# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2002


data_global

_journal_coden_Cambridge      182

_publ_requested_journal       'Chemical Communications'

_publ_contact_author                 'Dr. Nadia C. M\"osch-Zanetti'
_publ_contact_author_address
;
'Department of Inorganic Chemistry'
'Georg-August-University'
'Tammannstrasse 4'
'37077 G\"ottingen'
'Germany'
;
_publ_contact_author_email           'nmoesch@gwdg.de'
_publ_contact_author_fax             '(+49)551-39-3337'
_publ_contact_author_phone           '(+49)551-39-19405'


loop_
_publ_author_name
_publ_author_address
'Most, Kerstin'
; 
'Department of Inorganic Chemistry'
'Georg-August-University'
'Tammannstrasse 4'
'37077 G\"ottingen'
'Germany'
;
'M\"osch-Zanetti, Nadia C.'
;
'Department of Inorganic Chemistry'
'Georg-August-University'
'Tammannstrasse 4'
'37077 G\"ottingen'
'Germany'
;
'K\"opke, Sinje'
;
'Department of Structural Chemistry'
'Georg-August-University'
'Tammannstrasse 4'
'37077 G\"ottingen'
'Germany'
;
'Dall\' Antonia, Fabio'
;
'Department of Structural Chemistry'
'Georg-August-University'
'Tammannstrasse 4'
'37077 G\"ottingen'
'Germany'
;

_journal_name_full                   
;
'Chemical Communications (Chem. Comm.)'
;
_publ_section_title
;
The first molybdenum dioxo compounds with eta2-pyrazolate ligands:
crystal structure and oxo transfer properties
;

#==============================================================================
# STRUCTURE PART

data_publ 
_database_code_CSD                180085
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
'C11 H19 Cl Mo N2 O2' 
_chemical_formula_weight          342.67 

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' 
'Cl'  'Cl'   0.1484   0.1585 
'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    Cc 

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' 

_cell_length_a                    15.35(1) 
_cell_length_b                    10.28(1) 
_cell_length_c                    19.75(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  106.87(7) 
_cell_angle_gamma                 90.00 
_cell_volume                      2980(6) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     133(2) 
_cell_measurement_reflns_used     1024 
_cell_measurement_theta_min       2.98 
_cell_measurement_theta_max       27.85 

_exptl_crystal_description        blocks 
_exptl_crystal_colour             colourless 
_exptl_crystal_size_max           0.60 
_exptl_crystal_size_mid           0.50 
_exptl_crystal_size_min           0.30 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.528 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1392 
_exptl_absorpt_coefficient_mu     1.052 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.5708 
_exptl_absorpt_correction_T_max   0.7431 
_exptl_absorpt_process_details 
;
'Blessing, R. H. (1995). Acta Cryst. A51, 33-38'
;

_exptl_special_details 
; 
'Intensities were measured with a Siemens CCD area detector' 
; 

_diffrn_ambient_temperature       133(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 
'STOE-Siemens-Huber four circle diffractometer'
_diffrn_measurement_method        'phi and omega scans' 
_diffrn_detector_area_resol_mean  '8.192 pixels/mm' 
_diffrn_standards_number          0 
_diffrn_standards_interval_count  0 
_diffrn_standards_interval_time   0 
_diffrn_standards_decay_%         0 
_diffrn_reflns_number             21708 
_diffrn_reflns_av_R_equivalents   0.0363 
_diffrn_reflns_av_sigmaI/netI     0.0295 
_diffrn_reflns_limit_h_min        -20 
_diffrn_reflns_limit_h_max        18 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        13 
_diffrn_reflns_limit_l_min        -25 
_diffrn_reflns_limit_l_max        25 
_diffrn_reflns_theta_min          2.16 
_diffrn_reflns_theta_max          27.91 
_reflns_number_total              5532 
_reflns_number_gt                 5491 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        'Siemens SMART (V.4.202, Siemens 1996)'
_computing_cell_refinement        'Bruker AXS SAINT (V.5.00, Madison 1997)'
_computing_data_reduction         'Bruker AXS SAINT (V.5.00, Madison 1997)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'Bruker AXS SHELXTL (V. 5.10)'
_computing_publication_material   'SHELXL-97 (Sheldrick, 1997)'

_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. 
; 

_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^)+(0.0258P)^2^+2.8463P] 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     'riding model' 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.00219(12) 
_refine_ls_extinction_expression 
'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_abs_structure_details 
'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.11(3) 
_refine_ls_number_reflns          5532 
_refine_ls_number_parameters      321 
_refine_ls_number_restraints      2 
_refine_ls_R_factor_all           0.0220 
_refine_ls_R_factor_gt            0.0217 
_refine_ls_wR_factor_ref          0.0546 
_refine_ls_wR_factor_gt           0.0545 
_refine_ls_goodness_of_fit_ref    1.053 
_refine_ls_restrained_S_all       1.053 
_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 0.550099(13) 0.15306(2) 0.542989(11) 0.02152(6) Uani 1 1 d . . . 
Cl1 Cl 0.56559(5) -0.06778(6) 0.52788(4) 0.03008(15) Uani 1 1 d . . . 
O1 O 0.57985(15) 0.2264(2) 0.47590(13) 0.0364(5) Uani 1 1 d . . . 
O2 O 0.63544(15) 0.1847(2) 0.61676(13) 0.0360(5) Uani 1 1 d . . . 
N1 N 0.42685(17) 0.13494(18) 0.56895(13) 0.0178(5) Uani 1 1 d . . . 
N2 N 0.44510(15) 0.2624(2) 0.55564(12) 0.0188(4) Uani 1 1 d . . . 
C1 C 0.33806(18) 0.1254(2) 0.56493(14) 0.0181(5) Uani 1 1 d . . . 
C2 C 0.30020(19) 0.2501(2) 0.55157(14) 0.0209(5) Uani 1 1 d . . . 
H2 H 0.2391 0.2733 0.5480 0.025 Uiso 1 1 calc R . . 
C3 C 0.36847(18) 0.3341(2) 0.54444(13) 0.0182(5) Uani 1 1 d . . . 
C10 C 0.29570(19) -0.0039(2) 0.57356(15) 0.0229(5) Uani 1 1 d . . . 
C11 C 0.3600(3) -0.0765(3) 0.63503(18) 0.0506(10) Uani 1 1 d . . . 
H11A H 0.3750 -0.0212 0.6773 0.076 Uiso 1 1 calc R . . 
H11B H 0.4159 -0.0987 0.6231 0.076 Uiso 1 1 calc R . . 
H11C H 0.3306 -0.1564 0.6443 0.076 Uiso 1 1 calc R . . 
C12 C 0.2835(3) -0.0840(3) 0.50566(17) 0.0394(8) Uani 1 1 d . . . 
H12A H 0.2590 -0.1699 0.5115 0.059 Uiso 1 1 calc R . . 
H12B H 0.3426 -0.0942 0.4965 0.059 Uiso 1 1 calc R . . 
H12C H 0.2413 -0.0389 0.4657 0.059 Uiso 1 1 calc R . . 
C13 C 0.2049(3) 0.0184(3) 0.5873(4) 0.0806(19) Uani 1 1 d . . . 
H13A H 0.2135 0.0730 0.6294 0.121 Uiso 1 1 calc R . . 
H13B H 0.1788 -0.0655 0.5950 0.121 Uiso 1 1 calc R . . 
H13C H 0.1634 0.0619 0.5463 0.121 Uiso 1 1 calc R . . 
C30 C 0.36440(19) 0.4791(2) 0.53074(14) 0.0226(5) Uani 1 1 d . . . 
C31 C 0.4559(2) 0.5275(3) 0.52374(19) 0.0335(6) Uani 1 1 d . . . 
H31A H 0.5042 0.5081 0.5674 0.050 Uiso 1 1 calc R . . 
H31B H 0.4528 0.6217 0.5156 0.050 Uiso 1 1 calc R . . 
H31C H 0.4692 0.4837 0.4838 0.050 Uiso 1 1 calc R . . 
C32 C 0.2877(2) 0.5065(3) 0.46264(16) 0.0317(6) Uani 1 1 d . . . 
H32A H 0.2997 0.4593 0.4232 0.048 Uiso 1 1 calc R . . 
H32B H 0.2849 0.6001 0.4527 0.048 Uiso 1 1 calc R . . 
H32C H 0.2295 0.4777 0.4686 0.048 Uiso 1 1 calc R . . 
C33 C 0.3427(2) 0.5464(3) 0.59381(16) 0.0308(6) Uani 1 1 d . . . 
H33A H 0.2851 0.5128 0.5987 0.046 Uiso 1 1 calc R . . 
H33B H 0.3375 0.6405 0.5855 0.046 Uiso 1 1 calc R . . 
H33C H 0.3917 0.5287 0.6373 0.046 Uiso 1 1 calc R . . 
Mo2 Mo 0.403232(13) 0.13208(2) 0.338001(11) 0.02232(6) Uani 1 1 d . . . 
Cl2 Cl 0.39379(7) 0.35251(7) 0.32013(6) 0.0479(3) Uani 1 1 d . . . 
O3 O 0.40596(16) 0.1086(2) 0.42351(11) 0.0337(5) Uani 1 1 d . . . 
O4 O 0.30155(16) 0.0778(3) 0.28799(12) 0.0409(6) Uani 1 1 d . . . 
N3 N 0.49117(17) -0.0035(2) 0.32092(12) 0.0236(5) Uani 1 1 d . . . 
N4 N 0.52016(17) 0.1162(2) 0.30463(13) 0.0223(5) Uani 1 1 d . . . 
C4 C 0.5433(2) -0.0969(2) 0.30520(14) 0.0213(5) Uani 1 1 d . . . 
C5 C 0.6081(2) -0.0349(3) 0.27862(14) 0.0228(5) Uani 1 1 d . . . 
H5 H 0.6545 -0.0760 0.2633 0.027 Uiso 1 1 calc R . . 
C6 C 0.59140(18) 0.0989(2) 0.27893(13) 0.0205(5) Uani 1 1 d . . . 
C40 C 0.5284(2) -0.2403(2) 0.31578(15) 0.0264(6) Uani 1 1 d . . . 
C41 C 0.5003(3) -0.3074(3) 0.24318(19) 0.0503(10) Uani 1 1 d . . . 
H41A H 0.4461 -0.2646 0.2125 0.075 Uiso 1 1 calc R . . 
H41B H 0.4867 -0.3992 0.2491 0.075 Uiso 1 1 calc R . . 
H41C H 0.5502 -0.3014 0.2217 0.075 Uiso 1 1 calc R . . 
C42 C 0.6165(3) -0.2997(3) 0.3632(2) 0.0508(10) Uani 1 1 d . . . 
H42A H 0.6643 -0.2936 0.3396 0.076 Uiso 1 1 calc R . . 
H42B H 0.6060 -0.3913 0.3723 0.076 Uiso 1 1 calc R . . 
H42C H 0.6354 -0.2523 0.4082 0.076 Uiso 1 1 calc R . . 
C43 C 0.4524(3) -0.2579(3) 0.3511(2) 0.0397(8) Uani 1 1 d . . . 
H43A H 0.4690 -0.2125 0.3967 0.060 Uiso 1 1 calc R . . 
H43B H 0.4442 -0.3508 0.3587 0.060 Uiso 1 1 calc R . . 
H43C H 0.3955 -0.2217 0.3205 0.060 Uiso 1 1 calc R . . 
C60 C 0.6401(2) 0.2138(3) 0.25802(15) 0.0243(5) Uani 1 1 d . . . 
C61 C 0.6833(2) 0.2953(3) 0.32480(17) 0.0356(7) Uani 1 1 d . . . 
H61A H 0.6356 0.3250 0.3452 0.053 Uiso 1 1 calc R . . 
H61B H 0.7143 0.3709 0.3122 0.053 Uiso 1 1 calc R . . 
H61C H 0.7274 0.2420 0.3595 0.053 Uiso 1 1 calc R . . 
C62 C 0.7131(2) 0.1643(3) 0.22556(19) 0.0345(7) Uani 1 1 d . . . 
H62A H 0.7574 0.1113 0.2604 0.052 Uiso 1 1 calc R . . 
H62B H 0.7442 0.2386 0.2118 0.052 Uiso 1 1 calc R . . 
H62C H 0.6844 0.1114 0.1837 0.052 Uiso 1 1 calc R . . 
C63 C 0.5707(2) 0.2982(3) 0.20409(17) 0.0355(7) Uani 1 1 d . . . 
H63A H 0.5446 0.2479 0.1607 0.053 Uiso 1 1 calc R . . 
H63B H 0.6012 0.3756 0.1930 0.053 Uiso 1 1 calc R . . 
H63C H 0.5220 0.3247 0.2241 0.053 Uiso 1 1 calc R . . 

loop_ 
_atom_site_aniso_label 
_atom_site_aniso_U_11 
_atom_site_aniso_U_22 
_atom_site_aniso_U_33 
_atom_site_aniso_U_23 
_atom_site_aniso_U_13 
_atom_site_aniso_U_12 
Mo1 0.01515(11) 0.02048(9) 0.03112(13) -0.00002(9) 0.01018(9) 0.00134(8) 
Cl1 0.0258(4) 0.0243(3) 0.0411(4) -0.0040(3) 0.0111(3) 0.0073(2) 
O1 0.0314(12) 0.0365(11) 0.0496(14) 0.0059(9) 0.0251(11) 0.0001(9) 
O2 0.0192(11) 0.0355(11) 0.0486(13) -0.0067(10) 0.0025(10) 0.0026(9) 
N1 0.0186(12) 0.0117(9) 0.0245(12) 0.0017(7) 0.0084(10) 0.0015(7) 
N2 0.0170(10) 0.0151(9) 0.0255(11) -0.0015(8) 0.0081(9) -0.0008(8) 
C1 0.0194(13) 0.0166(10) 0.0195(12) -0.0020(8) 0.0077(10) -0.0016(9) 
C2 0.0159(12) 0.0202(11) 0.0266(13) -0.0036(9) 0.0063(10) 0.0018(9) 
C3 0.0200(13) 0.0147(10) 0.0205(12) -0.0005(8) 0.0067(10) 0.0028(9) 
C10 0.0235(13) 0.0146(10) 0.0337(14) -0.0041(10) 0.0132(11) -0.0036(9) 
C11 0.083(3) 0.0314(16) 0.0286(17) 0.0087(13) 0.0016(18) -0.0224(17) 
C12 0.056(2) 0.0256(13) 0.0319(16) -0.0054(11) 0.0058(15) -0.0143(14) 
C13 0.058(3) 0.0243(15) 0.194(6) -0.014(2) 0.090(4) -0.0111(16) 
C30 0.0257(14) 0.0131(10) 0.0280(13) 0.0016(9) 0.0065(11) 0.0007(9) 
C31 0.0332(16) 0.0202(12) 0.0506(18) 0.0027(12) 0.0174(14) -0.0050(11) 
C32 0.0324(16) 0.0279(13) 0.0309(15) 0.0062(11) 0.0030(13) 0.0078(12) 
C33 0.0397(17) 0.0204(12) 0.0321(15) -0.0053(10) 0.0098(14) 0.0040(11) 
Mo2 0.02524(13) 0.02073(9) 0.02532(12) 0.00080(8) 0.01415(10) -0.00053(9) 
Cl2 0.0637(6) 0.0235(3) 0.0725(7) 0.0097(3) 0.0452(6) 0.0116(4) 
O3 0.0409(13) 0.0374(11) 0.0284(11) 0.0005(8) 0.0191(10) 0.0016(9) 
O4 0.0294(13) 0.0521(14) 0.0401(13) -0.0021(10) 0.0082(11) -0.0010(10) 
N3 0.0295(13) 0.0176(10) 0.0266(11) 0.0017(8) 0.0128(10) -0.0024(9) 
N4 0.0272(14) 0.0156(9) 0.0294(13) 0.0002(9) 0.0164(11) -0.0021(9) 
C4 0.0257(13) 0.0175(11) 0.0200(12) -0.0006(9) 0.0056(10) 0.0021(10) 
C5 0.0226(14) 0.0234(12) 0.0238(13) -0.0003(10) 0.0090(11) 0.0037(10) 
C6 0.0213(13) 0.0218(11) 0.0198(12) 0.0008(9) 0.0082(10) -0.0018(10) 
C40 0.0325(16) 0.0164(11) 0.0276(14) -0.0007(10) 0.0045(12) 0.0006(10) 
C41 0.091(3) 0.0255(14) 0.0336(18) -0.0078(13) 0.0176(19) -0.0095(17) 
C42 0.043(2) 0.0271(15) 0.071(3) 0.0106(16) -0.0023(19) 0.0063(14) 
C43 0.051(2) 0.0245(13) 0.0473(19) 0.0008(13) 0.0199(17) -0.0089(14) 
C60 0.0247(14) 0.0244(12) 0.0255(13) 0.0053(10) 0.0098(11) -0.0023(11) 
C61 0.0416(19) 0.0313(15) 0.0323(16) 0.0013(12) 0.0086(14) -0.0154(13) 
C62 0.0239(15) 0.0421(16) 0.0421(18) 0.0042(13) 0.0172(14) -0.0028(12) 
C63 0.0280(16) 0.0423(16) 0.0378(17) 0.0184(13) 0.0121(13) 0.0014(13) 

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

loop_ 
_geom_bond_atom_site_label_1 
_geom_bond_atom_site_label_2 
_geom_bond_distance 
_geom_bond_site_symmetry_2 
_geom_bond_publ_flag 
Mo1 O2 1.684(3) . ? 
Mo1 O1 1.698(2) . ? 
Mo1 N2 2.038(3) . ? 
Mo1 N1 2.106(3) . ? 
Mo1 Cl1 2.310(3) . ? 
N1 C1 1.345(4) . ? 
N1 N2 1.380(3) . ? 
N2 C3 1.351(3) . ? 
C1 C2 1.400(4) . ? 
C1 C10 1.510(4) . ? 
C2 C3 1.396(4) . ? 
C2 H2 0.9500 . ? 
C3 C30 1.513(4) . ? 
C10 C13 1.512(4) . ? 
C10 C11 1.520(5) . ? 
C10 C12 1.538(4) . ? 
C11 H11A 0.9800 . ? 
C11 H11B 0.9800 . ? 
C11 H11C 0.9800 . ? 
C12 H12A 0.9800 . ? 
C12 H12B 0.9800 . ? 
C12 H12C 0.9800 . ? 
C13 H13A 0.9800 . ? 
C13 H13B 0.9800 . ? 
C13 H13C 0.9800 . ? 
C30 C31 1.533(4) . ? 
C30 C32 1.535(4) . ? 
C30 C33 1.543(4) . ? 
C31 H31A 0.9800 . ? 
C31 H31B 0.9800 . ? 
C31 H31C 0.9800 . ? 
C32 H32A 0.9800 . ? 
C32 H32B 0.9800 . ? 
C32 H32C 0.9800 . ? 
C33 H33A 0.9800 . ? 
C33 H33B 0.9800 . ? 
C33 H33C 0.9800 . ? 
Mo2 O4 1.681(3) . ? 
Mo2 O3 1.694(3) . ? 
Mo2 N3 2.035(3) . ? 
Mo2 N4 2.090(3) . ? 
Mo2 Cl2 2.291(3) . ? 
N3 C4 1.343(4) . ? 
N3 N4 1.377(3) . ? 
N4 C6 1.344(4) . ? 
C4 C5 1.404(4) . ? 
C4 C40 1.515(4) . ? 
C5 C6 1.398(4) . ? 
C5 H5 0.9500 . ? 
C6 C60 1.517(4) . ? 
C40 C42 1.530(5) . ? 
C40 C43 1.533(5) . ? 
C40 C41 1.536(4) . ? 
C41 H41A 0.9800 . ? 
C41 H41B 0.9800 . ? 
C41 H41C 0.9800 . ? 
C42 H42A 0.9800 . ? 
C42 H42B 0.9800 . ? 
C42 H42C 0.9800 . ? 
C43 H43A 0.9800 . ? 
C43 H43B 0.9800 . ? 
C43 H43C 0.9800 . ? 
C60 C62 1.530(4) . ? 
C60 C63 1.537(4) . ? 
C60 C61 1.541(4) . ? 
C61 H61A 0.9800 . ? 
C61 H61B 0.9800 . ? 
C61 H61C 0.9800 . ? 
C62 H62A 0.9800 . ? 
C62 H62B 0.9800 . ? 
C62 H62C 0.9800 . ? 
C63 H63A 0.9800 . ? 
C63 H63B 0.9800 . ? 
C63 H63C 0.9800 . ? 

loop_ 
_geom_angle_atom_site_label_1 
_geom_angle_atom_site_label_2 
_geom_angle_atom_site_label_3 
_geom_angle 
_geom_angle_site_symmetry_1 
_geom_angle_site_symmetry_3 
_geom_angle_publ_flag 
O2 Mo1 O1 105.76(14) . . ? 
O2 Mo1 N2 103.38(12) . . ? 
O1 Mo1 N2 104.61(12) . . ? 
O2 Mo1 N1 109.53(13) . . ? 
O1 Mo1 N1 133.86(11) . . ? 
N2 Mo1 N1 38.86(9) . . ? 
O2 Mo1 Cl1 102.61(8) . . ? 
O1 Mo1 Cl1 105.90(9) . . ? 
N2 Mo1 Cl1 132.21(7) . . ? 
N1 Mo1 Cl1 94.47(6) . . ? 
C1 N1 N2 108.4(2) . . ? 
C1 N1 Mo1 163.3(2) . . ? 
N2 N1 Mo1 67.89(13) . . ? 
C3 N2 N1 109.5(2) . . ? 
C3 N2 Mo1 164.25(19) . . ? 
N1 N2 Mo1 73.25(15) . . ? 
N1 C1 C2 107.6(2) . . ? 
N1 C1 C10 121.3(2) . . ? 
C2 C1 C10 131.1(3) . . ? 
C3 C2 C1 107.6(2) . . ? 
C3 C2 H2 126.2 . . ? 
C1 C2 H2 126.2 . . ? 
N2 C3 C2 106.8(2) . . ? 
N2 C3 C30 123.8(2) . . ? 
C2 C3 C30 129.3(2) . . ? 
C1 C10 C13 109.7(2) . . ? 
C1 C10 C11 108.7(3) . . ? 
C13 C10 C11 110.5(3) . . ? 
C1 C10 C12 108.7(2) . . ? 
C13 C10 C12 110.6(3) . . ? 
C11 C10 C12 108.7(3) . . ? 
C10 C11 H11A 109.5 . . ? 
C10 C11 H11B 109.5 . . ? 
H11A C11 H11B 109.5 . . ? 
C10 C11 H11C 109.5 . . ? 
H11A C11 H11C 109.5 . . ? 
H11B C11 H11C 109.5 . . ? 
C10 C12 H12A 109.5 . . ? 
C10 C12 H12B 109.5 . . ? 
H12A C12 H12B 109.5 . . ? 
C10 C12 H12C 109.5 . . ? 
H12A C12 H12C 109.5 . . ? 
H12B C12 H12C 109.5 . . ? 
C10 C13 H13A 109.5 . . ? 
C10 C13 H13B 109.5 . . ? 
H13A C13 H13B 109.5 . . ? 
C10 C13 H13C 109.5 . . ? 
H13A C13 H13C 109.5 . . ? 
H13B C13 H13C 109.5 . . ? 
C3 C30 C31 110.1(2) . . ? 
C3 C30 C32 108.6(2) . . ? 
C31 C30 C32 110.6(3) . . ? 
C3 C30 C33 107.7(2) . . ? 
C31 C30 C33 110.2(2) . . ? 
C32 C30 C33 109.6(2) . . ? 
C30 C31 H31A 109.5 . . ? 
C30 C31 H31B 109.5 . . ? 
H31A C31 H31B 109.5 . . ? 
C30 C31 H31C 109.5 . . ? 
H31A C31 H31C 109.5 . . ? 
H31B C31 H31C 109.5 . . ? 
C30 C32 H32A 109.5 . . ? 
C30 C32 H32B 109.5 . . ? 
H32A C32 H32B 109.5 . . ? 
C30 C32 H32C 109.5 . . ? 
H32A C32 H32C 109.5 . . ? 
H32B C32 H32C 109.5 . . ? 
C30 C33 H33A 109.5 . . ? 
C30 C33 H33B 109.5 . . ? 
H33A C33 H33B 109.5 . . ? 
C30 C33 H33C 109.5 . . ? 
H33A C33 H33C 109.5 . . ? 
H33B C33 H33C 109.5 . . ? 
O4 Mo2 O3 106.77(14) . . ? 
O4 Mo2 N3 102.84(13) . . ? 
O3 Mo2 N3 104.01(11) . . ? 
O4 Mo2 N4 121.61(12) . . ? 
O3 Mo2 N4 121.88(12) . . ? 
N3 Mo2 N4 38.99(9) . . ? 
O4 Mo2 Cl2 103.38(10) . . ? 
O3 Mo2 Cl2 106.05(8) . . ? 
N3 Mo2 Cl2 131.83(8) . . ? 
N4 Mo2 Cl2 92.89(7) . . ? 
C4 N3 N4 109.2(2) . . ? 
C4 N3 Mo2 175.2(2) . . ? 
N4 N3 Mo2 72.66(15) . . ? 
C6 N4 N3 108.9(2) . . ? 
C6 N4 Mo2 175.1(2) . . ? 
N3 N4 Mo2 68.34(14) . . ? 
N3 C4 C5 107.2(2) . . ? 
N3 C4 C40 122.6(2) . . ? 
C5 C4 C40 130.1(2) . . ? 
C6 C5 C4 107.1(2) . . ? 
C6 C5 H5 126.4 . . ? 
C4 C5 H5 126.4 . . ? 
N4 C6 C5 107.6(2) . . ? 
N4 C6 C60 121.2(2) . . ? 
C5 C6 C60 131.2(2) . . ? 
C4 C40 C42 109.3(3) . . ? 
C4 C40 C43 110.1(2) . . ? 
C42 C40 C43 109.1(3) . . ? 
C4 C40 C41 108.7(2) . . ? 
C42 C40 C41 110.5(3) . . ? 
C43 C40 C41 109.1(3) . . ? 
C40 C41 H41A 109.5 . . ? 
C40 C41 H41B 109.5 . . ? 
H41A C41 H41B 109.5 . . ? 
C40 C41 H41C 109.5 . . ? 
H41A C41 H41C 109.5 . . ? 
H41B C41 H41C 109.5 . . ? 
C40 C42 H42A 109.5 . . ? 
C40 C42 H42B 109.5 . . ? 
H42A C42 H42B 109.5 . . ? 
C40 C42 H42C 109.5 . . ? 
H42A C42 H42C 109.5 . . ? 
H42B C42 H42C 109.5 . . ? 
C40 C43 H43A 109.5 . . ? 
C40 C43 H43B 109.5 . . ? 
H43A C43 H43B 109.5 . . ? 
C40 C43 H43C 109.5 . . ? 
H43A C43 H43C 109.5 . . ? 
H43B C43 H43C 109.5 . . ? 
C6 C60 C62 109.5(2) . . ? 
C6 C60 C63 109.3(3) . . ? 
C62 C60 C63 110.0(3) . . ? 
C6 C60 C61 108.3(2) . . ? 
C62 C60 C61 110.7(3) . . ? 
C63 C60 C61 109.0(3) . . ? 
C60 C61 H61A 109.5 . . ? 
C60 C61 H61B 109.5 . . ? 
H61A C61 H61B 109.5 . . ? 
C60 C61 H61C 109.5 . . ? 
H61A C61 H61C 109.5 . . ? 
H61B C61 H61C 109.5 . . ? 
C60 C62 H62A 109.5 . . ? 
C60 C62 H62B 109.5 . . ? 
H62A C62 H62B 109.5 . . ? 
C60 C62 H62C 109.5 . . ? 
H62A C62 H62C 109.5 . . ? 
H62B C62 H62C 109.5 . . ? 
C60 C63 H63A 109.5 . . ? 
C60 C63 H63B 109.5 . . ? 
H63A C63 H63B 109.5 . . ? 
C60 C63 H63C 109.5 . . ? 
H63A C63 H63C 109.5 . . ? 
H63B C63 H63C 109.5 . . ? 

_diffrn_measured_fraction_theta_max    0.973 
_diffrn_reflns_theta_full              27.91 
_diffrn_measured_fraction_theta_full   0.973 
_refine_diff_density_max    0.284 
_refine_diff_density_min   -0.311 
_refine_diff_density_rms    0.059