# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2011


data_global
_journal_name_full               'Dalton Trans.'
_journal_coden_cambridge         0222
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
loop_
_publ_author_name
'Anita Drozdz'
'Martina Bubrin'
'Jan Fiedler'
'Stanislav Zalis'
'Wolfgang Kaim'
_publ_contact_author_name        'Anita Drozdz '
_publ_contact_author_email       iacdrozd@iac.uni-stuttgart.de

data_ac07
_database_code_depnum_ccdc_archive 'CCDC 833300'
#TrackingRef '- AC07.CIF'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C13 H20 Cl N2 O3 Re'
_chemical_formula_sum            'C13 H20 Cl N2 O3 Re'
_chemical_formula_weight         473.96

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'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'

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

_cell_length_a                   6.2459(8)
_cell_length_b                   13.6956(19)
_cell_length_c                   18.873(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1614.5(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3277
_cell_measurement_theta_min      1.84
_cell_measurement_theta_max      28.71

_exptl_crystal_description       needle
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.950
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             912
_exptl_absorpt_coefficient_mu    7.700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1487
_exptl_absorpt_correction_T_max  0.7482
_exptl_absorpt_process_details   'Blessing, 1995'

_exptl_special_details           
;
?
;

_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  'Bruker Kappa APEX II Duo'
_diffrn_measurement_method       'Omega + Phi Scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            7787
_diffrn_reflns_av_R_equivalents  0.1550
_diffrn_reflns_av_sigmaI/netI    0.2281
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.84
_diffrn_reflns_theta_max         28.71
_reflns_number_total             3931
_reflns_number_gt                3277
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX II Software Suite, 2008'
_computing_cell_refinement       'Bruker APEX II Software Suite, 2008'
_computing_data_reduction        'Bruker APEX II Software Suite, 2008'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-plus, XP (Sheldrick, 1991)'
_computing_publication_material  ?

_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^)+(0.0371P)^2^+38.4744P] 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    constr
_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   0.52(3)
_refine_ls_number_reflns         3931
_refine_ls_number_parameters     187
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1106
_refine_ls_R_factor_gt           0.0587
_refine_ls_wR_factor_ref         0.1416
_refine_ls_wR_factor_gt          0.1349
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_restrained_S_all      1.109
_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
Re1 Re 0.46527(8) 0.52568(3) 0.87513(3) 0.00926(13) Uani 1 1 d . . .
Cl1 Cl 0.7579(6) 0.6087(2) 0.9385(2) 0.0173(7) Uani 1 1 d . . .
C1 C 0.604(2) 0.3986(8) 0.8785(9) 0.010(2) Uani 1 1 d . . .
O1 O 0.6927(19) 0.3258(7) 0.8769(9) 0.028(3) Uani 1 1 d . . .
C2 C 0.601(3) 0.5434(9) 0.7850(8) 0.018(3) Uani 1 1 d . . .
O2 O 0.6808(19) 0.5506(8) 0.7290(7) 0.020(2) Uani 1 1 d . . .
C3 C 0.230(3) 0.4666(11) 0.8294(8) 0.021(3) Uani 1 1 d . . .
O3 O 0.0859(17) 0.4285(8) 0.7972(7) 0.021(3) Uani 1 1 d . . .
N1 N 0.3041(19) 0.6684(9) 0.8860(8) 0.017(3) Uani 1 1 d . . .
N2 N 0.3114(18) 0.5210(9) 0.9803(6) 0.011(2) Uani 1 1 d . . .
C4 C 0.231(3) 0.6010(11) 0.9993(9) 0.018(3) Uani 1 1 d . . .
H4A H 0.1741 0.6085 1.0456 0.021 Uiso 1 1 calc R . .
C5 C 0.227(2) 0.6832(10) 0.9485(8) 0.011(3) Uani 1 1 d U . .
H5A H 0.1690 0.7449 0.9615 0.013 Uiso 1 1 calc R . .
C6 C 0.303(3) 0.4328(11) 1.0290(8) 0.019(3) Uani 1 1 d . . .
C7 C 0.192(3) 0.3511(12) 0.9859(11) 0.030(4) Uani 1 1 d . . .
H7A H 0.0590 0.3763 0.9654 0.045 Uiso 1 1 calc R . .
H7B H 0.1598 0.2960 1.0172 0.045 Uiso 1 1 calc R . .
H7C H 0.2876 0.3294 0.9478 0.045 Uiso 1 1 calc R . .
C8 C 0.523(3) 0.4071(10) 1.0533(8) 0.021(3) Uani 1 1 d . . .
H8A H 0.6106 0.3892 1.0123 0.032 Uiso 1 1 calc R . .
H8B H 0.5150 0.3519 1.0862 0.032 Uiso 1 1 calc R . .
H8C H 0.5868 0.4634 1.0773 0.032 Uiso 1 1 calc R . .
C9 C 0.155(3) 0.4554(10) 1.0949(9) 0.019(3) Uani 1 1 d . . .
H9A H 0.2325 0.4964 1.1288 0.029 Uiso 1 1 calc R . .
H9B H 0.1134 0.3940 1.1178 0.029 Uiso 1 1 calc R . .
H9C H 0.0258 0.4898 1.0789 0.029 Uiso 1 1 calc R . .
C10 C 0.278(3) 0.7442(11) 0.8309(8) 0.020(3) Uani 1 1 d . . .
C11 C 0.149(3) 0.8340(11) 0.8574(9) 0.022(4) Uani 1 1 d . . .
H11A H -0.0001 0.8149 0.8656 0.033 Uiso 1 1 calc R . .
H11B H 0.1544 0.8857 0.8215 0.033 Uiso 1 1 calc R . .
H11C H 0.2117 0.8579 0.9017 0.033 Uiso 1 1 calc R . .
C12 C 0.494(2) 0.7794(10) 0.8053(8) 0.017(3) Uani 1 1 d . . .
H12A H 0.5752 0.8060 0.8454 0.026 Uiso 1 1 calc R . .
H12B H 0.4739 0.8305 0.7695 0.026 Uiso 1 1 calc R . .
H12C H 0.5730 0.7247 0.7845 0.026 Uiso 1 1 calc R . .
C13 C 0.147(3) 0.6963(12) 0.7696(9) 0.027(4) Uani 1 1 d . . .
H13A H 0.2360 0.6481 0.7451 0.040 Uiso 1 1 calc R . .
H13B H 0.1019 0.7469 0.7359 0.040 Uiso 1 1 calc R . .
H13C H 0.0200 0.6640 0.7892 0.040 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
Re1 0.0108(2) 0.00698(18) 0.01003(19) -0.0008(2) -0.0004(2) -0.00016(19)
Cl1 0.0160(19) 0.0199(16) 0.0160(17) -0.0029(12) -0.0022(14) -0.0013(14)
C1 0.008(6) 0.007(5) 0.014(6) -0.004(6) 0.008(6) -0.002(4)
O1 0.038(7) 0.015(5) 0.031(6) 0.002(6) 0.008(8) 0.012(4)
C2 0.041(10) 0.008(6) 0.006(6) 0.005(4) 0.006(6) 0.003(5)
O2 0.013(6) 0.021(6) 0.026(6) -0.002(4) 0.002(5) 0.000(4)
C3 0.035(10) 0.008(6) 0.018(7) 0.002(5) 0.011(6) 0.006(7)
O3 0.006(6) 0.026(5) 0.031(6) -0.011(5) -0.005(4) 0.000(4)
N1 0.009(6) 0.016(5) 0.026(8) -0.005(5) 0.003(6) 0.006(4)
N2 0.014(6) 0.010(5) 0.010(5) 0.001(5) -0.009(4) -0.001(5)
C4 0.016(8) 0.025(8) 0.012(7) 0.001(6) 0.005(6) 0.010(6)
C5 0.005(6) 0.012(5) 0.017(6) -0.001(4) -0.002(5) 0.006(4)
C6 0.037(10) 0.008(6) 0.013(7) 0.005(5) -0.002(7) -0.001(6)
C7 0.046(12) 0.012(7) 0.031(10) 0.008(7) -0.004(9) 0.000(7)
C8 0.024(9) 0.018(6) 0.021(7) 0.008(5) -0.007(7) -0.001(6)
C9 0.027(9) 0.013(7) 0.016(6) 0.004(5) 0.007(6) 0.006(5)
C10 0.032(10) 0.017(7) 0.011(7) -0.006(5) -0.001(6) 0.001(6)
C11 0.022(9) 0.016(7) 0.027(9) -0.003(6) 0.001(6) 0.007(6)
C12 0.012(10) 0.017(6) 0.023(7) -0.001(5) -0.005(6) 0.003(5)
C13 0.042(12) 0.020(8) 0.017(8) 0.009(6) -0.002(8) 0.000(7)

_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
Re1 C3 1.888(19) . ?
Re1 C2 1.915(15) . ?
Re1 C1 1.944(12) . ?
Re1 N2 2.206(12) . ?
Re1 N1 2.208(11) . ?
Re1 Cl1 2.463(4) . ?
C1 O1 1.142(15) . ?
C2 O2 1.173(19) . ?
C3 O3 1.20(2) . ?
N1 C5 1.29(2) . ?
N1 C10 1.48(2) . ?
N2 C4 1.26(2) . ?
N2 C6 1.519(18) . ?
C4 C5 1.48(2) . ?
C4 H4A 0.9500 . ?
C5 H5A 0.9500 . ?
C6 C8 1.49(2) . ?
C6 C7 1.55(2) . ?
C6 C9 1.58(2) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C12 1.51(2) . ?
C10 C11 1.55(2) . ?
C10 C13 1.56(2) . ?
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 . ?

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
C3 Re1 C2 89.6(7) . . ?
C3 Re1 C1 88.7(6) . . ?
C2 Re1 C1 86.9(6) . . ?
C3 Re1 N2 93.4(6) . . ?
C2 Re1 N2 174.4(5) . . ?
C1 Re1 N2 97.9(6) . . ?
C3 Re1 N1 93.8(6) . . ?
C2 Re1 N1 99.9(6) . . ?
C1 Re1 N1 172.7(7) . . ?
N2 Re1 N1 75.1(5) . . ?
C3 Re1 Cl1 176.7(5) . . ?
C2 Re1 Cl1 92.5(5) . . ?
C1 Re1 Cl1 93.9(4) . . ?
N2 Re1 Cl1 84.3(3) . . ?
N1 Re1 Cl1 83.4(4) . . ?
O1 C1 Re1 175.7(15) . . ?
O2 C2 Re1 177.3(13) . . ?
O3 C3 Re1 176.7(13) . . ?
C5 N1 C10 119.4(12) . . ?
C5 N1 Re1 113.3(10) . . ?
C10 N1 Re1 127.3(10) . . ?
C4 N2 C6 120.4(13) . . ?
C4 N2 Re1 113.9(11) . . ?
C6 N2 Re1 125.7(10) . . ?
N2 C4 C5 119.1(14) . . ?
N2 C4 H4A 120.5 . . ?
C5 C4 H4A 120.5 . . ?
N1 C5 C4 117.7(13) . . ?
N1 C5 H5A 121.1 . . ?
C4 C5 H5A 121.1 . . ?
C8 C6 N2 110.1(13) . . ?
C8 C6 C7 113.8(14) . . ?
N2 C6 C7 105.7(12) . . ?
C8 C6 C9 110.2(13) . . ?
N2 C6 C9 109.9(12) . . ?
C7 C6 C9 107.0(15) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N1 C10 C12 110.5(13) . . ?
N1 C10 C11 112.8(13) . . ?
C12 C10 C11 108.2(13) . . ?
N1 C10 C13 106.5(13) . . ?
C12 C10 C13 111.4(14) . . ?
C11 C10 C13 107.4(14) . . ?
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 . . ?

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
C3 Re1 C1 O1 102(20) . . . . ?
C2 Re1 C1 O1 12(20) . . . . ?
N2 Re1 C1 O1 -165(20) . . . . ?
N1 Re1 C1 O1 -148(18) . . . . ?
Cl1 Re1 C1 O1 -80(20) . . . . ?
C3 Re1 C2 O2 -37(33) . . . . ?
C1 Re1 C2 O2 51(33) . . . . ?
N2 Re1 C2 O2 -160(28) . . . . ?
N1 Re1 C2 O2 -131(33) . . . . ?
Cl1 Re1 C2 O2 145(33) . . . . ?
C2 Re1 C3 O3 15(23) . . . . ?
C1 Re1 C3 O3 -72(23) . . . . ?
N2 Re1 C3 O3 -170(23) . . . . ?
N1 Re1 C3 O3 115(23) . . . . ?
Cl1 Re1 C3 O3 145(18) . . . . ?
C3 Re1 N1 C5 100.5(12) . . . . ?
C2 Re1 N1 C5 -169.2(12) . . . . ?
C1 Re1 N1 C5 -10(5) . . . . ?
N2 Re1 N1 C5 8.0(10) . . . . ?
Cl1 Re1 N1 C5 -77.8(11) . . . . ?
C3 Re1 N1 C10 -79.3(13) . . . . ?
C2 Re1 N1 C10 10.9(14) . . . . ?
C1 Re1 N1 C10 170(4) . . . . ?
N2 Re1 N1 C10 -171.8(14) . . . . ?
Cl1 Re1 N1 C10 102.4(13) . . . . ?
C3 Re1 N2 C4 -100.7(12) . . . . ?
C2 Re1 N2 C4 21(7) . . . . ?
C1 Re1 N2 C4 170.1(12) . . . . ?
N1 Re1 N2 C4 -7.6(11) . . . . ?
Cl1 Re1 N2 C4 77.0(11) . . . . ?
C3 Re1 N2 C6 81.2(12) . . . . ?
C2 Re1 N2 C6 -157(6) . . . . ?
C1 Re1 N2 C6 -8.0(12) . . . . ?
N1 Re1 N2 C6 174.2(12) . . . . ?
Cl1 Re1 N2 C6 -101.2(11) . . . . ?
C6 N2 C4 C5 -175.3(13) . . . . ?
Re1 N2 C4 C5 6.4(19) . . . . ?
C10 N1 C5 C4 172.2(14) . . . . ?
Re1 N1 C5 C4 -7.6(18) . . . . ?
N2 C4 C5 N1 1(2) . . . . ?
C4 N2 C6 C8 -112.7(17) . . . . ?
Re1 N2 C6 C8 65.4(15) . . . . ?
C4 N2 C6 C7 124.0(16) . . . . ?
Re1 N2 C6 C7 -57.9(18) . . . . ?
C4 N2 C6 C9 9(2) . . . . ?
Re1 N2 C6 C9 -173.1(10) . . . . ?
C5 N1 C10 C12 119.6(15) . . . . ?
Re1 N1 C10 C12 -60.6(16) . . . . ?
C5 N1 C10 C11 -2(2) . . . . ?
Re1 N1 C10 C11 178.2(10) . . . . ?
C5 N1 C10 C13 -119.2(16) . . . . ?
Re1 N1 C10 C13 60.7(18) . . . . ?

_diffrn_measured_fraction_theta_max 0.969
_diffrn_reflns_theta_full        28.71
_diffrn_measured_fraction_theta_full 0.969
_refine_diff_density_max         4.608
_refine_diff_density_min         -4.754
_refine_diff_density_rms         0.576