 1 1 calc R . .
H1B H 0.0294 0.3811 0.0615 0.024 Uiso 1 1 calc R . .
C2 C 0.08474(10) 0.3458(5) 0.1260(3) 0.0213(7) Uani 1 1 d . . .
H2A H 0.0912 0.4757 0.1277 0.026 Uiso 1 1 calc R . .
H2B H 0.0955 0.2945 0.0574 0.026 Uiso 1 1 calc R . .
C3 C 0.10336(10) 0.2520(5) 0.2244(3) 0.0226(9) Uani 1 1 d . . .
H3A H 0.0958 0.3157 0.2924 0.027 Uiso 1 1 calc R . .
H3B H 0.1322 0.2570 0.2177 0.027 Uiso 1 1 calc R . .
C4 C 0.09019(10) 0.0552(5) 0.2313(3) 0.0212(7) Uani 1 1 d . . .
H4A H 0.1018 -0.0137 0.1700 0.025 Uiso 1 1 calc R . .
H4B H 0.0996 0.0018 0.3008 0.025 Uiso 1 1 calc R . .
C5 C 0.04586(10) 0.0420(5) 0.2262(3) 0.0186(7) Uani 1 1 d . . .
H5A H 0.0380 -0.0863 0.2259 0.022 Uiso 1 1 calc R . .
H5B H 0.0344 0.0997 0.2918 0.022 Uiso 1 1 calc R . .
Cl1 Cl 0.03769(3) 0.14396(14) -0.12771(10) 0.0339(2) Uani 1 1 d . . .
Cl2 Cl 0.04585(2) -0.23538(10) 0.01024(6) 0.01859(18) Uani 1 1 d . . .
Mo1 Mo 0.0000 0.0000 -0.00460(2) 0.01971(12) Uani 1 2 d S . .
O1 O 0.03097(6) 0.1302(3) 0.1276(2) 0.0167(5) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0187(15) 0.0141(16) 0.0262(17) -0.0025(14) -0.0048(15) 0.0003(13)
C2 0.0201(15) 0.0166(16) 0.0273(17) 0.0013(14) -0.0019(15) -0.0034(14)
C3 0.0156(14) 0.0260(17) 0.026(3) -0.0037(15) -0.0047(13) -0.0004(14)
C4 0.0179(15) 0.0248(17) 0.0209(18) 0.0004(15) -0.0008(14) 0.0026(13)
C5 0.0204(16) 0.0225(17) 0.0130(15) 0.0004(14) -0.0017(13) -0.0020(13)
Cl1 0.0392(5) 0.0297(5) 0.0328(5) 0.0039(4) -0.0005(4) 0.0010(4)
Cl2 0.0197(4) 0.0147(4) 0.0214(4) 0.0014(3) 0.0034(3) 0.0034(3)
Mo1 0.01916(19) 0.0207(2) 0.0193(2) 0.000 0.000 0.00648(17)
O1 0.0197(11) 0.0141(12) 0.0163(11) -0.0012(10) -0.0038(11) 0.0001(9)

_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
C1 O1 1.470(4) . ?
C1 C2 1.509(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.527(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.531(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.520(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 O1 1.461(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
Cl1 Mo1 2.2492(12) . ?
Cl2 Mo1 2.3544(8) . ?
Mo1 O1 2.158(2) . ?
Mo1 O1 2.158(2) 2 ?
Mo1 Cl1 2.2492(12) 2 ?
Mo1 Cl2 2.3544(8) 2 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 109.8(3) . . ?
O1 C1 H1A 109.7 . . ?
C2 C1 H1A 109.7 . . ?
O1 C1 H1B 109.7 . . ?
C2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
C1 C2 C3 110.8(3) . . ?
C1 C2 H2A 109.5 . . ?
C3 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C3 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
C2 C3 C4 110.9(3) . . ?
C2 C3 H3A 109.5 . . ?
C4 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 108.1 . . ?
C5 C4 C3 110.6(3) . . ?
C5 C4 H4A 109.5 . . ?
C3 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
O1 C5 C4 110.6(3) . . ?
O1 C5 H5A 109.5 . . ?
C4 C5 H5A 109.5 . . ?
O1 C5 H5B 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
O1 Mo1 O1 83.27(13) . 2 ?
O1 Mo1 Cl1 173.26(7) . 2 ?
O1 Mo1 Cl1 90.30(7) 2 2 ?
O1 Mo1 Cl1 90.30(7) . . ?
O1 Mo1 Cl1 173.26(7) 2 . ?
Cl1 Mo1 Cl1 96.19(6) 2 . ?
O1 Mo1 Cl2 86.37(6) . 2 ?
O1 Mo1 Cl2 87.05(6) 2 2 ?
Cl1 Mo1 Cl2 91.31(3) 2 2 ?
Cl1 Mo1 Cl2 94.58(4) . 2 ?
O1 Mo1 Cl2 87.05(6) . . ?
O1 Mo1 Cl2 86.37(6) 2 . ?
Cl1 Mo1 Cl2 94.58(4) 2 . ?
Cl1 Mo1 Cl2 91.31(3) . . ?
Cl2 Mo1 Cl2 171.18(4) 2 . ?
C5 O1 C1 111.1(3) . . ?
C5 O1 Mo1 125.83(19) . . ?
C1 O1 Mo1 123.1(2) . . ?

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
O1 C1 C2 C3 -57.6(4) . . . . ?
C1 C2 C3 C4 52.9(4) . . . . ?
C2 C3 C4 C5 -51.5(4) . . . . ?
C3 C4 C5 O1 55.6(4) . . . . ?
C4 C5 O1 C1 -61.3(4) . . . . ?
C4 C5 O1 Mo1 116.9(3) . . . . ?
C2 C1 O1 C5 62.2(4) . . . . ?
C2 C1 O1 Mo1 -116.1(3) . . . . ?
O1 Mo1 O1 C5 44.3(2) 2 . . . ?
Cl1 Mo1 O1 C5 61.7(7) 2 . . . ?
Cl1 Mo1 O1 C5 -133.7(2) . . . . ?
Cl2 Mo1 O1 C5 131.7(2) 2 . . . ?
Cl2 Mo1 O1 C5 -42.4(2) . . . . ?
O1 Mo1 O1 C1 -137.8(3) 2 . . . ?
Cl1 Mo1 O1 C1 -120.3(6) 2 . . . ?
Cl1 Mo1 O1 C1 44.2(2) . . . . ?
Cl2 Mo1 O1 C1 -50.3(2) 2 . . . ?
Cl2 Mo1 O1 C1 135.5(2) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.090
####################################################################### 
# 
# 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_1d
_database_code_depnum_ccdc_archive 'CCDC 1042927'
_audit_update_record             
;
2015-01-12 deposited with the CCDC.
2015-06-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H20 Cl4 Mo O2'
_chemical_formula_weight         410.00

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'
Cl Cl 0.1484 0.1585 '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           Orthorhombic
_symmetry_space_group_name_H-M   Fdd2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   34.185(15)
_cell_length_b                   7.413(3)
_cell_length_c                   12.197(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3091(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4352
_cell_measurement_theta_min      2.383
_cell_measurement_theta_max      28.387

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1648
_exptl_absorpt_coefficient_mu    1.528
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7106
_exptl_absorpt_correction_T_max  0.8379
_exptl_absorpt_process_details   
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1396 (selected reflections only, before parameter refinement)
 R(int) =  0.0527 (selected reflections only, after parameter refinement)
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5988
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.38
_diffrn_reflns_theta_max         26.97
_reflns_number_total             1668
_reflns_number_gt                1639
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1996)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) 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)+(0.0575P)²+18.4102P] 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_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.72(8)
_refine_ls_number_reflns         1668
_refine_ls_number_parameters     79
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0353
_refine_ls_wR_factor_ref         0.0951
_refine_ls_wR_factor_gt          0.0947
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.083
_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
C1 C 0.04091(12) 0.3226(6) 0.1276(5) 0.0232(8) Uani 1 1 d . . .
H1A H 0.0299 0.3814 0.1936 0.028 Uiso 1 1 calc R . .
H1B H 0.0294 0.3810 0.0621 0.028 Uiso 1 1 calc R . .
C2 C 0.08464(12) 0.3453(6) 0.1265(4) 0.0240(8) Uani 1 1 d . . .
H2A H 0.0912 0.4754 0.1283 0.029 Uiso 1 1 calc R . .
H2B H 0.0953 0.2940 0.0578 0.029 Uiso 1 1 calc R . .
C3 C 0.10348(13) 0.2515(6) 0.2245(4) 0.0258(11) Uani 1 1 d . . .
H3A H 0.0962 0.3159 0.2926 0.031 Uiso 1 1 calc R . .
H3B H 0.1323 0.2561 0.2171 0.031 Uiso 1 1 calc R . .
C4 C 0.09029(12) 0.0551(6) 0.2325(4) 0.0242(8) Uani 1 1 d . . .
H4A H 0.1020 -0.0150 0.1716 0.029 Uiso 1 1 calc R . .
H4B H 0.0996 0.0027 0.3024 0.029 Uiso 1 1 calc R . .
C5 C 0.04589(12) 0.0419(6) 0.2269(4) 0.0219(8) Uani 1 1 d . . .
H5A H 0.0380 -0.0867 0.2269 0.026 Uiso 1 1 calc R . .
H5B H 0.0344 0.0999 0.2924 0.026 Uiso 1 1 calc R . .
Cl1 Cl 0.03758(4) 0.14368(17) -0.12720(13) 0.0382(3) Uani 1 1 d . . .
Cl2 Cl 0.04582(3) -0.23549(12) 0.01070(8) 0.0217(2) Uani 1 1 d . . .
Mo1 Mo 0.0000 0.0000 -0.00462(3) 0.02293(16) Uani 1 2 d S . .
O1 O 0.03094(8) 0.1296(4) 0.1281(3) 0.0196(6) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0270(19) 0.0128(19) 0.030(2) -0.0017(17) -0.0048(18) 0.0003(16)
C2 0.0274(19) 0.0153(18) 0.029(2) 0.0001(17) -0.0012(19) -0.0023(16)
C3 0.0227(19) 0.026(2) 0.029(3) -0.0038(17) -0.0052(17) -0.0002(17)
C4 0.026(2) 0.023(2) 0.024(2) -0.0011(18) -0.0009(18) 0.0030(16)
C5 0.030(2) 0.0194(19) 0.0159(18) 0.0006(16) -0.0011(16) -0.0020(16)
Cl1 0.0485(7) 0.0287(6) 0.0373(6) 0.0038(5) -0.0009(6) 0.0012(5)
Cl2 0.0266(5) 0.0136(4) 0.0248(5) 0.0009(4) 0.0032(4) 0.0033(3)
Mo1 0.0263(2) 0.0206(2) 0.0219(2) 0.000 0.000 0.0069(2)
O1 0.0269(14) 0.0131(14) 0.0187(13) -0.0023(11) -0.0035(13) 0.0002(10)

_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
C1 O1 1.471(5) . ?
C1 C2 1.504(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.525(7) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.527(6) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.523(6) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 O1 1.461(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
Cl1 Mo1 2.2405(15) . ?
Cl2 Mo1 2.3529(12) . ?
Mo1 O1 2.159(3) 2 ?
Mo1 O1 2.159(3) . ?
Mo1 Cl1 2.2405(15) 2 ?
Mo1 Cl2 2.3529(12) 2 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 109.8(3) . . ?
O1 C1 H1A 109.7 . . ?
C2 C1 H1A 109.7 . . ?
O1 C1 H1B 109.7 . . ?
C2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
C1 C2 C3 111.2(4) . . ?
C1 C2 H2A 109.4 . . ?
C3 C2 H2A 109.4 . . ?
C1 C2 H2B 109.4 . . ?
C3 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
C2 C3 C4 111.1(4) . . ?
C2 C3 H3A 109.4 . . ?
C4 C3 H3A 109.4 . . ?
C2 C3 H3B 109.4 . . ?
C4 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
C5 C4 C3 110.7(4) . . ?
C5 C4 H4A 109.5 . . ?
C3 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
O1 C5 C4 110.9(3) . . ?
O1 C5 H5A 109.5 . . ?
C4 C5 H5A 109.5 . . ?
O1 C5 H5B 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 108.0 . . ?
O1 Mo1 O1 82.86(16) 2 . ?
O1 Mo1 Cl1 90.46(9) 2 2 ?
O1 Mo1 Cl1 173.05(9) . 2 ?
O1 Mo1 Cl1 173.05(9) 2 . ?
O1 Mo1 Cl1 90.46(9) . . ?
Cl1 Mo1 Cl1 96.28(8) 2 . ?
O1 Mo1 Cl2 86.35(8) 2 . ?
O1 Mo1 Cl2 86.82(8) . . ?
Cl1 Mo1 Cl2 94.70(5) 2 . ?
Cl1 Mo1 Cl2 91.37(5) . . ?
O1 Mo1 Cl2 86.82(8) 2 2 ?
O1 Mo1 Cl2 86.35(8) . 2 ?
Cl1 Mo1 Cl2 91.37(5) 2 2 ?
Cl1 Mo1 Cl2 94.70(5) . 2 ?
Cl2 Mo1 Cl2 170.89(5) . 2 ?
C5 O1 C1 110.8(3) . . ?
C5 O1 Mo1 126.3(2) . . ?
C1 O1 Mo1 122.9(3) . . ?

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
O1 C1 C2 C3 -57.5(5) . . . . ?
C1 C2 C3 C4 52.4(5) . . . . ?
C2 C3 C4 C5 -50.7(5) . . . . ?
C3 C4 C5 O1 55.1(5) . . . . ?
C4 C5 O1 C1 -61.2(4) . . . . ?
C4 C5 O1 Mo1 116.8(3) . . . . ?
C2 C1 O1 C5 62.2(5) . . . . ?
C2 C1 O1 Mo1 -115.9(4) . . . . ?
O1 Mo1 O1 C5 44.4(3) 2 . . . ?
Cl1 Mo1 O1 C5 60.6(8) 2 . . . ?
Cl1 Mo1 O1 C5 -133.6(3) . . . . ?
Cl2 Mo1 O1 C5 -42.3(3) . . . . ?
Cl2 Mo1 O1 C5 131.7(3) 2 . . . ?
O1 Mo1 O1 C1 -137.8(3) 2 . . . ?
Cl1 Mo1 O1 C1 -121.6(7) 2 . . . ?
Cl1 Mo1 O1 C1 44.2(3) . . . . ?
Cl2 Mo1 O1 C1 135.5(3) . . . . ?
Cl2 Mo1 O1 C1 -50.5(3) 2 . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.97
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.138
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.122
####################################################################### 
# 
# 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_1e
_database_code_depnum_ccdc_archive 'CCDC 1042928'
_audit_update_record             
;
2015-01-12 deposited with the CCDC.
2015-06-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H20 Cl4 Mo O2'
_chemical_formula_weight         410.00

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'
Cl Cl 0.1484 0.1585 '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           Orthorhombic
_symmetry_space_group_name_H-M   Fdd2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   34.19(6)
_cell_length_b                   7.486(12)
_cell_length_c                   12.28(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3143(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1662
_cell_measurement_theta_min      2.383
_cell_measurement_theta_max      27.1995

_exptl_crystal_description       plate
_exptl_crystal_colour            orange-red
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1648
_exptl_absorpt_coefficient_mu    1.503
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7633
_exptl_absorpt_correction_T_max  0.8402
_exptl_absorpt_process_details   
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1353 (selected reflections only, before parameter refinement)
 R(int) =  0.0883 (selected reflections only, after parameter refinement)
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5406
_diffrn_reflns_av_R_equivalents  0.0738
_diffrn_reflns_av_unetI/netI     0.0688
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.38
_diffrn_reflns_theta_max         26.00
_reflns_number_total             1540
_reflns_number_gt                1428
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1996)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) 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)+(0.0315P)²+0.0000P] 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_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.08(8)
_refine_ls_number_reflns         1540
_refine_ls_number_parameters     78
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0372
_refine_ls_wR_factor_ref         0.0851
_refine_ls_wR_factor_gt          0.0821
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.047
_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
C1 C 0.04108(14) 0.3234(6) 0.1442(5) 0.0192(10) Uani 1 1 d . . .
H1A H 0.0296 0.3818 0.2091 0.023 Uiso 1 1 calc R . .
H1B H 0.0298 0.3804 0.0786 0.023 Uiso 1 1 calc R . .
C2 C 0.08466(13) 0.3491(7) 0.1448(5) 0.0198(10) Uani 1 1 d . . .
H2A H 0.0908 0.4783 0.1475 0.024 Uiso 1 1 calc R . .
H2B H 0.0959 0.2999 0.0768 0.024 Uiso 1 1 calc R . .
C3 C 0.10311(14) 0.2553(7) 0.2430(4) 0.0216(14) Uani 1 1 d . . .
H3A H 0.0954 0.3185 0.3105 0.026 Uiso 1 1 calc R . .
H3B H 0.1320 0.2607 0.2368 0.026 Uiso 1 1 calc R . .
C4 C 0.09011(15) 0.0584(7) 0.2505(4) 0.0224(11) Uani 1 1 d . . .
H4A H 0.1019 -0.0104 0.1900 0.027 Uiso 1 1 calc R . .
H4B H 0.0994 0.0064 0.3199 0.027 Uiso 1 1 calc R . .
C5 C 0.04631(15) 0.0443(7) 0.2446(4) 0.0183(11) Uani 1 1 d . . .
H5A H 0.0386 -0.0831 0.2447 0.022 Uiso 1 1 calc R . .
H5B H 0.0346 0.1017 0.3095 0.022 Uiso 1 1 calc R . .
Cl1 Cl 0.03798(4) 0.14571(17) -0.11019(12) 0.0248(3) Uani 1 1 d . . .
Cl2 Cl 0.04605(4) -0.23418(14) 0.02861(10) 0.0193(3) Uani 1 1 d . . .
Mo1 Mo 0.0000 0.0000 0.01723(3) 0.01595(17) Uani 1 2 d S . .
O1 O 0.03117(8) 0.1317(4) 0.1448(3) 0.0167(7) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.025(3) 0.011(2) 0.022(3) 0.001(2) -0.003(2) -0.002(2)
C2 0.021(2) 0.015(2) 0.023(3) 0.001(2) 0.000(2) -0.003(2)
C3 0.015(2) 0.024(3) 0.026(4) 0.001(2) -0.002(2) -0.003(2)
C4 0.026(3) 0.025(3) 0.016(3) 0.000(2) 0.000(2) 0.003(2)
C5 0.026(3) 0.015(2) 0.014(3) 0.003(2) -0.003(2) -0.002(2)
Cl1 0.0316(7) 0.0227(7) 0.0203(6) 0.0054(6) 0.0030(6) -0.0001(6)
Cl2 0.0223(6) 0.0142(6) 0.0215(7) 0.0015(6) 0.0025(5) 0.0029(4)
Mo1 0.0193(3) 0.0141(3) 0.0144(3) 0.000 0.000 0.0025(3)
O1 0.0216(18) 0.0125(18) 0.0160(17) 0.0031(15) -0.0047(16) -0.0014(14)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.475(6) . ?
C1 C2 1.502(7) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.532(7) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.542(8) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.503(7) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 O1 1.482(6) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
Cl1 Mo1 2.308(3) . ?
Cl2 Mo1 2.360(3) . ?
Mo1 O1 2.136(4) . ?
Mo1 O1 2.136(4) 2 ?
Mo1 Cl1 2.308(3) 2 ?
Mo1 Cl2 2.360(3) 2 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 110.6(4) . . ?
O1 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
C1 C2 C3 110.7(4) . . ?
C1 C2 H2A 109.5 . . ?
C3 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C3 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
C2 C3 C4 111.5(4) . . ?
C2 C3 H3A 109.3 . . ?
C4 C3 H3A 109.3 . . ?
C2 C3 H3B 109.3 . . ?
C4 C3 H3B 109.3 . . ?
H3A C3 H3B 108.0 . . ?
C5 C4 C3 110.6(4) . . ?
C5 C4 H4A 109.5 . . ?
C3 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
O1 C5 C4 110.9(4) . . ?
O1 C5 H5A 109.5 . . ?
C4 C5 H5A 109.5 . . ?
O1 C5 H5B 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 108.0 . . ?
O1 Mo1 O1 85.6(2) . 2 ?
O1 Mo1 Cl1 175.12(10) . 2 ?
O1 Mo1 Cl1 89.91(15) 2 2 ?
O1 Mo1 Cl1 89.91(15) . . ?
O1 Mo1 Cl1 175.12(10) 2 . ?
Cl1 Mo1 Cl1 94.60(14) 2 . ?
O1 Mo1 Cl2 88.10(12) . . ?
O1 Mo1 Cl2 86.93(12) 2 . ?
Cl1 Mo1 Cl2 93.68(11) 2 . ?
Cl1 Mo1 Cl2 90.92(11) . . ?
O1 Mo1 Cl2 86.93(12) . 2 ?
O1 Mo1 Cl2 88.10(12) 2 2 ?
Cl1 Mo1 Cl2 90.92(11) 2 2 ?
Cl1 Mo1 Cl2 93.68(11) . 2 ?
Cl2 Mo1 Cl2 173.21(6) . 2 ?
C1 O1 C5 110.7(4) . . ?
C1 O1 Mo1 124.1(3) . . ?
C5 O1 Mo1 125.2(3) . . ?

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
O1 C1 C2 C3 -56.8(6) . . . . ?
C1 C2 C3 C4 51.9(6) . . . . ?
C2 C3 C4 C5 -51.3(6) . . . . ?
C3 C4 C5 O1 55.5(5) . . . . ?
C2 C1 O1 C5 61.5(6) . . . . ?
C2 C1 O1 Mo1 -117.6(4) . . . . ?
C4 C5 O1 C1 -61.1(5) . . . . ?
C4 C5 O1 Mo1 118.1(4) . . . . ?
O1 Mo1 O1 C1 -137.6(4) 2 . . . ?
Cl1 Mo1 O1 C1 -113.2(11) 2 . . . ?
Cl1 Mo1 O1 C1 44.4(3) . . . . ?
Cl2 Mo1 O1 C1 135.3(3) . . . . ?
Cl2 Mo1 O1 C1 -49.3(3) 2 . . . ?
O1 Mo1 O1 C5 43.4(3) 2 . . . ?
Cl1 Mo1 O1 C5 67.8(12) 2 . . . ?
Cl1 Mo1 O1 C5 -134.6(3) . . . . ?
Cl2 Mo1 O1 C5 -43.7(3) . . . . ?
Cl2 Mo1 O1 C5 131.7(3) 2 . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.111

