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

####################################################################### 
# 
# 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 1510385'
_audit_update_record             
;
2016-12-22 deposited with the CCDC.
2017-01-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C13 H16 Mo4 N2 O13'
_chemical_formula_weight         792.04

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   10.929(2)
_cell_length_b                   9.7226(19)
_cell_length_c                   19.633(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.82(3)
_cell_angle_gamma                90.00
_cell_volume                     2041.8(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    19051
_cell_measurement_theta_min      3.125
_cell_measurement_theta_max      27.52

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.577
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1520
_exptl_absorpt_coefficient_mu    2.473
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5242
_exptl_absorpt_correction_T_max  0.6376
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 Higashi, T. (1995) A program for absorption correction.
RIGAKU corporation, Tokyo, Japan. 
;

_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX area-detector diffractometer'
_diffrn_measurement_method       'φ and ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            15506
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0197
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.13
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3588
_reflns_number_gt                3392
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXS-97 (Sheldrick, 1990)'
_computing_publication_material  'SHELXS-97 (Sheldrick, 1990)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
During the refinement, the command 'omit -3 50' was used to omit the weak
 reflections above 50 degree. 
 The highest residual peak and the deepest hole are both close to the 
 heavy metal centers and featureless.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0696P)²+2.3300P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       shelxl
_refine_ls_number_reflns         3588
_refine_ls_number_parameters     289
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0252
_refine_ls_wR_factor_ref         0.0833
_refine_ls_wR_factor_gt          0.0813
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_restrained_S_all      0.951
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.003

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.07218(3) 0.69558(3) 0.065242(15) 0.01406(11) Uani 1 1 d . . .
Mo2 Mo -0.17729(3) 0.66748(3) -0.071961(16) 0.01594(11) Uani 1 1 d . . .
Mo3 Mo 0.25847(3) 0.95384(3) 0.073582(17) 0.01689(12) Uani 1 1 d . . .
Mo4 Mo 0.02279(3) 0.91605(3) -0.076455(15) 0.01421(11) Uani 1 1 d . . .
O1 O -0.1675(2) 0.8680(3) -0.06760(14) 0.0185(5) Uani 1 1 d . . .
O2 O -0.0535(2) 1.0891(3) -0.05154(13) 0.0158(5) Uani 1 1 d . . .
O3 O 0.2378(2) 0.7645(3) 0.05412(14) 0.0193(6) Uani 1 1 d . . .
O4 O 0.0276(2) 0.7312(3) -0.05629(13) 0.0174(5) Uani 1 1 d . . .
O5 O -0.0025(3) 0.9270(3) -0.16401(14) 0.0263(6) Uani 1 1 d . . .
O6 O -0.0969(2) 0.6820(3) 0.03947(13) 0.0179(6) Uani 1 1 d . . .
O7 O 0.0883(3) 0.6974(3) 0.15229(15) 0.0276(7) Uani 1 1 d . . .
O8 O 0.1162(3) 0.5223(3) 0.04800(14) 0.0208(6) Uani 1 1 d . . .
O9 O 0.1785(2) 0.9712(3) -0.04878(14) 0.0218(6) Uani 1 1 d . . .
O10 O 0.2902(3) 0.9491(3) 0.16192(15) 0.0277(7) Uani 1 1 d . . .
O11 O -0.1873(3) 0.6435(3) -0.15839(15) 0.0315(7) Uani 1 1 d . . .
O12 O 0.3957(3) 1.0014(3) 0.05182(17) 0.0306(7) Uani 1 1 d . . .
O13 O -0.3253(3) 0.6480(3) -0.05889(17) 0.0312(7) Uani 1 1 d . . .
N2 N -0.2028(3) 0.0353(4) -0.40096(18) 0.0276(8) Uani 1 1 d . . .
H2 H -0.1731 -0.0345 -0.4211 0.033 Uiso 1 1 calc R . .
N1 N -0.7227(4) 0.1788(4) -0.1159(2) 0.0344(9) Uani 1 1 d . . .
H1 H -0.7692 0.1240 -0.0960 0.041 Uiso 1 1 calc R . .
C1 C -0.5771(4) 0.3435(4) -0.1787(2) 0.0229(8) Uani 1 1 d . . .
C17 C -0.1423(4) 0.0764(5) -0.3390(2) 0.0305(10) Uani 1 1 d . . .
H17A H -0.0674 0.0313 -0.3171 0.037 Uiso 1 1 calc R . .
C18 C -0.6069(5) 0.2070(5) -0.0818(2) 0.0349(11) Uani 1 1 d . . .
H18A H -0.5762 0.1691 -0.0370 0.042 Uiso 1 1 calc R . .
C19 C -0.5321(4) 0.2914(5) -0.1121(2) 0.0292(10) Uani 1 1 d . . .
H19A H -0.4502 0.3140 -0.0878 0.035 Uiso 1 1 calc R . .
C2 C -0.1874(5) 0.1842(5) -0.3060(2) 0.0358(11) Uani 1 1 d . . .
H2A H -0.1447 0.2122 -0.2611 0.043 Uiso 1 1 calc R . .
C21 C -0.6989(4) 0.3139(5) -0.2115(2) 0.0279(9) Uani 1 1 d . . .
H21A H -0.7324 0.3509 -0.2562 0.034 Uiso 1 1 calc R . .
C22 C -0.3069(5) 0.0961(5) -0.4337(2) 0.0342(11) Uani 1 1 d . . .
H22A H -0.3477 0.0645 -0.4784 0.041 Uiso 1 1 calc R . .
C23 C -0.4906(4) 0.4180(4) -0.2168(2) 0.0258(9) Uani 1 1 d . . .
H23A H -0.4218 0.4623 -0.1834 0.031 Uiso 1 1 calc R . .
H23B H -0.5368 0.4899 -0.2475 0.031 Uiso 1 1 calc R . .
C24 C -0.2948(4) 0.2515(5) -0.3385(2) 0.0305(10) Uani 1 1 d . . .
C25 C -0.4385(4) 0.3092(4) -0.2604(3) 0.0325(10) Uani 1 1 d . . .
H25A H -0.3956 0.2368 -0.2288 0.039 Uiso 1 1 calc R . .
H25B H -0.5091 0.2654 -0.2927 0.039 Uiso 1 1 calc R . .
C26 C -0.3558(5) 0.2041(5) -0.4034(2) 0.0371(11) Uani 1 1 d . . .
H26A H -0.4312 0.2465 -0.4266 0.045 Uiso 1 1 calc R . .
C27 C -0.3475(5) 0.3668(5) -0.3021(2) 0.0353(11) Uani 1 1 d . . .
H27A H -0.3912 0.4334 -0.3369 0.042 Uiso 1 1 calc R . .
H27B H -0.2788 0.4156 -0.2707 0.042 Uiso 1 1 calc R . .
C28 C -0.7715(5) 0.2301(5) -0.1789(2) 0.0358(11) Uani 1 1 d . . .
H28A H -0.8552 0.2092 -0.2009 0.043 Uiso 1 1 calc R . .


_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 O7 1.682(3) . ?
Mo1 O8 1.803(3) . ?
Mo1 O6 1.818(3) . ?
Mo1 O3 1.983(3) . ?
Mo1 O2 2.116(3) 3_575 ?
Mo1 O4 2.361(3) . ?
Mo1 Mo3 3.2156(6) . ?
Mo2 O11 1.694(3) . ?
Mo2 O13 1.699(3) . ?
Mo2 O1 1.953(3) . ?
Mo2 O8 1.986(3) 3_565 ?
Mo2 O6 2.189(3) . ?
Mo2 O4 2.282(3) . ?
Mo3 O10 1.698(3) . ?
Mo3 O12 1.705(3) . ?
Mo3 O3 1.885(3) . ?
Mo3 O1 1.989(3) 3_575 ?
Mo3 O2 2.232(3) 3_575 ?
Mo3 O9 2.388(3) . ?
Mo4 O5 1.688(3) . ?
Mo4 O9 1.760(3) . ?
Mo4 O4 1.839(3) . ?
Mo4 O2 1.983(3) . ?
Mo4 O1 2.172(3) . ?
Mo4 O2 2.467(3) 3_575 ?
O1 Mo3 1.989(3) 3_575 ?
O2 Mo1 2.116(3) 3_575 ?
O2 Mo3 2.232(3) 3_575 ?
O2 Mo4 2.467(3) 3_575 ?
O8 Mo2 1.986(3) 3_565 ?
N2 C17 1.322(6) . ?
N2 C22 1.325(6) . ?
N2 H2 0.8800 . ?
N1 C18 1.333(7) . ?
N1 C28 1.339(6) . ?
N1 H1 0.8800 . ?
C1 C21 1.385(6) . ?
C1 C19 1.394(6) . ?
C1 C23 1.506(5) . ?
C17 C2 1.374(7) . ?
C17 H17A 0.9500 . ?
C18 C19 1.376(7) . ?
C18 H18A 0.9500 . ?
C19 H19A 0.9500 . ?
C2 C24 1.381(7) . ?
C2 H2A 0.9500 . ?
C21 C28 1.382(6) . ?
C21 H21A 0.9500 . ?
C22 C26 1.369(7) . ?
C22 H22A 0.9500 . ?
C23 C25 1.541(6) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C26 1.390(6) . ?
C24 C27 1.505(6) . ?
C25 C27 1.519(6) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9500 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O7 Mo1 O8 102.96(14) . . ?
O7 Mo1 O6 99.92(14) . . ?
O8 Mo1 O6 100.07(12) . . ?
O7 Mo1 O3 101.57(14) . . ?
O8 Mo1 O3 90.60(12) . . ?
O6 Mo1 O3 153.16(11) . . ?
O7 Mo1 O2 96.09(13) . 3_575 ?
O8 Mo1 O2 157.44(12) . 3_575 ?
O6 Mo1 O2 88.29(11) . 3_575 ?
O3 Mo1 O2 73.65(10) . 3_575 ?
O7 Mo1 O4 169.20(13) . . ?
O8 Mo1 O4 87.43(11) . . ?
O6 Mo1 O4 75.03(10) . . ?
O3 Mo1 O4 80.99(11) . . ?
O2 Mo1 O4 74.44(10) 3_575 . ?
O7 Mo1 Mo3 90.39(11) . . ?
O8 Mo1 Mo3 123.28(9) . . ?
O6 Mo1 Mo3 131.89(8) . . ?
O3 Mo1 Mo3 32.80(8) . . ?
O2 Mo1 Mo3 43.73(7) 3_575 . ?
O4 Mo1 Mo3 86.24(7) . . ?
O11 Mo2 O13 105.53(16) . . ?
O11 Mo2 O1 99.97(13) . . ?
O13 Mo2 O1 98.63(13) . . ?
O11 Mo2 O8 93.37(13) . 3_565 ?
O13 Mo2 O8 98.34(13) . 3_565 ?
O1 Mo2 O8 154.71(11) . 3_565 ?
O11 Mo2 O6 160.13(13) . . ?
O13 Mo2 O6 93.20(13) . . ?
O1 Mo2 O6 83.38(11) . . ?
O8 Mo2 O6 77.09(10) 3_565 . ?
O11 Mo2 O4 91.88(13) . . ?
O13 Mo2 O4 161.37(13) . . ?
O1 Mo2 O4 71.30(10) . . ?
O8 Mo2 O4 86.98(10) 3_565 . ?
O6 Mo2 O4 70.49(9) . . ?
O10 Mo3 O12 104.93(16) . . ?
O10 Mo3 O3 99.86(13) . . ?
O12 Mo3 O3 106.82(14) . . ?
O10 Mo3 O1 94.53(13) . 3_575 ?
O12 Mo3 O1 101.77(13) . 3_575 ?
O3 Mo3 O1 143.23(11) . 3_575 ?
O10 Mo3 O2 100.33(13) . 3_575 ?
O12 Mo3 O2 154.33(13) . 3_575 ?
O3 Mo3 O2 72.78(10) . 3_575 ?
O1 Mo3 O2 71.42(10) 3_575 3_575 ?
O10 Mo3 O9 170.15(12) . . ?
O12 Mo3 O9 83.59(13) . . ?
O3 Mo3 O9 82.01(11) . . ?
O1 Mo3 O9 78.67(10) 3_575 . ?
O2 Mo3 O9 70.86(9) 3_575 . ?
O10 Mo3 Mo1 91.44(11) . . ?
O12 Mo3 Mo1 141.17(11) . . ?
O3 Mo3 Mo1 34.74(8) . . ?
O1 Mo3 Mo1 111.92(8) 3_575 . ?
O2 Mo3 Mo1 40.92(7) 3_575 . ?
O9 Mo3 Mo1 84.63(7) . . ?
O5 Mo4 O9 103.98(15) . . ?
O5 Mo4 O4 105.82(13) . . ?
O9 Mo4 O4 104.37(12) . . ?
O5 Mo4 O2 102.01(13) . . ?
O9 Mo4 O2 95.39(12) . . ?
O4 Mo4 O2 140.45(11) . . ?
O5 Mo4 O1 97.77(13) . . ?
O9 Mo4 O1 157.10(11) . . ?
O4 Mo4 O1 75.99(11) . . ?
O2 Mo4 O1 72.86(10) . . ?
O5 Mo4 O2 177.05(12) . 3_575 ?
O9 Mo4 O2 76.74(11) . 3_575 ?
O4 Mo4 O2 76.64(10) . 3_575 ?
O2 Mo4 O2 75.05(11) . 3_575 ?
O1 Mo4 O2 81.18(10) . 3_575 ?
Mo2 O1 Mo3 147.59(15) . 3_575 ?
Mo2 O1 Mo4 104.84(11) . . ?
Mo3 O1 Mo4 106.45(12) 3_575 . ?
Mo4 O2 Mo1 147.46(14) . 3_575 ?
Mo4 O2 Mo3 104.44(11) . 3_575 ?
Mo1 O2 Mo3 95.35(10) 3_575 3_575 ?
Mo4 O2 Mo4 104.95(11) . 3_575 ?
Mo1 O2 Mo4 97.99(10) 3_575 3_575 ?
Mo3 O2 Mo4 96.61(10) 3_575 3_575 ?
Mo3 O3 Mo1 112.46(13) . . ?
Mo4 O4 Mo2 104.63(12) . . ?
Mo4 O4 Mo1 110.60(12) . . ?
Mo2 O4 Mo1 95.17(10) . . ?
Mo1 O6 Mo2 117.38(13) . . ?
Mo1 O8 Mo2 155.99(16) . 3_565 ?
Mo4 O9 Mo3 114.87(13) . . ?
C17 N2 C22 121.9(4) . . ?
C17 N2 H2 119.0 . . ?
C22 N2 H2 119.0 . . ?
C18 N1 C28 122.9(4) . . ?
C18 N1 H1 118.6 . . ?
C28 N1 H1 118.5 . . ?
C21 C1 C19 118.7(4) . . ?
C21 C1 C23 120.7(4) . . ?
C19 C1 C23 120.3(4) . . ?
N2 C17 C2 120.3(4) . . ?
N2 C17 H17A 119.9 . . ?
C2 C17 H17A 119.9 . . ?
N1 C18 C19 119.6(4) . . ?
N1 C18 H18A 120.2 . . ?
C19 C18 H18A 120.2 . . ?
C18 C19 C1 119.7(4) . . ?
C18 C19 H19A 120.2 . . ?
C1 C19 H19A 120.2 . . ?
C17 C2 C24 119.8(4) . . ?
C17 C2 H2A 120.1 . . ?
C24 C2 H2A 120.1 . . ?
C28 C21 C1 119.7(4) . . ?
C28 C21 H21A 120.1 . . ?
C1 C21 H21A 120.1 . . ?
N2 C22 C26 120.3(4) . . ?
N2 C22 H22A 119.8 . . ?
C26 C22 H22A 119.8 . . ?
C1 C23 C25 106.7(3) . . ?
C1 C23 H23A 110.4 . . ?
C25 C23 H23A 110.4 . . ?
C1 C23 H23B 110.4 . . ?
C25 C23 H23B 110.4 . . ?
H23A C23 H23B 108.6 . . ?
C2 C24 C26 117.9(4) . . ?
C2 C24 C27 120.4(4) . . ?
C26 C24 C27 121.6(4) . . ?
C27 C25 C23 113.8(4) . . ?
C27 C25 H25A 108.8 . . ?
C23 C25 H25A 108.8 . . ?
C27 C25 H25B 108.8 . . ?
C23 C25 H25B 108.8 . . ?
H25A C25 H25B 107.7 . . ?
C22 C26 C24 119.7(5) . . ?
C22 C26 H26A 120.1 . . ?
C24 C26 H26A 120.1 . . ?
C24 C27 C25 109.7(4) . . ?
C24 C27 H27A 109.7 . . ?
C25 C27 H27A 109.7 . . ?
C24 C27 H27B 109.7 . . ?
C25 C27 H27B 109.7 . . ?
H27A C27 H27B 108.2 . . ?
N1 C28 C21 119.3(4) . . ?
N1 C28 H28A 120.3 . . ?
C21 C28 H28A 120.3 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.565
_refine_diff_density_min         -1.121
_refine_diff_density_rms         0.164
####################################################################### 
# 
# 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 1510386'
_audit_update_record             
;
2016-12-22 deposited with the CCDC.
2017-01-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H18 Mo11 N6 O35'
_chemical_formula_weight         1933.72

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2/c

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

_cell_length_a                   13.2348(10)
_cell_length_b                   5.4270(4)
_cell_length_c                   29.837(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.396(2)
_cell_angle_gamma                90.00
_cell_volume                     2129.7(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    42876
_cell_measurement_theta_min      3.0005
_cell_measurement_theta_max      28.2533

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.016
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1820
_exptl_absorpt_coefficient_mu    3.237
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.335
_exptl_absorpt_correction_T_max  0.445
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 Higashi, T. (1995) A program for absorption correction.
RIGAKU corporation, Tokyo, Japan.
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX area-detector diffractometer'
_diffrn_measurement_method       'φ and ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            32836
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_sigmaI/netI    0.0215
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         2.75
_diffrn_reflns_theta_max         24.99
_reflns_number_total             3748
_reflns_number_gt                3116
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXS-97 (Sheldrick, 1990)'
_computing_publication_material  'SHELXS-97 (Sheldrick, 1990)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
During the refinement, the command 'omit -3 50' was used to omit the weak
 reflections above 50 degree. 
 The highest residual peak and the deepest hole are both close to the 
 heavy metal centers and featureless.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1000P)²+37.9574P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00091(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3748
_refine_ls_number_parameters     322
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0341
_refine_ls_wR_factor_ref         0.1503
_refine_ls_wR_factor_gt          0.1367
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_restrained_S_all      0.948
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 1.0000 0.34021(16) 0.2500 0.0055(2) Uani 1 2 d S . .
Mo2 Mo 1.07957(5) -0.60702(11) 0.436415(19) 0.0050(2) Uani 1 1 d . . .
Mo3 Mo 0.88363(5) -0.92810(11) 0.472502(19) 0.0059(2) Uani 1 1 d . . .
Mo4 Mo 1.04596(5) -0.14109(11) 0.345992(19) 0.0051(2) Uani 1 1 d . . .
Mo5 Mo 0.84815(5) -0.46688(11) 0.380085(19) 0.0062(2) Uani 1 1 d . . .
Mo6 Mo 0.82087(5) -0.00105(12) 0.28772(2) 0.0093(2) Uani 1 1 d . . .
O17 O 1.0560(4) -0.8866(9) 0.47534(17) 0.0085(11) Uani 1 1 d . . .
O16 O 1.0801(4) -0.3793(10) 0.47691(17) 0.0119(11) Uani 1 1 d . . .
O15 O 0.9898(4) 0.0245(9) 0.29565(17) 0.0101(11) Uani 1 1 d . . .
O14 O 0.8710(4) -0.1876(10) 0.34387(17) 0.0119(11) Uani 1 1 d . . .
O13 O 1.0199(4) -0.4183(9) 0.38586(16) 0.0082(11) Uani 1 1 d . . .
O12 O 0.9068(4) -0.6564(9) 0.43311(17) 0.0087(11) Uani 1 1 d . . .
O11 O 1.0148(4) 0.5357(10) 0.29580(17) 0.0130(12) Uani 1 1 d . . .
O10 O 0.8734(4) -1.1665(10) 0.43377(17) 0.0131(12) Uani 1 1 d . . .
O9 O 0.8586(4) 0.2472(9) 0.24740(17) 0.0104(11) Uani 1 1 d . . .
O8 O 1.0500(4) -0.9096(10) 0.38635(18) 0.0143(12) Uani 1 1 d . . .
O7 O 1.2026(4) -0.6266(11) 0.4280(2) 0.0199(13) Uani 1 1 d . . .
O6 O 0.7633(4) -0.8856(11) 0.4833(2) 0.0201(13) Uani 1 1 d . . .
O5 O 0.7237(5) -0.4600(11) 0.3865(2) 0.0211(13) Uani 1 1 d . . .
O4 O 0.8554(4) -0.6931(10) 0.34086(17) 0.0117(11) Uani 1 1 d . . .
O3 O 0.8052(5) -0.2484(11) 0.25302(18) 0.0216(13) Uani 1 1 d . . .
O2 O 0.6998(5) 0.0790(12) 0.2950(2) 0.0237(14) Uani 1 1 d . . .
O1 O 1.1696(4) -0.1813(11) 0.33949(19) 0.0183(13) Uani 1 1 d . . .
N2 N 0.4174(6) 0.2553(15) 0.3574(3) 0.0281(18) Uani 1 1 d . . .
N1 N 0.5342(7) -0.4451(16) 0.4916(3) 0.036(2) Uani 1 1 d . . .
C9 C 0.4449(8) 0.0761(17) 0.3922(3) 0.027(2) Uani 1 1 d . . .
N3 N 0.3275(7) 0.4497(16) 0.3044(3) 0.039(2) Uani 1 1 d . . .
H3 H 0.2761 0.4933 0.2847 0.047 Uiso 1 1 calc R . .
C8 C 0.4964(8) -0.2682(18) 0.4578(3) 0.032(2) Uani 1 1 d . . .
C7 C 0.3710(8) -0.045(2) 0.4131(3) 0.033(2) Uani 1 1 d . . .
H7A H 0.3013 -0.0073 0.4048 0.040 Uiso 1 1 calc R . .
C6 C 0.5736(7) -0.1498(18) 0.4378(3) 0.033(2) Uani 1 1 d . . .
H6A H 0.6430 -0.1874 0.4468 0.040 Uiso 1 1 calc R . .
C5 C 0.5469(7) 0.0250(19) 0.4041(4) 0.035(2) Uani 1 1 d . . .
H5A H 0.5978 0.1073 0.3897 0.042 Uiso 1 1 calc R . .
O1W O 0.5000 0.001(3) 0.2500 0.077(5) Uani 1 2 d S . .
C4 C 0.3969(7) -0.217(2) 0.4453(3) 0.033(2) Uani 1 1 d . . .
H4A H 0.3456 -0.3014 0.4590 0.039 Uiso 1 1 calc R . .
C3 C 0.4179(9) 0.564(2) 0.3109(4) 0.041(3) Uani 1 1 d . . .
H3A H 0.4375 0.7042 0.2949 0.049 Uiso 1 1 calc R . .
C2 C 0.3282(7) 0.262(2) 0.3325(3) 0.036(2) Uani 1 1 d . . .
H2A H 0.2738 0.1495 0.3344 0.043 Uiso 1 1 calc R . .
C1 C 0.4757(8) 0.445(2) 0.3437(4) 0.040(3) Uani 1 1 d . . .
H1A H 0.5436 0.4842 0.3553 0.048 Uiso 1 1 calc R . .
H1O H 0.438(9) 0.07(2) 0.244(4) 0.06(4) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 O11 1.724(5) 2_755 ?
Mo1 O11 1.724(5) . ?
Mo1 O9 1.931(5) 2_755 ?
Mo1 O9 1.931(5) . ?
Mo1 O15 2.202(5) 2_755 ?
Mo1 O15 2.202(5) . ?
Mo2 O7 1.678(6) . ?
Mo2 O16 1.728(5) . ?
Mo2 O13 1.919(5) . ?
Mo2 O17 1.957(5) . ?
Mo2 O8 2.225(6) . ?
Mo2 O12 2.293(5) . ?
Mo3 O6 1.676(6) . ?
Mo3 O10 1.730(5) . ?
Mo3 O12 1.931(5) . ?
Mo3 O17 1.948(5) 3_736 ?
Mo3 O16 2.265(5) 3_746 ?
Mo3 O17 2.284(5) . ?
Mo4 O1 1.683(6) . ?
Mo4 O8 1.737(5) 1_565 ?
Mo4 O15 1.835(5) . ?
Mo4 O13 1.972(5) . ?
Mo4 O11 2.313(5) 1_545 ?
Mo4 O14 2.323(5) . ?
Mo5 O5 1.680(6) . ?
Mo5 O4 1.706(5) . ?
Mo5 O14 1.905(5) . ?
Mo5 O12 1.972(5) . ?
Mo5 O13 2.275(5) . ?
Mo5 O10 2.284(5) 1_565 ?
Mo6 O3 1.694(6) . ?
Mo6 O2 1.697(6) . ?
Mo6 O9 1.910(5) . ?
Mo6 O14 2.006(5) . ?
Mo6 O15 2.226(5) . ?
Mo6 O4 2.314(5) 1_565 ?
O17 Mo3 1.948(5) 3_736 ?
O16 Mo3 2.265(5) 3_746 ?
O11 Mo4 2.313(5) 1_565 ?
O10 Mo5 2.284(5) 1_545 ?
O8 Mo4 1.737(5) 1_545 ?
O4 Mo6 2.314(5) 1_545 ?
N2 C2 1.324(12) . ?
N2 C1 1.376(12) . ?
N2 C9 1.439(12) . ?
N1 N1 1.236(17) 3_646 ?
N1 C8 1.440(12) . ?
C9 C7 1.383(14) . ?
C9 C5 1.386(14) . ?
N3 C2 1.318(13) . ?
N3 C3 1.342(14) . ?
C8 C4 1.357(13) . ?
C8 C6 1.396(14) . ?
C7 C4 1.355(14) . ?
C6 C5 1.398(14) . ?
C3 C1 1.339(15) . ?

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
O11 Mo1 O11 104.0(4) 2_755 . ?
O11 Mo1 O9 102.5(2) 2_755 2_755 ?
O11 Mo1 O9 96.0(2) . 2_755 ?
O11 Mo1 O9 96.0(2) 2_755 . ?
O11 Mo1 O9 102.5(2) . . ?
O9 Mo1 O9 149.7(3) 2_755 . ?
O11 Mo1 O15 89.89(19) 2_755 2_755 ?
O11 Mo1 O15 163.7(2) . 2_755 ?
O9 Mo1 O15 72.3(2) 2_755 2_755 ?
O9 Mo1 O15 84.1(2) . 2_755 ?
O11 Mo1 O15 163.7(2) 2_755 . ?
O11 Mo1 O15 89.89(19) . . ?
O9 Mo1 O15 84.1(2) 2_755 . ?
O9 Mo1 O15 72.3(2) . . ?
O15 Mo1 O15 77.8(3) 2_755 . ?
O7 Mo2 O16 102.8(3) . . ?
O7 Mo2 O13 103.8(3) . . ?
O16 Mo2 O13 97.9(2) . . ?
O7 Mo2 O17 105.2(3) . . ?
O16 Mo2 O17 97.4(2) . . ?
O13 Mo2 O17 143.2(2) . . ?
O7 Mo2 O8 87.4(3) . . ?
O16 Mo2 O8 169.7(3) . . ?
O13 Mo2 O8 80.8(2) . . ?
O17 Mo2 O8 78.4(2) . . ?
O7 Mo2 O12 164.9(2) . . ?
O16 Mo2 O12 92.3(2) . . ?
O13 Mo2 O12 73.0(2) . . ?
O17 Mo2 O12 73.2(2) . . ?
O8 Mo2 O12 77.6(2) . . ?
O6 Mo3 O10 103.1(3) . . ?
O6 Mo3 O12 103.4(3) . . ?
O10 Mo3 O12 99.8(2) . . ?
O6 Mo3 O17 103.4(3) . 3_736 ?
O10 Mo3 O17 98.2(2) . 3_736 ?
O12 Mo3 O17 143.3(2) . 3_736 ?
O6 Mo3 O16 84.6(3) . 3_746 ?
O10 Mo3 O16 172.3(3) . 3_746 ?
O12 Mo3 O16 78.9(2) . 3_746 ?
O17 Mo3 O16 79.1(2) 3_736 3_746 ?
O6 Mo3 O17 161.0(3) . . ?
O10 Mo3 O17 95.8(2) . . ?
O12 Mo3 O17 73.8(2) . . ?
O17 Mo3 O17 72.7(2) 3_736 . ?
O16 Mo3 O17 76.5(2) 3_746 . ?
O1 Mo4 O8 102.6(3) . 1_565 ?
O1 Mo4 O15 106.2(3) . . ?
O8 Mo4 O15 101.1(2) 1_565 . ?
O1 Mo4 O13 102.0(3) . . ?
O8 Mo4 O13 97.3(2) 1_565 . ?
O15 Mo4 O13 141.7(2) . . ?
O1 Mo4 O11 86.1(2) . 1_545 ?
O8 Mo4 O11 170.6(3) 1_565 1_545 ?
O15 Mo4 O11 79.31(19) . 1_545 ?
O13 Mo4 O11 77.4(2) . 1_545 ?
O1 Mo4 O14 164.1(2) . . ?
O8 Mo4 O14 92.9(2) 1_565 . ?
O15 Mo4 O14 73.7(2) . . ?
O13 Mo4 O14 72.1(2) . . ?
O11 Mo4 O14 78.15(19) 1_545 . ?
O5 Mo5 O4 103.0(3) . . ?
O5 Mo5 O14 105.4(3) . . ?
O4 Mo5 O14 99.2(2) . . ?
O5 Mo5 O12 103.0(3) . . ?
O4 Mo5 O12 97.3(2) . . ?
O14 Mo5 O12 142.8(2) . . ?
O5 Mo5 O13 166.6(2) . . ?
O4 Mo5 O13 90.2(2) . . ?
O14 Mo5 O13 74.4(2) . . ?
O12 Mo5 O13 72.5(2) . . ?
O5 Mo5 O10 88.5(3) . 1_565 ?
O4 Mo5 O10 168.4(3) . 1_565 ?
O14 Mo5 O10 79.0(2) . 1_565 ?
O12 Mo5 O10 78.22(19) . 1_565 ?
O13 Mo5 O10 78.30(19) . 1_565 ?
O3 Mo6 O2 103.2(3) . . ?
O3 Mo6 O9 101.3(2) . . ?
O2 Mo6 O9 102.5(3) . . ?
O3 Mo6 O14 96.7(2) . . ?
O2 Mo6 O14 104.6(3) . . ?
O9 Mo6 O14 142.8(2) . . ?
O3 Mo6 O15 99.6(3) . . ?
O2 Mo6 O15 157.2(3) . . ?
O9 Mo6 O15 72.1(2) . . ?
O14 Mo6 O15 73.0(2) . . ?
O3 Mo6 O4 173.0(2) . 1_565 ?
O2 Mo6 O4 81.1(3) . 1_565 ?
O9 Mo6 O4 82.9(2) . 1_565 ?
O14 Mo6 O4 76.7(2) . 1_565 ?
O15 Mo6 O4 76.29(19) . 1_565 ?
Mo3 O17 Mo2 142.7(3) 3_736 . ?
Mo3 O17 Mo3 107.3(2) 3_736 . ?
Mo2 O17 Mo3 106.2(2) . . ?
Mo2 O16 Mo3 167.7(3) . 3_746 ?
Mo4 O15 Mo1 147.2(3) . . ?
Mo4 O15 Mo6 111.5(2) . . ?
Mo1 O15 Mo6 96.5(2) . . ?
Mo5 O14 Mo6 144.8(3) . . ?
Mo5 O14 Mo4 106.9(2) . . ?
Mo6 O14 Mo4 101.8(2) . . ?
Mo2 O13 Mo4 142.8(3) . . ?
Mo2 O13 Mo5 108.6(2) . . ?
Mo4 O13 Mo5 106.5(2) . . ?
Mo3 O12 Mo5 144.2(3) . . ?
Mo3 O12 Mo2 106.7(2) . . ?
Mo5 O12 Mo2 106.0(2) . . ?
Mo1 O11 Mo4 167.4(3) . 1_565 ?
Mo3 O10 Mo5 175.4(3) . 1_545 ?
Mo6 O9 Mo1 118.7(3) . . ?
Mo4 O8 Mo2 171.4(3) 1_545 . ?
Mo5 O4 Mo6 165.4(3) . 1_545 ?
C2 N2 C1 107.9(8) . . ?
C2 N2 C9 124.2(8) . . ?
C1 N2 C9 127.9(8) . . ?
N1 N1 C8 113.2(11) 3_646 . ?
C7 C9 C5 120.5(9) . . ?
C7 C9 N2 120.8(9) . . ?
C5 C9 N2 118.7(9) . . ?
C2 N3 C3 108.8(9) . . ?
C4 C8 C6 121.4(9) . . ?
C4 C8 N1 125.4(9) . . ?
C6 C8 N1 113.2(9) . . ?
C4 C7 C9 120.7(9) . . ?
C8 C6 C5 118.8(9) . . ?
C9 C5 C6 118.7(9) . . ?
C7 C4 C8 119.9(10) . . ?
N3 C3 C1 108.1(9) . . ?
N3 C2 N2 108.7(9) . . ?
C3 C1 N2 106.5(9) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.362
_refine_diff_density_min         -1.434
_refine_diff_density_rms         0.186
