# 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 1579652'
_audit_update_record             
;
2018-02-01 deposited with the CCDC.
2018-02-16 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            'C2 H19 Co Mo N6 O11'
_chemical_formula_weight         458.10

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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   27.0371(12)
_cell_length_b                   7.9845(3)
_cell_length_c                   6.4776(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1398.37(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    6943
_cell_measurement_theta_min      3.8711
_cell_measurement_theta_max      41.0626

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.176
_exptl_crystal_F_000             920
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    2.151
_exptl_absorpt_correction_T_min  0.51457
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur Kappa CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 16.3426
_diffrn_reflns_number            9126
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         3.874
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             1628
_reflns_number_gt                1468
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0381P)²+0.1737P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1628
_refine_ls_number_parameters     139
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0223
_refine_ls_wR_factor_ref         0.0567
_refine_ls_wR_factor_gt          0.0558
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
O4 O 0.13804(8) 0.7500 0.2762(3) 0.0241(4) Uani 1 2 d S T P . .
N4 N 0.20661(9) 0.2500 0.5985(4) 0.0237(5) Uani 1 2 d S T P . .
O5 O -0.02371(6) 0.5762(2) 0.3006(3) 0.0392(4) Uani 1 1 d . . . . .
C1 C 0.01160(7) 0.6522(3) 0.2323(3) 0.0232(4) Uani 1 1 d . . . . .
O7 O 0.25034(10) 0.2500 0.5557(4) 0.0482(7) Uani 1 2 d S T P . .
O6 O 0.19087(10) 0.2500 0.7717(4) 0.0462(7) Uani 1 2 d S T P . .
O8 O 0.29441(10) 0.2500 0.0990(5) 0.0523(8) Uani 1 2 d S T P . .
H11 H 0.314(2) 0.2500 0.015(9) 0.078 Uiso 1 2 d S U P . .
H10 H 0.311(2) 0.2500 0.200(9) 0.078 Uiso 1 2 d S U P . .
Mo1 Mo 0.10879(2) 0.7500 0.03530(4) 0.01686(9) Uani 1 2 d S T P . .
O3 O 0.05088(5) 0.58702(18) 0.1574(2) 0.0256(3) Uani 1 1 d . . . . .
O1 O 0.13453(6) 0.57721(19) -0.0871(2) 0.0269(3) Uani 1 1 d . . . . .
O2 O 0.05299(10) 0.7500 -0.2282(4) 0.0363(6) Uani 1 2 d S T P . .
H9 H 0.0356(11) 0.836(4) -0.247(5) 0.054 Uiso 1 1 d . U . . .
Co1 Co 0.15922(2) 0.2500 0.36657(6) 0.01580(11) Uani 1 2 d S T P . .
N1 N 0.11120(11) 0.2500 0.1343(4) 0.0243(6) Uani 1 2 d S T P . .
H1 H 0.1263(16) 0.2500 0.014(6) 0.037 Uiso 1 2 d S U P . .
H2 H 0.0966(10) 0.166(3) 0.127(4) 0.037 Uiso 1 1 d . U . . .
N3 N 0.19902(7) 0.4220(2) 0.2281(3) 0.0253(4) Uani 1 1 d . . . . .
H3 H 0.2264(11) 0.394(3) 0.200(4) 0.038 Uiso 1 1 d . U . . .
H4 H 0.1823(10) 0.465(4) 0.117(4) 0.038 Uiso 1 1 d . U . . .
H5 H 0.2015(9) 0.512(4) 0.302(4) 0.038 Uiso 1 1 d . U . . .
N2 N 0.12030(7) 0.4228(3) 0.5039(3) 0.0225(4) Uani 1 1 d . . . . .
H7 H 0.1169(9) 0.516(4) 0.430(4) 0.034 Uiso 1 1 d . U . . .
H6 H 0.1292(10) 0.452(4) 0.611(5) 0.034 Uiso 1 1 d . U . . .
H8 H 0.0908(11) 0.398(4) 0.522(4) 0.034 Uiso 1 1 d . 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
O4 Mo1 1.750(2) . ?
N4 O6 1.200(4) . ?
N4 O7 1.215(4) . ?
N4 Co1 1.975(3) . ?
O5 C1 1.215(3) . ?
C1 O3 1.279(2) . ?
C1 C1 1.561(4) 8_575 ?
Mo1 O1 1.7368(15) . ?
Mo1 O1 1.7368(15) 8_575 ?
Mo1 O3 2.1842(14) . ?
Mo1 O3 2.1842(14) 8_575 ?
Mo1 O2 2.278(2) . ?
Co1 N2 1.9497(19) . ?
Co1 N2 1.9497(19) 8_565 ?
Co1 N3 1.9615(18) . ?
Co1 N3 1.9615(18) 8_565 ?
Co1 N1 1.988(3) . ?

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
O6 N4 O7 124.0(3) . . ?
O6 N4 Co1 118.8(2) . . ?
O7 N4 Co1 117.2(2) . . ?
O5 C1 O3 126.0(2) . . ?
O5 C1 C1 120.00(13) . 8_575 ?
O3 C1 C1 114.04(11) . 8_575 ?
O1 Mo1 O1 105.19(11) . 8_575 ?
O1 Mo1 O4 103.07(7) . . ?
O1 Mo1 O4 103.07(7) 8_575 . ?
O1 Mo1 O3 88.81(6) . . ?
O1 Mo1 O3 157.80(7) 8_575 . ?
O4 Mo1 O3 90.06(7) . . ?
O1 Mo1 O3 157.79(7) . 8_575 ?
O1 Mo1 O3 88.82(6) 8_575 8_575 ?
O4 Mo1 O3 90.06(7) . 8_575 ?
O3 Mo1 O3 73.14(8) . 8_575 ?
O1 Mo1 O2 85.60(7) . . ?
O1 Mo1 O2 85.60(7) 8_575 . ?
O4 Mo1 O2 165.40(10) . . ?
O3 Mo1 O2 78.26(7) . . ?
O3 Mo1 O2 78.26(7) 8_575 . ?
C1 O3 Mo1 119.36(13) . . ?
N2 Co1 N2 90.06(12) . 8_565 ?
N2 Co1 N3 90.54(9) . . ?
N2 Co1 N3 179.34(9) 8_565 . ?
N2 Co1 N3 179.33(9) . 8_565 ?
N2 Co1 N3 90.55(9) 8_565 8_565 ?
N3 Co1 N3 88.85(12) . 8_565 ?
N2 Co1 N4 90.17(8) . . ?
N2 Co1 N4 90.18(8) 8_565 . ?
N3 Co1 N4 89.55(8) . . ?
N3 Co1 N4 89.55(8) 8_565 . ?
N2 Co1 N1 89.59(9) . . ?
N2 Co1 N1 89.59(9) 8_565 . ?
N3 Co1 N1 90.69(9) . . ?
N3 Co1 N1 90.70(9) 8_565 . ?
N4 Co1 N1 179.66(12) . . ?

_refine_diff_density_max         0.338
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.141

####################################################################### 
# 
# 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 1579653'
_audit_update_record             
;
2017-10-12 deposited with the CCDC.
2018-02-16 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         
'C8 Mo4 O28, 2(C2 H2 Mo O8), 4(Co H18 N6), 10(H2 O)'
_chemical_formula_sum            'C12 H96 Co4 Mo6 N24 O54'
_chemical_formula_weight         2252.48

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                   10.2131(3)
_cell_length_b                   13.1299(4)
_cell_length_c                   13.2356(3)
_cell_angle_alpha                79.390(2)
_cell_angle_beta                 84.259(2)
_cell_angle_gamma                77.997(2)
_cell_volume                     1702.85(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    150.0(2)
_cell_measurement_reflns_used    9322
_cell_measurement_theta_min      3.7499
_cell_measurement_theta_max      39.0953

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.197
_exptl_crystal_F_000             1128
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    2.141
_exptl_absorpt_correction_T_min  0.67488
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      150.0(2)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur Kappa CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 16.3426
_diffrn_reflns_number            12170
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_av_R_equivalents  0.0203
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.760
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             7387
_reflns_number_gt                5877
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0218P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7387
_refine_ls_number_parameters     636
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0226
_refine_ls_wR_factor_ref         0.0473
_refine_ls_wR_factor_gt          0.0462
_refine_ls_goodness_of_fit_ref   0.908
_refine_ls_restrained_S_all      0.907
_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
H18 H 0.025(3) 0.258(3) -0.093(2) 0.036(10) Uiso 1 1 d . . . . .
O23 O 0.3496(3) 0.0318(2) -0.0558(2) 0.0430(7) Uani 1 1 d . . . . .
H1W H 0.352(4) 0.102(4) -0.069(3) 0.065 Uiso 1 1 d . U . . .
H2W H 0.346(4) 0.020(4) -0.115(3) 0.065 Uiso 1 1 d . U . . .
O24 O 0.4719(3) 0.2154(2) -0.26806(19) 0.0398(7) Uani 1 1 d . . . . .
H3W H 0.534(4) 0.262(4) -0.282(3) 0.060 Uiso 1 1 d . U . . .
H4W H 0.410(4) 0.233(4) -0.236(3) 0.060 Uiso 1 1 d . U . . .
O25 O 0.06406(18) 0.27194(17) 0.34262(14) 0.0179(4) Uani 1 1 d D . . . .
H5W H 0.017(2) 0.2250(18) 0.3895(17) 0.027 Uiso 1 1 d D U . . .
H6W H 0.1442(17) 0.2265(19) 0.321(2) 0.027 Uiso 1 1 d D U . . .
O26 O 0.4717(2) 0.30557(18) 0.45273(16) 0.0236(5) Uani 1 1 d . . . . .
H7W H 0.459(3) 0.349(3) 0.495(3) 0.035 Uiso 1 1 d . U . . .
H8W H 0.435(3) 0.338(3) 0.398(3) 0.035 Uiso 1 1 d . U . . .
O27 O 0.3322(2) -0.0634(2) 0.1498(2) 0.0405(7) Uani 1 1 d . . . . .
H9W H 0.354(4) -0.040(4) 0.087(3) 0.061 Uiso 1 1 d . U . . .
H10W H 0.397(4) -0.109(4) 0.173(3) 0.061 Uiso 1 1 d . U . . .
C6 C 0.6500(2) 0.4317(2) 0.30044(18) 0.0123(6) Uani 1 1 d . . . . .
C7 C 0.5781(2) 0.5269(2) 0.35063(18) 0.0133(6) Uani 1 1 d . . . . .
O12 O 0.76658(16) 0.39087(17) 0.31706(14) 0.0180(4) Uani 1 1 d . . . . .
O14 O 0.63342(18) 0.55332(17) 0.41745(14) 0.0228(5) Uani 1 1 d . . . . .
O22 O 0.11015(18) -0.14761(18) 0.53626(13) 0.0219(5) Uani 1 1 d . . . . .
C1 C 0.4989(2) 0.1969(2) 0.14002(19) 0.0130(6) Uani 1 1 d . . . . .
C2 C 0.3541(2) 0.2210(2) 0.18751(19) 0.0131(6) Uani 1 1 d . . . . .
C3 C 0.0903(2) -0.0273(2) 0.3753(2) 0.0143(6) Uani 1 1 d . . . . .
C4 C 0.0630(2) -0.1254(2) 0.45125(19) 0.0145(6) Uani 1 1 d . . . . .
N1 N -0.1609(2) 0.1945(2) 0.21828(17) 0.0123(5) Uani 1 1 d . . . . .
N2 N -0.1620(2) 0.1437(2) 0.02478(19) 0.0135(5) Uani 1 1 d . . . . .
N3 N 0.0783(2) 0.1442(2) 0.0954(2) 0.0144(5) Uani 1 1 d . . . . .
N4 N -0.2586(2) 0.3496(2) 0.05863(18) 0.0115(5) Uani 1 1 d . . . . .
N5 N -0.0218(3) 0.3069(2) -0.05729(17) 0.0139(5) Uani 1 1 d . . . . .
N6 N -0.0221(2) 0.3542(2) 0.13597(19) 0.0118(5) Uani 1 1 d . . . . .
N7 N 0.4612(2) -0.0239(2) 0.36544(18) 0.0147(5) Uani 1 1 d D . . . .
N8 N 0.6522(2) -0.1178(2) 0.50151(18) 0.0139(5) Uani 1 1 d D . . . .
N9 N 0.6222(3) 0.0932(2) 0.43299(18) 0.0152(5) Uani 1 1 d D . . . .
N10 N 0.8612(2) 0.6279(2) 0.4921(2) 0.0145(5) Uani 1 1 d D . . . .
N11 N 0.9928(3) 0.5054(2) 0.35132(18) 0.0162(5) Uani 1 1 d . . . . .
N12 N 1.1387(3) 0.5867(2) 0.4674(2) 0.0167(5) Uani 1 1 d . . . . .
O1 O 0.31238(19) 0.25181(17) -0.08245(14) 0.0211(4) Uani 1 1 d . . . . .
O2 O 0.45530(17) 0.41249(15) -0.11260(12) 0.0148(4) Uani 1 1 d . . . . .
O3 O 0.18913(17) 0.43963(16) -0.03113(13) 0.0158(4) Uani 1 1 d . . . . .
O4 O 0.51616(16) 0.24390(15) 0.04831(13) 0.0130(4) Uani 1 1 d . . . . .
O5 O 0.58552(17) 0.13466(17) 0.19132(14) 0.0193(4) Uani 1 1 d . . . . .
O6 O 0.26966(16) 0.27552(15) 0.12236(13) 0.0141(4) Uani 1 1 d . . . . .
O7 O 0.32631(18) 0.18767(17) 0.27761(14) 0.0221(5) Uani 1 1 d . . . . .
O8 O 0.38955(16) 0.44271(15) 0.09149(12) 0.0131(4) Uani 1 1 d . . . . .
O9 O 0.30214(17) 0.43528(17) 0.29553(13) 0.0183(4) Uani 1 1 d . . . . .
O10 O 0.27197(17) 0.62489(16) 0.16999(13) 0.0182(4) Uani 1 1 d . . . . .
O11 O 0.57695(16) 0.40249(15) 0.24175(12) 0.0122(4) Uani 1 1 d . . . . .
O13 O 0.46348(16) 0.57206(15) 0.31676(12) 0.0135(4) Uani 1 1 d . . . . .
O15 O -0.22672(17) -0.06939(17) 0.29368(13) 0.0185(4) Uani 1 1 d . . . . .
O16 O -0.04733(18) -0.08324(16) 0.12730(13) 0.0179(4) Uani 1 1 d . . . . .
O17 O -0.07600(18) -0.26485(16) 0.26697(13) 0.0186(4) Uani 1 1 d . . . . .
O18 O 0.1676(2) -0.1938(2) 0.24625(16) 0.0208(5) Uani 1 1 d . . . . .
O19 O 0.02744(17) -0.00970(15) 0.29199(13) 0.0148(4) Uani 1 1 d . . . . .
O20 O 0.16474(18) 0.02603(17) 0.39672(15) 0.0220(5) Uani 1 1 d . . . . .
O21 O -0.01213(17) -0.17791(15) 0.41869(13) 0.0146(4) Uani 1 1 d . . . . .
Co1 Co -0.09081(3) 0.24838(3) 0.07984(2) 0.00887(8) Uani 1 1 d . . . . .
Co2 Co 0.5000 0.0000 0.5000 0.00933(11) Uani 1 2 d S . P . .
Co3 Co 1.0000 0.5000 0.5000 0.00989(11) Uani 1 2 d S . P . .
M01 Mo 0.34297(2) 0.35132(2) -0.02439(2) 0.01048(5) Uani 1 1 d . . . . .
M21 Mo 0.38701(2) 0.50681(2) 0.19728(2) 0.00985(5) Uani 1 1 d . . . . .
M31 Mo -0.06726(2) -0.13236(2) 0.25877(2) 0.01088(6) Uani 1 1 d . . . . .
H32 H 1.063(3) 0.476(3) 0.320(2) 0.022(9) Uiso 1 1 d . . . . .
H31 H 0.973(3) 0.570(3) 0.322(2) 0.011(8) Uiso 1 1 d . . . . .
H35 H 1.198(4) 0.565(3) 0.417(3) 0.054(12) Uiso 1 1 d . . . . .
H34 H 1.111(3) 0.648(3) 0.454(2) 0.020(9) Uiso 1 1 d . . . . .
H24 H 0.701(3) -0.115(3) 0.439(2) 0.027(9) Uiso 1 1 d . . . . .
H27 H 0.643(3) 0.088(3) 0.3686(7) 0.027(9) Uiso 1 1 d D . . . .
H20 H 0.494(3) -0.082(3) 0.352(2) 0.023(10) Uiso 1 1 d . . . . .
H21 H 0.488(3) 0.012(3) 0.319(3) 0.041(12) Uiso 1 1 d . . . . .
H19 H 0.3762(8) -0.011(3) 0.355(3) 0.046(11) Uiso 1 1 d D . . . .
H7 H 0.073(3) 0.095(3) 0.154(3) 0.036(10) Uiso 1 1 d . . . . .
H8 H 0.094(3) 0.117(3) 0.039(2) 0.019(8) Uiso 1 1 d . . . . .
H9 H 0.147(3) 0.170(3) 0.106(2) 0.030(9) Uiso 1 1 d . . . . .
H13 H -0.084(3) 0.417(3) 0.121(2) 0.037(10) Uiso 1 1 d . . . . .
H12 H -0.239(3) 0.410(3) 0.032(2) 0.027(9) Uiso 1 1 d . . . . .
H16 H -0.083(3) 0.336(3) -0.098(2) 0.013(8) Uiso 1 1 d . . . . .
H11 H -0.308(3) 0.355(3) 0.116(3) 0.030(9) Uiso 1 1 d . . . . .
H6 H -0.249(4) 0.158(3) 0.022(2) 0.041(10) Uiso 1 1 d . . . . .
H4 H -0.143(3) 0.082(3) 0.061(2) 0.009(7) Uiso 1 1 d . . . . .
H26 H 0.594(3) 0.154(3) 0.436(2) 0.024(10) Uiso 1 1 d . . . . .
H23 H 0.710(2) -0.113(3) 0.5432(19) 0.047(11) Uiso 1 1 d D . . . .
H22 H 0.628(3) -0.177(3) 0.516(2) 0.029(10) Uiso 1 1 d . . . . .
H36 H 1.189(3) 0.586(3) 0.510(3) 0.041(11) Uiso 1 1 d . . . . .
H33 H 0.941(3) 0.476(3) 0.338(3) 0.035(11) Uiso 1 1 d . . . . .
H10 H -0.306(3) 0.331(3) 0.018(3) 0.039(10) Uiso 1 1 d . . . . .
H17 H 0.029(3) 0.348(3) -0.055(3) 0.042(11) Uiso 1 1 d . . . . .
H15 H 0.051(3) 0.361(3) 0.111(2) 0.037(11) Uiso 1 1 d . . . . .
H2 H -0.229(3) 0.173(3) 0.218(2) 0.031(10) Uiso 1 1 d . . . . .
H3 H -0.180(3) 0.239(3) 0.259(3) 0.039(11) Uiso 1 1 d . . . . .
H1 H -0.105(3) 0.140(3) 0.248(2) 0.027(9) Uiso 1 1 d . . . . .
H37 H 0.193(4) -0.251(4) 0.232(3) 0.052(14) Uiso 1 1 d . . . . .
H38 H 0.211(3) -0.149(3) 0.219(2) 0.025(10) Uiso 1 1 d . . . . .
H5 H -0.122(3) 0.137(3) -0.030(3) 0.033(10) Uiso 1 1 d . . . . .
H28 H 0.789(2) 0.604(3) 0.488(3) 0.075(15) Uiso 1 1 d D . . . .
H29 H 0.875(4) 0.666(3) 0.437(3) 0.049(12) Uiso 1 1 d . . . . .
H30 H 0.866(4) 0.658(4) 0.546(4) 0.087(16) Uiso 1 1 d . . . . .
H14 H -0.022(3) 0.339(3) 0.196(3) 0.035(11) Uiso 1 1 d . . . . .
H25 H 0.701(3) 0.077(3) 0.459(2) 0.035(10) Uiso 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
C6 O12 1.223(3) . ?
C6 O11 1.285(3) . ?
C6 C7 1.540(4) . ?
C7 O14 1.231(3) . ?
C7 O13 1.281(3) . ?
O22 C4 1.230(3) . ?
C1 O5 1.236(3) . ?
C1 O4 1.270(3) . ?
C1 C2 1.541(3) . ?
C2 O7 1.219(3) . ?
C2 O6 1.290(3) . ?
C3 O20 1.219(3) . ?
C3 O19 1.291(3) . ?
C3 C4 1.538(4) . ?
C4 O21 1.283(3) . ?
N1 Co1 1.960(2) . ?
N2 Co1 1.959(2) . ?
N3 Co1 1.971(2) . ?
N4 Co1 1.948(2) . ?
N5 Co1 1.959(2) . ?
N6 Co1 1.965(2) . ?
N7 Co2 1.956(2) . ?
N8 Co2 1.950(2) . ?
N9 Co2 1.963(2) . ?
N10 Co3 1.954(2) . ?
N11 Co3 1.964(2) . ?
N12 Co3 1.964(2) . ?
O1 M01 1.727(2) . ?
O2 M01 1.7590(17) . ?
O2 M21 2.2099(17) 2_665 ?
O3 M01 1.7474(18) . ?
O4 M01 2.2015(17) . ?
O6 M01 2.1519(17) . ?
O8 M21 1.7570(17) . ?
O8 M01 2.2538(17) . ?
O9 M21 1.7286(18) . ?
O10 M21 1.7423(19) . ?
O11 M21 2.1936(17) . ?
O13 M21 2.2067(17) . ?
O15 M31 1.7261(18) . ?
O16 M31 1.7481(17) . ?
O17 M31 1.743(2) . ?
O18 M31 2.365(2) . ?
O19 M31 2.1717(19) . ?
O21 M31 2.1880(17) . ?
Co2 N8 1.950(2) 2_656 ?
Co2 N7 1.956(2) 2_656 ?
Co2 N9 1.963(2) 2_656 ?
Co3 N10 1.954(2) 2_766 ?
Co3 N12 1.964(2) 2_766 ?
Co3 N11 1.964(2) 2_766 ?
M21 O2 2.2099(17) 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
O12 C6 O11 125.5(3) . . ?
O12 C6 C7 120.6(2) . . ?
O11 C6 C7 113.9(2) . . ?
O14 C7 O13 126.1(3) . . ?
O14 C7 C6 119.0(2) . . ?
O13 C7 C6 115.0(2) . . ?
O5 C1 O4 126.1(2) . . ?
O5 C1 C2 119.2(2) . . ?
O4 C1 C2 114.6(2) . . ?
O7 C2 O6 125.5(2) . . ?
O7 C2 C1 121.1(2) . . ?
O6 C2 C1 113.4(2) . . ?
O20 C3 O19 126.2(3) . . ?
O20 C3 C4 120.2(2) . . ?
O19 C3 C4 113.7(2) . . ?
O22 C4 O21 124.9(3) . . ?
O22 C4 C3 120.4(2) . . ?
O21 C4 C3 114.7(2) . . ?
M01 O2 M21 169.21(10) . 2_665 ?
C1 O4 M01 118.29(16) . . ?
C2 O6 M01 119.42(15) . . ?
M21 O8 M01 165.37(9) . . ?
C6 O11 M21 118.89(17) . . ?
C7 O13 M21 118.44(17) . . ?
C3 O19 M31 118.68(17) . . ?
C4 O21 M31 118.18(16) . . ?
N4 Co1 N2 90.74(11) . . ?
N4 Co1 N5 89.23(11) . . ?
N2 Co1 N5 91.90(11) . . ?
N4 Co1 N1 89.73(11) . . ?
N2 Co1 N1 89.71(11) . . ?
N5 Co1 N1 178.09(12) . . ?
N4 Co1 N6 88.56(11) . . ?
N2 Co1 N6 179.14(11) . . ?
N5 Co1 N6 88.57(11) . . ?
N1 Co1 N6 89.81(11) . . ?
N4 Co1 N3 177.45(11) . . ?
N2 Co1 N3 87.34(11) . . ?
N5 Co1 N3 89.17(11) . . ?
N1 Co1 N3 91.93(11) . . ?
N6 Co1 N3 93.38(11) . . ?
N8 Co2 N8 180.0 2_656 . ?
N8 Co2 N7 88.68(11) 2_656 2_656 ?
N8 Co2 N7 91.32(11) . 2_656 ?
N8 Co2 N7 91.32(11) 2_656 . ?
N8 Co2 N7 88.68(11) . . ?
N7 Co2 N7 180.0 2_656 . ?
N8 Co2 N9 87.82(12) 2_656 2_656 ?
N8 Co2 N9 92.18(12) . 2_656 ?
N7 Co2 N9 90.26(11) 2_656 2_656 ?
N7 Co2 N9 89.74(11) . 2_656 ?
N8 Co2 N9 92.18(12) 2_656 . ?
N8 Co2 N9 87.82(12) . . ?
N7 Co2 N9 89.74(11) 2_656 . ?
N7 Co2 N9 90.26(11) . . ?
N9 Co2 N9 180.00(11) 2_656 . ?
N10 Co3 N10 180.0 . 2_766 ?
N10 Co3 N12 89.98(11) . 2_766 ?
N10 Co3 N12 90.02(11) 2_766 2_766 ?
N10 Co3 N12 90.02(11) . . ?
N10 Co3 N12 89.98(11) 2_766 . ?
N12 Co3 N12 180.0 2_766 . ?
N10 Co3 N11 89.22(11) . . ?
N10 Co3 N11 90.79(11) 2_766 . ?
N12 Co3 N11 91.98(12) 2_766 . ?
N12 Co3 N11 88.02(12) . . ?
N10 Co3 N11 90.78(11) . 2_766 ?
N10 Co3 N11 89.21(11) 2_766 2_766 ?
N12 Co3 N11 88.02(12) 2_766 2_766 ?
N12 Co3 N11 91.98(12) . 2_766 ?
N11 Co3 N11 180.0 . 2_766 ?
O1 M01 O3 101.91(9) . . ?
O1 M01 O2 104.47(9) . . ?
O3 M01 O2 105.90(8) . . ?
O1 M01 O6 90.30(8) . . ?
O3 M01 O6 88.08(7) . . ?
O2 M01 O6 156.72(7) . . ?
O1 M01 O4 90.55(8) . . ?
O3 M01 O4 157.40(7) . . ?
O2 M01 O4 88.80(7) . . ?
O6 M01 O4 72.90(6) . . ?
O1 M01 O8 163.16(8) . . ?
O3 M01 O8 85.75(7) . . ?
O2 M01 O8 87.49(7) . . ?
O6 M01 O8 74.84(7) . . ?
O4 M01 O8 77.69(7) . . ?
O9 M21 O10 102.37(9) . . ?
O9 M21 O8 104.12(9) . . ?
O10 M21 O8 105.06(8) . . ?
O9 M21 O11 89.85(8) . . ?
O10 M21 O11 157.67(8) . . ?
O8 M21 O11 89.65(7) . . ?
O9 M21 O13 87.54(8) . . ?
O10 M21 O13 89.07(8) . . ?
O8 M21 O13 158.95(7) . . ?
O11 M21 O13 72.66(7) . . ?
O9 M21 O2 160.46(7) . 2_665 ?
O10 M21 O2 88.53(8) . 2_665 ?
O8 M21 O2 88.30(7) . 2_665 ?
O11 M21 O2 74.98(7) . 2_665 ?
O13 M21 O2 76.35(6) . 2_665 ?
O15 M31 O17 105.85(9) . . ?
O15 M31 O16 103.47(9) . . ?
O17 M31 O16 105.74(9) . . ?
O15 M31 O19 93.71(8) . . ?
O17 M31 O19 151.34(8) . . ?
O16 M31 O19 89.32(8) . . ?
O15 M31 O21 92.75(7) . . ?
O17 M31 O21 85.12(8) . . ?
O16 M31 O21 156.82(8) . . ?
O19 M31 O21 73.00(7) . . ?
O15 M31 O18 163.76(9) . . ?
O17 M31 O18 84.67(9) . . ?
O16 M31 O18 84.98(8) . . ?
O19 M31 O18 72.29(8) . . ?
O21 M31 O18 75.55(7) . . ?

_refine_diff_density_max         0.482
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.091

####################################################################### 
# 
# 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_4b
_database_code_depnum_ccdc_archive 'CCDC 1579658'
_audit_update_record             
;
2017-10-12 deposited with the CCDC.
2018-02-16 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT041_shelx               
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check
RESPONSE: A hydrogen atom of a solvent water molecule could not be located 
either from the elecron difference map, or assigned unequivocally based on 
hydrogen bonding pattern an was therefore not included in the model.
;
# end Validation Reply Form

_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 H46 Co2 Mo2 N8 O28'
_chemical_formula_weight         1108.35

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'
Mo Mo -1.6832 0.6857 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'

_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+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y, z-1/2'

_cell_length_a                   10.7699(5)
_cell_length_b                   22.3609(9)
_cell_length_c                   15.1262(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3642.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    4081
_cell_measurement_theta_min      4.3220
_cell_measurement_theta_max      28.9700

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.021
_exptl_crystal_F_000             2240
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    1.680
_exptl_absorpt_correction_T_min  0.76401
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur Kappa CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 16.3426
_diffrn_reflns_number            26808
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_av_R_equivalents  0.0776
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         4.201
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             3969
_reflns_number_gt                2979
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0355P)²+2.4720P] 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         3969
_refine_ls_number_parameters     296
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0423
_refine_ls_wR_factor_ref         0.0946
_refine_ls_wR_factor_gt          0.0855
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.006
_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
O15 O 0.0239(4) 0.6314(2) -0.1564(3) 0.0819(13) Uani 1 1 d D . . . .
H5W H 0.095(4) 0.607(2) -0.149(5) 0.123 Uiso 1 1 d D U . . .
O14 O 0.5000 0.3523(3) -0.2500 0.148(4) Uani 1 2 d DS T P . .
H3W H 0.522(8) 0.3822(3) -0.292(2) 0.222 Uiso 1 1 d D U . . .
O13 O 0.5332(5) 0.2650(3) -0.0958(4) 0.137(3) Uani 1 1 d D . . . .
H2W H 0.606(4) 0.270(4) -0.131(4) 0.206 Uiso 1 1 d D U . . .
H1W H 0.502(6) 0.3023(18) -0.117(5) 0.206 Uiso 1 1 d D U . . .
O8 O 0.6043(3) 0.38773(14) 0.0911(2) 0.0424(8) Uani 1 1 d . . . . .
Mo1 Mo 0.64584(3) 0.21464(2) 0.18622(2) 0.02919(12) Uani 1 1 d . . . . .
Co2 Co 0.25221(5) 0.47620(2) 0.05424(3) 0.02169(14) Uani 1 1 d . . . . .
O3 O 0.1573(2) 0.50595(13) -0.04330(17) 0.0278(6) Uani 1 1 d . . . . .
N1 N 0.3516(3) 0.44208(16) 0.1489(2) 0.0266(8) Uani 1 1 d . . . . .
N2 N 0.1905(3) 0.39537(16) 0.0360(2) 0.0309(8) Uani 1 1 d . . . . .
N3 N 0.1154(3) 0.49896(16) 0.1307(2) 0.0271(8) Uani 1 1 d D . . . .
N4 N 0.3206(3) 0.55515(16) 0.0787(2) 0.0285(8) Uani 1 1 d . . . . .
O2 O 0.3792(2) 0.46114(13) -0.03050(18) 0.0305(7) Uani 1 1 d . . . . .
O7 O 0.5774(3) 0.30264(13) 0.16461(18) 0.0340(7) Uani 1 1 d . . . . .
O1 O 0.4177(3) 0.47552(15) -0.17344(19) 0.0425(8) Uani 1 1 d . . . . .
O5 O 0.7535(2) 0.24982(13) 0.08399(19) 0.0324(7) Uani 1 1 d . . . . .
O11 O 0.5000 0.19824(19) 0.2500 0.0462(12) Uani 1 2 d S T P . .
O10 O 0.6955(3) 0.14474(13) 0.1577(2) 0.0414(8) Uani 1 1 d . . . . .
C4 C 0.3500(4) 0.47905(19) -0.1087(3) 0.0293(9) Uani 1 1 d . . . . .
C5 C 0.2191(4) 0.5062(2) -0.1160(3) 0.0299(9) Uani 1 1 d . . . . .
O9 O 0.7430(3) 0.23468(16) 0.2682(2) 0.0540(9) Uani 1 1 d . . . . .
C6 C 0.7338(4) 0.3033(2) 0.0570(3) 0.0311(10) Uani 1 1 d . . . . .
O4 O 0.1796(3) 0.52545(16) -0.18642(18) 0.0442(8) Uani 1 1 d . . . . .
C7 C 0.6296(4) 0.33613(18) 0.1072(3) 0.0283(9) Uani 1 1 d . . . . .
O12 O 0.5181(3) 0.20474(16) 0.0619(2) 0.0450(8) Uani 1 1 d D . . . .
C1 C 0.3115(4) 0.3803(2) 0.1662(3) 0.0345(10) Uani 1 1 d . . . . .
H1A H 0.2398 0.3799 0.2050 0.041 Uiso 1 1 calc R U . . .
H1B H 0.3778 0.3578 0.1941 0.041 Uiso 1 1 calc R U . . .
C020 C 0.2792(4) 0.3532(2) 0.0786(3) 0.0372(11) Uani 1 1 d . . . . .
H02A H 0.3530 0.3486 0.0425 0.045 Uiso 1 1 calc R U . . .
H02B H 0.2411 0.3143 0.0865 0.045 Uiso 1 1 calc R U . . .
C3 C 0.2493(4) 0.58334(18) 0.1520(3) 0.0320(10) Uani 1 1 d . . . . .
H3A H 0.2570 0.6265 0.1497 0.038 Uiso 1 1 calc R U . . .
H3B H 0.2797 0.5695 0.2088 0.038 Uiso 1 1 calc R U . . .
O6 O 0.7896(3) 0.32830(16) -0.0024(2) 0.0531(10) Uani 1 1 d . . . . .
C2 C 0.1164(4) 0.56475(19) 0.1388(3) 0.0340(10) Uani 1 1 d . . . . .
H2A H 0.0662 0.5772 0.1888 0.041 Uiso 1 1 calc R U . . .
H2B H 0.0829 0.5830 0.0857 0.041 Uiso 1 1 calc R U . . .
H1N H 0.420(4) 0.442(2) 0.129(3) 0.051 Uiso 1 1 d . U . . .
H2N H 0.358(4) 0.464(2) 0.197(3) 0.051 Uiso 1 1 d . U . . .
H3N H 0.121(4) 0.389(2) 0.063(3) 0.051 Uiso 1 1 d . U . . .
H4N H 0.182(4) 0.385(2) -0.018(3) 0.051 Uiso 1 1 d . U . . .
H6N H 0.126(5) 0.487(2) 0.179(3) 0.051 Uiso 1 1 d . U . . .
H5N H 0.049(2) 0.4851(19) 0.105(3) 0.051 Uiso 1 1 d D U . . .
H7N H 0.394(4) 0.554(2) 0.095(3) 0.051 Uiso 1 1 d . U . . .
H8N H 0.308(5) 0.574(2) 0.036(3) 0.051 Uiso 1 1 d . U . . .
H2O H 0.517(3) 0.2293(16) 0.0106(17) 0.051 Uiso 1 1 d D U . . .
H1O H 0.4317(9) 0.1974(19) 0.056(2) 0.051 Uiso 1 1 d D 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
O8 C7 1.210(5) . ?
Mo1 O9 1.684(3) . ?
Mo1 O10 1.707(3) . ?
Mo1 O11 1.8794(9) . ?
Mo1 O5 2.087(3) . ?
Mo1 O7 2.126(3) . ?
Mo1 O12 2.341(3) . ?
Co2 O2 1.904(3) . ?
Co2 O3 1.914(3) . ?
Co2 N3 1.941(3) . ?
Co2 N1 1.943(3) . ?
Co2 N2 1.946(4) . ?
Co2 N4 1.948(4) . ?
O3 C5 1.284(5) . ?
N1 C1 1.472(5) . ?
N2 C020 1.488(5) . ?
N3 C2 1.476(5) . ?
N4 C3 1.488(5) . ?
O2 C4 1.288(5) . ?
O7 C7 1.277(5) . ?
O1 C4 1.223(5) . ?
O5 C6 1.281(5) . ?
O11 Mo1 1.8794(9) 4_655 ?
C4 C5 1.539(6) . ?
C5 O4 1.226(5) . ?
C6 O6 1.218(5) . ?
C6 C7 1.541(6) . ?
C1 C020 1.498(6) . ?
C3 C2 1.505(6) . ?

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
O9 Mo1 O10 103.59(16) . . ?
O9 Mo1 O11 101.15(13) . . ?
O10 Mo1 O11 102.30(17) . . ?
O9 Mo1 O5 95.75(15) . . ?
O10 Mo1 O5 89.07(13) . . ?
O11 Mo1 O5 156.67(10) . . ?
O9 Mo1 O7 94.73(14) . . ?
O10 Mo1 O7 156.46(13) . . ?
O11 Mo1 O7 88.27(15) . . ?
O5 Mo1 O7 74.32(11) . . ?
O9 Mo1 O12 169.25(15) . . ?
O10 Mo1 O12 83.95(14) . . ?
O11 Mo1 O12 84.43(8) . . ?
O5 Mo1 O12 76.50(11) . . ?
O7 Mo1 O12 76.13(12) . . ?
O2 Co2 O3 85.76(11) . . ?
O2 Co2 N3 173.01(14) . . ?
O3 Co2 N3 87.89(13) . . ?
O2 Co2 N1 91.77(14) . . ?
O3 Co2 N1 176.61(14) . . ?
N3 Co2 N1 94.70(15) . . ?
O2 Co2 N2 89.17(14) . . ?
O3 Co2 N2 91.78(14) . . ?
N3 Co2 N2 93.95(16) . . ?
N1 Co2 N2 85.87(15) . . ?
O2 Co2 N4 90.96(14) . . ?
O3 Co2 N4 91.91(14) . . ?
N3 Co2 N4 86.33(15) . . ?
N1 Co2 N4 90.43(16) . . ?
N2 Co2 N4 176.30(16) . . ?
C5 O3 Co2 112.6(2) . . ?
C1 N1 Co2 109.8(3) . . ?
C020 N2 Co2 107.9(3) . . ?
C2 N3 Co2 107.8(3) . . ?
C3 N4 Co2 109.3(3) . . ?
C4 O2 Co2 112.8(2) . . ?
C7 O7 Mo1 119.7(3) . . ?
C6 O5 Mo1 119.7(3) . . ?
Mo1 O11 Mo1 157.5(3) 4_655 . ?
O1 C4 O2 124.7(4) . . ?
O1 C4 C5 121.0(4) . . ?
O2 C4 C5 114.3(3) . . ?
O4 C5 O3 124.5(4) . . ?
O4 C5 C4 121.2(4) . . ?
O3 C5 C4 114.3(3) . . ?
O6 C6 O5 125.6(4) . . ?
O6 C6 C7 120.3(4) . . ?
O5 C6 C7 114.1(4) . . ?
O8 C7 O7 126.7(4) . . ?
O8 C7 C6 121.3(4) . . ?
O7 C7 C6 112.1(4) . . ?
N1 C1 C020 106.8(3) . . ?
N2 C020 C1 106.1(4) . . ?
N4 C3 C2 106.0(3) . . ?
N3 C2 C3 107.0(3) . . ?

_refine_diff_density_max         0.629
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.100

####################################################################### 
# 
# 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 1579655'
_audit_update_record             
;
2017-10-12 deposited with the CCDC.
2018-02-16 downloaded from the CCDC.
;

# start Validation Reply Form

_vrf_PLAT306_3                   
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O23 Check 
RESPONSE: The structure contains a large amount of heavily disordered solvent 
water which could be modeled only approximately. While some of the water 
molecules (O23-O25) could be considered as positioned correctly with a degree 
certainty, several are modeled according to remaining voids in the structure 
and in order to account for the (highly disperded) residual electron density. 
Modeling hydrogen atoms on water molecules in given ciscumstances would, 
in our oppinion, be entirely unjustified, and we have therefore restrained 
from doing so.
;
_vrf_PLAT043_3                   
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      14.11 Check 
RESPONSE: The difference corresponds to 14 hydrogen atoms in the (disordered) 
solvent water molecules which could not be reasonably modeled.
;
_vrf_PLAT430_3                   
;
PROBLEM: Short Inter D...A Contact  O2     ..  O28     ..       2.59 Ang.  
RESPONSE: The positions of several water molecules (in particularly O29, O28,
and, to a somewhat lesser degree, O26 and O27) are only approximate, determined 
by voids in the crystal structure and extremely diffuse maxima of residual 
density.
;

# end Validation Reply Form

_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 H64 Co2 Mo3 N12 O29'
_chemical_formula_weight         1318.49

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      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

_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+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z'

_cell_length_a                   13.5465(3)
_cell_length_b                   11.6910(3)
_cell_length_c                   28.9847(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4590.37(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    11748
_cell_measurement_theta_min      3.7391
_cell_measurement_theta_max      35.0776

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.908
_exptl_crystal_F_000             2672
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_exptl_absorpt_coefficient_mu    1.607
_exptl_absorpt_correction_T_min  0.88039
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur Kappa CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 16.3426
_diffrn_reflns_number            23742
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         3.759
_diffrn_reflns_theta_max         26.994
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             9938
_reflns_number_gt                7811
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.962
_reflns_Friedel_fraction_max     0.997
_reflns_Friedel_fraction_full    0.997

_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion 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)+(0.0371P)²] 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_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.06(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         9938
_refine_ls_number_parameters     584
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0311
_refine_ls_wR_factor_ref         0.0688
_refine_ls_wR_factor_gt          0.0670
_refine_ls_goodness_of_fit_ref   0.913
_refine_ls_restrained_S_all      0.913
_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
O28 O 1.148(3) 0.3582(14) 0.6737(13) 0.59(4) Uani 1 1 d . . . . .
O29 O 0.920(4) 1.2163(16) 0.6463(9) 0.66(4) Uani 1 1 d . . . . .
Co1 Co 0.16994(6) 0.89501(6) 0.75779(3) 0.02299(17) Uani 1 1 d . . . . .
C1 C 0.1020(6) 0.9959(6) 0.8405(2) 0.0391(17) Uani 1 1 d . . . . .
H1A H 0.0942 1.0657 0.8582 0.047 Uiso 1 1 calc R U . . .
H1B H 0.1152 0.9335 0.8617 0.047 Uiso 1 1 calc R U . . .
C2 C 0.0092(5) 0.9717(7) 0.8131(3) 0.0434(19) Uani 1 1 d . . . . .
H2A H -0.0426 0.9446 0.8335 0.052 Uiso 1 1 calc R U . . .
H2B H -0.0136 1.0411 0.7981 0.052 Uiso 1 1 calc R U . . .
C3 C 0.2979(5) 0.9788(6) 0.6895(2) 0.0386(17) Uani 1 1 d . . . . .
H3A H 0.3619 1.0106 0.6818 0.046 Uiso 1 1 calc R U . . .
H3B H 0.2783 0.9267 0.6652 0.046 Uiso 1 1 calc R U . . .
C4 C 0.2241(5) 1.0714(6) 0.6946(2) 0.0384(17) Uani 1 1 d . . . . .
H4A H 0.2095 1.1056 0.6649 0.046 Uiso 1 1 calc R U . . .
H4B H 0.2486 1.1305 0.7151 0.046 Uiso 1 1 calc R U . . .
C5 C 0.1468(6) 0.6588(6) 0.7397(3) 0.0420(18) Uani 1 1 d . . . . .
H5A H 0.0836 0.6457 0.7545 0.050 Uiso 1 1 calc R U . . .
H5B H 0.1593 0.5963 0.7185 0.050 Uiso 1 1 calc R U . . .
C6 C 0.2262(6) 0.6650(6) 0.7747(3) 0.0410(18) Uani 1 1 d . . . . .
H6A H 0.2211 0.6009 0.7958 0.049 Uiso 1 1 calc R U . . .
H6B H 0.2903 0.6620 0.7599 0.049 Uiso 1 1 calc R U . . .
N1 N 0.1841(4) 1.0080(5) 0.80734(18) 0.0283(12) Uani 1 1 d . . . . .
H1C H 0.2414 0.9975 0.8218 0.034 Uiso 1 1 calc R U . . .
H1D H 0.1839 1.0782 0.7955 0.034 Uiso 1 1 calc R U . . .
N2 N 0.0324(4) 0.8833(5) 0.77799(18) 0.0292(12) Uani 1 1 d . . . . .
H2C H -0.0074 0.8918 0.7538 0.035 Uiso 1 1 calc R U . . .
H2D H 0.0219 0.8141 0.7899 0.035 Uiso 1 1 calc R U . . .
N3 N 0.3031(4) 0.9174(4) 0.73437(18) 0.0282(12) Uani 1 1 d . . . . .
H3C H 0.3383 0.9580 0.7545 0.034 Uiso 1 1 calc R U . . .
H3D H 0.3326 0.8500 0.7306 0.034 Uiso 1 1 calc R U . . .
N4 N 0.1340(4) 1.0167(4) 0.71433(18) 0.0290(13) Uani 1 1 d . . . . .
H4C H 0.0977 0.9874 0.6916 0.035 Uiso 1 1 calc R U . . .
H4D H 0.0980 1.0692 0.7288 0.035 Uiso 1 1 calc R U . . .
N5 N 0.1454(4) 0.7692(4) 0.71442(18) 0.0273(12) Uani 1 1 d . . . . .
H5C H 0.0871 0.7788 0.7009 0.033 Uiso 1 1 calc R U . . .
H5D H 0.1917 0.7689 0.6926 0.033 Uiso 1 1 calc R U . . .
N6 N 0.2152(4) 0.7740(5) 0.80027(19) 0.0316(13) Uani 1 1 d . . . . .
H6C H 0.2728 0.7938 0.8127 0.038 Uiso 1 1 calc R U . . .
H6D H 0.1716 0.7653 0.8230 0.038 Uiso 1 1 calc R U . . .
Co2 Co 0.20730(6) 0.38747(7) 0.97363(3) 0.02379(18) Uani 1 1 d . . . . .
C7 C 0.3687(5) 0.4606(6) 0.9184(3) 0.0396(17) Uani 1 1 d . . . . .
H7A H 0.4210 0.4336 0.8983 0.047 Uiso 1 1 calc R U . . .
H7B H 0.3909 0.5301 0.9334 0.047 Uiso 1 1 calc R U . . .
C8 C 0.2781(5) 0.4841(6) 0.8909(2) 0.0345(16) Uani 1 1 d . . . . .
H8A H 0.2868 0.5530 0.8728 0.041 Uiso 1 1 calc R U . . .
H8B H 0.2650 0.4209 0.8701 0.041 Uiso 1 1 calc R U . . .
C9 C 0.1564(6) 0.5673(7) 1.0339(3) 0.049(2) Uani 1 1 d . . . . .
H9A H 0.1707 0.6042 1.0631 0.059 Uiso 1 1 calc R U . . .
H9B H 0.1346 0.6253 1.0123 0.059 Uiso 1 1 calc R U . . .
C10 C 0.0796(6) 0.4816(7) 1.0400(3) 0.047(2) Uani 1 1 d . . . . .
H10A H 0.0960 0.4316 1.0656 0.056 Uiso 1 1 calc R U . . .
H10B H 0.0169 0.5183 1.0466 0.056 Uiso 1 1 calc R U . . .
C11 C 0.2320(6) 0.1549(6) 0.9952(3) 0.0455(19) Uani 1 1 d . . . . .
H11A H 0.2204 0.0931 1.0169 0.055 Uiso 1 1 calc R U . . .
H11B H 0.2963 0.1439 0.9812 0.055 Uiso 1 1 calc R U . . .
C12 C 0.1530(6) 0.1563(6) 0.9588(3) 0.047(2) Uani 1 1 d . . . . .
H12A H 0.1619 0.0924 0.9379 0.057 Uiso 1 1 calc R U . . .
H12B H 0.0885 0.1495 0.9731 0.057 Uiso 1 1 calc R U . . .
N7 N 0.3450(4) 0.3724(5) 0.95333(18) 0.0334(13) Uani 1 1 d . . . . .
H7C H 0.3851 0.3802 0.9775 0.040 Uiso 1 1 calc R U . . .
H7D H 0.3545 0.3032 0.9414 0.040 Uiso 1 1 calc R U . . .
N8 N 0.1945(4) 0.4985(5) 0.92345(18) 0.0329(13) Uani 1 1 d . . . . .
H8C H 0.1376 0.4877 0.9087 0.039 Uiso 1 1 calc R U . . .
H8D H 0.1947 0.5692 0.9349 0.039 Uiso 1 1 calc R U . . .
N9 N 0.2451(4) 0.5109(5) 1.01636(19) 0.0361(14) Uani 1 1 d . . . . .
H9C H 0.2796 0.4821 1.0397 0.043 Uiso 1 1 calc R U . . .
H9D H 0.2829 0.5616 1.0017 0.043 Uiso 1 1 calc R U . . .
N10 N 0.0732(4) 0.4165(5) 0.9977(2) 0.0382(14) Uani 1 1 d . . . . .
H10C H 0.0381 0.4552 0.9770 0.046 Uiso 1 1 calc R U . . .
H10D H 0.0428 0.3503 1.0031 0.046 Uiso 1 1 calc R U . . .
N11 N 0.2280(4) 0.2668(5) 1.01928(19) 0.0356(14) Uani 1 1 d . . . . .
H11C H 0.2843 0.2790 1.0344 0.043 Uiso 1 1 calc R U . . .
H11D H 0.1789 0.2670 1.0397 0.043 Uiso 1 1 calc R U . . .
N12 N 0.1598(4) 0.2643(5) 0.93341(19) 0.0341(14) Uani 1 1 d . . . . .
H12C H 0.1006 0.2827 0.9223 0.041 Uiso 1 1 calc R U . . .
H12D H 0.2009 0.2560 0.9097 0.041 Uiso 1 1 calc R U . . .
Mo1 Mo 0.90606(4) 0.37326(4) 0.86450(2) 0.02766(12) Uani 1 1 d . . . . .
Mo2 Mo 0.97519(3) 0.63293(4) 0.86496(2) 0.02572(12) Uani 1 1 d . . . . .
C13 C 0.9781(6) 0.3685(7) 0.7676(3) 0.049(2) Uani 1 1 d . . . . .
C14 C 1.0434(6) 0.2802(6) 0.7935(3) 0.0434(19) Uani 1 1 d . . . . .
C15 C 0.8405(5) 0.7284(6) 0.9358(3) 0.0367(17) Uani 1 1 d . . . . .
C16 C 0.9004(6) 0.6370(6) 0.9619(2) 0.0420(18) Uani 1 1 d . . . . .
O1 O 0.9078(3) 0.4084(4) 0.79117(16) 0.0349(11) Uani 1 1 d . . . . .
O2 O 0.9982(6) 0.3916(7) 0.7276(2) 0.094(3) Uani 1 1 d . . . . .
O3 O 1.0176(4) 0.2669(4) 0.83599(16) 0.0378(12) Uani 1 1 d . . . . .
O4 O 1.1081(4) 0.2283(5) 0.7749(2) 0.0587(15) Uani 1 1 d . . . . .
O5 O 0.8051(3) 0.2855(4) 0.85764(19) 0.0461(13) Uani 1 1 d . . . . .
O6 O 0.9511(3) 0.3342(4) 0.91779(17) 0.0396(11) Uani 1 1 d . . . . .
O7 O 1.0346(3) 0.4982(3) 0.85727(16) 0.0311(10) Uani 1 1 d . . . . .
O8 O 0.8491(3) 0.5118(3) 0.87133(16) 0.0302(10) Uani 1 1 d . . . . .
O9 O 1.0724(3) 0.7239(4) 0.87439(16) 0.0398(12) Uani 1 1 d . . . . .
O10 O 0.9326(3) 0.6745(4) 0.81108(15) 0.0356(11) Uani 1 1 d . . . . .
O11 O 0.8654(3) 0.7425(4) 0.89405(15) 0.0340(11) Uani 1 1 d . . . . .
O12 O 0.7757(4) 0.7830(4) 0.95649(18) 0.0518(14) Uani 1 1 d . . . . .
O13 O 0.9721(3) 0.5962(4) 0.93940(16) 0.0355(11) Uani 1 1 d . . . . .
O14 O 0.8759(6) 0.6059(6) 1.0001(2) 0.088(2) Uani 1 1 d . . . . .
Mo3 Mo 0.89049(5) 0.85774(6) 0.65394(2) 0.04351(17) Uani 1 1 d . . . . .
C17 C 1.0828(5) 0.8814(6) 0.6022(2) 0.0366(16) Uani 1 1 d . . . . .
C18 C 1.0162(5) 0.8106(7) 0.5703(2) 0.0419(19) Uani 1 1 d . . . . .
O15 O 1.0389(3) 0.9130(5) 0.63823(15) 0.0443(13) Uani 1 1 d . . . . .
O16 O 1.1697(4) 0.9003(5) 0.59291(17) 0.0507(14) Uani 1 1 d . . . . .
O17 O 0.9298(3) 0.7919(4) 0.58517(16) 0.0408(12) Uani 1 1 d . . . . .
O18 O 1.0494(4) 0.7749(5) 0.53277(17) 0.0572(16) Uani 1 1 d . . . . .
O19 O 0.9387(5) 0.7397(6) 0.6809(2) 0.074(2) Uani 1 1 d . . . . .
O20 O 0.7694(4) 0.8230(5) 0.64352(18) 0.0618(16) Uani 1 1 d . . . . .
O21 O 0.8903(5) 0.9549(6) 0.6995(2) 0.086(2) Uani 1 1 d . . . . .
O22 O 0.8689(6) 1.0080(6) 0.6051(3) 0.086(2) Uani 1 1 d D . . . .
H1O H 0.871(9) 0.984(8) 0.5738(11) 0.129 Uiso 1 1 d D U . . .
H2O H 0.901(7) 1.077(4) 0.597(3) 0.129 Uiso 1 1 d D U . . .
O23 O 1.0991(6) 0.8575(6) 0.9581(2) 0.094(2) Uani 1 1 d . . . . .
O24 O 1.0155(6) 1.0508(7) 0.5274(3) 0.115(3) Uani 1 1 d . . . . .
O25 O 1.1251(10) 1.2111(12) 0.5744(5) 0.188(5) Uani 1 1 d . . . . .
O27 O 0.8205(12) 1.1362(11) 0.7672(6) 0.237(8) Uani 1 1 d . . . . .
O26 O 0.5743(12) 0.9363(13) 0.6311(5) 0.226(7) 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 N3 1.945(5) . ?
Co1 N2 1.957(5) . ?
Co1 N1 1.961(5) . ?
Co1 N4 1.961(5) . ?
Co1 N5 1.963(5) . ?
Co1 N6 1.973(5) . ?
C1 N1 1.477(8) . ?
C1 C2 1.513(11) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N2 1.485(8) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.482(10) . ?
C3 N3 1.487(8) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N4 1.492(8) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.482(10) . ?
C5 N5 1.484(8) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 N6 1.481(9) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
N1 H1C 0.8900 . ?
N1 H1D 0.8900 . ?
N2 H2C 0.8900 . ?
N2 H2D 0.8900 . ?
N3 H3C 0.8900 . ?
N3 H3D 0.8900 . ?
N4 H4C 0.8900 . ?
N4 H4D 0.8900 . ?
N5 H5C 0.8900 . ?
N5 H5D 0.8900 . ?
N6 H6C 0.8900 . ?
N6 H6D 0.8900 . ?
Co2 N11 1.954(5) . ?
Co2 N8 1.957(5) . ?
Co2 N12 1.961(5) . ?
Co2 N7 1.964(6) . ?
Co2 N9 1.970(5) . ?
Co2 N10 1.976(6) . ?
C7 N7 1.480(8) . ?
C7 C8 1.488(10) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 N8 1.482(8) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.456(11) . ?
C9 N9 1.461(9) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N10 1.446(9) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N11 1.484(9) . ?
C11 C12 1.502(10) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 N12 1.465(9) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
N7 H7C 0.8900 . ?
N7 H7D 0.8900 . ?
N8 H8C 0.8900 . ?
N8 H8D 0.8900 . ?
N9 H9C 0.8900 . ?
N9 H9D 0.8900 . ?
N10 H10C 0.8900 . ?
N10 H10D 0.8900 . ?
N11 H11C 0.8900 . ?
N11 H11D 0.8900 . ?
N12 H12C 0.8900 . ?
N12 H12D 0.8900 . ?
Mo1 O5 1.721(5) . ?
Mo1 O6 1.722(5) . ?
Mo1 O8 1.805(4) . ?
Mo1 O3 2.124(5) . ?
Mo1 O1 2.165(5) . ?
Mo1 O7 2.283(4) . ?
Mo1 Mo2 3.1771(7) . ?
Mo2 O9 1.714(5) . ?
Mo2 O10 1.734(4) . ?
Mo2 O7 1.783(4) . ?
Mo2 O11 2.137(4) . ?
Mo2 O13 2.200(5) . ?
Mo2 O8 2.227(4) . ?
C13 O2 1.222(10) . ?
C13 O1 1.262(9) . ?
C13 C14 1.552(10) . ?
C14 O4 1.195(9) . ?
C14 O3 1.289(9) . ?
C15 O12 1.241(8) . ?
C15 O11 1.267(8) . ?
C15 C16 1.540(10) . ?
C16 O14 1.213(9) . ?
C16 O13 1.263(8) . ?
Mo3 O19 1.716(6) . ?
Mo3 O20 1.717(5) . ?
Mo3 O21 1.742(6) . ?
Mo3 O15 2.160(5) . ?
Mo3 O17 2.202(5) . ?
Mo3 O22 2.274(7) . ?
C17 O16 1.228(8) . ?
C17 O15 1.258(8) . ?
C17 C18 1.534(9) . ?
C18 O18 1.248(8) . ?
C18 O17 1.266(8) . ?
O22 H1O 0.950(3) . ?
O22 H2O 0.950(3) . ?

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
N3 Co1 N2 175.2(2) . . ?
N3 Co1 N1 94.3(2) . . ?
N2 Co1 N1 85.5(2) . . ?
N3 Co1 N4 84.8(2) . . ?
N2 Co1 N4 90.4(2) . . ?
N1 Co1 N4 90.4(2) . . ?
N3 Co1 N5 92.0(2) . . ?
N2 Co1 N5 88.7(2) . . ?
N1 Co1 N5 172.0(2) . . ?
N4 Co1 N5 95.2(2) . . ?
N3 Co1 N6 91.5(2) . . ?
N2 Co1 N6 93.3(2) . . ?
N1 Co1 N6 89.7(2) . . ?
N4 Co1 N6 176.2(2) . . ?
N5 Co1 N6 85.1(2) . . ?
N1 C1 C2 107.6(5) . . ?
N1 C1 H1A 110.2 . . ?
C2 C1 H1A 110.2 . . ?
N1 C1 H1B 110.2 . . ?
C2 C1 H1B 110.2 . . ?
H1A C1 H1B 108.5 . . ?
N2 C2 C1 108.2(5) . . ?
N2 C2 H2A 110.0 . . ?
C1 C2 H2A 110.1 . . ?
N2 C2 H2B 110.1 . . ?
C1 C2 H2B 110.1 . . ?
H2A C2 H2B 108.4 . . ?
C4 C3 N3 107.3(5) . . ?
C4 C3 H3A 110.2 . . ?
N3 C3 H3A 110.2 . . ?
C4 C3 H3B 110.2 . . ?
N3 C3 H3B 110.2 . . ?
H3A C3 H3B 108.5 . . ?
C3 C4 N4 106.0(5) . . ?
C3 C4 H4A 110.5 . . ?
N4 C4 H4A 110.5 . . ?
C3 C4 H4B 110.5 . . ?
N4 C4 H4B 110.5 . . ?
H4A C4 H4B 108.7 . . ?
C6 C5 N5 107.7(6) . . ?
C6 C5 H5A 110.2 . . ?
N5 C5 H5A 110.2 . . ?
C6 C5 H5B 110.2 . . ?
N5 C5 H5B 110.2 . . ?
H5A C5 H5B 108.5 . . ?
N6 C6 C5 108.2(6) . . ?
N6 C6 H6A 110.1 . . ?
C5 C6 H6A 110.1 . . ?
N6 C6 H6B 110.1 . . ?
C5 C6 H6B 110.1 . . ?
H6A C6 H6B 108.4 . . ?
C1 N1 Co1 109.8(4) . . ?
C1 N1 H1C 109.7 . . ?
Co1 N1 H1C 109.7 . . ?
C1 N1 H1D 109.7 . . ?
Co1 N1 H1D 109.7 . . ?
H1C N1 H1D 108.2 . . ?
C2 N2 Co1 111.0(4) . . ?
C2 N2 H2C 109.4 . . ?
Co1 N2 H2C 109.4 . . ?
C2 N2 H2D 109.4 . . ?
Co1 N2 H2D 109.4 . . ?
H2C N2 H2D 108.0 . . ?
C3 N3 Co1 109.0(4) . . ?
C3 N3 H3C 109.9 . . ?
Co1 N3 H3C 109.9 . . ?
C3 N3 H3D 109.9 . . ?
Co1 N3 H3D 109.9 . . ?
H3C N3 H3D 108.3 . . ?
C4 N4 Co1 110.8(4) . . ?
C4 N4 H4C 109.5 . . ?
Co1 N4 H4C 109.5 . . ?
C4 N4 H4D 109.5 . . ?
Co1 N4 H4D 109.5 . . ?
H4C N4 H4D 108.1 . . ?
C5 N5 Co1 109.5(4) . . ?
C5 N5 H5C 109.8 . . ?
Co1 N5 H5C 109.8 . . ?
C5 N5 H5D 109.8 . . ?
Co1 N5 H5D 109.8 . . ?
H5C N5 H5D 108.2 . . ?
C6 N6 Co1 109.7(4) . . ?
C6 N6 H6C 109.7 . . ?
Co1 N6 H6C 109.7 . . ?
C6 N6 H6D 109.7 . . ?
Co1 N6 H6D 109.7 . . ?
H6C N6 H6D 108.2 . . ?
N11 Co2 N8 174.0(2) . . ?
N11 Co2 N12 85.4(2) . . ?
N8 Co2 N12 90.9(2) . . ?
N11 Co2 N7 90.1(2) . . ?
N8 Co2 N7 85.5(2) . . ?
N12 Co2 N7 93.9(2) . . ?
N11 Co2 N9 93.8(2) . . ?
N8 Co2 N9 90.2(2) . . ?
N12 Co2 N9 175.6(2) . . ?
N7 Co2 N9 90.4(2) . . ?
N11 Co2 N10 90.9(2) . . ?
N8 Co2 N10 93.9(2) . . ?
N12 Co2 N10 92.0(2) . . ?
N7 Co2 N10 174.1(2) . . ?
N9 Co2 N10 83.7(2) . . ?
N7 C7 C8 108.4(5) . . ?
N7 C7 H7A 110.0 . . ?
C8 C7 H7A 110.0 . . ?
N7 C7 H7B 110.0 . . ?
C8 C7 H7B 110.0 . . ?
H7A C7 H7B 108.4 . . ?
N8 C8 C7 108.1(5) . . ?
N8 C8 H8A 110.1 . . ?
C7 C8 H8A 110.1 . . ?
N8 C8 H8B 110.1 . . ?
C7 C8 H8B 110.1 . . ?
H8A C8 H8B 108.4 . . ?
C10 C9 N9 108.6(6) . . ?
C10 C9 H9A 110.0 . . ?
N9 C9 H9A 110.0 . . ?
C10 C9 H9B 110.0 . . ?
N9 C9 H9B 110.0 . . ?
H9A C9 H9B 108.3 . . ?
N10 C10 C9 107.6(6) . . ?
N10 C10 H10A 110.2 . . ?
C9 C10 H10A 110.2 . . ?
N10 C10 H10B 110.2 . . ?
C9 C10 H10B 110.2 . . ?
H10A C10 H10B 108.5 . . ?
N11 C11 C12 107.1(6) . . ?
N11 C11 H11A 110.3 . . ?
C12 C11 H11A 110.3 . . ?
N11 C11 H11B 110.3 . . ?
C12 C11 H11B 110.3 . . ?
H11A C11 H11B 108.5 . . ?
N12 C12 C11 108.5(6) . . ?
N12 C12 H12A 110.0 . . ?
C11 C12 H12A 110.0 . . ?
N12 C12 H12B 110.0 . . ?
C11 C12 H12B 110.0 . . ?
H12A C12 H12B 108.4 . . ?
C7 N7 Co2 110.4(4) . . ?
C7 N7 H7C 109.6 . . ?
Co2 N7 H7C 109.6 . . ?
C7 N7 H7D 109.6 . . ?
Co2 N7 H7D 109.6 . . ?
H7C N7 H7D 108.1 . . ?
C8 N8 Co2 109.2(4) . . ?
C8 N8 H8C 109.8 . . ?
Co2 N8 H8C 109.8 . . ?
C8 N8 H8D 109.8 . . ?
Co2 N8 H8D 109.8 . . ?
H8C N8 H8D 108.3 . . ?
C9 N9 Co2 109.6(5) . . ?
C9 N9 H9C 109.8 . . ?
Co2 N9 H9C 109.8 . . ?
C9 N9 H9D 109.8 . . ?
Co2 N9 H9D 109.8 . . ?
H9C N9 H9D 108.2 . . ?
C10 N10 Co2 109.6(5) . . ?
C10 N10 H10C 109.8 . . ?
Co2 N10 H10C 109.8 . . ?
C10 N10 H10D 109.8 . . ?
Co2 N10 H10D 109.8 . . ?
H10C N10 H10D 108.2 . . ?
C11 N11 Co2 108.9(4) . . ?
C11 N11 H11C 109.9 . . ?
Co2 N11 H11C 109.9 . . ?
C11 N11 H11D 109.9 . . ?
Co2 N11 H11D 109.9 . . ?
H11C N11 H11D 108.3 . . ?
C12 N12 Co2 110.7(4) . . ?
C12 N12 H12C 109.5 . . ?
Co2 N12 H12C 109.5 . . ?
C12 N12 H12D 109.5 . . ?
Co2 N12 H12D 109.5 . . ?
H12C N12 H12D 108.1 . . ?
O5 Mo1 O6 103.1(2) . . ?
O5 Mo1 O8 102.0(2) . . ?
O6 Mo1 O8 106.9(2) . . ?
O5 Mo1 O3 99.9(2) . . ?
O6 Mo1 O3 86.7(2) . . ?
O8 Mo1 O3 150.70(19) . . ?
O5 Mo1 O1 90.5(2) . . ?
O6 Mo1 O1 158.0(2) . . ?
O8 Mo1 O1 86.66(19) . . ?
O3 Mo1 O1 73.84(17) . . ?
O5 Mo1 O7 167.7(2) . . ?
O6 Mo1 O7 89.0(2) . . ?
O8 Mo1 O7 76.25(16) . . ?
O3 Mo1 O7 78.23(17) . . ?
O1 Mo1 O7 77.30(17) . . ?
O5 Mo1 Mo2 143.53(16) . . ?
O6 Mo1 Mo2 98.34(16) . . ?
O8 Mo1 Mo2 42.97(12) . . ?
O3 Mo1 Mo2 110.56(13) . . ?
O1 Mo1 Mo2 79.59(12) . . ?
O7 Mo1 Mo2 33.29(10) . . ?
O9 Mo2 O10 103.0(2) . . ?
O9 Mo2 O7 102.8(2) . . ?
O10 Mo2 O7 106.6(2) . . ?
O9 Mo2 O11 95.7(2) . . ?
O10 Mo2 O11 87.5(2) . . ?
O7 Mo2 O11 153.32(19) . . ?
O9 Mo2 O13 88.8(2) . . ?
O10 Mo2 O13 158.6(2) . . ?
O7 Mo2 O13 87.63(19) . . ?
O11 Mo2 O13 73.55(17) . . ?
O9 Mo2 O8 166.0(2) . . ?
O10 Mo2 O8 89.9(2) . . ?
O7 Mo2 O8 78.17(16) . . ?
O11 Mo2 O8 79.31(17) . . ?
O13 Mo2 O8 77.27(17) . . ?
O9 Mo2 Mo1 145.07(16) . . ?
O10 Mo2 Mo1 99.57(16) . . ?
O7 Mo2 Mo1 44.64(13) . . ?
O11 Mo2 Mo1 111.69(13) . . ?
O13 Mo2 Mo1 79.15(12) . . ?
O8 Mo2 Mo1 33.54(10) . . ?
O2 C13 O1 126.9(7) . . ?
O2 C13 C14 118.6(8) . . ?
O1 C13 C14 114.5(7) . . ?
O4 C14 O3 124.6(7) . . ?
O4 C14 C13 122.5(7) . . ?
O3 C14 C13 112.8(7) . . ?
O12 C15 O11 125.6(7) . . ?
O12 C15 C16 119.5(7) . . ?
O11 C15 C16 114.8(6) . . ?
O14 C16 O13 124.7(7) . . ?
O14 C16 C15 120.8(7) . . ?
O13 C16 C15 114.4(6) . . ?
C13 O1 Mo1 118.0(4) . . ?
C14 O3 Mo1 119.6(4) . . ?
Mo2 O7 Mo1 102.08(17) . . ?
Mo1 O8 Mo2 103.49(18) . . ?
C15 O11 Mo2 118.9(4) . . ?
C16 O13 Mo2 116.6(4) . . ?
O19 Mo3 O20 104.7(3) . . ?
O19 Mo3 O21 100.3(4) . . ?
O20 Mo3 O21 106.6(3) . . ?
O19 Mo3 O15 89.0(3) . . ?
O20 Mo3 O15 157.4(2) . . ?
O21 Mo3 O15 88.1(2) . . ?
O19 Mo3 O17 92.3(3) . . ?
O20 Mo3 O17 89.4(2) . . ?
O21 Mo3 O17 156.2(3) . . ?
O15 Mo3 O17 71.87(17) . . ?
O19 Mo3 O22 162.6(3) . . ?
O20 Mo3 O22 87.2(3) . . ?
O21 Mo3 O22 88.2(3) . . ?
O15 Mo3 O22 76.0(2) . . ?
O17 Mo3 O22 74.8(3) . . ?
O16 C17 O15 125.6(6) . . ?
O16 C17 C18 122.0(6) . . ?
O15 C17 C18 112.4(6) . . ?
O18 C18 O17 124.9(7) . . ?
O18 C18 C17 119.5(6) . . ?
O17 C18 C17 115.5(6) . . ?
C17 O15 Mo3 121.8(4) . . ?
C18 O17 Mo3 118.1(4) . . ?
Mo3 O22 H1O 111(6) . . ?
Mo3 O22 H2O 139(6) . . ?
H1O O22 H2O 90.5(6) . . ?

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
N1 C1 C2 N2 45.6(8) . . . . ?
N3 C3 C4 N4 -50.3(7) . . . . ?
N5 C5 C6 N6 48.6(7) . . . . ?
C2 C1 N1 Co1 -39.4(6) . . . . ?
C1 C2 N2 Co1 -31.2(7) . . . . ?
C4 C3 N3 Co1 43.0(6) . . . . ?
C3 C4 N4 Co1 35.5(6) . . . . ?
C6 C5 N5 Co1 -38.7(6) . . . . ?
C5 C6 N6 Co1 -36.1(7) . . . . ?
N7 C7 C8 N8 46.6(7) . . . . ?
N9 C9 C10 N10 -50.1(8) . . . . ?
N11 C11 C12 N12 47.3(8) . . . . ?
C8 C7 N7 Co2 -32.5(7) . . . . ?
C7 C8 N8 Co2 -39.3(6) . . . . ?
C10 C9 N9 Co2 36.2(7) . . . . ?
C9 C10 N10 Co2 40.4(7) . . . . ?
C12 C11 N11 Co2 -41.2(7) . . . . ?
C11 C12 N12 Co2 -31.6(7) . . . . ?
O2 C13 C14 O4 -5.3(13) . . . . ?
O1 C13 C14 O4 174.2(7) . . . . ?
O2 C13 C14 O3 177.0(8) . . . . ?
O1 C13 C14 O3 -3.5(10) . . . . ?
O12 C15 C16 O14 10.9(11) . . . . ?
O11 C15 C16 O14 -170.9(8) . . . . ?
O12 C15 C16 O13 -172.0(6) . . . . ?
O11 C15 C16 O13 6.2(9) . . . . ?
O2 C13 O1 Mo1 -169.6(8) . . . . ?
C14 C13 O1 Mo1 10.9(9) . . . . ?
O4 C14 O3 Mo1 176.5(6) . . . . ?
C13 C14 O3 Mo1 -5.8(8) . . . . ?
O9 Mo2 O7 Mo1 165.2(2) . . . . ?
O10 Mo2 O7 Mo1 -86.9(2) . . . . ?
O11 Mo2 O7 Mo1 32.4(5) . . . . ?
O13 Mo2 O7 Mo1 76.9(2) . . . . ?
O8 Mo2 O7 Mo1 -0.57(19) . . . . ?
O5 Mo1 O8 Mo2 -168.1(2) . . . . ?
O6 Mo1 O8 Mo2 84.0(2) . . . . ?
O3 Mo1 O8 Mo2 -30.7(5) . . . . ?
O1 Mo1 O8 Mo2 -78.3(2) . . . . ?
O7 Mo1 O8 Mo2 -0.57(19) . . . . ?
O12 C15 O11 Mo2 -177.3(5) . . . . ?
C16 C15 O11 Mo2 4.6(8) . . . . ?
O14 C16 O13 Mo2 163.5(7) . . . . ?
C15 C16 O13 Mo2 -13.5(8) . . . . ?
O16 C17 C18 O18 -3.1(12) . . . . ?
O15 C17 C18 O18 178.8(7) . . . . ?
O16 C17 C18 O17 176.1(7) . . . . ?
O15 C17 C18 O17 -2.0(10) . . . . ?
O16 C17 O15 Mo3 -172.9(6) . . . . ?
C18 C17 O15 Mo3 5.1(8) . . . . ?
O18 C18 O17 Mo3 177.4(6) . . . . ?
C17 C18 O17 Mo3 -1.8(9) . . . . ?

_refine_diff_density_max         0.635
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.076

####################################################################### 
# 
# 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_4a
_database_code_depnum_ccdc_archive 'CCDC 1579657'
_audit_update_record             
;
2017-10-12 deposited with the CCDC.
2018-02-16 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT306_shelx               
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O13 Check 
RESPONSE: Due to weak diffraction of the sample (thin plate) and a large 
electron density of the oxomolybdenum anion, as well as large displacement 
parameters of solvent (water) oxygen atoms, it was not possible to reasonably 
locate hydrogen atoms on two independant water molecules from the electron 
difference map. As there is also no clear hydrogen bonding scheme which would 
allow a speculative positioning of the hydrogen, we have decided not to include 
these hydrogen atoms in the model. 
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H4 Mo2 O15, 2(C6 H16 Co N4 O4), 4(H2 O)'
_chemical_formula_sum            'C16 H44 Co2 Mo2 N8 O27'
_chemical_formula_weight         1090.33

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      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                   12.8719(10)
_cell_length_b                   10.4734(7)
_cell_length_c                   14.5744(10)
_cell_angle_alpha                90
_cell_angle_beta                 112.997(8)
_cell_angle_gamma                90
_cell_volume                     1808.7(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    9129
_cell_measurement_theta_min      3.8535
_cell_measurement_theta_max      36.6428

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.002
_exptl_crystal_F_000             1100
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.79
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    1.688
_exptl_absorpt_correction_T_min  0.35855
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur Kappa CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 16.3426
_diffrn_reflns_number            19135
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_av_R_equivalents  0.0787
_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       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.891
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             3921
_reflns_number_gt                2800
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0780P)²] 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         3921
_refine_ls_number_parameters     256
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0462
_refine_ls_wR_factor_ref         0.1248
_refine_ls_wR_factor_gt          0.1202
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_restrained_S_all      0.983
_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 0.93079(3) 0.15081(5) 0.93904(3) 0.03516(16) Uani 1 1 d . . . . .
Co1 Co 0.97590(4) 0.24770(5) 0.42089(4) 0.02292(16) Uani 1 1 d . . . . .
C1 C 0.8717(4) 0.2555(5) 0.7377(4) 0.0380(12) Uani 1 1 d . . . . .
O2 O 1.0285(4) 0.2597(5) 1.0041(3) 0.0705(14) Uani 1 1 d . . . . .
O1 O 0.8243(3) 0.1722(5) 0.9793(3) 0.0561(12) Uani 1 1 d . . . . .
O10 O 1.0864(3) 0.1225(3) 0.4910(2) 0.0333(7) Uani 1 1 d . . . . .
O11 O 1.2277(3) 0.0928(3) 0.6378(3) 0.0417(9) Uani 1 1 d . . . . .
O9 O 1.0450(2) 0.3490(3) 0.5381(2) 0.0275(7) Uani 1 1 d . . . . .
O8 O 0.8251(4) 0.3124(5) 0.6596(3) 0.0677(14) Uani 1 1 d . . . . .
O12 O 1.1828(3) 0.3387(3) 0.6882(2) 0.0422(9) Uani 1 1 d . . . . .
C4 C 1.1515(4) 0.1578(4) 0.5783(3) 0.0288(10) Uani 1 1 d . . . . .
O5 O 0.8497(3) 0.2662(3) 0.8160(2) 0.0399(8) Uani 1 1 d . . . . .
O4 O 0.8081(3) 0.0099(4) 0.8256(3) 0.0527(10) Uani 1 1 d D . . . .
N3 N 0.9191(3) 0.1389(4) 0.3051(3) 0.0323(9) Uani 1 1 d . . . . .
H3A H 0.9406 0.0588 0.3229 0.039 Uiso 1 1 calc R U . . .
H3B H 0.8440 0.1411 0.2792 0.039 Uiso 1 1 calc R U . . .
O7 O 0.9935(3) 0.1331(4) 0.6810(3) 0.0417(9) Uani 1 1 d . . . . .
O6 O 1.0089(3) 0.1123(3) 0.8374(2) 0.0352(8) Uani 1 1 d . . . . .
N2 N 0.8637(3) 0.3790(4) 0.3626(3) 0.0294(8) Uani 1 1 d . . . . .
H2A H 0.8970 0.4547 0.3681 0.035 Uiso 1 1 calc R U . . .
H2B H 0.8250 0.3628 0.2982 0.035 Uiso 1 1 calc R U . . .
N1 N 0.8690(3) 0.1780(3) 0.4725(3) 0.0289(8) Uani 1 1 d . . . . .
H1A H 0.8590 0.0951 0.4584 0.035 Uiso 1 1 calc R U . . .
H1B H 0.8965 0.1868 0.5385 0.035 Uiso 1 1 calc R U . . .
N4 N 1.0764(3) 0.3169(4) 0.3614(3) 0.0353(9) Uani 1 1 d . . . . .
H4A H 1.0510 0.3922 0.3332 0.042 Uiso 1 1 calc R U . . .
H4B H 1.1455 0.3277 0.4080 0.042 Uiso 1 1 calc R U . . .
C3 C 1.1263(4) 0.2926(4) 0.6072(3) 0.0281(10) Uani 1 1 d . . . . .
C7 C 0.9612(5) 0.1804(5) 0.2301(3) 0.0418(13) Uani 1 1 d . . . . .
H7A H 0.9150 0.2493 0.1903 0.050 Uiso 1 1 calc R U . . .
H7B H 0.9596 0.1102 0.1862 0.050 Uiso 1 1 calc R U . . .
C5 C 0.7605(4) 0.2445(5) 0.4282(4) 0.0353(11) Uani 1 1 d . . . . .
H5A H 0.7193 0.2378 0.4713 0.042 Uiso 1 1 calc R U . . .
H5B H 0.7150 0.2075 0.3639 0.042 Uiso 1 1 calc R U . . .
O3 O 1.0000 0.0000 1.0000 0.0663(19) Uani 1 2 d S . P . .
C2 C 0.9670(4) 0.1598(5) 0.7501(3) 0.0307(10) Uani 1 1 d . . . . .
C8 C 1.0793(5) 0.2249(6) 0.2855(4) 0.0475(14) Uani 1 1 d . . . . .
H8A H 1.1278 0.1533 0.3172 0.057 Uiso 1 1 calc R U . . .
H8B H 1.1079 0.2657 0.2404 0.057 Uiso 1 1 calc R U . . .
C6 C 0.7863(4) 0.3804(5) 0.4163(4) 0.0373(12) Uani 1 1 d . . . . .
H6A H 0.8223 0.4209 0.4809 0.045 Uiso 1 1 calc R U . . .
H6B H 0.7176 0.4266 0.3782 0.045 Uiso 1 1 calc R U . . .
H1O H 0.750(3) 0.013(5) 0.7607(15) 0.056 Uiso 1 1 d D U . . .
H2O H 0.771(3) -0.058(3) 0.843(3) 0.056 Uiso 1 1 d D U . . .
O14 O 0.6753(7) 0.0430(6) 0.6293(4) 0.146(3) Uani 1 1 d . . . . .
O13 O 1.0390(5) 0.4777(7) 0.7908(7) 0.132(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 O2 1.688(4) . ?
Mo1 O1 1.703(4) . ?
Mo1 O3 1.8599(5) . ?
Mo1 O5 2.075(3) . ?
Mo1 O6 2.129(3) . ?
Mo1 O4 2.316(4) . ?
Co1 O9 1.910(3) . ?
Co1 O10 1.911(3) . ?
Co1 N3 1.928(4) . ?
Co1 N2 1.934(4) . ?
Co1 N1 1.950(4) . ?
Co1 N4 1.957(4) . ?
C1 O8 1.216(6) . ?
C1 O5 1.283(6) . ?
C1 C2 1.539(7) . ?
O10 C4 1.274(5) . ?
O11 C4 1.229(5) . ?
O9 C3 1.279(5) . ?
O12 C3 1.219(5) . ?
C4 C3 1.543(6) . ?
N3 C7 1.463(7) . ?
O7 C2 1.215(6) . ?
O6 C2 1.273(5) . ?
N2 C6 1.488(6) . ?
N1 C5 1.465(6) . ?
N4 C8 1.478(7) . ?
C7 C8 1.490(8) . ?
C5 C6 1.486(7) . ?
O3 Mo1 1.8599(5) 3_757 ?

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 O1 103.9(2) . . ?
O2 Mo1 O3 101.12(19) . . ?
O1 Mo1 O3 104.29(15) . . ?
O2 Mo1 O5 96.0(2) . . ?
O1 Mo1 O5 91.16(17) . . ?
O3 Mo1 O5 153.26(10) . . ?
O2 Mo1 O6 93.92(19) . . ?
O1 Mo1 O6 157.95(15) . . ?
O3 Mo1 O6 84.46(9) . . ?
O5 Mo1 O6 73.95(13) . . ?
O2 Mo1 O4 169.11(19) . . ?
O1 Mo1 O4 85.04(18) . . ?
O3 Mo1 O4 82.26(11) . . ?
O5 Mo1 O4 77.41(15) . . ?
O6 Mo1 O4 76.01(14) . . ?
O9 Co1 O10 85.02(13) . . ?
O9 Co1 N3 174.93(15) . . ?
O10 Co1 N3 90.65(15) . . ?
O9 Co1 N2 90.28(14) . . ?
O10 Co1 N2 174.27(15) . . ?
N3 Co1 N2 94.19(16) . . ?
O9 Co1 N1 90.87(15) . . ?
O10 Co1 N1 91.55(15) . . ?
N3 Co1 N1 91.91(17) . . ?
N2 Co1 N1 85.23(16) . . ?
O9 Co1 N4 91.89(15) . . ?
O10 Co1 N4 90.46(16) . . ?
N3 Co1 N4 85.48(17) . . ?
N2 Co1 N4 92.97(17) . . ?
N1 Co1 N4 176.71(16) . . ?
O8 C1 O5 126.1(5) . . ?
O8 C1 C2 120.5(5) . . ?
O5 C1 C2 113.3(4) . . ?
C4 O10 Co1 113.4(3) . . ?
C3 O9 Co1 113.5(3) . . ?
O11 C4 O10 125.1(4) . . ?
O11 C4 C3 120.6(4) . . ?
O10 C4 C3 114.3(4) . . ?
C1 O5 Mo1 120.4(3) . . ?
C7 N3 Co1 110.7(3) . . ?
C2 O6 Mo1 119.4(3) . . ?
C6 N2 Co1 108.3(3) . . ?
C5 N1 Co1 110.3(3) . . ?
C8 N4 Co1 107.7(3) . . ?
O12 C3 O9 125.1(4) . . ?
O12 C3 C4 121.1(4) . . ?
O9 C3 C4 113.8(3) . . ?
N3 C7 C8 106.6(4) . . ?
N1 C5 C6 106.8(4) . . ?
Mo1 O3 Mo1 180.0 . 3_757 ?
O7 C2 O6 126.3(5) . . ?
O7 C2 C1 121.5(4) . . ?
O6 C2 C1 112.2(4) . . ?
N4 C8 C7 106.9(4) . . ?
C5 C6 N2 106.1(4) . . ?

_refine_diff_density_max         1.493
_refine_diff_density_min         -0.956
_refine_diff_density_rms         0.130

####################################################################### 
# 
# 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_4c
_database_code_depnum_ccdc_archive 'CCDC 1579659'
_audit_update_record             
;
2017-10-12 deposited with the CCDC.
2018-02-16 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT417_4c                  
;
PROBLEM: Short Inter D-H..H-D       H8W    ..  H12W    ..       2.09 Ang.  
RESPONSE: As the structure contains several heavy atoms (cobalt and molybdenum),
almost no hydrogen atoms of the 7 water molecules independant by symmetry could 
be located fom the electron difference map. 12 out of 14 hydrogen atoms 
situated on the water molecules were modeled with standard O-H bond lengths and 
H-O-H angles, with orientations of O-H bonds adjusted in order to make as 
sensible hydrogen bond network as possible. This has led to several relatibely 
short non-bonded H atoms in several cases of water molecules connected by a 
O-H...O hydrogen bond where the donor hydrogen appears relatively close to the 
hydrogen atoms of the acceptor molecule. This could not be avoided by looser 
restrainta on molecular geometry, as such models failed to satisfactorily 
converge.
;
_vrf_PLAT041_4c                  
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check
RESPONSE: Two hydrogen atoms on water molecules could not be unequivocally 
located from the hydrogen bonding pattern and are therefore missing from the 
structural model.
;
# end Validation Reply Form

_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            'C14 H48 Co2 Mo N8 O23'
_chemical_formula_weight         910.40

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                   10.0883(12)
_cell_length_b                   11.9280(13)
_cell_length_c                   15.268(4)
_cell_angle_alpha                67.802(7)
_cell_angle_beta                 86.402(2)
_cell_angle_gamma                75.040(10)
_cell_volume                     1642.2(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    5156
_cell_measurement_theta_min      3.7934
_cell_measurement_theta_max      37.4207

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.841
_exptl_crystal_F_000             936
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.73
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    1.475
_exptl_absorpt_correction_T_min  0.56096
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur Kappa CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 16.3426
_diffrn_reflns_number            11506
_diffrn_reflns_av_unetI/netI     0.0785
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.815
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measured_fraction_theta_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_point_group_measured_fraction_full 0.980
_reflns_number_total             6948
_reflns_number_gt                4549
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0807P)²] 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         6948
_refine_ls_number_parameters     475
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0571
_refine_ls_wR_factor_ref         0.1378
_refine_ls_wR_factor_gt          0.1320
_refine_ls_goodness_of_fit_ref   0.911
_refine_ls_restrained_S_all      0.909
_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
O17 O 0.7506(4) 0.5758(4) 0.4580(3) 0.0611(11) Uani 1 1 d D . . . .
H1W H 0.674(3) 0.575(5) 0.497(3) 0.092 Uiso 1 1 d D U . . .
H2W H 0.794(5) 0.493(2) 0.498(4) 0.092 Uiso 1 1 d D U . . .
O18 O 0.7647(4) 0.7755(4) 0.5147(3) 0.0593(11) Uani 1 1 d D . . . .
H3W H 0.854(2) 0.786(5) 0.499(5) 0.089 Uiso 1 1 d D U . . .
H4W H 0.783(5) 0.707(3) 0.494(4) 0.089 Uiso 1 1 d D U . . .
O22 O 0.3818(4) 0.6904(4) 0.9102(3) 0.0670(12) Uani 1 1 d D . . . .
H11W H 0.376(6) 0.608(2) 0.947(4) 0.100 Uiso 1 1 d D U . . .
H12W H 0.463(4) 0.678(5) 0.945(4) 0.100 Uiso 1 1 d D U . . .
O20 O 0.5134(4) 0.6816(5) 0.7504(3) 0.0667(12) Uani 1 1 d D . . . .
H7W H 0.477(6) 0.619(4) 0.744(4) 0.100 Uiso 1 1 d D U . . .
H8W H 0.472(6) 0.671(5) 0.810(2) 0.100 Uiso 1 1 d D U . . .
O19 O 0.4700(5) 0.8776(4) 0.5631(3) 0.0667(12) Uani 1 1 d D . . . .
H5W H 0.484(8) 0.814(5) 0.625(2) 0.100 Uiso 1 1 d D U . . .
O21 O 0.0979(6) 0.8306(6) 0.0616(5) 0.1051(19) Uani 1 1 d D . . . .
H9W H 0.112(9) 0.912(3) 0.032(7) 0.158 Uiso 1 1 d D U . . .
O23 O -0.0435(5) 0.8405(7) 0.2123(5) 0.109(2) Uani 1 1 d D . . . .
H13W H 0.009(6) 0.846(9) 0.157(2) 0.164 Uiso 1 1 d D U . . .
H14W H 0.034(4) 0.785(7) 0.252(4) 0.164 Uiso 1 1 d D U . . .
O16 O 0.0969(4) 0.6846(4) 0.4221(3) 0.0547(10) Uani 1 1 d . . . . .
Mo1 Mo 0.13094(4) 0.81490(4) 0.42824(3) 0.03563(15) Uani 1 1 d . . . . .
Co1 Co 0.43615(6) 0.17840(5) 0.81227(4) 0.02810(17) Uani 1 1 d . . . . .
O1 O 0.3743(3) 0.0518(3) 0.9137(2) 0.0332(8) Uani 1 1 d . . . . .
O12 O 0.3252(3) 0.5810(3) 0.6938(2) 0.0387(8) Uani 1 1 d . . . . .
O2 O 0.2872(3) 0.2944(3) 0.8401(2) 0.0306(7) Uani 1 1 d . . . . .
O10 O 0.3519(3) 0.7257(3) 0.4514(2) 0.0373(8) Uani 1 1 d . . . . .
O9 O 0.1727(3) 0.7176(3) 0.5804(2) 0.0381(8) Uani 1 1 d . . . . .
O15 O -0.0276(3) 0.8982(3) 0.4536(3) 0.0426(9) Uani 1 1 d . . . . .
C13 C 0.4004(5) 0.6537(4) 0.5342(3) 0.0322(11) Uani 1 1 d . . . . .
N2 N 0.5537(4) 0.1970(3) 0.8987(3) 0.0334(9) Uani 1 1 d . . . . .
H2A H 0.5122 0.1903 0.9530 0.040 Uiso 1 1 calc R U . . .
H2B H 0.6317 0.1369 0.9111 0.040 Uiso 1 1 calc R U . . .
N3 N 0.5770(4) 0.0514(3) 0.7860(3) 0.0319(9) Uani 1 1 d . . . . .
H3A H 0.6537 0.0770 0.7710 0.038 Uiso 1 1 calc R U . . .
H3B H 0.5952 -0.0189 0.8372 0.038 Uiso 1 1 calc R U . . .
N4 N 0.3175(4) 0.1621(4) 0.7247(3) 0.0379(10) Uani 1 1 d . . . . .
H4A H 0.2334 0.1652 0.7467 0.046 Uiso 1 1 calc R U . . .
H4B H 0.3119 0.2246 0.6687 0.046 Uiso 1 1 calc R U . . .
C6 C 0.2182(5) 0.2403(4) 0.9091(3) 0.0319(11) Uani 1 1 d . . . . .
N1 N 0.4957(4) 0.3144(3) 0.7165(3) 0.0324(9) Uani 1 1 d . . . . .
H1A H 0.5218 0.2944 0.6664 0.039 Uiso 1 1 calc R U . . .
H1B H 0.4260 0.3826 0.6980 0.039 Uiso 1 1 calc R U . . .
O4 O 0.1159(3) 0.2955(3) 0.9391(2) 0.0379(8) Uani 1 1 d . . . . .
O13 O 0.1627(4) 0.9027(3) 0.3126(2) 0.0511(10) Uani 1 1 d . . . . .
O3 O 0.2127(4) 0.0353(3) 1.0212(3) 0.0451(9) Uani 1 1 d . . . . .
C5 C 0.2688(5) 0.0970(4) 0.9531(3) 0.0327(11) Uani 1 1 d . . . . .
O11 O 0.5180(4) 0.5918(4) 0.5561(3) 0.0536(10) Uani 1 1 d . . . . .
C1 C 0.6109(5) 0.3409(5) 0.7533(4) 0.0386(12) Uani 1 1 d . . . . .
H1C H 0.6154 0.4266 0.7183 0.046 Uiso 1 1 calc R U . . .
H1D H 0.6972 0.2851 0.7480 0.046 Uiso 1 1 calc R U . . .
C2 C 0.5834(5) 0.3202(5) 0.8553(4) 0.0405(12) Uani 1 1 d . . . . .
H2C H 0.6629 0.3220 0.8868 0.049 Uiso 1 1 calc R U . . .
H2D H 0.5056 0.3850 0.8602 0.049 Uiso 1 1 calc R U . . .
C3 C 0.5288(5) 0.0273(5) 0.7058(4) 0.0413(13) Uani 1 1 d . . . . .
H3C H 0.5757 -0.0563 0.7091 0.050 Uiso 1 1 calc R U . . .
H3D H 0.5476 0.0873 0.6457 0.050 Uiso 1 1 calc R U . . .
C14 C 0.2915(5) 0.6494(4) 0.6111(4) 0.0330(11) Uani 1 1 d . . . . .
C4 C 0.3766(5) 0.0401(5) 0.7144(4) 0.0446(13) Uani 1 1 d . . . . .
H4C H 0.3373 0.0391 0.6584 0.054 Uiso 1 1 calc R U . . .
H4D H 0.3582 -0.0280 0.7693 0.054 Uiso 1 1 calc R U . . .
O14 O 0.2135(4) 0.9545(3) 0.4695(3) 0.0449(9) Uani 1 1 d D . . . .
H1O H 0.294(2) 0.925(5) 0.509(2) 0.067 Uiso 1 1 d D U . . .
H2O H 0.158(3) 0.953(5) 0.5224(18) 0.067 Uiso 1 1 d D U . . .
Co2 Co 0.92227(6) 0.67019(5) 0.80800(4) 0.02820(17) Uani 1 1 d . . . . .
C7 C 1.0214(5) 0.5036(5) 0.7138(4) 0.0416(13) Uani 1 1 d . . . . .
H7C H 1.0704 0.4182 0.7233 0.050 Uiso 1 1 calc R U . . .
H7D H 1.0393 0.5581 0.6511 0.050 Uiso 1 1 calc R U . . .
C8 C 0.8707(5) 0.5145(5) 0.7243(4) 0.0414(12) Uani 1 1 d . . . . .
H8C H 0.8320 0.5045 0.6720 0.050 Uiso 1 1 calc R U . . .
H8D H 0.8536 0.4510 0.7830 0.050 Uiso 1 1 calc R U . . .
C9 C 1.0884(5) 0.8404(5) 0.7436(4) 0.0380(12) Uani 1 1 d . . . . .
H9A H 1.0892 0.9265 0.7065 0.046 Uiso 1 1 calc R U . . .
H9B H 1.1770 0.7865 0.7397 0.046 Uiso 1 1 calc R U . . .
C10 C 1.0589(5) 0.8237(4) 0.8446(4) 0.0377(12) Uani 1 1 d . . . . .
H10A H 1.1354 0.8321 0.8749 0.045 Uiso 1 1 calc R U . . .
H10B H 0.9773 0.8862 0.8478 0.045 Uiso 1 1 calc R U . . .
C11 C 0.7019(4) 0.7363(4) 0.9008(3) 0.0298(10) Uani 1 1 d . . . . .
C12 C 0.7552(5) 0.5922(4) 0.9501(4) 0.0331(11) Uani 1 1 d . . . . .
N5 N 1.0660(4) 0.5414(3) 0.7874(3) 0.0318(9) Uani 1 1 d . . . . .
H5A H 1.1406 0.5696 0.7690 0.038 Uiso 1 1 calc R U . . .
H5B H 1.0874 0.4752 0.8413 0.038 Uiso 1 1 calc R U . . .
N6 N 0.8096(4) 0.6413(4) 0.7247(3) 0.0385(10) Uani 1 1 d . . . . .
H6A H 0.7244 0.6470 0.7450 0.046 Uiso 1 1 calc R U . . .
H6B H 0.8064 0.6985 0.6664 0.046 Uiso 1 1 calc R U . . .
N7 N 0.9778(4) 0.8065(3) 0.7083(3) 0.0313(9) Uani 1 1 d . . . . .
H7A H 1.0069 0.7837 0.6599 0.038 Uiso 1 1 calc R U . . .
H7B H 0.9060 0.8728 0.6878 0.038 Uiso 1 1 calc R U . . .
N8 N 1.0377(4) 0.6974(4) 0.8918(3) 0.0367(10) Uani 1 1 d . . . . .
H8A H 0.9971 0.6905 0.9464 0.044 Uiso 1 1 calc R U . . .
H8B H 1.1180 0.6405 0.9038 0.044 Uiso 1 1 calc R U . . .
O7 O 0.6971(4) 0.5335(3) 1.0176(3) 0.0494(10) Uani 1 1 d . . . . .
O5 O 0.8624(3) 0.5467(3) 0.9129(2) 0.0337(8) Uani 1 1 d . . . . .
O6 O 0.7708(3) 0.7875(3) 0.8316(2) 0.0313(7) Uani 1 1 d . . . . .
O8 O 0.5977(3) 0.7930(3) 0.9286(2) 0.0382(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
O16 Mo1 1.712(4) . ?
Mo1 O13 1.738(3) . ?
Mo1 O15 1.757(3) . ?
Mo1 O9 2.181(3) . ?
Mo1 O10 2.195(3) . ?
Mo1 O14 2.332(4) . ?
Co1 O2 1.909(3) . ?
Co1 O1 1.914(3) . ?
Co1 N1 1.932(4) . ?
Co1 N3 1.937(3) . ?
Co1 N2 1.937(4) . ?
Co1 N4 1.943(4) . ?
O1 C5 1.286(5) . ?
O12 C14 1.228(6) . ?
O2 C6 1.279(5) . ?
O10 C13 1.271(6) . ?
O9 C14 1.264(5) . ?
C13 O11 1.215(6) . ?
C13 C14 1.553(6) . ?
N2 C2 1.468(6) . ?
N3 C3 1.494(6) . ?
N4 C4 1.487(6) . ?
C6 O4 1.236(5) . ?
C6 C5 1.536(6) . ?
N1 C1 1.474(7) . ?
O3 C5 1.227(6) . ?
C1 C2 1.501(7) . ?
C3 C4 1.506(7) . ?
Co2 O6 1.905(3) . ?
Co2 O5 1.911(3) . ?
Co2 N5 1.929(3) . ?
Co2 N6 1.934(4) . ?
Co2 N7 1.941(4) . ?
Co2 N8 1.948(4) . ?
C7 N5 1.489(6) . ?
C7 C8 1.496(7) . ?
C8 N6 1.482(6) . ?
C9 N7 1.473(6) . ?
C9 C10 1.499(7) . ?
C10 N8 1.470(6) . ?
C11 O8 1.239(5) . ?
C11 O6 1.270(5) . ?
C11 C12 1.551(7) . ?
C12 O7 1.220(6) . ?
C12 O5 1.280(5) . ?

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
O16 Mo1 O13 104.7(2) . . ?
O16 Mo1 O15 104.22(18) . . ?
O13 Mo1 O15 105.80(17) . . ?
O16 Mo1 O9 90.03(17) . . ?
O13 Mo1 O9 156.30(17) . . ?
O15 Mo1 O9 87.90(15) . . ?
O16 Mo1 O10 92.07(16) . . ?
O13 Mo1 O10 88.49(15) . . ?
O15 Mo1 O10 154.42(16) . . ?
O9 Mo1 O10 72.27(12) . . ?
O16 Mo1 O14 165.30(17) . . ?
O13 Mo1 O14 85.49(17) . . ?
O15 Mo1 O14 82.57(15) . . ?
O9 Mo1 O14 77.06(13) . . ?
O10 Mo1 O14 77.44(12) . . ?
O2 Co1 O1 85.69(13) . . ?
O2 Co1 N1 90.69(14) . . ?
O1 Co1 N1 175.18(15) . . ?
O2 Co1 N3 175.13(16) . . ?
O1 Co1 N3 90.55(15) . . ?
N1 Co1 N3 93.24(16) . . ?
O2 Co1 N2 89.14(15) . . ?
O1 Co1 N2 91.35(15) . . ?
N1 Co1 N2 85.41(17) . . ?
N3 Co1 N2 94.04(16) . . ?
O2 Co1 N4 90.40(15) . . ?
O1 Co1 N4 89.20(17) . . ?
N1 Co1 N4 94.01(18) . . ?
N3 Co1 N4 86.45(17) . . ?
N2 Co1 N4 179.25(17) . . ?
C5 O1 Co1 112.9(3) . . ?
C6 O2 Co1 112.5(3) . . ?
C13 O10 Mo1 119.8(3) . . ?
C14 O9 Mo1 119.5(3) . . ?
O11 C13 O10 126.8(4) . . ?
O11 C13 C14 120.2(4) . . ?
O10 C13 C14 113.0(4) . . ?
C2 N2 Co1 109.0(3) . . ?
C3 N3 Co1 109.6(3) . . ?
C4 N4 Co1 108.3(3) . . ?
O4 C6 O2 124.4(4) . . ?
O4 C6 C5 120.4(4) . . ?
O2 C6 C5 115.2(4) . . ?
C1 N1 Co1 110.7(3) . . ?
O3 C5 O1 125.2(4) . . ?
O3 C5 C6 121.0(4) . . ?
O1 C5 C6 113.8(4) . . ?
N1 C1 C2 106.2(4) . . ?
N2 C2 C1 106.8(4) . . ?
N3 C3 C4 107.2(4) . . ?
O12 C14 O9 125.9(4) . . ?
O12 C14 C13 119.2(4) . . ?
O9 C14 C13 114.8(4) . . ?
N4 C4 C3 106.1(4) . . ?
O6 Co2 O5 85.57(13) . . ?
O6 Co2 N5 175.11(16) . . ?
O5 Co2 N5 90.42(15) . . ?
O6 Co2 N6 91.54(15) . . ?
O5 Co2 N6 88.82(16) . . ?
N5 Co2 N6 85.57(17) . . ?
O6 Co2 N7 89.87(14) . . ?
O5 Co2 N7 174.31(15) . . ?
N5 Co2 N7 94.29(16) . . ?
N6 Co2 N7 94.71(18) . . ?
O6 Co2 N8 89.20(15) . . ?
O5 Co2 N8 91.12(16) . . ?
N5 Co2 N8 93.68(17) . . ?
N6 Co2 N8 179.24(16) . . ?
N7 Co2 N8 85.41(17) . . ?
N5 C7 C8 106.4(4) . . ?
N6 C8 C7 105.8(4) . . ?
N7 C9 C10 106.3(4) . . ?
N8 C10 C9 106.8(4) . . ?
O8 C11 O6 124.6(4) . . ?
O8 C11 C12 120.2(4) . . ?
O6 C11 C12 115.1(4) . . ?
O7 C12 O5 126.2(4) . . ?
O7 C12 C11 120.7(4) . . ?
O5 C12 C11 113.1(4) . . ?
C7 N5 Co2 110.7(3) . . ?
C8 N6 Co2 108.2(3) . . ?
C9 N7 Co2 110.5(3) . . ?
C10 N8 Co2 108.1(3) . . ?
C12 O5 Co2 113.4(3) . . ?
C11 O6 Co2 112.8(3) . . ?

_refine_diff_density_max         1.443
_refine_diff_density_min         -1.566
_refine_diff_density_rms         0.146

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

data_2a
_database_code_depnum_ccdc_archive 'CCDC 1579654'
_audit_update_record             
;
2017-10-12 deposited with the CCDC.
2018-02-16 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT420_shelx               
;
PROBLEM: D-H Without Acceptor       O32    --  H8W    ...     Please Check 
RESPONSE: The large electron density of the polyoxometalate anion makes it 
difficult lo locate hydrogen atoms from the electron difference map. The 
hydrogen atoms were thus placed on most reasonable positions (whereever it 
was possible) 
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H2 Mo4 O28, 2(Co H18 N6), 6(H2 O)'
_chemical_formula_sum            'C8 H50 Co2 Mo4 N12 O34'
_chemical_formula_weight         1360.22

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      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   10.5531(3)
_cell_length_b                   16.1106(6)
_cell_length_c                   23.2787(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3957.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.0(2)
_cell_measurement_reflns_used    17444
_cell_measurement_theta_min      3.8379
_cell_measurement_theta_max      39.1771

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.283
_exptl_crystal_F_000             2704
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.71
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_exptl_absorpt_coefficient_mu    2.171
_exptl_absorpt_correction_T_min  0.79049
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      150.0(2)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur Kappa CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 16.3426
_diffrn_reflns_number            30194
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         3.862
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             8629
_reflns_number_gt                7889
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.799
_reflns_Friedel_fraction_max     0.999
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0234P)²] 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_abs_structure_details 
;
 Flack x determined using 3317 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(6)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8629
_refine_ls_number_parameters     592
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0198
_refine_ls_wR_factor_ref         0.0426
_refine_ls_wR_factor_gt          0.0421
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_restrained_S_all      0.964
_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
O29 O 0.6980(5) 0.7883(3) 0.8903(3) 0.0670(15) Uani 1 1 d D . . . .
H1W H 0.611(2) 0.803(5) 0.896(4) 0.101 Uiso 1 1 d D U . . .
O30 O 0.0435(3) 0.4248(2) 0.87728(16) 0.0251(8) Uani 1 1 d D . . . .
H3W H -0.028(3) 0.418(3) 0.9024(17) 0.038 Uiso 1 1 d D U . . .
H4W H 0.097(4) 0.460(3) 0.8999(19) 0.038 Uiso 1 1 d D U . . .
O31 O 0.2416(3) 0.2482(2) 1.01548(14) 0.0229(8) Uani 1 1 d D . . . .
H5W H 0.160(2) 0.243(3) 1.033(2) 0.034 Uiso 1 1 d D U . . .
H6W H 0.268(5) 0.2999(16) 1.032(2) 0.034 Uiso 1 1 d D U . . .
O32 O 1.0016(5) 0.5740(3) 1.04884(18) 0.0569(13) Uani 1 1 d D . . . .
H7W H 1.019(7) 0.568(5) 1.0087(7) 0.085 Uiso 1 1 d D U . . .
H8W H 0.979(8) 0.5174(16) 1.057(3) 0.085 Uiso 1 1 d D U . . .
O33 O 0.8768(4) 0.3988(3) 0.9652(2) 0.0488(11) Uani 1 1 d D . . . .
H9W H 0.824(5) 0.444(3) 0.977(3) 0.073 Uiso 1 1 d D U . . .
H10W H 0.826(5) 0.350(2) 0.969(3) 0.073 Uiso 1 1 d D U . . .
O34 O 0.9517(4) 0.4868(3) 0.7741(2) 0.0590(15) Uani 1 1 d D . . . .
H11W H 0.994(6) 0.488(5) 0.8105(15) 0.089 Uiso 1 1 d D U . . .
H12W H 1.021(4) 0.491(5) 0.748(2) 0.089 Uiso 1 1 d D U . . .
C1 C 0.2197(4) 0.2675(3) 1.15639(18) 0.0123(9) Uani 1 1 d . . . . .
C2 C 0.3579(4) 0.2614(3) 1.17912(18) 0.0145(9) Uani 1 1 d . . . . .
C3 C 0.2716(4) 0.5167(3) 0.96467(18) 0.0132(9) Uani 1 1 d . . . . .
C4 C 0.3622(4) 0.5731(3) 0.99994(19) 0.0147(9) Uani 1 1 d . . . . .
C5 C 0.8318(4) 0.6256(3) 0.91154(18) 0.0147(9) Uani 1 1 d . . . . .
C6 C 0.8141(4) 0.6475(3) 0.84682(19) 0.0148(10) Uani 1 1 d . . . . .
C7 C 0.5369(4) 0.4967(3) 0.68950(19) 0.0139(10) Uani 1 1 d . . . . .
C8 C 0.4639(4) 0.4169(3) 0.70447(18) 0.0126(9) Uani 1 1 d . . . . .
N1 N 0.3852(3) 0.1783(2) 0.88782(16) 0.0156(8) Uani 1 1 d . . . . .
H1A H 0.4533 0.1581 0.8701 0.023 Uiso 1 1 calc R U . . .
H1B H 0.3399 0.1367 0.9023 0.023 Uiso 1 1 calc R U . . .
H1C H 0.4094 0.2119 0.9161 0.023 Uiso 1 1 calc R U . . .
N2 N 0.1574(3) 0.2607(2) 0.89297(15) 0.0156(8) Uani 1 1 d . . . . .
H2A H 0.1931 0.2519 0.9270 0.023 Uiso 1 1 calc R U . . .
H2B H 0.0920 0.2264 0.8885 0.023 Uiso 1 1 calc R U . . .
H2C H 0.1304 0.3130 0.8910 0.023 Uiso 1 1 calc R U . . .
N3 N 0.1966(3) 0.1386(2) 0.80819(16) 0.0153(8) Uani 1 1 d . . . . .
H3A H 0.1948 0.1363 0.7700 0.023 Uiso 1 1 calc R U . . .
H3B H 0.1177 0.1380 0.8217 0.023 Uiso 1 1 calc R U . . .
H3C H 0.2387 0.0950 0.8218 0.023 Uiso 1 1 calc R U . . .
N4 N 0.1747(4) 0.3029(2) 0.77858(15) 0.0154(8) Uani 1 1 d . . . . .
H4A H 0.0959 0.3054 0.7920 0.023 Uiso 1 1 calc R U . . .
H4B H 0.1748 0.2775 0.7446 0.023 Uiso 1 1 calc R U . . .
H4C H 0.2052 0.3541 0.7746 0.023 Uiso 1 1 calc R U . . .
N5 N 0.4077(3) 0.2248(2) 0.77232(16) 0.0142(8) Uani 1 1 d . . . . .
H5A H 0.4022 0.2660 0.7469 0.021 Uiso 1 1 calc R U . . .
H5B H 0.3939 0.1767 0.7547 0.021 Uiso 1 1 calc R U . . .
H5C H 0.4848 0.2246 0.7879 0.021 Uiso 1 1 calc R U . . .
N6 N 0.3699(3) 0.3425(2) 0.85332(16) 0.0137(8) Uani 1 1 d . . . . .
H6A H 0.3285 0.3678 0.8816 0.021 Uiso 1 1 calc R U . . .
H6B H 0.3738 0.3759 0.8229 0.021 Uiso 1 1 calc R U . . .
H6C H 0.4481 0.3302 0.8649 0.021 Uiso 1 1 calc R U . . .
N7 N 0.5013(4) 0.6670(2) 1.11356(16) 0.0160(8) Uani 1 1 d . . . . .
H7A H 0.4688 0.7029 1.1386 0.024 Uiso 1 1 calc R U . . .
H7B H 0.4972 0.6160 1.1281 0.024 Uiso 1 1 calc R U . . .
H7C H 0.4573 0.6690 1.0810 0.024 Uiso 1 1 calc R U . . .
N8 N 0.7106(4) 0.5832(2) 1.07024(17) 0.0170(8) Uani 1 1 d . . . . .
H8A H 0.7328 0.5853 1.0334 0.026 Uiso 1 1 calc R U . . .
H8B H 0.6408 0.5527 1.0740 0.026 Uiso 1 1 calc R U . . .
H8C H 0.7730 0.5605 1.0906 0.026 Uiso 1 1 calc R U . . .
N9 N 0.6285(4) 0.7317(2) 1.02076(16) 0.0179(9) Uani 1 1 d . . . . .
H9A H 0.5609 0.7646 1.0231 0.027 Uiso 1 1 calc R U . . .
H9B H 0.6099 0.6875 0.9995 0.027 Uiso 1 1 calc R U . . .
H9C H 0.6923 0.7593 1.0047 0.027 Uiso 1 1 calc R U . . .
N10 N 0.8561(4) 0.7221(2) 1.08307(18) 0.0237(9) Uani 1 1 d . . . . .
H10A H 0.8607 0.7610 1.0560 0.035 Uiso 1 1 calc R U . . .
H10B H 0.8962 0.6766 1.0712 0.035 Uiso 1 1 calc R U . . .
H10C H 0.8923 0.7406 1.1151 0.035 Uiso 1 1 calc R U . . .
N11 N 0.6530(4) 0.8083(2) 1.12538(17) 0.0197(8) Uani 1 1 d . . . . .
H11A H 0.6565 0.8432 1.0958 0.030 Uiso 1 1 calc R U . . .
H11B H 0.7134 0.8211 1.1505 0.030 Uiso 1 1 calc R U . . .
H11C H 0.5776 0.8123 1.1423 0.030 Uiso 1 1 calc R U . . .
N12 N 0.7211(4) 0.6623(3) 1.17654(16) 0.0226(9) Uani 1 1 d . . . . .
H12A H 0.7773 0.6978 1.1911 0.034 Uiso 1 1 calc R U . . .
H12B H 0.7542 0.6115 1.1761 0.034 Uiso 1 1 calc R U . . .
H12C H 0.6515 0.6625 1.1981 0.034 Uiso 1 1 calc R U . . .
O1 O 0.2331(3) 0.50766(19) 1.10660(14) 0.0192(7) Uani 1 1 d . . . . .
O2 O 0.4769(3) 0.48777(18) 1.14204(13) 0.0161(7) Uani 1 1 d . . . . .
O3 O 0.3803(3) 0.38411(18) 1.05995(13) 0.0149(7) Uani 1 1 d . . . . .
O4 O 0.1928(3) 0.33689(18) 1.13289(13) 0.0141(6) Uani 1 1 d . . . . .
O5 O 0.4279(3) 0.32297(18) 1.16590(13) 0.0142(7) Uani 1 1 d . . . . .
O6 O 0.3910(3) 0.20080(19) 1.20652(15) 0.0220(8) Uani 1 1 d . . . . .
O7 O 0.1474(3) 0.20886(19) 1.16199(14) 0.0207(7) Uani 1 1 d . . . . .
O8 O 0.6308(3) 0.41131(19) 1.03564(13) 0.0161(7) Uani 1 1 d . . . . .
O9 O 0.4903(3) 0.31097(17) 0.96641(12) 0.0133(6) Uani 1 1 d . . . . .
O10 O 0.3155(3) 0.44415(18) 0.95599(12) 0.0135(6) Uani 1 1 d . . . . .
O11 O 0.4623(3) 0.53752(18) 1.01734(12) 0.0125(6) Uani 1 1 d . . . . .
O12 O 0.3334(3) 0.64639(17) 1.00882(13) 0.0187(7) Uani 1 1 d . . . . .
O13 O 0.1695(3) 0.54394(19) 0.94823(13) 0.0193(7) Uani 1 1 d . . . . .
O14 O 0.5621(3) 0.45906(18) 0.92503(12) 0.0126(6) Uani 1 1 d . . . . .
O15 O 0.5118(3) 0.62187(18) 0.90542(13) 0.0186(7) Uani 1 1 d . . . . .
O16 O 0.7340(3) 0.45183(19) 0.83730(14) 0.0178(7) Uani 1 1 d D . . . .
O17 O 0.7519(3) 0.57215(19) 0.92962(13) 0.0183(7) Uani 1 1 d . . . . .
O18 O 0.9137(3) 0.6600(2) 0.93968(14) 0.0233(8) Uani 1 1 d . . . . .
O19 O 0.8919(3) 0.6884(2) 0.82084(14) 0.0248(8) Uani 1 1 d . . . . .
O20 O 0.7125(3) 0.61677(18) 0.82496(13) 0.0135(7) Uani 1 1 d . . . . .
O21 O 0.4973(3) 0.51995(18) 0.81540(12) 0.0146(6) Uani 1 1 d . . . . .
O22 O 0.2463(3) 0.51389(19) 0.82510(13) 0.0170(7) Uani 1 1 d . . . . .
O23 O 0.3500(3) 0.65740(18) 0.78714(13) 0.0176(7) Uani 1 1 d . . . . .
O24 O 0.4835(3) 0.56295(18) 0.70617(12) 0.0129(6) Uani 1 1 d . . . . .
O25 O 0.3707(3) 0.42768(17) 0.73816(12) 0.0126(6) Uani 1 1 d . . . . .
O26 O 0.4985(3) 0.35025(18) 0.68424(14) 0.0213(7) Uani 1 1 d . . . . .
O27 O 0.6381(3) 0.49362(19) 0.66321(15) 0.0233(8) Uani 1 1 d . . . . .
O28 O 0.2136(3) 0.55746(19) 0.71334(12) 0.0150(7) Uani 1 1 d . . . . .
Co1 Co 0.28127(5) 0.24080(4) 0.83249(2) 0.00973(12) Uani 1 1 d . . . . .
Co2 Co 0.67807(6) 0.69557(3) 1.09826(2) 0.01099(12) Uani 1 1 d . . . . .
Mo1 Mo 0.33657(4) 0.43630(2) 1.13320(2) 0.01092(8) Uani 1 1 d . . . . .
Mo2 Mo 0.49082(3) 0.40596(2) 0.99950(2) 0.00910(7) Uani 1 1 d . . . . .
Mo3 Mo 0.59290(3) 0.54175(2) 0.87629(2) 0.00979(8) Uani 1 1 d . . . . .
Mo4 Mo 0.33355(3) 0.55437(2) 0.77046(2) 0.00957(8) Uani 1 1 d . . . . .
H1O H 0.790(3) 0.468(3) 0.8068(12) 0.014 Uiso 1 1 d D U . . .
H2O H 0.713(4) 0.3940(7) 0.8369(19) 0.014 Uiso 1 1 d D 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
C1 O7 1.221(5) . ?
C1 O4 1.277(5) . ?
C1 C2 1.554(6) . ?
C2 O6 1.218(5) . ?
C2 O5 1.274(5) . ?
C3 O13 1.224(5) . ?
C3 O10 1.274(5) . ?
C3 C4 1.554(6) . ?
C4 O12 1.237(5) . ?
C4 O11 1.268(5) . ?
C5 O18 1.217(5) . ?
C5 O17 1.277(5) . ?
C5 C6 1.559(6) . ?
C6 O19 1.214(5) . ?
C6 O20 1.285(5) . ?
C7 O27 1.232(5) . ?
C7 O24 1.268(5) . ?
C7 C8 1.538(6) . ?
C8 O26 1.228(5) . ?
C8 O25 1.270(5) . ?
N1 Co1 1.968(4) . ?
N2 Co1 1.948(3) . ?
N3 Co1 1.957(4) . ?
N4 Co1 1.960(4) . ?
N5 Co1 1.952(4) . ?
N6 Co1 1.948(3) . ?
N7 Co2 1.955(4) . ?
N8 Co2 1.954(4) . ?
N9 Co2 1.966(4) . ?
N10 Co2 1.959(4) . ?
N11 Co2 1.941(4) . ?
N12 Co2 1.953(4) . ?
O1 Mo1 1.702(3) . ?
O2 Mo1 1.710(3) . ?
O3 Mo2 1.861(3) . ?
O3 Mo1 1.957(3) . ?
O4 Mo1 2.206(3) . ?
O5 Mo1 2.200(3) . ?
O8 Mo2 1.702(3) . ?
O9 Mo2 1.713(3) . ?
O10 Mo2 2.197(3) . ?
O11 Mo2 2.181(3) . ?
O14 Mo3 1.780(3) . ?
O14 Mo2 2.074(3) . ?
O15 Mo3 1.691(3) . ?
O16 Mo3 2.267(3) . ?
O17 Mo3 2.144(3) . ?
O20 Mo3 2.117(3) . ?
O21 Mo3 1.775(3) . ?
O21 Mo4 2.095(3) . ?
O22 Mo4 1.700(3) . ?
O23 Mo4 1.713(3) . ?
O24 Mo4 2.182(3) . ?
O25 Mo4 2.210(3) . ?
O28 Mo4 1.836(3) . ?
O28 Mo1 1.942(3) 2_564 ?
Mo1 O28 1.942(3) 2_565 ?

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
O7 C1 O4 125.7(4) . . ?
O7 C1 C2 120.1(4) . . ?
O4 C1 C2 114.2(4) . . ?
O6 C2 O5 125.8(4) . . ?
O6 C2 C1 119.8(4) . . ?
O5 C2 C1 114.4(4) . . ?
O13 C3 O10 126.8(4) . . ?
O13 C3 C4 119.8(4) . . ?
O10 C3 C4 113.4(4) . . ?
O12 C4 O11 125.6(4) . . ?
O12 C4 C3 119.7(4) . . ?
O11 C4 C3 114.7(4) . . ?
O18 C5 O17 126.7(4) . . ?
O18 C5 C6 120.2(4) . . ?
O17 C5 C6 113.1(4) . . ?
O19 C6 O20 125.1(4) . . ?
O19 C6 C5 121.5(4) . . ?
O20 C6 C5 113.3(4) . . ?
O27 C7 O24 124.8(4) . . ?
O27 C7 C8 120.9(4) . . ?
O24 C7 C8 114.3(4) . . ?
O26 C8 O25 125.9(4) . . ?
O26 C8 C7 119.7(4) . . ?
O25 C8 C7 114.4(4) . . ?
Mo2 O3 Mo1 136.52(16) . . ?
C1 O4 Mo1 118.8(3) . . ?
C2 O5 Mo1 118.4(3) . . ?
C3 O10 Mo2 119.3(3) . . ?
C4 O11 Mo2 119.6(3) . . ?
Mo3 O14 Mo2 155.19(17) . . ?
C5 O17 Mo3 118.7(3) . . ?
C6 O20 Mo3 119.6(3) . . ?
Mo3 O21 Mo4 144.61(17) . . ?
C7 O24 Mo4 118.6(3) . . ?
C8 O25 Mo4 118.3(3) . . ?
Mo4 O28 Mo1 152.26(17) . 2_564 ?
N2 Co1 N6 90.22(16) . . ?
N2 Co1 N5 177.95(15) . . ?
N6 Co1 N5 87.76(15) . . ?
N2 Co1 N3 92.35(16) . . ?
N6 Co1 N3 177.33(16) . . ?
N5 Co1 N3 89.66(15) . . ?
N2 Co1 N4 89.63(15) . . ?
N6 Co1 N4 90.30(15) . . ?
N5 Co1 N4 89.99(16) . . ?
N3 Co1 N4 89.01(16) . . ?
N2 Co1 N1 89.16(15) . . ?
N6 Co1 N1 89.98(15) . . ?
N5 Co1 N1 91.22(15) . . ?
N3 Co1 N1 90.77(16) . . ?
N4 Co1 N1 178.77(16) . . ?
N11 Co2 N12 89.14(17) . . ?
N11 Co2 N8 177.63(17) . . ?
N12 Co2 N8 90.95(17) . . ?
N11 Co2 N7 91.78(16) . . ?
N12 Co2 N7 89.28(17) . . ?
N8 Co2 N7 90.59(16) . . ?
N11 Co2 N10 89.17(17) . . ?
N12 Co2 N10 90.29(18) . . ?
N8 Co2 N10 88.46(17) . . ?
N7 Co2 N10 178.95(16) . . ?
N11 Co2 N9 89.16(17) . . ?
N12 Co2 N9 177.56(16) . . ?
N8 Co2 N9 90.82(16) . . ?
N7 Co2 N9 89.02(16) . . ?
N10 Co2 N9 91.44(17) . . ?
O1 Mo1 O2 105.78(15) . . ?
O1 Mo1 O28 98.02(14) . 2_565 ?
O2 Mo1 O28 95.48(13) . 2_565 ?
O1 Mo1 O3 97.15(14) . . ?
O2 Mo1 O3 96.25(13) . . ?
O28 Mo1 O3 157.50(13) 2_565 . ?
O1 Mo1 O5 165.28(14) . . ?
O2 Mo1 O5 88.95(13) . . ?
O28 Mo1 O5 80.22(12) 2_565 . ?
O3 Mo1 O5 80.88(12) . . ?
O1 Mo1 O4 92.75(13) . . ?
O2 Mo1 O4 161.47(13) . . ?
O28 Mo1 O4 81.55(12) 2_565 . ?
O3 Mo1 O4 81.23(12) . . ?
O5 Mo1 O4 72.53(11) . . ?
O8 Mo2 O9 105.67(15) . . ?
O8 Mo2 O3 100.35(14) . . ?
O9 Mo2 O3 99.74(13) . . ?
O8 Mo2 O14 94.45(13) . . ?
O9 Mo2 O14 89.63(13) . . ?
O3 Mo2 O14 159.56(12) . . ?
O8 Mo2 O11 88.65(13) . . ?
O9 Mo2 O11 162.43(12) . . ?
O3 Mo2 O11 87.33(12) . . ?
O14 Mo2 O11 78.95(11) . . ?
O8 Mo2 O10 160.81(13) . . ?
O9 Mo2 O10 92.31(13) . . ?
O3 Mo2 O10 82.76(12) . . ?
O14 Mo2 O10 78.72(11) . . ?
O11 Mo2 O10 72.51(10) . . ?
O15 Mo3 O21 100.58(15) . . ?
O15 Mo3 O14 102.90(14) . . ?
O21 Mo3 O14 104.90(14) . . ?
O15 Mo3 O20 95.31(13) . . ?
O21 Mo3 O20 90.06(13) . . ?
O14 Mo3 O20 153.64(12) . . ?
O15 Mo3 O17 89.41(15) . . ?
O21 Mo3 O17 162.25(13) . . ?
O14 Mo3 O17 86.85(12) . . ?
O20 Mo3 O17 74.31(11) . . ?
O15 Mo3 O16 168.80(14) . . ?
O21 Mo3 O16 85.80(13) . . ?
O14 Mo3 O16 84.09(12) . . ?
O20 Mo3 O16 75.35(11) . . ?
O17 Mo3 O16 82.17(12) . . ?
O22 Mo4 O23 104.88(15) . . ?
O22 Mo4 O28 100.31(14) . . ?
O23 Mo4 O28 101.97(15) . . ?
O22 Mo4 O21 88.38(14) . . ?
O23 Mo4 O21 93.43(14) . . ?
O28 Mo4 O21 159.60(12) . . ?
O22 Mo4 O24 158.42(13) . . ?
O23 Mo4 O24 91.19(13) . . ?
O28 Mo4 O24 90.08(11) . . ?
O21 Mo4 O24 76.17(11) . . ?
O22 Mo4 O25 89.79(13) . . ?
O23 Mo4 O25 162.50(13) . . ?
O28 Mo4 O25 84.32(12) . . ?
O21 Mo4 O25 77.24(11) . . ?
O24 Mo4 O25 72.33(11) . . ?

_refine_diff_density_max         0.372
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.078

####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1579656'
_audit_update_record             
;
2017-10-12 deposited with the CCDC.
2018-02-16 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            'C20 H60 Co2 Mo4 N12 O33'
_chemical_formula_weight         1498.42

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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.5099(10)
_cell_length_b                   17.5536(10)
_cell_length_c                   9.9621(8)
_cell_angle_alpha                90
_cell_angle_beta                 87.737(6)
_cell_angle_gamma                90
_cell_volume                     2360.6(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2499
_cell_measurement_theta_min      3.7517
_cell_measurement_theta_max      35.9511

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.108
_exptl_crystal_F_000             1500
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    1.830
_exptl_absorpt_correction_T_min  0.69753
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur Kappa CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 16.3426
_diffrn_reflns_number            9053
_diffrn_reflns_av_unetI/netI     0.1267
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.763
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_full        24.995
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             4106
_reflns_number_gt                2202
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0704P)²] 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         4106
_refine_ls_number_parameters     343
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0534
_refine_ls_wR_factor_ref         0.1406
_refine_ls_wR_factor_gt          0.1317
_refine_ls_goodness_of_fit_ref   0.893
_refine_ls_restrained_S_all      0.915
_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
O10 O 0.5124(10) 0.5178(6) 0.4800(13) 0.037(3) Uani 0.5 1 d . U P . .
O2 O 0.1271(5) 0.7078(6) 0.6501(8) 0.095(3) Uani 1 1 d . . . . .
O3 O 0.1030(6) 0.5587(5) 0.6286(9) 0.093(3) Uani 1 1 d . . . . .
O11 O 0.3923(6) 0.5698(5) 0.3083(9) 0.094(3) Uani 1 1 d D U . . .
O16 O -0.2565(5) 0.7131(3) 0.5067(7) 0.0476(17) Uani 1 1 d D . . . .
H1W H -0.231(6) 0.6661(19) 0.472(6) 0.071 Uiso 1 1 d D U . . .
H2W H -0.283(6) 0.688(3) 0.584(4) 0.071 Uiso 1 1 d D U . . .
O17 O 0.3747(10) 0.7529(7) 0.3331(13) 0.165(5) Uani 1 1 d D U . . .
H3W H 0.413(6) 0.732(4) 0.402(6) 0.248 Uiso 1 1 d D U . . .
H4W H 0.375(10) 0.7051(16) 0.288(5) 0.248 Uiso 1 1 d D U . . .
O1 O 0.1736(6) 0.7246(4) 0.3742(8) 0.072(2) Uani 1 1 d D . . . .
Mo1 Mo 0.13826(6) 0.63438(5) 0.53766(8) 0.0404(3) Uani 1 1 d . . . . .
Co1 Co 0.75419(8) 0.93384(6) 0.49659(11) 0.0255(3) Uani 1 1 d . . . . .
Mo3 Mo 0.37804(6) 0.54818(6) 0.47218(9) 0.0560(3) Uani 1 1 d . . . . .
O6 O 0.0134(4) 0.5572(4) 0.1782(6) 0.0437(17) Uani 1 1 d . . . . .
O12 O 0.3818(4) 0.5533(3) 0.6924(6) 0.0370(15) Uani 1 1 d . . . . .
O15 O 0.4907(5) 0.5689(4) 0.8491(6) 0.0494(18) Uani 1 1 d . . . . .
N3 N 0.6634(5) 1.0190(4) 0.4631(7) 0.0383(19) Uani 1 1 d . . . . .
H3A H 0.6323 1.0108 0.3873 0.057 Uiso 1 1 calc R U . . .
H3B H 0.6180 1.0224 0.5300 0.057 Uiso 1 1 calc R U . . .
N6 N 0.8573(5) 0.8563(4) 0.5168(8) 0.041(2) Uani 1 1 d . . . . .
H6A H 0.8940 0.8676 0.5863 0.062 Uiso 1 1 calc R U . . .
H6B H 0.8297 0.8108 0.5313 0.062 Uiso 1 1 calc R U . . .
N1 N 0.6493(5) 0.8588(4) 0.4754(7) 0.0358(18) Uani 1 1 d . . . . .
H1A H 0.6144 0.8703 0.4042 0.054 Uiso 1 1 calc R U . . .
H1B H 0.6755 0.8127 0.4627 0.054 Uiso 1 1 calc R U . . .
O8 O 0.2707(4) 0.6221(3) 0.5137(6) 0.0392(15) Uani 1 1 d . . . . .
N2 N 0.7185(5) 0.9274(4) 0.6889(7) 0.0382(19) Uani 1 1 d . . . . .
H2A H 0.7730 0.9213 0.7352 0.057 Uiso 1 1 calc R U . . .
H2B H 0.6892 0.9704 0.7160 0.057 Uiso 1 1 calc R U . . .
N4 N 0.8496(5) 1.0145(4) 0.5348(8) 0.0395(19) Uani 1 1 d . . . . .
H4A H 0.8814 1.0029 0.6086 0.059 Uiso 1 1 calc R U . . .
H4B H 0.8942 1.0184 0.4669 0.059 Uiso 1 1 calc R U . . .
O5 O 0.1161(4) 0.5706(4) 0.3481(6) 0.0412(16) Uani 1 1 d . . . . .
O7 O -0.1190(4) 0.6465(4) 0.3227(6) 0.0511(19) Uani 1 1 d . . . . .
N5 N 0.7906(5) 0.9293(4) 0.3020(7) 0.0408(19) Uani 1 1 d . . . . .
H5A H 0.7363 0.9261 0.2545 0.061 Uiso 1 1 calc R U . . .
H5B H 0.8234 0.9713 0.2769 0.061 Uiso 1 1 calc R U . . .
C3 C 0.4587(6) 0.5823(5) 0.7386(8) 0.031(2) Uani 1 1 d . . . . .
C10 C 0.9198(7) 0.8551(6) 0.3910(9) 0.043(2) Uani 1 1 d . . . . .
H10A H 0.9663 0.8972 0.3900 0.052 Uiso 1 1 calc R U . . .
H10B H 0.9570 0.8079 0.3844 0.052 Uiso 1 1 calc R U . . .
C4 C 0.5151(7) 0.6377(6) 0.6432(9) 0.039(2) Uani 1 1 d . . . . .
O4 O -0.0048(4) 0.6615(4) 0.4735(7) 0.057(2) Uani 1 1 d . . . . .
O14 O 0.5905(5) 0.6682(4) 0.6830(6) 0.0505(18) Uani 1 1 d . . . . .
O13 O 0.4744(5) 0.6481(4) 0.5312(7) 0.061(2) Uani 1 1 d D . . . .
C5 C 0.5842(6) 0.8590(5) 0.5979(9) 0.039(2) Uani 1 1 d . . . . .
H5C H 0.5446 0.8129 0.6029 0.047 Uiso 1 1 calc R U . . .
H5D H 0.5401 0.9026 0.5981 0.047 Uiso 1 1 calc R U . . .
C2 C 0.0369(6) 0.5813(5) 0.2880(9) 0.033(2) Uani 1 1 d . . . . .
C7 C 0.7204(7) 1.0910(5) 0.4524(9) 0.038(2) Uani 1 1 d . . . . .
H7A H 0.7505 1.0965 0.3629 0.046 Uiso 1 1 calc R U . . .
H7B H 0.6774 1.1344 0.4705 0.046 Uiso 1 1 calc R U . . .
C1 C -0.0361(6) 0.6328(5) 0.3656(9) 0.038(2) Uani 1 1 d . . . . .
C8 C 0.7978(7) 1.0867(5) 0.5534(10) 0.042(3) Uani 1 1 d . . . . .
H8A H 0.8439 1.1287 0.5415 0.050 Uiso 1 1 calc R U . . .
H8B H 0.7678 1.0895 0.6434 0.050 Uiso 1 1 calc R U . . .
C6 C 0.6515(6) 0.8632(6) 0.7146(9) 0.043(2) Uani 1 1 d . . . . .
H6C H 0.6131 0.8710 0.7978 0.051 Uiso 1 1 calc R U . . .
H6D H 0.6888 0.8162 0.7218 0.051 Uiso 1 1 calc R U . . .
O9 O 0.3014(6) 0.4686(4) 0.4754(9) 0.078(2) Uani 1 1 d . U . . .
C9 C 0.8535(7) 0.8617(6) 0.2779(10) 0.049(3) Uani 1 1 d . . . . .
H9A H 0.8127 0.8164 0.2721 0.058 Uiso 1 1 calc R U . . .
H9B H 0.8920 0.8672 0.1942 0.058 Uiso 1 1 calc R U . . .
H1O H 0.164(6) 0.736(5) 0.282(3) 0.073 Uiso 1 1 d D U . . .
H2O H 0.235(3) 0.752(4) 0.371(7) 0.073 Uiso 1 1 d D 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
O10 O10 0.81(2) 3_666 ?
O10 Mo3 1.896(14) . ?
O10 Mo3 1.953(13) 3_666 ?
O2 Mo1 1.710(7) . ?
O3 Mo1 1.666(8) . ?
O11 Mo3 1.679(9) . ?
O1 Mo1 2.308(7) . ?
Mo1 O8 1.809(6) . ?
Mo1 O4 2.114(6) . ?
Mo1 O5 2.225(6) . ?
Co1 N1 1.953(7) . ?
Co1 N2 1.960(7) . ?
Co1 N4 1.962(7) . ?
Co1 N6 1.963(7) . ?
Co1 N3 1.972(7) . ?
Co1 N5 1.983(7) . ?
Mo3 O9 1.739(8) . ?
Mo3 O10 1.953(13) 3_666 ?
Mo3 O8 1.977(6) . ?
Mo3 O12 2.199(6) . ?
Mo3 O13 2.275(7) . ?
O6 C2 1.226(10) . ?
O12 C3 1.261(9) . ?
O15 C3 1.221(9) . ?
N3 C7 1.482(11) . ?
N6 C10 1.484(11) . ?
N1 C5 1.476(11) . ?
N2 C6 1.462(11) . ?
N4 C8 1.456(11) . ?
O5 C2 1.261(10) . ?
O7 C1 1.238(10) . ?
N5 C9 1.474(11) . ?
C3 C4 1.540(12) . ?
C10 C9 1.471(12) . ?
C4 O14 1.231(10) . ?
C4 O13 1.276(10) . ?
O4 C1 1.274(10) . ?
C5 C6 1.506(11) . ?
C2 C1 1.525(12) . ?
C7 C8 1.482(12) . ?

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
O10 O10 Mo3 81.9(19) 3_666 . ?
O10 O10 Mo3 74.0(18) 3_666 3_666 ?
Mo3 O10 Mo3 155.9(6) . 3_666 ?
O3 Mo1 O2 103.2(5) . . ?
O3 Mo1 O8 103.7(3) . . ?
O2 Mo1 O8 103.7(3) . . ?
O3 Mo1 O4 95.7(3) . . ?
O2 Mo1 O4 88.3(3) . . ?
O8 Mo1 O4 154.0(3) . . ?
O3 Mo1 O5 90.9(4) . . ?
O2 Mo1 O5 157.4(3) . . ?
O8 Mo1 O5 89.6(2) . . ?
O4 Mo1 O5 72.6(2) . . ?
O3 Mo1 O1 167.7(4) . . ?
O2 Mo1 O1 87.5(4) . . ?
O8 Mo1 O1 79.2(3) . . ?
O4 Mo1 O1 78.4(3) . . ?
O5 Mo1 O1 77.1(3) . . ?
N1 Co1 N2 85.1(3) . . ?
N1 Co1 N4 173.3(3) . . ?
N2 Co1 N4 89.5(3) . . ?
N1 Co1 N6 93.7(3) . . ?
N2 Co1 N6 90.4(3) . . ?
N4 Co1 N6 90.4(3) . . ?
N1 Co1 N3 92.0(3) . . ?
N2 Co1 N3 94.5(3) . . ?
N4 Co1 N3 84.5(3) . . ?
N6 Co1 N3 172.8(3) . . ?
N1 Co1 N5 91.2(3) . . ?
N2 Co1 N5 174.4(3) . . ?
N4 Co1 N5 94.5(3) . . ?
N6 Co1 N5 85.6(3) . . ?
N3 Co1 N5 89.8(3) . . ?
O11 Mo3 O9 104.2(4) . . ?
O11 Mo3 O10 91.7(5) . . ?
O9 Mo3 O10 110.1(4) . . ?
O11 Mo3 O10 108.2(5) . 3_666 ?
O9 Mo3 O10 88.6(4) . 3_666 ?
O10 Mo3 O10 24.1(6) . 3_666 ?
O11 Mo3 O8 96.3(3) . . ?
O9 Mo3 O8 95.3(3) . . ?
O10 Mo3 O8 150.6(4) . . ?
O10 Mo3 O8 153.4(4) 3_666 . ?
O11 Mo3 O12 162.6(4) . . ?
O9 Mo3 O12 92.9(3) . . ?
O10 Mo3 O12 84.9(4) . . ?
O10 Mo3 O12 74.5(4) 3_666 . ?
O8 Mo3 O12 79.0(2) . . ?
O11 Mo3 O13 91.8(4) . . ?
O9 Mo3 O13 164.0(3) . . ?
O10 Mo3 O13 69.4(4) . . ?
O10 Mo3 O13 86.9(4) 3_666 . ?
O8 Mo3 O13 82.1(3) . . ?
O12 Mo3 O13 71.0(2) . . ?
C3 O12 Mo3 115.6(6) . . ?
C7 N3 Co1 109.5(5) . . ?
C10 N6 Co1 107.8(5) . . ?
C5 N1 Co1 108.7(5) . . ?
Mo1 O8 Mo3 145.0(4) . . ?
C6 N2 Co1 110.0(5) . . ?
C8 N4 Co1 109.7(5) . . ?
C2 O5 Mo1 118.2(6) . . ?
C9 N5 Co1 108.1(6) . . ?
O15 C3 O12 125.3(8) . . ?
O15 C3 C4 119.6(8) . . ?
O12 C3 C4 115.1(7) . . ?
C9 C10 N6 107.6(7) . . ?
O14 C4 O13 127.6(9) . . ?
O14 C4 C3 118.1(8) . . ?
O13 C4 C3 114.3(8) . . ?
C1 O4 Mo1 120.2(6) . . ?
C4 O13 Mo3 112.7(6) . . ?
N1 C5 C6 106.3(7) . . ?
O6 C2 O5 128.8(9) . . ?
O6 C2 C1 118.1(8) . . ?
O5 C2 C1 113.1(8) . . ?
C8 C7 N3 106.6(7) . . ?
O7 C1 O4 123.3(9) . . ?
O7 C1 C2 121.0(8) . . ?
O4 C1 C2 115.6(7) . . ?
N4 C8 C7 107.9(7) . . ?
N2 C6 C5 106.9(7) . . ?
C10 C9 N5 107.7(7) . . ?

_refine_diff_density_max         1.294
_refine_diff_density_min         -0.927
_refine_diff_density_rms         0.145

