# Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2001
# CCDC Number: 186/2273

data_bqdi.cif
 
 
  
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C18 H26 Cl2 N6 O12 Os' 
_chemical_formula_weight          779.55 
_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' 
 'Os'  'Os'  -1.2165   7.6030 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    C2/c 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y, -z+1/2' 
 'x+1/2, y+1/2, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y, z-1/2' 
 '-x+1/2, -y+1/2, -z' 
 'x+1/2, -y+1/2, z-1/2' 
  
_cell_length_a                    18.5600(1) 
_cell_length_b                    9.3076(1) 
_cell_length_c                    15.9116(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  100.416(1) 
_cell_angle_gamma                 90.00 
_cell_volume                      2703.42(5) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     295(2) 
_cell_measurement_reflns_used     7902 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
  
_exptl_crystal_description        plate 
_exptl_crystal_colour             purple 
_exptl_crystal_size_max           0.45 
_exptl_crystal_size_mid           0.12 
_exptl_crystal_size_min           0.03 
_exptl_crystal_density_meas       not_measured 
_exptl_crystal_density_diffrn     1.915 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1528 
_exptl_absorpt_coefficient_mu     4.984 
_exptl_absorpt_correction_type    ' empirical used sadabs' 
_exptl_absorpt_correction_T_min   0.2825 
_exptl_absorpt_correction_T_max   0.4932 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       295(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        'Siemens SMART' 
_diffrn_measurement_method        '\w scans' 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         0 
_diffrn_reflns_number             9882 
_diffrn_reflns_av_R_equivalents   0.0402 
_diffrn_reflns_av_sigmaI/netI     0.0411 
_diffrn_reflns_limit_h_min        -24 
_diffrn_reflns_limit_h_max        24 
_diffrn_reflns_limit_k_min        -10 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -20 
_diffrn_reflns_limit_l_max        21 
_diffrn_reflns_theta_min          2.23 
_diffrn_reflns_theta_max          27.50 
_reflns_number_total              3116 
_reflns_number_observed           2841 
_reflns_observed_criterion        >2sigma(I) 
  
_computing_data_collection        'Siemens SMART' 
_computing_cell_refinement        'Siemens SAINT' 
_computing_data_reduction         'Siemens SAINT' 
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     'Siemens SHELXTL' 
_computing_publication_material   'Siemens SHELXTL' 
  
_refine_special_details 
; 
 Refinement on F^2^ for ALL reflections except for 47 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^)+(0.0330P)^2^+0.3739P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     ? 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.00004(6) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_number_reflns          3069 
_refine_ls_number_parameters      190 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0341 
_refine_ls_R_factor_obs           0.0285 
_refine_ls_wR_factor_all          0.0651 
_refine_ls_wR_factor_obs          0.0626 
_refine_ls_goodness_of_fit_all    1.053 
_refine_ls_goodness_of_fit_obs    1.064 
_refine_ls_restrained_S_all       1.054 
_refine_ls_restrained_S_obs       1.064 
_refine_ls_shift/esd_max          -0.294 
_refine_ls_shift/esd_mean         0.017 
  
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 
Os Os 0.0000 -0.04363(2) 0.2500 0.02874(8) Uani 1 d S . 
N1 N -0.0715(2) 0.0445(4) 0.3140(2) 0.0489(9) Uani 1 d . . 
H1A H -0.1178(2) 0.0356(4) 0.2954(2) 0.059 Uiso 1 calc R . 
N2 N 0.0617(2) 0.0427(4) 0.3532(2) 0.0488(9) Uani 1 d . . 
H2A H 0.1085(2) 0.0329(4) 0.3621(2) 0.059 Uiso 1 calc R . 
N3 N 0.0662(2) -0.2118(4) 0.2699(3) 0.0530(10) Uani 1 d . . 
H3A H 0.1128(2) -0.1994(4) 0.2838(3) 0.064 Uiso 1 calc R . 
C1 C -0.0476(2) 0.1168(4) 0.3853(2) 0.0407(9) Uani 1 d . . 
C2 C -0.0901(3) 0.1943(7) 0.4355(3) 0.068(2) Uani 1 d . . 
H2B H -0.1410(3) 0.1943(7) 0.4215(3) 0.082 Uiso 1 calc R . 
C3 C -0.0553(3) 0.2683(7) 0.5039(3) 0.074(2) Uani 1 d . . 
H3B H -0.0826(3) 0.3214(7) 0.5365(3) 0.089 Uiso 1 calc R . 
C4 C 0.0223(3) 0.2662(6) 0.5270(3) 0.0639(13) Uani 1 d . . 
H4A H 0.0447(3) 0.3179(6) 0.5746(3) 0.077 Uiso 1 calc R . 
C5 C 0.0645(3) 0.1912(6) 0.4817(3) 0.0604(13) Uani 1 d . . 
H5A H 0.1151(3) 0.1893(6) 0.4983(3) 0.072 Uiso 1 calc R . 
C6 C 0.0296(2) 0.1156(5) 0.4084(2) 0.0410(9) Uani 1 d . . 
C7 C 0.0389(2) -0.3428(4) 0.2617(3) 0.0434(9) Uani 1 d . . 
C8 C 0.0775(4) -0.4742(5) 0.2732(4) 0.070(2) Uani 1 d . . 
H8A H 0.1283(4) -0.4759(5) 0.2884(4) 0.084 Uiso 1 calc R . 
C9 C 0.0385(3) -0.5976(5) 0.2613(4) 0.069(2) Uani 1 d . . 
H9A H 0.0631(3) -0.6849(5) 0.2684(4) 0.083 Uiso 1 calc R . 
Cl Cl 0.24715(7) -0.2668(2) 0.16894(9) 0.0705(4) Uani 1 d . . 
O1 O 0.2157(4) -0.1333(9) 0.1756(5) 0.170(3) Uani 1 d . . 
O2 O 0.2918(4) -0.2615(10) 0.1089(5) 0.168(3) Uani 1 d . . 
O3 O 0.2881(3) -0.3088(10) 0.2441(4) 0.191(4) Uani 1 d . . 
O4 O 0.1889(3) -0.3580(9) 0.1446(5) 0.171(3) Uani 1 d . . 
O5 O 0.2093(3) -0.1435(11) 0.3791(4) 0.122(2) Uani 1 d . . 
O6 O 0.2790(5) -0.0728(10) 0.5452(6) 0.164(4) Uani 1 d . . 
H5B H 0.2134(37) -0.2483(76) 0.3830(47) 0.079(26) Uiso 1 d . . 
H5C H 0.2439(60) -0.1112(133) 0.3411(71) 0.185(44) Uiso 1 d . . 
H6A H 0.2409(68) -0.0092(112) 0.5533(76) 0.156(43) Uiso 1 d . . 
H6B H 0.2403 -0.0800 0.4785 0.165 Uiso 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 
Os 0.02555(11) 0.02711(11) 0.03273(12) 0.000 0.00310(7) 0.000 
N1 0.025(2) 0.071(3) 0.049(2) -0.017(2) 0.0017(15) 0.004(2) 
N2 0.026(2) 0.075(3) 0.044(2) -0.017(2) 0.0033(14) -0.001(2) 
N3 0.031(2) 0.035(2) 0.089(3) 0.001(2) -0.002(2) 0.0039(14) 
C1 0.038(2) 0.045(2) 0.039(2) 0.000(2) 0.005(2) 0.009(2) 
C2 0.059(3) 0.100(4) 0.046(3) -0.015(3) 0.010(2) 0.030(3) 
C3 0.097(4) 0.081(4) 0.048(3) -0.011(3) 0.019(3) 0.030(3) 
C4 0.081(4) 0.071(3) 0.039(2) -0.016(2) 0.010(2) -0.009(3) 
C5 0.051(3) 0.085(4) 0.046(2) -0.016(2) 0.009(2) -0.016(3) 
C6 0.046(2) 0.046(2) 0.032(2) -0.002(2) 0.009(2) -0.005(2) 
C7 0.051(2) 0.036(2) 0.043(2) 0.003(2) 0.009(2) 0.010(2) 
C8 0.070(4) 0.038(3) 0.098(5) 0.010(2) 0.005(3) 0.014(2) 
C9 0.103(4) 0.031(2) 0.074(3) 0.003(2) 0.018(3) 0.013(2) 
Cl 0.0471(7) 0.0925(10) 0.0731(8) 0.0127(7) 0.0141(6) 0.0102(7) 
O1 0.146(6) 0.159(6) 0.211(8) 0.018(6) 0.046(5) 0.087(5) 
O2 0.134(5) 0.238(9) 0.160(6) 0.018(6) 0.104(4) 0.018(6) 
O3 0.122(5) 0.311(11) 0.122(5) 0.044(6) -0.024(4) 0.106(6) 
O4 0.084(4) 0.200(8) 0.219(8) 0.024(6) -0.002(4) -0.046(5) 
O5 0.059(3) 0.192(8) 0.113(5) 0.002(5) 0.009(3) -0.005(4) 
O6 0.137(6) 0.172(7) 0.171(7) -0.069(6) -0.006(5) 0.011(6) 
  
_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 
Os N3 1.980(3) 2 ? 
Os N3 1.980(3) . ? 
Os N1 1.990(4) 2 ? 
Os N1 1.990(4) . ? 
Os N2 1.994(3) 2 ? 
Os N2 1.994(3) . ? 
N1 C1 1.326(5) . ? 
N2 C6 1.333(5) . ? 
N3 C7 1.318(5) . ? 
C1 C6 1.413(5) . ? 
C1 C2 1.416(6) . ? 
C2 C3 1.350(7) . ? 
C3 C4 1.421(8) . ? 
C4 C5 1.350(7) . ? 
C5 C6 1.415(6) . ? 
C7 C8 1.413(6) . ? 
C7 C7 1.425(8) 2 ? 
C8 C9 1.353(8) . ? 
C9 C9 1.408(12) 2 ? 
Cl O3 1.354(5) . ? 
Cl O2 1.374(6) . ? 
Cl O4 1.375(6) . ? 
Cl O1 1.385(7) . ? 
  
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 
N3 Os N3 75.5(2) 2 . ? 
N3 Os N1 134.1(2) 2 2 ? 
N3 Os N1 87.4(2) . 2 ? 
N3 Os N1 87.4(2) 2 . ? 
N3 Os N1 134.1(2) . . ? 
N1 Os N1 131.3(2) 2 . ? 
N3 Os N2 86.52(15) 2 2 ? 
N3 Os N2 134.2(2) . 2 ? 
N1 Os N2 75.50(14) 2 2 ? 
N1 Os N2 85.3(2) . 2 ? 
N3 Os N2 134.2(2) 2 . ? 
N3 Os N2 86.52(15) . . ? 
N1 Os N2 85.3(2) 2 . ? 
N1 Os N2 75.50(14) . . ? 
N2 Os N2 132.5(2) 2 . ? 
C1 N1 Os 119.7(3) . . ? 
C6 N2 Os 119.3(3) . . ? 
C7 N3 Os 119.9(3) . . ? 
N1 C1 C6 112.7(4) . . ? 
N1 C1 C2 127.3(4) . . ? 
C6 C1 C2 120.0(4) . . ? 
C3 C2 C1 118.7(5) . . ? 
C2 C3 C4 121.1(5) . . ? 
C5 C4 C3 121.9(5) . . ? 
C4 C5 C6 118.3(5) . . ? 
N2 C6 C1 112.7(3) . . ? 
N2 C6 C5 127.2(4) . . ? 
C1 C6 C5 120.1(4) . . ? 
N3 C7 C8 127.7(4) . . ? 
N3 C7 C7 112.3(2) . 2 ? 
C8 C7 C7 120.0(3) . 2 ? 
C9 C8 C7 118.0(5) . . ? 
C8 C9 C9 121.9(3) . 2 ? 
O3 Cl O2 108.2(4) . . ? 
O3 Cl O4 111.0(5) . . ? 
O2 Cl O4 111.6(5) . . ? 
O3 Cl O1 111.6(6) . . ? 
O2 Cl O1 109.7(5) . . ? 
O4 Cl O1 104.7(5) . . ? 
  
_refine_diff_density_max    1.398 
_refine_diff_density_min   -0.913 
_refine_diff_density_rms    0.115