Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2001


data_global

_journal_coden_Cambridge      186

_publ_requested_journal       'Dalton Transactions'

loop_
_publ_author_name
'D.Collison'


_publ_contact_author_name     	'Dr D. Collison'  
_publ_contact_author_address 
;
Chemistry Dept
The University
Oxford Road
MANCHESTER
M13 9PL
UK
;

_publ_contact_author_email       'david.collison@man.ac.uk'
	


_audit_creation_date '19101-03-14' 
_audit_creation_method 'by teXsan v1.7' 
_audit_update_record 
; 
? 
; 
#---------------------------------------------------------------------------

_publ_section_references 
; 
ENTER OTHER REFERENCES
Molecular Structure Corporation. (1995). teXsan. 
Single Crystal Structure Analysis Software. Version 1.7. 
MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA.
Walker, N. & Stuart. D. (1983). Acta Cryst. A39, 158-166.
Altomare, A., Cascarano, M., 
Giacovazzo, C., Guagliardi, A. (1993). 
J. Appl. Cryst., 26, 343. 
;
_publ_section_acknowledgements 
; 
ENTER ACKNOWLEDGEMENTS 
;
_publ_section_table_legends 
; 
ENTER TABLE LEGENDS 
;
_publ_section_figure_captions 
; 
ENTER FIGURE CAPTIONS 
; 

data_s428 

_database_code_CSD	168519


#---------------------------------------------------------------------------
#-- 
_computing_data_collection 'MSC/AFC Diffractometer Control' 
_computing_cell_refinement 'MSC/AFC Diffractometer Control' 
_computing_data_reduction 'teXsan (MSC, 1995)' 
_computing_structure_solution 
; 
SIR92 (Altomare, et. al. 1993) 
; 
_computing_structure_refinement 'teXsan (MSC, 1995)' 
_computing_publication_material 'teXsan (MSC, 1995)' 
#---------------------------------------------------------------------------
#-- 
_cell_length_a 7.956(10) 
_cell_length_b 28.043(6) 
_cell_length_c 15.47(1) 
_cell_angle_alpha 90 
_cell_angle_beta 91.54(8) 
_cell_angle_gamma 90 
_cell_volume 3450(4) 
_cell_formula_units_Z 4 
_cell_measurement_temperature 296.2 
_cell_measurement_reflns_used 16 
_cell_measurement_theta_min 11.2 
_cell_measurement_theta_max 20.4 
#---------------------------------------------------------------------------
#-- 
_symmetry_cell_setting monoclinic 
_symmetry_space_group_name_H-M 'P 21/c ' 
_symmetry_Int_Tables_number 14 
_symmetry_space_group_name_Hall ? 
loop_ 
_symmetry_equiv_pos_as_xyz 
' +x, +y, +z' 
' -x,1/2+y,1/2-z' 
' -x, -y, -z' 
' +x,1/2-y,1/2+z' 
#---------------------------------------------------------------------------
#-- 
_exptl_crystal_description 'block' 
_exptl_crystal_colour 'brown' 
_exptl_crystal_size_max 0.35 
_exptl_crystal_size_mid 0.25 
_exptl_crystal_size_min 0.20 
_exptl_crystal_density_diffrn 1.564 
_exptl_crystal_density_meas 'not measured' 
_chemical_formula_weight 812.43 
_chemical_formula_analytical ? 
_chemical_formula_sum 'C33 H30 Cl2 N2 Mo O10 P ' 
_chemical_formula_moiety '?' 
_chemical_formula_structural ? 
_chemical_compound_source ? 
_exptl_crystal_F_000 1652.00 
_exptl_absorpt_coefficient_mu 5.576 
_exptl_absorpt_correction_type 
; 
\DF (DIFABS; Walker & Stuart, 1983) 
; 
_exptl_absorpt_correction_T_max 1.207 
_exptl_absorpt_correction_T_min 0.583 
_exptl_special_details 
; 
The scan width was (1.21+0.30tan\q)\% with an \w 
scan speed of 8\% per minute 
(up to 4 scans to achieve I/\s(I) > 10). 
Stationary background counts were recorded at each end of the 
scan, and the scan time:background time ratio was 2:1. 
; 
#---------------------------------------------------------------------------
#-- 
_diffrn_special_details 
; 
? 
; 
_diffrn_ambient_temperature 296.2 
_diffrn_radiation_wavelength 1.5418 
_diffrn_radiation_type 'Cu K\a' 
_diffrn_radiation_source 'Rigaku rotating anode' 
_diffrn_radiation_monochromator graphite 
_diffrn_radiation_detector 'scintillation counter' 
_diffrn_measurement_device 'Rigaku AFC5R' 
_diffrn_measurement_method \w-2\q
_diffrn_standards_number 3 
_diffrn_standards_interval_count 150 
_diffrn_standards_decay_% -0.60 
loop_ 
_diffrn_standard_refln_index_h 
_diffrn_standard_refln_index_k 
_diffrn_standard_refln_index_l 
? ? ? ? ? ? ? ? ? 
_diffrn_reflns_number 5679 
_reflns_number_total 5257 
_reflns_number_observed 3765 
_reflns_observed_criterion >3.00\s(I) 
_diffrn_reflns_av_R_equivalents 0.04572 
_diffrn_reflns_av_sigmaI/netI ? 
_diffrn_reflns_limit_h_min 100 
_diffrn_reflns_limit_h_max -100 
_diffrn_reflns_limit_k_min 100 
_diffrn_reflns_limit_k_max -100 
_diffrn_reflns_limit_l_min 100 
_diffrn_reflns_limit_l_max -100 
_diffrn_reflns_theta_min 0.00 
_diffrn_reflns_theta_max 60.03 
_diffrn_reflns_reduction_process 'Lp corrections applied' 
_diffrn_orient_matrix_UB_11 0.00595 
_diffrn_orient_matrix_UB_12 -0.00763 
_diffrn_orient_matrix_UB_13 -0.06298 
_diffrn_orient_matrix_UB_21 0.01037 
_diffrn_orient_matrix_UB_22 0.03474 
_diffrn_orient_matrix_UB_23 -0.01341 
_diffrn_orient_matrix_UB_31 0.12516 
_diffrn_orient_matrix_UB_32 -0.00252 
_diffrn_orient_matrix_UB_33 0.00585 
#---------------------------------------------------------------------------
#-- 
loop_ 
_atom_type_symbol 
_atom_type_oxidation_number 
_atom_type_number_in_cell 
_atom_type_scat_dispersion_real 
_atom_type_scat_dispersion_imag 
_atom_type_scat_source 
C 0 132 0.018 0.009 
;International Tables for Crystallography 
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) 
; 
H 0 120 0.000 0.000 
;International Tables for Crystallography 
(1992, Vol. C, Table 6.1.1.2) 
; 
Cl 0 8 0.364 0.702 
;International Tables for Crystallography 
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) 
; 
Mo 0 4 -0.048 2.734 
;International Tables for Crystallography 
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) 
; 
N 0 8 0.031 0.018 
;International Tables for Crystallography 
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) 
; 
O 0 40 0.049 0.032 
;International Tables for Crystallography 
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) 
; 
P 0 4 0.295 0.434 
;International Tables for Crystallography 
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) 
; 
#---------------------------------------------------------------------------
#-- 
loop_ 
_atom_site_label 
_atom_site_fract_x 
_atom_site_fract_y 
_atom_site_fract_z 
_atom_site_U_iso_or_equiv 
_atom_site_occupancy 
_atom_site_refinement_flags 
_atom_site_thermal_displace_type 
_atom_site_calc_flag 
_atom_site_calc_attached_atom 
Mo1 0.1394(2) 0.05095(4) 0.22814(7) 0.0426(3) 1.000 . Uani d ? 
O1 -0.023(1) 0.0328(3) 0.1314(5) 0.049(3) 1.000 . Uani d ? 
O2 -0.275(1) 0.0019(5) 0.0939(7) 0.081(4) 1.000 . Uani d ? 
O3 -0.065(1) 0.0856(3) 0.2693(6) 0.055(3) 1.000 . Uani d ? 
O4 0.141(2) 0.0559(4) 0.4938(6) 0.071(4) 1.000 . Uani d ? 
O5 0.217(1) 0.0606(3) 0.3538(6) 0.056(3) 1.000 . Uani d ? 
O6 0.180(1) 0.1156(3) 0.1723(6) 0.054(3) 1.000 . Uani d ? 
O7 0.298(2) 0.1536(4) 0.0613(9) 0.093(5) 1.000 . Uani d ? 
O8 0.389(1) 0.0471(3) 0.2180(4) 0.038(2) 1.000 . Uani d ? 
O9 0.300(1) -0.0866(4) 0.2004(6) 0.062(3) 1.000 . Uani d ? 
O10 0.169(1) -0.0220(3) 0.2453(5) 0.047(3) 1.000 . Uani d ? 
N1 -0.079(2) 0.0381(4) 0.2967(6) 0.040(3) 1.000 . Uani d ? 
N2 0.313(1) 0.0346(4) 0.1340(7) 0.045(3) 1.000 . Uani d ? 
C1 -0.172(2) 0.0154(6) 0.1461(8) 0.053(5) 1.000 . Uani d ? 
C2 -0.207(2) 0.0113(5) 0.242(1) 0.055(5) 1.000 . Uani d ? 
C3 -0.062(2) 0.0291(6) 0.387(1) 0.062(5) 1.000 . Uani d ? 
C4 0.110(2) 0.0501(5) 0.4128(9) 0.052(4) 1.000 . Uani d ? 
C5 0.264(2) 0.1178(6) 0.105(1) 0.068(6) 1.000 . Uani d ? 
C6 0.343(2) 0.0701(6) 0.071(1) 0.070(6) 1.000 . Uani d ? 
C7 0.332(2) -0.0164(5) 0.1170(8) 0.050(4) 1.000 . Uani d ? 
C8 0.263(2) -0.0439(5) 0.1910(8) 0.043(4) 1.000 . Uani d ? 
P1 0.9396(5) 0.1827(1) 0.5792(2) 0.047(1) 1.000 . Uani d ? 
C9 1.080(2) 0.1593(5) 0.6613(9) 0.047(4) 1.000 . Uani d ? 
C10 1.024(2) 0.1499(6) 0.740(1) 0.063(5) 1.000 . Uani d ? 
C11 1.124(3) 0.1323(7) 0.809(1) 0.078(6) 1.000 . Uani d ? 
C12 1.287(3) 0.1195(6) 0.785(1) 0.073(6) 1.000 . Uani d ? 
C13 1.347(2) 0.1277(7) 0.706(1) 0.084(7) 1.000 . Uani d ? 
C14 1.245(2) 0.1468(6) 0.643(1) 0.068(6) 1.000 . Uani d ? 
C15 0.794(2) 0.1384(5) 0.5407(10) 0.050(4) 1.000 . Uani d ? 
C16 0.774(2) 0.0970(6) 0.5875(9) 0.054(5) 1.000 . Uani d ? 
C17 0.650(2) 0.0643(5) 0.5616(8) 0.051(5) 1.000 . Uani d ? 
C18 0.551(2) 0.0718(6) 0.488(1) 0.064(5) 1.000 . Uani d ? 
C19 0.578(2) 0.1137(6) 0.440(1) 0.068(6) 1.000 . Uani d ? 
C20 0.697(2) 0.1463(5) 0.466(1) 0.066(6) 1.000 . Uani d ? 
C21 1.059(2) 0.2038(5) 0.4918(8) 0.046(4) 1.000 . Uani d ? 
C22 1.093(2) 0.1759(5) 0.422(1) 0.059(5) 1.000 . Uani d ? 
C23 1.199(3) 0.1908(6) 0.356(1) 0.071(6) 1.000 . Uani d ? 
C24 1.272(2) 0.2344(6) 0.3600(9) 0.068(6) 1.000 . Uani d ? 
C25 1.235(3) 0.2632(6) 0.431(1) 0.079(6) 1.000 . Uani d ? 
C26 1.134(2) 0.2487(6) 0.4943(9) 0.064(5) 1.000 . Uani d ? 
C27 0.823(2) 0.2305(5) 0.6287(9) 0.047(4) 1.000 . Uani d ? 
C28 0.904(2) 0.2639(6) 0.677(1) 0.069(6) 1.000 . Uani d ? 
C29 0.816(3) 0.3020(6) 0.716(1) 0.083(7) 1.000 . Uani d ? 
C30 0.646(3) 0.3047(6) 0.701(1) 0.078(7) 1.000 . Uani d ? 
C31 0.566(2) 0.2719(7) 0.653(1) 0.086(7) 1.000 . Uani d ? 
C32 0.653(2) 0.2331(6) 0.614(1) 0.062(5) 1.000 . Uani d ? 
Cl1 0.7230(9) 0.2126(2) 0.8943(4) 0.117(2) 1.000 . Uani d ? 
Cl2 0.8232(9) 0.1356(3) 1.0078(4) 0.129(3) 1.000 . Uani d ? 
C33 0.659(3) 0.1622(7) 0.950(1) 0.097(8) 1.000 . Uani d ? 
H2A -0.2037 -0.0214 0.2586 0.066 1.000 . Uiso c ? 
H2B -0.3152 0.0240 0.2529 0.066 1.000 . Uiso c ? 
H3A -0.1487 0.0444 0.4170 0.074 1.000 . Uiso c ? 
H3B -0.0641 -0.0041 0.3980 0.074 1.000 . Uiso c ? 
H6A 0.4606 0.0740 0.0640 0.084 1.000 . Uiso c ? 
H6B 0.2913 0.0615 0.0173 0.084 1.000 . Uiso c ? 
H7A 0.2716 -0.0245 0.0652 0.060 1.000 . Uiso c ? 
H7B 0.4474 -0.0238 0.1110 0.060 1.000 . Uiso c ? 
H10 0.9079 0.1554 0.7492 0.075 1.000 . Uiso c ? 
H11 1.0843 0.1293 0.8665 0.093 1.000 . Uiso c ? 
H12 1.3578 0.1044 0.8272 0.088 1.000 . Uiso c ? 
H13 1.4608 0.1201 0.6941 0.101 1.000 . Uiso c ? 
H14 1.2856 0.1516 0.5860 0.081 1.000 . Uiso c ? 
H16 0.8434 0.0909 0.6371 0.064 1.000 . Uiso c ? 
H17 0.6332 0.0364 0.5952 0.062 1.000 . Uiso c ? 
H18 0.4684 0.0494 0.4701 0.077 1.000 . Uiso c ? 
H19 0.5119 0.1194 0.3895 0.081 1.000 . Uiso c ? 
H20 0.7124 0.1744 0.4331 0.079 1.000 . Uiso c ? 
H22 1.0416 0.1453 0.4177 0.070 1.000 . Uiso c ? 
H23 1.2212 0.1700 0.3094 0.086 1.000 . Uiso c ? 
H24 1.3444 0.2452 0.3162 0.081 1.000 . Uiso c ? 
H25 1.2834 0.2941 0.4351 0.095 1.000 . Uiso c ? 
H26 1.1133 0.2694 0.5414 0.076 1.000 . Uiso c ? 
H28 1.0225 0.2618 0.6854 0.083 1.000 . Uiso c ? 
H29 0.8723 0.3248 0.7522 0.100 1.000 . Uiso c ? 
H30 0.5836 0.3306 0.7236 0.094 1.000 . Uiso c ? 
H31 0.4474 0.2742 0.6455 0.103 1.000 . Uiso c ? 
H32 0.5949 0.2102 0.5789 0.074 1.000 . Uiso c ? 
H33A 0.5741 0.1710 0.9883 0.117 1.000 . Uiso c ? 
H33B 0.6149 0.1397 0.9088 0.117 1.000 . Uiso c ?
loop_ 
_atom_site_aniso_label 
_atom_site_aniso_U_11 
_atom_site_aniso_U_22 
_atom_site_aniso_U_33 
_atom_site_aniso_U_12 
_atom_site_aniso_U_13 
_atom_site_aniso_U_23 
Mo1 0.0551(7) 0.0424(7) 0.0305(6) -0.0012(6) 0.0020(5) 0.0002(5) 
O1 0.063(6) 0.060(6) 0.024(5) 0.000(5) 0.000(5) 0.013(4) 
O2 0.073(8) 0.12(1) 0.047(7) -0.023(8) -0.015(6) 0.001(7) 
O3 0.068(7) 0.036(5) 0.059(6) 0.004(5) 0.007(6) -0.002(5) 
O4 0.089(8) 0.090(9) 0.033(6) -0.005(7) 0.005(6) -0.002(6) 
O5 0.068(7) 0.062(7) 0.038(6) -0.010(6) 0.021(5) -0.001(5) 
O6 0.077(7) 0.044(6) 0.043(6) -0.011(5) 0.024(6) 0.007(5) 
O7 0.11(1) 0.053(7) 0.12(1) -0.011(7) 0.017(9) 0.037(7) 
O8 0.080(6) 0.033(5) 0.002(3) -0.003(5) 0.004(4) 0.000(3) 
O9 0.086(8) 0.048(6) 0.053(6) 0.011(6) 0.010(6) 0.010(5) 
O10 0.083(7) 0.044(5) 0.016(4) 0.001(5) 0.015(5) 0.004(4) 
N1 0.068(8) 0.040(6) 0.014(5) 0.004(6) 0.012(5) 0.008(4) 
N2 0.049(7) 0.048(7) 0.040(7) -0.009(6) 0.006(6) -0.011(5) 
C1 0.062(10) 0.08(1) 0.013(7) 0.005(9) 0.003(7) 0.003(7) 
C2 0.063(10) 0.039(8) 0.061(10) -0.008(8) -0.015(8) 0.005(7) 
C3 0.055(10) 0.050(9) 0.08(1) -0.001(8) 0.012(9) 0.008(9) 
C4 0.069(10) 0.041(8) 0.045(9) 0.022(8) -0.025(8) -0.013(7) 
C5 0.09(1) 0.047(10) 0.07(1) -0.014(9) -0.01(1) 0.005(9) 
C6 0.09(1) 0.054(10) 0.06(1) -0.021(10) 0.01(1) -0.001(8) 
C7 0.071(10) 0.063(10) 0.017(7) 0.004(8) 0.012(7) -0.011(6) 
C8 0.061(9) 0.045(9) 0.023(7) -0.010(7) 0.005(6) 0.004(6) 
P1 0.060(2) 0.035(2) 0.045(2) -0.002(2) 0.003(2) -0.002(2) 
C9 0.066(10) 0.037(8) 0.040(8) -0.010(7) 0.011(7) -0.002(6) 
C10 0.054(10) 0.07(1) 0.06(1) 0.009(9) -0.003(8) 0.007(9) 
C11 0.09(1) 0.07(1) 0.07(1) 0.00(1) 0.00(1) 0.011(10) 
C12 0.11(2) 0.06(1) 0.05(1) 0.01(1) -0.01(1) 0.000(9) 
C13 0.06(1) 0.09(1) 0.10(2) 0.02(1) -0.02(1) -0.02(1) 
C14 0.07(1) 0.08(1) 0.05(1) 0.006(10) 0.001(9) -0.016(9) 
C15 0.047(8) 0.043(8) 0.060(10) 0.001(7) 0.005(8) -0.001(7) 
C16 0.061(10) 0.07(1) 0.033(8) 0.003(9) -0.003(7) 0.009(7) 
C17 0.08(1) 0.055(9) 0.018(7) -0.004(8) 0.025(8) -0.009(6) 
C18 0.06(1) 0.06(1) 0.07(1) -0.015(9) -0.009(9) -0.009(9) 
C19 0.07(1) 0.06(1) 0.07(1) 0.010(9) -0.016(9) -0.012(9) 
C20 0.09(1) 0.039(9) 0.07(1) 0.000(9) -0.01(1) -0.008(8) 
C21 0.068(10) 0.033(7) 0.036(8) -0.003(7) -0.003(7) -0.004(6) 
C22 0.08(1) 0.034(8) 0.07(1) -0.005(8) 0.007(9) -0.008(7) 
C23 0.11(1) 0.06(1) 0.044(10) -0.01(1) 0.02(1) -0.008(8) 
C24 0.10(1) 0.09(1) 0.014(7) -0.02(1) 0.017(8) 0.014(7) 
C25 0.11(2) 0.07(1) 0.06(1) -0.03(1) 0.00(1) -0.006(9) 
C26 0.09(1) 0.07(1) 0.031(8) -0.020(10) 0.016(9) -0.005(8) 
C27 0.058(9) 0.036(8) 0.048(9) -0.003(7) 0.003(7) 0.003(7) 
C28 0.07(1) 0.07(1) 0.06(1) 0.00(1) 0.007(10) -0.011(9) 
C29 0.12(2) 0.06(1) 0.07(1) 0.00(1) 0.03(1) -0.001(10) 
C30 0.10(2) 0.04(1) 0.09(1) 0.00(1) 0.04(1) -0.003(9) 
C31 0.07(1) 0.08(1) 0.11(2) 0.02(1) 0.01(1) 0.02(1) 
C32 0.07(1) 0.049(9) 0.06(1) -0.005(9) 0.004(9) -0.015(8) 
Cl1 0.145(6) 0.091(4) 0.117(5) -0.002(4) 0.032(4) -0.009(4) 
Cl2 0.147(6) 0.144(6) 0.094(4) 0.034(5) -0.012(4) -0.011(4) 
C33 0.11(2) 0.08(1) 0.11(2) 0.00(1) 0.04(1) -0.02(1) 
#---------------------------------------------------------------------------
#-- 
_refine_special_details 
; 
? 
; 
_refine_ls_structure_factor_coef F 
_refine_ls_matrix_type full 
_refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]' 
_refine_ls_hydrogen_treatment noref 
_refine_ls_extinction_method none 
_refine_ls_extinction_coef ? 
_refine_ls_abs_structure_details ? 
_refine_ls_abs_structure_Flack ? 
_refine_ls_number_reflns 3765 
_refine_ls_number_parameters 442 
_refine_ls_number_restraints 0 
_refine_ls_number_constraints 0 
_refine_ls_R_factor_all ? 
_refine_ls_R_factor_obs 0.0981 
_refine_ls_wR_factor_all ? 
_refine_ls_wR_factor_obs 0.1297 
_refine_ls_goodness_of_fit_all ? 
_refine_ls_goodness_of_fit_obs 3.581 
_refine_ls_shift/esd_max 0.1420 
_refine_ls_shift/esd_mean 0.0000 
_refine_diff_density_min -1.08 
_refine_diff_density_max 1.09 
#---------------------------------------------------------------------------
#-- 
_geom_special_details 
; 
? 
; 
loop_ 
_geom_bond_atom_site_label_1 
_geom_bond_atom_site_label_2 
_geom_bond_distance 
_geom_bond_site_symmetry_1 
_geom_bond_site_symmetry_2 
_geom_bond_publ_flag 
MO1 O1 2.014(9) . . yes 
MO1 O3 2.01(1) . . yes 
MO1 O5 2.042(10) . . yes 
MO1 O6 2.038(9) . . yes 
MO1 O8 2.00(1) . . yes 
MO1 O10 2.074(9) . . yes 
MO1 N1 2.09(1) . . yes 
MO1 N2 2.09(1) . . yes 
O1 C1 1.31(2) . . yes 
O2 C1 1.20(2) . . yes 
O3 N1 1.41(1) . . yes 
O4 C4 1.28(2) . . yes 
O5 C4 1.30(2) . . yes 
O6 C5 1.26(2) . . yes 
O7 C5 1.24(2) . . yes 
O8 N2 1.46(1) . . yes 
O9 C8 1.24(2) . . yes 
O10 C8 1.30(2) . . yes 
N1 C2 1.50(2) . . yes 
N1 C3 1.42(2) . . yes 
N2 C6 1.42(2) . . yes 
N2 C7 1.46(2) . . yes 
C1 C2 1.53(2) . . yes 
C2 H2A 0.95 . . no 
C2 H2B 0.95 . . no 
C3 C4 1.53(2) . . yes 
C3 H3A 0.95 . . no 
C3 H3B 0.95 . . no 
C5 C6 1.57(2) . . yes 
C6 H6A 0.95 . . no 
C6 H6B 0.95 . . no 
C7 C8 1.50(2) . . yes 
C7 H7A 0.95 . . no 
C7 H7B 0.95 . . no 
P1 C9 1.80(1) . . yes 
P1 C15 1.79(1) . . yes 
P1 C21 1.78(1) . . yes 
P1 C27 1.81(1) . . yes 
C9 C10 1.33(2) . . yes 
C9 C14 1.39(2) . . yes 
C10 C11 1.41(2) . . yes 
C10 H10 0.95 . . no 
C11 C12 1.41(3) . . yes 
C11 H11 0.95 . . no 
C12 C13 1.35(3) . . yes 
C12 H12 0.95 . . no 
C13 C14 1.37(3) . . yes 
C13 H13 0.95 . . no 
C14 H14 0.95 . . no 
C15 C16 1.38(2) . . yes 
C15 C20 1.39(2) . . yes 
C16 C17 1.40(2) . . yes 
C16 H16 0.95 . . no 
C17 C18 1.38(2) . . yes 
C17 H17 0.95 . . no 
C18 C19 1.41(2) . . yes 
C18 H18 0.95 . . no 
C19 C20 1.37(2) . . yes 
C19 H19 0.95 . . no 
C20 H20 0.95 . . no 
C21 C22 1.36(2) . . yes 
C21 C26 1.39(2) . . yes 
C22 C23 1.41(2) . . yes 
C22 H22 0.95 . . no 
C23 C24 1.35(3) . . yes 
C23 H23 0.95 . . no 
C24 C25 1.40(2) . . yes 
C24 H24 0.95 . . no 
C25 C26 1.34(2) . . yes 
C25 H25 0.95 . . no 
C26 H26 0.95 . . no 
C27 C28 1.35(2) . . yes 
C27 C32 1.37(2) . . yes 
C28 C29 1.42(3) . . yes 
C28 H28 0.95 . . no 
C29 C30 1.37(3) . . yes 
C29 H29 0.95 . . no 
C30 C31 1.32(3) . . yes 
C30 H30 0.95 . . no 
C31 C32 1.43(3) . . yes 
C31 H31 0.95 . . no 
C32 H32 0.95 . . no 
CL1 C33 1.74(2) . . yes 
CL2 C33 1.73(2) . . yes 
C33 H33A 0.95 . . no 
C33 H33B 0.95 . . no 
#---------------------------------------------------------------------------
#-- 
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_2 
_geom_angle_site_symmetry_3 
_geom_angle_publ_flag 
O1 MO1 O3 81.4(4) . . . yes 
O1 MO1 O5 155.8(4) . . . yes 
O1 MO1 O6 90.8(4) . . . yes 
O1 MO1 O8 123.1(3) . . . yes 
O1 MO1 O10 85.1(4) . . . yes 
O1 MO1 N1 79.0(4) . . . yes 
O1 MO1 N2 81.3(4) . . . yes 
O3 MO1 O5 82.0(4) . . . yes 
O3 MO1 O6 80.8(4) . . . yes 
O3 MO1 O8 149.7(4) . . . yes 
O3 MO1 O10 121.7(4) . . . yes 
O3 MO1 N1 40.0(4) . . . yes 
O3 MO1 N2 152.1(4) . . . yes 
O5 MO1 O6 103.8(4) . . . yes 
O5 MO1 O8 78.8(4) . . . yes 
O5 MO1 O10 88.8(3) . . . yes 
O5 MO1 N1 77.0(4) . . . yes 
O5 MO1 N2 120.3(4) . . . yes 
O6 MO1 O8 81.3(4) . . . yes 
O6 MO1 O10 156.0(4) . . . yes 
O6 MO1 N1 120.7(4) . . . yes 
O6 MO1 N2 77.6(4) . . . yes 
O8 MO1 O10 81.2(4) . . . yes 
O8 MO1 N1 150.6(4) . . . yes 
O8 MO1 N2 41.9(4) . . . yes 
O10 MO1 N1 81.8(4) . . . yes 
O10 MO1 N2 78.3(4) . . . yes 
N1 MO1 N2 153.0(4) . . . yes 
MO1 O1 C1 122.1(8) . . . yes 
MO1 O3 N1 73.1(6) . . . yes 
MO1 O5 C4 116.9(9) . . . yes 
MO1 O6 C5 119.2(9) . . . yes 
MO1 O8 N2 72.3(6) . . . yes 
MO1 O10 C8 116.8(8) . . . yes 
MO1 N1 O3 66.9(6) . . . yes 
MO1 N1 C2 111.2(8) . . . yes 
MO1 N1 C3 117.8(9) . . . yes 
O3 N1 C2 111.4(10) . . . yes 
O3 N1 C3 117(1) . . . yes 
C2 N1 C3 120(1) . . . yes 
MO1 N2 O8 65.8(6) . . . yes 
MO1 N2 C6 116.8(10) . . . yes 
MO1 N2 C7 114.4(8) . . . yes 
O8 N2 C6 111(1) . . . yes 
O8 N2 C7 110.7(9) . . . yes 
C6 N2 C7 123(1) . . . yes 
O1 C1 O2 127(1) . . . yes 
O1 C1 C2 112(1) . . . yes 
O2 C1 C2 119(1) . . . yes 
N1 C2 C1 111(1) . . . yes 
N1 C2 H2A 108.9 . . . no 
N1 C2 H2B 108.8 . . . no 
C1 C2 H2A 108.9 . . . no 
C1 C2 H2B 109.0 . . . no 
H2A C2 H2B 109.4 . . . no 
N1 C3 C4 104(1) . . . yes 
N1 C3 H3A 110.6 . . . no 
N1 C3 H3B 110.8 . . . no 
C4 C3 H3A 110.5 . . . no 
C4 C3 H3B 110.7 . . . no 
H3A C3 H3B 109.5 . . . no 
O4 C4 O5 123(1) . . . yes 
O4 C4 C3 117(1) . . . yes 
O5 C4 C3 119(1) . . . yes 
O6 C5 O7 128(1) . . . yes 
O6 C5 C6 117(1) . . . yes 
O7 C5 C6 114(1) . . . yes 
N2 C6 C5 107(1) . . . yes 
N2 C6 H6A 110.1 . . . no 
N2 C6 H6B 110.2 . . . no 
C5 C6 H6A 110.1 . . . no 
C5 C6 H6B 110.1 . . . no 
H6A C6 H6B 109.3 . . . no 
N2 C7 C8 109(1) . . . yes 
N2 C7 H7A 109.7 . . . no 
N2 C7 H7B 109.6 . . . no 
C8 C7 H7A 109.7 . . . no 
C8 C7 H7B 109.5 . . . no 
H7A C7 H7B 109.3 . . . no 
O9 C8 O10 121(1) . . . yes 
O9 C8 C7 120(1) . . . yes 
O10 C8 C7 118(1) . . . yes 
C9 P1 C15 111.6(7) . . . yes 
C9 P1 C21 108.9(7) . . . yes 
C9 P1 C27 106.7(7) . . . yes 
C15 P1 C21 109.5(7) . . . yes 
C15 P1 C27 108.6(7) . . . yes 
C21 P1 C27 111.5(6) . . . yes 
P1 C9 C10 119(1) . . . yes 
P1 C9 C14 121(1) . . . yes 
C10 C9 C14 118(1) . . . yes 
C9 C10 C11 124(1) . . . yes 
C9 C10 H10 117.7 . . . no 
C11 C10 H10 117.8 . . . no 
C10 C11 C12 113(1) . . . yes 
C10 C11 H11 123.4 . . . no 
C12 C11 H11 123.5 . . . no 
C11 C12 C13 123(1) . . . yes 
C11 C12 H12 118.1 . . . no 
C13 C12 H12 118.4 . . . no 
C12 C13 C14 119(1) . . . yes 
C12 C13 H13 120.0 . . . no 
C14 C13 H13 120.3 . . . no 
C9 C14 C13 119(1) . . . yes 
C9 C14 H14 120.2 . . . no 
C13 C14 H14 120.1 . . . no 
P1 C15 C16 119(1) . . . yes 
P1 C15 C20 120(1) . . . yes 
C16 C15 C20 120(1) . . . yes 
C15 C16 C17 119(1) . . . yes 
C15 C16 H16 120.3 . . . no 
C17 C16 H16 120.2 . . . no 
C16 C17 C18 121(1) . . . yes 
C16 C17 H17 119.5 . . . no 
C18 C17 H17 119.3 . . . no 
C17 C18 C19 117(1) . . . yes 
C17 C18 H18 121.1 . . . no 
C19 C18 H18 120.9 . . . no 
C18 C19 C20 121(1) . . . yes 
C18 C19 H19 119.3 . . . no 
C20 C19 H19 119.4 . . . no 
C15 C20 C19 119(1) . . . yes 
C15 C20 H20 120.1 . . . no 
C19 C20 H20 120.0 . . . no 
P1 C21 C22 122(1) . . . yes 
P1 C21 C26 121(1) . . . yes 
C22 C21 C26 116(1) . . . yes 
C21 C22 C23 122(1) . . . yes 
C21 C22 H22 118.8 . . . no 
C23 C22 H22 118.8 . . . no 
C22 C23 C24 120(1) . . . yes 
C22 C23 H23 119.9 . . . no 
C24 C23 H23 119.8 . . . no 
C23 C24 C25 117(1) . . . yes 
C23 C24 H24 121.6 . . . no 
C25 C24 H24 121.3 . . . no 
C24 C25 C26 122(1) . . . yes 
C24 C25 H25 118.8 . . . no 
C26 C25 H25 118.6 . . . no 
C21 C26 C25 121(1) . . . yes 
C21 C26 H26 119.5 . . . no 
C25 C26 H26 119.4 . . . no 
P1 C27 C28 120(1) . . . yes 
P1 C27 C32 118(1) . . . yes 
C28 C27 C32 120(1) . . . yes 
C27 C28 C29 121(1) . . . yes 
C27 C28 H28 119.2 . . . no 
C29 C28 H28 119.2 . . . no 
C28 C29 C30 117(1) . . . yes 
C28 C29 H29 121.4 . . . no 
C30 C29 H29 121.1 . . . no 
C29 C30 C31 120(1) . . . yes 
C29 C30 H30 119.6 . . . no 
C31 C30 H30 119.4 . . . no 
C30 C31 C32 122(1) . . . yes 
C30 C31 H31 118.8 . . . no 
C32 C31 H31 118.9 . . . no 
C27 C32 C31 117(1) . . . yes 
C27 C32 H32 121.3 . . . no 
C31 C32 H32 121.6 . . . no 
CL1 C33 CL2 112(1) . . . yes 
CL1 C33 H33A 108.9 . . . no 
CL1 C33 H33B 108.7 . . . no 
CL2 C33 H33A 108.8 . . . no 
CL2 C33 H33B 108.7 . . . no 
H33A C33 H33B 109.4 . . . no 
#---------------------------------------------------------------------------
#-- 
loop_ 
_geom_contact_atom_site_label_1 
_geom_contact_atom_site_label_2 
_geom_contact_distance 
_geom_contact_site_symmetry_1 
_geom_contact_site_symmetry_2 
_geom_contact_publ_flag 
O2 C7 3.20(2) . 1_455 no 
O2 C6 3.29(2) . 3 no 
O4 C3 3.09(2) . 3_556 no 
O4 C18 3.30(2) . . no 
O7 C25 3.11(2) . 4_454 no 
O7 C26 3.20(2) . 4_454 no 
O7 C31 3.28(2) . 4_554 no 
O9 C33 3.17(2) . 3_656 no 
O9 C10 3.28(2) . 3_656 no 
#---------------------------------------------------------------------------
#-- 
loop_ 
_geom_torsion_atom_site_label_1 
_geom_torsion_atom_site_label_2 
_geom_torsion_atom_site_label_3 
_geom_torsion_atom_site_label_4 
_geom_torsion 
_geom_torsion_site_symmetry_1 
_geom_torsion_site_symmetry_2 
_geom_torsion_site_symmetry_3 
_geom_torsion_site_symmetry_4 
_geom_torsion_publ_flag 
MO1 O1 C1 O2 . . . . -177(1) no 
MO1 O1 C1 C2 . . . . 0(1) no 
MO1 O3 N1 C2 . . . . -104.8(9) no 
MO1 O3 N1 C3 . . . . 110(1) no 
MO1 O5 C4 O4 . . . . -177(1) no 
MO1 O5 C4 C3 . . . . 3(1) no 
MO1 O6 C5 O7 . . . . 177(1) no 
MO1 O6 C5 C6 . . . . -3(1) no 
MO1 O8 N2 C6 . . . . 110(1) no 
MO1 O8 N2 C7 . . . . -108.3(10) no 
MO1 O10 C8 O9 . . . . 173(1) no 
MO1 O10 C8 C7 . . . . -4(1) no 
MO1 N1 C2 C1 . . . . -19(1) no 
MO1 N1 C3 C4 . . . . 20(1) no 
MO1 N2 C6 C5 . . . . 13(1) no 
MO1 N2 C7 C8 . . . . -18(1) no 
O1 MO1 O3 N1 . . . . 83.0(6) no 
O1 MO1 O5 C4 . . . . 0(1) no 
O1 MO1 O6 C5 . . . . -72(1) no 
O1 MO1 O8 N2 . . . . 4.0(7) no 
O1 MO1 O10 C8 . . . . 77.5(9) no 
O1 MO1 N1 O3 . . . . -89.8(6) no 
O1 MO1 N1 C2 . . . . 15.4(8) no 
O1 MO1 N1 C3 . . . . 160(1) no 
O1 MO1 N2 O8 . . . . -176.6(6) no 
O1 MO1 N2 C6 . . . . 80(1) no 
O1 MO1 N2 C7 . . . . -73.7(9) no 
O1 C1 C2 N1 . . . . 12(1) no 
O2 C1 C2 N1 . . . . -169(1) no 
O3 MO1 O1 C1 . . . . -49(1) no 
O3 MO1 O5 C4 . . . . 47.2(10) no 
O3 MO1 O6 C5 . . . . -153(1) no 
O3 MO1 O8 N2 . . . . -135.6(8) no 
O3 MO1 O10 C8 . . . . 154.2(9) no 
O3 MO1 N1 C2 . . . . 105(1) no 
O3 MO1 N1 C3 . . . . -109(1) no 
O3 MO1 N2 O8 . . . . 131.1(8) no 
O3 MO1 N2 C6 . . . . 28(1) no 
O3 MO1 N2 C7 . . . . -126(1) no 
O3 N1 MO1 O5 . . . . 93.0(6) no 
O3 N1 MO1 O6 . . . . -5.4(7) no 
O3 N1 MO1 O8 . . . . 128.4(7) no 
O3 N1 MO1 O10 . . . . -176.3(6) no 
O3 N1 MO1 N2 . . . . -133.5(9) no 
O3 N1 C2 C1 . . . . 53(1) no 
O3 N1 C3 C4 . . . . -55(1) no 
O4 C4 C3 N1 . . . . 165(1) no 
O5 MO1 O1 C1 . . . . -2(1) no 
O5 MO1 O3 N1 . . . . -79.3(6) no 
O5 MO1 O6 C5 . . . . 127(1) no 
O5 MO1 O8 N2 . . . . 172.8(6) no 
O5 MO1 O10 C8 . . . . -126.0(9) no 
O5 MO1 N1 C2 . . . . -161.9(9) no 
O5 MO1 N1 C3 . . . . -16.7(9) no 
O5 MO1 N2 O8 . . . . -8.2(7) no 
O5 MO1 N2 C6 . . . . -111(1) no 
O5 MO1 N2 C7 . . . . 94.6(9) no 
O5 C4 C3 N1 . . . . -15(1) no 
O6 MO1 O1 C1 . . . . -130(1) no 
O6 MO1 O3 N1 . . . . 175.3(6) no 
O6 MO1 O5 C4 . . . . 125.7(10) no 
O6 MO1 O8 N2 . . . . -81.2(6) no 
O6 MO1 O10 C8 . . . . -3(1) no 
O6 MO1 N1 C2 . . . . 99.7(9) no 
O6 MO1 N1 C3 . . . . -115.2(10) no 
O6 MO1 N2 O8 . . . . 90.6(6) no 
O6 MO1 N2 C6 . . . . -12(1) no 
O6 MO1 N2 C7 . . . . -166.5(9) no 
O6 C5 C6 N2 . . . . -6(2) no 
O7 C5 C6 N2 . . . . 172(1) no 
O8 MO1 O1 C1 . . . . 149(1) no 
O8 MO1 O3 N1 . . . . -130.3(7) no 
O8 MO1 O5 C4 . . . . -156.3(10) no 
O8 MO1 O6 C5 . . . . 50(1) no 
O8 MO1 O10 C8 . . . . -47.1(9) no 
O8 MO1 N1 C2 . . . . -126.5(9) no 
O8 MO1 N1 C3 . . . . 18(1) no 
O8 MO1 N2 C6 . . . . -103(1) no 
O8 MO1 N2 C7 . . . . 102(1) no 
O8 N2 MO1 O10 . . . . -89.8(5) no 
O8 N2 MO1 N1 . . . . -133.3(8) no 
O8 N2 C6 C5 . . . . -59(1) no 
O8 N2 C7 C8 . . . . 53(1) no 
O9 C8 C7 N2 . . . . -163(1) no 
O10 MO1 O1 C1 . . . . 73(1) no 
O10 MO1 O3 N1 . . . . 4.3(7) no 
O10 MO1 O5 C4 . . . . -75.1(10) no 
O10 MO1 O6 C5 . . . . 7(1) no 
O10 MO1 O8 N2 . . . . 82.3(6) no 
O10 MO1 N1 C2 . . . . -71.2(8) no 
O10 MO1 N1 C3 . . . . 73.9(10) no 
O10 MO1 N2 C6 . . . . 167(1) no 
O10 MO1 N2 C7 . . . . 13.0(9) no 
O10 C8 C7 N2 . . . . 15(1) no 
N1 MO1 O1 C1 . . . . -9(1) no 
N1 MO1 O5 C4 . . . . 6.8(9) no 
N1 MO1 O6 C5 . . . . -150(1) no 
N1 MO1 O8 N2 . . . . 137.7(8) no 
N1 MO1 O10 C8 . . . . 157.0(10) no 
N1 MO1 N2 C6 . . . . 123(1) no 
N1 MO1 N2 C7 . . . . -30(1) no 
N1 O3 MO1 N2 . . . . 135.3(9) no 
N2 MO1 O1 C1 . . . . 152(1) no 
N2 MO1 O5 C4 . . . . -150.8(9) no 
N2 MO1 O6 C5 . . . . 8(1) no 
N2 MO1 O10 C8 . . . . -4.6(9) no 
N2 MO1 N1 C2 . . . . -28(1) no 
N2 MO1 N1 C3 . . . . 116(1) no 
C1 C2 N1 C3 . . . . -163(1) no 
C2 N1 C3 C4 . . . . 162(1) no 
C5 C6 N2 C7 . . . . 165(1) no 
C6 N2 C7 C8 . . . . -170(1) no 
P1 C9 C10 C11 . . . . -178(1) no 
P1 C9 C14 C13 . . . . -177(1) no 
P1 C15 C16 C17 . . . . 174(1) no 
P1 C15 C20 C19 . . . . -175(1) no 
P1 C21 C22 C23 . . . . -174(1) no 
P1 C21 C26 C25 . . . . 174(1) no 
P1 C27 C28 C29 . . . . 179(1) no 
P1 C27 C32 C31 . . . . -179(1) no 
C9 P1 C15 C16 . . . . 15(1) no 
C9 P1 C15 C20 . . . . -167(1) no 
C9 P1 C21 C22 . . . . 93(1) no 
C9 P1 C21 C26 . . . . -81(1) no 
C9 P1 C27 C28 . . . . 46(1) no 
C9 P1 C27 C32 . . . . -135(1) no 
C9 C10 C11 C12 . . . . -7(2) no 
C9 C14 C13 C12 . . . . 2(2) no 
C10 C9 P1 C15 . . . . -71(1) no 
C10 C9 P1 C21 . . . . 167(1) no 
C10 C9 P1 C27 . . . . 46(1) no 
C10 C9 C14 C13 . . . . -3(2) no 
C10 C11 C12 C13 . . . . 6(2) no 
C11 C10 C9 C14 . . . . 6(2) no 
C11 C12 C13 C14 . . . . -3(2) no 
C14 C9 P1 C15 . . . . 102(1) no 
C14 C9 P1 C21 . . . . -18(1) no 
C14 C9 P1 C27 . . . . -139(1) no 
C15 P1 C21 C22 . . . . -28(1) no 
C15 P1 C21 C26 . . . . 155(1) no 
C15 P1 C27 C28 . . . . 167(1) no 
C15 P1 C27 C32 . . . . -14(1) no 
C15 C16 C17 C18 . . . . 2(2) no 
C15 C20 C19 C18 . . . . 0(2) no 
C16 C15 P1 C21 . . . . 135(1) no 
C16 C15 P1 C27 . . . . -102(1) no 
C16 C15 C20 C19 . . . . 1(2) no 
C16 C17 C18 C19 . . . . 0(2) no 
C17 C16 C15 C20 . . . . -2(2) no 
C17 C18 C19 C20 . . . . 0(2) no 
C20 C15 P1 C21 . . . . -46(1) no 
C20 C15 P1 C27 . . . . 75(1) no 
C21 P1 C27 C28 . . . . -71(1) no 
C21 P1 C27 C32 . . . . 105(1) no 
C21 C22 C23 C24 . . . . -1(2) no 
C21 C26 C25 C24 . . . . 0(2) no 
C22 C21 P1 C27 . . . . -149(1) no 
C22 C21 C26 C25 . . . . 0(2) no 
C22 C23 C24 C25 . . . . 0(2) no 
C23 C22 C21 C26 . . . . 1(2) no 
C23 C24 C25 C26 . . . . 0(2) no 
C26 C21 P1 C27 . . . . 35(1) no 
C27 C28 C29 C30 . . . . -2(2) no 
C27 C32 C31 C30 . . . . 1(2) no 
C28 C27 C32 C31 . . . . -1(2) no 
C28 C29 C30 C31 . . . . 2(2) no 
C29 C28 C27 C32 . . . . 1(2) no 
C29 C30 C31 C32 . . . . -2(3)
no#-------------------------------------------------------------------------
#---- 
#===END

data_S588 

_database_code_CSD	168520

#---------------------------------------------------------------------------
#-- 
_audit_creation_date '19100-08-10' 
_audit_creation_method 'by teXsan v1.7' 
_audit_update_record 
; 
? 
; 
#---------------------------------------------------------------------------
#-- 

_publ_section_references 
; 
ENTER OTHER REFERENCES
Molecular Structure Corporation. (1995). teXsan. 
Single Crystal Structure Analysis Software. Version 1.7. 
MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA.
North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). 
Acta Cryst. A24, 351-359.
Sheldrick, G.M. (1985). In: "Crystallographic 
Computing 3" (Eds G.M. Sheldrick, C. Kruger and 
R. Goddard) Oxford University Press, pp. 175-189. 
;
_publ_section_acknowledgements 
; 
ENTER ACKNOWLEDGEMENTS 
;
_publ_section_table_legends 
; 
ENTER TABLE LEGENDS 
;
_publ_section_figure_captions 
; 
ENTER FIGURE CAPTIONS 
; 
#---------------------------------------------------------------------------
#-- 
_computing_data_collection 'MSC/AFC Diffractometer Control' 
_computing_cell_refinement 'MSC/AFC Diffractometer Control' 
_computing_data_reduction 'teXsan (MSC, 1995)' 
_computing_structure_solution 
; 
SHELXS86 (Sheldrick, 1985) 
; 
_computing_structure_refinement 'teXsan (MSC, 1995)' 
_computing_publication_material 'teXsan (MSC, 1995)' 
#---------------------------------------------------------------------------
#-- 
_cell_length_a 28.23(1) 
_cell_length_b 30.29(1) 
_cell_length_c 11.64(1) 
_cell_angle_alpha 90 
_cell_angle_beta 90 
_cell_angle_gamma 90 
_cell_volume 9956(17) 
_cell_formula_units_Z 16 
_cell_measurement_temperature 293.2 
_cell_measurement_reflns_used 24 
_cell_measurement_theta_min 31.8 
_cell_measurement_theta_max 37.9 
#---------------------------------------------------------------------------
#-- 
_symmetry_cell_setting orthorhombic 
_symmetry_space_group_name_H-M 'F d d d ' 
_symmetry_Int_Tables_number 70 
_symmetry_space_group_name_Hall ? 
loop_ 
_symmetry_equiv_pos_as_xyz 
' +x, +y, +z' 
' +x,1/2+y,1/2+z' 
'1/2+x, +y,1/2+z' 
'1/2+x,1/2+y, +z' 
' +x,1/4-y,1/4-z' 
' +x,3/4-y,3/4-z' 
'1/2+x,1/4-y,3/4-z' 
'1/2+x,3/4-y,1/4-z' 
'1/4-x, +y,1/4-z' 
'1/4-x,1/2+y,3/4-z' 
'3/4-x, +y,3/4-z' 
'3/4-x,1/2+y,1/4-z' 
'1/4-x,1/4-y, +z' 
'1/4-x,3/4-y,1/2+z' 
'3/4-x,1/4-y,1/2+z' 
'3/4-x,3/4-y, +z' 
' -x, -y, -z' 
' -x,1/2-y,1/2-z' 
'1/2-x, -y,1/2-z' 
'1/2-x,1/2-y, -z' 
' -x,1/4+y,1/4+z' 
' -x,3/4+y,3/4+z' 
'1/2-x,1/4+y,3/4+z' 
'1/2-x,3/4+y,1/4+z' 
'1/4+x, -y,1/4+z' 
'1/4+x,1/2-y,3/4+z' 
'3/4+x, -y,3/4+z' 
'3/4+x,1/2-y,1/4+z' 
'1/4+x,1/4+y, -z' 
'1/4+x,3/4+y,1/2-z' 
'3/4+x,1/4+y,1/2-z' 
'3/4+x,3/4+y, -z' 
#---------------------------------------------------------------------------
#-- 
_exptl_crystal_description 'block' 
_exptl_crystal_colour 'red' 
_exptl_crystal_size_max 0.25 
_exptl_crystal_size_mid 0.17 
_exptl_crystal_size_min 0.17 
_exptl_crystal_density_diffrn 1.460 
_exptl_crystal_density_meas 'not measured' 
_chemical_formula_weight 547.32 
_chemical_formula_analytical ? 
_chemical_formula_sum 'C18 H24 N2 Mo Na O10 ' 
_chemical_formula_moiety '?' 
_chemical_formula_structural ? 
_chemical_compound_source ? 
_exptl_crystal_F_000 4464.00 
_exptl_absorpt_coefficient_mu 4.933 
_exptl_absorpt_correction_type 
; 
\y scans (North,Phillips & Matthews, 1968) 
; 
_exptl_absorpt_correction_T_max 1.000 
_exptl_absorpt_correction_T_min 0.919 
_exptl_special_details 
; 
The scan width was (1.73+0.30tan\q)\% with an \w 
scan speed of 8\% per minute 
(up to 4 scans to achieve I/\s(I) > 10). 
Stationary background counts were recorded at each end of the 
scan, and the scan time:background time ratio was 2:1. 
; 
#---------------------------------------------------------------------------
#-- 
_diffrn_special_details 
; 
? 
; 
_diffrn_ambient_temperature 293.2 
_diffrn_radiation_wavelength 1.5418 
_diffrn_radiation_type 'Cu K\a' 
_diffrn_radiation_source 'Rigaku rotating anode' 
_diffrn_radiation_monochromator graphite 
_diffrn_radiation_detector 'scintillation counter' 
_diffrn_measurement_device 'Rigaku AFC5R' 
_diffrn_measurement_method \w-2\q
_diffrn_standards_number 3 
_diffrn_standards_interval_count 150 
_diffrn_standards_decay_% -3.02 
loop_ 
_diffrn_standard_refln_index_h 
_diffrn_standard_refln_index_k 
_diffrn_standard_refln_index_l 
5 5 1 
6 2 0 
3 7 1 
_diffrn_reflns_number 2857 
_reflns_number_total 2857 
_reflns_number_observed 1583 
_reflns_observed_criterion >2.00\s(I) 
_diffrn_reflns_av_R_equivalents 0.00000 
_diffrn_reflns_av_sigmaI/netI 0.140 
_diffrn_reflns_limit_h_min -22 
_diffrn_reflns_limit_h_max 36 
_diffrn_reflns_limit_k_min -26 
_diffrn_reflns_limit_k_max 38 
_diffrn_reflns_limit_l_min -14 
_diffrn_reflns_limit_l_max 14 
_diffrn_reflns_theta_min 2.91 
_diffrn_reflns_theta_max 79.45 
_diffrn_reflns_reduction_process 'Lp corrections applied' 
_diffrn_orient_matrix_UB_11 -0.02446 
_diffrn_orient_matrix_UB_12 0.02262 
_diffrn_orient_matrix_UB_13 -0.01995 
_diffrn_orient_matrix_UB_21 0.02471 
_diffrn_orient_matrix_UB_22 0.02362 
_diffrn_orient_matrix_UB_23 0.00323 
_diffrn_orient_matrix_UB_31 0.00680 
_diffrn_orient_matrix_UB_32 -0.00449 
_diffrn_orient_matrix_UB_33 -0.08347 
#---------------------------------------------------------------------------
#-- 
loop_ 
_atom_type_symbol 
_atom_type_oxidation_number 
_atom_type_number_in_cell 
_atom_type_scat_dispersion_real 
_atom_type_scat_dispersion_imag 
_atom_type_scat_source 
C 0 288 0.018 0.009 
;International Tables for Crystallography 
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) 
; 
H 0 384 0.000 0.000 
;International Tables for Crystallography 
(1992, Vol. C, Table 6.1.1.2) 
; 
N 0 32 0.031 0.018 
;International Tables for Crystallography 
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) 
; 
O 0 160 0.049 0.032 
;International Tables for Crystallography 
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) 
; 
Mo 0 16 -0.048 2.734 
;International Tables for Crystallography 
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) 
; 
Na 0 16 0.135 0.124 
;International Tables for Crystallography 
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) 
; 
#---------------------------------------------------------------------------
#-- 
loop_ 
_atom_site_label 
_atom_site_fract_x 
_atom_site_fract_y 
_atom_site_fract_z 
_atom_site_U_iso_or_equiv 
_atom_site_occupancy 
_atom_site_refinement_flags 
_atom_site_thermal_displace_type 
_atom_site_calc_flag 
_atom_site_calc_attached_atom 
Mo(1) 0.98762(4) 0.1250 0.1250 0.0430(2) 0.500 ST Uani d ? 
Na(1) 0.8750 -0.0241(1) -0.1250 0.056(1) 0.500 ST Uani d ? 
O(1) 1.0421(2) 0.1677(2) 0.0889(5) 0.047(2) 1.000 . Uani d ? 
O(2) 1.1040(2) 0.1801(2) -0.0205(5) 0.065(2) 1.000 . Uani d ? 
O(3) 0.9679(2) 0.1394(2) -0.0359(5) 0.053(2) 1.000 . Uani d ? 
O(4) 0.9245(3) 0.0177(2) -0.0229(6) 0.074(3) 1.000 . Uani d ? 
O(5) 0.9441(2) 0.0724(2) 0.0971(5) 0.058(2) 1.000 . Uani d ? 
N(1) 1.0049(3) 0.1085(2) -0.0452(6) 0.047(2) 1.000 . Uani d ? 
C(1) 1.0675(3) 0.1607(3) -0.0015(8) 0.049(3) 1.000 . Uani d ? 
C(2) 1.0490(3) 0.1269(4) -0.0867(7) 0.048(2) 1.000 . Uani d ? 
C(3) 0.9895(4) 0.0634(3) -0.0775(8) 0.059(3) 1.000 . Uani d ? 
C(4) 0.9491(4) 0.0490(3) 0.0022(9) 0.055(3) 1.000 . Uani d ? 
C(5) 1.0457(4) 0.1478(4) -0.2083(9) 0.081(5) 1.000 . Uani d ? 
C(6) 1.0208(5) 0.1907(5) -0.220(1) 0.117(6) 1.000 . Uani d ? 
C(7) 0.9773(6) 0.0571(5) -0.205(1) 0.113(6) 1.000 . Uani d ? 
C(8) 0.9369(6) 0.0829(7) -0.249(1) 0.152(8) 1.000 . Uani d ? 
H(2) 1.0714 0.1036 -0.0904 0.058 1.000 . Uiso c ? 
H(3) 1.0154 0.0444 -0.0617 0.071 1.000 . Uiso c ? 
H(5a) 1.0298 0.1272 -0.2563 0.098 1.000 . Uiso c ? 
H(5b) 1.0772 0.1519 -0.2351 0.098 1.000 . Uiso c ? 
H(6b) 1.0221 0.2004 -0.2972 0.141 1.000 . Uiso c ? 
H(6c) 0.9887 0.1874 -0.1970 0.141 1.000 . Uiso c ? 
H(6a) 1.0357 0.2121 -0.1717 0.141 1.000 . Uiso c ? 
H(7b) 0.9703 0.0267 -0.2160 0.136 1.000 . Uiso c ? 
H(7a) 1.0045 0.0648 -0.2482 0.136 1.000 . Uiso c ? 
H(8a) 0.9433 0.1136 -0.2412 0.183 1.000 . Uiso c ? 
H(8b) 0.9320 0.0762 -0.3279 0.183 1.000 . Uiso c ? 
H(8c) 0.9090 0.0758 -0.2068 0.183 1.000 . Uiso c ? 
C(9) 0.899(1) -0.023(1) 0.296(3) 0.19(2) 0.500 . Uani d ? 
C(10) 0.880(2) 0.031(1) 0.324(3) 0.16(2) 0.500 . Uani 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_12 
_atom_site_aniso_U_13 
_atom_site_aniso_U_23 
Mo(1) 0.0484(5) 0.0395(4) 0.0412(5) 0.0000 0.0000 -0.0041(7) 
Na(1) 0.068(3) 0.048(3) 0.052(3) 0.0000 -0.010(3) 0.0000 
O(1) 0.053(4) 0.045(3) 0.043(4) -0.008(3) 0.003(3) -0.008(3) 
O(2) 0.067(5) 0.078(5) 0.052(4) -0.027(4) 0.002(4) -0.006(4) 
O(3) 0.058(4) 0.061(5) 0.040(4) 0.011(4) -0.006(3) -0.001(3) 
O(4) 0.088(6) 0.065(5) 0.069(5) -0.030(4) -0.020(4) -0.008(4) 
O(5) 0.062(4) 0.057(4) 0.054(5) -0.009(3) 0.002(3) -0.004(3) 
N(1) 0.058(5) 0.047(4) 0.038(4) -0.004(4) 0.001(4) -0.007(4) 
C(1) 0.042(5) 0.058(6) 0.047(6) -0.009(5) -0.003(5) 0.005(5) 
C(2) 0.049(5) 0.052(5) 0.044(5) -0.009(6) 0.003(4) -0.003(5) 
C(3) 0.068(7) 0.051(6) 0.058(6) -0.014(6) 0.006(6) -0.026(5) 
C(4) 0.066(7) 0.050(6) 0.050(6) -0.008(5) -0.016(6) -0.006(5) 
C(5) 0.093(10) 0.11(1) 0.043(7) -0.031(8) -0.004(7) -0.006(7) 
C(6) 0.13(1) 0.13(1) 0.09(1) -0.01(1) -0.022(10) 0.053(10) 
C(7) 0.15(1) 0.13(1) 0.055(9) -0.08(1) 0.021(9) -0.041(8) 
C(8) 0.15(2) 0.22(2) 0.08(1) -0.09(1) -0.06(1) 0.04(1) 
C(9) 0.14(3) 0.19(3) 0.23(4) -0.06(2) -0.16(3) 0.03(3) 
C(10) 0.08(2) 0.23(3) 0.16(4) -0.07(3) 0.00(3) 0.05(3) 
#---------------------------------------------------------------------------
#-- 
_refine_special_details 
; 
? 
; 
_refine_ls_structure_factor_coef F 
_refine_ls_matrix_type full 
_refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]' 
_refine_ls_hydrogen_treatment noref 
_refine_ls_extinction_method none 
_refine_ls_extinction_coef ? 
_refine_ls_abs_structure_details ? 
_refine_ls_abs_structure_Flack ? 
_refine_ls_number_reflns 1583 
_refine_ls_number_parameters 155 
_refine_ls_number_restraints 0 
_refine_ls_number_constraints 0 
_refine_ls_R_factor_all 0.1355 
_refine_ls_R_factor_obs 0.0638 
_refine_ls_wR_factor_all 0.0589 
_refine_ls_wR_factor_obs 0.0532 
_refine_ls_goodness_of_fit_all 1.644 
_refine_ls_goodness_of_fit_obs 1.944 
_refine_ls_shift/esd_max 0.0000 
_refine_ls_shift/esd_mean 0.0000 
_refine_diff_density_min -0.64 
_refine_diff_density_max 0.54 
#---------------------------------------------------------------------------
#-- 
_geom_special_details 
; 
? 
; 
loop_ 
_geom_bond_atom_site_label_1 
_geom_bond_atom_site_label_2 
_geom_bond_distance 
_geom_bond_site_symmetry_1 
_geom_bond_site_symmetry_2 
_geom_bond_publ_flag 
Mo(1) O(1) 2.053(6) . . yes 
Mo(1) O(1) 2.053(6) . 2 yes 
Mo(1) O(3) 2.003(6) . . yes 
Mo(1) O(3) 2.003(6) . 2 yes 
Mo(1) O(5) 2.039(6) . . yes 
Mo(1) O(5) 2.039(6) . 2 yes 
Mo(1) N(1) 2.101(7) . . yes 
Mo(1) N(1) 2.101(7) . 2 yes 
Na(1) O(2) 2.269(7) . 32_445 yes 
Na(1) O(2) 2.269(7) . 14_744 yes 
Na(1) O(4) 2.229(7) . . yes 
Na(1) O(4) 2.229(7) . 19_654 yes 
O(1) C(1) 1.292(10) . . yes 
O(2) C(1) 1.206(9) . . yes 
O(3) N(1) 1.406(7) . . yes 
O(4) C(4) 1.21(1) . . yes 
O(5) C(4) 1.32(1) . . yes 
N(1) C(2) 1.45(1) . . yes 
N(1) C(3) 1.48(1) . . yes 
C(1) C(2) 1.52(1) . . yes 
C(2) C(5) 1.55(1) . . yes 
C(2) H(2) 0.95 . . no 
C(3) C(4) 1.53(1) . . yes 
C(3) C(7) 1.53(1) . . yes 
C(3) H(3) 0.95 . . no 
C(5) C(6) 1.48(2) . . yes 
C(5) H(5a) 0.95 . . no 
C(5) H(5b) 0.95 . . no 
C(6) H(6b) 0.95 . . no 
C(6) H(6c) 0.95 . . no 
C(6) H(6a) 0.95 . . no 
C(7) C(8) 1.48(2) . . yes 
C(7) H(7b) 0.95 . . no 
C(7) H(7a) 0.95 . . no 
C(8) H(8a) 0.95 . . no 
C(8) H(8b) 0.95 . . no 
C(8) H(8c) 0.95 . . no 
C(9) C(10) 1.77(4) . . yes 
C(10) C(10) 1.21(6) . 19_655 yes 
#---------------------------------------------------------------------------
#-- 
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_2 
_geom_angle_site_symmetry_3 
_geom_angle_publ_flag 
O(1) Mo(1) O(1) 83.1(3) . . 2 yes 
O(1) Mo(1) O(3) 83.1(2) . . . yes 
O(1) Mo(1) O(3) 122.5(3) . . 2 yes 
O(1) Mo(1) O(5) 155.7(2) . . . yes 
O(1) Mo(1) O(5) 89.5(2) . . 2 yes 
O(1) Mo(1) N(1) 77.5(2) . . . yes 
O(1) Mo(1) N(1) 82.5(3) . . 2 yes 
O(1) Mo(1) O(3) 122.5(3) 2 . . yes 
O(1) Mo(1) O(3) 83.1(2) 2 . 2 yes 
O(1) Mo(1) O(5) 89.5(2) 2 . . yes 
O(1) Mo(1) O(5) 155.7(2) 2 . 2 yes 
O(1) Mo(1) N(1) 82.5(3) 2 . . yes 
O(1) Mo(1) N(1) 77.5(2) 2 . 2 yes 
O(3) Mo(1) O(3) 147.7(4) . . 2 yes 
O(3) Mo(1) O(5) 81.6(2) . . . yes 
O(3) Mo(1) O(5) 79.1(3) . . 2 yes 
O(3) Mo(1) N(1) 40.0(2) . . . yes 
O(3) Mo(1) N(1) 153.5(2) . . 2 yes 
O(3) Mo(1) O(5) 79.1(3) 2 . . yes 
O(3) Mo(1) O(5) 81.6(2) 2 . 2 yes 
O(3) Mo(1) N(1) 153.5(2) 2 . . yes 
O(3) Mo(1) N(1) 40.0(2) 2 . 2 yes 
O(5) Mo(1) O(5) 105.9(4) . . 2 yes 
O(5) Mo(1) N(1) 78.7(3) . . . yes 
O(5) Mo(1) N(1) 118.4(3) . . 2 yes 
O(5) Mo(1) N(1) 118.4(3) 2 . . yes 
O(5) Mo(1) N(1) 78.7(3) 2 . 2 yes 
N(1) Mo(1) N(1) 153.2(4) . . 2 yes 
O(2) Na(1) O(2) 104.6(4) 32_445 . 14_744 yes 
O(2) Na(1) O(4) 96.5(2) 32_445 . . yes 
O(2) Na(1) O(4) 125.6(3) 32_445 . 19_654 yes 
O(2) Na(1) O(4) 125.6(3) 14_744 . . yes 
O(2) Na(1) O(4) 96.5(2) 14_744 . 19_654 yes 
O(4) Na(1) O(4) 110.8(4) . . 19_654 yes 
Mo(1) O(1) C(1) 118.6(6) . . . yes 
Na(1) O(2) C(1) 112.7(6) 6_755 . . yes 
Mo(1) O(3) N(1) 73.8(4) . . . yes 
Na(1) O(4) C(4) 158.9(7) . . . yes 
Mo(1) O(5) C(4) 119.2(6) . . . yes 
Mo(1) N(1) O(3) 66.3(4) . . . yes 
Mo(1) N(1) C(2) 115.0(5) . . . yes 
Mo(1) N(1) C(3) 112.9(6) . . . yes 
O(3) N(1) C(2) 114.1(7) . . . yes 
O(3) N(1) C(3) 114.5(7) . . . yes 
C(2) N(1) C(3) 121.5(8) . . . yes 
O(1) C(1) O(2) 122.9(9) . . . yes 
O(1) C(1) C(2) 116.9(8) . . . yes 
O(2) C(1) C(2) 120.2(9) . . . yes 
N(1) C(2) C(1) 109.7(7) . . . yes 
N(1) C(2) C(5) 114.2(8) . . . yes 
N(1) C(2) H(2) 107.5 . . . no 
C(1) C(2) C(5) 110.0(9) . . . yes 
C(1) C(2) H(2) 107.6 . . . no 
C(5) C(2) H(2) 107.5 . . . no 
N(1) C(3) C(4) 109.1(8) . . . yes 
N(1) C(3) C(7) 115.2(9) . . . yes 
N(1) C(3) H(3) 106.5 . . . no 
C(4) C(3) C(7) 112.5(10) . . . yes 
C(4) C(3) H(3) 106.5 . . . no 
C(7) C(3) H(3) 106.5 . . . no 
O(4) C(4) O(5) 124(1) . . . yes 
O(4) C(4) C(3) 120.2(10) . . . yes 
O(5) C(4) C(3) 115.8(8) . . . yes 
C(2) C(5) C(6) 117(1) . . . yes 
C(2) C(5) H(5a) 107.3 . . . no 
C(2) C(5) H(5b) 107.3 . . . no 
C(6) C(5) H(5a) 107.3 . . . no 
C(6) C(5) H(5b) 107.5 . . . no 
H(5a) C(5) H(5b) 109.5 . . . no 
C(5) C(6) H(6b) 109.6 . . . no 
C(5) C(6) H(6c) 109.6 . . . no 
C(5) C(6) H(6a) 109.4 . . . no 
H(6b) C(6) H(6c) 109.6 . . . no 
H(6b) C(6) H(6a) 109.3 . . . no 
H(6c) C(6) H(6a) 109.3 . . . no 
C(3) C(7) C(8) 116(1) . . . yes 
C(3) C(7) H(7b) 107.6 . . . no 
C(3) C(7) H(7a) 107.7 . . . no 
C(8) C(7) H(7b) 107.7 . . . no 
C(8) C(7) H(7a) 107.8 . . . no 
H(7b) C(7) H(7a) 109.4 . . . no 
C(7) C(8) H(8a) 109.6 . . . no 
C(7) C(8) H(8b) 109.9 . . . no 
C(7) C(8) H(8c) 109.6 . . . no 
H(8a) C(8) H(8b) 109.3 . . . no 
H(8a) C(8) H(8c) 109.0 . . . no 
H(8b) C(8) H(8c) 109.4 . . . no 
C(9) C(10) C(10) 104(2) . . 19_655 yes 
#---------------------------------------------------------------------------
#-- 
loop_ 
_geom_contact_atom_site_label_1 
_geom_contact_atom_site_label_2 
_geom_contact_distance 
_geom_contact_site_symmetry_1 
_geom_contact_site_symmetry_2 
_geom_contact_publ_flag 
O(1) O(4) 3.558(9) . 6_755 no 
O(2) C(2) 3.33(1) . 4_755 no 
O(2) O(4) 3.356(9) . 8 no 
O(2) C(1) 3.54(1) . 4_755 no 
O(2) O(2) 3.54(1) . 4_755 no 
O(2) O(2) 3.59(1) . 3_755 no 
O(3) C(10) 3.49(3) . 2 no 
O(5) C(10) 3.45(3) . . no 
#---------------------------------------------------------------------------
#-- 
loop_ 
_geom_torsion_atom_site_label_1 
_geom_torsion_atom_site_label_2 
_geom_torsion_atom_site_label_3 
_geom_torsion_atom_site_label_4 
_geom_torsion 
_geom_torsion_site_symmetry_1 
_geom_torsion_site_symmetry_2 
_geom_torsion_site_symmetry_3 
_geom_torsion_site_symmetry_4 
_geom_torsion_publ_flag 
Mo(1) O(1) C(1) O(2) . . . . -169.2(7) no 
Mo(1) O(1) C(1) C(2) . . . . 12(1) no 
Mo(1) O(1) C(1) O(2) . 2 2 2 -169.2(7) no 
Mo(1) O(1) C(1) C(2) . 2 2 2 12(1) no 
Mo(1) O(3) N(1) C(2) . . . . -108.0(7) no 
Mo(1) O(3) N(1) C(3) . . . . 105.5(7) no 
Mo(1) O(3) N(1) C(2) . 2 2 2 -108.0(7) no 
Mo(1) O(3) N(1) C(3) . 2 2 2 105.5(7) no 
Mo(1) O(5) C(4) O(4) . . . . -178.7(8) no 
Mo(1) O(5) C(4) C(3) . . . . 2(1) no 
Mo(1) O(5) C(4) O(4) . 2 2 2 -178.7(8) no 
Mo(1) O(5) C(4) C(3) . 2 2 2 2(1) no 
Mo(1) N(1) C(2) C(1) . . . . -10.2(10) no 
Mo(1) N(1) C(2) C(5) . . . . -134.2(8) no 
Mo(1) N(1) C(3) C(4) . . . . 22(1) no 
Mo(1) N(1) C(3) C(7) . . . . 150.2(10) no 
Mo(1) N(1) C(2) C(1) . 2 2 2 -10.2(10) no 
Mo(1) N(1) C(2) C(5) . 2 2 2 -134.2(8) no 
Mo(1) N(1) C(3) C(4) . 2 2 2 22(1) no 
Mo(1) N(1) C(3) C(7) . 2 2 2 150.2(10) no 
Na(1) O(4) C(4) O(5) . . . . 122(1) no 
Na(1) O(4) C(4) C(3) . . . . -58(2) no 
Na(1) O(4) C(4) O(5) . 19_654 19_654 19_654 122(1) no 
Na(1) O(4) C(4) C(3) . 19_654 19_654 19_654 -58(2) no 
O(1) Mo(1) O(1) C(1) . . 2 2 70.2(6) no 
O(1) Mo(1) O(3) N(1) . . . . 78.7(4) no 
O(1) Mo(1) O(3) N(1) . . 2 2 1.6(4) no 
O(1) Mo(1) O(5) C(4) . . . . -2(1) no 
O(1) Mo(1) O(5) C(4) . . 2 2 -73.9(7) no 
O(1) Mo(1) N(1) O(3) . . . . -94.2(4) no 
O(1) Mo(1) N(1) C(2) . . . . 12.5(6) no 
O(1) Mo(1) N(1) C(3) . . . . 158.0(7) no 
O(1) Mo(1) N(1) O(3) . . 2 2 -178.7(4) no 
O(1) Mo(1) N(1) C(2) . . 2 2 -72.0(7) no 
O(1) Mo(1) N(1) C(3) . . 2 2 73.5(7) no 
O(1) C(1) C(2) N(1) . . . . 0(1) no 
O(1) C(1) C(2) C(5) . . . . 125.6(9) no 
O(2) Na(1) O(2) C(1) . 6_755 3_755 3_755 69.8(7) no 
O(2) C(1) C(2) N(1) . . . . -179.6(9) no 
O(2) C(1) C(2) C(5) . . . . -53(1) no 
O(3) Mo(1) O(1) C(1) . . . . -53.9(6) no 
O(3) Mo(1) O(1) C(1) . . 2 2 147.4(6) no 
O(3) Mo(1) O(3) N(1) . . 2 2 -136.1(3) no 
O(3) Mo(1) O(5) C(4) . . . . 49.1(7) no 
O(3) Mo(1) O(5) C(4) . . 2 2 -156.9(7) no 
O(3) Mo(1) N(1) C(2) . . . . 106.7(7) no 
O(3) Mo(1) N(1) C(3) . . . . -107.8(8) no 
O(3) Mo(1) N(1) C(2) . . 2 2 -129.5(7) no 
O(3) Mo(1) N(1) C(3) . . 2 2 15(1) no 
O(3) N(1) Mo(1) O(5) . . . . 90.4(4) no 
O(3) N(1) Mo(1) O(5) . . . 2 -11.7(4) no 
O(3) N(1) Mo(1) N(1) . . . 2 -136.8(3) no 
O(3) N(1) C(2) C(1) . . . . 63.7(10) no 
O(3) N(1) C(2) C(5) . . . . -60(1) no 
O(3) N(1) C(3) C(4) . . . . -50(1) no 
O(3) N(1) C(3) C(7) . . . . 76(1) no 
O(4) Na(1) O(4) C(4) . . 19_654 19_654 -31(2) no 
O(4) C(4) C(3) N(1) . . . . 164.4(9) no 
O(4) C(4) C(3) C(7) . . . . 35(1) no 
O(5) Mo(1) O(1) C(1) . . . . -2.8(10) no 
O(5) Mo(1) O(1) C(1) . . 2 2 -133.0(6) no 
O(5) Mo(1) O(3) N(1) . . . . -82.4(4) no 
O(5) Mo(1) O(3) N(1) . . 2 2 169.5(4) no 
O(5) Mo(1) O(5) C(4) . . 2 2 125.2(7) no 
O(5) Mo(1) N(1) C(2) . . . . -162.9(7) no 
O(5) Mo(1) N(1) C(3) . . . . -17.4(7) no 
O(5) Mo(1) N(1) C(2) . . 2 2 95.0(7) no 
O(5) Mo(1) N(1) C(3) . . 2 2 -119.5(7) no 
O(5) C(4) C(3) N(1) . . . . -16(1) no 
O(5) C(4) C(3) C(7) . . . . -145(1) no 
N(1) Mo(1) O(1) C(1) . . . . -13.7(6) no 
N(1) Mo(1) O(1) C(1) . . 2 2 148.4(7) no 
N(1) Mo(1) O(5) C(4) . . . . 8.6(7) no 
N(1) Mo(1) O(5) C(4) . . 2 2 -149.3(7) no 
N(1) Mo(1) N(1) C(2) . . 2 2 -30.1(6) no 
N(1) Mo(1) N(1) C(3) . . 2 2 115.4(7) no 
N(1) C(2) C(5) C(6) . . . . 73(1) no 
N(1) C(3) C(7) C(8) . . . . -63(1) no 
C(1) C(2) N(1) C(3) . . . . -152.4(9) no 
C(1) C(2) C(5) C(6) . . . . -50(1) no 
C(2) N(1) C(3) C(4) . . . . 165.6(8) no 
C(2) N(1) C(3) C(7) . . . . -66(1) no 
C(3) N(1) C(2) C(5) . . . . 83(1) no 
C(4) C(3) C(7) C(8) . . . . 62(1) no 
C(9) C(10) C(10) C(9) . . 19_655 19_655 -30(5)
no#-------------------------------------------------------------------------
#---- 
#===END

data_manmo1

_database_code_CSD	168521


_audit_creation_method SHELXL
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_formula_moiety ?
_chemical_formula_structural ?
_chemical_formula_analytical ?
_chemical_formula_sum 'C12 H21 Mo N2 O12'
_chemical_formula_weight 481.25
_chemical_melting_point ?
_chemical_compound_source ?

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'

_symmetry_cell_setting orthorombic
_symmetry_space_group_name_H-M 'P2(1)2(1)2'

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

_cell_length_a 10.3610(10)
_cell_length_b 13.9210(10)
_cell_length_c 6.8470(10)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 987.6(2)
_cell_formula_units_Z 2
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used ?
_cell_measurement_theta_min ?
_cell_measurement_theta_max ?

_exptl_crystal_description ?
_exptl_crystal_colour ?
_exptl_crystal_size_max ?
_exptl_crystal_size_mid ?
_exptl_crystal_size_min ?
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.618
_exptl_crystal_density_method ?
_exptl_crystal_F_000 490
_exptl_absorpt_coefficient_mu 0.725
_exptl_absorpt_correction_type ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_T_max ?

_exptl_special_details
;
?
;

_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 ?
_diffrn_measurement_method ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 1674
_diffrn_reflns_av_R_equivalents 0.0000
_diffrn_reflns_av_sigmaI/netI 0.0190
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_limit_l_max 9
_diffrn_reflns_theta_min 2.93
_diffrn_reflns_theta_max 29.98
_reflns_number_total 1674
_reflns_number_observed 1605
_reflns_observed_criterion 2sigma(I)

_computing_data_collection ?
_computing_cell_refinement ?
_computing_data_reduction ?
_computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics ?
_computing_publication_material ?

_refine_special_details
;
Refinement on F^2^ for ALL reflections except for 0 with very negative
F^2^
or flagged by the user for potential systematic errors. Weighted
R-factors
wR and all goodnesses 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 observed
criterion
of F^2^ 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0476P)^2^+0.2832P] 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 ?
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack -0.02(6)
_refine_ls_number_reflns 1674
_refine_ls_number_parameters 125
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0297
_refine_ls_R_factor_obs 0.0279
_refine_ls_wR_factor_all 0.0760
_refine_ls_wR_factor_obs 0.0749
_refine_ls_goodness_of_fit_all 1.098
_refine_ls_goodness_of_fit_obs 1.106
_refine_ls_restrained_S_all 1.098
_refine_ls_restrained_S_obs 1.106
_refine_ls_shift/esd_max 0.000
_refine_ls_shift/esd_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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Mo1 Mo 0.0000 0.0000 0.11587(4) 0.02303(10) Uani 1 d S .
O1 O 0.1364(2) -0.01984(13) 0.3317(3) 0.0311(5) Uani 1 d . .
O2 O 0.2328(2) -0.1243(2) 0.5270(4) 0.0463(6) Uani 1 d . .
O3 O -0.1524(2) -0.0386(2) -0.0613(4) 0.0340(5) Uani 1 d . .
O4 O -0.2992(2) -0.1483(2) -0.1302(5) 0.0492(7) Uani 1 d . .
O5 O 0.0618(2) -0.13008(14) 0.0335(3) 0.0293(4) Uani 1 d . .
N1 N -0.0249(2) -0.1433(2) 0.1868(4) 0.0250(5) Uani 1 d . .
C1 C 0.0430(3) -0.1778(2) 0.3644(5) 0.0309(6) Uani 1 d . .
H1 H 0.0844(3) -0.2396(2) 0.3362(5) 0.037 Uiso 1 calc R .
C2 C 0.1466(3) -0.1036(2) 0.4114(5) 0.0315(6) Uani 1 d . .
C3 C -0.0468(4) -0.1895(3) 0.5375(5) 0.0469(8) Uani 1 d . .
H3A H -0.1043(22) -0.2423(16) 0.5141(23) 0.070 Uiso 1 calc R .
H3B H -0.0960(24) -0.1317(9) 0.5549(31) 0.070 Uiso 1 calc R .
H3C H 0.0030(4) -0.2019(24) 0.6530(11) 0.070 Uiso 1 calc R .
C4 C -0.1483(3) -0.1879(2) 0.1210(5) 0.0313(6) Uani 1 d . .
H4 H -0.2079(3) -0.1885(2) 0.2321(5) 0.038 Uiso 1 calc R .
C5 C -0.2048(3) -0.1217(2) -0.0361(5) 0.0334(6) Uani 1 d . .
C6 C -0.1298(3) -0.2905(2) 0.0532(6) 0.0403(7) Uani 1 d . .
H6A H -0.0968(27) -0.3284(5) 0.1591(14) 0.060 Uiso 1 calc R .
H6B H -0.0697(23) -0.2918(3) -0.0535(30) 0.060 Uiso 1 calc R .
H6C H -0.2111(7) -0.3163(7) 0.0111(41) 0.060 Uiso 1 calc R .
O6 O -0.3877(2) -0.0237(2) 0.6118(4) 0.0542(7) Uani 1 d . .
H6WA H -0.3385(2) 0.0267(2) 0.5952(4) 0.081 Uiso 1 d R .
H6WB H -0.3579(2) -0.0684(2) 0.6973(4) 0.081 Uiso 1 d R .
H6WC H -0.4741(2) -0.0119(2) 0.5953(4) 0.081 Uiso 0.50 d PR .

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 0.01861(14) 0.02289(14) 0.02760(15) 0.000 0.000 -0.00147(11)
O1 0.0260(9) 0.0273(10) 0.0401(10) 0.0004(8) -0.0100(9) 0.0000(7)
O2 0.0409(13) 0.0419(12) 0.056(2) 0.0067(12) -0.0216(12) 0.0022(11)
O3 0.0290(10) 0.0329(9) 0.0402(11) 0.0005(9) -0.0107(10) -0.0063(9)
O4 0.0380(12) 0.0426(12) 0.067(2) 0.0024(13) -0.0222(13) -0.0117(10)
O5 0.0253(9) 0.0263(9) 0.0363(10) -0.0029(8) 0.0080(9) -0.0016(8)
N1 0.0202(11) 0.0234(9) 0.0315(10) -0.0011(8) 0.0021(8) -0.0015(8)
C1 0.0315(12) 0.0251(11) 0.0362(14) 0.0007(11) -0.0045(11) 0.0005(10)
C2 0.0287(13) 0.0295(12) 0.0362(14) -0.0020(11) -0.0053(12) 0.0048(11)
C3 0.053(2) 0.052(2) 0.036(2) 0.008(2) 0.0016(15) -0.012(2)
C4 0.0252(12) 0.0313(12) 0.0373(14) -0.0001(12) -0.0007(12) -0.0068(10)

C5 0.0255(12) 0.0356(14) 0.0390(15) -0.0022(13) -0.0044(12) -0.0032(11)

C6 0.041(2) 0.0314(13) 0.048(2) -0.0010(14) -0.005(2) -0.0088(13)
O6 0.0341(12) 0.0546(15) 0.074(2) 0.0149(13) -0.0042(13) -0.0010(11)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 O5 2.002(2) . ?
Mo1 O5 2.002(2) 2 ?
Mo1 O3 2.062(2) 2 ?
Mo1 O3 2.062(2) . ?
Mo1 O1 2.064(2) . ?
Mo1 O1 2.064(2) 2 ?
Mo1 N1 2.070(2) 2 ?
Mo1 N1 2.070(2) . ?
O1 C2 1.291(3) . ?
O2 C2 1.228(4) . ?
O3 C5 1.290(4) . ?
O4 C5 1.229(4) . ?
O5 N1 1.394(3) . ?
N1 C1 1.485(4) . ?
N1 C4 1.491(3) . ?
C1 C3 1.515(5) . ?
C1 C2 1.524(4) . ?
C4 C6 1.514(4) . ?
C4 C5 1.532(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Mo1 O5 147.26(13) . 2 ?
O5 Mo1 O3 79.94(9) . 2 ?
O5 Mo1 O3 80.97(9) 2 2 ?
O5 Mo1 O3 80.97(9) . . ?
O5 Mo1 O3 79.94(9) 2 . ?
O3 Mo1 O3 107.93(14) 2 . ?
O5 Mo1 O1 82.06(8) . . ?
O5 Mo1 O1 122.81(8) 2 . ?
O3 Mo1 O1 86.09(10) 2 . ?
O3 Mo1 O1 155.61(8) . . ?
O5 Mo1 O1 122.81(8) . 2 ?
O5 Mo1 O1 82.06(8) 2 2 ?
O3 Mo1 O1 155.61(8) 2 2 ?
O3 Mo1 O1 86.09(10) . 2 ?
O1 Mo1 O1 88.53(13) . 2 ?
O5 Mo1 N1 153.96(8) . 2 ?
O5 Mo1 N1 39.99(9) 2 2 ?
O3 Mo1 N1 77.96(9) 2 2 ?
O3 Mo1 N1 118.99(9) . 2 ?
O1 Mo1 N1 82.86(8) . 2 ?
O1 Mo1 N1 77.77(8) 2 2 ?
O5 Mo1 N1 39.99(9) . . ?
O5 Mo1 N1 153.96(8) 2 . ?
O3 Mo1 N1 118.99(9) 2 . ?
O3 Mo1 N1 77.96(9) . . ?
O1 Mo1 N1 77.77(8) . . ?
O1 Mo1 N1 82.86(8) 2 . ?
N1 Mo1 N1 152.85(14) 2 . ?
C2 O1 Mo1 118.6(2) . . ?
C5 O3 Mo1 118.5(2) . . ?
N1 O5 Mo1 72.63(12) . . ?
O5 N1 C1 110.8(2) . . ?
O5 N1 C4 112.3(2) . . ?
C1 N1 C4 121.3(2) . . ?
O5 N1 Mo1 67.38(11) . . ?
C1 N1 Mo1 116.4(2) . . ?
C4 N1 Mo1 115.9(2) . . ?
N1 C1 C3 112.6(3) . . ?
N1 C1 C2 106.7(2) . . ?
C3 C1 C2 109.9(3) . . ?
O2 C2 O1 122.9(3) . . ?
O2 C2 C1 119.3(3) . . ?
O1 C2 C1 117.8(3) . . ?
N1 C4 C6 112.1(2) . . ?
N1 C4 C5 106.9(2) . . ?
C6 C4 C5 113.6(3) . . ?
O4 C5 O3 122.4(3) . . ?
O4 C5 C4 119.4(3) . . ?
O3 C5 C4 118.2(3) . . ?

_refine_diff_density_max 1.255
_refine_diff_density_min -1.135
_refine_diff_density_rms 0.083
#===END