# Electronic Supplementary Material (ESI) for Nanoscale.
# This journal is © The Royal Society of Chemistry 2017

# CIF files for compounds 1-2#
data_global
_publ_section_title               ?
loop_
  _publ_author_name
 'Jiangwei Zhang'
 'Gao Li'

loop_
  _publ_contact_author_name
  _publ_contact_author_address
  _publ_contact_author_email
 'Gao Li'
;
Dalian Institute of Chemical Physics, Chinese Academy of Sciences (CAS)
Dalian 116023, 
P.R.China
;
 'gaoli@dicp.ac.cn'
  
  'Jiangwei Zhang'
;
Dalian Institute of Chemical Physics, Chinese Academy of Sciences (CAS)
Dalian 116023, 
P.R.China
;
 'jwzhang@dicp.ac.cn'

 data_compound1
_audit_creation_date              2017-05-15
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_shelx_SHELXL_version_number      '2016/6'
_publ_contact_author_address      ?
_publ_contact_author_email        ?
_publ_contact_author_id_orcid     ?
_publ_contact_author_name         ''
_publ_contact_author_phone        ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common             ?
_chemical_name_systematic         ?
_chemical_formula_moiety          '1(Co1 Mo9 O32), 12(H2 O), 6(H4 N)'
_chemical_formula_sum             'Co H48 Mo9 N6 O44'
_chemical_formula_weight          1758.78
_chemical_absolute_configuration  ?
_chemical_melting_point           ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'Co' 'Co' 0.3494 0.9721 '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'
 'Mo' 'Mo' -1.6832 0.6857
 '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'

_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.
;
_space_group_crystal_system       'trigonal'
_space_group_IT_number            155
_space_group_name_H-M_alt         'R 3 2'
_space_group_name_Hall            'R 3 2"'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-y, x-y, z'
 'y, x, -z'
 '-x+y, -x, z'
 'x-y, -y, -z'
 '-x, -x+y, -z'
 'x+2/3, y+1/3, z+1/3'
 '-y+2/3, x-y+1/3, z+1/3'
 'y+2/3, x+1/3, -z+1/3'
 '-x+y+2/3, -x+1/3, z+1/3'
 'x-y+2/3, -y+1/3, -z+1/3'
 '-x+2/3, -x+y+1/3, -z+1/3'
 'x+1/3, y+2/3, z+2/3'
 '-y+1/3, x-y+2/3, z+2/3'
 'y+1/3, x+2/3, -z+2/3'
 '-x+y+1/3, -x+2/3, z+2/3'
 'x-y+1/3, -y+2/3, -z+2/3'
 '-x+1/3, -x+y+2/3, -z+2/3'

_cell_length_a                    16.1035(7)
_cell_length_b                    16.1035(7)
_cell_length_c                    12.2637(6)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      2754.2(3)
_cell_formula_units_Z             2.9988
_cell_measurement_reflns_used     1382
_cell_measurement_temperature     293(2)
_cell_measurement_theta_max       29.240
_cell_measurement_theta_min       3.361
_shelx_estimated_absorpt_T_max    ?
_shelx_estimated_absorpt_T_min    ?
_exptl_absorpt_coefficient_mu     3.551
_exptl_absorpt_correction_T_max   0.701
_exptl_absorpt_correction_T_min   0.431
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_exptl_crystal_colour             atrovirens
_exptl_crystal_density_diffrn     3.209
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_description        block
_exptl_crystal_F_000              2586
_exptl_crystal_size_max           0.4
_exptl_crystal_size_mid           0.2
_exptl_crystal_size_min           0.1
_exptl_transmission_factor_max    ?
_exptl_transmission_factor_min    ?
_diffrn_reflns_av_R_equivalents   0.0225
_diffrn_reflns_av_unetI/netI      0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_limit_h_max        20
_diffrn_reflns_limit_h_min        -14
_diffrn_reflns_limit_k_max        20
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_l_max        11
_diffrn_reflns_limit_l_min        -16
_diffrn_reflns_number             2287
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.837
_diffrn_reflns_theta_full         25.242
_diffrn_reflns_theta_max          29.240
_diffrn_reflns_theta_min          3.361
_diffrn_ambient_temperature       293(2)
_diffrn_detector_area_resol_mean  16.0971
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device_type   'Xcalibur, Eos, Gemini'
_diffrn_measurement_method        'ω scans'
_diffrn_radiation_type            MoK\a
_diffrn_radiation_wavelength      0.71073
_diffrn_source                    ?
_reflns_Friedel_coverage          0.678
_reflns_Friedel_fraction_full     0.952
_reflns_Friedel_fraction_max      0.751
_reflns_number_gt                 1582
_reflns_number_total              1598
_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.
;
_reflns_threshold_expression      'I > 2σ(I)'
_computing_cell_refinement        ?
_computing_data_collection        ?
_computing_data_reduction         ?
_computing_molecular_graphics     'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material   'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement   'ShelXL (Sheldrick, 2015)'
_computing_structure_solution     ?
_refine_diff_density_max          1.066
_refine_diff_density_min          -1.582
_refine_diff_density_rms          0.357
_refine_ls_abs_structure_details
;
 Flack x determined using 547 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack    0.49(5)
_refine_ls_extinction_coef        .
_refine_ls_extinction_method      none
_refine_ls_goodness_of_fit_ref    1.091
_refine_ls_hydrogen_treatment     mixed
_refine_ls_matrix_type            full
_refine_ls_number_parameters      131
_refine_ls_number_reflns          1598
_refine_ls_number_restraints      43
_refine_ls_R_factor_all           0.0392
_refine_ls_R_factor_gt            0.0387
_refine_ls_restrained_S_all       1.091
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0682P)²+18.8678P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme       calc
_refine_ls_wR_factor_gt           0.0861
_refine_ls_wR_factor_ref          0.0866
_refine_special_details           ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All N(H,H) groups, All O(H,H) groups
2. Restrained distances
 O7-O7_$1
 2.1 with sigma of 0.02
 N1-H1B_$2 = N1-H1D_$2 = N1-H1A_$2 = N1-H1C_$2
 0.9 with sigma of 0.02
 N2-H2D_$3 = N2-H2C_$3 = N2-H2B_$3 = N2-H2A_$3
 0.9 with sigma of 0.02
 O8_$4-O8
 2.1 with sigma of 0.02
 O8-H8A
 0.9 with sigma of 0.02
 O8-H8B
 0.9 with sigma of 0.02
 H8B-H8A
 1.2 with sigma of 0.02
 H1A-H1C \\sim H1A-H1B \\sim H1A-H1D \\sim H1C-H1B \\sim H1C-H1D \\sim H1B-H1D
 with sigma of 0.02
 H2A-H2B \\sim H2A-H2D \\sim H2A-H2C \\sim H2B-H2D \\sim H2B-H2C \\sim H2D-H2C
 with sigma of 0.02
3. Others
 Fixed Sof: H2A(0.5) H2B(0.5) H1D(0.5)
4.a Free rotating group:
 O7(H7A,H7B), N2(H2A,H2B)
;
_atom_sites_solution_hydrogens    difmap
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
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 0.58028(6) 0.38615(6) 0.53559(6) 0.0099(2) Uani 1 1 d . . . . .
 Mo2 Mo 0.666667 0.53375(7) 0.333333 0.0115(3) Uani 1 2 d S T P . .
 Co1 Co 0.666667 0.333333 0.333333 0.0117(7) Uani 1 6 d S T P . .
 O5 O 0.6286(7) 0.4757(6) 0.6287(6) 0.0244(17) Uani 1 1 d . . . . .
 O1 O 0.7096(5) 0.4416(5) 0.4254(5) 0.0078(12) Uani 1 1 d . . . . .
 O3 O 0.5528(6) 0.4464(6) 0.4203(6) 0.0135(14) Uani 1 1 d . . . . .
 O4 O 0.6062(6) 0.5682(7) 0.2469(7) 0.0252(19) Uani 1 1 d . . . . .
 O7 O 0.465(2) 0.4066(11) 0.820(3) 0.196(16) Uani 1 1 d D . . . .
 H7A H 0.503967 0.459232 0.788867 0.294 Uiso 1 1 d G . . . .
 H7B H 0.447722 0.365780 0.768926 0.294 Uiso 1 1 d G . . . .
 O2 O 0.666667 0.333333 0.5946(9) 0.011(2) Uani 1 3 d S T P . .
 O6 O 0.4669(6) 0.3084(6) 0.5862(7) 0.0196(16) Uani 1 1 d . . . . .
 N1 N 0.7769(11) 0.666667 0.666667 0.036(4) Uani 1 2 d DS T P . .
 N2 N 0.3690(11) 0.333333 0.333333 0.067(9) Uani 1 2 d DS T P . .
 H2A H 0.399314 0.393825 0.341711 0.101 Uiso 0.5 1 d DG . . . .
 H2B H 0.350504 0.319950 0.267527 0.101 Uiso 0.5 1 d DG . . . .
 O8 O 0.5940(10) 0.403(3) 0.8496(19) 0.20(2) Uani 1 1 d D . . . .
 H1A H 0.759(7) 0.607(5) 0.641(12) 0.02(4) Uiso 1 1 d D . . . .
 H1B H 0.838(3) 0.707(7) 0.648(9) 0.01(4) Uiso 1 1 d D . . . .
 H1C H 0.739(8) 0.687(9) 0.636(12) 0.0(3) Uiso 1 1 d D . . . .
 H1D H 0.771(9) 0.665(11) 0.740(3) 0.01(8) Uiso 0.5 1 d D . . . .
 H2C H 0.323(6) 0.305(8) 0.380(7) 0.02(3) Uiso 1 1 d D . . . .
 H2D H 0.411(9) 0.310(15) 0.347(12) 0.8(3) Uiso 1 1 d D . . . .
 H8A H 0.641(5) 0.459(9) 0.890(10) 0.03(5) Uiso 1 1 d D . . . .
 H8B H 0.535(5) 0.379(7) 0.920(7) 0.02(2) Uiso 1 1 d D . . . .

loop_
  _atom_site_aniso_label
  _atom_site_aniso_U_11
  _atom_site_aniso_U_22
  _atom_site_aniso_U_33
  _atom_site_aniso_U_23
  _atom_site_aniso_U_13
  _atom_site_aniso_U_12
 Mo1 0.0111(4) 0.0119(4) 0.0075(4) -0.0019(3) 0.0019(3) 0.0063(4)
 Mo2 0.0152(6) 0.0093(4) 0.0118(5) 0.0006(2) 0.0011(4) 0.0076(3)
 Co1 0.0127(10) 0.0127(10) 0.0095(13) 0.000 0.000 0.0064(5)
 O5 0.033(5) 0.023(4) 0.019(4) -0.004(3) -0.001(4) 0.014(4)
 O1 0.010(3) 0.010(3) 0.007(2) -0.003(3) -0.004(2) 0.007(3)
 O3 0.014(4) 0.018(4) 0.014(3) 0.002(3) 0.002(3) 0.012(3)
 O4 0.031(5) 0.035(5) 0.023(4) -0.004(4) -0.002(3) 0.027(4)
 O7 0.13(3) 0.24(4) 0.23(3) 0.14(3) 0.09(2) 0.11(3)
 O2 0.016(4) 0.016(4) 0.002(4) 0.000 0.000 0.0078(19)
 O6 0.016(4) 0.019(4) 0.020(4) 0.000(3) 0.007(3) 0.006(3)
 N1 0.025(6) 0.033(9) 0.054(12) -0.027(9) -0.013(4) 0.017(5)
 N2 0.027(6) 0.066(15) 0.12(2) -0.071(17) -0.036(8) 0.033(8)
 O8 0.14(2) 0.23(4) 0.101(15) -0.08(2) 0.041(17) -0.02(3)

_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 O5 1.693(8) . ?
 Mo1 O1 2.258(7) . ?
 Mo1 O1 2.214(6) 2_655 ?
 Mo1 O3 1.888(7) . ?
 Mo1 O2 2.090(4) . ?
 Mo1 O6 1.732(8) . ?
 Mo2 O1 2.231(7) 18_655 ?
 Mo2 O1 2.231(7) . ?
 Mo2 O3 1.975(8) . ?
 Mo2 O3 1.975(8) 18_655 ?
 Mo2 O4 1.708(8) . ?
 Mo2 O4 1.708(8) 18_655 ?
 Co1 O1 1.894(7) 17 ?
 Co1 O1 1.894(7) . ?
 Co1 O1 1.894(7) 2_655 ?
 Co1 O1 1.894(7) 18_655 ?
 Co1 O1 1.894(7) 4_665 ?
 Co1 O1 1.894(7) 15_545 ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 O5 Mo1 O1 97.3(4) . . ?
 O5 Mo1 O1 162.1(4) . 2_655 ?
 O5 Mo1 O3 101.2(4) . . ?
 O5 Mo1 O2 89.8(4) . . ?
 O5 Mo1 O6 104.1(4) . . ?
 O1 Mo1 O1 72.2(4) 2_655 . ?
 O3 Mo1 O1 75.8(3) . . ?
 O3 Mo1 O1 90.4(3) . 2_655 ?
 O3 Mo1 O2 147.5(3) . . ?
 O2 Mo1 O1 72.5(3) . . ?
 O2 Mo1 O1 73.4(3) . 2_655 ?
 O6 Mo1 O1 158.5(3) . . ?
 O6 Mo1 O1 86.6(4) . 2_655 ?
 O6 Mo1 O3 101.9(4) . . ?
 O6 Mo1 O2 104.9(3) . . ?
 O1 Mo2 O1 69.9(4) . 18_655 ?
 O3 Mo2 O1 74.9(3) . . ?
 O3 Mo2 O1 81.6(3) 18_655 . ?
 O3 Mo2 O1 81.6(3) . 18_655 ?
 O3 Mo2 O1 74.8(3) 18_655 18_655 ?
 O3 Mo2 O3 151.2(5) 18_655 . ?
 O4 Mo2 O1 161.1(4) . . ?
 O4 Mo2 O1 161.1(4) 18_655 18_655 ?
 O4 Mo2 O1 93.1(4) 18_655 . ?
 O4 Mo2 O1 93.1(4) . 18_655 ?
 O4 Mo2 O3 102.3(4) . 18_655 ?
 O4 Mo2 O3 95.2(4) 18_655 18_655 ?
 O4 Mo2 O3 102.3(4) 18_655 . ?
 O4 Mo2 O3 95.1(4) . . ?
 O4 Mo2 O4 104.9(6) 18_655 . ?
 O1 Co1 O1 169.0(4) 17 . ?
 O1 Co1 O1 88.1(3) 2_655 . ?
 O1 Co1 O1 169.0(4) 4_665 18_655 ?
 O1 Co1 O1 84.8(4) 17 2_655 ?
 O1 Co1 O1 88.1(3) 17 18_655 ?
 O1 Co1 O1 88.1(3) 4_665 . ?
 O1 Co1 O1 100.0(4) 4_665 17 ?
 O1 Co1 O1 100.0(4) 2_655 18_655 ?
 O1 Co1 O1 84.8(4) 18_655 . ?
 O1 Co1 O1 100.0(4) 15_545 . ?
 O1 Co1 O1 88.1(3) 4_665 2_655 ?
 O1 Co1 O1 84.8(4) 4_665 15_545 ?
 O1 Co1 O1 169.0(4) 15_545 2_655 ?
 O1 Co1 O1 88.1(3) 15_545 17 ?
 O1 Co1 O1 88.1(3) 15_545 18_655 ?
 Mo1 O1 Mo1 98.8(2) 4_665 . ?
 Mo1 O1 Mo2 152.8(4) 4_665 . ?
 Mo2 O1 Mo1 92.0(2) . . ?
 Co1 O1 Mo1 98.8(3) . . ?
 Co1 O1 Mo1 100.3(3) . 4_665 ?
 Co1 O1 Mo2 102.7(3) . . ?
 Mo1 O3 Mo2 113.5(4) . . ?
 Mo1 O2 Mo1 108.7(3) 4_665 . ?
 Mo1 O2 Mo1 108.7(3) 2_655 . ?
 Mo1 O2 Mo1 108.7(3) 2_655 4_665 ?

#===END

data_compound2
_audit_creation_date              2017-05-15
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_shelxl_version_number            2013-4
_publ_contact_author_address      ?
_publ_contact_author_email        ?
_publ_contact_author_name         ''
_publ_contact_author_phone        ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common             ?
_chemical_name_systematic
;
 ?
;
_chemical_formula_moiety          'Co H8 Mo6 O24, 8(H2 O), (H4 N)'
_chemical_formula_sum             'Co H28 Mo6 N O32'
_chemical_formula_weight          1188.78
_chemical_melting_point           ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'Co' 'Co' 0.3494 0.9721 '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'
 'Mo' 'Mo' -1.6832 0.6857
 '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'

_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.
;
_space_group_crystal_system       'monoclinic'
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 1 21/c 1'
_space_group_name_Hall            '-P 2ybc'
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                    11.432(2)
_cell_length_b                    10.997(2)
_cell_length_c                    11.725(2)
_cell_angle_alpha                 90
_cell_angle_beta                  99.86(3)
_cell_angle_gamma                 90
_cell_volume                      1452.2(5)
_cell_formula_units_Z             2
_cell_measurement_reflns_used     3293
_cell_measurement_temperature     293(2)
_cell_measurement_theta_max       26.000
_cell_measurement_theta_min       3.302
_shelx_estimated_absorpt_T_max    ?
_shelx_estimated_absorpt_T_min    ?
_exptl_absorpt_coefficient_mu     3.179
_exptl_absorpt_correction_T_max   0.530
_exptl_absorpt_correction_T_min   0.237
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_process_details    ?
_exptl_crystal_colour             green
_exptl_crystal_density_diffrn     2.755
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_description        block
_exptl_crystal_F_000              1162
_exptl_crystal_size_max           0.5
_exptl_crystal_size_mid           0.4
_exptl_crystal_size_min           0.2
_exptl_special_details
;
 ?
;
_exptl_transmission_factor_max    ?
_exptl_transmission_factor_min    ?
_diffrn_reflns_av_R_equivalents   0.0897
_diffrn_reflns_av_unetI/netI      0.0820
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max        14
_diffrn_reflns_limit_h_min        -14
_diffrn_reflns_limit_k_max        14
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_l_max        15
_diffrn_reflns_limit_l_min        -15
_diffrn_reflns_number             13481
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full         25.242
_diffrn_reflns_theta_max          27.430
_diffrn_reflns_theta_min          3.302
_diffrn_ambient_temperature       293(2)
_diffrn_detector_area_resol_mean  16.0971
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type   'Xcalibur, Eos, Gemini'
_diffrn_measurement_method        'ω scans'
_diffrn_radiation_type            MoK\a
_diffrn_radiation_wavelength      0.71073
_diffrn_source                    ?
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_full     .
_reflns_Friedel_fraction_max      .
_reflns_number_gt                 3060
_reflns_number_total              3293
_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.
;
_reflns_threshold_expression      'I > 2σ(I)'
_computing_cell_refinement        ?
_computing_data_collection        ?
_computing_data_reduction         ?
_computing_molecular_graphics     'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material   'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement   'ShelXL (Sheldrick, 2015)'
_computing_structure_solution     ?
_refine_diff_density_max          1.087
_refine_diff_density_min          -1.074
_refine_diff_density_rms          0.207
_refine_ls_extinction_coef        0.0094(10)
_refine_ls_extinction_expression  'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_extinction_method      SHELXL
_refine_ls_goodness_of_fit_ref    1.026
_refine_ls_hydrogen_treatment     mixed
_refine_ls_matrix_type            full
_refine_ls_number_parameters      221
_refine_ls_number_reflns          3293
_refine_ls_number_restraints      32
_refine_ls_R_factor_all           0.0617
_refine_ls_R_factor_gt            0.0588
_refine_ls_restrained_S_all       1.021
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0757P)²+7.8400P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme       calc
_refine_ls_wR_factor_gt           0.1064
_refine_ls_wR_factor_ref          0.1184
_refine_special_details
;
 ?
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H) groups
 At 1.5 times of:
  All N(H,H) groups, All O(H,H) groups
2. Restrained distances
 O6-H6
 0.9 with sigma of 0.02
 H2A-H2B \\sim H2A-H2C \\sim H2A-H2D \\sim H2B-H2C \\sim H2B-H2D \\sim H2C-H2D
 with sigma of 0.02
3.a Free rotating group:
 O1(H1A,H1B), O15(H15A,H15B), N2(H2A,H2B), O13(H13A,H13B), O14(H14A,H14B)
3.b Ternary CH refined with riding coordinates:
 O2(H2), O3(H3), O0AA(H0AA)
;
_atom_sites_solution_hydrogens    mixed
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 Co1 Co 0.0000 0.0000 0.0000 0.0156(3) Uani 1 2 d S T P . .
 Mo3 Mo -0.15844(5) -0.23377(5) 0.06938(5) 0.0227(2) Uani 1 1 d . . . . .
 Mo1 Mo -0.13557(5) 0.24532(4) -0.12043(4) 0.0221(2) Uani 1 1 d . . . . .
 Mo2 Mo -0.29498(5) 0.01514(5) -0.04726(5) 0.0243(2) Uani 1 1 d . . . . .
 O2 O -0.1205(4) 0.1099(4) 0.0306(3) 0.0182(8) Uani 1 1 d . . . . .
 H2 H -0.1136 0.1430 0.1091 0.022 Uiso 1 1 calc R . . . .
 O5 O -0.2540(4) -0.0926(4) 0.0842(4) 0.0264(9) Uani 1 1 d . . . . .
 O3 O 0.1307(4) 0.0986(4) 0.0730(3) 0.0192(8) Uani 1 1 d . . . . .
 H3 H 0.1280 0.1308 0.1504 0.023 Uiso 1 1 calc R . . . .
 O11 O -0.2547(5) -0.3194(5) -0.0254(4) 0.0385(12) Uani 1 1 d . . . . .
 O12 O -0.1567(5) -0.2949(5) 0.2046(4) 0.0364(12) Uani 1 1 d . . . . .
 O6 O 0.0132(4) 0.3059(4) -0.0345(4) 0.0241(9) Uani 1 1 d D . . . .
 H6 H 0.025(7) 0.376(4) 0.006(6) 0.029 Uiso 1 1 d DR . . . .
 O7 O -0.1295(5) 0.3020(5) -0.2553(4) 0.0360(11) Uani 1 1 d . . . . .
 O9 O -0.3928(5) -0.0713(5) -0.1400(5) 0.0415(13) Uani 1 1 d . . . . .
 O1 O 0.0055(4) 0.1031(4) -0.1310(3) 0.0193(8) Uani 1 1 d . . . . .
 H0AA H 0.0043 0.0633 -0.2059 0.03(2) Uiso 1 1 calc R . . . .
 O4 O -0.2443(4) 0.1145(4) -0.1659(4) 0.0270(10) Uani 1 1 d . . . . .
 O8 O -0.2245(5) 0.3443(5) -0.0605(5) 0.0364(11) Uani 1 1 d . . . . .
 O10 O -0.3793(5) 0.1164(5) 0.0146(5) 0.0399(12) Uani 1 1 d . . . . .
 O16 O -0.0158(10) 0.0415(6) -0.3481(5) 0.081(3) Uani 1 1 d . . . A 2
 H1A H 0.0527 0.0733 -0.3416 0.121 Uiso 1 1 d G . . A 2
 H1B H -0.0198 -0.0198 -0.3928 0.121 Uiso 1 1 d G . . A 2
 O15 O -0.3320(8) -0.5395(8) 0.1100(6) 0.068(2) Uani 1 1 d . . . . .
 H15A H -0.3216 -0.5779 0.1739 0.102 Uiso 1 1 d G . . . .
 H15B H -0.3247 -0.4636 0.1231 0.102 Uiso 1 1 d G . . . .
 N1 N -0.3568(9) -0.0125(9) 0.2685(8) 0.063(2) Uani 1 1 d . . . . .
 H2A H -0.3021 -0.0353 0.2325 0.095 Uiso 1 1 d DG . . . .
 H2B H -0.3921 -0.0744 0.2896 0.095 Uiso 1 1 d DG . . . .
 O13 O -0.5085(10) -0.2068(11) 0.2963(14) 0.117(4) Uani 1 1 d . . . . .
 H13A H -0.5089 -0.2770 0.3267 0.176 Uiso 1 1 d G . . . .
 H13B H -0.4395 -0.1914 0.2822 0.176 Uiso 1 1 d G . . . .
 O14 O -0.4938(10) -0.3397(12) 0.0881(14) 0.140(5) Uani 1 1 d . . . B 2
 H14A H -0.4857 -0.4165 0.0862 0.209 Uiso 1 1 d G . . B 2
 H14B H -0.4631 -0.3075 0.0342 0.209 Uiso 1 1 d G . . B 2
 H2C H -0.400(11) 0.039(9) 0.236(14) 2(3) Uiso 1 1 d D . . . .
 H2D H -0.317(12) 0.019(12) 0.336(10) 0.14(7) Uiso 1 1 d D . . . .

loop_
  _atom_site_aniso_label
  _atom_site_aniso_U_11
  _atom_site_aniso_U_22
  _atom_site_aniso_U_33
  _atom_site_aniso_U_23
  _atom_site_aniso_U_13
  _atom_site_aniso_U_12
 Co1 0.0248(6) 0.0083(5) 0.0135(5) 0.0002(4) 0.0029(4) 0.0000(4)
 Mo3 0.0326(4) 0.0142(3) 0.0216(3) 0.00334(17) 0.0051(2) -0.0039(2)
 Mo1 0.0328(4) 0.0134(3) 0.0196(3) 0.00397(17) 0.0034(2) 0.00454(19)
 Mo2 0.0257(3) 0.0220(3) 0.0247(3) 0.00243(19) 0.0029(2) 0.0003(2)
 O2 0.027(2) 0.0116(18) 0.0166(18) 0.0000(14) 0.0041(15) 0.0039(15)
 O5 0.031(2) 0.024(2) 0.025(2) 0.0046(17) 0.0082(18) 0.0009(18)
 O3 0.028(2) 0.0146(19) 0.0149(18) -0.0011(14) 0.0018(15) -0.0030(16)
 O11 0.048(3) 0.027(3) 0.040(3) 0.001(2) 0.006(2) -0.009(2)
 O12 0.051(3) 0.027(3) 0.036(3) 0.010(2) 0.017(2) -0.001(2)
 O6 0.040(2) 0.0094(19) 0.023(2) -0.0015(15) 0.0046(18) 0.0013(17)
 O7 0.053(3) 0.029(3) 0.026(2) 0.0104(19) 0.006(2) 0.005(2)
 O9 0.040(3) 0.044(3) 0.037(3) 0.006(2) -0.003(2) -0.011(2)
 O1 0.031(2) 0.0127(19) 0.0145(17) 0.0025(14) 0.0060(15) 0.0000(16)
 O4 0.034(2) 0.023(2) 0.023(2) 0.0066(17) -0.0001(18) 0.0007(19)
 O8 0.042(3) 0.026(3) 0.042(3) 0.001(2) 0.008(2) 0.011(2)
 O10 0.038(3) 0.040(3) 0.045(3) 0.003(2) 0.015(2) 0.007(2)
 O16 0.197(10) 0.020(3) 0.028(3) -0.003(2) 0.029(5) -0.005(4)
 O15 0.080(5) 0.086(6) 0.038(3) 0.004(3) 0.008(3) 0.012(5)
 N1 0.081(6) 0.064(6) 0.049(5) -0.020(4) 0.021(4) -0.005(5)
 O13 0.094(7) 0.070(7) 0.180(12) 0.054(7) 0.004(8) 0.025(6)
 O14 0.079(7) 0.102(9) 0.218(15) 0.056(10) -0.033(8) 0.008(6)

_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Co1 O2 1.912(4) 3 ?
 Co1 O2 1.912(4) . ?
 Co1 O3 1.925(4) 3 ?
 Co1 O3 1.925(4) . ?
 Co1 O1 1.918(4) 3 ?
 Co1 O1 1.918(4) . ?
 Mo3 O5 1.923(5) . ?
 Mo3 O3 2.297(4) 3 ?
 Mo3 O11 1.706(5) . ?
 Mo3 O12 1.718(5) . ?
 Mo3 O6 1.946(5) 3 ?
 Mo3 O1 2.283(4) 3 ?
 Mo1 O2 2.297(4) . ?
 Mo1 O6 1.940(5) . ?
 Mo1 O7 1.712(5) . ?
 Mo1 O1 2.265(4) . ?
 Mo1 O4 1.916(5) . ?
 Mo1 O8 1.719(5) . ?
 Mo2 O2 2.297(4) . ?
 Mo2 O5 1.937(4) . ?
 Mo2 O3 2.319(4) 3 ?
 Mo2 O9 1.709(5) . ?
 Mo2 O4 1.934(4) . ?
 Mo2 O10 1.712(5) . ?
 O2 H2 0.9800 . ?
 O3 Mo3 2.297(4) 3 ?
 O3 Mo2 2.319(4) 3 ?
 O3 H3 0.9800 . ?
 O6 Mo3 1.946(5) 3 ?
 O6 H6 0.90(2) . ?
 O1 Mo3 2.283(4) 3 ?
 O1 H0AA 0.9800 . ?
 O16 H1A 0.8499 . ?
 O16 H1B 0.8502 . ?
 O15 H15A 0.8502 . ?
 O15 H15B 0.8500 . ?
 N1 H2A 0.8496 . ?
 N1 H2B 0.8493 . ?
 N1 H2C 0.80(7) . ?
 N1 H2D 0.91(9) . ?
 O13 H13A 0.8502 . ?
 O13 H13B 0.8503 . ?
 O14 H14A 0.8503 . ?
 O14 H14B 0.8503 . ?

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 Co1 O2 180.0 3 . ?
 O2 Co1 O3 95.14(18) . . ?
 O2 Co1 O3 84.86(18) 3 . ?
 O2 Co1 O3 84.86(18) . 3 ?
 O2 Co1 O3 95.14(18) 3 3 ?
 O2 Co1 O1 95.74(17) 3 . ?
 O2 Co1 O1 84.26(17) 3 3 ?
 O2 Co1 O1 95.74(17) . 3 ?
 O2 Co1 O1 84.26(17) . . ?
 O3 Co1 O3 180.0 . 3 ?
 O1 Co1 O3 83.89(17) . . ?
 O1 Co1 O3 83.89(17) 3 3 ?
 O1 Co1 O3 96.11(17) 3 . ?
 O1 Co1 O3 96.11(17) . 3 ?
 O1 Co1 O1 180.0 . 3 ?
 O5 Mo3 O3 72.24(16) . 3 ?
 O5 Mo3 O6 150.06(18) . 3 ?
 O5 Mo3 O1 83.09(18) . 3 ?
 O11 Mo3 O5 101.0(2) . . ?
 O11 Mo3 O3 92.2(2) . 3 ?
 O11 Mo3 O12 106.8(3) . . ?
 O11 Mo3 O6 96.7(2) . 3 ?
 O11 Mo3 O1 157.9(2) . 3 ?
 O12 Mo3 O5 98.6(2) . . ?
 O12 Mo3 O3 160.4(2) . 3 ?
 O12 Mo3 O6 99.1(2) . 3 ?
 O12 Mo3 O1 93.8(2) . 3 ?
 O6 Mo3 O3 83.22(16) 3 3 ?
 O6 Mo3 O1 71.82(16) 3 3 ?
 O1 Mo3 O3 68.23(14) 3 3 ?
 O6 Mo1 O2 83.03(16) . . ?
 O6 Mo1 O1 72.34(16) . . ?
 O7 Mo1 O2 159.8(2) . . ?
 O7 Mo1 O6 100.6(2) . . ?
 O7 Mo1 O1 93.4(2) . . ?
 O7 Mo1 O4 98.2(2) . . ?
 O7 Mo1 O8 105.5(3) . . ?
 O1 Mo1 O2 68.56(14) . . ?
 O4 Mo1 O2 71.80(16) . . ?
 O4 Mo1 O6 150.62(18) . . ?
 O4 Mo1 O1 84.27(18) . . ?
 O8 Mo1 O2 93.8(2) . . ?
 O8 Mo1 O6 95.6(2) . . ?
 O8 Mo1 O1 159.3(2) . . ?
 O8 Mo1 O4 100.9(2) . . ?
 O2 Mo2 O3 68.23(14) . 3 ?
 O5 Mo2 O2 83.46(17) . . ?
 O5 Mo2 O3 71.51(17) . 3 ?
 O9 Mo2 O2 159.2(2) . . ?
 O9 Mo2 O5 102.0(2) . . ?
 O9 Mo2 O3 94.2(2) . 3 ?
 O9 Mo2 O4 95.8(2) . . ?
 O9 Mo2 O10 106.1(3) . . ?
 O4 Mo2 O2 71.51(16) . . ?
 O4 Mo2 O5 148.94(19) . . ?
 O4 Mo2 O3 82.08(17) . 3 ?
 O10 Mo2 O2 92.9(2) . . ?
 O10 Mo2 O5 97.9(2) . . ?
 O10 Mo2 O3 158.9(2) . 3 ?
 O10 Mo2 O4 101.4(2) . . ?
 Co1 O2 Mo1 103.08(17) . . ?
 Co1 O2 Mo2 104.06(17) . . ?
 Co1 O2 H2 117.8 . . ?
 Mo1 O2 H2 117.8 . . ?
 Mo2 O2 Mo1 92.41(14) . . ?
 Mo2 O2 H2 117.8 . . ?
 Mo3 O5 Mo2 119.0(2) . . ?
 Co1 O3 Mo3 103.58(16) . 3 ?
 Co1 O3 Mo2 102.86(17) . 3 ?
 Co1 O3 H3 118.0 . . ?
 Mo3 O3 Mo2 92.24(15) 3 3 ?
 Mo3 O3 H3 118.0 3 . ?
 Mo2 O3 H3 118.0 3 . ?
 Mo3 O6 H6 114(5) 3 . ?
 Mo1 O6 Mo3 117.0(2) . 3 ?
 Mo1 O6 H6 127(5) . . ?
 Co1 O1 Mo3 104.30(18) . 3 ?
 Co1 O1 Mo1 104.08(17) . . ?
 Co1 O1 H0AA 117.2 . . ?
 Mo3 O1 H0AA 117.2 3 . ?
 Mo1 O1 Mo3 93.55(15) . 3 ?
 Mo1 O1 H0AA 117.2 . . ?
 Mo1 O4 Mo2 118.9(2) . . ?
 H1A O16 H1B 109.5 . . ?
 H15A O15 H15B 109.5 . . ?
 H2A N1 H2B 109.5 . . ?
 H2A N1 H2C 114.7 . . ?
 H2A N1 H2D 104.2 . . ?
 H2B N1 H2C 114.7 . . ?
 H2B N1 H2D 104.1 . . ?
 H2C N1 H2D 108(3) . . ?
 H13A O13 H13B 109.4 . . ?
 H14A O14 H14B 109.4 . . ?

#===END