# Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2000
# CCDC Number: 186/1862
 
data_cr 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C14 H10 As0.25 Cr2 O4 P5.75' 
_chemical_formula_weight          542.92 
 
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' 
 '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' 
 'As'  'As'   0.0499   2.0058 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cr'  'Cr'   0.3209   0.6236 
 '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                    11.287(2) 
_cell_length_b                    14.365(3) 
_cell_length_c                    13.237(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  114.99(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      1945.3(7) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     190(1) 
_cell_measurement_reflns_used     1945
_cell_measurement_theta_min       2.44
_cell_measurement_theta_max       26.00
 
_exptl_crystal_description        plate
_exptl_crystal_colour             red
_exptl_crystal_size_max           0.20
_exptl_crystal_size_mid           0.10
_exptl_crystal_size_min           0.02
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.854 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1074 
_exptl_absorpt_coefficient_mu     2.025 
_exptl_absorpt_correction_type    numerical
_exptl_absorpt_correction_T_min   0.6823
_exptl_absorpt_correction_T_max   0.8912
_exptl_absorpt_process_details    'program faceit'
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       190(1) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'STOE IPDS'
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             8261 
_diffrn_reflns_av_R_equivalents   0.0541 
_diffrn_reflns_av_sigmaI/netI     0.0427 
_diffrn_reflns_limit_h_min        -13 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        -17 
_diffrn_reflns_limit_k_max        14 
_diffrn_reflns_limit_l_min        -12 
_diffrn_reflns_limit_l_max        16 
_diffrn_reflns_theta_min          2.44 
_diffrn_reflns_theta_max          26.00 
_reflns_number_total              3414 
_reflns_number_gt                 2692 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'STOE IPDS software'
_computing_cell_refinement        'STOE IPDS software'
_computing_data_reduction         'STOE IPDS software'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'SIEMENS-XP'
_computing_publication_material   'SHELXL-97'
 
_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^)+(0.0715P)^2^+1.0233P] 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     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          3414 
_refine_ls_number_parameters      237 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0560 
_refine_ls_R_factor_gt            0.0403 
_refine_ls_wR_factor_ref          0.1162 
_refine_ls_wR_factor_gt           0.1044 
_refine_ls_goodness_of_fit_ref    1.032 
_refine_ls_restrained_S_all       1.032 
_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_symetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Cr1 Cr 0.97337(5) 0.14809(4) 0.73747(5) 0.02236(18) Uani 1 1 d . . . 
P1 P 1.09343(9) 0.10953(7) 0.62497(9) 0.0333(3) Uani 0.956(2) 1 d P . . 
As1 As 1.09343(9) 0.10953(7) 0.62497(9) 0.0333(3) Uani 0.044(2) 1 d P . . 
P2 P 0.98179(11) -0.00123(7) 0.65225(9) 0.0400(3) Uani 0.956(2) 1 d P . . 
As2 As 0.98179(11) -0.00123(7) 0.65225(9) 0.0400(3) Uani 0.044(2) 1 d P . . 
P3 P 0.88366(10) 0.10567(8) 0.53432(8) 0.0382(3) Uani 0.956(2) 1 d P . . 
As3 As 0.88366(10) 0.10567(8) 0.53432(8) 0.0382(3) Uani 0.044(2) 1 d P . . 
C1 C 0.9440(4) 0.2645(3) 0.6676(3) 0.0316(8) Uani 1 1 d . . . 
O1 O 0.9282(3) 0.3367(2) 0.6271(3) 0.0490(8) Uani 1 1 d . . . 
C2 C 0.7941(4) 0.1332(3) 0.6922(4) 0.0318(8) Uani 1 1 d . . . 
O2 O 0.6839(3) 0.1253(2) 0.6670(3) 0.0497(8) Uani 1 1 d . . . 
C3 C 0.9842(4) 0.1948(4) 0.8971(4) 0.0476(11) Uani 1 1 d . . . 
H3 H 0.9157 0.2289 0.9035 0.057 Uiso 1 1 calc R . . 
C4 C 0.9969(4) 0.0967(3) 0.8996(4) 0.0427(10) Uani 1 1 d . . . 
H4 H 0.9378 0.0532 0.9072 0.051 Uiso 1 1 calc R . . 
C5 C 1.1127(3) 0.0751(3) 0.8887(3) 0.0336(8) Uani 1 1 d . . . 
H5 H 1.1460 0.0144 0.8886 0.040 Uiso 1 1 calc R . . 
C6 C 1.1703(3) 0.1587(3) 0.8783(3) 0.0338(8) Uani 1 1 d . . . 
H6 H 1.2491 0.1641 0.8692 0.041 Uiso 1 1 calc R . . 
C7 C 1.0925(4) 0.2329(3) 0.8833(4) 0.0447(10) Uani 1 1 d . . . 
H7 H 1.1092 0.2971 0.8784 0.054 Uiso 1 1 calc R . . 
Cr2 Cr 0.46951(5) 0.40314(4) 0.74001(5) 0.02553(18) Uani 1 1 d . . . 
P4 P 0.61713(10) 0.48873(8) 0.67528(11) 0.0441(3) Uani 0.962(3) 1 d P . . 
As4 As 0.61713(10) 0.48873(8) 0.67528(11) 0.0441(3) Uani 0.038(3) 1 d P . . 
P5 P 0.52646(9) 0.36573(8) 0.58479(9) 0.0400(3) Uani 0.962(3) 1 d P . . 
As5 As 0.52646(9) 0.36573(8) 0.58479(9) 0.0400(3) Uani 0.038(3) 1 d P . . 
P6 P 0.68260(9) 0.35637(9) 0.75020(10) 0.0450(3) Uani 0.962(3) 1 d P . . 
As6 As 0.68260(9) 0.35637(9) 0.75020(10) 0.0450(3) Uani 0.038(3) 1 d P . . 
C8 C 0.5532(3) 0.4888(3) 0.8562(3) 0.0321(8) Uani 1 1 d . . . 
O3 O 0.5996(3) 0.5405(2) 0.9267(3) 0.0480(8) Uani 1 1 d . . . 
C9 C 0.3654(3) 0.4990(3) 0.6527(3) 0.0302(8) Uani 1 1 d . . . 
O4 O 0.2994(3) 0.5584(2) 0.6004(3) 0.0428(7) Uani 1 1 d . . . 
C10 C 0.3258(4) 0.3715(3) 0.8043(4) 0.0466(11) Uani 1 1 d . . . 
H10 H 0.2833 0.4187 0.8270 0.056 Uiso 1 1 calc R . . 
C11 C 0.2819(4) 0.3339(3) 0.6964(4) 0.0477(11) Uani 1 1 d . . . 
H11 H 0.2047 0.3517 0.6337 0.057 Uiso 1 1 calc R . . 
C12 C 0.3710(5) 0.2657(3) 0.6965(5) 0.0528(12) Uani 1 1 d . . . 
H12 H 0.3650 0.2295 0.6345 0.063 Uiso 1 1 calc R . . 
C13 C 0.4710(5) 0.2610(3) 0.8056(5) 0.0544(13) Uani 1 1 d . . . 
H13 H 0.5443 0.2204 0.8298 0.065 Uiso 1 1 calc R . . 
C14 C 0.4445(5) 0.3265(3) 0.8732(4) 0.0496(11) Uani 1 1 d . . . 
H14 H 0.4963 0.3382 0.9500 0.060 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 
Cr1 0.0257(3) 0.0204(3) 0.0213(3) 0.0004(2) 0.0102(2) 0.00191(19) 
P1 0.0389(5) 0.0343(5) 0.0342(5) -0.0065(4) 0.0227(4) -0.0028(4) 
As1 0.0389(5) 0.0343(5) 0.0342(5) -0.0065(4) 0.0227(4) -0.0028(4) 
P2 0.0617(6) 0.0236(5) 0.0382(6) -0.0041(4) 0.0246(5) -0.0031(4) 
As2 0.0617(6) 0.0236(5) 0.0382(6) -0.0041(4) 0.0246(5) -0.0031(4) 
P3 0.0444(5) 0.0411(6) 0.0239(5) -0.0024(4) 0.0093(4) 0.0023(4) 
As3 0.0444(5) 0.0411(6) 0.0239(5) -0.0024(4) 0.0093(4) 0.0023(4) 
C1 0.0375(18) 0.031(2) 0.028(2) -0.0024(16) 0.0164(15) 0.0006(15) 
O1 0.080(2) 0.0246(16) 0.047(2) 0.0083(14) 0.0305(17) 0.0082(14) 
C2 0.0358(19) 0.027(2) 0.031(2) 0.0027(16) 0.0129(15) 0.0004(14) 
O2 0.0293(14) 0.059(2) 0.058(2) 0.0069(17) 0.0162(14) -0.0038(13) 
C3 0.050(2) 0.067(3) 0.023(2) -0.003(2) 0.0132(17) 0.027(2) 
C4 0.0362(19) 0.065(3) 0.025(2) 0.0102(19) 0.0122(16) -0.0029(18) 
C5 0.0339(18) 0.032(2) 0.027(2) 0.0026(16) 0.0050(14) 0.0071(15) 
C6 0.0301(17) 0.038(2) 0.028(2) -0.0028(16) 0.0072(14) -0.0043(14) 
C7 0.060(3) 0.028(2) 0.030(2) -0.0104(17) 0.0031(18) 0.0007(18) 
Cr2 0.0265(3) 0.0227(3) 0.0267(3) -0.0004(2) 0.0106(2) -0.0010(2) 
P4 0.0396(5) 0.0455(7) 0.0560(7) -0.0022(5) 0.0288(5) -0.0077(4) 
As4 0.0396(5) 0.0455(7) 0.0560(7) -0.0022(5) 0.0288(5) -0.0077(4) 
P5 0.0393(5) 0.0508(7) 0.0299(6) -0.0088(5) 0.0148(4) 0.0008(4) 
As5 0.0393(5) 0.0508(7) 0.0299(6) -0.0088(5) 0.0148(4) 0.0008(4) 
P6 0.0336(5) 0.0584(8) 0.0387(6) -0.0056(5) 0.0111(4) 0.0144(4) 
As6 0.0336(5) 0.0584(8) 0.0387(6) -0.0056(5) 0.0111(4) 0.0144(4) 
C8 0.0322(16) 0.032(2) 0.031(2) 0.0017(17) 0.0129(15) 0.0063(15) 
O3 0.0432(15) 0.0481(19) 0.044(2) -0.0187(16) 0.0102(13) -0.0014(13) 
C9 0.0274(15) 0.034(2) 0.030(2) -0.0067(16) 0.0135(14) -0.0040(15) 
O4 0.0397(14) 0.0435(18) 0.0404(18) 0.0089(14) 0.0122(12) 0.0119(13) 
C10 0.049(2) 0.044(3) 0.062(3) 0.004(2) 0.039(2) -0.0102(19) 
C11 0.039(2) 0.048(3) 0.054(3) 0.004(2) 0.0165(19) -0.0211(19) 
C12 0.074(3) 0.033(2) 0.060(3) -0.014(2) 0.037(3) -0.024(2) 
C13 0.069(3) 0.029(2) 0.069(4) 0.013(2) 0.033(3) 0.005(2) 
C14 0.068(3) 0.044(3) 0.039(3) 0.009(2) 0.024(2) -0.011(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 
Cr1 C2 1.864(4) . ? 
Cr1 C1 1.872(4) . ? 
Cr1 C3 2.171(4) . ? 
Cr1 C4 2.177(4) . ? 
Cr1 C7 2.197(4) . ? 
Cr1 C5 2.218(4) . ? 
Cr1 C6 2.222(4) . ? 
Cr1 P2 2.4441(12) . ? 
Cr1 P1 2.4630(11) . ? 
Cr1 P3 2.5154(13) . ? 
P1 P2 2.1528(14) . ? 
P1 P3 2.1560(15) . ? 
P2 P3 2.1356(16) . ? 
C1 O1 1.146(5) . ? 
C2 O2 1.149(4) . ? 
C3 C4 1.414(7) . ? 
C3 C7 1.420(7) . ? 
C4 C5 1.409(5) . ? 
C5 C6 1.399(6) . ? 
C6 C7 1.400(6) . ? 
Cr2 C9 1.862(4) . ? 
Cr2 C8 1.883(4) . ? 
Cr2 C10 2.174(4) . ? 
Cr2 C11 2.185(4) . ? 
Cr2 C14 2.195(4) . ? 
Cr2 C13 2.216(5) . ? 
Cr2 C12 2.219(4) . ? 
Cr2 P6 2.4454(11) . ? 
Cr2 P5 2.4575(12) . ? 
Cr2 P4 2.4956(12) . ? 
P4 P6 2.1273(17) . ? 
P4 P5 2.1373(16) . ? 
P5 P6 2.1581(18) . ? 
C8 O3 1.132(5) . ? 
C9 O4 1.151(5) . ? 
C10 C11 1.407(7) . ? 
C10 C14 1.419(7) . ? 
C11 C12 1.403(7) . ? 
C12 C13 1.410(8) . ? 
C13 C14 1.414(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 
C2 Cr1 C1 90.14(16) . . ? 
C2 Cr1 C3 87.44(18) . . ? 
C1 Cr1 C3 97.49(18) . . ? 
C2 Cr1 C4 86.64(17) . . ? 
C1 Cr1 C4 135.43(18) . . ? 
C3 Cr1 C4 37.98(19) . . ? 
C2 Cr1 C7 121.64(18) . . ? 
C1 Cr1 C7 81.59(18) . . ? 
C3 Cr1 C7 37.94(19) . . ? 
C4 Cr1 C7 63.07(18) . . ? 
C2 Cr1 C5 119.67(16) . . ? 
C1 Cr1 C5 141.11(16) . . ? 
C3 Cr1 C5 62.64(16) . . ? 
C4 Cr1 C5 37.38(15) . . ? 
C7 Cr1 C5 62.05(16) . . ? 
C2 Cr1 C6 147.43(17) . . ? 
C1 Cr1 C6 105.01(16) . . ? 
C3 Cr1 C6 62.43(15) . . ? 
C4 Cr1 C6 62.24(15) . . ? 
C7 Cr1 C6 36.94(15) . . ? 
C5 Cr1 C6 36.74(15) . . ? 
C2 Cr1 P2 89.97(13) . . ? 
C1 Cr1 P2 126.12(12) . . ? 
C3 Cr1 P2 136.32(14) . . ? 
C4 Cr1 P2 98.35(14) . . ? 
C7 Cr1 P2 139.77(12) . . ? 
C5 Cr1 P2 81.42(11) . . ? 
C6 Cr1 P2 103.12(11) . . ? 
C2 Cr1 P1 125.43(14) . . ? 
C1 Cr1 P1 85.99(11) . . ? 
C3 Cr1 P1 147.03(12) . . ? 
C4 Cr1 P1 130.60(12) . . ? 
C7 Cr1 P1 111.54(13) . . ? 
C5 Cr1 P1 94.48(11) . . ? 
C6 Cr1 P1 84.93(11) . . ? 
P2 Cr1 P1 52.04(3) . . ? 
C2 Cr1 P3 74.73(14) . . ? 
C1 Cr1 P3 77.35(12) . . ? 
C3 Cr1 P3 161.31(11) . . ? 
C4 Cr1 P3 142.95(14) . . ? 
C7 Cr1 P3 153.43(14) . . ? 
C5 Cr1 P3 131.46(11) . . ? 
C6 Cr1 P3 136.18(11) . . ? 
P2 Cr1 P3 50.99(4) . . ? 
P1 Cr1 P3 51.31(4) . . ? 
P2 P1 P3 59.42(5) . . ? 
P2 P1 Cr1 63.53(4) . . ? 
P3 P1 Cr1 65.60(4) . . ? 
P3 P2 P1 60.36(5) . . ? 
P3 P2 Cr1 66.23(4) . . ? 
P1 P2 Cr1 64.43(4) . . ? 
P2 P3 P1 60.21(5) . . ? 
P2 P3 Cr1 62.78(4) . . ? 
P1 P3 Cr1 63.09(5) . . ? 
O1 C1 Cr1 178.4(4) . . ? 
O2 C2 Cr1 178.1(4) . . ? 
C4 C3 C7 107.6(3) . . ? 
C4 C3 Cr1 71.2(3) . . ? 
C7 C3 Cr1 72.0(2) . . ? 
C5 C4 C3 107.8(4) . . ? 
C5 C4 Cr1 72.9(2) . . ? 
C3 C4 Cr1 70.8(3) . . ? 
C6 C5 C4 108.1(4) . . ? 
C6 C5 Cr1 71.8(2) . . ? 
C4 C5 Cr1 69.7(2) . . ? 
C5 C6 C7 108.8(3) . . ? 
C5 C6 Cr1 71.5(2) . . ? 
C7 C6 Cr1 70.5(2) . . ? 
C6 C7 C3 107.7(4) . . ? 
C6 C7 Cr1 72.5(2) . . ? 
C3 C7 Cr1 70.0(2) . . ? 
C9 Cr2 C8 89.47(17) . . ? 
C9 Cr2 C10 91.01(17) . . ? 
C8 Cr2 C10 90.97(18) . . ? 
C9 Cr2 C11 83.42(17) . . ? 
C8 Cr2 C11 127.55(18) . . ? 
C10 Cr2 C11 37.66(19) . . ? 
C9 Cr2 C14 127.42(18) . . ? 
C8 Cr2 C14 82.08(19) . . ? 
C10 Cr2 C14 37.89(19) . . ? 
C11 Cr2 C14 62.94(18) . . ? 
C9 Cr2 C13 145.40(18) . . ? 
C8 Cr2 C13 111.3(2) . . ? 
C10 Cr2 C13 62.45(18) . . ? 
C11 Cr2 C13 61.98(19) . . ? 
C14 Cr2 C13 37.40(19) . . ? 
C9 Cr2 C12 112.41(19) . . ? 
C8 Cr2 C12 144.79(19) . . ? 
C10 Cr2 C12 62.65(18) . . ? 
C11 Cr2 C12 37.14(19) . . ? 
C14 Cr2 C12 62.7(2) . . ? 
C13 Cr2 C12 37.1(2) . . ? 
C9 Cr2 P6 125.86(11) . . ? 
C8 Cr2 P6 89.55(11) . . ? 
C10 Cr2 P6 143.13(14) . . ? 
C11 Cr2 P6 135.25(14) . . ? 
C14 Cr2 P6 105.97(14) . . ? 
C13 Cr2 P6 83.15(13) . . ? 
C12 Cr2 P6 98.23(14) . . ? 
C9 Cr2 P5 87.85(12) . . ? 
C8 Cr2 P5 127.42(12) . . ? 
C10 Cr2 P5 141.55(14) . . ? 
C11 Cr2 P5 104.23(14) . . ? 
C14 Cr2 P5 136.84(14) . . ? 
C13 Cr2 P5 99.49(15) . . ? 
C12 Cr2 P5 82.41(14) . . ? 
P6 Cr2 P5 52.23(4) . . ? 
C9 Cr2 P4 76.14(11) . . ? 
C8 Cr2 P4 77.35(12) . . ? 
C10 Cr2 P4 162.55(13) . . ? 
C11 Cr2 P4 147.84(14) . . ? 
C14 Cr2 P4 148.62(14) . . ? 
C13 Cr2 P4 133.85(13) . . ? 
C12 Cr2 P4 133.09(14) . . ? 
P6 Cr2 P4 50.99(4) . . ? 
P5 Cr2 P4 51.12(4) . . ? 
P6 P4 P5 60.80(6) . . ? 
P6 P4 Cr2 63.28(4) . . ? 
P5 P4 Cr2 63.52(4) . . ? 
P4 P5 P6 59.37(6) . . ? 
P4 P5 Cr2 65.36(4) . . ? 
P6 P5 Cr2 63.60(4) . . ? 
P4 P6 P5 59.83(5) . . ? 
P4 P6 Cr2 65.72(4) . . ? 
P5 P6 Cr2 64.17(4) . . ? 
O3 C8 Cr2 177.5(3) . . ? 
O4 C9 Cr2 178.4(3) . . ? 
C11 C10 C14 108.0(4) . . ? 
C11 C10 Cr2 71.6(2) . . ? 
C14 C10 Cr2 71.8(2) . . ? 
C12 C11 C10 108.8(4) . . ? 
C12 C11 Cr2 72.8(2) . . ? 
C10 C11 Cr2 70.8(2) . . ? 
C11 C12 C13 107.3(4) . . ? 
C11 C12 Cr2 70.1(2) . . ? 
C13 C12 Cr2 71.4(3) . . ? 
C12 C13 C14 108.9(5) . . ? 
C12 C13 Cr2 71.6(3) . . ? 
C14 C13 Cr2 70.5(3) . . ? 
C13 C14 C10 106.9(5) . . ? 
C13 C14 Cr2 72.1(3) . . ? 
C10 C14 Cr2 70.3(3) . . ? 
 
_diffrn_measured_fraction_theta_max    0.892 
_diffrn_reflns_theta_full              26.00 
_diffrn_measured_fraction_theta_full   0.892 
_refine_diff_density_max    0.508 
_refine_diff_density_min   -0.623 
_refine_diff_density_rms    0.087 

data_2

_audit_creation_method            SHELXL
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_formula_moiety          ?
_chemical_formula_structural      ?
_chemical_formula_analytical      ?
_chemical_formula_sum             'C10 H10 Cl4 Cr2'
_chemical_formula_weight          375.98
_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'
 'Cl'  'Cl'   0.1484   0.1585
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cr'  'Cr'   0.3209   0.6236
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting            orthorhombic
_symmetry_space_group_name_H-M    Pbca

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'
 '-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                    11.144(2)
_cell_length_b                    9.852(2)
_cell_length_c                    12.139(2)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      1332.7(5)
_cell_formula_units_Z             4
_cell_measurement_temperature     203(2)
_cell_measurement_reflns_used     42
_cell_measurement_theta_min       5
_cell_measurement_theta_max       25

_exptl_crystal_description        route
_exptl_crystal_colour             black
_exptl_crystal_size_max           0.76
_exptl_crystal_size_mid           0.38
_exptl_crystal_size_min           0.15
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.874
_exptl_crystal_density_method     ?
_exptl_crystal_F_000              744
_exptl_absorpt_coefficient_mu     2.399
_exptl_absorpt_correction_type    'Psi-scans (10)'
_exptl_absorpt_correction_T_min   0.1702
_exptl_absorpt_correction_T_max   0.4866

_exptl_special_details
;
 ?
;

_diffrn_ambient_temperature       203(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        'STOE STADI4'
_diffrn_measurement_method        'omega-scans'
_diffrn_standards_number          2
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   120
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             2892
_diffrn_reflns_av_R_equivalents   0.0388
_diffrn_reflns_av_sigmaI/netI     0.0346
_diffrn_reflns_limit_h_min        0
_diffrn_reflns_limit_h_max        14
_diffrn_reflns_limit_k_min        -12
_diffrn_reflns_limit_k_max        12
_diffrn_reflns_limit_l_min        0
_diffrn_reflns_limit_l_max        15
_diffrn_reflns_theta_min          3.23
_diffrn_reflns_theta_max          27.53
_reflns_number_total              1532
_reflns_number_observed           1327
_reflns_observed_criterion        >2sigma(I)

_computing_data_collection        'Stoe DIF4'
_computing_cell_refinement        'Stoe DIF4'
_computing_data_reduction         'Stoe REDU4'
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics     'SIEMENS XP'
_computing_publication_material   'SHELXL-93'

_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^)+(0.0397P)^2^+0.4047P] 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     riding
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          1530
_refine_ls_number_parameters      73
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0375
_refine_ls_R_factor_obs           0.0299
_refine_ls_wR_factor_all          0.0842
_refine_ls_wR_factor_obs          0.0765
_refine_ls_goodness_of_fit_all    1.124
_refine_ls_goodness_of_fit_obs    1.117
_refine_ls_restrained_S_all       1.141
_refine_ls_restrained_S_obs       1.117
_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
Cr Cr 0.96499(3) 0.14792(4) 0.55945(3) 0.02046(13) Uani 1 d . .
Cl1 Cl 0.88598(5) 0.02043(6) 0.41048(5) 0.0292(2) Uani 1 d . .
Cl2 Cl 0.83122(5) 0.07250(7) 0.68747(5) 0.0362(2) Uani 1 d . .
C1 C 0.9590(4) 0.3347(3) 0.4584(3) 0.0593(11) Uani 1 d . .
H1 H 0.9206(4) 0.3392(3) 0.3896(3) 0.071 Uiso 1 calc R .
C2 C 0.9075(3) 0.3614(3) 0.5589(4) 0.0595(12) Uani 1 d . .
H2 H 0.8270(3) 0.3856(3) 0.5711(4) 0.071 Uiso 1 calc R .
C3 C 0.9945(5) 0.3464(3) 0.6389(3) 0.0631(11) Uani 1 d . .
H3 H 0.9841(5) 0.3595(3) 0.7150(3) 0.076 Uiso 1 calc R .
C4 C 1.0995(3) 0.3087(3) 0.5871(4) 0.0614(11) Uani 1 d . .
H4 H 1.1734(3) 0.2919(3) 0.6218(4) 0.074 Uiso 1 calc R .
C5 C 1.0777(4) 0.3002(3) 0.4768(4) 0.0610(11) Uani 1 d . .
H5 H 1.1336(4) 0.2751(3) 0.4226(4) 0.073 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
Cr 0.0233(2) 0.0135(2) 0.0245(2) -0.00022(13) -0.00097(12) -0.00181(12)
Cl1 0.0317(3) 0.0226(3) 0.0333(3) -0.0052(2) -0.0123(2) 0.0047(2)
Cl2 0.0335(3) 0.0417(4) 0.0333(3) 0.0093(3) 0.0026(2) -0.0080(3)
C1 0.109(3) 0.0180(14) 0.050(2) 0.0130(13) -0.031(2) -0.015(2)
C2 0.040(2) 0.0134(13) 0.125(4) 0.001(2) 0.019(2) 0.0047(10)
C3 0.130(3) 0.023(2) 0.037(2) -0.0108(13) 0.008(2) -0.030(2)
C4 0.045(2) 0.029(2) 0.110(3) 0.008(2) -0.029(2) -0.0176(14)
C5 0.074(2) 0.026(2) 0.083(3) 0.004(2) 0.047(2) -0.0106(15)

_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
Cr C2 2.198(3) . ?
Cr C5 2.199(3) . ?
Cr C3 2.205(3) . ?
Cr C4 2.207(3) . ?
Cr C1 2.213(3) . ?
Cr Cl2 2.2781(7) . ?
Cr Cl1 2.3713(7) . ?
Cr Cl1 2.3754(7) 5_756 ?
Cl1 Cr 2.3753(7) 5_756 ?
C1 C2 1.374(5) . ?
C1 C5 1.384(6) . ?
C2 C3 1.380(6) . ?
C3 C4 1.380(6) . ?
C4 C5 1.363(6) . ?

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 Cr C5 60.82(13) . . ?
C2 Cr C3 36.5(2) . . ?
C5 Cr C3 60.62(14) . . ?
C2 Cr C4 60.76(13) . . ?
C5 Cr C4 36.0(2) . . ?
C3 Cr C4 36.4(2) . . ?
C2 Cr C1 36.29(14) . . ?
C5 Cr C1 36.6(2) . . ?
C3 Cr C1 60.63(13) . . ?
C4 Cr C1 60.49(13) . . ?
C2 Cr Cl2 97.08(10) . . ?
C5 Cr Cl2 155.18(10) . . ?
C3 Cr Cl2 95.07(10) . . ?
C4 Cr Cl2 125.11(13) . . ?
C1 Cr Cl2 129.03(13) . . ?
C2 Cr Cl1 113.35(12) . . ?
C5 Cr Cl1 103.04(12) . . ?
C3 Cr Cl1 149.18(11) . . ?
C4 Cr Cl1 138.45(13) . . ?
C1 Cr Cl1 90.38(9) . . ?
Cl2 Cr Cl1 96.00(3) . . ?
C2 Cr Cl1 150.70(10) . 5_756 ?
C5 Cr Cl1 98.46(11) . 5_756 ?
C3 Cr Cl1 116.59(13) . 5_756 ?
C4 Cr Cl1 90.17(10) . 5_756 ?
C1 Cr Cl1 133.40(12) . 5_756 ?
Cl2 Cr Cl1 97.18(3) . 5_756 ?
Cl1 Cr Cl1 90.40(2) . 5_756 ?
Cr Cl1 Cr 89.60(2) . 5_756 ?
C2 C1 C5 107.6(3) . . ?
C2 C1 Cr 71.3(2) . . ?
C5 C1 Cr 71.2(2) . . ?
C1 C2 C3 108.1(3) . . ?
C1 C2 Cr 72.4(2) . . ?
C3 C2 Cr 72.0(2) . . ?
C4 C3 C2 107.7(3) . . ?
C4 C3 Cr 71.8(2) . . ?
C2 C3 Cr 71.5(2) . . ?
C5 C4 C3 108.3(3) . . ?
C5 C4 Cr 71.6(2) . . ?
C3 C4 Cr 71.7(2) . . ?
C4 C5 C1 108.3(3) . . ?
C4 C5 Cr 72.3(2) . . ?
C1 C5 Cr 72.3(2) . . ?

_refine_diff_density_max    0.504
_refine_diff_density_min   -0.570
_refine_diff_density_rms    0.096