# Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2000
# CCDC Number: 186/1921
 
data_str671 
 
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C20 H25 Br N O7 Re' 
_chemical_formula_weight          657.52 
_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' 
 'Br'  'Br'  -0.2901   2.4595 
 '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            trigonal 
_symmetry_space_group_name_H-M    P3(2)2(1) 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-y, x-y, z+2/3' 
 '-x+y, -x, z+1/3' 
 'y, x, -z' 
 'x-y, -y, -z+1/3' 
 '-x, -x+y, -z+2/3' 
 
_cell_length_a                    14.438(2) 
_cell_length_b                    14.438(2) 
_cell_length_c                    19.673(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 120.00 
_cell_volume                      3551.5(10) 
_cell_formula_units_Z             6 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     22 
_cell_measurement_theta_min       7.5 
_cell_measurement_theta_max       16 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             colourless 
_exptl_crystal_size_max           0.65 
_exptl_crystal_size_mid           0.62 
_exptl_crystal_size_min           0.47 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.845 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1908 
_exptl_absorpt_coefficient_mu     6.858 
_exptl_absorpt_correction_type    'psi scans' 
_exptl_absorpt_correction_T_min   0.98 
_exptl_absorpt_correction_T_max   0.21 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'normal-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device        'Nicolet R3mV' 
_diffrn_measurement_method        ? 
_diffrn_standards_number          3 
_diffrn_standards_interval_count  97 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         <2 
_diffrn_reflns_number             4700 
_diffrn_reflns_av_R_equivalents   0.0552 
_diffrn_reflns_av_sigmaI/netI     0.0597 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        14 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        14 
_diffrn_reflns_limit_l_min        -23 
_diffrn_reflns_limit_l_max        23 
_diffrn_reflns_theta_min          2.63 
_diffrn_reflns_theta_max          25.05 
_reflns_number_total              2366 
_reflns_number_observed           2141 
_reflns_observed_criterion        >2sigma(I) 
 
_computing_data_collection        'Nicolet R3' 
_computing_cell_refinement        'Nicolet R3' 
_computing_data_reduction         XDISK 
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     XP 
_computing_publication_material   CIFTAB 
 
_refine_special_details 
; 
 Refinement on F^2^ for ALL reflections except for 3 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^)+(0.0517P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      'Direct Methods' 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     'fixed contribution' 
_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(2) 
_refine_ls_number_reflns          2363 
_refine_ls_number_parameters      271 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0405 
_refine_ls_R_factor_obs           0.0348 
_refine_ls_wR_factor_all          0.0856 
_refine_ls_wR_factor_obs          0.0814 
_refine_ls_goodness_of_fit_all    1.007 
_refine_ls_goodness_of_fit_obs    1.028 
_refine_ls_restrained_S_all       1.023 
_refine_ls_restrained_S_obs       1.028 
_refine_ls_shift/esd_max          -0.001 
_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 
Re1 Re 0.63398(3) 0.91178(3) 0.88569(2) 0.03574(14) Uani 1 d . . 
Br1 Br 0.64219(10) 0.85033(10) 1.00889(5) 0.0539(3) Uani 1 d . . 
N1 N 0.8118(6) 1.0044(6) 0.8967(4) 0.033(2) Uani 1 d . . 
O1 O 0.3962(7) 0.7522(9) 0.8635(6) 0.089(4) Uani 1 d . . 
O2 O 0.5520(7) 1.0540(8) 0.9416(5) 0.076(3) Uani 1 d . . 
O3 O 0.6369(10) 0.9836(10) 0.7393(4) 0.098(4) Uani 1 d . . 
O4 O 0.6946(5) 0.8079(5) 0.8518(3) 0.042(2) Uani 1 d . . 
O5 O 0.8518(6) 0.8050(6) 0.8337(4) 0.045(2) Uani 1 d . . 
O6 O 0.8215(7) 1.1922(6) 0.8237(4) 0.051(2) Uani 1 d . . 
O7 O 0.8972(6) 1.2835(6) 0.9248(4) 0.052(2) Uani 1 d . . 
C1 C 0.4866(11) 0.8146(11) 0.8731(6) 0.054(3) Uani 1 d . . 
C2 C 0.5863(7) 1.0009(9) 0.9176(6) 0.049(3) Uani 1 d . . 
C3 C 0.6384(10) 0.9588(10) 0.7955(6) 0.057(3) Uani 1 d . . 
C4 C 0.5757(12) 0.6203(10) 0.8887(8) 0.077(4) Uani 1 d . . 
H4A H 0.5333(12) 0.6402(10) 0.9160(8) 0.080 Uiso 1 d R . 
H4B H 0.5323(12) 0.5476(10) 0.8738(8) 0.080 Uiso 1 d R . 
H4C H 0.6345(12) 0.6267(10) 0.9151(8) 0.080 Uiso 1 d R . 
C5 C 0.6256(9) 0.6968(10) 0.8280(6) 0.055(3) Uani 1 d . . 
H5A H 0.5673(9) 0.6933(10) 0.8024(6) 0.080 Uiso 1 d R . 
C6 C 0.6909(9) 0.6674(10) 0.7818(6) 0.054(3) Uani 1 d . . 
H6A H 0.7057(9) 0.7068(10) 0.7400(6) 0.080 Uiso 1 d R . 
H6B H 0.6506(9) 0.5927(10) 0.7708(6) 0.080 Uiso 1 d R . 
C7 C 0.7963(9) 0.6915(9) 0.8138(6) 0.046(3) Uani 1 d . . 
H7A H 0.7836(9) 0.6465(9) 0.8527(6) 0.080 Uiso 1 d R . 
C8 C 0.8699(10) 0.6796(12) 0.7651(6) 0.066(3) Uani 1 d . . 
H8A H 0.9346(10) 0.6955(12) 0.7885(6) 0.080 Uiso 1 d R . 
H8B H 0.8367(10) 0.6081(12) 0.7475(6) 0.080 Uiso 1 d R . 
H8C H 0.8864(10) 0.7291(12) 0.7283(6) 0.080 Uiso 1 d R . 
C9 C 0.7928(8) 0.8250(8) 0.8814(5) 0.038(2) Uani 1 d . . 
H9A H 0.7791(8) 0.7814(8) 0.9211(5) 0.080 Uiso 1 d R . 
C10 C 0.8591(8) 0.9439(8) 0.8985(4) 0.032(2) Uani 1 d . . 
C11 C 0.9657(8) 0.9843(9) 0.9135(5) 0.038(2) Uani 1 d . . 
H11A H 0.9952(8) 0.9378(9) 0.9173(5) 0.080 Uiso 1 d R . 
C12 C 1.0296(8) 1.0930(9) 0.9237(5) 0.039(2) Uani 1 d . . 
H12A H 1.1046(8) 1.1240(9) 0.9328(5) 0.080 Uiso 1 d R . 
C13 C 0.9840(7) 1.1583(8) 0.9188(4) 0.035(2) Uani 1 d . . 
H13A H 1.0261(7) 1.2343(8) 0.9252(4) 0.080 Uiso 1 d R . 
C14 C 0.8764(7) 1.1101(7) 0.9051(4) 0.030(2) Uani 1 d . . 
C15 C 0.8281(8) 1.1834(8) 0.8940(5) 0.042(2) Uani 1 d . . 
H15A H 0.7581(8) 1.1520(8) 0.9140(5) 0.080 Uiso 1 d R . 
C16 C 0.7726(14) 1.2604(14) 0.7299(7) 0.092(5) Uani 1 d . . 
H16A H 0.7281(14) 1.1882(14) 0.7145(7) 0.080 Uiso 1 d R . 
H16B H 0.7428(14) 1.3033(14) 0.7149(7) 0.080 Uiso 1 d R . 
H16C H 0.8432(14) 1.2887(14) 0.7114(7) 0.080 Uiso 1 d R . 
C17 C 0.7765(11) 1.2600(12) 0.8071(7) 0.065(4) Uani 1 d . . 
H17A H 0.7053(11) 1.2282(12) 0.8251(7) 0.080 Uiso 1 d R . 
C18 C 0.8418(10) 1.3665(9) 0.8397(8) 0.066(4) Uani 1 d . . 
H18A H 0.8073(10) 1.4080(9) 0.8332(8) 0.080 Uiso 1 d R . 
H18B H 0.9098(10) 1.4027(9) 0.8170(8) 0.080 Uiso 1 d R . 
C19 C 0.8604(11) 1.3592(9) 0.9138(8) 0.063(3) Uani 1 d . . 
H19A H 0.9166(11) 1.4280(9) 0.9283(8) 0.080 Uiso 1 d R . 
C20 C 0.7630(14) 1.3342(14) 0.9587(8) 0.088(5) Uani 1 d . . 
H20A H 0.7792(14) 1.3311(14) 1.0057(8) 0.080 Uiso 1 d R . 
H20B H 0.7426(14) 1.3876(14) 0.9528(8) 0.080 Uiso 1 d R . 
H20C H 0.7052(14) 1.2658(14) 0.9448(8) 0.080 Uiso 1 d 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 0.0250(2) 0.0377(2) 0.0413(2) -0.0007(2) -0.0032(2) 0.0133(2) 
Br1 0.0499(7) 0.0622(7) 0.0449(5) 0.0098(5) 0.0055(5) 0.0246(6) 
N1 0.033(4) 0.034(4) 0.033(3) -0.002(3) -0.003(3) 0.019(4) 
O1 0.025(4) 0.079(7) 0.129(9) -0.032(7) -0.009(5) 0.001(5) 
O2 0.041(5) 0.078(7) 0.116(8) -0.015(5) 0.013(5) 0.034(5) 
O3 0.124(9) 0.117(9) 0.044(4) 0.005(5) -0.014(5) 0.054(8) 
O4 0.022(3) 0.038(4) 0.057(4) -0.007(3) 0.000(3) 0.008(3) 
O5 0.041(4) 0.041(4) 0.052(4) -0.004(4) 0.005(3) 0.020(3) 
O6 0.055(5) 0.057(5) 0.051(4) 0.008(4) 0.001(4) 0.035(4) 
O7 0.041(4) 0.032(4) 0.075(5) -0.010(4) -0.011(4) 0.011(3) 
C1 0.063(8) 0.062(8) 0.053(6) -0.011(6) -0.014(6) 0.043(7) 
C2 0.013(4) 0.044(6) 0.068(6) 0.007(5) 0.005(4) -0.001(4) 
C3 0.059(8) 0.057(7) 0.054(6) 0.001(5) -0.007(6) 0.028(6) 
C4 0.056(8) 0.045(7) 0.109(11) 0.000(7) 0.033(8) 0.009(6) 
C5 0.040(6) 0.046(6) 0.075(7) -0.025(6) -0.012(6) 0.018(5) 
C6 0.043(6) 0.053(7) 0.067(7) -0.018(6) -0.016(6) 0.025(6) 
C7 0.043(6) 0.043(6) 0.053(6) -0.009(5) -0.002(5) 0.022(5) 
C8 0.052(7) 0.081(10) 0.071(7) -0.032(7) -0.009(6) 0.036(6) 
C9 0.033(5) 0.034(5) 0.042(5) -0.005(4) -0.001(4) 0.012(5) 
C10 0.030(5) 0.038(5) 0.029(4) -0.007(4) -0.003(4) 0.017(4) 
C11 0.036(5) 0.041(6) 0.037(5) -0.003(5) -0.005(4) 0.019(5) 
C12 0.025(5) 0.049(6) 0.042(5) -0.006(5) -0.006(4) 0.017(5) 
C13 0.028(5) 0.032(5) 0.039(5) -0.005(4) -0.004(4) 0.010(4) 
C14 0.031(5) 0.023(4) 0.031(4) 0.004(4) -0.001(4) 0.010(4) 
C15 0.029(5) 0.030(5) 0.057(6) -0.005(5) 0.000(5) 0.005(5) 
C16 0.093(12) 0.110(14) 0.102(11) 0.026(11) -0.007(10) 0.072(11) 
C17 0.061(8) 0.075(9) 0.081(8) 0.018(7) 0.009(7) 0.051(7) 
C18 0.040(7) 0.038(6) 0.119(12) 0.021(7) 0.006(7) 0.019(5) 
C19 0.052(8) 0.033(6) 0.100(10) -0.004(6) 0.003(7) 0.018(6) 
C20 0.097(12) 0.078(10) 0.108(12) -0.008(9) 0.027(10) 0.058(10) 
 
_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 C2 1.847(12) . ? 
Re1 C1 1.890(14) . ? 
Re1 C3 1.889(11) . ? 
Re1 O4 2.184(7) . ? 
Re1 N1 2.234(8) . ? 
Re1 Br1 2.6041(12) . ? 
N1 C14 1.343(12) . ? 
N1 C10 1.352(12) . ? 
O1 C1 1.173(15) . ? 
O2 C2 1.197(14) . ? 
O3 C3 1.165(12) . ? 
O4 C9 1.436(12) . ? 
O4 C5 1.479(13) . ? 
O5 C9 1.390(12) . ? 
O5 C7 1.472(13) . ? 
O6 C15 1.396(12) . ? 
O6 C17 1.457(14) . ? 
O7 C15 1.417(12) . ? 
O7 C19 1.451(14) . ? 
C4 C5 1.54(2) . ? 
C5 C6 1.52(2) . ? 
C6 C7 1.519(15) . ? 
C7 C8 1.503(15) . ? 
C9 C10 1.528(14) . ? 
C10 C11 1.378(13) . ? 
C11 C12 1.38(2) . ? 
C12 C13 1.397(15) . ? 
C13 C14 1.375(13) . ? 
C14 C15 1.546(15) . ? 
C16 C17 1.52(2) . ? 
C17 C18 1.49(2) . ? 
C18 C19 1.50(2) . ? 
C19 C20 1.54(2) . ? 
 
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 
C2 Re1 C1 83.6(5) . . ? 
C2 Re1 C3 91.5(5) . . ? 
C1 Re1 C3 88.1(5) . . ? 
C2 Re1 O4 177.6(4) . . ? 
C1 Re1 O4 98.0(4) . . ? 
C3 Re1 O4 90.4(4) . . ? 
C2 Re1 N1 105.5(3) . . ? 
C1 Re1 N1 170.8(4) . . ? 
C3 Re1 N1 93.1(4) . . ? 
O4 Re1 N1 72.9(2) . . ? 
C2 Re1 Br1 91.0(4) . . ? 
C1 Re1 Br1 95.5(4) . . ? 
C3 Re1 Br1 175.8(4) . . ? 
O4 Re1 Br1 87.0(2) . . ? 
N1 Re1 Br1 83.1(2) . . ? 
C14 N1 C10 116.3(8) . . ? 
C14 N1 Re1 129.0(6) . . ? 
C10 N1 Re1 114.6(6) . . ? 
C9 O4 C5 112.7(8) . . ? 
C9 O4 Re1 117.3(5) . . ? 
C5 O4 Re1 123.9(6) . . ? 
C9 O5 C7 111.2(8) . . ? 
C15 O6 C17 110.9(9) . . ? 
C15 O7 C19 111.6(9) . . ? 
O1 C1 Re1 177.4(11) . . ? 
O2 C2 Re1 175.8(10) . . ? 
O3 C3 Re1 176.9(12) . . ? 
O4 C5 C6 108.5(9) . . ? 
O4 C5 C4 110.7(10) . . ? 
C6 C5 C4 113.5(11) . . ? 
C7 C6 C5 112.3(9) . . ? 
O5 C7 C8 105.9(9) . . ? 
O5 C7 C6 106.9(8) . . ? 
C8 C7 C6 113.2(9) . . ? 
O5 C9 O4 110.3(8) . . ? 
O5 C9 C10 106.1(8) . . ? 
O4 C9 C10 107.0(8) . . ? 
N1 C10 C11 123.4(9) . . ? 
N1 C10 C9 119.0(8) . . ? 
C11 C10 C9 117.5(9) . . ? 
C10 C11 C12 118.8(10) . . ? 
C11 C12 C13 119.0(9) . . ? 
C14 C13 C12 117.8(9) . . ? 
N1 C14 C13 124.5(9) . . ? 
N1 C14 C15 117.8(8) . . ? 
C13 C14 C15 117.6(8) . . ? 
O6 C15 O7 112.1(8) . . ? 
O6 C15 C14 106.1(8) . . ? 
O7 C15 C14 107.9(8) . . ? 
O6 C17 C18 109.4(11) . . ? 
O6 C17 C16 104.9(11) . . ? 
C18 C17 C16 115.6(13) . . ? 
C17 C18 C19 112.9(11) . . ? 
O7 C19 C18 110.1(11) . . ? 
O7 C19 C20 112.0(11) . . ? 
C18 C19 C20 113.5(12) . . ? 
 
_refine_diff_density_max    0.814 
_refine_diff_density_min   -1.377 
_refine_diff_density_rms    0.145