# Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 1999
# CCDC Number: 186/1656

data_global

_publ_contact_author_name      'Animesh Chakravorty'
_publ_contact_author_address
;
Department of Inorganic Chemistry
Indian Association for the Cultivation of Science
Calcutta 700 032, India

e-mail: icac@mahendra.iacs.res.in
;
_publ_requested_journal       'J. Chem. Soc. Dalton Trans'
_publ_section_title
;
Synthesis, structure and properties of [Re(V)L(O)Cl3], [Re(V)L(NAr)Cl3]
,[Re(III)L(OPPh3)Cl3] and [Re(III)L(PPh3)Cl3] [L = 1-methyl-2-(arylazo)
imidazole]
;
_publ_requested_letter
;
Please find the cif files for the four structures e.g. 2a, 3a, 4c and 
5c. 
;

data_[ReL1(O)Cl3,2a 
  
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C10 H10 Cl3 N4 O Re' 
_chemical_formula_weight          494.77 
_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' 
 '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            Monoclinic 
_symmetry_space_group_name_H-M    P2(1)/c 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y-1/2, z-1/2' 
  
_cell_length_a                    14.231(7) 
_cell_length_b                    7.716(3) 
_cell_length_c                    13.409(6) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  101.41(4) 
_cell_angle_gamma                 90.00 
_cell_volume                      1443.3(11) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     30 
_cell_measurement_theta_min       7 
_cell_measurement_theta_max       14 
  
_exptl_crystal_description        parallelopiped 
_exptl_crystal_colour             dark 
_exptl_crystal_size_max           0.35 
_exptl_crystal_size_mid           0.20 
_exptl_crystal_size_min           0.15 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     2.277 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              928 
_exptl_absorpt_coefficient_mu     8.970 
_exptl_absorpt_correction_type    'semi-empirical' 
_exptl_absorpt_correction_T_min   0.068 
_exptl_absorpt_correction_T_max   0.129 
  
_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_type        'Siemens R3m/V' 
_diffrn_measurement_method        '\w scans' 
_diffrn_standards_number          2 
_diffrn_standards_interval_count  198 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         nil 
_diffrn_reflns_number             2477 
_diffrn_reflns_av_R_equivalents   0.0162 
_diffrn_reflns_av_sigmaI/netI     0.0366 
_diffrn_reflns_limit_h_min        -16 
_diffrn_reflns_limit_h_max        16 
_diffrn_reflns_limit_k_min        -9 
_diffrn_reflns_limit_k_max        0 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        15 
_diffrn_reflns_theta_min          2.92 
_diffrn_reflns_theta_max          24.93 
_reflns_number_total              2287 
_reflns_number_observed           1881 
_reflns_observed_criterion        >2sigma(I) 
  
_computing_data_collection        'Siemens p3' 
_computing_cell_refinement        'Siemens p3' 
_computing_data_reduction         'Siemens P3' 
_computing_structure_solution     'Siemens SHELXTL V-5.03 (Sheldrick, 1994)' 
_computing_structure_refinement   'Siemens SHELXTL V-5.03 (Sheldrick, 1994)'
_computing_molecular_graphics     'Siemens SHELXTL V-5.03 (Sheldrick, 1994)' 
_computing_publication_material   'Siemens SHELXTL V-5.03 (Sheldrick, 1994)' 
_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^)+(0.0371P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      'Heavey atom method' 
_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_number_reflns          2287 
_refine_ls_number_parameters      172 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0450 
_refine_ls_R_factor_obs           0.0301 
_refine_ls_wR_factor_all          0.0693 
_refine_ls_wR_factor_obs          0.0637 
_refine_ls_goodness_of_fit_all    1.045 
_refine_ls_goodness_of_fit_obs    1.068 
_refine_ls_restrained_S_all       1.045 
_refine_ls_restrained_S_obs       1.068 
_refine_ls_shift/su_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 
Re Re 0.71802(2) 0.77915(4) 0.34782(2) 0.03248(12) Uani 1 d . . 
Cl1 Cl 0.62959(14) 0.8635(3) 0.1922(2) 0.0483(5) Uani 1 d . . 
Cl3 Cl 0.58469(14) 0.6077(3) 0.3644(2) 0.0483(5) Uani 1 d . . 
Cl2 Cl 0.82485(15) 1.0057(3) 0.3332(2) 0.0543(6) Uani 1 d . . 
O1 O 0.7889(3) 0.6174(7) 0.3278(4) 0.0439(13) Uani 1 d . . 
N1 N 0.6479(4) 0.9779(7) 0.4219(5) 0.0338(14) Uani 1 d . . 
N2 N 0.6462(4) 1.1227(8) 0.5618(5) 0.040(2) Uani 1 d . . 
N3 N 0.7562(4) 0.8830(8) 0.5671(4) 0.0362(15) Uani 1 d . . 
N4 N 0.7749(4) 0.7706(8) 0.5036(5) 0.0370(15) Uani 1 d . . 
C1 C 0.5796(5) 1.1043(10) 0.4003(6) 0.041(2) Uani 1 d . . 
H1A H 0.5409(5) 1.1255(10) 0.3370(6) 0.049 Uiso 1 calc R . 
C2 C 0.5780(6) 1.1928(10) 0.4865(6) 0.048(2) Uani 1 d . . 
H2A H 0.5377(6) 1.2850(10) 0.4935(6) 0.057 Uiso 1 calc R . 
C3 C 0.6865(5) 0.9925(9) 0.5187(6) 0.035(2) Uani 1 d . . 
C4 C 0.6705(7) 1.1745(11) 0.6692(6) 0.058(2) Uani 1 d . . 
H4A H 0.6314(7) 1.2711(11) 0.6804(6) 0.088 Uiso 1 calc R . 
H4B H 0.7368(7) 1.2071(11) 0.6861(6) 0.088 Uiso 1 calc R . 
H4C H 0.6592(7) 1.0791(11) 0.7112(6) 0.088 Uiso 1 calc R . 
C5 C 0.8458(5) 0.6458(10) 0.5483(6) 0.034(2) Uani 1 d . . 
C6 C 0.9298(6) 0.6976(11) 0.6092(6) 0.048(2) Uani 1 d . . 
H6A H 0.9420(6) 0.8145(11) 0.6229(6) 0.058 Uiso 1 calc R . 
C7 C 0.9961(6) 0.5740(13) 0.6498(7) 0.057(2) Uani 1 d . . 
H7A H 1.0536(6) 0.6092(13) 0.6905(7) 0.069 Uiso 1 calc R . 
C8 C 0.9799(6) 0.4028(12) 0.6325(7) 0.055(2) Uani 1 d . . 
H8A H 1.0253(6) 0.3218(12) 0.6621(7) 0.066 Uiso 1 calc R . 
C9 C 0.8962(6) 0.3490(12) 0.5711(7) 0.058(2) Uani 1 d . . 
H9A H 0.8849(6) 0.2318(12) 0.5577(7) 0.069 Uiso 1 calc R . 
C10 C 0.8281(5) 0.4725(10) 0.5290(6) 0.044(2) Uani 1 d . . 
H10A H 0.7707(5) 0.4376(10) 0.4880(6) 0.052 Uiso 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 
Re 0.0292(2) 0.0347(2) 0.0325(2) -0.00282(15) 0.00381(11) 0.00235(13) 
Cl1 0.0474(11) 0.0516(12) 0.0413(12) 0.0005(10) -0.0021(9) 0.0057(9) 
Cl3 0.0391(10) 0.0485(13) 0.0577(14) -0.0023(10) 0.0103(9) -0.0090(9) 
Cl2 0.0492(12) 0.0590(14) 0.0552(14) 0.0013(11) 0.0117(10) -0.0165(10) 
O1 0.040(3) 0.048(4) 0.045(3) -0.010(3) 0.009(2) 0.010(2) 
N1 0.039(3) 0.029(3) 0.032(4) -0.001(3) 0.003(3) 0.003(3) 
N2 0.053(4) 0.032(4) 0.037(4) 0.002(3) 0.009(3) 0.010(3) 
N3 0.047(4) 0.033(4) 0.031(4) -0.007(3) 0.013(3) 0.005(3) 
N4 0.030(3) 0.040(4) 0.041(4) 0.000(3) 0.004(3) 0.006(3) 
C1 0.037(4) 0.043(5) 0.042(5) 0.010(4) 0.009(4) 0.016(3) 
C2 0.060(5) 0.038(5) 0.051(5) 0.008(4) 0.024(4) 0.017(4) 
C3 0.040(4) 0.029(4) 0.039(5) 0.000(3) 0.014(4) -0.001(3) 
C4 0.092(7) 0.042(5) 0.038(5) -0.012(4) 0.007(5) 0.014(5) 
C5 0.031(4) 0.038(4) 0.034(4) 0.002(3) 0.008(3) 0.006(3) 
C6 0.047(5) 0.052(5) 0.045(5) -0.006(4) 0.009(4) 0.018(4) 
C7 0.039(5) 0.078(7) 0.050(6) 0.005(5) -0.004(4) 0.019(5) 
C8 0.037(5) 0.063(7) 0.064(6) 0.019(5) 0.012(4) 0.025(4) 
C9 0.065(6) 0.050(5) 0.063(6) 0.015(5) 0.025(5) 0.020(5) 
C10 0.036(4) 0.046(5) 0.047(5) 0.009(4) 0.004(4) 0.002(4) 
  
_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 
Re O1 1.660(5) . y 
Re N4 2.086(6) . y 
Re N1 2.174(6) . y 
Re Cl1 2.307(2) . y 
Re Cl2 2.350(2) . y 
Re Cl3 2.359(2) . y 
N1 C3 1.311(9) . y 
N1 C1 1.367(9) . ? 
N2 C3 1.342(9) . ? 
N2 C2 1.366(10) . ? 
N2 C4 1.468(10) . ? 
N3 N4 1.280(8) . y 
N3 C3 1.365(9) . y 
N4 C5 1.437(9) . ? 
C1 C2 1.346(11) . ? 
C5 C6 1.368(11) . ? 
C5 C10 1.376(11) . ? 
C6 C7 1.375(11) . ? 
C7 C8 1.354(13) . ? 
C8 C9 1.371(12) . ? 
C9 C10 1.396(11) . ? 
  
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 
O1 Re N4 90.6(2) . . y 
O1 Re N1 162.4(2) . . y 
N4 Re N1 71.8(2) . . y 
O1 Re Cl1 107.8(2) . . y 
N4 Re Cl1 161.5(2) . . y 
N1 Re Cl1 89.8(2) . . y 
O1 Re Cl2 97.0(2) . . y 
N4 Re Cl2 88.7(2) . . y 
N1 Re Cl2 82.9(2) . . y 
Cl1 Re Cl2 87.75(8) . . y 
O1 Re Cl3 96.9(2) . . y 
N4 Re Cl3 92.7(2) . . y 
N1 Re Cl3 84.4(2) . . y 
Cl1 Re Cl3 86.47(8) . . y 
Cl2 Re Cl3 166.04(8) . . y 
C3 N1 C1 106.8(6) . . ? 
C3 N1 Re 111.9(5) . . y 
C1 N1 Re 141.1(5) . . ? 
C3 N2 C2 106.3(6) . . ? 
C3 N2 C4 125.9(7) . . ? 
C2 N2 C4 127.8(6) . . ? 
N4 N3 C3 109.3(6) . . y 
N3 N4 C5 113.4(6) . . ? 
N3 N4 Re 123.7(5) . . y 
C5 N4 Re 122.7(5) . . ? 
C2 C1 N1 108.2(7) . . ? 
C1 C2 N2 107.7(7) . . ? 
N1 C3 N2 111.1(6) . . ? 
N1 C3 N3 122.7(7) . . y 
N2 C3 N3 126.3(7) . . ? 
C6 C5 C10 120.1(7) . . ? 
C6 C5 N4 120.8(7) . . ? 
C10 C5 N4 119.1(7) . . ? 
C5 C6 C7 119.0(8) . . ? 
C8 C7 C6 121.9(8) . . ? 
C7 C8 C9 119.8(8) . . ? 
C8 C9 C10 119.1(9) . . ? 
C5 C10 C9 120.1(8) . . ? 
  
_refine_diff_density_max    1.126 
_refine_diff_density_min   -0.562 
_refine_diff_density_rms    0.135 
  
#END#*** 

data_[ReL2(NC6H4Me)Cl3],3a 
  
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C21 H22 Cl3 N5 Re' 
_chemical_formula_weight          636.99 
_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' 
 '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    Pbcn 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, -y+1/2, z+1/2' 
 '-x, y, -z+1/2' 
 'x+1/2, -y+1/2, -z' 
 '-x, -y, -z' 
 'x-1/2, y-1/2, -z-1/2' 
 'x, -y, z-1/2' 
 '-x-1/2, y-1/2, z' 
  
_cell_length_a                    28.204(6) 
_cell_length_b                    11.364(2) 
_cell_length_c                    14.954(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      4792.8(17) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     30 
_cell_measurement_theta_min       7 
_cell_measurement_theta_max       14 
  
_exptl_crystal_description        parallelopiped 
_exptl_crystal_colour             dark 
_exptl_crystal_size_max           0.42 
_exptl_crystal_size_mid           0.28 
_exptl_crystal_size_min           0.26 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.766 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              2472 
_exptl_absorpt_coefficient_mu     5.423 
_exptl_absorpt_correction_type    'semi-empirical' 
_exptl_absorpt_correction_T_min   0.057 
_exptl_absorpt_correction_T_max   0.101 
  
_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_type   'Siemens R3m/V' 
_diffrn_measurement_method        '\w scans' 
_diffrn_standards_number          2 
_diffrn_standards_interval_count  198 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         nil 
_diffrn_reflns_number             3613 
_diffrn_reflns_av_R_equivalents   0.0528 
_diffrn_reflns_av_sigmaI/netI     0.0512 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        31 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -6 
_diffrn_reflns_limit_l_max        16 
_diffrn_reflns_theta_min          1.93 
_diffrn_reflns_theta_max          23.55 
_reflns_number_total              3539 
_reflns_number_observed           2274 
_reflns_observed_criterion        >2sigma(I) 
  
_computing_data_collection        'Siemens P3' 
_computing_cell_refinement        'Siemens P3' 
_computing_data_reduction         'Siemens P3' 
_computing_structure_solution     'Siemens SHELXTL V-5.03 (Sheldrick, 1994)' 
_computing_structure_refinement   'Siemens SHELXTL V-5.03 (Sheldrick, 1994)'  
_computing_molecular_graphics     'Siemens SHELXTL V-5.03 (Sheldrick, 1994)'  
_computing_publication_material   'Siemens SHELXTL V-5.03 (Sheldrick, 1994)'  
  
_refine_special_details 
; 
 Refinement on F^2^ for ALL reflections except for 5 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^)+(0.0522P)^2^+11.6616P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      'Heavy atom method' 
_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_number_reflns          3534 
_refine_ls_number_parameters      271 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0852 
_refine_ls_R_factor_obs           0.0434 
_refine_ls_wR_factor_all          0.1192 
_refine_ls_wR_factor_obs          0.0948 
_refine_ls_goodness_of_fit_all    1.038 
_refine_ls_goodness_of_fit_obs    1.101 
_refine_ls_restrained_S_all       1.087 
_refine_ls_restrained_S_obs       1.101 
_refine_ls_shift/su_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 
Re Re 0.124554(15) 0.08927(4) 0.15096(3) 0.0449(2) Uani 1 d . . 
Cl1 Cl 0.08747(11) 0.0094(4) 0.2774(2) 0.0809(11) Uani 1 d . . 
Cl2 Cl 0.10742(11) 0.2773(3) 0.2117(2) 0.0708(9) Uani 1 d . . 
Cl3 Cl 0.12322(11) -0.1045(3) 0.0916(2) 0.0690(8) Uani 1 d . . 
N1 N 0.0570(3) 0.1135(7) 0.0885(5) 0.041(2) Uani 1 d . . 
N4 N 0.1381(3) 0.1493(7) 0.0261(5) 0.042(2) Uani 1 d . . 
N3 N 0.1048(3) 0.1702(7) -0.0337(5) 0.040(2) Uani 1 d . . 
N2 N 0.0192(3) 0.1709(8) -0.0331(6) 0.050(2) Uani 1 d . . 
N5 N 0.1834(3) 0.0909(9) 0.1820(6) 0.053(2) Uani 1 d . . 
C1 C 0.0096(4) 0.1066(10) 0.1054(8) 0.053(3) Uani 1 d . . 
H1A H -0.0043(4) 0.0808(10) 0.1583(8) 0.064 Uiso 1 calc R . 
C2 C -0.0133(4) 0.1439(10) 0.0318(8) 0.053(3) Uani 1 d . . 
H2A H -0.0461(4) 0.1503(10) 0.0259(8) 0.064 Uiso 1 calc R . 
C3 C 0.0617(3) 0.1519(9) 0.0042(7) 0.041(3) Uani 1 d . . 
C4 C 0.0092(4) 0.2149(11) -0.1217(7) 0.065(3) Uani 1 d . . 
H4A H -0.0245(4) 0.2195(11) -0.1302(7) 0.097 Uiso 1 calc R . 
H4B H 0.0226(4) 0.1626(11) -0.1654(7) 0.097 Uiso 1 calc R . 
H4C H 0.0229(4) 0.2917(11) -0.1285(7) 0.097 Uiso 1 calc R . 
C5 C 0.1854(4) 0.1560(11) -0.0079(7) 0.045(3) Uani 1 d . . 
C6 C 0.2034(4) 0.0652(10) -0.0589(7) 0.055(3) Uani 1 d . . 
H6A H 0.1834(4) 0.0053(10) -0.0785(7) 0.065 Uiso 1 calc R . 
C7 C 0.2507(4) 0.0627(11) -0.0810(7) 0.057(3) Uani 1 d . . 
H7A H 0.2625(4) 0.0005(11) -0.1147(7) 0.069 Uiso 1 calc R . 
C8 C 0.2808(4) 0.1512(11) -0.0539(8) 0.054(3) Uani 1 d . . 
C9 C 0.2626(4) 0.2431(11) -0.0049(7) 0.058(3) Uani 1 d . . 
H9A H 0.2824(4) 0.3044(11) 0.0124(7) 0.070 Uiso 1 calc R . 
C10 C 0.2146(3) 0.2457(10) 0.0194(7) 0.051(3) Uani 1 d . . 
H10A H 0.2028(3) 0.3074(10) 0.0536(7) 0.061 Uiso 1 calc R . 
C11 C 0.3331(4) 0.1436(14) -0.0745(9) 0.084(5) Uani 1 d . . 
H11A H 0.3393(4) 0.0741(14) -0.1091(9) 0.126 Uiso 1 calc R . 
H11B H 0.3507(4) 0.1402(14) -0.0196(9) 0.126 Uiso 1 calc R . 
H11C H 0.3426(4) 0.2118(14) -0.1079(9) 0.126 Uiso 1 calc R . 
C12 C 0.2313(4) 0.1022(10) 0.1975(7) 0.043(3) Uani 1 d . . 
C13 C 0.2616(4) 0.0142(11) 0.1702(8) 0.058(3) Uani 1 d . . 
H13A H 0.2501(4) -0.0520(11) 0.1407(8) 0.070 Uiso 1 calc R . 
C14 C 0.3098(4) 0.0268(11) 0.1879(8) 0.060(3) Uani 1 d . . 
H14A H 0.3307(4) -0.0318(11) 0.1699(8) 0.073 Uiso 1 calc R . 
C15 C 0.3269(4) 0.1227(10) 0.2309(8) 0.053(3) Uani 1 d . . 
C16 C 0.2968(4) 0.2089(11) 0.2576(8) 0.066(3) Uani 1 d . . 
H16A H 0.3085(4) 0.2749(11) 0.2870(8) 0.080 Uiso 1 calc R . 
C17 C 0.2485(4) 0.1992(10) 0.2412(8) 0.054(3) Uani 1 d . . 
H17A H 0.2279(4) 0.2582(10) 0.2599(8) 0.065 Uiso 1 calc R . 
C18 C 0.3813(4) 0.1339(13) 0.2489(11) 0.088(4) Uani 1 d . . 
H18A H 0.3876(4) 0.2064(13) 0.2798(11) 0.131 Uiso 1 calc R . 
H18B H 0.3981(4) 0.1333(13) 0.1931(11) 0.131 Uiso 1 calc R . 
H18C H 0.3917(4) 0.0690(13) 0.2850(11) 0.131 Uiso 1 calc R . 
C19 C -0.0365(8) 0.4567(18) 0.0589(18) 0.128(7) Uani 1 d . . 
H19A H -0.0553(8) 0.4218(18) 0.1053(18) 0.153 Uiso 1 d R . 
C20 C 0.0120(10) 0.4398(15) 0.0758(20) 0.155(11) Uani 1 d . . 
H20A H 0.0210(10) 0.3983(15) 0.1266(20) 0.187 Uiso 1 calc R . 
C21 C 0.0477(7) 0.4833(19) 0.0183(21) 0.136(9) Uani 1 d . . 
H21A H 0.0785(7) 0.4626(19) 0.0409(21) 0.163 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 
Re 0.0279(2) 0.0606(3) 0.0462(3) 0.0072(2) 0.0012(2) 0.0002(2) 
Cl1 0.053(2) 0.117(3) 0.073(2) 0.038(2) 0.019(2) 0.008(2) 
Cl2 0.058(2) 0.079(2) 0.075(2) -0.021(2) -0.008(2) 0.003(2) 
Cl3 0.050(2) 0.056(2) 0.102(2) -0.001(2) 0.002(2) 0.000(2) 
N1 0.030(5) 0.051(6) 0.041(5) 0.002(4) 0.000(4) -0.005(4) 
N4 0.041(5) 0.045(5) 0.041(5) 0.001(4) 0.002(4) -0.010(4) 
N3 0.026(4) 0.053(5) 0.041(5) 0.000(4) -0.008(4) 0.004(4) 
N2 0.037(5) 0.050(6) 0.065(6) 0.000(5) -0.010(5) 0.005(5) 
N5 0.037(5) 0.085(7) 0.039(5) 0.009(5) 0.001(4) 0.008(5) 
C1 0.027(6) 0.066(8) 0.067(8) 0.008(7) 0.004(6) -0.012(6) 
C2 0.026(6) 0.060(8) 0.075(8) -0.006(7) -0.008(6) -0.003(5) 
C3 0.029(6) 0.037(6) 0.056(7) -0.011(5) -0.006(5) -0.003(5) 
C4 0.047(7) 0.075(8) 0.073(8) 0.009(7) -0.015(6) -0.004(7) 
C5 0.034(6) 0.062(8) 0.038(6) 0.016(6) -0.002(5) -0.001(6) 
C6 0.049(7) 0.058(8) 0.056(7) -0.008(6) 0.004(6) -0.010(6) 
C7 0.048(7) 0.068(9) 0.056(7) -0.007(6) 0.028(6) 0.013(7) 
C8 0.028(6) 0.073(8) 0.062(8) 0.011(7) 0.008(6) -0.002(6) 
C9 0.044(8) 0.069(9) 0.061(8) 0.001(7) 0.002(5) -0.014(6) 
C10 0.030(6) 0.060(8) 0.062(7) -0.004(6) 0.005(5) -0.006(6) 
C11 0.031(6) 0.138(13) 0.083(10) -0.006(9) 0.017(6) -0.004(8) 
C12 0.038(6) 0.051(7) 0.039(6) 0.002(6) 0.003(5) 0.005(6) 
C13 0.043(7) 0.056(8) 0.076(8) -0.017(7) -0.004(6) 0.005(6) 
C14 0.035(6) 0.059(8) 0.087(9) -0.006(7) -0.009(6) 0.012(6) 
C15 0.035(6) 0.060(8) 0.064(8) 0.010(6) -0.008(6) -0.006(6) 
C16 0.056(8) 0.068(9) 0.076(9) -0.012(7) -0.005(7) 0.000(7) 
C17 0.042(7) 0.048(7) 0.071(8) -0.016(6) -0.003(6) 0.006(6) 
C18 0.042(8) 0.100(10) 0.120(12) 0.010(10) -0.013(8) -0.017(8) 
C19 0.110(18) 0.107(16) 0.166(21) -0.006(15) -0.003(16) -0.007(13) 
C20 0.117(17) 0.074(13) 0.275(33) -0.014(16) -0.097(22) -0.017(13) 
C21 0.083(14) 0.080(14) 0.243(31) -0.031(17) -0.058(18) -0.004(12) 
  
_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 
Re N5 1.723(9) . y 
Re N4 2.024(8) . y 
Re N1 2.140(8) . y 
Re Cl1 2.344(3) . y 
Re Cl2 2.371(3) . y 
Re Cl3 2.374(3) . y 
N1 C3 1.341(12) . y 
N1 C1 1.362(12) . ? 
N4 N3 1.319(10) . y 
N4 C5 1.429(12) . ? 
N3 C3 1.357(12) . y 
N2 C3 1.339(12) . ? 
N2 C2 1.370(13) . ? 
N2 C4 1.443(13) . ? 
N5 C12 1.377(13) . y 
C1 C2 1.346(15) . ? 
C5 C10 1.373(14) . ? 
C5 C6 1.381(15) . ? 
C6 C7 1.375(15) . ? 
C7 C8 1.38(2) . ? 
C8 C9 1.38(2) . ? 
C8 C11 1.509(14) . ? 
C9 C10 1.400(14) . ? 
C12 C17 1.369(14) . ? 
C12 C13 1.378(14) . ? 
C13 C14 1.392(15) . ? 
C14 C15 1.35(2) . ? 
C15 C16 1.36(2) . ? 
C15 C18 1.564(14) . ? 
C16 C17 1.388(15) . ? 
C19 C21 1.38(3) 5_565 ? 
C19 C20 1.40(2) . ? 
C20 C21 1.41(3) . ? 
C21 C19 1.38(3) 5_565 ? 
  
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 
N5 Re N4 93.7(4) . . y 
N5 Re N1 166.9(4) . . y 
N4 Re N1 73.9(3) . . y 
N5 Re Cl1 102.5(3) . . y 
N4 Re Cl1 163.5(2) . . y 
N1 Re Cl1 90.3(2) . . y 
N5 Re Cl2 94.8(3) . . y 
N4 Re Cl2 95.0(3) . . y 
N1 Re Cl2 82.5(2) . . y 
Cl1 Re Cl2 87.09(14) . . y 
N5 Re Cl3 97.2(3) . . y 
N4 Re Cl3 88.3(3) . . y 
N1 Re Cl3 86.7(2) . . y 
Cl1 Re Cl3 86.29(14) . . y 
Cl2 Re Cl3 167.28(11) . . y 
C3 N1 C1 106.9(9) . . ? 
C3 N1 Re 111.4(6) . . y 
C1 N1 Re 141.7(8) . . ? 
N3 N4 C5 114.5(8) . . y 
N3 N4 Re 123.5(6) . . y 
C5 N4 Re 121.5(6) . . ? 
N4 N3 C3 109.1(8) . . y 
C3 N2 C2 105.5(9) . . ? 
C3 N2 C4 127.7(10) . . ? 
C2 N2 C4 126.7(9) . . ? 
C12 N5 Re 172.4(8) . . y 
C2 C1 N1 107.6(10) . . ? 
C1 C2 N2 109.2(9) . . ? 
N2 C3 N1 110.9(9) . . ? 
N2 C3 N3 127.1(10) . . ? 
N1 C3 N3 122.0(9) . . y 
C10 C5 C6 119.9(10) . . ? 
C10 C5 N4 119.7(10) . . ? 
C6 C5 N4 120.0(10) . . ? 
C7 C6 C5 120.3(11) . . ? 
C6 C7 C8 120.8(11) . . ? 
C9 C8 C7 118.7(10) . . ? 
C9 C8 C11 121.1(12) . . ? 
C7 C8 C11 120.1(12) . . ? 
C8 C9 C10 121.0(11) . . ? 
C5 C10 C9 119.2(11) . . ? 
C17 C12 N5 120.2(10) . . ? 
C17 C12 C13 120.4(10) . . ? 
N5 C12 C13 119.4(10) . . ? 
C12 C13 C14 118.3(11) . . ? 
C15 C14 C13 121.4(11) . . ? 
C14 C15 C16 119.8(11) . . ? 
C14 C15 C18 119.8(11) . . ? 
C16 C15 C18 120.4(12) . . ? 
C15 C16 C17 120.3(12) . . ? 
C12 C17 C16 119.7(11) . . ? 
C21 C19 C20 116.3(22) 5_565 . ? 
C19 C20 C21 122.5(23) . . ? 
C19 C21 C20 121.3(20) 5_565 . ? 
  
_refine_diff_density_max    0.769 
_refine_diff_density_min   -0.687 
_refine_diff_density_rms    0.129 
  
#END#....... 

data_[ReL3(OPPh3)Cl3],4c 
  
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C28 H24 Cl4 N4 O P Re' 
_chemical_formula_weight          791.48 
_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' 
 'P'  'P'   0.1023   0.0942 
 '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            Monoclinic 
_symmetry_space_group_name_H-M    P2(1)/n 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y-1/2, z-1/2' 
  
_cell_length_a                    11.588(6) 
_cell_length_b                    15.007(5) 
_cell_length_c                    17.661(8) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  96.52(4) 
_cell_angle_gamma                 90.00 
_cell_volume                      3051.5(23) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     30 
_cell_measurement_theta_min       7 
_cell_measurement_theta_max       14 
  
_exptl_crystal_description        parallelopiped 
_exptl_crystal_colour             dark 
_exptl_crystal_size_max           0.4 
_exptl_crystal_size_mid           0.3 
_exptl_crystal_size_min           0.15 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.723 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1544 
_exptl_absorpt_coefficient_mu     4.414 
_exptl_absorpt_correction_type    'semi-empirical' 
_exptl_absorpt_correction_T_min   0.127 
_exptl_absorpt_correction_T_max   0.213 
  
_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_type   'Siemens R3m/V' 
_diffrn_measurement_method        '\w scans' 
_diffrn_standards_number          2 
_diffrn_standards_interval_count  198 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         nil 
_diffrn_reflns_number             5194 
_diffrn_reflns_av_R_equivalents   0.0962 
_diffrn_reflns_av_sigmaI/netI     0.0880 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        17 
_diffrn_reflns_limit_l_min        -20 
_diffrn_reflns_limit_l_max        20 
_diffrn_reflns_theta_min          1.79 
_diffrn_reflns_theta_max          24.00 
_reflns_number_total              4774 
_reflns_number_observed           2611 
_reflns_observed_criterion        >2sigma(I) 
  
_computing_data_collection        'Siemens P3/P4 PC V-4.27' 
_computing_cell_refinement        'Siemens P3/P4 PC V-4.27' 
_computing_data_reduction         'Siemens P3/P4 PC V-4.27' 
_computing_structure_solution     'Siemens SHELXTL V-5.03 (Sheldrick, 1994)' 
_computing_structure_refinement   'Siemens SHELXTL V-5.03 (Sheldrick, 1994)' 
_computing_molecular_graphics     'Siemens SHELXTL V-5.03 (Sheldrick, 1994)' 
_computing_publication_material   'Siemens SHELXTL V-5.03 (Sheldrick, 1994)' 
  
_refine_special_details 
; 
 Refinement on F^2^ for ALL reflections except for 1 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^)+(0.1059P)^2^+8.9067P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      'Heavey atom method'
_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_number_reflns          4773 
_refine_ls_number_parameters      352 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1354 
_refine_ls_R_factor_obs           0.0658 
_refine_ls_wR_factor_all          0.2205 
_refine_ls_wR_factor_obs          0.1582 
_refine_ls_goodness_of_fit_all    1.113 
_refine_ls_goodness_of_fit_obs    1.117 
_refine_ls_restrained_S_all       1.126 
_refine_ls_restrained_S_obs       1.117 
_refine_ls_shift/su_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 
Re Re 0.88690(6) 0.74820(6) 0.55420(3) 0.0420(3) Uani 1 d . . 
Cl1 Cl 0.6972(5) 0.7956(4) 0.5074(3) 0.080(2) Uani 1 d . . 
Cl2 Cl 0.8855(7) 0.6463(4) 0.4541(3) 0.095(2) Uani 1 d . . 
Cl3 Cl 0.8792(4) 0.8433(3) 0.6601(3) 0.0567(12) Uani 1 d . . 
P1 P 0.7590(4) 0.6035(3) 0.6733(3) 0.0460(12) Uani 1 d . . 
O1 O 0.8279(10) 0.6472(8) 0.6168(7) 0.049(3) Uani 1 d . . 
N1 N 0.9608(13) 0.8403(10) 0.4936(8) 0.049(4) Uani 1 d . . 
N3 N 1.1371(14) 0.7882(10) 0.5602(8) 0.050(4) Uani 1 d . . 
N4 N 1.0557(13) 0.7328(10) 0.5828(10) 0.057(4) Uani 1 d . . 
N2 N 1.1187(17) 0.9083(11) 0.4667(9) 0.065(5) Uani 1 d . . 
C1 C 0.9320(18) 0.9037(13) 0.4395(9) 0.055(5) Uani 1 d . . 
H1A H 0.8570(18) 0.9179(13) 0.4185(9) 0.066 Uiso 1 calc R . 
C2 C 1.0289(21) 0.9420(14) 0.4216(11) 0.066(6) Uani 1 d . . 
H2A H 1.0333(21) 0.9848(14) 0.3840(11) 0.080 Uiso 1 calc R . 
C3 C 1.0769(19) 0.8444(12) 0.5111(11) 0.058(5) Uani 1 d . . 
C4 C 1.2406(21) 0.9329(17) 0.4681(16) 0.102(9) Uani 1 d . . 
H4A H 1.2865(21) 0.8982(17) 0.5061(16) 0.153 Uiso 1 calc R . 
H4B H 1.2498(21) 0.9951(17) 0.4802(16) 0.153 Uiso 1 calc R . 
H4C H 1.2658(21) 0.9218(17) 0.4191(16) 0.153 Uiso 1 calc R . 
C5 C 1.1073(16) 0.6678(12) 0.6367(11) 0.052(5) Uani 1 d . . 
C6 C 1.0836(20) 0.5804(13) 0.6250(11) 0.068(6) Uani 1 d . . 
H6A H 1.0321(20) 0.5617(13) 0.5839(11) 0.081 Uiso 1 calc R . 
C7 C 1.1379(21) 0.5196(14) 0.6758(13) 0.072(6) Uani 1 d . . 
H7A H 1.1180(21) 0.4598(14) 0.6700(13) 0.087 Uiso 1 calc R . 
C8 C 1.2184(18) 0.5433(13) 0.7334(13) 0.066(6) Uani 1 d . . 
C9 C 1.2385(21) 0.6340(15) 0.7479(13) 0.081(7) Uani 1 d . . 
H9A H 1.2874(21) 0.6525(15) 0.7904(13) 0.097 Uiso 1 calc R . 
C10 C 1.1846(16) 0.6945(13) 0.6984(11) 0.057(5) Uani 1 d . . 
H10A H 1.2000(16) 0.7548(13) 0.7060(11) 0.068 Uiso 1 calc R . 
C11 C 0.6916(19) 0.5047(13) 0.6306(10) 0.063(6) Uani 1 d . . 
C12 C 0.5939(21) 0.4669(16) 0.6577(13) 0.084(8) Uani 1 d . . 
H12A H 0.5621(21) 0.4929(16) 0.6984(13) 0.101 Uiso 1 calc R . 
C13 C 0.5450(26) 0.3915(21) 0.6243(16) 0.117(12) Uani 1 d . . 
H13A H 0.4811(26) 0.3657(21) 0.6430(16) 0.141 Uiso 1 calc R . 
C14 C 0.5896(35) 0.3544(21) 0.5637(20) 0.135(13) Uani 1 d . . 
H14A H 0.5537(35) 0.3054(21) 0.5388(20) 0.162 Uiso 1 calc R . 
C15 C 0.6913(32) 0.3914(21) 0.5393(16) 0.134(13) Uani 1 d . . 
H15A H 0.7284(32) 0.3625(21) 0.5023(16) 0.160 Uiso 1 calc R . 
C16 C 0.7342(23) 0.4677(15) 0.5693(12) 0.092(9) Uani 1 d . . 
H16A H 0.7942(23) 0.4959(15) 0.5480(12) 0.110 Uiso 1 calc R . 
C17 C 0.8540(15) 0.5734(12) 0.7558(10) 0.048(5) Uani 1 d . . 
C18 C 0.8533(18) 0.4921(13) 0.7905(12) 0.062(5) Uani 1 d . . 
H18A H 0.8001(18) 0.4490(13) 0.7713(12) 0.074 Uiso 1 calc R . 
C19 C 0.9317(22) 0.4730(17) 0.8546(13) 0.078(8) Uani 1 d . . 
H19A H 0.9350(22) 0.4167(17) 0.8767(13) 0.094 Uiso 1 calc R . 
C20 C 1.0036(23) 0.5402(22) 0.8838(14) 0.094(9) Uani 1 d . . 
H20A H 1.0541(23) 0.5288(22) 0.9274(14) 0.113 Uiso 1 calc R . 
C21 C 1.0047(18) 0.6209(16) 0.8528(12) 0.067(6) Uani 1 d . . 
H21A H 1.0548(18) 0.6653(16) 0.8733(12) 0.081 Uiso 1 calc R . 
C22 C 0.9267(18) 0.6354(14) 0.7878(10) 0.063(6) Uani 1 d . . 
H22A H 0.9253(18) 0.6915(14) 0.7654(10) 0.075 Uiso 1 calc R . 
C23 C 0.6465(16) 0.6750(14) 0.7026(10) 0.057(5) Uani 1 d . . 
C24 C 0.5529(18) 0.6944(16) 0.6501(12) 0.068(6) Uani 1 d . . 
H24A H 0.5489(18) 0.6708(16) 0.6012(12) 0.082 Uiso 1 calc R . 
C25 C 0.4655(19) 0.7482(19) 0.6697(17) 0.091(8) Uani 1 d . . 
H25A H 0.4029(19) 0.7625(19) 0.6341(17) 0.109 Uiso 1 calc R . 
C26 C 0.4716(23) 0.7796(18) 0.7401(20) 0.096(9) Uani 1 d . . 
H26A H 0.4112(23) 0.8148(18) 0.7537(20) 0.115 Uiso 1 calc R . 
C27 C 0.5608(23) 0.7626(18) 0.7920(16) 0.091(8) Uani 1 d . . 
H27A H 0.5632(23) 0.7874(18) 0.8404(16) 0.110 Uiso 1 calc R . 
C28 C 0.6507(18) 0.7078(15) 0.7743(12) 0.066(6) Uani 1 d . . 
H28A H 0.7124(18) 0.6940(15) 0.8109(12) 0.079 Uiso 1 calc R . 
Cl4 Cl 1.2837(7) 0.4643(4) 0.7947(4) 0.102(2) Uani 1 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_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
Re 0.0528(4) 0.0374(4) 0.0356(4) 0.0004(4) 0.0032(2) -0.0098(4) 
Cl1 0.065(3) 0.084(4) 0.084(4) 0.028(3) -0.021(3) -0.013(3) 
Cl2 0.166(7) 0.068(4) 0.053(3) -0.021(3) 0.025(4) -0.038(4) 
Cl3 0.075(3) 0.042(3) 0.053(3) -0.008(2) 0.009(2) 0.001(2) 
P1 0.051(3) 0.041(3) 0.045(3) 0.003(2) 0.002(2) -0.012(2) 
O1 0.051(7) 0.044(7) 0.053(7) -0.001(6) 0.008(6) -0.012(6) 
N1 0.063(10) 0.047(9) 0.038(8) 0.011(7) 0.004(7) -0.009(8) 
N3 0.065(10) 0.041(8) 0.045(8) 0.021(7) 0.010(7) -0.008(8) 
N4 0.047(9) 0.048(11) 0.079(11) -0.017(9) 0.021(8) 0.003(7) 
N2 0.094(14) 0.050(10) 0.055(10) -0.010(9) 0.024(10) -0.011(10) 
C1 0.072(14) 0.055(13) 0.033(10) 0.003(9) -0.010(9) 0.000(11) 
C2 0.095(18) 0.053(13) 0.053(12) 0.004(10) 0.013(12) -0.034(13) 
C3 0.084(15) 0.035(11) 0.059(12) -0.018(10) 0.026(11) -0.028(11) 
C4 0.089(19) 0.085(19) 0.141(24) 0.003(18) 0.053(18) -0.033(16) 
C5 0.059(12) 0.039(11) 0.062(12) 0.007(9) 0.025(10) 0.014(9) 
C6 0.106(18) 0.039(12) 0.054(12) -0.007(10) -0.007(11) -0.015(12) 
C7 0.098(18) 0.037(12) 0.081(16) -0.003(11) 0.005(14) 0.005(12) 
C8 0.060(14) 0.039(12) 0.096(17) -0.016(12) -0.011(12) 0.004(10) 
C9 0.098(18) 0.065(15) 0.073(14) 0.006(12) -0.023(13) -0.020(14) 
C10 0.063(13) 0.039(12) 0.062(12) 0.000(9) -0.027(10) -0.022(9) 
C11 0.091(16) 0.055(13) 0.038(10) 0.000(10) -0.011(10) -0.033(12) 
C12 0.098(18) 0.074(17) 0.075(16) 0.005(13) -0.005(13) -0.057(15) 
C13 0.130(25) 0.126(25) 0.095(20) 0.012(18) 0.006(18) -0.115(22) 
C14 0.206(41) 0.081(22) 0.116(26) -0.026(20) 0.008(26) -0.056(24) 
C15 0.208(37) 0.116(25) 0.079(19) -0.047(18) 0.018(21) -0.085(26) 
C16 0.139(23) 0.074(16) 0.064(14) -0.033(13) 0.022(14) -0.074(16) 
C17 0.044(11) 0.046(12) 0.056(11) 0.003(9) 0.014(9) 0.007(9) 
C18 0.069(14) 0.046(12) 0.072(14) 0.002(11) 0.013(11) -0.005(10) 
C19 0.104(20) 0.074(17) 0.063(14) 0.037(13) 0.038(14) 0.054(15) 
C20 0.094(20) 0.114(25) 0.067(16) -0.008(17) -0.025(14) 0.042(18) 
C21 0.058(13) 0.071(16) 0.069(14) -0.022(12) -0.012(11) -0.001(12) 
C22 0.091(15) 0.056(13) 0.036(10) -0.003(9) -0.011(10) -0.017(12) 
C23 0.056(12) 0.082(15) 0.036(10) -0.004(10) 0.020(9) -0.019(11) 
C24 0.054(13) 0.087(17) 0.058(13) -0.002(12) -0.021(10) -0.023(12) 
C25 0.054(13) 0.107(21) 0.115(21) 0.037(20) 0.026(13) 0.023(16) 
C26 0.067(18) 0.087(20) 0.141(27) 0.011(19) 0.042(19) 0.015(14) 
C27 0.078(17) 0.109(23) 0.092(18) -0.015(17) 0.031(15) 0.013(17) 
C28 0.057(13) 0.071(14) 0.068(14) -0.010(12) -0.001(10) -0.010(11) 
Cl4 0.127(6) 0.056(4) 0.109(5) 0.003(4) -0.041(4) 0.016(4) 
  
_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 
Re N4 1.978(15) . y 
Re N1 1.999(14) . y 
Re O1 2.039(11) . y 
Re Cl2 2.336(6) . y 
Re Cl3 2.363(5) . y 
Re Cl1 2.369(6) . y 
P1 O1 1.498(12) . y 
P1 C17 1.78(2) . ? 
P1 C11 1.80(2) . ? 
P1 C23 1.81(2) . ? 
N1 C3 1.35(2) . y 
N1 C1 1.36(2) . ? 
N3 C3 1.35(2) . y 
N3 N4 1.351(20) . y 
N4 C5 1.44(2) . ? 
N2 C2 1.34(3) . ? 
N2 C3 1.36(2) . ? 
N2 C4 1.46(3) . ? 
C1 C2 1.33(3) . ? 
C5 C6 1.35(2) . ? 
C5 C10 1.39(2) . ? 
C6 C7 1.38(3) . ? 
C7 C8 1.35(3) . ? 
C8 C9 1.40(3) . ? 
C8 Cl4 1.72(2) . ? 
C9 C10 1.36(3) . ? 
C11 C16 1.36(3) . ? 
C11 C12 1.40(3) . ? 
C12 C13 1.37(3) . ? 
C13 C14 1.36(4) . ? 
C14 C15 1.41(4) . ? 
C15 C16 1.33(3) . ? 
C17 C22 1.34(2) . ? 
C17 C18 1.37(3) . ? 
C18 C19 1.40(3) . ? 
C19 C20 1.37(3) . ? 
C20 C21 1.33(3) . ? 
C21 C22 1.40(3) . ? 
C23 C28 1.35(3) . ? 
C23 C24 1.38(3) . ? 
C24 C25 1.37(3) . ? 
C25 C26 1.32(4) . ? 
C26 C27 1.33(4) . ? 
C27 C28 1.39(3) . ? 
  
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 
N4 Re N1 75.3(6) . . y 
N4 Re O1 99.0(6) . . y 
N1 Re O1 173.9(5) . . y 
N4 Re Cl2 92.2(5) . . y 
N1 Re Cl2 90.8(5) . . y 
O1 Re Cl2 87.1(4) . . y 
N4 Re Cl3 89.7(4) . . y 
N1 Re Cl3 93.6(4) . . y 
O1 Re Cl3 88.6(4) . . y 
Cl2 Re Cl3 175.5(2) . . y 
N4 Re Cl1 167.5(5) . . y 
N1 Re Cl1 92.4(5) . . y 
O1 Re Cl1 93.3(4) . . y 
Cl2 Re Cl1 90.4(3) . . y 
Cl3 Re Cl1 88.7(2) . . y 
O1 P1 C17 109.2(8) . . ? 
O1 P1 C11 108.7(8) . . ? 
C17 P1 C11 109.4(9) . . ? 
O1 P1 C23 112.8(8) . . ? 
C17 P1 C23 108.3(8) . . ? 
C11 P1 C23 108.4(10) . . ? 
P1 O1 Re 157.4(8) . . y 
C3 N1 C1 106.6(16) . . ? 
C3 N1 Re 112.8(12) . . y 
C1 N1 Re 140.6(14) . . ? 
C3 N3 N4 104.4(15) . . y 
N3 N4 C5 111.1(15) . . ? 
N3 N4 Re 123.7(13) . . y 
C5 N4 Re 124.8(12) . . ? 
C2 N2 C3 107.8(18) . . ? 
C2 N2 C4 127.0(19) . . ? 
C3 N2 C4 125.2(21) . . ? 
C2 C1 N1 108.8(18) . . ? 
C1 C2 N2 108.4(19) . . ? 
N1 C3 N3 123.3(16) . . y 
N1 C3 N2 108.2(19) . . ? 
N3 C3 N2 128.3(20) . . ? 
C6 C5 C10 120.1(18) . . ? 
C6 C5 N4 119.5(19) . . ? 
C10 C5 N4 120.4(17) . . ? 
C5 C6 C7 118.2(20) . . ? 
C8 C7 C6 122.8(20) . . ? 
C7 C8 C9 118.7(21) . . ? 
C7 C8 Cl4 120.7(16) . . ? 
C9 C8 Cl4 120.2(18) . . ? 
C10 C9 C8 118.4(20) . . ? 
C9 C10 C5 121.3(18) . . ? 
C16 C11 C12 119.2(19) . . ? 
C16 C11 P1 119.4(16) . . ? 
C12 C11 P1 121.4(17) . . ? 
C13 C12 C11 119.9(25) . . ? 
C14 C13 C12 120.2(25) . . ? 
C13 C14 C15 118.9(27) . . ? 
C16 C15 C14 120.1(30) . . ? 
C15 C16 C11 121.0(24) . . ? 
C22 C17 C18 117.9(19) . . ? 
C22 C17 P1 118.1(15) . . ? 
C18 C17 P1 124.0(16) . . ? 
C17 C18 C19 120.6(21) . . ? 
C20 C19 C18 117.7(21) . . ? 
C21 C20 C19 123.3(22) . . ? 
C20 C21 C22 116.4(22) . . ? 
C17 C22 C21 123.9(20) . . ? 
C28 C23 C24 119.7(20) . . ? 
C28 C23 P1 122.2(16) . . ? 
C24 C23 P1 118.1(15) . . ? 
C25 C24 C23 120.3(22) . . ? 
C26 C25 C24 118.9(25) . . ? 
C25 C26 C27 122.4(25) . . ? 
C26 C27 C28 120.2(24) . . ? 
C23 C28 C27 118.5(21) . . ? 
  
_refine_diff_density_max    1.624 
_refine_diff_density_min   -1.292 
_refine_diff_density_rms    0.209 
  
#END#...... 

data_[ReL3(PPh3)Cl3],5c 
  
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C28 H24 Cl4 N4 P Re' 
_chemical_formula_weight          775.48 
_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' 
 'P'  'P'   0.1023   0.0942 
 '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            Monoclinic 
_symmetry_space_group_name_H-M    P2(1)/n 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y-1/2, z-1/2' 
  
_cell_length_a                    9.785(2) 
_cell_length_b                    21.183(8) 
_cell_length_c                    14.937(5) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  109.00(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      2927.3(16) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     30 
_cell_measurement_theta_min       7 
_cell_measurement_theta_max       14 
  
_exptl_crystal_description        Parallelopiped 
_exptl_crystal_colour             orange 
_exptl_crystal_size_max           0.4 
_exptl_crystal_size_mid           0.3 
_exptl_crystal_size_min           0.16 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.760 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1512 
_exptl_absorpt_coefficient_mu     4.596 
_exptl_absorpt_correction_type    'psi-scan' 
_exptl_absorpt_correction_T_min   0.2194 
_exptl_absorpt_correction_T_max   0.5389 
  
_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_type   'Siemens R3m/V' 
_diffrn_measurement_method        '\w scans' 
_diffrn_standards_number          2 
_diffrn_standards_interval_count  198 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         nil 
_diffrn_reflns_number             5561 
_diffrn_reflns_av_R_equivalents   0.0372 
_diffrn_reflns_av_sigmaI/netI     0.0545 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        11 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        25 
_diffrn_reflns_limit_l_min        -17 
_diffrn_reflns_limit_l_max        16 
_diffrn_reflns_theta_min          1.73 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              5138 
_reflns_number_observed           3719 
_reflns_observed_criterion        >2sigma(I) 
  
_computing_data_collection        'Siemens P3/P4 PC V-4.27' 
_computing_cell_refinement        'Siemens P3/P4 PC V-4.27' 
_computing_data_reduction         'Siemens P3/P4 PC V-4.27' 
_computing_structure_solution     'Siemens SHELXTL V-5.03 (Sheldrick, 1994)' 
_computing_structure_refinement   'Siemens SHELXTL V-5.03 (Sheldrick, 1994)' 
_computing_molecular_graphics     'Siemens SHELXTL V-5.03 (Sheldrick, 1994)' 
_computing_publication_material   'Siemens SHELXTL V-5.03 (Sheldrick, 1994)' 
  
_refine_special_details 
; 
 Refinement on F^2^ for ALL reflections except for 2 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^)+(0.0635P)^2^+7.2286P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      'heavy atom method' 
_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_number_reflns          5136 
_refine_ls_number_parameters      343 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0824 
_refine_ls_R_factor_obs           0.0477 
_refine_ls_wR_factor_all          0.1332 
_refine_ls_wR_factor_obs          0.1063 
_refine_ls_goodness_of_fit_all    1.119 
_refine_ls_goodness_of_fit_obs    1.091 
_refine_ls_restrained_S_all       1.149 
_refine_ls_restrained_S_obs       1.091 
_refine_ls_shift/su_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 
Re Re 0.70764(4) 0.69885(2) 0.31884(2) 0.02983(14) Uani 1 d . . 
P1 P 0.7019(3) 0.60547(12) 0.2180(2) 0.0341(6) Uani 1 d . . 
Cl1 Cl 0.7428(3) 0.78582(13) 0.4269(2) 0.0514(7) Uani 1 d . . 
Cl2 Cl 0.9508(2) 0.70152(12) 0.3281(2) 0.0427(6) Uani 1 d . . 
Cl3 Cl 0.7331(3) 0.62931(13) 0.4460(2) 0.0490(7) Uani 1 d . . 
N1 N 0.4940(9) 0.6976(4) 0.2921(6) 0.042(2) Uani 1 d . . 
N2 N 0.2757(8) 0.7333(4) 0.2038(6) 0.046(2) Uani 1 d . . 
N3 N 0.4884(8) 0.7717(4) 0.1728(5) 0.035(2) Uani 1 d . . 
N4 N 0.6303(8) 0.7610(3) 0.2103(5) 0.032(2) Uani 1 d . . 
C1 C 0.3875(11) 0.6707(6) 0.3232(9) 0.055(3) Uani 1 d . . 
H1A H 0.4033(11) 0.6424(6) 0.3732(9) 0.066 Uiso 1 calc R . 
C2 C 0.2572(12) 0.6928(5) 0.2685(8) 0.054(3) Uani 1 d . . 
H2A H 0.1686(12) 0.6817(5) 0.2746(8) 0.065 Uiso 1 calc R . 
C3 C 0.4193(9) 0.7361(4) 0.2182(6) 0.032(2) Uani 1 d . . 
C4 C 0.1669(12) 0.7704(6) 0.1344(9) 0.065(3) Uani 1 d . . 
H4A H 0.2120(12) 0.7950(6) 0.0979(9) 0.097 Uiso 1 calc R . 
H4B H 0.1200(12) 0.7980(6) 0.1663(9) 0.097 Uiso 1 calc R . 
H4C H 0.0966(12) 0.7427(6) 0.0931(9) 0.097 Uiso 1 calc R . 
C5 C 0.7084(10) 0.8030(4) 0.1699(6) 0.030(2) Uani 1 d . . 
C6 C 0.6531(11) 0.8174(4) 0.0737(7) 0.038(2) Uani 1 d . . 
H6A H 0.5674(11) 0.7991(4) 0.0358(7) 0.046 Uiso 1 calc R . 
C7 C 0.7282(12) 0.8597(5) 0.0348(8) 0.048(3) Uani 1 d . . 
H7A H 0.6936(12) 0.8698(5) -0.0292(8) 0.057 Uiso 1 calc R . 
C8 C 0.8530(11) 0.8858(5) 0.0928(7) 0.039(2) Uani 1 d . . 
C9 C 0.9062(11) 0.8738(5) 0.1873(7) 0.043(2) Uani 1 d . . 
H9A H 0.9899(11) 0.8938(5) 0.2248(7) 0.052 Uiso 1 calc R . 
C10 C 0.8351(10) 0.8317(4) 0.2270(7) 0.035(2) Uani 1 d . . 
H10A H 0.8712(10) 0.8225(4) 0.2913(7) 0.042 Uiso 1 calc R . 
C11 C 0.5251(10) 0.5666(5) 0.1771(7) 0.038(2) Uani 1 d . . 
C12 C 0.4354(13) 0.5615(8) 0.0866(9) 0.080(4) Uani 1 d . . 
H12A H 0.4645(13) 0.5780(8) 0.0380(9) 0.096 Uiso 1 calc R . 
C13 C 0.3031(16) 0.5326(10) 0.0644(10) 0.113(7) Uani 1 d . . 
H13A H 0.2444(16) 0.5298(10) 0.0015(10) 0.135 Uiso 1 calc R . 
C14 C 0.2567(13) 0.5080(7) 0.1340(11) 0.076(4) Uani 1 d . . 
H14A H 0.1675(13) 0.4879(7) 0.1189(11) 0.091 Uiso 1 calc R . 
C15 C 0.3423(13) 0.5131(6) 0.2252(10) 0.065(3) Uani 1 d . . 
H15A H 0.3113(13) 0.4974(6) 0.2735(10) 0.078 Uiso 1 calc R . 
C16 C 0.4770(12) 0.5420(6) 0.2467(9) 0.059(3) Uani 1 d . . 
H16A H 0.5358(12) 0.5448(6) 0.3095(9) 0.070 Uiso 1 calc R . 
C17 C 0.8227(10) 0.5396(4) 0.2670(7) 0.037(2) Uani 1 d . . 
C18 C 0.8074(11) 0.4856(5) 0.2127(7) 0.044(2) Uani 1 d . . 
H18A H 0.7320(11) 0.4827(5) 0.1556(7) 0.052 Uiso 1 calc R . 
C19 C 0.9031(13) 0.4356(5) 0.2421(9) 0.057(3) Uani 1 d . . 
H19A H 0.8904(13) 0.3993(5) 0.2052(9) 0.068 Uiso 1 calc R . 
C20 C 1.0166(13) 0.4394(5) 0.3254(9) 0.062(3) Uani 1 d . . 
H20A H 1.0825(13) 0.4064(5) 0.3441(9) 0.074 Uiso 1 calc R . 
C21 C 1.0316(13) 0.4918(5) 0.3801(9) 0.061(3) Uani 1 d . . 
H21A H 1.1061(13) 0.4940(5) 0.4376(9) 0.074 Uiso 1 calc R . 
C22 C 0.9360(11) 0.5424(5) 0.3506(8) 0.048(3) Uani 1 d . . 
H22A H 0.9491(11) 0.5785(5) 0.3880(8) 0.057 Uiso 1 calc R . 
C23 C 0.7526(10) 0.6262(4) 0.1139(6) 0.036(2) Uani 1 d . . 
C24 C 0.6595(13) 0.6619(5) 0.0404(7) 0.055(3) Uani 1 d . . 
H24A H 0.5693(13) 0.6740(5) 0.0428(7) 0.066 Uiso 1 calc R . 
C25 C 0.7026(16) 0.6793(6) -0.0362(8) 0.071(4) Uani 1 d . . 
H25A H 0.6395(16) 0.7017(6) -0.0863(8) 0.085 Uiso 1 calc R . 
C26 C 0.8373(17) 0.6636(6) -0.0381(9) 0.075(4) Uani 1 d . . 
H26A H 0.8672(17) 0.6765(6) -0.0883(9) 0.090 Uiso 1 calc R . 
C27 C 0.9277(14) 0.6290(6) 0.0344(8) 0.061(3) Uani 1 d . . 
H27A H 1.0188(14) 0.6182(6) 0.0323(8) 0.074 Uiso 1 calc R . 
C28 C 0.8878(10) 0.6096(5) 0.1107(7) 0.043(2) Uani 1 d . . 
H28A H 0.9506(10) 0.5857(5) 0.1591(7) 0.052 Uiso 1 calc R . 
Cl4 Cl 0.9453(4) 0.9379(2) 0.0419(2) 0.0699(9) Uani 1 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_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
Re 0.0265(2) 0.0299(2) 0.0333(2) 0.0021(2) 0.00995(14) 0.0005(2) 
P1 0.0313(13) 0.0301(13) 0.0378(13) -0.0017(11) 0.0068(10) 0.0009(11) 
Cl1 0.069(2) 0.043(2) 0.0445(14) -0.0078(11) 0.0221(13) 0.0000(13) 
Cl2 0.0243(11) 0.0475(14) 0.0540(14) -0.0006(13) 0.0095(10) -0.0011(12) 
Cl3 0.060(2) 0.048(2) 0.0406(13) 0.0137(12) 0.0177(12) 0.0021(13) 
N1 0.053(5) 0.033(4) 0.056(5) 0.006(4) 0.040(4) 0.006(4) 
N2 0.019(4) 0.059(6) 0.065(6) 0.004(5) 0.021(4) 0.011(4) 
N3 0.024(4) 0.035(4) 0.045(4) 0.007(4) 0.010(4) 0.008(4) 
N4 0.030(4) 0.030(4) 0.034(4) 0.001(3) 0.009(3) -0.001(3) 
C1 0.030(6) 0.060(7) 0.084(8) 0.022(6) 0.031(6) -0.008(5) 
C2 0.039(6) 0.059(7) 0.075(8) 0.011(6) 0.034(6) -0.003(6) 
C3 0.024(5) 0.031(5) 0.042(5) -0.003(4) 0.013(4) -0.002(4) 
C4 0.034(6) 0.083(9) 0.074(8) 0.006(7) 0.014(6) 0.021(6) 
C5 0.034(5) 0.022(4) 0.041(5) 0.007(4) 0.019(4) 0.007(4) 
C6 0.036(5) 0.038(6) 0.040(5) -0.001(4) 0.012(4) -0.004(4) 
C7 0.055(7) 0.039(6) 0.055(6) 0.011(5) 0.025(6) -0.002(5) 
C8 0.042(6) 0.036(6) 0.046(6) 0.004(4) 0.025(5) -0.006(5) 
C9 0.046(6) 0.037(6) 0.054(6) -0.007(5) 0.025(5) -0.014(5) 
C10 0.035(5) 0.030(5) 0.034(5) -0.002(4) 0.005(4) 0.000(4) 
C11 0.027(5) 0.035(5) 0.046(6) -0.005(5) 0.003(4) 0.004(4) 
C12 0.052(8) 0.118(13) 0.066(8) -0.021(8) 0.015(7) -0.035(8) 
C13 0.069(10) 0.190(21) 0.063(9) -0.034(11) 0.001(8) -0.057(12) 
C14 0.040(7) 0.088(11) 0.093(10) -0.026(9) 0.011(7) -0.025(7) 
C15 0.055(8) 0.051(8) 0.090(9) 0.007(7) 0.024(7) -0.011(6) 
C16 0.045(7) 0.056(7) 0.066(7) 0.019(6) 0.006(6) -0.012(6) 
C17 0.027(5) 0.029(5) 0.051(6) 0.010(4) 0.009(4) -0.003(4) 
C18 0.038(6) 0.037(6) 0.048(6) 0.005(5) 0.003(5) 0.002(5) 
C19 0.069(8) 0.027(6) 0.083(9) 0.004(6) 0.038(7) -0.002(6) 
C20 0.057(8) 0.039(7) 0.090(9) 0.018(6) 0.024(7) 0.021(6) 
C21 0.052(7) 0.040(7) 0.079(8) 0.006(6) 0.005(6) 0.020(6) 
C22 0.043(6) 0.026(5) 0.070(7) 0.005(5) 0.011(6) 0.010(5) 
C23 0.040(6) 0.028(5) 0.033(5) -0.001(4) 0.003(4) -0.004(4) 
C24 0.069(8) 0.048(7) 0.045(6) 0.000(5) 0.013(6) 0.020(6) 
C25 0.110(12) 0.061(8) 0.045(7) 0.012(6) 0.029(7) 0.028(8) 
C26 0.116(12) 0.070(9) 0.054(7) 0.014(7) 0.048(8) 0.025(9) 
C27 0.069(8) 0.058(8) 0.069(8) 0.008(6) 0.039(7) 0.006(7) 
C28 0.032(5) 0.042(6) 0.052(6) 0.006(5) 0.010(5) 0.006(5) 
Cl4 0.095(2) 0.061(2) 0.069(2) -0.002(2) 0.048(2) -0.037(2) 
  
_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 
Re N1 1.997(8) . y 
Re N4 2.035(7) . y 
Re Cl2 2.338(2) . y 
Re Cl3 2.352(2) . y 
Re Cl1 2.399(3) . y 
Re P1 2.476(3) . y 
P1 C17 1.822(10) . ? 
P1 C11 1.831(10) . ? 
P1 C23 1.833(10) . ? 
N1 C3 1.376(12) . y 
N1 C1 1.393(11) . ? 
N2 C2 1.349(13) . ? 
N2 C3 1.352(11) . y 
N2 C4 1.451(13) . y 
N3 C3 1.335(11) . y 
N3 N4 1.337(10) . y 
N4 C5 1.427(11) . ? 
C1 C2 1.355(15) . ? 
C5 C6 1.394(12) . ? 
C5 C10 1.395(13) . ? 
C6 C7 1.399(13) . ? 
C7 C8 1.363(14) . ? 
C8 C9 1.360(13) . ? 
C8 Cl4 1.748(9) . ? 
C9 C10 1.379(13) . ? 
C11 C12 1.356(15) . ? 
C11 C16 1.375(14) . ? 
C12 C13 1.37(2) . ? 
C13 C14 1.37(2) . ? 
C14 C15 1.35(2) . ? 
C15 C16 1.393(15) . ? 
C17 C22 1.376(14) . ? 
C17 C18 1.382(14) . ? 
C18 C19 1.386(14) . ? 
C19 C20 1.37(2) . ? 
C20 C21 1.36(2) . ? 
C21 C22 1.396(14) . ? 
C23 C28 1.384(13) . ? 
C23 C24 1.399(13) . ? 
C24 C25 1.39(2) . ? 
C25 C26 1.37(2) . ? 
C26 C27 1.37(2) . ? 
C27 C28 1.383(14) . ? 
  
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 
N1 Re N4 75.9(3) . . y 
N1 Re Cl2 172.3(2) . . y 
N4 Re Cl2 98.0(2) . . y 
N1 Re Cl3 89.0(2) . . y 
N4 Re Cl3 164.5(2) . . y 
Cl2 Re Cl3 97.41(10) . . y 
N1 Re Cl1 93.2(2) . . y 
N4 Re Cl1 88.5(2) . . y 
Cl2 Re Cl1 91.23(10) . . y 
Cl3 Re Cl1 89.04(10) . . y 
N1 Re P1 93.0(2) . . y 
N4 Re P1 95.9(2) . . y 
Cl2 Re P1 82.92(9) . . y 
Cl3 Re P1 88.07(10) . . y 
Cl1 Re P1 173.08(9) . . y 
C17 P1 C11 102.0(4) . . ? 
C17 P1 C23 101.8(4) . . ? 
C11 P1 C23 108.2(4) . . ? 
C17 P1 Re 119.0(3) . . ? 
C11 P1 Re 113.2(3) . . ? 
C23 P1 Re 111.5(3) . . ? 
C3 N1 C1 104.5(8) . . ? 
C3 N1 Re 113.6(6) . . y 
C1 N1 Re 141.9(7) . . ? 
C2 N2 C3 106.8(8) . . ? 
C2 N2 C4 128.2(9) . . ? 
C3 N2 C4 124.9(9) . . ? 
C3 N3 N4 108.7(7) . . y 
N3 N4 C5 110.1(7) . . ? 
N3 N4 Re 120.6(6) . . y 
C5 N4 Re 129.0(6) . . ? 
C2 C1 N1 108.5(10) . . ? 
N2 C2 C1 109.4(9) . . ? 
N3 C3 N2 128.0(9) . . ? 
N3 C3 N1 121.2(8) . . y 
N2 C3 N1 110.8(8) . . ? 
C6 C5 C10 120.3(8) . . ? 
C6 C5 N4 119.4(8) . . ? 
C10 C5 N4 120.3(8) . . ? 
C5 C6 C7 119.2(9) . . ? 
C8 C7 C6 118.6(10) . . ? 
C9 C8 C7 123.0(9) . . ? 
C9 C8 Cl4 119.5(8) . . ? 
C7 C8 Cl4 117.6(8) . . ? 
C8 C9 C10 119.4(10) . . ? 
C9 C10 C5 119.4(9) . . ? 
C12 C11 C16 117.0(10) . . ? 
C12 C11 P1 127.1(9) . . ? 
C16 C11 P1 115.9(8) . . ? 
C11 C12 C13 122.0(13) . . ? 
C14 C13 C12 120.5(13) . . ? 
C15 C14 C13 119.1(12) . . ? 
C14 C15 C16 119.8(12) . . ? 
C11 C16 C15 121.6(11) . . ? 
C22 C17 C18 118.1(9) . . ? 
C22 C17 P1 123.8(8) . . ? 
C18 C17 P1 117.8(7) . . ? 
C17 C18 C19 120.9(10) . . ? 
C20 C19 C18 120.4(11) . . ? 
C21 C20 C19 119.3(11) . . ? 
C20 C21 C22 120.6(11) . . ? 
C17 C22 C21 120.8(10) . . ? 
C28 C23 C24 119.7(9) . . ? 
C28 C23 P1 119.6(7) . . ? 
C24 C23 P1 120.5(8) . . ? 
C25 C24 C23 119.6(11) . . ? 
C26 C25 C24 120.3(12) . . ? 
C27 C26 C25 119.6(12) . . ? 
C26 C27 C28 121.9(12) . . ? 
C27 C28 C23 118.9(10) . . ? 
  
_refine_diff_density_max    1.202 
_refine_diff_density_min   -1.696 
_refine_diff_density_rms    0.177 
  
#END#....