# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2012


data_global
_journal_name_full               'Dalton Trans.'
_journal_coden_cambridge         0222
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
_publ_contact_author_name        'Yongheng Xing'
_publ_contact_author_email       yhxing2000@yahoo.com
loop_
_publ_author_name
'Na Xing'
'Hui Shan'
'Xing Tian'
'Qiang Yao'
'Li-Ting Xu'
'Yongheng Xing'
'Shi Zhan'

data_1
_database_code_depnum_ccdc_archive 'CCDC 891375'
#TrackingRef '- 1.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H22 B2 Mo2 N12 O6'
_chemical_formula_weight         715.98

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'
B B 0.0013 0.0007 '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'

_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                   7.6897(13)
_cell_length_b                   12.978(2)
_cell_length_c                   14.815(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.387(3)
_cell_angle_gamma                90.00
_cell_volume                     1466.1(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    2311
_cell_measurement_theta_min      2.09
_cell_measurement_theta_max      24.08

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             712
_exptl_absorpt_coefficient_mu    0.909
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9082
_exptl_absorpt_correction_T_max  0.9383
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      273(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 AXS SMART APEX II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6550
_diffrn_reflns_av_R_equivalents  0.0699
_diffrn_reflns_av_sigmaI/netI    0.0806
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.09
_diffrn_reflns_theta_max         24.08
_reflns_number_total             2311
_reflns_number_gt                1517
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger. The oxygen atom (O1W) of the lattice water molecule is disordered and modeled over two split positions with occupancy in ratio of 0.5:0.5.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0768P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2311
_refine_ls_number_parameters     197
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0500
_refine_ls_wR_factor_ref         0.1504
_refine_ls_wR_factor_gt          0.1286
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1BW O 0.0623(17) 0.8452(11) 0.0029(8) 0.078(6) Uani 0.548(17) 1 d P . .
O1AW O -0.101(2) 0.8420(13) 0.0281(10) 0.078(7) Uani 0.452(17) 1 d P . .
Mo Mo 0.41370(9) 0.59621(5) 0.07759(4) 0.0371(3) Uani 1 1 d . . .
B B 0.4999(11) 0.5205(8) 0.3036(7) 0.042(2) Uani 1 1 d . . .
H10 H 0.5214 0.5015 0.3681 0.051 Uiso 1 1 calc R . .
C1 C 0.3242(10) 0.3518(7) 0.2743(7) 0.050(2) Uani 1 1 d . . .
H1 H 0.3418 0.3242 0.3327 0.060 Uiso 1 1 calc R . .
C2 C 0.2278(12) 0.3083(7) 0.1998(7) 0.056(2) Uani 1 1 d . . .
H2 H 0.1670 0.2462 0.1972 0.068 Uiso 1 1 calc R . .
C3 C 0.2403(11) 0.3762(7) 0.1296(7) 0.056(3) Uani 1 1 d . . .
H3 H 0.1868 0.3670 0.0702 0.068 Uiso 1 1 calc R . .
C4 C 0.8400(11) 0.5204(7) 0.2992(6) 0.051(2) Uani 1 1 d . . .
H4 H 0.8779 0.5010 0.3589 0.061 Uiso 1 1 calc R . .
C5 C 0.9452(11) 0.5404(7) 0.2343(7) 0.056(3) Uani 1 1 d . . .
H5 H 1.0671 0.5383 0.2408 0.067 Uiso 1 1 calc R . .
C6 C 0.8326(11) 0.5645(6) 0.1565(7) 0.051(2) Uani 1 1 d . . .
H6 H 0.8676 0.5806 0.1003 0.061 Uiso 1 1 calc R . .
C7 C 0.3538(11) 0.6899(7) 0.3529(6) 0.050(2) Uani 1 1 d . . .
H7 H 0.3720 0.6802 0.4156 0.060 Uiso 1 1 calc R . .
C8 C 0.2700(11) 0.7726(7) 0.3084(7) 0.058(3) Uani 1 1 d . . .
H8 H 0.2204 0.8290 0.3343 0.070 Uiso 1 1 calc R . .
C9 C 0.2753(10) 0.7539(7) 0.2180(6) 0.046(2) Uani 1 1 d . . .
H9 H 0.2291 0.7972 0.1710 0.055 Uiso 1 1 calc R . .
N1 N 0.3878(8) 0.4400(5) 0.2483(4) 0.0352(15) Uani 1 1 d . . .
N2 N 0.3396(8) 0.4571(5) 0.1584(4) 0.0399(16) Uani 1 1 d . . .
N3 N 0.6727(8) 0.5334(5) 0.2628(5) 0.0413(17) Uani 1 1 d . . .
N4 N 0.6661(8) 0.5614(5) 0.1739(5) 0.0423(17) Uani 1 1 d . . .
N5 N 0.4049(8) 0.6256(5) 0.2902(4) 0.0377(16) Uani 1 1 d . . .
N6 N 0.3559(8) 0.6650(5) 0.2066(4) 0.0379(16) Uani 1 1 d . . .
O1 O 0.5101(8) 0.7078(4) 0.0502(4) 0.0546(16) Uani 1 1 d . . .
O2 O 0.1998(7) 0.6082(5) 0.0320(4) 0.0606(18) Uani 1 1 d . . .
O3 O 0.5000 0.5000 0.0000 0.048(2) Uani 1 2 d S . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1BW 0.079(11) 0.105(11) 0.056(8) -0.004(7) 0.033(7) 0.004(8)
O1AW 0.082(13) 0.093(13) 0.065(10) -0.007(9) 0.025(9) -0.012(10)
Mo 0.0447(5) 0.0333(4) 0.0342(4) -0.0018(4) 0.0083(3) -0.0028(4)
B 0.035(5) 0.049(7) 0.043(6) 0.003(5) 0.007(4) 0.006(5)
C1 0.043(5) 0.040(5) 0.070(6) 0.015(5) 0.018(5) 0.011(4)
C2 0.066(6) 0.030(5) 0.075(7) 0.013(5) 0.016(5) -0.008(5)
C3 0.059(6) 0.049(6) 0.064(6) -0.009(5) 0.016(5) -0.008(5)
C4 0.042(5) 0.044(6) 0.066(6) 0.002(5) -0.002(5) 0.006(4)
C5 0.029(5) 0.044(6) 0.095(8) -0.008(6) 0.008(5) 0.006(4)
C6 0.050(6) 0.039(5) 0.069(6) 0.001(5) 0.024(5) -0.004(4)
C7 0.054(5) 0.054(6) 0.044(5) -0.018(5) 0.013(4) -0.005(5)
C8 0.061(6) 0.042(6) 0.075(7) -0.021(5) 0.023(5) 0.001(5)
C9 0.038(5) 0.043(6) 0.058(6) -0.002(4) 0.010(4) 0.002(4)
N1 0.036(4) 0.032(4) 0.040(4) 0.007(3) 0.012(3) 0.000(3)
N2 0.046(4) 0.031(4) 0.044(4) -0.003(3) 0.011(3) -0.003(3)
N3 0.035(4) 0.038(4) 0.050(4) 0.005(3) 0.002(3) 0.000(3)
N4 0.034(4) 0.040(4) 0.055(4) 0.006(3) 0.015(3) 0.004(3)
N5 0.035(4) 0.041(4) 0.038(4) -0.002(3) 0.009(3) 0.000(3)
N6 0.039(4) 0.033(4) 0.041(4) -0.002(3) 0.004(3) 0.003(3)
O1 0.074(4) 0.045(4) 0.046(3) 0.004(3) 0.010(3) -0.017(3)
O2 0.052(4) 0.084(5) 0.043(3) 0.000(3) -0.004(3) 0.004(3)
O3 0.061(5) 0.045(5) 0.042(5) -0.006(4) 0.022(4) -0.013(4)

_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
O1BW O1AW 1.356(17) . ?
Mo O1 1.699(5) . ?
Mo O2 1.703(5) . ?
Mo O3 1.8753(7) . ?
Mo N6 2.206(6) . ?
Mo N2 2.278(6) . ?
Mo N4 2.301(6) . ?
B N1 1.524(11) . ?
B N3 1.537(10) . ?
B N5 1.548(11) . ?
B H10 0.9800 . ?
C1 N1 1.321(10) . ?
C1 C2 1.370(12) . ?
C1 H1 0.9300 . ?
C2 C3 1.376(12) . ?
C2 H2 0.9300 . ?
C3 N2 1.336(10) . ?
C3 H3 0.9300 . ?
C4 N3 1.340(9) . ?
C4 C5 1.358(12) . ?
C4 H4 0.9300 . ?
C5 C6 1.386(12) . ?
C5 H5 0.9300 . ?
C6 N4 1.339(10) . ?
C6 H6 0.9300 . ?
C7 N5 1.345(9) . ?
C7 C8 1.375(12) . ?
C7 H7 0.9300 . ?
C8 C9 1.368(12) . ?
C8 H8 0.9300 . ?
C9 N6 1.330(10) . ?
C9 H9 0.9300 . ?
N1 N2 1.355(8) . ?
N3 N4 1.362(9) . ?
N5 N6 1.348(8) . ?
O3 Mo 1.8753(7) 3_665 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mo O2 104.8(3) . . ?
O1 Mo O3 102.8(2) . . ?
O2 Mo O3 102.6(2) . . ?
O1 Mo N6 90.3(2) . . ?
O2 Mo N6 90.8(3) . . ?
O3 Mo N6 157.99(17) . . ?
O1 Mo N2 161.2(2) . . ?
O2 Mo N2 89.2(3) . . ?
O3 Mo N2 85.79(16) . . ?
N6 Mo N2 76.9(2) . . ?
O1 Mo N4 87.5(3) . . ?
O2 Mo N4 163.4(3) . . ?
O3 Mo N4 84.98(17) . . ?
N6 Mo N4 77.9(2) . . ?
N2 Mo N4 76.5(2) . . ?
N1 B N3 108.7(7) . . ?
N1 B N5 108.0(6) . . ?
N3 B N5 105.7(7) . . ?
N1 B H10 111.4 . . ?
N3 B H10 111.4 . . ?
N5 B H10 111.4 . . ?
N1 C1 C2 107.7(8) . . ?
N1 C1 H1 126.2 . . ?
C2 C1 H1 126.2 . . ?
C1 C2 C3 105.2(8) . . ?
C1 C2 H2 127.4 . . ?
C3 C2 H2 127.4 . . ?
N2 C3 C2 110.8(9) . . ?
N2 C3 H3 124.6 . . ?
C2 C3 H3 124.6 . . ?
N3 C4 C5 108.6(8) . . ?
N3 C4 H4 125.7 . . ?
C5 C4 H4 125.7 . . ?
C4 C5 C6 105.5(7) . . ?
C4 C5 H5 127.3 . . ?
C6 C5 H5 127.3 . . ?
N4 C6 C5 110.1(8) . . ?
N4 C6 H6 125.0 . . ?
C5 C6 H6 125.0 . . ?
N5 C7 C8 108.3(8) . . ?
N5 C7 H7 125.9 . . ?
C8 C7 H7 125.9 . . ?
C9 C8 C7 105.0(8) . . ?
C9 C8 H8 127.5 . . ?
C7 C8 H8 127.5 . . ?
N6 C9 C8 110.6(8) . . ?
N6 C9 H9 124.7 . . ?
C8 C9 H9 124.7 . . ?
C1 N1 N2 111.4(7) . . ?
C1 N1 B 129.9(7) . . ?
N2 N1 B 118.7(6) . . ?
C3 N2 N1 104.9(7) . . ?
C3 N2 Mo 128.8(6) . . ?
N1 N2 Mo 126.3(5) . . ?
C4 N3 N4 109.7(7) . . ?
C4 N3 B 131.4(7) . . ?
N4 N3 B 118.9(6) . . ?
C6 N4 N3 106.1(7) . . ?
C6 N4 Mo 128.8(6) . . ?
N3 N4 Mo 125.2(5) . . ?
C7 N5 N6 109.1(7) . . ?
C7 N5 B 129.3(7) . . ?
N6 N5 B 121.6(6) . . ?
C9 N6 N5 107.0(7) . . ?
C9 N6 Mo 127.6(6) . . ?
N5 N6 Mo 125.4(5) . . ?
Mo O3 Mo 180.0 . 3_665 ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        24.08
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.137

# Attachment '- 2.cif'

data_2
_database_code_depnum_ccdc_archive 'CCDC 891376'
#TrackingRef '- 2.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H14 B2 I6 Mo2 N12 O5'
_chemical_formula_weight         1453.31

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'
B B 0.0013 0.0007 '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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   16.0143(7)
_cell_length_b                   13.1374(5)
_cell_length_c                   18.3143(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.9610(10)
_cell_angle_gamma                90.00
_cell_volume                     3598.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4512
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      28.09

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.683
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2632
_exptl_absorpt_coefficient_mu    5.893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7501
_exptl_absorpt_correction_T_max  0.9838
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(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 AXS SMART APEX II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11115
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.06
_diffrn_reflns_theta_max         28.29
_reflns_number_total             4337
_reflns_number_gt                3540
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger. The iodine atoms(I2 and I3) are disordered and modeled over two split positions with occupancies in ratio of 0.4:0.6, respectively.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+24.5820P] where P=(Fo^2^+2Fc^2^)/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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4337
_refine_ls_number_parameters     227
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0367
_refine_ls_wR_factor_ref         0.0872
_refine_ls_wR_factor_gt          0.0816
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
I2A I 0.1055(2) 0.6671(4) 0.55497(16) 0.0747(7) Uani 0.599(17) 1 d P A 1
I3A I 0.6907(3) 1.0101(3) 0.8722(3) 0.0887(10) Uani 0.599(17) 1 d P A 1
I2B I 0.1129(5) 0.6931(9) 0.5588(3) 0.1056(17) Uani 0.401(17) 1 d P A 2
I3B I 0.6671(9) 1.0218(5) 0.8533(6) 0.107(2) Uani 0.401(17) 1 d P A 2
H7 H 0.323(3) 0.898(4) 0.846(3) 0.041(14) Uiso 1 1 d . . .
I1 I 0.39138(3) 0.67666(4) 1.14691(2) 0.06788(16) Uani 1 1 d . . .
C1 C 0.3556(3) 0.7737(4) 0.9836(3) 0.0415(11) Uani 1 1 d . . .
H1 H 0.3288 0.8319 0.9939 0.050 Uiso 1 1 calc R . .
C2 C 0.3862(3) 0.6928(4) 1.0332(3) 0.0418(11) Uani 1 1 d . . .
C3 C 0.4207(3) 0.6250(4) 0.9936(3) 0.0404(11) Uani 1 1 d . . .
H2 H 0.4463 0.5625 1.0129 0.048 Uiso 1 1 calc R . .
C4 C 0.2277(4) 0.7776(5) 0.7119(3) 0.0464(13) Uani 1 1 d . A .
H3 H 0.1919 0.8351 0.7054 0.056 Uiso 1 1 calc R . .
C5 C 0.2114(4) 0.6962(5) 0.6620(3) 0.0502(14) Uani 1 1 d . . .
C6 C 0.2809(3) 0.6280(4) 0.6951(3) 0.0404(11) Uani 1 1 d . A .
H4 H 0.2872 0.5650 0.6744 0.049 Uiso 1 1 calc R . .
C7 C 0.4936(5) 0.9362(4) 0.8491(3) 0.0557(15) Uani 1 1 d . A .
H5 H 0.4702 1.0008 0.8499 0.067 Uiso 1 1 calc R . .
C8 C 0.5782(4) 0.9156(4) 0.8535(3) 0.0512(14) Uani 1 1 d . . .
C9 C 0.5835(4) 0.8099(4) 0.8511(3) 0.0416(11) Uani 1 1 d . A .
H6 H 0.6342 0.7732 0.8538 0.050 Uiso 1 1 calc R . .
O1 O 0.5697(2) 0.5839(3) 0.91437(19) 0.0430(8) Uani 1 1 d . A .
O2 O 0.4154(2) 0.4871(3) 0.8384(2) 0.0468(9) Uani 1 1 d . A .
O3 O 0.5000 0.5923(3) 0.7500 0.0338(9) Uani 1 2 d S . .
N1 N 0.3710(3) 0.7546(3) 0.9175(2) 0.0370(9) Uani 1 1 d . . .
N2 N 0.4117(3) 0.6627(3) 0.9237(2) 0.0357(9) Uani 1 1 d . A .
N3 N 0.3046(3) 0.7598(3) 0.7720(2) 0.0383(9) Uani 1 1 d . . .
N4 N 0.3378(3) 0.6682(3) 0.7620(2) 0.0343(8) Uani 1 1 d . A .
N5 N 0.4489(3) 0.8477(3) 0.8433(2) 0.0410(9) Uani 1 1 d . . .
N6 N 0.5048(3) 0.7695(3) 0.8444(2) 0.0344(8) Uani 1 1 d . A .
B B 0.3555(4) 0.8230(4) 0.8449(3) 0.0404(13) Uani 1 1 d . A .
Mo Mo 0.47010(2) 0.59871(3) 0.84042(2) 0.02737(10) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
I2A 0.0595(7) 0.0992(15) 0.0438(8) 0.0169(9) -0.0077(7) -0.0100(8)
I3A 0.0868(14) 0.0611(9) 0.143(3) -0.0496(12) 0.0720(13) -0.0393(8)
I2B 0.0746(19) 0.125(4) 0.0692(15) -0.0091(17) -0.0321(13) 0.017(2)
I3B 0.168(5) 0.0710(19) 0.112(3) -0.0396(17) 0.089(4) -0.078(3)
I1 0.0842(3) 0.0957(4) 0.03367(19) 0.01245(19) 0.03322(19) 0.0328(2)
C1 0.044(3) 0.052(3) 0.032(2) -0.002(2) 0.019(2) 0.011(2)
C2 0.039(3) 0.061(3) 0.029(2) 0.003(2) 0.0169(19) 0.005(2)
C3 0.049(3) 0.047(3) 0.031(2) 0.010(2) 0.021(2) 0.006(2)
C4 0.044(3) 0.064(4) 0.035(2) 0.021(2) 0.020(2) 0.023(3)
C5 0.038(3) 0.080(4) 0.032(2) 0.015(3) 0.012(2) 0.007(3)
C6 0.040(3) 0.050(3) 0.031(2) 0.001(2) 0.012(2) -0.001(2)
C7 0.095(5) 0.028(3) 0.058(3) -0.003(2) 0.045(3) -0.003(3)
C8 0.072(4) 0.040(3) 0.054(3) -0.017(2) 0.038(3) -0.019(3)
C9 0.050(3) 0.043(3) 0.039(3) -0.010(2) 0.026(2) -0.012(2)
O1 0.0435(19) 0.048(2) 0.0342(17) 0.0065(15) 0.0095(14) 0.0073(16)
O2 0.048(2) 0.0321(18) 0.066(2) 0.0086(16) 0.0284(18) -0.0023(15)
O3 0.043(3) 0.036(2) 0.028(2) 0.000 0.0195(19) 0.000
N1 0.044(2) 0.041(2) 0.0313(19) 0.0032(16) 0.0205(17) 0.0090(17)
N2 0.046(2) 0.036(2) 0.0312(19) 0.0078(16) 0.0205(17) 0.0106(17)
N3 0.045(2) 0.041(2) 0.0322(19) 0.0084(16) 0.0172(17) 0.0133(18)
N4 0.038(2) 0.036(2) 0.0283(18) 0.0046(15) 0.0114(16) 0.0055(16)
N5 0.061(3) 0.030(2) 0.040(2) 0.0011(16) 0.028(2) 0.0062(18)
N6 0.049(2) 0.0269(19) 0.0332(19) -0.0043(15) 0.0217(17) 0.0000(16)
B 0.056(4) 0.038(3) 0.035(3) 0.006(2) 0.025(3) 0.013(3)
Mo 0.03296(19) 0.02671(18) 0.02573(17) 0.00340(14) 0.01449(14) 0.00213(14)

_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
I2A C5 2.119(6) . ?
I3A C8 2.113(6) . ?
I2B C5 1.983(8) . ?
I3B C8 1.994(8) . ?
I1 C2 2.065(5) . ?
C1 N1 1.342(6) . ?
C1 C2 1.369(7) . ?
C1 H1 0.9300 . ?
C2 C3 1.382(7) . ?
C3 N2 1.332(6) . ?
C3 H2 0.9300 . ?
C4 N3 1.346(6) . ?
C4 C5 1.369(8) . ?
C4 H3 0.9300 . ?
C5 C6 1.388(7) . ?
C6 N4 1.345(6) . ?
C6 H4 0.9300 . ?
C7 N5 1.350(7) . ?
C7 C8 1.354(9) . ?
C7 H5 0.9300 . ?
C8 C9 1.393(7) . ?
C9 N6 1.331(6) . ?
C9 H6 0.9300 . ?
O1 Mo 1.695(3) . ?
O2 Mo 1.701(3) . ?
O3 Mo 1.8830(4) 2_656 ?
O3 Mo 1.8830(4) . ?
N1 N2 1.357(5) . ?
N1 B 1.548(6) . ?
N2 Mo 2.221(4) . ?
N3 N4 1.355(5) . ?
N3 B 1.536(7) . ?
N4 Mo 2.283(4) . ?
N5 N6 1.358(5) . ?
N5 B 1.542(8) . ?
N6 Mo 2.306(4) . ?
B H7 1.12(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 108.5(4) . . ?
N1 C1 H1 125.8 . . ?
C2 C1 H1 125.8 . . ?
C1 C2 C3 105.5(4) . . ?
C1 C2 I1 128.7(4) . . ?
C3 C2 I1 125.6(4) . . ?
N2 C3 C2 109.8(4) . . ?
N2 C3 H2 125.1 . . ?
C2 C3 H2 125.1 . . ?
N3 C4 C5 108.1(5) . . ?
N3 C4 H3 126.0 . . ?
C5 C4 H3 126.0 . . ?
C4 C5 C6 106.3(5) . . ?
C4 C5 I2B 123.3(5) . . ?
C6 C5 I2B 130.0(5) . . ?
C4 C5 I2A 131.0(4) . . ?
C6 C5 I2A 122.6(5) . . ?
I2B C5 I2A 9.3(4) . . ?
N4 C6 C5 108.6(5) . . ?
N4 C6 H4 125.7 . . ?
C5 C6 H4 125.7 . . ?
N5 C7 C8 108.9(5) . . ?
N5 C7 H5 125.6 . . ?
C8 C7 H5 125.6 . . ?
C7 C8 C9 105.6(5) . . ?
C7 C8 I3B 124.0(6) . . ?
C9 C8 I3B 130.2(6) . . ?
C7 C8 I3A 132.0(4) . . ?
C9 C8 I3A 122.2(5) . . ?
I3B C8 I3A 11.8(4) . . ?
N6 C9 C8 109.5(5) . . ?
N6 C9 H6 125.2 . . ?
C8 C9 H6 125.2 . . ?
Mo O3 Mo 174.9(3) 2_656 . ?
C1 N1 N2 109.1(4) . . ?
C1 N1 B 129.8(4) . . ?
N2 N1 B 120.9(4) . . ?
C3 N2 N1 107.2(4) . . ?
C3 N2 Mo 126.3(3) . . ?
N1 N2 Mo 125.9(3) . . ?
C4 N3 N4 109.3(4) . . ?
C4 N3 B 131.5(4) . . ?
N4 N3 B 119.1(4) . . ?
C6 N4 N3 107.6(4) . . ?
C6 N4 Mo 126.1(3) . . ?
N3 N4 Mo 126.2(3) . . ?
C7 N5 N6 108.8(4) . . ?
C7 N5 B 132.2(5) . . ?
N6 N5 B 118.6(4) . . ?
C9 N6 N5 107.2(4) . . ?
C9 N6 Mo 126.9(3) . . ?
N5 N6 Mo 125.8(3) . . ?
N3 B N5 108.3(4) . . ?
N3 B N1 107.7(4) . . ?
N5 B N1 106.3(4) . . ?
N3 B H7 112(3) . . ?
N5 B H7 106(3) . . ?
N1 B H7 116(3) . . ?
O1 Mo O2 104.39(18) . . ?
O1 Mo O3 103.58(12) . . ?
O2 Mo O3 103.46(18) . . ?
O1 Mo N2 90.11(16) . . ?
O2 Mo N2 90.09(16) . . ?
O3 Mo N2 157.41(15) . . ?
O1 Mo N4 161.04(16) . . ?
O2 Mo N4 88.62(16) . . ?
O3 Mo N4 86.29(11) . . ?
N2 Mo N4 75.91(14) . . ?
O1 Mo N6 86.51(16) . . ?
O2 Mo N6 162.84(16) . . ?
O3 Mo N6 86.39(16) . . ?
N2 Mo N6 76.46(14) . . ?
N4 Mo N6 77.89(14) . . ?

_diffrn_measured_fraction_theta_max 0.970
_diffrn_reflns_theta_full        28.29
_diffrn_measured_fraction_theta_full 0.970
_refine_diff_density_max         2.168
_refine_diff_density_min         -2.156
_refine_diff_density_rms         0.120