# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1831755'
_audit_update_record             
;
2018-07-04 deposited with the CCDC.
2018-09-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H30 Co3 Mo8 N16 O36'
_chemical_formula_weight         1966.87

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'
N N 0.0061 0.0033 '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'
Co Co 0.3494 0.9721 '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      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                   10.490(3)
_cell_length_b                   11.480(3)
_cell_length_c                   11.803(3)
_cell_angle_alpha                71.177(5)
_cell_angle_beta                 80.960(5)
_cell_angle_gamma                69.147(4)
_cell_volume                     1255.8(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1767
_cell_measurement_theta_min      2.3589
_cell_measurement_theta_max      24.9613

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.601
_exptl_crystal_F_000             923
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    3.002
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5815
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Smart Apex II'
_diffrn_measurement_method       'w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6476
_diffrn_reflns_av_unetI/netI     0.0743
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.825
_diffrn_reflns_theta_max         25.011
_diffrn_reflns_theta_full        25.011
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             4425
_reflns_number_gt                3163
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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 Smart'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0785P)²-2.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4380
_refine_ls_number_parameters     358
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0475
_refine_ls_wR_factor_ref         0.1342
_refine_ls_wR_factor_gt          0.1185
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.007
_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
Co1 Co 1.0000 0.0000 0.5000 0.0334(5) Uani 1 2 d S . P . .
N1 N 1.2027(7) -0.0501(8) 0.4189(6) 0.0249(19) Uani 1 1 d . . . . .
C1 C 1.2082(9) -0.0166(9) 0.3004(8) 0.024(2) Uani 1 1 d . . . . .
Mo1 Mo 0.78867(7) 0.19762(8) -0.03095(7) 0.0174(2) Uani 1 1 d . . . . .
O1W O 1.3177(7) 0.1406(7) 0.0295(6) 0.0322(17) Uani 1 1 d . . . . .
O1 O 0.7645(6) 0.0491(6) 0.0172(5) 0.0221(14) Uani 1 1 d . . . . .
Mo2 Mo 0.49511(8) 0.72553(8) -0.20399(7) 0.0196(2) Uani 1 1 d . . . . .
Co2 Co 1.14454(12) 0.15289(12) -0.04162(11) 0.0193(3) Uani 1 1 d . . . . .
N2 N 0.9669(7) 0.0439(9) 0.3168(7) 0.032(2) Uani 1 1 d . . . . .
C2 C 1.0791(8) 0.0437(9) 0.2426(8) 0.022(2) Uani 1 1 d . . . . .
O2W O 1.0568(7) 0.3564(7) -0.0536(6) 0.0366(18) Uani 1 1 d . . . . .
O2 O 0.9559(6) 0.1680(6) -0.0915(5) 0.0184(13) Uani 1 1 d . . . . .
Mo3 Mo 0.68835(8) 0.45585(8) -0.25443(7) 0.0220(2) Uani 1 1 d . . . . .
O3 O 0.5790(7) 0.4837(7) -0.3576(6) 0.0338(17) Uani 1 1 d . . . . .
C3 C 1.4387(10) 0.1656(10) -0.3410(8) 0.027(2) Uani 1 1 d . . . . .
N3 N 1.0470(7) 0.0995(7) 0.1310(6) 0.0179(16) Uani 1 1 d . . . . .
O3W O 0.9846(8) 0.1967(8) 0.4609(7) 0.049(2) Uani 1 1 d . . . . .
O4W O 0.7286(9) 0.3808(10) 0.4419(8) 0.065(3) Uani 1 1 d . . . . .
Mo4 Mo 0.33994(7) 0.51985(8) -0.03991(7) 0.0176(2) Uani 1 1 d . . . . .
O4 O 0.6223(6) 0.6475(6) -0.0331(5) 0.0211(14) Uani 1 1 d . . . . .
N4 N 1.2341(7) 0.1905(8) -0.2144(7) 0.0266(19) Uani 1 1 d . . . . .
C4 C 1.4122(9) -0.1080(10) 0.3447(8) 0.025(2) Uani 1 1 d . . . . .
O5W O 1.0946(10) 0.3194(11) 0.2364(10) 0.083(3) Uani 1 1 d . . . . .
O5 O 0.5145(6) 0.5165(6) -0.1218(5) 0.0185(13) Uani 1 1 d . . . . .
C5 C 1.3687(9) 0.1460(9) -0.2300(8) 0.026(2) Uani 1 1 d . . . . .
H5A H 1.4197 0.0986 -0.1624 0.031 Uiso 1 1 calc R U . . .
N5 N 0.9092(7) 0.1357(7) 0.1350(6) 0.0202(17) Uani 1 1 d . . . . .
O6 O 0.5144(7) 0.8661(7) -0.2150(6) 0.0363(18) Uani 1 1 d . . . . .
N6 N 1.3351(7) -0.0504(8) 0.2502(6) 0.0214(17) Uani 1 1 d . . . . .
C6 C 1.3643(11) 0.2369(13) -0.4398(10) 0.052(3) Uani 1 1 d . U . . .
H6A H 1.4081 0.2550 -0.5151 0.062 Uiso 1 1 calc R U . . .
O7 O 0.8440(7) 0.4170(7) -0.3237(6) 0.0365(18) Uani 1 1 d . . . . .
C7 C 1.2238(12) 0.2822(17) -0.4278(11) 0.090(6) Uani 1 1 d . . . . .
H7A H 1.1712 0.3287 -0.4945 0.108 Uiso 1 1 calc R U . . .
N7 N 1.3333(8) -0.1083(9) 0.4457(7) 0.036(2) Uani 1 1 d . . . . .
H7B H 1.3626 -0.1411 0.5170 0.044 Uiso 1 1 calc R U . . .
O8 O 0.6858(6) 0.2782(6) -0.1611(6) 0.0252(15) Uani 1 1 d . . . . .
N8 N 0.8608(8) 0.1008(9) 0.2469(7) 0.036(2) Uani 1 1 d . . . . .
C8 C 1.1624(12) 0.2563(13) -0.3122(10) 0.057(4) Uani 1 1 d . U . . .
H8A H 1.0676 0.2863 -0.3034 0.069 Uiso 1 1 calc R U . . .
O9 O 0.6715(6) 0.6293(6) -0.2621(5) 0.0246(15) Uani 1 1 d . . . . .
O10 O 0.4090(6) 0.7539(7) -0.3261(5) 0.0277(15) Uani 1 1 d . . . . .
O11 O 0.2387(7) 0.5478(7) -0.1494(6) 0.0333(17) Uani 1 1 d . . . . .
O12 O 0.3476(6) 0.7160(6) -0.0813(5) 0.0210(14) Uani 1 1 d . . . . .
O13 O 0.2170(6) 0.5927(6) 0.0731(5) 0.0219(14) Uani 1 1 d . . . . .


_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
Co1 O3W 2.104(8) 2_756 ?
Co1 O3W 2.104(8) . ?
Co1 N2 2.111(8) . ?
Co1 N2 2.111(8) 2_756 ?
Co1 N1 2.148(7) 2_756 ?
Co1 N1 2.148(7) . ?
N1 C1 1.323(11) . ?
N1 N7 1.331(10) . ?
C1 N6 1.345(11) . ?
C1 C2 1.448(12) . ?
Mo1 O1 1.713(6) . ?
Mo1 O2 1.744(6) . ?
Mo1 O8 1.810(6) . ?
Mo1 O12 2.007(6) 2_665 ?
Mo1 O13 2.276(6) 2_665 ?
Mo1 N5 2.276(7) . ?
O1W Co2 2.061(6) . ?
O1 Co2 2.109(6) 2_755 ?
Mo2 O6 1.659(7) . ?
Mo2 O10 1.702(6) . ?
Mo2 O9 1.937(6) . ?
Mo2 O12 1.954(6) . ?
Mo2 O5 2.226(6) . ?
Mo2 O4 2.341(6) . ?
Co2 N4 2.084(7) . ?
Co2 O2 2.085(6) . ?
Co2 O1 2.109(6) 2_755 ?
Co2 N3 2.135(7) . ?
Co2 O2W 2.150(7) . ?
N2 N8 1.331(11) . ?
N2 C2 1.352(11) . ?
C2 N3 1.303(11) . ?
Mo3 O3 1.681(7) . ?
Mo3 O7 1.683(6) . ?
Mo3 O9 1.908(7) . ?
Mo3 O8 1.988(7) . ?
Mo3 O5 2.272(6) . ?
Mo3 O13 2.320(6) 2_665 ?
C3 C6 1.361(14) . ?
C3 C5 1.390(12) . ?
C3 C4 1.465(13) 2_855 ?
N3 N5 1.352(10) . ?
Mo4 O11 1.679(7) . ?
Mo4 O4 1.757(6) 2_665 ?
Mo4 O13 1.885(6) . ?
Mo4 O5 1.925(6) . ?
Mo4 O12 2.173(6) . ?
Mo4 O5 2.469(6) 2_665 ?
O4 Mo4 1.757(6) 2_665 ?
N4 C5 1.325(11) . ?
N4 C8 1.333(13) . ?
C4 N6 1.328(12) . ?
C4 N7 1.340(11) . ?
C4 C3 1.465(13) 2_855 ?
O5 Mo4 2.469(6) 2_665 ?
N5 N8 1.325(10) . ?
C6 C7 1.378(15) . ?
C7 C8 1.401(15) . ?
O12 Mo1 2.007(6) 2_665 ?
O13 Mo1 2.276(6) 2_665 ?
O13 Mo3 2.320(6) 2_665 ?

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
O3W Co1 O3W 180.0 2_756 . ?
O3W Co1 N2 94.1(3) 2_756 . ?
O3W Co1 N2 85.9(3) . . ?
O3W Co1 N2 85.9(3) 2_756 2_756 ?
O3W Co1 N2 94.1(3) . 2_756 ?
N2 Co1 N2 180.0 . 2_756 ?
O3W Co1 N1 92.5(3) 2_756 2_756 ?
O3W Co1 N1 87.5(3) . 2_756 ?
N2 Co1 N1 103.6(3) . 2_756 ?
N2 Co1 N1 76.4(3) 2_756 2_756 ?
O3W Co1 N1 87.5(3) 2_756 . ?
O3W Co1 N1 92.5(3) . . ?
N2 Co1 N1 76.4(3) . . ?
N2 Co1 N1 103.6(3) 2_756 . ?
N1 Co1 N1 180.0 2_756 . ?
C1 N1 N7 103.3(7) . . ?
C1 N1 Co1 114.6(6) . . ?
N7 N1 Co1 142.1(6) . . ?
N1 C1 N6 114.4(8) . . ?
N1 C1 C2 116.9(8) . . ?
N6 C1 C2 128.6(8) . . ?
O1 Mo1 O2 105.3(3) . . ?
O1 Mo1 O8 101.6(3) . . ?
O2 Mo1 O8 103.7(3) . . ?
O1 Mo1 O12 98.8(3) . 2_665 ?
O2 Mo1 O12 144.5(3) . 2_665 ?
O8 Mo1 O12 96.3(3) . 2_665 ?
O1 Mo1 O13 168.9(2) . 2_665 ?
O2 Mo1 O13 85.5(2) . 2_665 ?
O8 Mo1 O13 77.8(3) . 2_665 ?
O12 Mo1 O13 70.3(2) 2_665 2_665 ?
O1 Mo1 N5 88.1(3) . . ?
O2 Mo1 N5 78.2(3) . . ?
O8 Mo1 N5 169.0(3) . . ?
O12 Mo1 N5 76.9(2) 2_665 . ?
O13 Mo1 N5 91.6(2) 2_665 . ?
Mo1 O1 Co2 146.0(3) . 2_755 ?
O6 Mo2 O10 105.6(3) . . ?
O6 Mo2 O9 102.7(3) . . ?
O10 Mo2 O9 96.2(3) . . ?
O6 Mo2 O12 103.2(3) . . ?
O10 Mo2 O12 99.0(3) . . ?
O9 Mo2 O12 145.1(3) . . ?
O6 Mo2 O5 156.4(3) . . ?
O10 Mo2 O5 98.1(3) . . ?
O9 Mo2 O5 74.6(2) . . ?
O12 Mo2 O5 72.3(2) . . ?
O6 Mo2 O4 84.3(3) . . ?
O10 Mo2 O4 169.8(3) . . ?
O9 Mo2 O4 78.8(2) . . ?
O12 Mo2 O4 80.9(2) . . ?
O5 Mo2 O4 72.1(2) . . ?
O1W Co2 N4 91.1(3) . . ?
O1W Co2 O2 172.2(2) . . ?
N4 Co2 O2 96.3(3) . . ?
O1W Co2 O1 85.7(3) . 2_755 ?
N4 Co2 O1 90.2(3) . 2_755 ?
O2 Co2 O1 96.4(2) . 2_755 ?
O1W Co2 N3 92.8(3) . . ?
N4 Co2 N3 174.0(3) . . ?
O2 Co2 N3 79.9(2) . . ?
O1 Co2 N3 85.6(3) 2_755 . ?
O1W Co2 O2W 91.1(3) . . ?
N4 Co2 O2W 92.7(3) . . ?
O2 Co2 O2W 86.4(3) . . ?
O1 Co2 O2W 175.7(3) 2_755 . ?
N3 Co2 O2W 91.7(3) . . ?
N8 N2 C2 106.0(7) . . ?
N8 N2 Co1 137.0(6) . . ?
C2 N2 Co1 114.9(6) . . ?
N3 C2 N2 111.6(8) . . ?
N3 C2 C1 133.0(8) . . ?
N2 C2 C1 115.4(8) . . ?
Mo1 O2 Co2 137.4(3) . . ?
O3 Mo3 O7 104.9(3) . . ?
O3 Mo3 O9 101.3(3) . . ?
O7 Mo3 O9 97.7(3) . . ?
O3 Mo3 O8 97.0(3) . . ?
O7 Mo3 O8 99.5(3) . . ?
O9 Mo3 O8 150.7(2) . . ?
O3 Mo3 O5 91.9(3) . . ?
O7 Mo3 O5 162.5(3) . . ?
O9 Mo3 O5 74.0(2) . . ?
O8 Mo3 O5 82.8(2) . . ?
O3 Mo3 O13 162.4(3) . 2_665 ?
O7 Mo3 O13 91.5(3) . 2_665 ?
O9 Mo3 O13 82.5(2) . 2_665 ?
O8 Mo3 O13 73.5(2) . 2_665 ?
O5 Mo3 O13 72.5(2) . 2_665 ?
C6 C3 C5 118.0(9) . . ?
C6 C3 C4 124.0(8) . 2_855 ?
C5 C3 C4 118.1(8) . 2_855 ?
C2 N3 N5 104.5(7) . . ?
C2 N3 Co2 139.2(6) . . ?
N5 N3 Co2 116.3(5) . . ?
O11 Mo4 O4 104.0(3) . 2_665 ?
O11 Mo4 O13 103.1(3) . . ?
O4 Mo4 O13 101.4(3) 2_665 . ?
O11 Mo4 O5 103.9(3) . . ?
O4 Mo4 O5 98.7(3) 2_665 . ?
O13 Mo4 O5 141.0(3) . . ?
O11 Mo4 O12 97.8(3) . . ?
O4 Mo4 O12 158.1(3) 2_665 . ?
O13 Mo4 O12 74.9(2) . . ?
O5 Mo4 O12 74.0(2) . . ?
O11 Mo4 O5 178.7(3) . 2_665 ?
O4 Mo4 O5 77.0(2) 2_665 2_665 ?
O13 Mo4 O5 75.8(2) . 2_665 ?
O5 Mo4 O5 76.7(2) . 2_665 ?
O12 Mo4 O5 81.2(2) . 2_665 ?
Mo4 O4 Mo2 115.3(3) 2_665 . ?
C5 N4 C8 117.3(8) . . ?
C5 N4 Co2 119.5(6) . . ?
C8 N4 Co2 123.3(7) . . ?
N6 C4 N7 110.0(8) . . ?
N6 C4 C3 125.7(8) . 2_855 ?
N7 C4 C3 124.4(8) . 2_855 ?
Mo4 O5 Mo2 104.2(2) . . ?
Mo4 O5 Mo3 153.4(3) . . ?
Mo2 O5 Mo3 91.6(2) . . ?
Mo4 O5 Mo4 103.3(2) . 2_665 ?
Mo2 O5 Mo4 95.4(2) . 2_665 ?
Mo3 O5 Mo4 96.2(2) . 2_665 ?
N4 C5 C3 124.1(9) . . ?
N8 N5 N3 110.5(7) . . ?
N8 N5 Mo1 124.9(6) . . ?
N3 N5 Mo1 122.7(5) . . ?
C4 N6 C1 102.7(7) . . ?
C3 C6 C7 119.8(10) . . ?
C6 C7 C8 118.1(11) . . ?
N1 N7 C4 109.7(8) . . ?
Mo1 O8 Mo3 116.7(3) . . ?
N5 N8 N2 107.3(7) . . ?
N4 C8 C7 122.8(10) . . ?
Mo3 O9 Mo2 113.9(3) . . ?
Mo2 O12 Mo1 147.3(3) . 2_665 ?
Mo2 O12 Mo4 105.2(3) . . ?
Mo1 O12 Mo4 107.2(3) 2_665 . ?
Mo4 O13 Mo1 107.5(3) . 2_665 ?
Mo4 O13 Mo3 113.9(3) . 2_665 ?
Mo1 O13 Mo3 89.4(2) 2_665 2_665 ?

_refine_diff_density_max         1.563
_refine_diff_density_min         -0.970
_refine_diff_density_rms         0.221

####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1831756'
_audit_update_record             
;
2018-07-04 deposited with the CCDC.
2018-09-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H40 Co3 Mo6 N16 O38 Te'
_chemical_formula_weight         1944.67

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'
N N 0.0061 0.0033 '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'
Co Co 0.3494 0.9721 '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'
Te Te -0.5308 1.6751 '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                   10.6300(5)
_cell_length_b                   11.3860(5)
_cell_length_c                   11.4910(5)
_cell_angle_alpha                100.1280(10)
_cell_angle_beta                 105.9920(10)
_cell_angle_gamma                91.2080(10)
_cell_volume                     1312.58(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4357
_cell_measurement_theta_min      2.3562
_cell_measurement_theta_max      25.1281

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.460
_exptl_crystal_F_000             907
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    2.966
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6196
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Smart Apex II'
_diffrn_measurement_method       'w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7667
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_av_R_equivalents  0.0146
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.822
_diffrn_reflns_theta_max         25.131
_diffrn_reflns_theta_full        25.131
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             4698
_reflns_number_gt                4154
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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 Smart'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0542P)²+4.7526P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4680
_refine_ls_number_parameters     364
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0296
_refine_ls_wR_factor_ref         0.0948
_refine_ls_wR_factor_gt          0.0918
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_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
Te1 Te 0.0000 0.0000 0.0000 0.01257(12) Uani 1 2 d S . P . .
Co1 Co 0.39943(6) -0.34338(5) 0.01617(6) 0.01528(15) Uani 1 1 d . . . . .
O1 O 0.3073(3) -0.2448(3) 0.1321(3) 0.0204(7) Uani 1 1 d . . . . .
C1 C 0.4557(5) -0.3972(4) -0.2240(4) 0.0171(9) Uani 1 1 d . . . . .
N1 N 0.4809(4) -0.4380(3) -0.1187(3) 0.0168(8) Uani 1 1 d . . . . .
Mo1 Mo -0.30449(4) -0.07912(4) -0.16373(4) 0.01799(12) Uani 1 1 d . . . . .
O1W O 0.5568(3) -0.2143(3) 0.1014(3) 0.0278(8) Uani 1 1 d . . . . .
Co2 Co 0.5000 -0.5000 -0.5000 0.0219(2) Uani 1 2 d S . P . .
N2 N 0.3488(4) -0.2427(3) -0.1329(4) 0.0180(8) Uani 1 1 d . . . . .
C2 C 0.3841(4) -0.2907(4) -0.2320(4) 0.0163(9) Uani 1 1 d . . . . .
Mo2 Mo -0.13216(4) -0.26950(3) -0.01615(4) 0.02002(12) Uani 1 1 d . . . . .
O2W O 0.2175(3) -0.4361(3) -0.0773(3) 0.0270(8) Uani 1 1 d . . . . .
O2 O 0.1704(3) -0.0618(3) 0.0133(3) 0.0150(6) Uani 1 1 d . . . . .
N3 N 0.4984(4) -0.4696(4) -0.3083(4) 0.0213(9) Uani 1 1 d . . . . .
C3 C 0.2871(5) -0.1404(4) -0.2801(4) 0.0177(9) Uani 1 1 d . . . . .
Mo3 Mo 0.16570(4) -0.18692(3) 0.15705(4) 0.01661(12) Uani 1 1 d . . . . .
O3 O 0.0531(3) -0.2927(3) 0.0141(3) 0.0207(7) Uani 1 1 d . . . . .
O3W O 0.6718(6) -0.3901(5) -0.4571(5) 0.0761(19) Uani 1 1 d . . . . .
N4 N 0.5414(4) -0.5389(3) -0.1384(4) 0.0207(9) Uani 1 1 d . . . . .
C4 C 0.2327(5) -0.0465(4) -0.3481(4) 0.0202(10) Uani 1 1 d . . . . .
O4 O -0.0166(3) -0.0994(3) 0.1153(3) 0.0171(7) Uani 1 1 d . . . . .
O4W O 0.3880(6) -0.3575(5) -0.5334(4) 0.0707(19) Uani 1 1 d . . . . .
C5 C 0.1953(5) 0.0296(4) -0.5314(4) 0.0239(11) Uani 1 1 d . . . . .
H5A H 0.2020 0.0222 -0.6113 0.029 Uiso 1 1 calc R U . . .
N5 N 0.5518(4) -0.5587(4) -0.2514(4) 0.0240(9) Uani 1 1 d . . . . .
O5 O -0.0934(3) -0.1326(3) -0.1246(3) 0.0166(7) Uani 1 1 d . . . . .
O5W O 0.5047(11) -0.1350(13) -0.5913(13) 0.214(7) Uani 1 1 d . . . . .
N6 N 0.3485(4) -0.2308(3) -0.3256(3) 0.0179(8) Uani 1 1 d . . . . .
C6 C 0.2417(6) -0.0538(5) -0.4672(5) 0.0324(13) Uani 1 1 d . . . . .
H6A H 0.2805 -0.1178 -0.5024 0.039 Uiso 1 1 calc R U . . .
O6 O -0.2816(3) -0.1691(3) -0.0341(3) 0.0236(8) Uani 1 1 d . . . . .
O6W O 0.0735(14) -0.4676(9) 0.3409(14) 0.205(6) Uani 1 1 d . . . . .
O7 O -0.3542(4) -0.1904(3) -0.2905(4) 0.0319(9) Uani 1 1 d . . . . .
N7 N 0.2859(4) -0.1462(3) -0.1653(4) 0.0177(8) Uani 1 1 d . . . . .
H7A H 0.2510 -0.0970 -0.1197 0.021 Uiso 1 1 calc R U . . .
C7 C 0.1399(7) 0.1227(6) -0.4867(6) 0.0451(16) Uani 1 1 d . . . . .
H7B H 0.1066 0.1781 -0.5357 0.054 Uiso 1 1 calc R U . . .
O7W O 0.0037(6) -0.2711(6) -0.3106(5) 0.0752(17) Uani 1 1 d . . . . .
O8 O -0.1623(4) -0.3248(3) 0.1044(4) 0.0317(9) Uani 1 1 d . . . . .
C8 C 0.1775(6) 0.0508(5) -0.2977(6) 0.0366(14) Uani 1 1 d . . . . .
H8A H 0.1711 0.0581 -0.2177 0.044 Uiso 1 1 calc R U . . .
N8 N 0.1311(7) 0.1384(6) -0.3663(7) 0.070(2) Uani 1 1 d . . . . .
O9 O -0.1880(4) -0.3777(3) -0.1432(4) 0.0356(9) Uani 1 1 d . . . . .
O10 O 0.1380(4) -0.2449(3) 0.2757(4) 0.0308(9) Uani 1 1 d . . . . .
O11 O -0.2386(3) 0.0315(3) -0.2511(3) 0.0193(7) Uani 1 1 d . . . . .
O12 O -0.4412(3) -0.0090(3) -0.1474(4) 0.0278(8) Uani 1 1 d . . . . .


_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
Te1 O5 1.926(3) . ?
Te1 O5 1.926(3) 2 ?
Te1 O4 1.927(3) 2 ?
Te1 O4 1.927(3) . ?
Te1 O2 1.933(3) . ?
Te1 O2 1.933(3) 2 ?
Co1 O1 2.058(3) . ?
Co1 N4 2.092(4) 2_645 ?
Co1 O2W 2.093(4) . ?
Co1 O1W 2.099(4) . ?
Co1 N1 2.122(4) . ?
Co1 N2 2.178(4) . ?
O1 Mo3 1.730(3) . ?
C1 N1 1.333(6) . ?
C1 N3 1.342(6) . ?
C1 C2 1.448(6) . ?
N1 N4 1.344(5) . ?
Mo1 O7 1.704(4) . ?
Mo1 O12 1.712(3) . ?
Mo1 O6 1.917(3) . ?
Mo1 O11 1.970(3) . ?
Mo1 O2 2.272(3) 2 ?
Mo1 O5 2.282(3) . ?
Co2 O4W 2.060(4) 2_644 ?
Co2 O4W 2.060(4) . ?
Co2 O3W 2.082(5) 2_644 ?
Co2 O3W 2.082(5) . ?
Co2 N3 2.174(4) . ?
Co2 N3 2.174(4) 2_644 ?
N2 C2 1.328(6) . ?
N2 N7 1.353(5) . ?
C2 N6 1.345(6) . ?
Mo2 O9 1.691(4) . ?
Mo2 O8 1.720(4) . ?
Mo2 O3 1.936(3) . ?
Mo2 O6 1.963(3) . ?
Mo2 O5 2.257(3) . ?
Mo2 O4 2.322(3) . ?
O2 Mo1 2.272(3) 2 ?
O2 Mo3 2.373(3) . ?
N3 N5 1.354(5) . ?
C3 N6 1.336(6) . ?
C3 N7 1.337(6) . ?
C3 C4 1.469(6) . ?
Mo3 O10 1.706(3) . ?
Mo3 O11 1.926(3) 2 ?
Mo3 O3 1.934(3) . ?
Mo3 O4 2.172(3) . ?
N4 N5 1.313(5) . ?
N4 Co1 2.092(4) 2_645 ?
C4 C8 1.378(7) . ?
C4 C6 1.386(7) . ?
C5 C7 1.317(8) . ?
C5 C6 1.325(7) . ?
C7 N8 1.393(9) . ?
C8 N8 1.394(8) . ?
O11 Mo3 1.926(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
O5 Te1 O5 180.0 . 2 ?
O5 Te1 O4 94.88(14) . 2 ?
O5 Te1 O4 85.12(14) 2 2 ?
O5 Te1 O4 85.12(14) . . ?
O5 Te1 O4 94.88(14) 2 . ?
O4 Te1 O4 180.0 2 . ?
O5 Te1 O2 94.52(13) . . ?
O5 Te1 O2 85.48(13) 2 . ?
O4 Te1 O2 94.02(13) 2 . ?
O4 Te1 O2 85.98(13) . . ?
O5 Te1 O2 85.48(13) . 2 ?
O5 Te1 O2 94.51(13) 2 2 ?
O4 Te1 O2 85.98(13) 2 2 ?
O4 Te1 O2 94.02(13) . 2 ?
O2 Te1 O2 180.0 . 2 ?
O1 Co1 N4 91.42(14) . 2_645 ?
O1 Co1 O2W 87.58(13) . . ?
N4 Co1 O2W 95.35(15) 2_645 . ?
O1 Co1 O1W 84.44(13) . . ?
N4 Co1 O1W 96.08(15) 2_645 . ?
O2W Co1 O1W 166.21(14) . . ?
O1 Co1 N1 173.97(14) . . ?
N4 Co1 N1 94.08(14) 2_645 . ?
O2W Co1 N1 89.46(15) . . ?
O1W Co1 N1 97.41(14) . . ?
O1 Co1 N2 98.04(13) . . ?
N4 Co1 N2 170.37(15) 2_645 . ?
O2W Co1 N2 83.30(15) . . ?
O1W Co1 N2 86.69(15) . . ?
N1 Co1 N2 76.39(14) . . ?
Mo3 O1 Co1 149.4(2) . . ?
N1 C1 N3 111.1(4) . . ?
N1 C1 C2 117.7(4) . . ?
N3 C1 C2 131.1(4) . . ?
C1 N1 N4 105.3(4) . . ?
C1 N1 Co1 115.1(3) . . ?
N4 N1 Co1 139.1(3) . . ?
O7 Mo1 O12 107.06(18) . . ?
O7 Mo1 O6 100.98(17) . . ?
O12 Mo1 O6 99.06(16) . . ?
O7 Mo1 O11 94.05(16) . . ?
O12 Mo1 O11 98.75(16) . . ?
O6 Mo1 O11 152.12(14) . . ?
O7 Mo1 O2 159.50(15) . 2 ?
O12 Mo1 O2 91.75(15) . 2 ?
O6 Mo1 O2 83.53(14) . 2 ?
O11 Mo1 O2 74.66(12) . 2 ?
O7 Mo1 O5 91.56(15) . . ?
O12 Mo1 O5 161.22(15) . . ?
O6 Mo1 O5 74.38(12) . . ?
O11 Mo1 O5 81.93(13) . . ?
O2 Mo1 O5 70.22(11) 2 . ?
O4W Co2 O4W 180.00(16) 2_644 . ?
O4W Co2 O3W 90.9(3) 2_644 2_644 ?
O4W Co2 O3W 89.1(3) . 2_644 ?
O4W Co2 O3W 89.1(3) 2_644 . ?
O4W Co2 O3W 90.9(3) . . ?
O3W Co2 O3W 180.0 2_644 . ?
O4W Co2 N3 88.23(16) 2_644 . ?
O4W Co2 N3 91.77(16) . . ?
O3W Co2 N3 88.16(19) 2_644 . ?
O3W Co2 N3 91.84(19) . . ?
O4W Co2 N3 91.77(16) 2_644 2_644 ?
O4W Co2 N3 88.23(16) . 2_644 ?
O3W Co2 N3 91.84(19) 2_644 2_644 ?
O3W Co2 N3 88.16(19) . 2_644 ?
N3 Co2 N3 180.0 . 2_644 ?
C2 N2 N7 103.9(4) . . ?
C2 N2 Co1 114.1(3) . . ?
N7 N2 Co1 141.9(3) . . ?
N2 C2 N6 114.0(4) . . ?
N2 C2 C1 116.5(4) . . ?
N6 C2 C1 129.6(4) . . ?
O9 Mo2 O8 106.72(19) . . ?
O9 Mo2 O3 97.84(17) . . ?
O8 Mo2 O3 99.97(16) . . ?
O9 Mo2 O6 100.69(17) . . ?
O8 Mo2 O6 93.77(16) . . ?
O3 Mo2 O6 152.65(14) . . ?
O9 Mo2 O5 93.34(17) . . ?
O8 Mo2 O5 158.35(15) . . ?
O3 Mo2 O5 84.91(13) . . ?
O6 Mo2 O5 74.13(12) . . ?
O9 Mo2 O4 160.35(16) . . ?
O8 Mo2 O4 91.90(16) . . ?
O3 Mo2 O4 72.19(12) . . ?
O6 Mo2 O4 83.90(13) . . ?
O5 Mo2 O4 69.35(11) . . ?
Te1 O2 Mo1 102.18(13) . 2 ?
Te1 O2 Mo3 98.01(12) . . ?
Mo1 O2 Mo3 91.24(11) 2 . ?
C1 N3 N5 105.0(4) . . ?
C1 N3 Co2 143.1(3) . . ?
N5 N3 Co2 111.7(3) . . ?
N6 C3 N7 110.8(4) . . ?
N6 C3 C4 123.5(4) . . ?
N7 C3 C4 125.7(4) . . ?
O10 Mo3 O1 106.66(17) . . ?
O10 Mo3 O11 97.07(16) . 2 ?
O1 Mo3 O11 99.09(15) . 2 ?
O10 Mo3 O3 102.27(17) . . ?
O1 Mo3 O3 93.08(15) . . ?
O11 Mo3 O3 153.14(14) 2 . ?
O10 Mo3 O4 95.71(15) . . ?
O1 Mo3 O4 156.77(14) . . ?
O11 Mo3 O4 83.98(13) 2 . ?
O3 Mo3 O4 75.76(13) . . ?
O10 Mo3 O2 163.58(14) . . ?
O1 Mo3 O2 88.13(13) . . ?
O11 Mo3 O2 73.05(12) 2 . ?
O3 Mo3 O2 83.58(13) . . ?
O4 Mo3 O2 70.62(11) . . ?
Mo3 O3 Mo2 114.68(16) . . ?
N5 N4 N1 109.7(4) . . ?
N5 N4 Co1 123.4(3) . 2_645 ?
N1 N4 Co1 126.7(3) . 2_645 ?
C8 C4 C6 118.3(5) . . ?
C8 C4 C3 123.2(4) . . ?
C6 C4 C3 118.5(4) . . ?
Te1 O4 Mo3 105.38(13) . . ?
Te1 O4 Mo2 101.58(14) . . ?
Mo3 O4 Mo2 92.89(11) . . ?
C7 C5 C6 122.7(5) . . ?
N4 N5 N3 108.9(4) . . ?
Te1 O5 Mo2 103.95(14) . . ?
Te1 O5 Mo1 102.08(13) . . ?
Mo2 O5 Mo1 92.10(11) . . ?
C3 N6 C2 102.8(4) . . ?
C5 C6 C4 120.5(5) . . ?
Mo1 O6 Mo2 114.73(16) . . ?
C3 N7 N2 108.5(4) . . ?
C5 C7 N8 120.3(5) . . ?
C4 C8 N8 120.2(5) . . ?
C7 N8 C8 118.0(6) . . ?
Mo3 O11 Mo1 116.96(16) 2 . ?

_refine_diff_density_max         1.717
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.169

####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1831757'
_audit_update_record             
;
2018-07-04 deposited with the CCDC.
2018-09-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H32 Co3 Mo8 N14 O36'
_chemical_formula_weight         1964.88

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'
N N 0.0061 0.0033 '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'
Co Co 0.3494 0.9721 '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      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                   10.6530(17)
_cell_length_b                   11.3800(18)
_cell_length_c                   12.165(2)
_cell_angle_alpha                93.925(4)
_cell_angle_beta                 114.034(3)
_cell_angle_gamma                96.044(3)
_cell_volume                     1329.3(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    900
_cell_measurement_theta_min      2.5778
_cell_measurement_theta_max      21.5335

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.454
_exptl_crystal_F_000             923
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    2.835
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6651
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Smart Apex II'
_diffrn_measurement_method       'w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7800
_diffrn_reflns_av_unetI/netI     0.1021
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.813
_diffrn_reflns_theta_max         25.135
_diffrn_reflns_theta_full        25.135
_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             4764
_reflns_number_gt                3143
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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 Smart'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0856P)²+9.6561P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4754
_refine_ls_number_parameters     358
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0605
_refine_ls_wR_factor_ref         0.1813
_refine_ls_wR_factor_gt          0.1570
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_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 0.00465(11) -0.03885(9) 0.81030(10) 0.0162(3) Uani 1 1 d . . . . .
Co1 Co 0.0000 -0.5000 1.0000 0.0312(7) Uani 1 2 d S . P . .
O1 O -0.1553(9) -0.0589(8) 0.8142(8) 0.025(2) Uani 1 1 d . . . . .
O1W O 0.0933(14) -0.4130(10) 0.8940(12) 0.064(4) Uani 1 1 d . . . . .
N1 N -0.0388(11) -0.3325(10) 1.0501(10) 0.031(3) Uani 1 1 d . . . . .
C1 C 0.0194(13) -0.2368(10) 1.1302(12) 0.024(3) Uani 1 1 d . . . . .
H1A H 0.1041 -0.2313 1.1972 0.029 Uiso 1 1 calc R U . . .
Mo2 Mo 0.16339(12) -0.19598(10) 0.68836(10) 0.0216(3) Uani 1 1 d . . . . .
Co2 Co -0.28728(17) -0.05977(15) 0.90690(16) 0.0204(4) Uani 1 1 d . . . . .
O2W O -0.3781(12) 0.0761(10) 0.8110(10) 0.050(3) Uani 1 1 d . . . . .
N2 N -0.1954(12) -0.4920(11) 0.8646(12) 0.039(3) Uani 1 1 d . . . . .
C2 C -0.1576(13) -0.2993(11) 0.9717(12) 0.024(3) Uani 1 1 d . . . . .
O2 O -0.1249(9) 0.0558(7) 1.0455(8) 0.0213(19) Uani 1 1 d . . . . .
Mo3 Mo 0.21796(12) -0.11038(11) 0.46126(11) 0.0253(3) Uani 1 1 d . . . . .
O3 O -0.0045(9) -0.1831(7) 0.7208(7) 0.0215(19) Uani 1 1 d . . . . .
N3 N -0.1732(10) -0.1911(9) 0.9985(9) 0.018(2) Uani 1 1 d . . . . .
C3 C -0.2499(13) -0.3908(11) 0.8682(12) 0.026(3) Uani 1 1 d . . . . .
O3W O -0.3913(9) -0.0625(8) 1.0229(8) 0.029(2) Uani 1 1 d . . . . .
Mo4 Mo 0.11640(11) 0.09493(10) 0.62256(10) 0.0179(3) Uani 1 1 d . . . . .
N4 N -0.0575(10) -0.1490(9) 1.1038(9) 0.016(2) Uani 1 1 d . . . . .
O4W O -0.4377(9) -0.1724(8) 0.7668(9) 0.034(2) Uani 1 1 d . . . . .
O4 O -0.0619(8) 0.0505(8) 0.6636(8) 0.0216(19) Uani 1 1 d . . . . .
C4 C -0.3989(14) -0.5041(13) 0.7230(13) 0.033(3) Uani 1 1 d . . . . .
O5 O 0.0423(8) -0.1076(7) 0.5236(7) 0.0173(18) Uani 1 1 d . . . . .
N5 N -0.3767(11) -0.3941(9) 0.7826(11) 0.031(3) Uani 1 1 d . . . . .
H5A H -0.4306 -0.3405 0.7686 0.037 Uiso 1 1 calc R U . . .
C5 C -0.5282(16) -0.5599(13) 0.6189(14) 0.040(4) Uani 1 1 d . . . . .
O5W O -0.563(4) -0.265(2) 1.070(2) 0.29(2) Uani 1 1 d . . . . .
O6 O 0.2975(9) -0.1391(8) 0.6302(8) 0.026(2) Uani 1 1 d . . . . .
N6 N -0.2943(12) -0.5675(11) 0.7701(12) 0.043(3) Uani 1 1 d . . . . .
C6 C -0.6438(17) -0.5010(17) 0.5756(16) 0.057(5) Uani 1 1 d . . . . .
H6A H -0.6382 -0.4237 0.6094 0.069 Uiso 1 1 calc R U . . .
O7 O 0.1642(10) 0.2355(8) 0.6945(9) 0.032(2) Uani 1 1 d . . . . .
N7 N -0.7698(15) -0.6623(15) 0.4295(13) 0.056(4) Uani 1 1 d . . . . .
C7 C -0.7634(19) -0.5548(19) 0.485(2) 0.077(7) Uani 1 1 d . . . . .
H7A H -0.8421 -0.5172 0.4613 0.092 Uiso 1 1 calc R U . . .
O8 O 0.0985(11) -0.3341(8) 0.6080(9) 0.035(2) Uani 1 1 d . . . . .
C8 C -0.6609(19) -0.7184(15) 0.4668(14) 0.048(5) Uani 1 1 d . . . . .
H8A H -0.6681 -0.7935 0.4276 0.057 Uiso 1 1 calc R U . . .
O9 O 0.1777(8) -0.0001(7) 0.7534(7) 0.0170(18) Uani 1 1 d . . . . .
C9 C -0.5356(18) -0.6703(14) 0.5620(15) 0.046(4) Uani 1 1 d . . . . .
H9A H -0.4596 -0.7114 0.5863 0.055 Uiso 1 1 calc R U . . .
O10 O 0.2364(9) 0.0762(8) 0.5619(8) 0.025(2) Uani 1 1 d . . . . .
O11 O 0.1781(13) -0.2543(10) 0.4013(9) 0.052(3) Uani 1 1 d . . . . .
O12 O 0.2759(10) -0.2203(9) 0.8296(9) 0.036(3) Uani 1 1 d . . . . .
O13 O 0.3515(10) -0.0573(11) 0.4294(10) 0.051(3) Uani 1 1 d . . . . .


_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 O1 1.716(8) . ?
Mo1 O2 1.738(8) 2_557 ?
Mo1 O3 1.878(8) . ?
Mo1 O4 2.022(8) . ?
Mo1 N4 2.223(10) 2_557 ?
Mo1 O9 2.232(8) . ?
Co1 N2 2.078(12) . ?
Co1 N2 2.078(12) 2_547 ?
Co1 N1 2.095(11) . ?
Co1 N1 2.095(11) 2_547 ?
Co1 O1W 2.154(12) . ?
Co1 O1W 2.154(12) 2_547 ?
O1 Co2 2.130(9) . ?
N1 C1 1.319(16) . ?
N1 C2 1.349(15) . ?
C1 N4 1.331(15) . ?
Mo2 O8 1.707(9) . ?
Mo2 O12 1.709(9) . ?
Mo2 O6 1.911(9) . ?
Mo2 O3 2.000(9) . ?
Mo2 O5 2.266(8) . ?
Mo2 O9 2.282(8) . ?
Co2 O4W 2.040(9) . ?
Co2 O2W 2.080(10) . ?
Co2 O2 2.099(9) . ?
Co2 N3 2.112(10) . ?
Co2 O3W 2.119(9) . ?
N2 C3 1.350(17) . ?
N2 N6 1.363(16) . ?
C2 N3 1.297(16) . ?
C2 C3 1.495(18) . ?
O2 Mo1 1.738(8) 2_557 ?
Mo3 O11 1.683(11) . ?
Mo3 O13 1.685(10) . ?
Mo3 O6 1.944(9) . ?
Mo3 O4 1.964(8) 2_556 ?
Mo3 O5 2.289(8) . ?
Mo3 O10 2.325(9) . ?
N3 N4 1.377(13) . ?
C3 N5 1.322(16) . ?
Mo4 O7 1.691(9) . ?
Mo4 O10 1.740(9) . ?
Mo4 O9 1.915(8) . ?
Mo4 O5 1.918(8) 2_556 ?
Mo4 O4 2.173(8) . ?
Mo4 O5 2.418(8) . ?
N4 Mo1 2.223(10) 2_557 ?
O4 Mo3 1.964(8) 2_556 ?
C4 N6 1.341(18) . ?
C4 N5 1.349(18) . ?
C4 C5 1.480(19) . ?
O5 Mo4 1.918(8) 2_556 ?
C5 C9 1.37(2) . ?
C5 C6 1.39(2) . ?
C6 C7 1.35(2) . ?
N7 C8 1.31(2) . ?
N7 C7 1.34(2) . ?
C8 C9 1.39(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 Mo1 O2 106.4(4) . 2_557 ?
O1 Mo1 O3 100.2(4) . . ?
O2 Mo1 O3 102.0(4) 2_557 . ?
O1 Mo1 O4 93.3(4) . . ?
O2 Mo1 O4 151.6(4) 2_557 . ?
O3 Mo1 O4 94.2(4) . . ?
O1 Mo1 N4 94.1(4) . 2_557 ?
O2 Mo1 N4 80.0(4) 2_557 2_557 ?
O3 Mo1 N4 164.2(4) . 2_557 ?
O4 Mo1 N4 78.3(3) . 2_557 ?
O1 Mo1 O9 163.9(4) . . ?
O2 Mo1 O9 89.7(3) 2_557 . ?
O3 Mo1 O9 77.4(3) . . ?
O4 Mo1 O9 71.2(3) . . ?
N4 Mo1 O9 87.0(3) 2_557 . ?
N2 Co1 N2 180.0 . 2_547 ?
N2 Co1 N1 78.0(4) . . ?
N2 Co1 N1 102.0(4) 2_547 . ?
N2 Co1 N1 102.0(4) . 2_547 ?
N2 Co1 N1 78.0(4) 2_547 2_547 ?
N1 Co1 N1 180.0 . 2_547 ?
N2 Co1 O1W 89.4(5) . . ?
N2 Co1 O1W 90.6(5) 2_547 . ?
N1 Co1 O1W 87.5(5) . . ?
N1 Co1 O1W 92.5(5) 2_547 . ?
N2 Co1 O1W 90.6(5) . 2_547 ?
N2 Co1 O1W 89.4(5) 2_547 2_547 ?
N1 Co1 O1W 92.5(5) . 2_547 ?
N1 Co1 O1W 87.5(5) 2_547 2_547 ?
O1W Co1 O1W 180.0 . 2_547 ?
Mo1 O1 Co2 152.5(5) . . ?
C1 N1 C2 102.8(11) . . ?
C1 N1 Co1 141.9(9) . . ?
C2 N1 Co1 115.0(9) . . ?
N1 C1 N4 112.1(11) . . ?
O8 Mo2 O12 105.2(5) . . ?
O8 Mo2 O6 102.3(4) . . ?
O12 Mo2 O6 98.2(4) . . ?
O8 Mo2 O3 93.6(4) . . ?
O12 Mo2 O3 98.9(4) . . ?
O6 Mo2 O3 152.7(3) . . ?
O8 Mo2 O5 91.4(4) . . ?
O12 Mo2 O5 163.1(4) . . ?
O6 Mo2 O5 75.3(3) . . ?
O3 Mo2 O5 82.2(3) . . ?
O8 Mo2 O9 160.7(4) . . ?
O12 Mo2 O9 91.3(4) . . ?
O6 Mo2 O9 84.6(3) . . ?
O3 Mo2 O9 73.9(3) . . ?
O5 Mo2 O9 72.7(3) . . ?
O4W Co2 O2W 85.5(4) . . ?
O4W Co2 O2 176.6(4) . . ?
O2W Co2 O2 94.5(4) . . ?
O4W Co2 N3 97.0(4) . . ?
O2W Co2 N3 172.6(4) . . ?
O2 Co2 N3 82.6(4) . . ?
O4W Co2 O3W 96.3(4) . . ?
O2W Co2 O3W 97.4(4) . . ?
O2 Co2 O3W 87.1(3) . . ?
N3 Co2 O3W 89.3(4) . . ?
O4W Co2 O1 90.1(4) . . ?
O2W Co2 O1 88.9(4) . . ?
O2 Co2 O1 86.5(3) . . ?
N3 Co2 O1 84.1(4) . . ?
O3W Co2 O1 171.4(3) . . ?
C3 N2 N6 106.2(11) . . ?
C3 N2 Co1 117.1(9) . . ?
N6 N2 Co1 136.6(9) . . ?
N3 C2 N1 114.0(12) . . ?
N3 C2 C3 130.0(11) . . ?
N1 C2 C3 116.1(11) . . ?
Mo1 O2 Co2 133.8(4) 2_557 . ?
O11 Mo3 O13 104.2(6) . . ?
O11 Mo3 O6 96.5(4) . . ?
O13 Mo3 O6 106.7(4) . . ?
O11 Mo3 O4 97.8(4) . 2_556 ?
O13 Mo3 O4 101.5(4) . 2_556 ?
O6 Mo3 O4 143.9(4) . 2_556 ?
O11 Mo3 O5 97.0(5) . . ?
O13 Mo3 O5 158.4(5) . . ?
O6 Mo3 O5 74.2(3) . . ?
O4 Mo3 O5 71.3(3) 2_556 . ?
O11 Mo3 O10 167.0(5) . . ?
O13 Mo3 O10 88.8(5) . . ?
O6 Mo3 O10 77.9(3) . . ?
O4 Mo3 O10 80.8(3) 2_556 . ?
O5 Mo3 O10 70.2(3) . . ?
Mo1 O3 Mo2 114.0(4) . . ?
C2 N3 N4 104.8(9) . . ?
C2 N3 Co2 137.2(9) . . ?
N4 N3 Co2 115.3(7) . . ?
N5 C3 N2 113.7(12) . . ?
N5 C3 C2 132.7(12) . . ?
N2 C3 C2 113.5(11) . . ?
O7 Mo4 O10 104.7(4) . . ?
O7 Mo4 O9 103.0(4) . . ?
O10 Mo4 O9 100.6(4) . . ?
O7 Mo4 O5 103.4(4) . 2_556 ?
O10 Mo4 O5 99.3(4) . 2_556 ?
O9 Mo4 O5 141.4(3) . 2_556 ?
O7 Mo4 O4 96.9(4) . . ?
O10 Mo4 O4 158.3(4) . . ?
O9 Mo4 O4 74.5(3) . . ?
O5 Mo4 O4 74.8(3) 2_556 . ?
O7 Mo4 O5 177.8(4) . . ?
O10 Mo4 O5 77.4(3) . . ?
O9 Mo4 O5 76.0(3) . . ?
O5 Mo4 O5 76.6(3) 2_556 . ?
O4 Mo4 O5 81.0(3) . . ?
C1 N4 N3 106.4(10) . . ?
C1 N4 Mo1 129.0(8) . 2_557 ?
N3 N4 Mo1 124.0(7) . 2_557 ?
Mo3 O4 Mo1 147.6(5) 2_556 . ?
Mo3 O4 Mo4 106.2(4) 2_556 . ?
Mo1 O4 Mo4 106.2(4) . . ?
N6 C4 N5 114.5(12) . . ?
N6 C4 C5 119.4(14) . . ?
N5 C4 C5 126.0(13) . . ?
Mo4 O5 Mo2 154.3(4) 2_556 . ?
Mo4 O5 Mo3 103.4(4) 2_556 . ?
Mo2 O5 Mo3 90.6(3) . . ?
Mo4 O5 Mo4 103.4(3) 2_556 . ?
Mo2 O5 Mo4 96.6(3) . . ?
Mo3 O5 Mo4 95.3(3) . . ?
C3 N5 C4 101.4(11) . . ?
C9 C5 C6 118.7(15) . . ?
C9 C5 C4 120.5(15) . . ?
C6 C5 C4 120.8(14) . . ?
Mo2 O6 Mo3 114.2(4) . . ?
C4 N6 N2 104.2(12) . . ?
C7 C6 C5 120.5(18) . . ?
C8 N7 C7 120.0(15) . . ?
N7 C7 C6 120(2) . . ?
N7 C8 C9 122.9(17) . . ?
Mo4 O9 Mo1 107.8(4) . . ?
Mo4 O9 Mo2 112.6(4) . . ?
Mo1 O9 Mo2 92.2(3) . . ?
C5 C9 C8 117.3(17) . . ?
Mo4 O10 Mo3 117.0(4) . . ?

_refine_diff_density_max         2.963
_refine_diff_density_min         -1.127
_refine_diff_density_rms         0.251

