# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2010


data_global

_journal_name_full               'Dalton Trans.'
_journal_coden_cambridge         0222
_journal_page_first              ?
_journal_page_last               ?
_journal_volume                  ?
_journal_year                    ?
loop_
_publ_author_name
W.Darwish
E.Seikel
K.Harms
O.Burghaus
J.Sundermeyer
_publ_contact_author_name        'Sundermeyer, Jorg'
_publ_contact_author_email       jsu@staff.uni-marburg.de

#data_63
data_1
_database_code_depnum_ccdc_archive 'CCDC 792993'

_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;

;

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         'C36 H25 Cl Mo N9, 7(H2 O)'

_chemical_formula_sum            'C36 H39 Cl Mo N9 O7'

_chemical_formula_weight         841.15

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           tetragonal

_symmetry_space_group_name_H-M   'P 4/n'

loop_

_symmetry_equiv_pos_as_xyz

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

_cell_length_a                   13.8148(12)

_cell_length_b                   13.8148(12)

_cell_length_c                   10.0926(9)

_cell_angle_alpha                90.00

_cell_angle_beta                 90.00

_cell_angle_gamma                90.00

_cell_volume                     1926.2(3)

_cell_formula_units_Z            2

_cell_measurement_temperature    100(2)

_cell_measurement_reflns_used    8979

_cell_measurement_theta_min      1.47

_cell_measurement_theta_max      25.96

_exptl_crystal_description       plate

_exptl_crystal_colour            'dark green'

_exptl_crystal_size_max          0.18

_exptl_crystal_size_mid          0.15

_exptl_crystal_size_min          0.01

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.450

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             866

_exptl_absorpt_coefficient_mu    0.469

_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.9432

_exptl_absorpt_correction_T_max  0.9836

_exptl_absorpt_process_details   
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]

;

_exptl_special_details           
;
Crystallographic 4-fold disorder of the N-tbutyl ligand.
Heavy disordered solvent has been refined as water.
;

_diffrn_ambient_temperature      100(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 IPDS2'

_diffrn_measurement_method       ?

_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         ?

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  ?

_diffrn_standards_decay_%        ?

_diffrn_reflns_number            12104

_diffrn_reflns_av_R_equivalents  0.0865

_diffrn_reflns_av_sigmaI/netI    0.0492

_diffrn_reflns_limit_h_min       -16

_diffrn_reflns_limit_h_max       16

_diffrn_reflns_limit_k_min       -16

_diffrn_reflns_limit_k_max       16

_diffrn_reflns_limit_l_min       -11

_diffrn_reflns_limit_l_max       11

_diffrn_reflns_theta_min         2.08

_diffrn_reflns_theta_max         24.99

_reflns_number_total             1702

_reflns_number_gt                1424

_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'STOE X-AREA'

_computing_cell_refinement       'STOE X-AREA'

_computing_data_reduction        'STOE X-AREA'

_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'

_computing_molecular_graphics    'DIAMOND 3.2 (Crystal Impact)'

_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_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^ > 2\s(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^)+(0.0387P)^2^+1.4570P] 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    noref

_refine_ls_extinction_method     none

_refine_ls_extinction_coef       ?

_refine_ls_number_reflns         1702

_refine_ls_number_parameters     151

_refine_ls_number_restraints     26

_refine_ls_R_factor_all          0.0672

_refine_ls_R_factor_gt           0.0497

_refine_ls_wR_factor_ref         0.0978

_refine_ls_wR_factor_gt          0.0930

_refine_ls_goodness_of_fit_ref   1.100

_refine_ls_restrained_S_all      1.099

_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

Mo1 Mo 0.2500 0.2500 0.77005(7) 0.0299(2) Uani 1 4 d S . .
Cl1 Cl 0.2500 0.2500 1.0276(2) 0.0399(5) Uani 1 4 d S . .
N1 N 0.3161(2) 0.3813(2) 0.8003(3) 0.0360(8) Uani 1 1 d . . .
C2 C 0.4148(3) 0.3954(3) 0.8104(4) 0.0359(9) Uani 1 1 d . . .
C3 C 0.4321(3) 0.4992(3) 0.8256(4) 0.0370(9) Uani 1 1 d . . .
C4 C 0.5164(3) 0.5534(3) 0.8403(4) 0.0441(10) Uani 1 1 d . . .
H4 H 0.5783 0.5234 0.8400 0.053 Uiso 1 1 calc R . .
C5 C 0.5066(3) 0.6529(3) 0.8556(4) 0.0472(11) Uani 1 1 d . . .
H5 H 0.5630 0.6916 0.8667 0.057 Uiso 1 1 calc R . .
C6 C 0.4157(3) 0.6974(3) 0.8548(5) 0.0501(12) Uani 1 1 d . . .
H6 H 0.4115 0.7657 0.8638 0.060 Uiso 1 1 calc R . .
C7 C 0.3317(3) 0.6437(3) 0.8414(5) 0.0456(10) Uani 1 1 d . . .
H7 H 0.2700 0.6739 0.8425 0.055 Uiso 1 1 calc R . .
C8 C 0.3407(3) 0.5438(3) 0.8260(4) 0.0369(9) Uani 1 1 d . . .
C9 C 0.2685(3) 0.4683(3) 0.8110(4) 0.0362(9) Uani 1 1 d . . .
N10 N 0.4836(2) 0.3273(2) 0.8133(3) 0.0375(8) Uani 1 1 d . . .
N11 N 0.2500 0.2500 0.6013(7) 0.0422(15) Uani 1 4 d S . .
C10 C 0.245(2) 0.2201(12) 0.4664(14) 0.089(11) Uani 0.25 1 d PG A -1
C11 C 0.187(2) 0.2918(18) 0.380(5) 0.131(15) Uiso 0.25 1 d PG A -1
H20D H 0.2141 0.3571 0.3913 0.196 Uiso 0.25 1 calc PR A -1
H20E H 0.1193 0.2916 0.4081 0.196 Uiso 0.25 1 calc PR A -1
H20F H 0.1919 0.2726 0.2872 0.196 Uiso 0.25 1 calc PR A -1
C12 C 0.3470(15) 0.215(2) 0.405(4) 0.091(9) Uiso 0.25 1 d PG A -1
H20A H 0.3868 0.1695 0.4570 0.137 Uiso 0.25 1 calc PR A -1
H20B H 0.3768 0.2789 0.4068 0.137 Uiso 0.25 1 calc PR A -1
H20C H 0.3423 0.1917 0.3138 0.137 Uiso 0.25 1 calc PR A -1
C13 C 0.1986(13) 0.1203(13) 0.444(3) 0.065(6) Uiso 0.25 1 d PG A -1
H20G H 0.2328 0.0715 0.4965 0.097 Uiso 0.25 1 calc PR A -1
H20H H 0.2030 0.1033 0.3496 0.097 Uiso 0.25 1 calc PR A -1
H20I H 0.1304 0.1223 0.4704 0.097 Uiso 0.25 1 calc PR A -1
O1 O 0.293(4) 0.755(9) 0.497(9) 0.19(3) Uani 0.25 1 d PDU B -2
O2 O 0.156(5) 0.638(6) 0.511(3) 0.30(2) Uani 0.50 1 d PDU C -3
O3 O 0.112(4) 0.755(6) 0.497(3) 0.27(2) Uani 0.50 1 d PDU D -4
O4 O 0.121(2) 0.947(2) 0.4799(16) 0.242(11) Uani 0.50 1 d PU E -5

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 0.0266(2) 0.0266(2) 0.0366(4) 0.000 0.000 0.000
Cl1 0.0381(7) 0.0381(7) 0.0436(13) 0.000 0.000 0.000
N1 0.0298(16) 0.0336(16) 0.044(2) 0.0022(14) 0.0006(13) 0.0001(12)
C2 0.0313(18) 0.0338(19) 0.043(3) 0.0031(16) 0.0016(16) -0.0033(14)
C3 0.034(2) 0.0317(19) 0.046(2) 0.0034(17) 0.0008(17) -0.0033(15)
C4 0.036(2) 0.044(2) 0.052(3) 0.0029(19) 0.0003(18) -0.0044(18)
C5 0.049(2) 0.039(2) 0.054(3) -0.0004(18) 0.0009(19) -0.0144(19)
C6 0.052(3) 0.031(2) 0.067(4) -0.0026(19) 0.004(2) -0.0070(18)
C7 0.045(2) 0.031(2) 0.061(3) 0.0008(18) 0.004(2) -0.0027(17)
C8 0.036(2) 0.0287(18) 0.046(2) 0.0019(16) -0.0006(17) -0.0035(15)
C9 0.0361(19) 0.0272(18) 0.045(3) 0.0024(15) 0.0000(16) 0.0011(14)
N10 0.0296(16) 0.0327(16) 0.050(2) 0.0010(14) 0.0035(14) 0.0000(12)
N11 0.049(2) 0.049(2) 0.028(4) 0.000 0.000 0.000
C10 0.14(3) 0.048(13) 0.080(14) -0.041(12) 0.07(3) -0.039(15)
O1 0.27(7) 0.23(4) 0.079(18) 0.01(2) 0.05(5) -0.04(7)
O2 0.35(5) 0.47(8) 0.098(18) 0.02(2) -0.05(3) -0.06(6)
O3 0.43(5) 0.33(5) 0.047(10) -0.025(19) 0.00(2) -0.05(5)
O4 0.31(3) 0.37(3) 0.047(8) -0.027(15) 0.007(11) 0.04(3)

_geom_special_details            
;

All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)

are estimated using the full covariance matrix. The cell s.u.'s are taken

into account individually in the estimation of s.u.'s in distances, angles

and torsion angles; correlations between s.u.'s in cell parameters are only

used when they are defined by crystal symmetry. An approximate (isotropic)

treatment of cell s.u.'s is used for estimating s.u.'s 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 N11 1.704(7) . ?
Mo1 N1 2.054(3) . ?
Mo1 N1 2.054(3) 3 ?
Mo1 N1 2.054(3) 2 ?
Mo1 N1 2.054(3) 4 ?
Mo1 Cl1 2.600(2) . ?
N1 C9 1.374(5) . ?
N1 C2 1.381(5) . ?
C2 N10 1.338(5) . ?
C2 C3 1.463(5) . ?
C3 C4 1.392(5) . ?
C3 C8 1.406(5) . ?
C4 C5 1.390(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.398(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.384(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.394(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.451(5) . ?
C9 N10 1.340(5) 3 ?
N10 C9 1.340(5) 4 ?
N11 C10 1.424(15) 4 ?
N11 C10 1.424(15) . ?
N11 C10 1.424(15) 3 ?
N11 C10 1.424(15) 2 ?
C10 C13 1.5389 . ?
C10 C12 1.5392 . ?
C10 C11 1.5396 . ?
C11 H20D 0.9800 . ?
C11 H20E 0.9800 . ?
C11 H20F 0.9800 . ?
C12 H20A 0.9800 . ?
C12 H20B 0.9800 . ?
C12 H20C 0.9800 . ?
C13 H20G 0.9800 . ?
C13 H20H 0.9800 . ?
C13 H20I 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

N11 Mo1 N1 98.55(9) . . ?
N11 Mo1 N1 98.55(9) . 3 ?
N1 Mo1 N1 88.73(3) . 3 ?
N11 Mo1 N1 98.55(9) . 2 ?
N1 Mo1 N1 162.90(19) . 2 ?
N1 Mo1 N1 88.73(3) 3 2 ?
N11 Mo1 N1 98.55(9) . 4 ?
N1 Mo1 N1 88.73(3) . 4 ?
N1 Mo1 N1 162.90(19) 3 4 ?
N1 Mo1 N1 88.73(3) 2 4 ?
N11 Mo1 Cl1 180.000(1) . . ?
N1 Mo1 Cl1 81.45(9) . . ?
N1 Mo1 Cl1 81.45(9) 3 . ?
N1 Mo1 Cl1 81.45(9) 2 . ?
N1 Mo1 Cl1 81.45(9) 4 . ?
C9 N1 C2 110.1(3) . . ?
C9 N1 Mo1 124.9(2) . . ?
C2 N1 Mo1 125.0(2) . . ?
N10 C2 N1 127.2(3) . . ?
N10 C2 C3 124.8(3) . . ?
N1 C2 C3 107.9(3) . . ?
C4 C3 C8 121.1(4) . . ?
C4 C3 C2 132.5(4) . . ?
C8 C3 C2 106.4(3) . . ?
C5 C4 C3 117.5(4) . . ?
C5 C4 H4 121.2 . . ?
C3 C4 H4 121.2 . . ?
C4 C5 C6 121.4(4) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C7 C6 C5 121.2(4) . . ?
C7 C6 H6 119.4 . . ?
C5 C6 H6 119.4 . . ?
C6 C7 C8 117.9(4) . . ?
C6 C7 H7 121.1 . . ?
C8 C7 H7 121.1 . . ?
C7 C8 C3 120.9(4) . . ?
C7 C8 C9 131.5(4) . . ?
C3 C8 C9 107.6(3) . . ?
N10 C9 N1 127.7(3) 3 . ?
N10 C9 C8 124.3(3) 3 . ?
N1 C9 C8 108.0(3) . . ?
C2 N10 C9 125.6(3) . 4 ?
C10 N11 Mo1 162.9(7) 4 . ?
C10 N11 Mo1 162.9(7) . . ?
C10 N11 Mo1 162.9(7) 3 . ?
C10 N11 Mo1 162.9(7) 2 . ?
N11 C10 C13 115.0(13) . . ?
N11 C10 C12 111(3) . . ?
C13 C10 C12 106.1 . . ?
N11 C10 C11 112(2) . . ?
C13 C10 C11 106.1 . . ?
C12 C10 C11 106.3 . . ?
C10 C11 H20D 109.5 . . ?
C10 C11 H20E 109.5 . . ?
H20D C11 H20E 109.5 . . ?
C10 C11 H20F 109.5 . . ?
H20D C11 H20F 109.5 . . ?
H20E C11 H20F 109.5 . . ?
C10 C12 H20A 109.5 . . ?
C10 C12 H20B 109.5 . . ?
H20A C12 H20B 109.5 . . ?
C10 C12 H20C 109.5 . . ?
H20A C12 H20C 109.5 . . ?
H20B C12 H20C 109.5 . . ?
C10 C13 H20G 109.5 . . ?
C10 C13 H20H 109.5 . . ?
H20G C13 H20H 109.5 . . ?
C10 C13 H20I 109.5 . . ?
H20G C13 H20I 109.5 . . ?
H20H C13 H20I 109.5 . . ?

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

N11 Mo1 N1 C9 89.5(3) . . . . ?
N1 Mo1 N1 C9 -8.9(4) 3 . . . ?
N1 Mo1 N1 C9 -90.5(3) 2 . . . ?
N1 Mo1 N1 C9 -172.0(2) 4 . . . ?
Cl1 Mo1 N1 C9 -90.5(3) . . . . ?
N11 Mo1 N1 C2 -89.2(3) . . . . ?
N1 Mo1 N1 C2 172.4(2) 3 . . . ?
N1 Mo1 N1 C2 90.8(3) 2 . . . ?
N1 Mo1 N1 C2 9.3(4) 4 . . . ?
Cl1 Mo1 N1 C2 90.8(3) . . . . ?
C9 N1 C2 N10 175.3(4) . . . . ?
Mo1 N1 C2 N10 -5.8(6) . . . . ?
C9 N1 C2 C3 -1.4(4) . . . . ?
Mo1 N1 C2 C3 177.5(3) . . . . ?
N10 C2 C3 C4 2.9(7) . . . . ?
N1 C2 C3 C4 179.7(4) . . . . ?
N10 C2 C3 C8 -175.9(4) . . . . ?
N1 C2 C3 C8 0.9(4) . . . . ?
C8 C3 C4 C5 0.1(6) . . . . ?
C2 C3 C4 C5 -178.5(4) . . . . ?
C3 C4 C5 C6 -0.6(7) . . . . ?
C4 C5 C6 C7 1.2(7) . . . . ?
C5 C6 C7 C8 -1.2(7) . . . . ?
C6 C7 C8 C3 0.6(7) . . . . ?
C6 C7 C8 C9 179.3(4) . . . . ?
C4 C3 C8 C7 -0.1(7) . . . . ?
C2 C3 C8 C7 178.9(4) . . . . ?
C4 C3 C8 C9 -179.1(4) . . . . ?
C2 C3 C8 C9 -0.2(5) . . . . ?
C2 N1 C9 N10 -176.0(4) . . . 3 ?
Mo1 N1 C9 N10 5.1(6) . . . 3 ?
C2 N1 C9 C8 1.3(4) . . . . ?
Mo1 N1 C9 C8 -177.6(3) . . . . ?
C7 C8 C9 N10 -2.1(7) . . . 3 ?
C3 C8 C9 N10 176.8(4) . . . 3 ?
C7 C8 C9 N1 -179.6(4) . . . . ?
C3 C8 C9 N1 -0.7(5) . . . . ?
N1 C2 N10 C9 -2.2(7) . . . 4 ?
C3 C2 N10 C9 173.9(4) . . . 4 ?
N1 Mo1 N11 C10 -107(4) . . . 4 ?
N1 Mo1 N11 C10 -17(4) 3 . . 4 ?
N1 Mo1 N11 C10 73(4) 2 . . 4 ?
N1 Mo1 N11 C10 163(4) 4 . . 4 ?
N1 Mo1 N11 C10 163(4) . . . . ?
N1 Mo1 N11 C10 -107(4) 3 . . . ?
N1 Mo1 N11 C10 -17(4) 2 . . . ?
N1 Mo1 N11 C10 73(4) 4 . . . ?
N1 Mo1 N11 C10 73(4) . . . 3 ?
N1 Mo1 N11 C10 163(4) 3 . . 3 ?
N1 Mo1 N11 C10 -107(4) 2 . . 3 ?
N1 Mo1 N11 C10 -17(4) 4 . . 3 ?
N1 Mo1 N11 C10 -17(4) . . . 2 ?
N1 Mo1 N11 C10 73(4) 3 . . 2 ?
N1 Mo1 N11 C10 163(4) 2 . . 2 ?
N1 Mo1 N11 C10 -107(4) 4 . . 2 ?
C10 N11 C10 C13 -117(6) 4 . . . ?
C10 N11 C10 C13 151(6) 3 . . . ?
C10 N11 C10 C13 -163(6) 2 . . . ?
Mo1 N11 C10 C13 17(6) . . . . ?
C10 N11 C10 C12 123(4) 4 . . . ?
C10 N11 C10 C12 30(4) 3 . . . ?
C10 N11 C10 C12 77(4) 2 . . . ?
Mo1 N11 C10 C12 -103(4) . . . . ?
C10 N11 C10 C11 5(4) 4 . . . ?
C10 N11 C10 C11 -88(4) 3 . . . ?
C10 N11 C10 C11 -42(4) 2 . . . ?
Mo1 N11 C10 C11 138(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.998

_diffrn_reflns_theta_full        24.99

_diffrn_measured_fraction_theta_full 0.998

_refine_diff_density_max         0.672

_refine_diff_density_min         -0.506

_refine_diff_density_rms         0.064