# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_dk130315
_database_code_depnum_ccdc_archive 'CCDC 1496098'
_audit_update_record             
;
2016-07-26 deposited with the CCDC.
2016-09-08 downloaded from the CCDC.
;

_publ_contact_name               'Fedyanin, Ivan V.'
_publ_contact_email              octy@xrlab.ineos.ac.ru

_audit_creation_method           'Modified SHELXL output'
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H33 Cl3 Mo3 O10'
_chemical_formula_sum            'C10 H33 Cl3 Mo3 O10'
_chemical_formula_weight         707.53

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'

_space_group_crystal_system      trigonal
_space_group_IT_number           160
_space_group_name_H-M_alt        'R 3 m :H'
_space_group_name_Hall           'R 3 -2"'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   16.8738(12)
_cell_length_b                   16.8738(12)
_cell_length_c                   6.7163(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1656.1(3)
_cell_formula_units_Z            3
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    2937
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      29.87

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.128
_exptl_crystal_F_000             1050
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    2.082
_shelx_estimated_absorpt_T_min   0.669
_shelx_estimated_absorpt_T_max   0.835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.113
_exptl_absorpt_correction_T_max  0.155
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker SMART APEX II diffractometer'
_diffrn_detector_type            'Bruker APEX II CCD area detector'
_diffrn_measurement_method       'ο scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7179
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.414
_diffrn_reflns_theta_max         29.989
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1181
_reflns_number_gt                1120
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.982
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0160P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 528 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1181
_refine_ls_number_parameters     70
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0209
_refine_ls_R_factor_gt           0.0183
_refine_ls_wR_factor_ref         0.0361
_refine_ls_wR_factor_gt          0.0351
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_restrained_S_all      0.990
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.27995(2) 0.72005(2) 0.48524(8) 0.02085(10) Uani 1 2 d S T P . .
Cl1 Cl 0.21253(6) 0.78747(6) 0.2800(2) 0.0317(3) Uani 1 2 d S T P A .
O1 O 0.39021(15) 0.7804(3) 0.3055(8) 0.0214(13) Uani 1 2 d S T P A .
O2 O 0.3333 0.6667 0.6951(12) 0.023(2) Uani 1 6 d S T P A .
C1 C 0.3333 0.6667 0.9095(13) 0.041(2) Uani 1 6 d S T P . .
H1 H 0.3021 0.6042 0.9534 0.061 Uiso 1 2 d R U P A .
C2 C 0.4313(2) 0.8626(4) 0.1859(10) 0.0384(15) Uani 1 2 d S T P . .
H2A H 0.4916 0.8753 0.1398 0.058 Uiso 0.5 1 calc R U P A .
H2B H 0.4380 0.9141 0.2661 0.058 Uiso 0.5 1 calc R U P . .
H2C H 0.3921 0.8541 0.0708 0.058 Uiso 0.5 1 calc R U P . .
O3 O 0.1571(7) 0.6471(4) 0.6357(12) 0.0321(19) Uani 0.5 1 d . . P A 1
H3 H 0.1535 0.5965 0.6661 0.038 Uiso 0.5 1 d R U P A 1
C3 C 0.102(2) 0.676(2) 0.713(4) 0.040(5) Uani 0.5 1 d . . P A 1
H3A H 0.0448 0.6234 0.7573 0.060 Uiso 0.5 1 calc R U P A 1
H3B H 0.0895 0.7100 0.6115 0.060 Uiso 0.5 1 calc R U P A 1
H3C H 0.1329 0.7165 0.8269 0.060 Uiso 0.5 1 calc R U P A 1
O3' O 0.1896(5) 0.6861(4) 0.6707(11) 0.0262(15) Uani 0.5 1 d . . P A 2
C3' C 0.1080(17) 0.690(2) 0.707(4) 0.034(6) Uani 0.5 1 d . . P A 2
H3'A H 0.0608 0.6315 0.7623 0.051 Uiso 0.5 1 calc R U P A 2
H3'B H 0.0861 0.7018 0.5814 0.051 Uiso 0.5 1 calc R U P A 2
H3'C H 0.1212 0.7393 0.8015 0.051 Uiso 0.5 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 O3' 1.825(8) 4_665 ?
Mo1 O3' 1.825(8) . ?
Mo1 O1 2.015(4) . ?
Mo1 O1 2.015(4) 2_665 ?
Mo1 O3 2.070(8) . ?
Mo1 O3 2.070(8) 4_665 ?
Mo1 O2 2.103(6) . ?
Mo1 Cl1 2.4047(15) . ?
Mo1 Mo1 2.7024(8) 3_565 ?
Mo1 Mo1 2.7024(8) 2_665 ?
O1 C2 1.444(7) . ?
O1 Mo1 2.015(4) 3_565 ?
O2 C1 1.440(12) . ?
O2 Mo1 2.103(6) 2_665 ?
O2 Mo1 2.103(6) 3_565 ?
C1 H1 0.9599 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
O3 C3 1.35(3) . ?
O3 H3 0.8500 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
O3' C3' 1.43(2) . ?
C3' H3'A 0.9800 . ?
C3' H3'B 0.9800 . ?
C3' H3'C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3' Mo1 O3' 70.2(4) 4_665 . ?
O3' Mo1 O1 99.3(2) 4_665 . ?
O3' Mo1 O1 169.4(2) . . ?
O3' Mo1 O1 169.4(2) 4_665 2_665 ?
O3' Mo1 O1 99.3(2) . 2_665 ?
O1 Mo1 O1 91.2(3) . 2_665 ?
O1 Mo1 O3 172.0(3) . . ?
O1 Mo1 O3 81.4(2) 2_665 . ?
O1 Mo1 O3 81.4(2) . 4_665 ?
O1 Mo1 O3 172.0(3) 2_665 4_665 ?
O3 Mo1 O3 105.9(4) . 4_665 ?
O3' Mo1 O2 83.0(3) 4_665 . ?
O3' Mo1 O2 83.0(3) . . ?
O1 Mo1 O2 97.65(10) . . ?
O1 Mo1 O2 97.65(10) 2_665 . ?
O3 Mo1 O2 86.2(3) . . ?
O3 Mo1 O2 86.2(3) 4_665 . ?
O3' Mo1 Cl1 91.2(3) 4_665 . ?
O3' Mo1 Cl1 91.2(3) . . ?
O1 Mo1 Cl1 87.31(11) . . ?
O1 Mo1 Cl1 87.31(11) 2_665 . ?
O3 Mo1 Cl1 89.5(3) . . ?
O3 Mo1 Cl1 89.5(3) 4_665 . ?
O2 Mo1 Cl1 172.89(18) . . ?
O3' Mo1 Mo1 95.9(2) 4_665 3_565 ?
O3' Mo1 Mo1 132.7(3) . 3_565 ?
O1 Mo1 Mo1 47.89(10) . 3_565 ?
O1 Mo1 Mo1 92.51(10) 2_665 3_565 ?
O3 Mo1 Mo1 134.8(3) . 3_565 ?
O3 Mo1 Mo1 84.61(19) 4_665 3_565 ?
O2 Mo1 Mo1 50.01(13) . 3_565 ?
Cl1 Mo1 Mo1 135.20(3) . 3_565 ?
O3' Mo1 Mo1 132.7(3) 4_665 2_665 ?
O3' Mo1 Mo1 95.9(2) . 2_665 ?
O1 Mo1 Mo1 92.51(10) . 2_665 ?
O1 Mo1 Mo1 47.89(10) 2_665 2_665 ?
O3 Mo1 Mo1 84.61(19) . 2_665 ?
O3 Mo1 Mo1 134.8(3) 4_665 2_665 ?
O2 Mo1 Mo1 50.01(13) . 2_665 ?
Cl1 Mo1 Mo1 135.20(3) . 2_665 ?
Mo1 Mo1 Mo1 60.0 3_565 2_665 ?
C2 O1 Mo1 134.18(17) . 3_565 ?
C2 O1 Mo1 134.18(17) . . ?
Mo1 O1 Mo1 84.2(2) 3_565 . ?
C1 O2 Mo1 132.09(17) . 2_665 ?
C1 O2 Mo1 132.09(17) . 3_565 ?
Mo1 O2 Mo1 80.0(3) 2_665 3_565 ?
C1 O2 Mo1 132.09(17) . . ?
Mo1 O2 Mo1 80.0(3) 2_665 . ?
Mo1 O2 Mo1 80.0(3) 3_565 . ?
O2 C1 H1 107.9 . . ?
O1 C2 H2A 109.5 . . ?
O1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
O1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C3 O3 Mo1 129.5(14) . . ?
C3 O3 H3 123.8 . . ?
Mo1 O3 H3 105.1 . . ?
O3 C3 H3A 109.5 . . ?
O3 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
O3 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C3' O3' Mo1 140.6(13) . . ?
O3' C3' H3'A 109.5 . . ?
O3' C3' H3'B 109.5 . . ?
H3'A C3' H3'B 109.5 . . ?
O3' C3' H3'C 109.5 . . ?
H3'A C3' H3'C 109.5 . . ?
H3'B C3' H3'C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3' Mo1 O3' C3' 91.5(19) 4_665 . . . ?
O1 Mo1 O3' C3' 83(2) . . . . ?
O1 Mo1 O3' C3' -86.8(19) 2_665 . . . ?
O2 Mo1 O3' C3' 176.5(19) . . . . ?
Cl1 Mo1 O3' C3' 0.6(19) . . . . ?
Mo1 Mo1 O3' C3' 170.9(18) 3_565 . . . ?
Mo1 Mo1 O3' C3' -135.1(19) 2_665 . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3 O3 0.85 1.50 2.314(13) 157.7 6_565

_refine_diff_density_max         0.382
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.063

####################################################################### 
# 
# 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_dk160312
_database_code_depnum_ccdc_archive 'CCDC 1496099'
_audit_update_record             
;
2016-07-26 deposited with the CCDC.
2016-09-08 downloaded from the CCDC.
;

_publ_contact_name               'Fedyanin, Ivan V.'
_publ_contact_email              octy@xrlab.ineos.ac.ru

_audit_creation_method           'Modified SHELXL output'
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H38 Cl4 Mo4 O12'
_chemical_formula_sum            'C12 H38 Cl4 Mo4 O12'
_chemical_formula_weight         899.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.7762(3)
_cell_length_b                   8.8015(3)
_cell_length_c                   9.9874(4)
_cell_angle_alpha                68.8208(18)
_cell_angle_beta                 89.0869(19)
_cell_angle_gamma                72.587(2)
_cell_volume                     682.70(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    4403
_cell_measurement_theta_min      4.77
_cell_measurement_theta_max      72.06

_exptl_crystal_description       needle
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.189
_exptl_crystal_F_000             442
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    18.766
_shelx_estimated_absorpt_T_min   0.110
_shelx_estimated_absorpt_T_max   0.283
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.039
_exptl_absorpt_correction_T_max  0.171
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX DUO diffractometer'
_diffrn_detector_type            'Bruker APEX II CCD area detector'
_diffrn_measurement_method       'ο and φ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11018
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         4.774
_diffrn_reflns_theta_max         72.075
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measured_fraction_theta_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_point_group_measured_fraction_full 0.971
_reflns_number_total             2563
_reflns_number_gt                2347
_reflns_threshold_expression     'I > 2σ(I)'

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0400P)²+5.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2563
_refine_ls_number_parameters     151
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0392
_refine_ls_wR_factor_ref         0.0979
_refine_ls_wR_factor_gt          0.0966
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.69892(6) 0.32673(6) 0.69294(5) 0.02834(15) Uani 1 1 d . . . . .
Mo2 Mo 0.58088(5) 0.41751(6) 0.41849(5) 0.02613(14) Uani 1 1 d . . . . .
Cl1 Cl 0.94763(18) 0.2949(2) 0.81547(17) 0.0376(3) Uani 1 1 d . . . . .
Cl3 Cl 0.68680(19) 0.13259(19) 0.42016(16) 0.0354(3) Uani 1 1 d . . . . .
O1 O 0.6001(5) 0.2846(6) 0.8862(4) 0.0330(9) Uani 1 1 d . . . . .
O2 O 0.7588(5) 0.0894(5) 0.7352(4) 0.0316(9) Uani 1 1 d . . . . .
O3 O 0.6287(5) 0.5724(5) 0.6752(4) 0.0325(9) Uani 1 1 d . . . . .
O4 O 0.8005(5) 0.3928(6) 0.5055(4) 0.0318(9) Uani 1 1 d . . . . .
O5 O 0.4810(5) 0.3230(5) 0.6084(4) 0.0281(8) Uani 1 1 d . . . . .
O6 O 0.6595(5) 0.5126(6) 0.2159(4) 0.0332(9) Uani 1 1 d . . . . .
H6 H 0.5789 0.6089 0.1503 0.040 Uiso 1 1 d R U . . .
C1 C 0.6523(9) 0.1299(9) 1.0089(7) 0.0412(15) Uani 1 1 d . . . . .
H1A H 0.5931 0.1443 1.0898 0.062 Uiso 1 1 calc R U . . .
H1B H 0.7674 0.1011 1.0350 0.062 Uiso 1 1 calc R U . . .
H1C H 0.6326 0.0371 0.9868 0.062 Uiso 1 1 calc R U . . .
C2 C 0.9053(8) -0.0490(9) 0.7854(8) 0.0418(16) Uani 1 1 d . . . . .
H2A H 0.8948 -0.1476 0.7669 0.063 Uiso 1 1 calc R U . . .
H2B H 0.9291 -0.0813 0.8894 0.063 Uiso 1 1 calc R U . . .
H2C H 0.9926 -0.0134 0.7346 0.063 Uiso 1 1 calc R U . . .
C3 C 0.6767(8) 0.6798(9) 0.7336(8) 0.0407(15) Uani 1 1 d . . . . .
H3A H 0.6672 0.7903 0.6563 0.061 Uiso 1 1 calc R U . . .
H3B H 0.7884 0.6238 0.7767 0.061 Uiso 1 1 calc R U . . .
H3C H 0.6074 0.6987 0.8078 0.061 Uiso 1 1 calc R U . . .
C4 C 0.9598(8) 0.3316(10) 0.4701(8) 0.0407(15) Uani 1 1 d . . . . .
H4A H 1.0372 0.3242 0.5436 0.061 Uiso 1 1 calc R U . . .
H4B H 0.9730 0.4109 0.3756 0.061 Uiso 1 1 calc R U . . .
H4C H 0.9782 0.2176 0.4667 0.061 Uiso 1 1 calc R U . . .
C5 C 0.3976(8) 0.1980(8) 0.6578(7) 0.0331(13) Uani 1 1 d . . . . .
H5A H 0.3080 0.2277 0.5861 0.050 Uiso 1 1 calc R U . . .
H5B H 0.3563 0.1970 0.7498 0.050 Uiso 1 1 calc R U . . .
H5C H 0.4717 0.0842 0.6713 0.050 Uiso 1 1 calc R U . . .
C6 C 0.7666(9) 0.4320(9) 0.1358(7) 0.0424(16) Uani 1 1 d . . . . .
H6A H 0.8375 0.5001 0.0926 0.064 Uiso 1 1 calc R U . . .
H6B H 0.7050 0.4235 0.0593 0.064 Uiso 1 1 calc R U . . .
H6C H 0.8313 0.3167 0.2001 0.064 Uiso 1 1 calc R U . . .


_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 1.879(4) . ?
Mo1 O3 2.004(4) . ?
Mo1 O4 2.027(4) . ?
Mo1 O1 2.059(4) . ?
Mo1 O5 2.117(4) . ?
Mo1 Cl1 2.4109(15) . ?
Mo1 Mo2 2.6903(6) . ?
Mo1 Mo2 2.7027(7) 2_666 ?
Mo2 O3 2.040(4) 2_666 ?
Mo2 O4 2.045(4) . ?
Mo2 O5 2.074(4) . ?
Mo2 O6 2.085(4) . ?
Mo2 O5 2.098(4) 2_666 ?
Mo2 Cl3 2.3934(16) . ?
Mo2 Mo2 2.6787(9) 2_666 ?
Mo2 Mo1 2.7027(7) 2_666 ?
O1 C1 1.416(7) . ?
O2 C2 1.425(7) . ?
O3 C3 1.434(7) . ?
O3 Mo2 2.040(4) 2_666 ?
O4 C4 1.429(8) . ?
O5 C5 1.438(7) . ?
O5 Mo2 2.098(4) 2_666 ?
O6 C6 1.420(8) . ?
O6 H6 0.9500 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Mo1 O3 172.40(18) . . ?
O2 Mo1 O4 97.69(18) . . ?
O3 Mo1 O4 89.65(18) . . ?
O2 Mo1 O1 88.31(18) . . ?
O3 Mo1 O1 84.25(18) . . ?
O4 Mo1 O1 173.18(18) . . ?
O2 Mo1 O5 82.64(17) . . ?
O3 Mo1 O5 98.37(16) . . ?
O4 Mo1 O5 97.96(16) . . ?
O1 Mo1 O5 85.98(16) . . ?
O2 Mo1 Cl1 91.29(14) . . ?
O3 Mo1 Cl1 87.01(12) . . ?
O4 Mo1 Cl1 87.70(12) . . ?
O1 Mo1 Cl1 88.92(13) . . ?
O5 Mo1 Cl1 172.18(11) . . ?
O2 Mo1 Mo2 94.95(13) . . ?
O3 Mo1 Mo2 91.37(12) . . ?
O4 Mo1 Mo2 48.95(12) . . ?
O1 Mo1 Mo2 134.04(12) . . ?
O5 Mo1 Mo2 49.36(11) . . ?
Cl1 Mo1 Mo2 136.64(4) . . ?
O2 Mo1 Mo2 132.28(13) . 2_666 ?
O3 Mo1 Mo2 48.64(12) . 2_666 ?
O4 Mo1 Mo2 93.37(12) . 2_666 ?
O1 Mo1 Mo2 84.90(12) . 2_666 ?
O5 Mo1 Mo2 49.82(11) . 2_666 ?
Cl1 Mo1 Mo2 135.59(4) . 2_666 ?
Mo2 Mo1 Mo2 59.564(19) . 2_666 ?
O3 Mo2 O4 175.31(17) 2_666 . ?
O3 Mo2 O5 83.26(16) 2_666 . ?
O4 Mo2 O5 98.77(16) . . ?
O3 Mo2 O6 90.58(17) 2_666 . ?
O4 Mo2 O6 87.35(17) . . ?
O5 Mo2 O6 173.82(16) . . ?
O3 Mo2 O5 97.82(16) 2_666 2_666 ?
O4 Mo2 O5 86.02(17) . 2_666 ?
O5 Mo2 O5 100.10(14) . 2_666 ?
O6 Mo2 O5 81.06(16) . 2_666 ?
O3 Mo2 Cl3 86.58(13) 2_666 . ?
O4 Mo2 Cl3 89.19(13) . . ?
O5 Mo2 Cl3 89.61(12) . . ?
O6 Mo2 Cl3 89.64(13) . . ?
O5 Mo2 Cl3 169.72(12) 2_666 . ?
O3 Mo2 Mo2 90.90(12) 2_666 2_666 ?
O4 Mo2 Mo2 93.65(12) . 2_666 ?
O5 Mo2 Mo2 50.46(11) . 2_666 ?
O6 Mo2 Mo2 130.39(12) . 2_666 ?
O5 Mo2 Mo2 49.65(11) 2_666 2_666 ?
Cl3 Mo2 Mo2 139.94(5) . 2_666 ?
O3 Mo2 Mo1 133.99(12) 2_666 . ?
O4 Mo2 Mo1 48.35(12) . . ?
O5 Mo2 Mo1 50.76(11) . . ?
O6 Mo2 Mo1 135.41(12) . . ?
O5 Mo2 Mo1 89.74(11) 2_666 . ?
Cl3 Mo2 Mo1 93.87(4) . . ?
Mo2 Mo2 Mo1 60.45(2) 2_666 . ?
O3 Mo2 Mo1 47.49(12) 2_666 2_666 ?
O4 Mo2 Mo1 136.44(12) . 2_666 ?
O5 Mo2 Mo1 89.92(11) . 2_666 ?
O6 Mo2 Mo1 86.18(12) . 2_666 ?
O5 Mo2 Mo1 50.42(11) 2_666 2_666 ?
Cl3 Mo2 Mo1 133.74(4) . 2_666 ?
Mo2 Mo2 Mo1 59.99(2) 2_666 2_666 ?
Mo1 Mo2 Mo1 120.436(19) . 2_666 ?
C1 O1 Mo1 124.7(4) . . ?
C2 O2 Mo1 134.8(4) . . ?
C3 O3 Mo1 139.0(4) . . ?
C3 O3 Mo2 135.0(4) . 2_666 ?
Mo1 O3 Mo2 83.87(16) . 2_666 ?
C4 O4 Mo1 132.0(4) . . ?
C4 O4 Mo2 132.4(4) . . ?
Mo1 O4 Mo2 82.71(16) . . ?
C5 O5 Mo2 133.0(4) . . ?
C5 O5 Mo2 132.9(4) . 2_666 ?
Mo2 O5 Mo2 79.90(14) . 2_666 ?
C5 O5 Mo1 130.6(3) . . ?
Mo2 O5 Mo1 79.88(14) . . ?
Mo2 O5 Mo1 79.77(14) 2_666 . ?
C6 O6 Mo2 132.5(4) . . ?
C6 O6 H6 108.6 . . ?
Mo2 O6 H6 112.0 . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O2 C2 H2A 109.5 . . ?
O2 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
O2 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O3 C3 H3A 109.5 . . ?
O3 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
O3 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O4 C4 H4A 109.5 . . ?
O4 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
O4 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O5 C5 H5A 109.5 . . ?
O5 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
O5 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O6 C6 H6A 109.5 . . ?
O6 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
O6 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 Mo1 O2 C2 73.8(6) . . . . ?
O1 Mo1 O2 C2 -102.9(6) . . . . ?
O5 Mo1 O2 C2 170.9(6) . . . . ?
Cl1 Mo1 O2 C2 -14.0(6) . . . . ?
Mo2 Mo1 O2 C2 123.0(6) . . . . ?
Mo2 Mo1 O2 C2 175.5(5) 2_666 . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O6 H6 O1 0.95 1.54 2.396(6) 147.6 2_666

_refine_diff_density_max         1.380
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.153

####################################################################### 
# 
# 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_dk150717
_database_code_depnum_ccdc_archive 'CCDC 1496100'
_audit_update_record             
;
2016-07-26 deposited with the CCDC.
2016-09-08 downloaded from the CCDC.
;

_publ_contact_name               'Fedyanin, Ivan V.'
_publ_contact_email              octy@xrlab.ineos.ac.ru

_audit_creation_method           'Modified SHELXL output'
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H39 Cl3 Mo4 O13'
_chemical_formula_sum            'C12 H39 Cl3 Mo4 O13'
_chemical_formula_weight         881.54

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_H-M_alt        'P n'
_space_group_name_Hall           'P -2yac'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   7.1547(3)
_cell_length_b                   19.2160(6)
_cell_length_c                   10.1221(4)
_cell_angle_alpha                90
_cell_angle_beta                 104.388(2)
_cell_angle_gamma                90
_cell_volume                     1347.99(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    5861
_cell_measurement_theta_min      4.60
_cell_measurement_theta_max      72.32

_exptl_crystal_description       plate
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.172
_exptl_crystal_F_000             868
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    18.127
_shelx_estimated_absorpt_T_min   0.063
_shelx_estimated_absorpt_T_max   0.139
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.091
_exptl_absorpt_correction_T_max  0.241
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX DUO diffractometer'
_diffrn_detector_type            'Bruker APEX II CCD area detector'
_diffrn_measurement_method       'ο and φ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14951
_diffrn_reflns_av_unetI/netI     0.0546
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.299
_diffrn_reflns_theta_max         70.936
_diffrn_reflns_theta_full        70.936
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4916
_reflns_number_gt                4498
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.991
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.998

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_refine_special_details          
'Refined as a 2-component inversion twin., Twin'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0400P)²+0.4000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.07(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4916
_refine_ls_number_parameters     302
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0353
_refine_ls_wR_factor_ref         0.0864
_refine_ls_wR_factor_gt          0.0840
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.003
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.61009(13) 0.14265(4) 0.56056(10) 0.0252(2) Uani 1 1 d . . . . .
Mo2 Mo 0.52843(12) 0.23187(4) 0.35521(9) 0.0234(2) Uani 1 1 d . . . . .
Mo3 Mo 0.54892(12) 0.27486(4) 0.60051(8) 0.0228(2) Uani 1 1 d . . . . .
Mo4 Mo 0.46323(14) 0.36676(4) 0.39489(10) 0.0262(2) Uani 1 1 d . . . . .
Cl1 Cl 0.4881(5) 0.03113(13) 0.6184(4) 0.0358(7) Uani 1 1 d . . . . .
Cl2 Cl 0.3162(6) 0.23119(15) 0.1271(4) 0.0376(8) Uani 1 1 d . . . . .
Cl3 Cl 0.5974(5) 0.47579(13) 0.3440(3) 0.0363(7) Uani 1 1 d . . . . .
O1 O 0.7567(15) 0.2315(3) 0.5247(10) 0.023(2) Uani 1 1 d . . . . .
O2 O 0.4056(16) 0.1396(4) 0.3857(11) 0.027(2) Uani 1 1 d . . . . .
O3 O 0.7986(15) 0.0974(4) 0.4745(10) 0.038(2) Uani 1 1 d . . . . .
O4 O 0.8182(17) 0.1452(4) 0.7428(10) 0.037(3) Uani 1 1 d . . . . .
O5 O 0.4243(14) 0.1876(4) 0.6581(9) 0.0266(18) Uani 1 1 d . . . . .
O6 O 0.7326(14) 0.1755(4) 0.2746(8) 0.0286(18) Uani 1 1 d . . . . .
H6 H 0.7528 0.1406 0.3359 0.034 Uiso 1 1 d R U . . .
O7 O 0.6482(15) 0.3221(4) 0.3034(9) 0.0281(19) Uani 1 1 d . . . . .
O8 O 0.3155(15) 0.2768(4) 0.4323(10) 0.026(2) Uani 1 1 d . . . . .
O9 O 0.6766(17) 0.3674(4) 0.5728(11) 0.029(3) Uani 1 1 d . . . . .
O10 O 0.2547(16) 0.3763(4) 0.2412(11) 0.036(2) Uani 1 1 d . . . . .
O11 O 0.3041(16) 0.4170(4) 0.5059(10) 0.039(2) Uani 1 1 d . . . . .
O12 O 0.3637(14) 0.3348(4) 0.7022(12) 0.039(2) Uani 1 1 d . . . . .
H12 H 0.3421 0.3645 0.6313 0.046 Uiso 1 1 d R U . . .
O13 O 0.7478(18) 0.2665(4) 0.8019(10) 0.034(3) Uani 1 1 d . . . . .
H13 H 0.7735 0.2227 0.7803 0.041 Uiso 1 1 d R U . . .
C2 C 0.261(2) 0.0955(6) 0.3113(14) 0.051(4) Uani 1 1 d . . . . .
H2A H 0.3182 0.0508 0.2963 0.077 Uiso 1 1 calc R U . . .
H2B H 0.2009 0.1170 0.2231 0.077 Uiso 1 1 calc R U . . .
H2C H 0.1631 0.0880 0.3624 0.077 Uiso 1 1 calc R U . . .
C3 C 0.855(3) 0.0259(7) 0.4736(18) 0.048(4) Uani 1 1 d . . . . .
H3A H 0.8760 0.0142 0.3842 0.072 Uiso 1 1 calc R U . . .
H3B H 0.7528 -0.0038 0.4919 0.072 Uiso 1 1 calc R U . . .
H3C H 0.9746 0.0184 0.5443 0.072 Uiso 1 1 calc R U . . .
C4 C 0.869(3) 0.0932(6) 0.8410(17) 0.046(4) Uani 1 1 d . . . . .
H4A H 0.9443 0.1135 0.9266 0.068 Uiso 1 1 calc R U . . .
H4B H 0.9472 0.0579 0.8095 0.068 Uiso 1 1 calc R U . . .
H4C H 0.7524 0.0715 0.8561 0.068 Uiso 1 1 calc R U . . .
C5 C 0.301(3) 0.1689(7) 0.740(2) 0.060(5) Uani 1 1 d . . . . .
H5A H 0.2925 0.1181 0.7439 0.090 Uiso 1 1 calc R U . . .
H5B H 0.1725 0.1884 0.7018 0.090 Uiso 1 1 calc R U . . .
H5C H 0.3523 0.1872 0.8326 0.090 Uiso 1 1 calc R U . . .
C6 C 0.703(3) 0.1431(8) 0.1444(18) 0.056(5) Uani 1 1 d . . . . .
H6A H 0.8171 0.1154 0.1414 0.085 Uiso 1 1 calc R U . . .
H6B H 0.6826 0.1789 0.0733 0.085 Uiso 1 1 calc R U . . .
H6C H 0.5898 0.1128 0.1290 0.085 Uiso 1 1 calc R U . . .
C7 C 0.726(2) 0.3388(7) 0.1888(15) 0.042(3) Uani 1 1 d . . . . .
H7A H 0.8092 0.3799 0.2104 0.063 Uiso 1 1 calc R U . . .
H7B H 0.6205 0.3483 0.1086 0.063 Uiso 1 1 calc R U . . .
H7C H 0.8024 0.2994 0.1695 0.063 Uiso 1 1 calc R U . . .
C8 C 0.1116(18) 0.2597(6) 0.4076(14) 0.042(3) Uani 1 1 d . . . . .
H8A H 0.0950 0.2218 0.4686 0.063 Uiso 1 1 calc R U . . .
H8B H 0.0627 0.2449 0.3126 0.063 Uiso 1 1 calc R U . . .
H8C H 0.0399 0.3007 0.4249 0.063 Uiso 1 1 calc R U . . .
C9 C 0.8736(19) 0.3867(6) 0.5905(13) 0.041(3) Uani 1 1 d . . . . .
H9A H 0.9056 0.4245 0.6574 0.061 Uiso 1 1 calc R U . . .
H9B H 0.8944 0.4025 0.5032 0.061 Uiso 1 1 calc R U . . .
H9C H 0.9564 0.3465 0.6231 0.061 Uiso 1 1 calc R U . . .
C10 C 0.208(2) 0.4203(7) 0.1230(15) 0.046(4) Uani 1 1 d . . . . .
H10A H 0.0954 0.4015 0.0569 0.069 Uiso 1 1 calc R U . . .
H10B H 0.3180 0.4222 0.0816 0.069 Uiso 1 1 calc R U . . .
H10C H 0.1787 0.4673 0.1499 0.069 Uiso 1 1 calc R U . . .
C11 C 0.210(2) 0.4816(6) 0.4764(17) 0.039(3) Uani 1 1 d . . . . .
H11A H 0.2005 0.5039 0.5616 0.059 Uiso 1 1 calc R U . . .
H11B H 0.0803 0.4743 0.4177 0.059 Uiso 1 1 calc R U . . .
H11C H 0.2839 0.5116 0.4295 0.059 Uiso 1 1 calc R U . . .
C12 C 0.397(3) 0.3581(7) 0.829(2) 0.049(4) Uani 1 1 d . . . . .
H12A H 0.2842 0.3838 0.8411 0.074 Uiso 1 1 calc R U . . .
H12B H 0.5096 0.3891 0.8478 0.074 Uiso 1 1 calc R U . . .
H12C H 0.4226 0.3187 0.8926 0.074 Uiso 1 1 calc R U . . .
C13 C 0.886(2) 0.3054(8) 0.8717(14) 0.055(4) Uani 1 1 d . . . . .
H13A H 0.9114 0.2933 0.9686 0.083 Uiso 1 1 calc R U . . .
H13B H 0.8482 0.3544 0.8592 0.083 Uiso 1 1 calc R U . . .
H13C H 1.0032 0.2978 0.8399 0.083 Uiso 1 1 calc R U . . .


_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 O3 1.979(10) . ?
Mo1 O2 1.998(10) . ?
Mo1 O5 2.035(9) . ?
Mo1 O4 2.063(10) . ?
Mo1 O1 2.083(8) . ?
Mo1 Cl1 2.439(3) . ?
Mo1 Mo3 2.6262(11) . ?
Mo1 Mo2 2.6454(14) . ?
Mo2 O2 2.036(9) . ?
Mo2 O1 2.054(10) . ?
Mo2 O7 2.058(8) . ?
Mo2 O8 2.066(11) . ?
Mo2 O6 2.137(9) . ?
Mo2 Cl2 2.428(4) . ?
Mo2 Mo3 2.5861(9) . ?
Mo2 Mo4 2.6815(12) . ?
Mo3 O1 2.015(11) . ?
Mo3 O5 2.050(8) . ?
Mo3 O9 2.051(9) . ?
Mo3 O8 2.068(10) . ?
Mo3 O13 2.182(10) . ?
Mo3 O12 2.196(9) . ?
Mo3 Mo4 2.6819(13) . ?
Mo4 O10 1.878(10) . ?
Mo4 O7 1.989(10) . ?
Mo4 O11 2.032(9) . ?
Mo4 O9 2.051(10) . ?
Mo4 O8 2.108(9) . ?
Mo4 Cl3 2.413(3) . ?
O2 C2 1.403(15) . ?
O3 C3 1.433(14) . ?
O4 C4 1.394(16) . ?
O5 C5 1.400(19) . ?
O6 C6 1.425(19) . ?
O6 H6 0.9001 . ?
O7 C7 1.444(18) . ?
O8 C8 1.455(16) . ?
O9 C9 1.425(18) . ?
O10 C10 1.434(16) . ?
O11 C11 1.408(14) . ?
O12 C12 1.33(2) . ?
O12 H12 0.9000 . ?
O13 C13 1.301(18) . ?
O13 H13 0.9001 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Mo1 O2 91.5(4) . . ?
O3 Mo1 O5 177.2(4) . . ?
O2 Mo1 O5 91.1(4) . . ?
O3 Mo1 O4 89.1(5) . . ?
O2 Mo1 O4 179.1(5) . . ?
O5 Mo1 O4 88.2(4) . . ?
O3 Mo1 O1 81.7(4) . . ?
O2 Mo1 O1 99.1(4) . . ?
O5 Mo1 O1 98.9(4) . . ?
O4 Mo1 O1 81.6(4) . . ?
O3 Mo1 Cl1 92.5(3) . . ?
O2 Mo1 Cl1 87.7(3) . . ?
O5 Mo1 Cl1 86.6(2) . . ?
O4 Mo1 Cl1 91.6(3) . . ?
O1 Mo1 Cl1 171.1(3) . . ?
O3 Mo1 Mo3 130.6(3) . . ?
O2 Mo1 Mo3 92.9(2) . . ?
O5 Mo1 Mo3 50.2(2) . . ?
O4 Mo1 Mo3 87.1(2) . . ?
O1 Mo1 Mo3 49.0(3) . . ?
Cl1 Mo1 Mo3 136.85(10) . . ?
O3 Mo1 Mo2 88.9(3) . . ?
O2 Mo1 Mo2 49.6(3) . . ?
O5 Mo1 Mo2 93.6(2) . . ?
O4 Mo1 Mo2 131.0(3) . . ?
O1 Mo1 Mo2 49.8(3) . . ?
Cl1 Mo1 Mo2 137.35(10) . . ?
Mo3 Mo1 Mo2 58.76(3) . . ?
O2 Mo2 O1 98.9(4) . . ?
O2 Mo2 O7 174.0(4) . . ?
O1 Mo2 O7 85.4(3) . . ?
O2 Mo2 O8 85.4(4) . . ?
O1 Mo2 O8 101.2(4) . . ?
O7 Mo2 O8 97.9(4) . . ?
O2 Mo2 O6 88.8(4) . . ?
O1 Mo2 O6 80.8(4) . . ?
O7 Mo2 O6 87.8(4) . . ?
O8 Mo2 O6 174.1(3) . . ?
O2 Mo2 Cl2 87.0(3) . . ?
O1 Mo2 Cl2 166.9(3) . . ?
O7 Mo2 Cl2 87.9(3) . . ?
O8 Mo2 Cl2 90.9(3) . . ?
O6 Mo2 Cl2 87.7(2) . . ?
O2 Mo2 Mo3 93.2(3) . . ?
O1 Mo2 Mo3 49.9(3) . . ?
O7 Mo2 Mo3 92.7(3) . . ?
O8 Mo2 Mo3 51.3(3) . . ?
O6 Mo2 Mo3 130.3(2) . . ?
Cl2 Mo2 Mo3 141.97(10) . . ?
O2 Mo2 Mo1 48.4(3) . . ?
O1 Mo2 Mo1 50.7(2) . . ?
O7 Mo2 Mo1 136.2(2) . . ?
O8 Mo2 Mo1 90.8(3) . . ?
O6 Mo2 Mo1 86.2(2) . . ?
Cl2 Mo2 Mo1 135.04(9) . . ?
Mo3 Mo2 Mo1 60.25(3) . . ?
O2 Mo2 Mo4 136.2(3) . . ?
O1 Mo2 Mo4 90.6(2) . . ?
O7 Mo2 Mo4 47.4(3) . . ?
O8 Mo2 Mo4 50.7(2) . . ?
O6 Mo2 Mo4 135.1(2) . . ?
Cl2 Mo2 Mo4 93.25(8) . . ?
Mo3 Mo2 Mo4 61.18(4) . . ?
Mo1 Mo2 Mo4 121.43(6) . . ?
O1 Mo3 O5 100.7(3) . . ?
O1 Mo3 O9 84.9(4) . . ?
O5 Mo3 O9 171.2(4) . . ?
O1 Mo3 O8 102.4(4) . . ?
O5 Mo3 O8 86.0(4) . . ?
O9 Mo3 O8 99.6(4) . . ?
O1 Mo3 O13 87.4(4) . . ?
O5 Mo3 O13 84.4(4) . . ?
O9 Mo3 O13 89.0(4) . . ?
O8 Mo3 O13 167.4(4) . . ?
O1 Mo3 O12 169.7(4) . . ?
O5 Mo3 O12 86.5(3) . . ?
O9 Mo3 O12 87.1(4) . . ?
O8 Mo3 O12 85.3(4) . . ?
O13 Mo3 O12 86.0(4) . . ?
O1 Mo3 Mo2 51.2(3) . . ?
O5 Mo3 Mo2 95.0(2) . . ?
O9 Mo3 Mo2 93.8(3) . . ?
O8 Mo3 Mo2 51.2(3) . . ?
O13 Mo3 Mo2 137.8(3) . . ?
O12 Mo3 Mo2 136.1(3) . . ?
O1 Mo3 Mo1 51.3(2) . . ?
O5 Mo3 Mo1 49.7(2) . . ?
O9 Mo3 Mo1 136.2(3) . . ?
O8 Mo3 Mo1 91.3(2) . . ?
O13 Mo3 Mo1 88.7(2) . . ?
O12 Mo3 Mo1 136.3(2) . . ?
Mo2 Mo3 Mo1 60.99(4) . . ?
O1 Mo3 Mo4 91.4(2) . . ?
O5 Mo3 Mo4 136.7(3) . . ?
O9 Mo3 Mo4 49.2(3) . . ?
O8 Mo3 Mo4 50.7(2) . . ?
O13 Mo3 Mo4 138.0(2) . . ?
O12 Mo3 Mo4 88.3(3) . . ?
Mo2 Mo3 Mo4 61.17(3) . . ?
Mo1 Mo3 Mo4 122.16(5) . . ?
O10 Mo4 O7 98.1(4) . . ?
O10 Mo4 O11 88.4(5) . . ?
O7 Mo4 O11 172.7(4) . . ?
O10 Mo4 O9 172.5(4) . . ?
O7 Mo4 O9 88.6(4) . . ?
O11 Mo4 O9 84.8(5) . . ?
O10 Mo4 O8 84.2(4) . . ?
O7 Mo4 O8 98.7(4) . . ?
O11 Mo4 O8 85.2(4) . . ?
O9 Mo4 O8 98.3(4) . . ?
O10 Mo4 Cl3 90.8(3) . . ?
O7 Mo4 Cl3 86.0(3) . . ?
O11 Mo4 Cl3 90.7(3) . . ?
O9 Mo4 Cl3 86.2(3) . . ?
O8 Mo4 Cl3 173.6(3) . . ?
O10 Mo4 Mo2 95.9(3) . . ?
O7 Mo4 Mo2 49.6(2) . . ?
O11 Mo4 Mo2 133.2(3) . . ?
O9 Mo4 Mo2 91.1(2) . . ?
O8 Mo4 Mo2 49.3(3) . . ?
Cl3 Mo4 Mo2 135.56(10) . . ?
O10 Mo4 Mo3 133.5(3) . . ?
O7 Mo4 Mo3 91.5(2) . . ?
O11 Mo4 Mo3 86.3(2) . . ?
O9 Mo4 Mo3 49.2(2) . . ?
O8 Mo4 Mo3 49.4(3) . . ?
Cl3 Mo4 Mo3 135.32(9) . . ?
Mo2 Mo4 Mo3 57.66(3) . . ?
Mo3 O1 Mo2 78.9(4) . . ?
Mo3 O1 Mo1 79.7(4) . . ?
Mo2 O1 Mo1 79.5(3) . . ?
C2 O2 Mo1 140.6(8) . . ?
C2 O2 Mo2 137.1(8) . . ?
Mo1 O2 Mo2 82.0(4) . . ?
C3 O3 Mo1 130.3(9) . . ?
C4 O4 Mo1 128.6(9) . . ?
C5 O5 Mo1 139.7(8) . . ?
C5 O5 Mo3 139.6(8) . . ?
Mo1 O5 Mo3 80.0(3) . . ?
C6 O6 Mo2 128.1(10) . . ?
C6 O6 H6 105.9 . . ?
Mo2 O6 H6 97.0 . . ?
C7 O7 Mo4 135.5(8) . . ?
C7 O7 Mo2 131.3(7) . . ?
Mo4 O7 Mo2 83.0(4) . . ?
C8 O8 Mo2 129.9(7) . . ?
C8 O8 Mo3 135.0(9) . . ?
Mo2 O8 Mo3 77.4(4) . . ?
C8 O8 Mo4 132.9(7) . . ?
Mo2 O8 Mo4 79.9(4) . . ?
Mo3 O8 Mo4 79.9(3) . . ?
C9 O9 Mo4 127.5(9) . . ?
C9 O9 Mo3 131.9(7) . . ?
Mo4 O9 Mo3 81.7(3) . . ?
C10 O10 Mo4 136.1(9) . . ?
C11 O11 Mo4 127.3(9) . . ?
C12 O12 Mo3 130.3(10) . . ?
C12 O12 H12 120.9 . . ?
Mo3 O12 H12 87.9 . . ?
C13 O13 Mo3 134.2(9) . . ?
C13 O13 H13 119.7 . . ?
Mo3 O13 H13 88.2 . . ?
O2 C2 H2A 109.5 . . ?
O2 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
O2 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O3 C3 H3A 109.5 . . ?
O3 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
O3 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O4 C4 H4A 109.5 . . ?
O4 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
O4 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O5 C5 H5A 109.5 . . ?
O5 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
O5 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O6 C6 H6A 109.5 . . ?
O6 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
O6 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O7 C7 H7A 109.5 . . ?
O7 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
O7 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O8 C8 H8A 109.5 . . ?
O8 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O8 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O9 C9 H9A 109.5 . . ?
O9 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
O9 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O10 C10 H10A 109.5 . . ?
O10 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
O10 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O11 C11 H11A 109.5 . . ?
O11 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
O11 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O12 C12 H12A 109.5 . . ?
O12 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O12 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O13 C13 H13A 109.5 . . ?
O13 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
O13 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O7 Mo4 O10 C10 -73.9(14) . . . . ?
O11 Mo4 O10 C10 102.8(15) . . . . ?
O8 Mo4 O10 C10 -171.9(14) . . . . ?
Cl3 Mo4 O10 C10 12.1(14) . . . . ?
Mo2 Mo4 O10 C10 -123.9(14) . . . . ?
Mo3 Mo4 O10 C10 -173.8(12) . . . . ?

_refine_diff_density_max         0.769
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.120

####################################################################### 
# 
# 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_dk150528
_database_code_depnum_ccdc_archive 'CCDC 1496101'
_audit_update_record             
;
2016-07-26 deposited with the CCDC.
2016-09-08 downloaded from the CCDC.
;

_publ_contact_name               'Fedyanin, Ivan V.'
_publ_contact_email              octy@xrlab.ineos.ac.ru

_audit_creation_method           'Modified SHELXL output'
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H44 Cl2 Mo4 O14'
_chemical_formula_sum            'C14 H44 Cl2 Mo4 O14'
_chemical_formula_weight         891.15

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   9.6392(4)
_cell_length_b                   10.3534(4)
_cell_length_c                   14.8342(7)
_cell_angle_alpha                90
_cell_angle_beta                 105.179(2)
_cell_angle_gamma                90
_cell_volume                     1428.78(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9948
_cell_measurement_theta_min      4.95
_cell_measurement_theta_max      72.08

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.071
_exptl_crystal_F_000             884
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    16.297
_shelx_estimated_absorpt_T_min   0.092
_shelx_estimated_absorpt_T_max   0.293
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0342
_exptl_absorpt_correction_T_max  0.1711
_exptl_absorpt_process_details   'Bruker TWINABS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX DUO diffractometer'
_diffrn_detector_type            'Bruker APEX II CCD area detector'
_diffrn_measurement_method       'ο and φ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14868
_diffrn_reflns_av_unetI/netI     0.1046
_diffrn_reflns_av_R_equivalents  0.0859
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         4.945
_diffrn_reflns_theta_max         70.986
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             14868
_reflns_number_gt                12199
_reflns_threshold_expression     'I > 2σ(I)'

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_refine_special_details          
;Refined as a 2-component twin 
 with a twin law -1 0 0 0 -1 0 0.802 0 1
 and basf 0.42073, Twin
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²+12.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14868
_refine_ls_number_parameters     162
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_gt           0.0759
_refine_ls_wR_factor_ref         0.2056
_refine_ls_wR_factor_gt          0.1883
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.066
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.60934(13) 0.66356(11) 0.43367(8) 0.0241(3) Uani 1 1 d . . . . .
Mo2 Mo 0.55893(13) 0.40902(10) 0.45743(8) 0.0233(3) Uani 1 1 d . . . . .
Cl1 Cl 0.5805(5) 0.8045(4) 0.3001(3) 0.0366(8) Uani 1 1 d . . . . .
O1 O 0.8076(13) 0.5976(10) 0.4232(8) 0.033(2) Uani 1 1 d . . . . .
H1 H 0.7812 0.5171 0.4346 0.040 Uiso 1 1 d R U . . .
O2 O 0.4105(13) 0.7178(10) 0.4340(7) 0.030(2) Uani 1 1 d . . . . .
O3 O 0.7143(14) 0.7934(10) 0.5125(8) 0.036(3) Uani 1 1 d . . . . .
O4 O 0.5295(13) 0.5217(10) 0.3405(7) 0.030(2) Uani 1 1 d . . . . .
O5 O 0.6572(11) 0.5513(9) 0.5575(7) 0.024(2) Uani 1 1 d . . . . .
O6 O 0.7711(13) 0.3759(10) 0.4613(8) 0.031(2) Uani 1 1 d . . . . .
O7 O 0.4956(12) 0.2605(14) 0.3593(7) 0.041(3) Uani 1 1 d . . . . .
C1 C 0.886(2) 0.6347(19) 0.3563(15) 0.047(4) Uani 1 1 d . . . . .
H1B H 0.9684 0.5772 0.3624 0.071 Uiso 1 1 calc R U . . .
H1C H 0.9194 0.7240 0.3683 0.071 Uiso 1 1 calc R U . . .
H1D H 0.8223 0.6281 0.2930 0.071 Uiso 1 1 calc R U . . .
C2 C 0.293(2) 0.7727(17) 0.3690(12) 0.041(4) Uani 1 1 d . . . . .
H2A H 0.2047 0.7529 0.3867 0.062 Uiso 1 1 calc R U . . .
H2B H 0.2875 0.7371 0.3069 0.062 Uiso 1 1 calc R U . . .
H2C H 0.3060 0.8666 0.3679 0.062 Uiso 1 1 calc R U . . .
C3 C 0.783(3) 0.9063(19) 0.4984(16) 0.055(5) Uani 1 1 d . . . . .
H3A H 0.8629 0.9238 0.5532 0.083 Uiso 1 1 calc R U . . .
H3B H 0.7145 0.9782 0.4887 0.083 Uiso 1 1 calc R U . . .
H3C H 0.8200 0.8966 0.4432 0.083 Uiso 1 1 calc R U . . .
C4 C 0.527(3) 0.4933(18) 0.2472(11) 0.048(5) Uani 1 1 d . . . . .
H4A H 0.4848 0.4078 0.2306 0.072 Uiso 1 1 calc R U . . .
H4B H 0.6260 0.4937 0.2406 0.072 Uiso 1 1 calc R U . . .
H4C H 0.4703 0.5585 0.2058 0.072 Uiso 1 1 calc R U . . .
C5 C 0.778(2) 0.5634(17) 0.6370(11) 0.039(4) Uani 1 1 d . . . . .
H5A H 0.8665 0.5463 0.6185 0.059 Uiso 1 1 calc R U . . .
H5B H 0.7688 0.5010 0.6849 0.059 Uiso 1 1 calc R U . . .
H5C H 0.7808 0.6511 0.6623 0.059 Uiso 1 1 calc R U . . .
C6 C 0.826(2) 0.2670(18) 0.4192(14) 0.049(5) Uani 1 1 d . . . . .
H6A H 0.9311 0.2686 0.4376 0.073 Uiso 1 1 calc R U . . .
H6B H 0.7912 0.2725 0.3511 0.073 Uiso 1 1 calc R U . . .
H6C H 0.7920 0.1862 0.4407 0.073 Uiso 1 1 calc R U . . .
C7 C 0.480(3) 0.1434(19) 0.3715(15) 0.053(5) Uani 1 1 d . . . . .
H7A H 0.5268 0.0938 0.3313 0.080 Uiso 1 1 calc R U . . .
H7B H 0.3777 0.1224 0.3558 0.080 Uiso 1 1 calc R U . . .
H7C H 0.5245 0.1215 0.4370 0.080 Uiso 1 1 calc R U . . .


_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 O3 1.892(11) . ?
Mo1 O2 1.999(12) . ?
Mo1 O4 2.025(10) . ?
Mo1 O1 2.073(12) . ?
Mo1 O5 2.120(10) . ?
Mo1 Cl1 2.418(4) . ?
Mo1 Mo2 2.6792(17) 3_666 ?
Mo1 Mo2 2.7194(16) . ?
Mo2 O2 2.038(10) 3_666 ?
Mo2 O4 2.048(11) . ?
Mo2 O6 2.060(12) . ?
Mo2 O5 2.078(11) 3_666 ?
Mo2 O7 2.095(14) . ?
Mo2 O5 2.129(9) . ?
Mo2 Mo1 2.6792(17) 3_666 ?
Mo2 Mo2 2.681(2) 3_666 ?
O1 C1 1.45(2) . ?
O1 H1 0.9000 . ?
O2 C2 1.40(2) . ?
O2 Mo2 2.038(10) 3_666 ?
O3 C3 1.39(2) . ?
O4 C4 1.409(18) . ?
O5 C5 1.429(19) . ?
O5 Mo2 2.078(11) 3_666 ?
O6 C6 1.45(2) . ?
O7 C7 1.24(2) . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 H1D 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Mo1 O2 99.0(5) . . ?
O3 Mo1 O4 169.5(5) . . ?
O2 Mo1 O4 90.7(4) . . ?
O3 Mo1 O1 85.7(5) . . ?
O2 Mo1 O1 175.0(4) . . ?
O4 Mo1 O1 84.4(5) . . ?
O3 Mo1 O5 83.9(4) . . ?
O2 Mo1 O5 98.2(4) . . ?
O4 Mo1 O5 98.7(4) . . ?
O1 Mo1 O5 83.6(4) . . ?
O3 Mo1 Cl1 90.3(3) . . ?
O2 Mo1 Cl1 85.9(3) . . ?
O4 Mo1 Cl1 86.4(3) . . ?
O1 Mo1 Cl1 92.8(3) . . ?
O5 Mo1 Cl1 173.4(3) . . ?
O3 Mo1 Mo2 97.9(3) . 3_666 ?
O2 Mo1 Mo2 49.1(3) . 3_666 ?
O4 Mo1 Mo2 91.5(3) . 3_666 ?
O1 Mo1 Mo2 131.9(3) . 3_666 ?
O5 Mo1 Mo2 49.6(3) . 3_666 ?
Cl1 Mo1 Mo2 134.88(11) . 3_666 ?
O3 Mo1 Mo2 133.9(3) . . ?
O2 Mo1 Mo2 93.9(3) . . ?
O4 Mo1 Mo2 48.5(3) . . ?
O1 Mo1 Mo2 83.7(3) . . ?
O5 Mo1 Mo2 50.3(2) . . ?
Cl1 Mo1 Mo2 134.84(11) . . ?
Mo2 Mo1 Mo2 59.54(5) 3_666 . ?
O2 Mo2 O4 174.5(4) 3_666 . ?
O2 Mo2 O6 86.2(4) 3_666 . ?
O4 Mo2 O6 92.0(4) . . ?
O2 Mo2 O5 98.3(4) 3_666 3_666 ?
O4 Mo2 O5 83.4(4) . 3_666 ?
O6 Mo2 O5 175.3(4) . 3_666 ?
O2 Mo2 O7 91.8(4) 3_666 . ?
O4 Mo2 O7 83.1(4) . . ?
O6 Mo2 O7 90.2(4) . . ?
O5 Mo2 O7 88.3(4) 3_666 . ?
O2 Mo2 O5 87.1(4) 3_666 . ?
O4 Mo2 O5 97.7(4) . . ?
O6 Mo2 O5 80.7(4) . . ?
O5 Mo2 O5 100.8(4) 3_666 . ?
O7 Mo2 O5 170.9(4) . . ?
O2 Mo2 Mo1 47.8(3) 3_666 3_666 ?
O4 Mo2 Mo1 134.4(3) . 3_666 ?
O6 Mo2 Mo1 133.6(3) . 3_666 ?
O5 Mo2 Mo1 51.0(3) 3_666 3_666 ?
O7 Mo2 Mo1 95.8(3) . 3_666 ?
O5 Mo2 Mo1 90.2(3) . 3_666 ?
O2 Mo2 Mo2 94.1(3) 3_666 3_666 ?
O4 Mo2 Mo2 91.0(3) . 3_666 ?
O6 Mo2 Mo2 130.1(3) . 3_666 ?
O5 Mo2 Mo2 51.3(2) 3_666 3_666 ?
O7 Mo2 Mo2 139.5(3) . 3_666 ?
O5 Mo2 Mo2 49.6(3) . 3_666 ?
Mo1 Mo2 Mo2 60.97(5) 3_666 3_666 ?
O2 Mo2 Mo1 137.1(3) 3_666 . ?
O4 Mo2 Mo1 47.8(3) . . ?
O6 Mo2 Mo1 87.4(3) . . ?
O5 Mo2 Mo1 90.2(3) 3_666 . ?
O7 Mo2 Mo1 130.6(3) . . ?
O5 Mo2 Mo1 50.1(3) . . ?
Mo1 Mo2 Mo1 120.46(5) 3_666 . ?
Mo2 Mo2 Mo1 59.48(5) 3_666 . ?
C1 O1 Mo1 128.3(10) . . ?
C1 O1 H1 126.7 . . ?
Mo1 O1 H1 88.8 . . ?
C2 O2 Mo1 135.5(10) . . ?
C2 O2 Mo2 136.9(10) . 3_666 ?
Mo1 O2 Mo2 83.2(4) . 3_666 ?
C3 O3 Mo1 134.8(12) . . ?
C4 O4 Mo1 136.6(11) . . ?
C4 O4 Mo2 132.5(10) . . ?
Mo1 O4 Mo2 83.8(4) . . ?
C5 O5 Mo2 130.3(10) . 3_666 ?
C5 O5 Mo1 127.8(10) . . ?
Mo2 O5 Mo1 79.3(4) 3_666 . ?
C5 O5 Mo2 138.9(9) . . ?
Mo2 O5 Mo2 79.2(4) 3_666 . ?
Mo1 O5 Mo2 79.6(3) . . ?
C6 O6 Mo2 125.9(12) . . ?
C7 O7 Mo2 129.8(12) . . ?
O1 C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C1 H1D 109.5 . . ?
H1B C1 H1D 109.5 . . ?
H1C C1 H1D 109.5 . . ?
O2 C2 H2A 109.5 . . ?
O2 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
O2 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O3 C3 H3A 109.5 . . ?
O3 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
O3 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O4 C4 H4A 109.5 . . ?
O4 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
O4 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O5 C5 H5A 109.5 . . ?
O5 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
O5 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O6 C6 H6A 109.5 . . ?
O6 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
O6 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O7 C7 H7A 109.5 . . ?
O7 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
O7 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Mo1 O3 C3 -102.3(19) . . . . ?
O4 Mo1 O3 C3 55(4) . . . . ?
O1 Mo1 O3 C3 76.3(19) . . . . ?
O5 Mo1 O3 C3 160(2) . . . . ?
Cl1 Mo1 O3 C3 -16.4(19) . . . . ?
Mo2 Mo1 O3 C3 -151.9(19) 3_666 . . . ?
Mo2 Mo1 O3 C3 153.4(17) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 O6 0.90 1.52 2.411(15) 168 .

_refine_diff_density_max         1.414
_refine_diff_density_min         -1.477
_refine_diff_density_rms         0.303

####################################################################### 
# 
# 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_dk150622
_database_code_depnum_ccdc_archive 'CCDC 1496102'
_audit_update_record             
;
2016-07-26 deposited with the CCDC.
2016-09-08 downloaded from the CCDC.
;

_publ_contact_name               'Fedyanin, Ivan V.'
_publ_contact_email              octy@xrlab.ineos.ac.ru

_audit_creation_method           'Modified SHELXL output'
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H38 Cl4 Mo6 O18'
_chemical_formula_sum            'C12 H38 Cl4 Mo6 O18'
_chemical_formula_weight         1187.86

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   12.0042(6)
_cell_length_b                   9.5495(5)
_cell_length_c                   14.9585(8)
_cell_angle_alpha                90
_cell_angle_beta                 103.0060(10)
_cell_angle_gamma                90
_cell_volume                     1670.76(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9892
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      30.49

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.361
_exptl_crystal_F_000             1148
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.220
_exptl_absorpt_coefficient_mu    2.569
_shelx_estimated_absorpt_T_min   0.458
_shelx_estimated_absorpt_T_max   0.602
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.118
_exptl_absorpt_correction_T_max  0.172
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker SMART APEX II diffractometer'
_diffrn_detector_type            'Bruker APEX II CCD area detector'
_diffrn_measurement_method       'ο scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28885
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.972
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4869
_reflns_number_gt                4346
_reflns_threshold_expression     'I > 2σ(I)'

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0250P)²+5.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4869
_refine_ls_number_parameters     191
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0263
_refine_ls_wR_factor_ref         0.0681
_refine_ls_wR_factor_gt          0.0658
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.002
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.51119(2) 0.59535(2) 0.56197(2) 0.01095(6) Uani 1 1 d . . . . .
Mo2 Mo 0.30625(2) 0.49823(3) 0.49036(2) 0.01348(6) Uani 1 1 d . . . . .
Mo3 Mo 0.41771(2) 0.38325(3) 0.71058(2) 0.01921(7) Uani 1 1 d . . . . .
Cl1 Cl 0.58485(7) 0.83266(8) 0.59893(5) 0.02133(15) Uani 1 1 d . . . . .
Cl2 Cl 0.12237(7) 0.59267(10) 0.41838(6) 0.02942(18) Uani 1 1 d . . . . .
O1 O 0.45076(17) 0.3950(2) 0.56594(13) 0.0127(4) Uani 1 1 d . . . . .
O2 O 0.66503(18) 0.5213(2) 0.63414(14) 0.0176(4) Uani 1 1 d . . . . .
O3 O 0.36143(18) 0.6930(2) 0.50591(14) 0.0155(4) Uani 1 1 d . . . . .
O4 O 0.46873(19) 0.5882(2) 0.69074(14) 0.0173(4) Uani 1 1 d . . . . .
O5 O 0.2268(2) 0.2972(3) 0.46278(18) 0.0240(5) Uani 1 1 d . . . . .
H5 H 0.263(4) 0.245(4) 0.450(3) 0.020(11) Uiso 1 1 d . . . . .
O6 O 0.26667(18) 0.4810(2) 0.60994(15) 0.0171(4) Uani 1 1 d . . . . .
O7 O 0.3417(2) 0.2143(2) 0.67249(17) 0.0252(5) Uani 1 1 d . . . . .
O8 O 0.3635(2) 0.4261(3) 0.80236(17) 0.0293(6) Uani 1 1 d . . . . .
O9 O 0.5514(2) 0.3196(3) 0.75381(17) 0.0283(5) Uani 1 1 d . . . . .
C2 C 0.7329(3) 0.5422(5) 0.7253(2) 0.0293(8) Uani 1 1 d . . . . .
H2A H 0.7768 0.4571 0.7459 0.044 Uiso 1 1 calc R U . . .
H2B H 0.6826 0.5630 0.7670 0.044 Uiso 1 1 calc R U . . .
H2C H 0.7854 0.6207 0.7253 0.044 Uiso 1 1 calc R U . . .
C3 C 0.3325(3) 0.8151(4) 0.4491(3) 0.0289(8) Uani 1 1 d . . . . .
H3A H 0.2515 0.8376 0.4432 0.043 Uiso 1 1 calc R U . . .
H3B H 0.3467 0.7965 0.3882 0.043 Uiso 1 1 calc R U . . .
H3C H 0.3795 0.8943 0.4771 0.043 Uiso 1 1 calc R U . . .
C4 C 0.4234(3) 0.7073(4) 0.7302(2) 0.0255(7) Uani 1 1 d . . . . .
H4A H 0.3975 0.6777 0.7849 0.038 Uiso 1 1 calc R U . . .
H4B H 0.3588 0.7466 0.6852 0.038 Uiso 1 1 calc R U . . .
H4C H 0.4832 0.7786 0.7474 0.038 Uiso 1 1 calc R U . . .
C5 C 0.1250(3) 0.2409(4) 0.4841(3) 0.0319(8) Uani 1 1 d . . . . .
H5A H 0.0919 0.1705 0.4381 0.048 Uiso 1 1 calc R U . . .
H5B H 0.0697 0.3165 0.4837 0.048 Uiso 1 1 calc R U . . .
H5C H 0.1440 0.1974 0.5449 0.048 Uiso 1 1 calc R U . . .
C6 C 0.1658(3) 0.5213(4) 0.6394(3) 0.0285(7) Uani 1 1 d . . . . .
H6A H 0.1091 0.5580 0.5870 0.043 Uiso 1 1 calc R U . . .
H6B H 0.1851 0.5938 0.6867 0.043 Uiso 1 1 calc R U . . .
H6C H 0.1342 0.4396 0.6646 0.043 Uiso 1 1 calc R U . . .
C7 C 0.3923(4) 0.0913(4) 0.6453(3) 0.0330(8) Uani 1 1 d . . . . .
H7A H 0.3369 0.0144 0.6371 0.049 Uiso 1 1 calc R U . . .
H7B H 0.4599 0.0661 0.6927 0.049 Uiso 1 1 calc R U . . .
H7C H 0.4149 0.1089 0.5873 0.049 Uiso 1 1 calc R U . . .


_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 O3 2.031(2) . ?
Mo1 O2 2.044(2) . ?
Mo1 O1 2.052(2) . ?
Mo1 O1 2.067(2) 3_666 ?
Mo1 O4 2.102(2) . ?
Mo1 Cl1 2.4501(8) . ?
Mo1 Mo1 2.5692(5) 3_666 ?
Mo1 Mo2 2.6218(4) . ?
Mo1 Mo2 2.6431(4) 3_666 ?
Mo2 O6 1.958(2) . ?
Mo2 O3 1.971(2) . ?
Mo2 O2 1.978(2) 3_666 ?
Mo2 O1 2.092(2) . ?
Mo2 O5 2.142(2) . ?
Mo2 Cl2 2.4031(8) . ?
Mo2 Mo1 2.6431(4) 3_666 ?
Mo3 O8 1.696(2) . ?
Mo3 O9 1.702(3) . ?
Mo3 O7 1.878(2) . ?
Mo3 O4 2.092(2) . ?
Mo3 O6 2.280(2) . ?
Mo3 O1 2.288(2) . ?
O1 Mo1 2.067(2) 3_666 ?
O2 C2 1.436(4) . ?
O2 Mo2 1.978(2) 3_666 ?
O3 C3 1.439(4) . ?
O4 C4 1.443(4) . ?
O5 C5 1.434(4) . ?
O5 H5 0.72(4) . ?
O6 C6 1.431(4) . ?
O7 C7 1.423(4) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Mo1 O2 170.83(9) . . ?
O3 Mo1 O1 98.88(8) . . ?
O2 Mo1 O1 86.88(9) . . ?
O3 Mo1 O1 87.52(8) . 3_666 ?
O2 Mo1 O1 98.21(8) . 3_666 ?
O1 Mo1 O1 102.81(7) . 3_666 ?
O3 Mo1 O4 91.06(9) . . ?
O2 Mo1 O4 83.19(9) . . ?
O1 Mo1 O4 77.46(8) . . ?
O1 Mo1 O4 178.58(8) 3_666 . ?
O3 Mo1 Cl1 84.80(6) . . ?
O2 Mo1 Cl1 87.90(7) . . ?
O1 Mo1 Cl1 165.46(6) . . ?
O1 Mo1 Cl1 91.36(6) 3_666 . ?
O4 Mo1 Cl1 88.45(6) . . ?
O3 Mo1 Mo1 95.07(6) . 3_666 ?
O2 Mo1 Mo1 94.09(6) . 3_666 ?
O1 Mo1 Mo1 51.66(6) . 3_666 ?
O1 Mo1 Mo1 51.15(6) 3_666 3_666 ?
O4 Mo1 Mo1 129.11(6) . 3_666 ?
Cl1 Mo1 Mo1 142.39(2) . 3_666 ?
O3 Mo1 Mo2 48.07(6) . . ?
O2 Mo1 Mo2 138.30(7) . . ?
O1 Mo1 Mo2 51.44(6) . . ?
O1 Mo1 Mo2 91.15(6) 3_666 . ?
O4 Mo1 Mo2 87.94(6) . . ?
Cl1 Mo1 Mo2 132.62(2) . . ?
Mo1 Mo1 Mo2 61.206(11) 3_666 . ?
O3 Mo1 Mo2 138.48(6) . 3_666 ?
O2 Mo1 Mo2 47.84(6) . 3_666 ?
O1 Mo1 Mo2 90.88(6) . 3_666 ?
O1 Mo1 Mo2 50.97(6) 3_666 3_666 ?
O4 Mo1 Mo2 130.45(6) . 3_666 ?
Cl1 Mo1 Mo2 95.65(2) . 3_666 ?
Mo1 Mo1 Mo2 60.378(11) 3_666 3_666 ?
Mo2 Mo1 Mo2 121.584(11) . 3_666 ?
O6 Mo2 O3 96.63(9) . . ?
O6 Mo2 O2 169.05(10) . 3_666 ?
O3 Mo2 O2 94.31(9) . 3_666 ?
O6 Mo2 O1 78.99(8) . . ?
O3 Mo2 O1 99.51(8) . . ?
O2 Mo2 O1 99.51(8) 3_666 . ?
O6 Mo2 O5 84.94(9) . . ?
O3 Mo2 O5 172.73(9) . . ?
O2 Mo2 O5 84.17(9) 3_666 . ?
O1 Mo2 O5 87.75(9) . . ?
O6 Mo2 Cl2 93.07(7) . . ?
O3 Mo2 Cl2 87.08(7) . . ?
O2 Mo2 Cl2 87.18(7) 3_666 . ?
O1 Mo2 Cl2 170.15(6) . . ?
O5 Mo2 Cl2 85.74(8) . . ?
O6 Mo2 Mo1 93.13(6) . . ?
O3 Mo2 Mo1 50.08(6) . . ?
O2 Mo2 Mo1 94.11(6) 3_666 . ?
O1 Mo2 Mo1 50.08(6) . . ?
O5 Mo2 Mo1 137.05(7) . . ?
Cl2 Mo2 Mo1 137.15(3) . . ?
O6 Mo2 Mo1 129.04(6) . 3_666 ?
O3 Mo2 Mo1 94.30(6) . 3_666 ?
O2 Mo2 Mo1 50.00(6) 3_666 3_666 ?
O1 Mo2 Mo1 50.11(5) . 3_666 ?
O5 Mo2 Mo1 90.16(7) . 3_666 ?
Cl2 Mo2 Mo1 137.17(2) . 3_666 ?
Mo1 Mo2 Mo1 58.415(10) . 3_666 ?
O8 Mo3 O9 106.20(13) . . ?
O8 Mo3 O7 101.77(12) . . ?
O9 Mo3 O7 99.27(12) . . ?
O8 Mo3 O4 93.84(11) . . ?
O9 Mo3 O4 96.13(11) . . ?
O7 Mo3 O4 153.98(10) . . ?
O8 Mo3 O6 92.46(11) . . ?
O9 Mo3 O6 159.90(10) . . ?
O7 Mo3 O6 83.78(10) . . ?
O4 Mo3 O6 74.80(8) . . ?
O8 Mo3 O1 158.92(10) . . ?
O9 Mo3 O1 91.57(10) . . ?
O7 Mo3 O1 86.05(9) . . ?
O4 Mo3 O1 72.64(8) . . ?
O6 Mo3 O1 68.72(7) . . ?
Mo1 O1 Mo1 77.19(7) . 3_666 ?
Mo1 O1 Mo2 78.48(7) . . ?
Mo1 O1 Mo2 78.92(7) 3_666 . ?
Mo1 O1 Mo3 102.16(8) . . ?
Mo1 O1 Mo3 177.28(11) 3_666 . ?
Mo2 O1 Mo3 103.58(8) . . ?
C2 O2 Mo2 136.5(2) . 3_666 ?
C2 O2 Mo1 134.9(2) . . ?
Mo2 O2 Mo1 82.16(8) 3_666 . ?
C3 O3 Mo2 131.7(2) . . ?
C3 O3 Mo1 133.6(2) . . ?
Mo2 O3 Mo1 81.84(8) . . ?
C4 O4 Mo3 122.02(19) . . ?
C4 O4 Mo1 122.73(19) . . ?
Mo3 O4 Mo1 107.43(9) . . ?
C5 O5 Mo2 131.1(2) . . ?
C5 O5 H5 113(3) . . ?
Mo2 O5 H5 114(3) . . ?
C6 O6 Mo2 130.9(2) . . ?
C6 O6 Mo3 120.6(2) . . ?
Mo2 O6 Mo3 108.49(9) . . ?
C7 O7 Mo3 125.9(2) . . ?
O2 C2 H2A 109.5 . . ?
O2 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
O2 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O3 C3 H3A 109.5 . . ?
O3 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
O3 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O4 C4 H4A 109.5 . . ?
O4 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
O4 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O5 C5 H5A 109.5 . . ?
O5 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
O5 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O6 C6 H6A 109.5 . . ?
O6 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
O6 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O7 C7 H7A 109.5 . . ?
O7 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
O7 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O8 Mo3 O7 C7 -136.7(3) . . . . ?
O9 Mo3 O7 C7 -27.8(3) . . . . ?
O4 Mo3 O7 C7 97.7(3) . . . . ?
O6 Mo3 O7 C7 132.1(3) . . . . ?
O1 Mo3 O7 C7 63.1(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5 Cl1 0.72(4) 2.24(4) 2.905(3) 154(4) 3_666

_refine_diff_density_max         0.964
_refine_diff_density_min         -1.401
_refine_diff_density_rms         0.135


