# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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 1940279'
loop_
_audit_author_name
_audit_author_address
'Xiang Pan'
;The Cambridge Crystallographic Data Centre
China
;
_audit_update_record             
;
2019-07-13 deposited with the CCDC.	2019-09-25 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            'C7 H10 Co Mo3 N3 O15'
_chemical_formula_weight         722.93

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                   8.0668(11)
_cell_length_b                   10.2716(15)
_cell_length_c                   12.5958(17)
_cell_angle_alpha                110.184(2)
_cell_angle_beta                 95.022(2)
_cell_angle_gamma                105.308(2)
_cell_volume                     926.3(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3955
_cell_measurement_theta_min      1.757
_cell_measurement_theta_max      28.386

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            PINK
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.592
_exptl_crystal_F_000             692
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    2.946
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'sealed tube'
_diffrn_measurement_method       graphite
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6872
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_av_R_equivalents  0.0179
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.757
_diffrn_reflns_theta_max         28.386
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4603
_reflns_number_gt                4103
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0556P)²+4.6248P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4603
_refine_ls_number_parameters     262
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0335
_refine_ls_wR_factor_ref         0.1026
_refine_ls_wR_factor_gt          0.0992
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.44094(5) -0.00864(4) 0.61576(3) 0.01227(10) Uani 1 1 d . . . . .
Co1 Co 0.13426(7) -0.24419(6) 0.71795(5) 0.01049(13) Uani 1 1 d . . . . .
O1 O 0.2775(5) -0.3104(4) 0.8301(3) 0.0267(8) Uani 1 1 d . . . . .
N1 N 0.1837(6) -0.0716(5) 0.8804(4) 0.0202(8) Uani 1 1 d . . . . .
C1 C 0.2250(7) 0.1212(6) 1.0413(5) 0.0269(11) Uani 1 1 d . . . . .
H1A H 0.2239 0.2154 1.0919 0.032 Uiso 1 1 d R U . . .
O1W O 0.4239(11) -0.6535(11) 0.3133(8) 0.111(3) Uani 1 1 d . . . . .
H1WA H 0.3348 -0.6288 0.2982 0.133 Uiso 1 1 d R U . . .
H1WB H 0.4963 -0.6307 0.2725 0.133 Uiso 1 1 d R U . . .
Mo2 Mo 0.15608(5) -0.17426(4) 0.30583(3) 0.01329(10) Uani 1 1 d . . . . .
O2 O 0.3654(4) -0.1343(4) 0.6775(3) 0.0204(7) Uani 1 1 d . . . . .
N2 N 0.1628(6) 0.0588(5) 0.9266(4) 0.0248(9) Uani 1 1 d . . . . .
H2A H 0.1117 0.0995 0.8859 0.030 Uiso 1 1 d R U . . .
C2 C 0.2911(7) 0.0256(6) 1.0725(4) 0.0249(10) Uani 1 1 d . . . . .
H2B H 0.3439 0.0378 1.1481 0.030 Uiso 1 1 d R U . . .
O2W O 0.3820(11) -0.4087(11) 0.4508(9) 0.115(3) Uani 1 1 d . . . . .
H2WA H 0.4008 -0.3216 0.4547 0.138 Uiso 1 1 d R U . . .
H2WB H 0.3017 -0.4260 0.4882 0.138 Uiso 1 1 d R U . . .
Mo3 Mo -0.14327(5) -0.14595(4) 0.51832(3) 0.01321(10) Uani 1 1 d . . . . .
O3 O 0.2903(4) 0.0835(4) 0.6251(3) 0.0183(6) Uani 1 1 d . . . . .
N3 N 0.3712(6) -0.2656(5) 1.0187(3) 0.0222(9) Uani 1 1 d . . . . .
H3A H 0.3786 -0.2046 1.0914 0.027 Uiso 1 1 d R U . . .
C3 C 0.2630(6) -0.0929(5) 0.9687(4) 0.0179(9) Uani 1 1 d . . . . .
O4 O 0.3816(4) -0.1227(4) 0.4588(3) 0.0150(6) Uani 1 1 d . . . . .
C4 C 0.3043(6) -0.2325(5) 0.9345(4) 0.0175(9) Uani 1 1 d . . . . .
O5 O 0.0965(5) -0.3535(4) 0.2866(3) 0.0274(8) Uani 1 1 d . . . . .
C5 C 0.4332(7) -0.3868(5) 1.0057(4) 0.0209(9) Uani 1 1 d . . . . .
O6 O 0.3740(4) -0.1360(4) 0.2548(3) 0.0167(6) Uani 1 1 d . . . . .
C6 C 0.5485(9) -0.3752(6) 1.0993(5) 0.0311(13) Uani 1 1 d . . . . .
H6A H 0.5823 -0.2882 1.1683 0.037 Uiso 1 1 d R U . . .
O7 O 0.0258(5) -0.1713(4) 0.1928(3) 0.0257(8) Uani 1 1 d . . . . .
C7 C 0.6171(8) -0.4866(6) 1.0942(5) 0.0321(13) Uani 1 1 d . . . . .
H7A H 0.7007 -0.4946 1.1756 0.048 Uiso 1 1 d R U . . .
O8 O 0.0397(4) -0.0940(4) 0.4281(3) 0.0161(6) Uani 1 1 d . . . . .
O9 O -0.2557(5) -0.3196(4) 0.4228(3) 0.0260(8) Uani 1 1 d . . . . .
O10 O -0.2995(4) -0.0803(4) 0.6019(3) 0.0181(6) Uani 1 1 d . . . . .
O11 O 0.1452(5) -0.4331(4) 0.5861(3) 0.0301(8) Uani 1 1 d . . . . .
O12 O -0.0981(5) -0.3664(4) 0.7463(4) 0.0336(9) Uani 1 1 d . . . . .
O13 O -0.0092(4) -0.1711(4) 0.6195(3) 0.0230(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
Mo1 O3 1.715(3) . ?
Mo1 O2 1.734(3) . ?
Mo1 O4 1.857(3) . ?
Mo1 O6 1.956(3) 2_656 ?
Mo1 O4 2.201(3) 2_656 ?
Mo1 O10 2.397(3) 1_655 ?
Mo1 Mo2 3.1631(6) 2_656 ?
Mo1 Mo1 3.1934(8) 2_656 ?
Co1 O13 2.071(3) . ?
Co1 O11 2.103(4) . ?
Co1 O12 2.098(4) . ?
Co1 O2 2.112(3) . ?
Co1 N1 2.114(4) . ?
Co1 O1 2.141(3) . ?
O1 C4 1.244(6) . ?
N1 N2 1.327(6) . ?
N1 C3 1.345(6) . ?
C1 N2 1.347(7) . ?
C1 C2 1.381(7) . ?
Mo2 O5 1.698(4) . ?
Mo2 O7 1.707(3) . ?
Mo2 O6 1.914(3) . ?
Mo2 O8 1.928(3) . ?
Mo2 O4 2.340(3) . ?
Mo2 O10 2.366(4) 2_556 ?
Mo2 Mo1 3.1631(6) 2_656 ?
C2 C3 1.395(7) . ?
Mo3 O9 1.711(4) . ?
Mo3 O13 1.731(3) . ?
Mo3 O10 1.828(3) . ?
Mo3 O8 2.012(3) . ?
Mo3 O8 2.212(3) 2_556 ?
Mo3 O3 2.431(3) 2_556 ?
O3 Mo3 2.431(3) 2_556 ?
N3 C4 1.334(6) . ?
N3 C5 1.424(6) . ?
C3 C4 1.485(6) . ?
O4 Mo1 2.201(3) 2_656 ?
C5 C6 1.387(7) . ?
C5 C7 1.394(7) 2_647 ?
O6 Mo1 1.956(3) 2_656 ?
C6 C7 1.382(7) . ?
C7 C5 1.394(7) 2_647 ?
O8 Mo3 2.212(3) 2_556 ?
O10 Mo2 2.366(4) 2_556 ?
O10 Mo1 2.397(3) 1_455 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Mo1 O2 104.90(16) . . ?
O3 Mo1 O4 99.56(15) . . ?
O2 Mo1 O4 103.00(15) . . ?
O3 Mo1 O6 99.37(15) . 2_656 ?
O2 Mo1 O6 98.46(15) . 2_656 ?
O4 Mo1 O6 146.52(14) . 2_656 ?
O3 Mo1 O4 95.50(14) . 2_656 ?
O2 Mo1 O4 159.31(14) . 2_656 ?
O4 Mo1 O4 76.52(14) . 2_656 ?
O6 Mo1 O4 74.39(13) 2_656 2_656 ?
O3 Mo1 O10 165.17(15) . 1_655 ?
O2 Mo1 O10 88.59(14) . 1_655 ?
O4 Mo1 O10 83.00(12) . 1_655 ?
O6 Mo1 O10 72.07(13) 2_656 1_655 ?
O4 Mo1 O10 70.76(12) 2_656 1_655 ?
O3 Mo1 Mo2 118.54(12) . 2_656 ?
O2 Mo1 Mo2 116.66(11) . 2_656 ?
O4 Mo1 Mo2 111.81(10) . 2_656 ?
O6 Mo1 Mo2 34.75(9) 2_656 2_656 ?
O4 Mo1 Mo2 47.69(8) 2_656 2_656 ?
O10 Mo1 Mo2 47.97(9) 1_655 2_656 ?
O3 Mo1 Mo1 99.36(11) . 2_656 ?
O2 Mo1 Mo1 140.85(12) . 2_656 ?
O4 Mo1 Mo1 42.08(10) . 2_656 ?
O6 Mo1 Mo1 107.43(10) 2_656 2_656 ?
O4 Mo1 Mo1 34.44(8) 2_656 2_656 ?
O10 Mo1 Mo1 72.67(8) 1_655 2_656 ?
Mo2 Mo1 Mo1 75.654(16) 2_656 2_656 ?
O13 Co1 O11 98.83(15) . . ?
O13 Co1 O12 90.33(15) . . ?
O11 Co1 O12 90.12(17) . . ?
O13 Co1 O2 89.21(13) . . ?
O11 Co1 O2 85.74(15) . . ?
O12 Co1 O2 175.72(16) . . ?
O13 Co1 N1 99.56(15) . . ?
O11 Co1 N1 161.30(15) . . ?
O12 Co1 N1 93.10(17) . . ?
O2 Co1 N1 91.17(16) . . ?
O13 Co1 O1 176.01(14) . . ?
O11 Co1 O1 84.94(15) . . ?
O12 Co1 O1 88.34(17) . . ?
O2 Co1 O1 92.39(15) . . ?
N1 Co1 O1 76.76(14) . . ?
C4 O1 Co1 114.8(3) . . ?
N2 N1 C3 105.4(4) . . ?
N2 N1 Co1 139.9(3) . . ?
C3 N1 Co1 114.7(3) . . ?
N2 C1 C2 107.6(5) . . ?
O5 Mo2 O7 103.89(19) . . ?
O5 Mo2 O6 105.58(17) . . ?
O7 Mo2 O6 98.21(16) . . ?
O5 Mo2 O8 102.33(16) . . ?
O7 Mo2 O8 99.30(16) . . ?
O6 Mo2 O8 142.20(14) . . ?
O5 Mo2 O4 89.67(15) . . ?
O7 Mo2 O4 165.13(16) . . ?
O6 Mo2 O4 71.85(12) . . ?
O8 Mo2 O4 83.42(12) . . ?
O5 Mo2 O10 158.09(15) . 2_556 ?
O7 Mo2 O10 97.86(16) . 2_556 ?
O6 Mo2 O10 73.47(12) . 2_556 ?
O8 Mo2 O10 71.13(12) . 2_556 ?
O4 Mo2 O10 69.04(11) . 2_556 ?
O5 Mo2 Mo1 118.31(13) . 2_656 ?
O7 Mo2 Mo1 121.99(13) . 2_656 ?
O6 Mo2 Mo1 35.61(9) . 2_656 ?
O8 Mo2 Mo1 107.75(10) . 2_656 ?
O4 Mo2 Mo1 44.06(8) . 2_656 ?
O10 Mo2 Mo1 48.81(8) 2_556 2_656 ?
Mo1 O2 Co1 141.26(19) . . ?
N1 N2 C1 111.9(4) . . ?
C1 C2 C3 103.9(4) . . ?
O9 Mo3 O13 103.95(18) . . ?
O9 Mo3 O10 106.33(17) . . ?
O13 Mo3 O10 101.60(16) . . ?
O9 Mo3 O8 98.58(16) . . ?
O13 Mo3 O8 97.16(15) . . ?
O10 Mo3 O8 143.90(15) . . ?
O9 Mo3 O8 154.04(16) . 2_556 ?
O13 Mo3 O8 100.56(15) . 2_556 ?
O10 Mo3 O8 76.62(14) . 2_556 ?
O8 Mo3 O8 69.75(14) . 2_556 ?
O9 Mo3 O3 81.89(15) . 2_556 ?
O13 Mo3 O3 171.06(15) . 2_556 ?
O10 Mo3 O3 82.93(13) . 2_556 ?
O8 Mo3 O3 75.07(12) . 2_556 ?
O8 Mo3 O3 72.79(12) 2_556 2_556 ?
Mo1 O3 Mo3 130.74(17) . 2_556 ?
C4 N3 C5 126.8(4) . . ?
N1 C3 C2 111.1(4) . . ?
N1 C3 C4 114.1(4) . . ?
C2 C3 C4 134.7(4) . . ?
Mo1 O4 Mo1 103.48(14) . 2_656 ?
Mo1 O4 Mo2 136.18(16) . . ?
Mo1 O4 Mo2 88.24(11) 2_656 . ?
O1 C4 N3 123.9(4) . . ?
O1 C4 C3 118.9(4) . . ?
N3 C4 C3 117.3(4) . . ?
C6 C5 C7 119.7(5) . 2_647 ?
C6 C5 N3 116.8(4) . . ?
C7 C5 N3 123.5(4) 2_647 . ?
Mo2 O6 Mo1 109.63(15) . 2_656 ?
C7 C6 C5 120.9(5) . . ?
C6 C7 C5 119.4(5) . 2_647 ?
Mo2 O8 Mo3 143.95(18) . . ?
Mo2 O8 Mo3 105.73(14) . 2_556 ?
Mo3 O8 Mo3 110.25(14) . 2_556 ?
Mo3 O10 Mo2 103.29(15) . 2_556 ?
Mo3 O10 Mo1 151.23(17) . 1_455 ?
Mo2 O10 Mo1 83.22(11) 2_556 1_455 ?
Mo3 O13 Co1 168.6(2) . . ?

_refine_diff_density_max         2.263
_refine_diff_density_min         -1.197
_refine_diff_density_rms         0.178

####################################################################### 
# 
# 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 1940280'
loop_
_audit_author_name
_audit_author_address
'Xiang Pan'
;The Cambridge Crystallographic Data Centre
China
;
_audit_update_record             
;
2019-07-13 deposited with the CCDC.	2019-09-25 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            'C7 H10 Mo3 N3 Ni O15'
_chemical_formula_weight         722.71

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'
Ni Ni 0.3393 1.1124 '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                   8.0455(3)
_cell_length_b                   10.2229(4)
_cell_length_c                   12.4994(5)
_cell_angle_alpha                109.5950(10)
_cell_angle_beta                 94.9980(10)
_cell_angle_gamma                105.4480(10)
_cell_volume                     915.73(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4082
_cell_measurement_theta_min      1.763
_cell_measurement_theta_max      28.267

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            GREEN
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.621
_exptl_crystal_F_000             694
_exptl_transmission_factor_min   0.653
_exptl_transmission_factor_max   0.727
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    3.102
_shelx_estimated_absorpt_T_min   0.653
_shelx_estimated_absorpt_T_max   0.727
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'sealed tube'
_diffrn_measurement_method       graphite
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6773
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_av_R_equivalents  0.0138
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.763
_diffrn_reflns_theta_max         28.267
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4504
_reflns_number_gt                4044
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0370P)²+1.7789P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4504
_refine_ls_number_parameters     262
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0253
_refine_ls_wR_factor_ref         0.0706
_refine_ls_wR_factor_gt          0.0680
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_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
Ni1 Ni 0.14000(6) -0.24094(5) 0.72098(4) 0.01448(10) Uani 1 1 d . . . . .
C1 C 0.4329(5) -0.3868(4) 1.0053(3) 0.0191(7) Uani 1 1 d . . . . .
O1 O 0.2801(4) -0.3071(3) 0.8286(2) 0.0216(5) Uani 1 1 d . . . . .
N1 N 0.1825(4) -0.0726(3) 0.8778(3) 0.0187(6) Uani 1 1 d . . . . .
O1W O -0.4226(6) -0.3518(6) 0.6896(5) 0.0841(16) Uani 1 1 d . . . . .
H1WA H -0.3229 -0.2984 0.7322 0.101 Uiso 1 1 d R U . . .
H1WB H -0.4771 -0.2956 0.6782 0.101 Uiso 1 1 d R U . . .
Mo1 Mo 0.44132(3) -0.00708(3) 0.61736(2) 0.01095(7) Uani 1 1 d . . . . .
Mo2 Mo 0.15578(3) -0.17635(3) 0.30716(2) 0.01199(7) Uani 1 1 d . . . . .
C2 C 0.5479(6) -0.3760(4) 1.0990(3) 0.0294(9) Uani 1 1 d . . . . .
H2B H 0.5798 -0.2898 1.1683 0.035 Uiso 1 1 d R U . . .
N2 N 0.1606(4) 0.0578(3) 0.9221(3) 0.0210(6) Uani 1 1 d . . . . .
H2A H 0.1112 0.0988 0.8801 0.025 Uiso 1 1 d R U . . .
O2 O -0.0054(3) -0.1695(3) 0.6239(2) 0.0208(5) Uani 1 1 d . . . . .
O2W O 0.3814(7) -0.4078(7) 0.4556(6) 0.1005(19) Uani 1 1 d . . . . .
H2WA H 0.2879 -0.4190 0.4830 0.121 Uiso 1 1 d R U . . .
H2WB H 0.4157 -0.3205 0.4580 0.121 Uiso 1 1 d R U . . .
Mo3 Mo -0.14170(3) -0.14549(3) 0.52191(2) 0.01188(7) Uani 1 1 d . . . . .
O3 O -0.2544(4) -0.3192(3) 0.4284(2) 0.0256(6) Uani 1 1 d . . . . .
N3 N 0.3708(4) -0.2658(3) 1.0182(3) 0.0202(6) Uani 1 1 d . . . . .
H3A H 0.3775 -0.2057 1.0911 0.024 Uiso 1 1 d R U . . .
C3 C 0.6163(6) -0.4884(4) 1.0943(3) 0.0296(9) Uani 1 1 d . . . . .
H3B H 0.6925 -0.4623 1.1667 0.044 Uiso 1 1 d R U . . .
O4 O -0.2980(3) -0.0785(3) 0.6053(2) 0.0161(5) Uani 1 1 d . . . . .
C4 C 0.3040(5) -0.2317(4) 0.9337(3) 0.0175(7) Uani 1 1 d . . . . .
O5 O 0.0395(3) -0.0953(2) 0.4290(2) 0.0137(4) Uani 1 1 d . . . . .
C5 C 0.2609(4) -0.0937(4) 0.9665(3) 0.0167(6) Uani 1 1 d . . . . .
O6 O 0.0245(3) -0.1756(3) 0.1927(2) 0.0242(6) Uani 1 1 d . . . . .
C6 C 0.2886(5) 0.0256(4) 1.0704(3) 0.0237(8) Uani 1 1 d . . . . .
H6A H 0.3412 0.0378 1.1465 0.028 Uiso 1 1 d R U . . .
O7 O -0.0877(4) -0.3597(3) 0.7526(3) 0.0274(6) Uani 1 1 d . . . . .
C7 C 0.2212(5) 0.1208(4) 1.0377(3) 0.0253(8) Uani 1 1 d . . . . .
H7A H 0.2195 0.2148 1.0878 0.030 Uiso 1 1 d R U . . .
O8 O 0.3643(3) -0.1318(3) 0.6812(2) 0.0187(5) Uani 1 1 d . . . . .
O9 O 0.0978(4) -0.3553(3) 0.2917(3) 0.0257(6) Uani 1 1 d . . . . .
O10 O 0.3740(3) -0.1386(3) 0.2541(2) 0.0149(5) Uani 1 1 d . . . . .
O11 O 0.3822(3) -0.1231(2) 0.4600(2) 0.0130(4) Uani 1 1 d . . . . .
O12 O 0.2917(3) 0.0867(3) 0.6256(2) 0.0174(5) Uani 1 1 d . . . . .
O13 O 0.1422(4) -0.4260(3) 0.5876(2) 0.0278(6) 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
Ni1 O2 2.044(2) . ?
Ni1 O8 2.051(2) . ?
Ni1 N1 2.056(3) . ?
Ni1 O7 2.061(3) . ?
Ni1 O13 2.065(3) . ?
Ni1 O1 2.071(2) . ?
C1 C2 1.382(5) . ?
C1 C3 1.383(5) 2_647 ?
C1 N3 1.419(4) . ?
O1 C4 1.247(4) . ?
N1 N2 1.328(4) . ?
N1 C5 1.336(4) . ?
Mo1 O12 1.717(2) . ?
Mo1 O8 1.730(2) . ?
Mo1 O11 1.863(2) . ?
Mo1 O10 1.951(2) 2_656 ?
Mo1 O11 2.196(2) 2_656 ?
Mo1 O4 2.398(2) 1_655 ?
Mo1 Mo2 3.1554(4) 2_656 ?
Mo1 Mo1 3.1962(5) 2_656 ?
Mo2 O9 1.702(3) . ?
Mo2 O6 1.706(2) . ?
Mo2 O10 1.920(2) . ?
Mo2 O5 1.923(2) . ?
Mo2 O11 2.331(2) . ?
Mo2 O4 2.362(2) 2_556 ?
Mo2 Mo1 3.1554(4) 2_656 ?
C2 C3 1.387(5) . ?
N2 C7 1.351(5) . ?
O2 Mo3 1.731(2) . ?
Mo3 O3 1.705(3) . ?
Mo3 O4 1.829(2) . ?
Mo3 O5 2.008(2) . ?
Mo3 O5 2.221(2) 2_556 ?
Mo3 O12 2.441(2) 2_556 ?
N3 C4 1.332(4) . ?
C3 C1 1.383(5) 2_647 ?
O4 Mo2 2.362(2) 2_556 ?
O4 Mo1 2.398(2) 1_455 ?
C4 C5 1.474(5) . ?
O5 Mo3 2.221(2) 2_556 ?
C5 C6 1.402(5) . ?
C6 C7 1.385(5) . ?
O10 Mo1 1.951(2) 2_656 ?
O11 Mo1 2.196(2) 2_656 ?
O12 Mo3 2.441(2) 2_556 ?

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 Ni1 O8 89.74(10) . . ?
O2 Ni1 N1 98.15(11) . . ?
O8 Ni1 N1 91.45(11) . . ?
O2 Ni1 O7 89.85(11) . . ?
O8 Ni1 O7 176.92(11) . . ?
N1 Ni1 O7 91.63(12) . . ?
O2 Ni1 O13 96.84(11) . . ?
O8 Ni1 O13 86.94(11) . . ?
N1 Ni1 O13 164.91(11) . . ?
O7 Ni1 O13 90.08(12) . . ?
O2 Ni1 O1 176.18(11) . . ?
O8 Ni1 O1 92.40(10) . . ?
N1 Ni1 O1 78.64(11) . . ?
O7 Ni1 O1 88.19(11) . . ?
O13 Ni1 O1 86.43(11) . . ?
C2 C1 C3 119.8(3) . 2_647 ?
C2 C1 N3 116.6(3) . . ?
C3 C1 N3 123.5(3) 2_647 . ?
C4 O1 Ni1 114.3(2) . . ?
N2 N1 C5 105.9(3) . . ?
N2 N1 Ni1 140.2(2) . . ?
C5 N1 Ni1 113.8(2) . . ?
O12 Mo1 O8 105.00(12) . . ?
O12 Mo1 O11 99.98(11) . . ?
O8 Mo1 O11 102.80(11) . . ?
O12 Mo1 O10 98.76(11) . 2_656 ?
O8 Mo1 O10 98.79(11) . 2_656 ?
O11 Mo1 O10 146.51(10) . 2_656 ?
O12 Mo1 O11 94.83(10) . 2_656 ?
O8 Mo1 O11 159.90(10) . 2_656 ?
O11 Mo1 O11 76.42(10) . 2_656 ?
O10 Mo1 O11 74.55(9) 2_656 2_656 ?
O12 Mo1 O4 164.61(10) . 1_655 ?
O8 Mo1 O4 88.89(10) . 1_655 ?
O11 Mo1 O4 82.96(9) . 1_655 ?
O10 Mo1 O4 72.11(9) 2_656 1_655 ?
O11 Mo1 O4 71.04(8) 2_656 1_655 ?
O12 Mo1 Mo2 117.86(8) . 2_656 ?
O8 Mo1 Mo2 117.36(8) . 2_656 ?
O11 Mo1 Mo2 111.49(7) . 2_656 ?
O10 Mo1 Mo2 35.06(7) 2_656 2_656 ?
O11 Mo1 Mo2 47.60(6) 2_656 2_656 ?
O4 Mo1 Mo2 47.98(6) 1_655 2_656 ?
O12 Mo1 Mo1 99.14(8) . 2_656 ?
O8 Mo1 Mo1 140.75(9) . 2_656 ?
O11 Mo1 Mo1 41.90(7) . 2_656 ?
O10 Mo1 Mo1 107.65(7) 2_656 2_656 ?
O11 Mo1 Mo1 34.52(6) 2_656 2_656 ?
O4 Mo1 Mo1 72.86(6) 1_655 2_656 ?
Mo2 Mo1 Mo1 75.539(11) 2_656 2_656 ?
O9 Mo2 O6 104.21(14) . . ?
O9 Mo2 O10 105.51(12) . . ?
O6 Mo2 O10 97.96(12) . . ?
O9 Mo2 O5 102.19(12) . . ?
O6 Mo2 O5 99.35(12) . . ?
O10 Mo2 O5 142.39(10) . . ?
O9 Mo2 O11 89.17(11) . . ?
O6 Mo2 O11 165.21(11) . . ?
O10 Mo2 O11 71.95(9) . . ?
O5 Mo2 O11 83.64(9) . . ?
O9 Mo2 O4 158.04(11) . 2_556 ?
O6 Mo2 O4 97.60(11) . 2_556 ?
O10 Mo2 O4 73.48(9) . 2_556 ?
O5 Mo2 O4 71.32(9) . 2_556 ?
O11 Mo2 O4 69.48(8) . 2_556 ?
O9 Mo2 Mo1 117.99(9) . 2_656 ?
O6 Mo2 Mo1 121.96(9) . 2_656 ?
O10 Mo2 Mo1 35.72(7) . 2_656 ?
O5 Mo2 Mo1 107.88(7) . 2_656 ?
O11 Mo2 Mo1 44.07(6) . 2_656 ?
O4 Mo2 Mo1 48.98(5) 2_556 2_656 ?
C1 C2 C3 120.8(4) . . ?
N1 N2 C7 111.7(3) . . ?
Mo3 O2 Ni1 168.31(17) . . ?
O3 Mo3 O2 104.00(13) . . ?
O3 Mo3 O4 106.37(12) . . ?
O2 Mo3 O4 102.17(11) . . ?
O3 Mo3 O5 98.34(12) . . ?
O2 Mo3 O5 97.07(10) . . ?
O4 Mo3 O5 143.66(10) . . ?
O3 Mo3 O5 153.45(11) . 2_556 ?
O2 Mo3 O5 101.06(11) . 2_556 ?
O4 Mo3 O5 76.38(10) . 2_556 ?
O5 Mo3 O5 69.81(10) . 2_556 ?
O3 Mo3 O12 81.36(11) . 2_556 ?
O2 Mo3 O12 171.00(10) . 2_556 ?
O4 Mo3 O12 82.91(9) . 2_556 ?
O5 Mo3 O12 74.82(9) . 2_556 ?
O5 Mo3 O12 72.70(8) 2_556 2_556 ?
C4 N3 C1 126.9(3) . . ?
C2 C3 C1 119.4(3) . 2_647 ?
Mo3 O4 Mo2 103.44(10) . 2_556 ?
Mo3 O4 Mo1 151.09(13) . 1_455 ?
Mo2 O4 Mo1 83.04(8) 2_556 1_455 ?
O1 C4 N3 124.0(3) . . ?
O1 C4 C5 118.0(3) . . ?
N3 C4 C5 117.9(3) . . ?
Mo2 O5 Mo3 144.14(13) . . ?
Mo2 O5 Mo3 105.61(10) . 2_556 ?
Mo3 O5 Mo3 110.19(10) . 2_556 ?
N1 C5 C6 111.0(3) . . ?
N1 C5 C4 114.2(3) . . ?
C6 C5 C4 134.7(3) . . ?
C7 C6 C5 103.9(3) . . ?
N2 C7 C6 107.4(3) . . ?
Mo1 O8 Ni1 142.20(14) . . ?
Mo2 O10 Mo1 109.22(11) . 2_656 ?
Mo1 O11 Mo1 103.58(10) . 2_656 ?
Mo1 O11 Mo2 135.82(11) . . ?
Mo1 O11 Mo2 88.33(8) 2_656 . ?
Mo1 O12 Mo3 130.64(13) . 2_556 ?

_refine_diff_density_max         0.850
_refine_diff_density_min         -1.042
_refine_diff_density_rms         0.134

####################################################################### 
# 
# 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 1940282'
loop_
_audit_author_name
_audit_author_address
'Xiang Pan'
;The Cambridge Crystallographic Data Centre
China
;
_audit_update_record             
;
2019-07-13 deposited with the CCDC.	2019-09-25 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            'C21 H22 Cd Mo4 N9 O18'
_chemical_formula_weight         1184.63

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'
Cd Cd -0.8075 1.2024 '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                   12.2427(5)
_cell_length_b                   12.7055(5)
_cell_length_c                   12.9947(5)
_cell_angle_alpha                117.2860(10)
_cell_angle_beta                 101.6580(10)
_cell_angle_gamma                104.9900(10)
_cell_volume                     1609.69(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4716
_cell_measurement_theta_min      1.856
_cell_measurement_theta_max      28.426

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.444
_exptl_crystal_F_000             1142
_exptl_transmission_factor_min   0.728
_exptl_transmission_factor_max   0.789
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    2.261
_shelx_estimated_absorpt_T_min   0.728
_shelx_estimated_absorpt_T_max   0.789
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'sealed tube'
_diffrn_measurement_method       graphite
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12065
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_av_R_equivalents  0.0173
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.856
_diffrn_reflns_theta_max         28.426
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8031
_reflns_number_gt                6530
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0211P)²+4.7524P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8031
_refine_ls_number_parameters     478
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0335
_refine_ls_wR_factor_ref         0.0734
_refine_ls_wR_factor_gt          0.0677
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_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
Cd1 Cd 0.14299(3) 0.34999(3) 0.73274(3) 0.02666(8) Uani 1 1 d . . . . .
Mo1 Mo 0.24981(3) 0.71140(3) 0.83785(3) 0.02221(8) Uani 1 1 d . . . . .
O1 O 0.3217(2) 0.3319(3) 0.7128(3) 0.0283(6) Uani 1 1 d . . . . .
C1 C 0.1468(4) 0.3694(5) 0.3985(5) 0.0426(12) Uani 1 1 d . . . . .
H1A H 0.1190 0.3784 0.3295 0.051 Uiso 1 1 d R U . . .
N1 N 0.1501(3) 0.3468(4) 0.5573(3) 0.0261(7) Uani 1 1 d . . . . .
O1W O 1.4767(3) 0.4011(4) 1.0201(3) 0.0453(9) Uani 1 1 d . . . . .
H1WB H 1.4954 0.3444 1.0276 0.054 Uiso 1 1 d R U . . .
Mo2 Mo 0.49837(3) 0.74072(3) 0.76815(3) 0.02267(8) Uani 1 1 d . . . . .
O2 O 0.9947(3) 0.3935(3) 0.7968(3) 0.0315(7) Uani 1 1 d . . . . .
C2 C 0.2545(4) 0.3601(5) 0.4372(5) 0.0375(11) Uani 1 1 d . . . . .
H2A H 0.3179 0.3639 0.4042 0.045 Uiso 1 1 d R U . . .
N2 N 0.0872(3) 0.3614(4) 0.4716(4) 0.0342(9) Uani 1 1 d . . . . .
H2B H 0.0171 0.3652 0.4646 0.041 Uiso 1 1 calc R U . . .
O2W O -0.1401(3) 0.3318(4) 0.4863(3) 0.0462(9) Uani 1 1 d . . . . .
H2WB H -0.1918 0.3150 0.4205 0.055 Uiso 1 1 d R U . . .
Mo3 Mo 0.75852(3) 1.02540(4) 0.94171(4) 0.02715(9) Uani 1 1 d . . . . .
C3 C 0.2529(3) 0.3457(4) 0.5374(4) 0.0221(8) Uani 1 1 d . . . . .
O3 O -0.1454(3) 0.1402(4) 0.5338(4) 0.0452(9) Uani 1 1 d . . . . .
N3 N 0.4383(3) 0.3215(3) 0.5955(3) 0.0225(7) Uani 1 1 d . . . . .
H3A H 0.4370 0.3078 0.5208 0.027 Uiso 1 1 d R U . . .
Mo4 Mo 0.42874(3) 1.04645(4) 0.90270(4) 0.03495(10) Uani 1 1 d . . . . .
O4 O 0.2511(3) 0.5757(3) 0.8363(3) 0.0326(7) Uani 1 1 d . . . . .
N4 N 0.8612(3) 0.3371(3) 0.8787(3) 0.0227(7) Uani 1 1 d . . . . .
H4A H 0.8526 0.3183 0.9363 0.027 Uiso 1 1 d R U . . .
C4 C 0.3406(3) 0.3318(4) 0.6218(4) 0.0217(8) Uani 1 1 d . . . . .
N5 N 1.1684(3) 0.3631(3) 0.9272(3) 0.0266(7) Uani 1 1 d . . . . .
C5 C 0.5441(3) 0.3279(4) 0.6721(4) 0.0204(8) Uani 1 1 d . . . . .
O5 O 0.4961(3) 0.6021(3) 0.7549(3) 0.0417(8) Uani 1 1 d . . . . .
C6 C 0.5439(4) 0.2949(5) 0.7592(4) 0.0311(10) Uani 1 1 d . . . . .
H6A H 0.4701 0.2670 0.7721 0.037 Uiso 1 1 d R U . . .
N6 N 1.2360(3) 0.3394(4) 1.0023(3) 0.0331(8) Uani 1 1 d . . . . .
H6B H 1.3088 0.3448 1.0085 0.040 Uiso 1 1 calc R U . . .
O6 O 0.6572(3) 0.8561(3) 0.8992(4) 0.0500(10) Uani 1 1 d . . . . .
C7 C 0.6507(4) 0.3017(5) 0.8272(4) 0.0320(10) Uani 1 1 d . . . . .
H7A H 0.6508 0.2797 0.8887 0.038 Uiso 1 1 d R U . . .
N7 N 0.0613(3) 0.1304(4) 0.6582(4) 0.0313(8) Uani 1 1 d . . . . .
O7 O 0.7593(3) 0.9881(3) 0.7992(3) 0.0440(8) Uani 1 1 d . . . . .
O8 O 0.5221(3) 0.7302(4) 0.6402(3) 0.0482(9) Uani 1 1 d . . . . .
C8 C 0.7579(3) 0.3397(4) 0.8089(4) 0.0211(8) Uani 1 1 d . . . . .
N8 N 0.1345(3) 0.0885(4) 0.7061(4) 0.0362(9) Uani 1 1 d . . . . .
H8A H 0.2123 0.1191 0.7267 0.043 Uiso 1 1 calc R U . . .
O9 O 0.5163(3) 0.9616(3) 0.8400(3) 0.0459(9) Uani 1 1 d . . . . .
C9 C 0.7577(4) 0.3750(5) 0.7218(4) 0.0300(9) Uani 1 1 d . . . . .
H9B H 0.8313 0.4032 0.7085 0.036 Uiso 1 1 d R U . . .
N9 N -0.2607(3) 0.0236(4) 0.5937(4) 0.0325(8) Uani 1 1 d . . . . .
H9A H -0.2538 -0.0146 0.6370 0.039 Uiso 1 1 d R U . . .
C10 C 0.6510(4) 0.3688(5) 0.6548(4) 0.0313(10) Uani 1 1 d . . . . .
H10A H 0.6504 0.3935 0.5951 0.038 Uiso 1 1 d R U . . .
O10 O 0.8974(3) 1.0518(3) 1.0253(3) 0.0385(8) Uani 1 1 d . . . . .
C11 C 0.9698(3) 0.3598(4) 0.8686(4) 0.0225(8) Uani 1 1 d . . . . .
O11 O 0.5387(3) 1.1914(3) 1.0473(3) 0.0274(6) Uani 1 1 d . . . . .
C12 C 1.0629(3) 0.3425(4) 0.9445(4) 0.0216(8) Uani 1 1 d . . . . .
O12 O 0.3669(3) 1.0900(3) 0.8077(3) 0.0428(9) Uani 1 1 d . . . . .
C13 C 1.0634(4) 0.3075(5) 1.0312(4) 0.0333(10) Uani 1 1 d . . . . .
H13A H 0.9999 0.2897 1.0613 0.040 Uiso 1 1 d R U . . .
O13 O 0.3310(2) 0.7127(3) 0.7250(3) 0.0267(6) Uani 1 1 d . . . . .
C14 C 1.1779(4) 0.3068(5) 1.0659(5) 0.0383(11) Uani 1 1 d . . . . .
H14A H 1.2089 0.2860 1.1249 0.046 Uiso 1 1 d R U . . .
O14 O 0.3052(3) 0.9256(3) 0.8986(3) 0.0304(7) Uani 1 1 d . . . . .
C15 C 0.0737(5) -0.0055(5) 0.7184(5) 0.0428(12) Uani 1 1 d . . . . .
H15A H 0.1080 -0.0506 0.7484 0.051 Uiso 1 1 d R U . . .
O15 O 0.1072(3) 0.6647(4) 0.7432(3) 0.0422(8) Uani 1 1 d . . . . .
C16 C -0.0464(4) -0.0270(5) 0.6783(5) 0.0393(11) Uani 1 1 d . . . . .
H16A H -0.1136 -0.0887 0.6755 0.047 Uiso 1 1 d R U . . .
O16 O 0.7601(3) 1.1955(3) 1.0011(3) 0.0287(6) Uani 1 1 d . . . . .
C17 C -0.0509(4) 0.0598(4) 0.6410(4) 0.0288(9) Uani 1 1 d . . . . .
C18 C -0.1563(4) 0.0800(4) 0.5851(4) 0.0282(9) Uani 1 1 d . . . . .
C19 C -0.3798(4) 0.0152(4) 0.5456(4) 0.0278(9) Uani 1 1 d . . . . .
C20 C -0.4149(4) 0.0444(5) 0.4574(4) 0.0358(10) Uani 1 1 d . . . . .
H20A H -0.3570 0.0753 0.4271 0.043 Uiso 1 1 d R U . . .
C21 C -0.5353(4) 0.0287(5) 0.4128(4) 0.0362(11) Uani 1 1 d . . . . .
H21A H -0.5460 0.0527 0.3526 0.054 Uiso 1 1 d R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 O2 2.237(3) 1_455 ?
Cd1 N1 2.282(3) . ?
Cd1 O1 2.312(3) . ?
Cd1 N7 2.326(4) . ?
Cd1 O4 2.359(3) . ?
Cd1 N5 2.404(3) 1_455 ?
Mo1 O15 1.686(3) . ?
Mo1 O4 1.720(3) . ?
Mo1 O16 1.924(3) 2_677 ?
Mo1 O13 1.934(3) . ?
Mo1 O14 2.312(3) . ?
Mo1 O11 2.356(3) 2_677 ?
O1 C4 1.250(5) . ?
C1 N2 1.334(6) . ?
C1 C2 1.369(6) . ?
N1 C3 1.337(5) . ?
N1 N2 1.335(5) . ?
Mo2 O5 1.682(3) . ?
Mo2 O8 1.696(3) . ?
Mo2 O13 1.901(3) . ?
Mo2 O6 1.931(3) . ?
Mo2 O11 2.334(3) 2_677 ?
Mo2 O9 2.448(3) . ?
O2 C11 1.248(5) . ?
O2 Cd1 2.237(3) 1_655 ?
C2 C3 1.399(6) . ?
Mo3 O10 1.676(3) . ?
Mo3 O7 1.691(3) . ?
Mo3 O16 1.926(3) . ?
Mo3 O6 1.930(3) . ?
Mo3 O14 2.241(3) 2_677 ?
C3 C4 1.479(5) . ?
O3 C18 1.223(5) . ?
N3 C4 1.330(5) . ?
N3 C5 1.424(5) . ?
Mo4 O12 1.695(3) . ?
Mo4 O9 1.766(4) . ?
Mo4 O11 1.805(3) . ?
Mo4 O14 1.827(3) . ?
N4 C11 1.333(5) . ?
N4 C8 1.418(5) . ?
N5 C12 1.336(5) . ?
N5 N6 1.341(5) . ?
N5 Cd1 2.404(3) 1_655 ?
C5 C6 1.374(5) . ?
C5 C10 1.382(5) . ?
C6 C7 1.380(6) . ?
N6 C14 1.327(6) . ?
C7 C8 1.384(5) . ?
N7 C17 1.340(5) . ?
N7 N8 1.341(5) . ?
C8 C9 1.395(5) . ?
N8 C15 1.329(6) . ?
C9 C10 1.377(6) . ?
N9 C18 1.348(5) . ?
N9 C19 1.421(5) . ?
C11 C12 1.482(5) . ?
O11 Mo2 2.334(3) 2_677 ?
O11 Mo1 2.356(3) 2_677 ?
C12 C13 1.387(6) . ?
C13 C14 1.387(6) . ?
O14 Mo3 2.242(3) 2_677 ?
C15 C16 1.364(7) . ?
C16 C17 1.400(6) . ?
O16 Mo1 1.924(3) 2_677 ?
C17 C18 1.492(6) . ?
C19 C21 1.374(6) 2_456 ?
C19 C20 1.382(6) . ?
C20 C21 1.394(6) . ?
C21 C19 1.374(6) 2_456 ?

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 Cd1 N1 117.63(11) 1_455 . ?
O2 Cd1 O1 167.43(11) 1_455 . ?
N1 Cd1 O1 72.50(11) . . ?
O2 Cd1 N7 96.37(12) 1_455 . ?
N1 Cd1 N7 101.89(13) . . ?
O1 Cd1 N7 88.24(12) . . ?
O2 Cd1 O4 86.80(11) 1_455 . ?
N1 Cd1 O4 84.77(12) . . ?
O1 Cd1 O4 86.82(11) . . ?
N7 Cd1 O4 170.12(12) . . ?
O2 Cd1 N5 70.06(11) 1_455 1_455 ?
N1 Cd1 N5 171.30(11) . 1_455 ?
O1 Cd1 N5 99.34(10) . 1_455 ?
N7 Cd1 N5 80.49(13) . 1_455 ?
O4 Cd1 N5 91.87(11) . 1_455 ?
O15 Mo1 O4 104.73(17) . . ?
O15 Mo1 O16 100.71(15) . 2_677 ?
O4 Mo1 O16 98.46(13) . 2_677 ?
O15 Mo1 O13 97.82(14) . . ?
O4 Mo1 O13 101.94(14) . . ?
O16 Mo1 O13 147.85(13) 2_677 . ?
O15 Mo1 O14 93.56(15) . . ?
O4 Mo1 O14 160.87(13) . . ?
O16 Mo1 O14 72.19(11) 2_677 . ?
O13 Mo1 O14 80.67(11) . . ?
O15 Mo1 O11 166.56(14) . 2_677 ?
O4 Mo1 O11 86.76(13) . 2_677 ?
O16 Mo1 O11 84.14(11) 2_677 2_677 ?
O13 Mo1 O11 72.58(11) . 2_677 ?
O14 Mo1 O11 75.87(10) . 2_677 ?
C4 O1 Cd1 115.4(2) . . ?
N2 C1 C2 108.0(4) . . ?
C3 N1 N2 106.0(3) . . ?
C3 N1 Cd1 114.7(3) . . ?
N2 N1 Cd1 138.7(3) . . ?
O5 Mo2 O8 104.40(18) . . ?
O5 Mo2 O13 102.83(15) . . ?
O8 Mo2 O13 101.09(14) . . ?
O5 Mo2 O6 98.25(15) . . ?
O8 Mo2 O6 102.88(17) . . ?
O13 Mo2 O6 142.81(15) . . ?
O5 Mo2 O11 91.69(14) . 2_677 ?
O8 Mo2 O11 163.86(15) . 2_677 ?
O13 Mo2 O11 73.66(11) . 2_677 ?
O6 Mo2 O11 75.45(14) . 2_677 ?
O5 Mo2 O9 166.44(15) . . ?
O8 Mo2 O9 87.93(16) . . ?
O13 Mo2 O9 79.84(12) . . ?
O6 Mo2 O9 73.09(13) . . ?
O11 Mo2 O9 76.19(12) 2_677 . ?
C11 O2 Cd1 116.7(3) . 1_655 ?
C1 C2 C3 104.5(4) . . ?
C1 N2 N1 111.4(4) . . ?
O10 Mo3 O7 106.21(17) . . ?
O10 Mo3 O16 104.71(15) . . ?
O7 Mo3 O16 97.90(15) . . ?
O10 Mo3 O6 103.60(15) . . ?
O7 Mo3 O6 99.26(18) . . ?
O16 Mo3 O6 141.06(15) . . ?
O10 Mo3 O14 93.72(14) . 2_677 ?
O7 Mo3 O14 159.88(14) . 2_677 ?
O16 Mo3 O14 73.81(11) . 2_677 ?
O6 Mo3 O14 78.21(15) . 2_677 ?
N1 C3 C2 110.1(4) . . ?
N1 C3 C4 117.0(3) . . ?
C2 C3 C4 132.8(4) . . ?
C4 N3 C5 126.9(3) . . ?
O12 Mo4 O9 110.05(17) . . ?
O12 Mo4 O11 108.36(15) . . ?
O9 Mo4 O11 104.13(14) . . ?
O12 Mo4 O14 108.18(14) . . ?
O9 Mo4 O14 103.53(14) . . ?
O11 Mo4 O14 122.09(13) . . ?
Mo1 O4 Cd1 143.98(17) . . ?
C11 N4 C8 127.0(3) . . ?
O1 C4 N3 123.6(4) . . ?
O1 C4 C3 120.1(3) . . ?
N3 C4 C3 116.3(3) . . ?
C12 N5 N6 104.6(3) . . ?
C12 N5 Cd1 110.6(3) . 1_655 ?
N6 N5 Cd1 139.5(3) . 1_655 ?
C6 C5 C10 119.9(4) . . ?
C6 C5 N3 123.7(3) . . ?
C10 C5 N3 116.5(3) . . ?
C5 C6 C7 119.4(4) . . ?
C14 N6 N5 112.4(4) . . ?
Mo3 O6 Mo2 127.35(17) . . ?
C6 C7 C8 121.4(4) . . ?
C17 N7 N8 104.8(4) . . ?
C17 N7 Cd1 127.0(3) . . ?
N8 N7 Cd1 115.8(3) . . ?
C7 C8 C9 118.9(4) . . ?
C7 C8 N4 117.2(3) . . ?
C9 C8 N4 124.0(3) . . ?
C15 N8 N7 112.7(4) . . ?
Mo4 O9 Mo2 132.54(18) . . ?
C10 C9 C8 119.4(4) . . ?
C18 N9 C19 130.2(4) . . ?
C9 C10 C5 121.1(4) . . ?
O2 C11 N4 122.3(4) . . ?
O2 C11 C12 119.5(3) . . ?
N4 C11 C12 118.2(3) . . ?
Mo4 O11 Mo2 120.73(13) . 2_677 ?
Mo4 O11 Mo1 138.56(15) . 2_677 ?
Mo2 O11 Mo1 90.31(10) 2_677 2_677 ?
N5 C12 C13 111.8(4) . . ?
N5 C12 C11 115.2(3) . . ?
C13 C12 C11 133.0(4) . . ?
C12 C13 C14 103.8(4) . . ?
Mo2 O13 Mo1 120.21(14) . . ?
N6 C14 C13 107.4(4) . . ?
Mo4 O14 Mo3 121.63(16) . 2_677 ?
Mo4 O14 Mo1 136.07(15) . . ?
Mo3 O14 Mo1 92.98(11) 2_677 . ?
N8 C15 C16 107.1(4) . . ?
C15 C16 C17 105.2(4) . . ?
Mo1 O16 Mo3 118.20(14) 2_677 . ?
N7 C17 C16 110.3(4) . . ?
N7 C17 C18 118.8(4) . . ?
C16 C17 C18 130.9(4) . . ?
O3 C18 N9 125.2(4) . . ?
O3 C18 C17 120.8(4) . . ?
N9 C18 C17 114.0(4) . . ?
C21 C19 C20 119.0(4) 2_456 . ?
C21 C19 N9 117.2(4) 2_456 . ?
C20 C19 N9 123.7(4) . . ?
C19 C20 C21 119.4(4) . . ?
C19 C21 C20 121.7(4) 2_456 . ?

_refine_diff_density_max         1.985
_refine_diff_density_min         -3.684
_refine_diff_density_rms         0.129

####################################################################### 
# 
# 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 1940281'
loop_
_audit_author_name
_audit_author_address
'Xiang Pan'
;The Cambridge Crystallographic Data Centre
China
;
_audit_update_record             
;
2019-07-13 deposited with the CCDC.	2019-09-25 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            'C14 H18 Mo4 N6 O18 Zn'
_chemical_formula_weight         1007.47

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Zn Zn 0.2839 1.4301 '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                   8.1287(11)
_cell_length_b                   11.5708(16)
_cell_length_c                   15.695(2)
_cell_angle_alpha                105.595(3)
_cell_angle_beta                 101.843(2)
_cell_angle_gamma                104.487(2)
_cell_volume                     1316.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2446
_cell_measurement_theta_min      1.931
_cell_measurement_theta_max      28.510

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.541
_exptl_crystal_F_000             972
_exptl_transmission_factor_min   0.675
_exptl_transmission_factor_max   0.745
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    2.846
_shelx_estimated_absorpt_T_min   0.675
_shelx_estimated_absorpt_T_max   0.745
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'sealed tube'
_diffrn_measurement_method       graphite
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9924
_diffrn_reflns_av_unetI/netI     0.0580
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.931
_diffrn_reflns_theta_max         28.510
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6608
_reflns_number_gt                5077
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0314P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6608
_refine_ls_number_parameters     388
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0361
_refine_ls_wR_factor_ref         0.0811
_refine_ls_wR_factor_gt          0.0729
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.013
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo -0.54009(5) -0.46827(4) -0.31661(3) 0.01270(9) Uani 1 1 d . . . . .
Zn1 Zn 0.32004(8) 0.03023(6) 0.12974(4) 0.02733(15) Uani 1 1 d . . . . .
O1 O 0.1277(5) -0.1443(3) 0.1047(2) 0.0306(9) Uani 1 1 d . . . . .
N1 N 0.3847(5) 0.0018(4) 0.2549(3) 0.0245(9) Uani 1 1 d . . . . .
C1 C 0.5151(7) -0.0243(5) 0.3839(4) 0.0306(12) Uani 1 1 d . . . . .
H1A H 0.5939 -0.0074 0.4413 0.037 Uiso 1 1 calc R U . . .
O1W O 0.2638(5) -0.0275(3) -0.0109(2) 0.0324(9) Uani 1 1 d . . . . .
H1WA H 0.3221 -0.0625 -0.0427 0.039 Uiso 1 1 d R U . . .
H1WB H 0.1576 -0.0505 -0.0451 0.039 Uiso 1 1 d R U . . .
Mo2 Mo 0.00186(5) -0.35089(4) -0.49331(3) 0.01259(9) Uani 1 1 d . . . . .
O2 O -0.5325(5) -0.8547(3) -0.0667(3) 0.0397(10) Uani 1 1 d . . . . .
C2 C 0.2985(6) -0.1147(4) 0.2538(3) 0.0213(10) Uani 1 1 d . . . . .
N2 N 0.5151(5) 0.0535(4) 0.3350(3) 0.0251(9) Uani 1 1 d . . . . .
H2A H 0.5903 0.1286 0.3528 0.030 Uiso 1 1 calc R U . . .
O2W O 0.5777(4) 0.1341(3) 0.1511(2) 0.0293(8) Uani 1 1 d . . . . .
H2WA H 0.6370 0.2125 0.1691 0.035 Uiso 1 1 d R U . . .
Mo3 Mo -0.13220(5) -0.44489(4) -0.32191(3) 0.01255(9) Uani 1 1 d . . . . .
O3 O -0.5492(4) -0.5920(3) -0.2765(2) 0.0235(8) Uani 1 1 d . . . . .
N3 N 0.0527(5) -0.3028(4) 0.1636(3) 0.0216(9) Uani 1 1 d . . . . .
H3A H 0.0799 -0.3230 0.2123 0.026 Uiso 1 1 calc R U . . .
C3 C 0.1514(6) -0.1901(5) 0.1684(3) 0.0234(11) Uani 1 1 d . . . . .
O3W O 0.1742(5) 0.1466(4) 0.1360(3) 0.0423(10) Uani 1 1 d . . . . .
H3WB H 0.1655 0.2046 0.1798 0.051 Uiso 1 1 d R U . . .
Mo4 Mo -0.39466(5) -0.34237(3) -0.47942(3) 0.01137(9) Uani 1 1 d . . . . .
O4 O -0.6223(4) -0.3731(3) -0.2467(2) 0.0230(7) Uani 1 1 d . . . . .
N4 N -0.5049(5) -0.6901(4) -0.1226(3) 0.0227(9) Uani 1 1 d . . . . .
H4A H -0.5446 -0.6705 -0.1700 0.027 Uiso 1 1 calc R U . . .
C4 C -0.0912(6) -0.3947(4) 0.0899(3) 0.0209(10) Uani 1 1 d . . . . .
O5 O -0.4061(4) -0.5289(3) -0.4260(2) 0.0123(6) Uani 1 1 d . . . . .
N5 N -0.9376(5) -1.0578(4) -0.2994(3) 0.0288(10) Uani 1 1 d . . . . .
H5A H -1.0060 -1.1354 -0.3221 0.035 Uiso 1 1 calc R U . . .
C5 C -0.1920(6) -0.4942(5) 0.1095(3) 0.0254(11) Uani 1 1 d . . . . .
H5B H -0.1678 -0.4939 0.1701 0.030 Uiso 1 1 calc R U . . .
O6 O -0.2867(4) -0.3755(3) -0.2605(2) 0.0161(7) Uani 1 1 d . . . . .
C6 C -0.3274(6) -0.5938(5) 0.0415(3) 0.0247(11) Uani 1 1 d . . . . .
H6B H -0.3926 -0.6607 0.0557 0.030 Uiso 1 1 calc R U . . .
N6 N -0.8029(5) -1.0109(4) -0.2204(3) 0.0264(9) Uani 1 1 d . . . . .
O7 O -0.4830(4) -0.3129(3) -0.3865(2) 0.0158(6) Uani 1 1 d . . . . .
C7 C -0.3648(6) -0.5925(4) -0.0486(3) 0.0208(10) Uani 1 1 d . . . . .
O8 O -0.3736(4) -0.2122(3) -0.5105(2) 0.0225(7) Uani 1 1 d . . . . .
C8 C -0.2660(7) -0.4928(5) -0.0687(4) 0.0286(12) Uani 1 1 d . . . . .
H8A H -0.2907 -0.4926 -0.1292 0.034 Uiso 1 1 calc R U . . .
O9 O -0.2788(4) -0.4470(3) -0.5685(2) 0.0145(6) Uani 1 1 d . . . . .
C9 C -0.1316(7) -0.3939(5) -0.0001(3) 0.0269(12) Uani 1 1 d . . . . .
H9A H -0.0677 -0.3263 -0.0141 0.032 Uiso 1 1 calc R U . . .
C10 C -0.5825(6) -0.8098(4) -0.1266(3) 0.0224(10) Uani 1 1 d . . . . .
O10 O -0.1479(4) -0.3083(3) -0.4064(2) 0.0140(6) Uani 1 1 d . . . . .
O11 O -0.1456(4) -0.5759(3) -0.2900(2) 0.0228(7) Uani 1 1 d . . . . .
C11 C -0.7347(6) -0.8877(4) -0.2100(3) 0.0191(10) Uani 1 1 d . . . . .
O12 O 0.0564(4) -0.3323(3) -0.2470(2) 0.0226(7) Uani 1 1 d . . . . .
C12 C -0.9535(7) -0.9704(5) -0.3387(4) 0.0337(13) Uani 1 1 d . . . . .
H12A H -1.0366 -0.9833 -0.3937 0.040 Uiso 1 1 calc R U . . .
O13 O 0.1916(4) -0.2741(3) -0.4038(2) 0.0219(7) Uani 1 1 d . . . . .
C13 C 0.3756(7) -0.1353(5) 0.3333(4) 0.0313(12) Uani 1 1 d . . . . .
H13A H 0.3413 -0.2077 0.3492 0.038 Uiso 1 1 calc R U . . .
O14 O 0.0539(4) -0.4900(3) -0.5686(2) 0.0145(6) Uani 1 1 d . . . . .
C14 C -0.8243(6) -0.8579(5) -0.2826(4) 0.0292(12) Uani 1 1 d . . . . .
H14A H -0.8018 -0.7796 -0.2912 0.035 Uiso 1 1 calc R U . . .
O15 O 0.0083(4) -0.2500(3) -0.5541(2) 0.0269(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
Mo1 O4 1.698(3) . ?
Mo1 O3 1.704(3) . ?
Mo1 O9 1.902(3) 2_444 ?
Mo1 O6 1.952(3) . ?
Mo1 O5 2.265(3) . ?
Mo1 O7 2.346(3) . ?
Mo1 Mo4 3.2062(7) 2_444 ?
Zn1 O3W 2.001(4) . ?
Zn1 O1W 2.041(3) . ?
Zn1 O2W 2.044(3) . ?
Zn1 N1 2.063(4) . ?
Zn1 O1 2.102(3) . ?
O1 C3 1.255(6) . ?
N1 N2 1.339(5) . ?
N1 C2 1.348(6) . ?
C1 N2 1.331(6) . ?
C1 C13 1.386(7) . ?
Mo2 O15 1.693(3) . ?
Mo2 O13 1.702(3) . ?
Mo2 O14 1.920(3) . ?
Mo2 O10 2.051(3) . ?
Mo2 O9 2.180(3) . ?
Mo2 O14 2.294(3) 2_544 ?
O2 C10 1.237(6) . ?
C2 C13 1.386(7) . ?
C2 C3 1.476(6) . ?
Mo3 O12 1.693(3) . ?
Mo3 O11 1.705(3) . ?
Mo3 O6 1.933(3) . ?
Mo3 O14 1.980(3) 2_544 ?
Mo3 O5 2.267(3) . ?
Mo3 O10 2.331(3) . ?
N3 C3 1.322(6) . ?
N3 C4 1.413(6) . ?
Mo4 O8 1.684(3) . ?
Mo4 O7 1.744(3) . ?
Mo4 O5 1.914(3) 2_444 ?
Mo4 O10 1.977(3) . ?
Mo4 O9 2.123(3) . ?
Mo4 O5 2.505(3) . ?
Mo4 Mo1 3.2062(7) 2_444 ?
N4 C10 1.349(6) . ?
N4 C7 1.424(6) . ?
C4 C5 1.383(6) . ?
C4 C9 1.387(6) . ?
O5 Mo4 1.914(3) 2_444 ?
N5 C12 1.336(7) . ?
N5 N6 1.347(5) . ?
C5 C6 1.379(6) . ?
C6 C7 1.389(6) . ?
N6 C11 1.344(6) . ?
C7 C8 1.384(6) . ?
C8 C9 1.376(7) . ?
O9 Mo1 1.902(3) 2_444 ?
C10 C11 1.483(6) . ?
C11 C14 1.395(7) . ?
C12 C14 1.376(7) . ?
O14 Mo3 1.980(3) 2_544 ?
O14 Mo2 2.294(3) 2_544 ?

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
O4 Mo1 O3 104.35(16) . . ?
O4 Mo1 O9 106.65(14) . 2_444 ?
O3 Mo1 O9 99.45(14) . 2_444 ?
O4 Mo1 O6 99.30(14) . . ?
O3 Mo1 O6 98.15(14) . . ?
O9 Mo1 O6 143.71(13) 2_444 . ?
O4 Mo1 O5 158.07(14) . . ?
O3 Mo1 O5 97.28(14) . . ?
O9 Mo1 O5 72.71(11) 2_444 . ?
O6 Mo1 O5 73.76(11) . . ?
O4 Mo1 O7 87.43(13) . . ?
O3 Mo1 O7 167.55(13) . . ?
O9 Mo1 O7 80.59(12) 2_444 . ?
O6 Mo1 O7 75.61(11) . . ?
O5 Mo1 O7 70.75(10) . . ?
O4 Mo1 Mo4 146.06(11) . 2_444 ?
O3 Mo1 Mo4 89.06(12) . 2_444 ?
O9 Mo1 Mo4 39.66(9) 2_444 2_444 ?
O6 Mo1 Mo4 109.62(9) . 2_444 ?
O5 Mo1 Mo4 36.02(7) . 2_444 ?
O7 Mo1 Mo4 83.08(8) . 2_444 ?
O3W Zn1 O1W 94.64(15) . . ?
O3W Zn1 O2W 108.45(15) . . ?
O1W Zn1 O2W 93.57(14) . . ?
O3W Zn1 N1 109.55(17) . . ?
O1W Zn1 N1 152.26(16) . . ?
O2W Zn1 N1 91.47(15) . . ?
O3W Zn1 O1 101.60(15) . . ?
O1W Zn1 O1 84.29(14) . . ?
O2W Zn1 O1 149.94(15) . . ?
N1 Zn1 O1 77.87(14) . . ?
C3 O1 Zn1 114.4(3) . . ?
N2 N1 C2 105.0(4) . . ?
N2 N1 Zn1 138.5(3) . . ?
C2 N1 Zn1 114.5(3) . . ?
N2 C1 C13 107.1(5) . . ?
O15 Mo2 O13 102.25(16) . . ?
O15 Mo2 O14 103.85(15) . . ?
O13 Mo2 O14 103.59(13) . . ?
O15 Mo2 O10 106.67(14) . . ?
O13 Mo2 O10 90.60(13) . . ?
O14 Mo2 O10 142.59(12) . . ?
O15 Mo2 O9 89.35(14) . . ?
O13 Mo2 O9 160.42(14) . . ?
O14 Mo2 O9 88.59(12) . . ?
O10 Mo2 O9 70.81(11) . . ?
O15 Mo2 O14 169.61(14) . 2_544 ?
O13 Mo2 O14 88.14(13) . 2_544 ?
O14 Mo2 O14 73.13(13) . 2_544 ?
O10 Mo2 O14 72.95(11) . 2_544 ?
O9 Mo2 O14 80.70(11) . 2_544 ?
N1 C2 C13 110.8(4) . . ?
N1 C2 C3 113.6(4) . . ?
C13 C2 C3 135.6(5) . . ?
C1 N2 N1 112.4(4) . . ?
O12 Mo3 O11 105.35(16) . . ?
O12 Mo3 O6 94.15(14) . . ?
O11 Mo3 O6 100.77(14) . . ?
O12 Mo3 O14 102.34(14) . 2_544 ?
O11 Mo3 O14 94.59(14) . 2_544 ?
O6 Mo3 O14 153.63(12) . 2_544 ?
O12 Mo3 O5 158.44(13) . . ?
O11 Mo3 O5 94.70(13) . . ?
O6 Mo3 O5 74.03(11) . . ?
O14 Mo3 O5 83.52(11) 2_544 . ?
O12 Mo3 O10 87.75(13) . . ?
O11 Mo3 O10 164.04(14) . . ?
O6 Mo3 O10 87.05(11) . . ?
O14 Mo3 O10 73.36(11) 2_544 . ?
O5 Mo3 O10 73.93(10) . . ?
C3 N3 C4 129.2(4) . . ?
O1 C3 N3 123.9(4) . . ?
O1 C3 C2 118.4(4) . . ?
N3 C3 C2 117.7(4) . . ?
O8 Mo4 O7 104.44(15) . . ?
O8 Mo4 O5 104.87(14) . 2_444 ?
O7 Mo4 O5 101.28(13) . 2_444 ?
O8 Mo4 O10 101.19(14) . . ?
O7 Mo4 O10 97.10(13) . . ?
O5 Mo4 O10 142.99(12) 2_444 . ?
O8 Mo4 O9 101.81(14) . . ?
O7 Mo4 O9 153.39(13) . . ?
O5 Mo4 O9 75.86(12) 2_444 . ?
O10 Mo4 O9 73.41(11) . . ?
O8 Mo4 O5 176.27(13) . . ?
O7 Mo4 O5 75.51(12) . . ?
O5 Mo4 O5 78.73(12) 2_444 . ?
O10 Mo4 O5 75.17(11) . . ?
O9 Mo4 O5 78.01(10) . . ?
O8 Mo4 Mo1 94.98(12) . 2_444 ?
O7 Mo4 Mo1 144.32(10) . 2_444 ?
O5 Mo4 Mo1 44.09(8) 2_444 2_444 ?
O10 Mo4 Mo1 108.27(9) . 2_444 ?
O9 Mo4 Mo1 34.87(8) . 2_444 ?
O5 Mo4 Mo1 86.98(7) . 2_444 ?
C10 N4 C7 127.4(4) . . ?
C5 C4 C9 118.8(4) . . ?
C5 C4 N3 116.8(4) . . ?
C9 C4 N3 124.3(4) . . ?
Mo4 O5 Mo1 99.89(11) 2_444 . ?
Mo4 O5 Mo3 156.91(15) 2_444 . ?
Mo1 O5 Mo3 92.68(11) . . ?
Mo4 O5 Mo4 101.27(11) 2_444 . ?
Mo1 O5 Mo4 95.19(10) . . ?
Mo3 O5 Mo4 96.74(10) . . ?
C12 N5 N6 112.6(4) . . ?
C6 C5 C4 121.7(4) . . ?
Mo3 O6 Mo1 115.09(15) . . ?
C5 C6 C7 118.8(4) . . ?
C11 N6 N5 104.1(4) . . ?
Mo4 O7 Mo1 118.31(15) . . ?
C8 C7 C6 119.9(4) . . ?
C8 C7 N4 117.6(4) . . ?
C6 C7 N4 122.5(4) . . ?
C9 C8 C7 120.6(5) . . ?
Mo1 O9 Mo4 105.47(13) 2_444 . ?
Mo1 O9 Mo2 149.08(16) 2_444 . ?
Mo4 O9 Mo2 100.08(12) . . ?
C8 C9 C4 120.1(4) . . ?
O2 C10 N4 123.9(5) . . ?
O2 C10 C11 120.9(4) . . ?
N4 C10 C11 115.2(4) . . ?
Mo4 O10 Mo2 109.95(14) . . ?
Mo4 O10 Mo3 111.69(13) . . ?
Mo2 O10 Mo3 103.02(12) . . ?
N6 C11 C14 111.6(4) . . ?
N6 C11 C10 116.4(4) . . ?
C14 C11 C10 132.0(4) . . ?
N5 C12 C14 107.3(5) . . ?
C1 C13 C2 104.7(5) . . ?
Mo2 O14 Mo3 146.44(16) . 2_544 ?
Mo2 O14 Mo2 106.87(13) . 2_544 ?
Mo3 O14 Mo2 106.67(13) 2_544 2_544 ?
C12 C14 C11 104.4(5) . . ?

_refine_diff_density_max         0.730
_refine_diff_density_min         -0.865
_refine_diff_density_rms         0.165

####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1940283'
loop_
_audit_author_name
_audit_author_address
'Xiang Pan'
;The Cambridge Crystallographic Data Centre
China
;
_audit_update_record             
;
2019-07-13 deposited with the CCDC.	2019-09-25 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            'C10 H14 Mo3 N6 O13 Zn'
_chemical_formula_weight         779.46

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'
Zn Zn 0.2839 1.4301 '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                   12.9855(5)
_cell_length_b                   19.6775(7)
_cell_length_c                   7.6312(3)
_cell_angle_alpha                90
_cell_angle_beta                 102.9260(10)
_cell_angle_gamma                90
_cell_volume                     1900.53(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6397
_cell_measurement_theta_min      1.609
_cell_measurement_theta_max      28.263

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.724
_exptl_crystal_F_000             1504
_exptl_transmission_factor_min   0.640
_exptl_transmission_factor_max   0.715
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    3.267
_shelx_estimated_absorpt_T_min   0.640
_shelx_estimated_absorpt_T_max   0.715
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'sealed tube'
_diffrn_measurement_method       graphite
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13794
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_av_R_equivalents  0.0200
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         1.609
_diffrn_reflns_theta_max         28.263
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4701
_reflns_number_gt                4069
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0306P)²+2.6599P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4701
_refine_ls_number_parameters     298
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0228
_refine_ls_wR_factor_ref         0.0608
_refine_ls_wR_factor_gt          0.0578
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo -0.02926(2) 0.35276(2) 0.02688(3) 0.01271(6) Uani 1 1 d . . . . .
Zn1 Zn 0.28352(3) 0.36700(2) -0.37617(5) 0.02243(9) Uani 1 1 d . . . . .
O1 O 0.19031(16) 0.32047(10) -0.1863(3) 0.0195(4) Uani 1 1 d . . . . .
C1 C 0.3760(3) 0.21983(17) -0.3201(5) 0.0308(7) Uani 1 1 d . . . . .
H1A H 0.3154 0.1952 -0.3844 0.037 Uiso 1 1 d R U . . .
O1W O 0.5745(4) 0.0817(2) -0.0580(6) 0.1148(19) Uani 1 1 d . . . . .
H1WA H 0.5934 0.0731 -0.1553 0.138 Uiso 1 1 d R U . . .
H1WB H 0.6257 0.1017 0.0121 0.138 Uiso 1 1 d R U . . .
N1 N 0.1925(2) 0.45203(12) -0.3876(3) 0.0208(5) Uani 1 1 d . . . . .
Mo2 Mo -0.17276(2) 0.25174(2) 0.22949(3) 0.01214(6) Uani 1 1 d . . . . .
O2 O 0.33304(18) 0.41971(11) -0.5874(3) 0.0254(5) Uani 1 1 d . . . . .
N2 N 0.3837(2) 0.28706(14) -0.3102(3) 0.0235(5) Uani 1 1 d . . . . .
C2 C 0.4822(2) 0.30070(17) -0.2041(4) 0.0255(7) Uani 1 1 d . . . . .
Mo3 Mo 0.10609(2) 0.25326(2) -0.18281(3) 0.01026(6) Uani 1 1 d . . . . .
O3 O 0.43010(19) 0.41335(13) -0.1945(3) 0.0348(6) Uani 1 1 d . . . . .
C3 C 0.5332(3) 0.24121(18) -0.1513(5) 0.0332(8) Uani 1 1 d . . . . .
H3A H 0.6028 0.2357 -0.0769 0.040 Uiso 1 1 d R U . . .
N3 N 0.7160(2) 0.49339(14) -0.2203(4) 0.0274(6) Uani 1 1 d . . . . .
H3B H 0.7504 0.4534 -0.2016 0.033 Uiso 1 1 d R U . . .
O4 O -0.02837(15) 0.31481(10) -0.2106(2) 0.0136(4) Uani 1 1 d . . . . .
C4 C 0.5041(2) 0.37174(16) -0.1566(4) 0.0236(6) Uani 1 1 d . . . . .
N4 N 0.0984(2) 0.54448(14) -0.3867(4) 0.0299(6) Uani 1 1 d . . . . .
H4A H 0.0550 0.5750 -0.3529 0.036 Uiso 1 1 d R U . . .
O5 O 0.08167(15) 0.26645(10) 0.0691(2) 0.0144(4) Uani 1 1 d . . . . .
N5 N 0.4652(2) 0.19144(15) -0.2261(4) 0.0366(7) Uani 1 1 d . . . . .
H5B H 0.4783 0.1466 -0.2148 0.044 Uiso 1 1 d R U . . .
C5 C 0.1437(3) 0.55062(16) -0.5298(4) 0.0272(7) Uani 1 1 d . . . . .
H5A H 0.1365 0.5879 -0.6129 0.033 Uiso 1 1 d R U . . .
O6 O 0.07455(19) 0.40789(11) 0.0643(3) 0.0295(5) Uani 1 1 d . . . . .
C6 C 0.6302(3) 0.45401(16) 0.0161(4) 0.0258(7) Uani 1 1 d . . . . .
H6A H 0.6970 0.4494 0.0999 0.031 Uiso 1 1 d R U . . .
H6B H 0.5786 0.4664 0.0829 0.031 Uiso 1 1 d R U . . .
N6 N 0.6013(2) 0.38842(14) -0.0690(4) 0.0294(6) Uani 1 1 d . . . . .
H6C H 0.6524 0.3571 -0.0632 0.035 Uiso 1 1 d R U . . .
O7 O -0.13879(19) 0.40394(11) -0.0239(3) 0.0271(5) Uani 1 1 d . . . . .
C7 C 0.6398(3) 0.51056(17) -0.1145(5) 0.0280(7) Uani 1 1 d . . . . .
H7A H 0.5720 0.5179 -0.1935 0.034 Uiso 1 1 d R U . . .
H7B H 0.6609 0.5519 -0.0497 0.034 Uiso 1 1 d R U . . .
O8 O -0.03079(15) 0.32044(10) 0.2645(2) 0.0138(4) Uani 1 1 d . . . . .
C8 C 0.2763(2) 0.47049(15) -0.6381(4) 0.0221(6) Uani 1 1 d . . . . .
O9 O -0.25447(17) 0.31970(12) 0.2247(3) 0.0251(5) Uani 1 1 d . . . . .
C9 C 0.1293(3) 0.48470(17) -0.3024(4) 0.0262(7) Uani 1 1 d . . . . .
H9A H 0.1083 0.4682 -0.1973 0.031 Uiso 1 1 d R U . . .
O10 O -0.14063(16) 0.23838(10) 0.4879(2) 0.0155(4) Uani 1 1 d . . . . .
C10 C 0.2012(2) 0.49302(15) -0.5317(4) 0.0204(6) Uani 1 1 d . . . . .
O11 O -0.25690(17) 0.18487(11) 0.1641(3) 0.0244(5) Uani 1 1 d . . . . .
O12 O 0.18944(16) 0.18806(10) -0.0904(2) 0.0184(4) 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 O6 1.704(2) . ?
Mo1 O7 1.715(2) . ?
Mo1 O8 1.9261(18) . ?
Mo1 O4 1.9625(18) . ?
Mo1 O5 2.2035(19) . ?
Mo1 O10 2.281(2) 4_565 ?
Zn1 N2 2.031(3) . ?
Zn1 N1 2.039(3) . ?
Zn1 O12 2.1084(19) 4_565 ?
Zn1 O2 2.133(2) . ?
Zn1 O1 2.277(2) . ?
Zn1 O3 2.279(2) . ?
O1 Mo3 1.720(2) . ?
C1 N2 1.328(4) . ?
C1 N5 1.341(4) . ?
N1 C9 1.322(4) . ?
N1 C10 1.389(4) . ?
Mo2 O9 1.702(2) . ?
Mo2 O11 1.712(2) . ?
Mo2 O10 1.9400(18) . ?
Mo2 O10 1.9888(18) 4_565 ?
Mo2 O4 2.2485(19) 4_566 ?
Mo2 O8 2.2533(19) . ?
O2 C8 1.251(4) . ?
N2 C2 1.379(4) . ?
C2 C3 1.361(5) . ?
C2 C4 1.456(4) . ?
Mo3 O12 1.7244(19) . ?
Mo3 O5 1.8890(18) 4_565 ?
Mo3 O5 2.0334(18) . ?
Mo3 O4 2.0964(19) . ?
Mo3 O8 2.2593(19) 4_565 ?
O3 C4 1.246(4) . ?
C3 N5 1.356(5) . ?
N3 C8 1.316(4) 3_664 ?
N3 C7 1.450(4) . ?
O4 Mo2 2.2485(19) 4_565 ?
C4 N6 1.331(4) . ?
N4 C5 1.356(4) . ?
N4 C9 1.358(4) . ?
O5 Mo3 1.8890(18) 4_566 ?
C5 C10 1.360(4) . ?
C6 N6 1.456(4) . ?
C6 C7 1.517(4) . ?
O8 Mo3 2.2594(19) 4_566 ?
C8 N3 1.316(4) 3_664 ?
C8 C10 1.469(4) . ?
O10 Mo2 1.9887(18) 4_566 ?
O10 Mo1 2.281(2) 4_566 ?
O12 Zn1 2.1084(19) 4_566 ?

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 Mo1 O7 104.43(12) . . ?
O6 Mo1 O8 103.12(9) . . ?
O7 Mo1 O8 102.94(9) . . ?
O6 Mo1 O4 103.24(9) . . ?
O7 Mo1 O4 100.99(9) . . ?
O8 Mo1 O4 138.34(8) . . ?
O6 Mo1 O5 89.97(10) . . ?
O7 Mo1 O5 165.39(10) . . ?
O8 Mo1 O5 75.64(7) . . ?
O4 Mo1 O5 72.72(7) . . ?
O6 Mo1 O10 167.71(10) . 4_565 ?
O7 Mo1 O10 87.86(10) . 4_565 ?
O8 Mo1 O10 73.94(7) . 4_565 ?
O4 Mo1 O10 73.43(7) . 4_565 ?
O5 Mo1 O10 77.74(7) . 4_565 ?
N2 Zn1 N1 168.21(10) . . ?
N2 Zn1 O12 91.25(9) . 4_565 ?
N1 Zn1 O12 99.13(9) . 4_565 ?
N2 Zn1 O2 106.21(9) . . ?
N1 Zn1 O2 80.72(9) . . ?
O12 Zn1 O2 83.36(8) 4_565 . ?
N2 Zn1 O1 86.16(9) . . ?
N1 Zn1 O1 88.37(9) . . ?
O12 Zn1 O1 89.34(7) 4_565 . ?
O2 Zn1 O1 165.70(8) . . ?
N2 Zn1 O3 75.99(10) . . ?
N1 Zn1 O3 95.46(9) . . ?
O12 Zn1 O3 159.60(9) 4_565 . ?
O2 Zn1 O3 85.02(9) . . ?
O1 Zn1 O3 105.33(8) . . ?
Mo3 O1 Zn1 138.53(11) . . ?
N2 C1 N5 109.9(3) . . ?
C9 N1 C10 106.1(3) . . ?
C9 N1 Zn1 142.7(2) . . ?
C10 N1 Zn1 111.17(19) . . ?
O9 Mo2 O11 104.09(11) . . ?
O9 Mo2 O10 96.86(9) . . ?
O11 Mo2 O10 99.80(9) . . ?
O9 Mo2 O10 99.35(9) . 4_565 ?
O11 Mo2 O10 93.30(9) . 4_565 ?
O10 Mo2 O10 156.00(12) . 4_565 ?
O9 Mo2 O4 161.66(9) . 4_566 ?
O11 Mo2 O4 93.47(9) . 4_566 ?
O10 Mo2 O4 74.60(7) . 4_566 ?
O10 Mo2 O4 84.67(7) 4_565 4_566 ?
O9 Mo2 O8 91.19(9) . . ?
O11 Mo2 O8 161.38(9) . . ?
O10 Mo2 O8 88.65(7) . . ?
O10 Mo2 O8 73.47(7) 4_565 . ?
O4 Mo2 O8 72.68(7) 4_566 . ?
C8 O2 Zn1 111.5(2) . . ?
C1 N2 C2 106.0(3) . . ?
C1 N2 Zn1 136.2(2) . . ?
C2 N2 Zn1 117.0(2) . . ?
C3 C2 N2 109.4(3) . . ?
C3 C2 C4 134.2(3) . . ?
N2 C2 C4 115.9(3) . . ?
O1 Mo3 O12 103.61(10) . . ?
O1 Mo3 O5 96.14(9) . 4_565 ?
O12 Mo3 O5 101.91(9) . 4_565 ?
O1 Mo3 O5 98.67(9) . . ?
O12 Mo3 O5 85.69(8) . . ?
O5 Mo3 O5 161.27(11) 4_565 . ?
O1 Mo3 O4 94.15(9) . . ?
O12 Mo3 O4 154.64(8) . . ?
O5 Mo3 O4 93.90(8) 4_565 . ?
O5 Mo3 O4 73.70(7) . . ?
O1 Mo3 O8 165.55(8) . 4_565 ?
O12 Mo3 O8 89.54(8) . 4_565 ?
O5 Mo3 O8 74.98(7) 4_565 4_565 ?
O5 Mo3 O8 88.13(7) . 4_565 ?
O4 Mo3 O8 75.43(7) . 4_565 ?
C4 O3 Zn1 112.0(2) . . ?
N5 C3 C2 105.6(3) . . ?
C8 N3 C7 121.2(3) 3_664 . ?
Mo1 O4 Mo3 107.65(8) . . ?
Mo1 O4 Mo2 103.45(8) . 4_565 ?
Mo3 O4 Mo2 108.78(8) . 4_565 ?
O3 C4 N6 123.4(3) . . ?
O3 C4 C2 118.4(3) . . ?
N6 C4 C2 118.2(3) . . ?
C5 N4 C9 108.9(3) . . ?
Mo3 O5 Mo3 153.46(11) 4_566 . ?
Mo3 O5 Mo1 105.21(8) 4_566 . ?
Mo3 O5 Mo1 101.27(8) . . ?
C1 N5 C3 109.1(3) . . ?
N4 C5 C10 105.8(3) . . ?
N6 C6 C7 114.1(3) . . ?
C4 N6 C6 124.3(3) . . ?
N3 C7 C6 111.2(3) . . ?
Mo1 O8 Mo2 105.48(8) . . ?
Mo1 O8 Mo3 101.90(8) . 4_566 ?
Mo2 O8 Mo3 103.08(8) . 4_566 ?
O2 C8 N3 122.5(3) . 3_664 ?
O2 C8 C10 119.2(3) . . ?
N3 C8 C10 118.2(3) 3_664 . ?
N1 C9 N4 109.8(3) . . ?
Mo2 O10 Mo2 152.50(11) . 4_566 ?
Mo2 O10 Mo1 103.00(8) . 4_566 ?
Mo2 O10 Mo1 102.37(8) 4_566 4_566 ?
C5 C10 N1 109.5(3) . . ?
C5 C10 C8 133.7(3) . . ?
N1 C10 C8 116.4(3) . . ?
Mo3 O12 Zn1 154.32(11) . 4_566 ?

_refine_diff_density_max         0.832
_refine_diff_density_min         -1.319
_refine_diff_density_rms         0.107

