# Copyright The Royal Society of Chemistry, 1999
# CCDC Number: 186/1427

data_1 
  
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C26 H46 F6 P3 Rh' 
_chemical_formula_weight          668.45 
_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' 
 'F'  'F'   0.0171   0.0103 
 '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' 
 'Rh'  'Rh'  -1.1178   0.9187 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    Cc 
  
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' 
  
_cell_length_a                    18.8181(6) 
_cell_length_b                    10.8572(3) 
_cell_length_c                    29.2564(10) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  96.7910(10) 
_cell_angle_gamma                 90.00 
_cell_volume                      5935.5(3) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     223(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
  
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.30 
_exptl_crystal_size_mid           0.18 
_exptl_crystal_size_min           0.10 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.496 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              2768 
_exptl_absorpt_coefficient_mu     0.789 
_exptl_absorpt_correction_type    empirical 
_exptl_absorpt_correction_T_min   0.721 
_exptl_absorpt_correction_T_max   0.792 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       223(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'normal-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device        'Siemens SMART' 
_diffrn_measurement_method        '\w scans' 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             14637 
_diffrn_reflns_av_R_equivalents   0.0536 
_diffrn_reflns_av_sigmaI/netI     0.0567 
_diffrn_reflns_limit_h_min        -24 
_diffrn_reflns_limit_h_max        25 
_diffrn_reflns_limit_k_min        -13 
_diffrn_reflns_limit_k_max        14 
_diffrn_reflns_limit_l_min        -38 
_diffrn_reflns_limit_l_max        15 
_diffrn_reflns_theta_min          2.17 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              7016 
_reflns_number_observed           6057 
_reflns_observed_criterion        2sigma(I) 
  
_computing_data_collection        'Siemens XSCANS' 
_computing_cell_refinement        'Siemens XSCANS' 
_computing_data_reduction         'Siemens SHELXTL' 
_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 131 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^)+(0.0311P)^2^+33.2706P] 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      none 
_refine_ls_extinction_coef        ? 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.78(6) 
_refine_ls_number_reflns          6885 
_refine_ls_number_parameters      660 
_refine_ls_number_restraints      2 
_refine_ls_R_factor_all           0.0673 
_refine_ls_R_factor_obs           0.0537 
_refine_ls_wR_factor_all          0.1142 
_refine_ls_wR_factor_obs          0.1060 
_refine_ls_goodness_of_fit_all    1.139 
_refine_ls_goodness_of_fit_obs    1.162 
_refine_ls_restrained_S_all       1.155 
_refine_ls_restrained_S_obs       1.162 
_refine_ls_shift/esd_max          -0.455 
_refine_ls_shift/esd_mean         0.076 
  
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 
Rh1 Rh 0.24690(3) 0.13550(6) 0.08244(3) 0.0285(2) Uani 1 d . . 
Rh2 Rh 0.65055(3) 0.89110(6) 0.38202(3) 0.0290(2) Uani 1 d . . 
P1 P 0.33008(14) 0.0244(3) 0.12503(10) 0.0288(7) Uani 1 d . . 
P2 P 0.33440(14) 0.2633(2) 0.10827(10) 0.0258(6) Uani 1 d . . 
P3 P 0.5681(2) 0.7769(3) 0.34024(11) 0.0344(7) Uani 1 d . . 
P4 P 0.56119(14) 1.0157(2) 0.35575(10) 0.0263(6) Uani 1 d . . 
P5 P 0.1234(2) 0.6226(3) 0.0922(2) 0.0370(9) Uani 1 d . . 
P6 P 0.2752(3) 0.8721(4) 0.3674(2) 0.0564(14) Uani 1 d . . 
C1 C 0.1216(7) 0.1044(12) 0.0850(6) 0.045(4) Uani 1 d . . 
C2 C 0.1517(8) 0.0143(12) 0.0549(7) 0.062(5) Uani 1 d . . 
H2A H 0.1529(8) -0.0720(12) 0.0646(7) 0.074 Uiso 1 calc R . 
C3 C 0.1870(8) 0.0441(14) 0.0169(5) 0.062(4) Uani 1 d . . 
H3A H 0.2100(8) -0.0197(14) 0.0001(5) 0.075 Uiso 1 calc R . 
C4 C 0.1948(8) 0.1673(14) 0.0070(5) 0.059(4) Uani 1 d . . 
H4A H 0.2250(8) 0.1913(14) -0.0166(5) 0.070 Uiso 1 calc R . 
C5 C 0.1717(6) 0.2562(12) 0.0357(5) 0.045(3) Uani 1 d . . 
H5A H 0.1848(6) 0.3423(12) 0.0313(5) 0.054 Uiso 1 calc R . 
C6 C 0.1358(7) 0.2269(12) 0.0720(6) 0.046(4) Uani 1 d . . 
H6A H 0.1261(7) 0.2932(12) 0.0932(6) 0.056 Uiso 1 calc R . 
C7 C 0.0754(10) 0.0624(19) 0.1190(9) 0.123(8) Uani 1 d . . 
H7A H 0.0267(16) 0.0588(137) 0.1049(16) 0.184 Uiso 1 calc R . 
H7B H 0.0789(64) 0.1189(82) 0.1444(26) 0.184 Uiso 1 calc R . 
H7C H 0.0903(55) -0.0180(66) 0.1299(42) 0.184 Uiso 1 calc R . 
C8 C 0.3110(6) -0.0620(10) 0.1767(4) 0.045(3) Uani 1 d . . 
H8A H 0.3140(6) -0.1499(10) 0.1696(4) 0.054 Uiso 1 calc R . 
C9 C 0.2375(7) -0.0379(14) 0.1893(5) 0.076(5) Uani 1 d . . 
H9A H 0.2305(19) -0.0841(69) 0.2164(19) 0.113 Uiso 1 calc R . 
H9B H 0.2025(7) -0.0626(78) 0.1644(14) 0.113 Uiso 1 calc R . 
H9C H 0.2322(18) 0.0484(20) 0.1952(31) 0.113 Uiso 1 calc R . 
C10 C 0.3660(8) -0.0357(15) 0.2198(5) 0.084(5) Uani 1 d . . 
H10A H 0.3594(40) -0.0942(67) 0.2436(15) 0.127 Uiso 1 calc R . 
H10B H 0.3587(40) 0.0461(41) 0.2308(24) 0.127 Uiso 1 calc R . 
H10C H 0.4138(8) -0.0427(101) 0.2116(11) 0.127 Uiso 1 calc R . 
C11 C 0.3799(6) -0.0889(9) 0.0936(4) 0.039(3) Uani 1 d . . 
H11A H 0.3966(6) -0.0444(9) 0.0677(4) 0.047 Uiso 1 calc R . 
C12 C 0.3304(7) -0.1895(10) 0.0727(5) 0.060(4) Uani 1 d . . 
H12A H 0.3577(10) -0.2497(45) 0.0582(28) 0.090 Uiso 1 calc R . 
H12B H 0.2950(31) -0.1542(17) 0.0501(23) 0.090 Uiso 1 calc R . 
H12C H 0.3073(37) -0.2282(56) 0.0964(7) 0.090 Uiso 1 calc R . 
C13 C 0.4464(6) -0.1433(12) 0.1210(5) 0.062(4) Uani 1 d . . 
H13A H 0.4768(22) -0.1781(71) 0.1002(5) 0.092 Uiso 1 calc R . 
H13B H 0.4325(6) -0.2065(57) 0.1411(22) 0.092 Uiso 1 calc R . 
H13C H 0.4718(26) -0.0797(21) 0.1389(23) 0.092 Uiso 1 calc R . 
C14 C 0.3139(5) 0.3887(9) 0.1475(4) 0.032(2) Uani 1 d . . 
H14A H 0.2784(5) 0.4421(9) 0.1301(4) 0.039 Uiso 1 calc R . 
C15 C 0.3788(5) 0.4702(9) 0.1643(4) 0.041(3) Uani 1 d . . 
H15A H 0.4153(5) 0.4212(9) 0.1821(4) 0.049 Uiso 1 calc R . 
H15B H 0.3992(5) 0.5047(9) 0.1382(4) 0.049 Uiso 1 calc R . 
C16 C 0.3542(7) 0.5733(10) 0.1940(5) 0.059(4) Uani 1 d . . 
H16A H 0.3195(7) 0.6242(10) 0.1755(5) 0.071 Uiso 1 calc R . 
H16B H 0.3948(7) 0.6248(10) 0.2049(5) 0.071 Uiso 1 calc R . 
C17 C 0.3209(7) 0.5236(11) 0.2348(4) 0.054(3) Uani 1 d . . 
H17A H 0.3558(7) 0.4754(11) 0.2542(4) 0.064 Uiso 1 calc R . 
H17B H 0.3056(7) 0.5913(11) 0.2530(4) 0.064 Uiso 1 calc R . 
C18 C 0.2579(7) 0.4445(11) 0.2181(5) 0.050(3) Uani 1 d . . 
H18A H 0.2217(7) 0.4944(11) 0.2005(5) 0.061 Uiso 1 calc R . 
H18B H 0.2373(7) 0.4108(11) 0.2443(5) 0.061 Uiso 1 calc R . 
C19 C 0.2799(6) 0.3393(10) 0.1880(4) 0.044(3) Uani 1 d . . 
H19A H 0.3137(6) 0.2860(10) 0.2062(4) 0.053 Uiso 1 calc R . 
H19B H 0.2382(6) 0.2906(10) 0.1770(4) 0.053 Uiso 1 calc R . 
C20 C 0.3878(5) 0.3370(8) 0.0667(4) 0.030(2) Uani 1 d . . 
H20A H 0.4305(5) 0.3725(8) 0.0843(4) 0.036 Uiso 1 calc R . 
C21 C 0.3460(5) 0.4435(8) 0.0409(4) 0.030(2) Uani 1 d . . 
H21A H 0.3031(5) 0.4115(8) 0.0233(4) 0.036 Uiso 1 calc R . 
H21B H 0.3317(5) 0.5024(8) 0.0630(4) 0.036 Uiso 1 calc R . 
C22 C 0.3922(6) 0.5075(9) 0.0088(4) 0.038(3) Uani 1 d . . 
H22A H 0.4329(6) 0.5455(9) 0.0268(4) 0.045 Uiso 1 calc R . 
H22B H 0.3645(6) 0.5721(9) -0.0079(4) 0.045 Uiso 1 calc R . 
C23 C 0.4189(7) 0.4165(12) -0.0258(5) 0.049(4) Uani 1 d . . 
H23A H 0.3785(7) 0.3848(12) -0.0460(5) 0.059 Uiso 1 calc R . 
H23B H 0.4504(7) 0.4590(12) -0.0445(5) 0.059 Uiso 1 calc R . 
C24 C 0.4591(7) 0.3098(12) -0.0005(5) 0.046(4) Uani 1 d . . 
H24A H 0.5026(7) 0.3405(12) 0.0169(5) 0.055 Uiso 1 calc R . 
H24B H 0.4726(7) 0.2507(12) -0.0228(5) 0.055 Uiso 1 calc R . 
C25 C 0.4130(5) 0.2451(9) 0.0325(4) 0.034(3) Uani 1 d . . 
H25A H 0.3718(5) 0.2073(9) 0.0148(4) 0.040 Uiso 1 calc R . 
H25B H 0.4408(5) 0.1805(9) 0.0491(4) 0.040 Uiso 1 calc R . 
C27 C 0.7754(9) 0.8494(15) 0.3859(5) 0.047(4) Uani 1 d . . 
C28 C 0.7660(6) 0.9767(11) 0.3906(5) 0.040(3) Uani 1 d . . 
H28A H 0.7811(6) 1.0352(11) 0.3681(5) 0.049 Uiso 1 calc R . 
C29 C 0.7264(6) 1.0158(12) 0.4268(5) 0.044(3) Uani 1 d . . 
H29A H 0.7144(6) 1.1032(12) 0.4290(5) 0.053 Uiso 1 calc R . 
C30 C 0.6993(7) 0.9317(12) 0.4570(5) 0.055(4) Uani 1 d . . 
H30A H 0.6691(7) 0.9598(12) 0.4800(5) 0.066 Uiso 1 calc R . 
C31 C 0.7087(7) 0.8084(12) 0.4492(5) 0.054(4) Uani 1 d . . 
H31A H 0.6829(7) 0.7490(12) 0.4664(5) 0.065 Uiso 1 calc R . 
C32 C 0.7431(7) 0.7656(11) 0.4124(5) 0.042(3) Uani 1 d . . 
H32A H 0.7428(7) 0.6776(11) 0.4049(5) 0.051 Uiso 1 calc R . 
C33 C 0.8205(7) 0.8086(14) 0.3493(5) 0.060(4) Uani 1 d . . 
H33A H 0.8702(8) 0.8198(76) 0.3602(12) 0.090 Uiso 1 calc R . 
H33B H 0.8084(34) 0.8569(56) 0.3220(11) 0.090 Uiso 1 calc R . 
H33C H 0.8115(35) 0.7232(25) 0.3423(22) 0.090 Uiso 1 calc R . 
C34 C 0.5857(6) 0.6932(14) 0.2884(5) 0.067(4) Uani 1 d . . 
H34A H 0.5746(6) 0.6079(14) 0.2960(5) 0.080 Uiso 1 calc R . 
C35 C 0.6587(8) 0.6854(20) 0.2807(6) 0.112(7) Uani 1 d . . 
H35A H 0.6617(9) 0.6586(125) 0.2497(16) 0.169 Uiso 1 calc R . 
H35B H 0.6830(19) 0.6273(92) 0.3019(32) 0.169 Uiso 1 calc R . 
H35C H 0.6807(21) 0.7648(32) 0.2854(46) 0.169 Uiso 1 calc R . 
C36 C 0.5389(12) 0.7141(24) 0.2472(7) 0.184(14) Uani 1 d . . 
H36A H 0.5456(100) 0.6504(137) 0.2253(34) 0.276 Uiso 1 calc R . 
H36B H 0.5495(89) 0.7926(111) 0.2345(46) 0.276 Uiso 1 calc R . 
H36C H 0.4903(12) 0.7133(230) 0.2539(17) 0.276 Uiso 1 calc R . 
C37 C 0.5205(6) 0.6625(9) 0.3729(5) 0.050(3) Uani 1 d . . 
H37A H 0.5036(6) 0.7070(9) 0.3986(5) 0.060 Uiso 1 calc R . 
C38 C 0.5709(7) 0.5648(10) 0.3935(5) 0.060(4) Uani 1 d . . 
H38A H 0.5453(13) 0.5074(49) 0.4103(27) 0.091 Uiso 1 calc R . 
H38B H 0.6084(29) 0.6023(14) 0.4139(25) 0.091 Uiso 1 calc R . 
H38C H 0.5913(38) 0.5222(57) 0.3694(6) 0.091 Uiso 1 calc R . 
C39 C 0.4540(6) 0.6063(12) 0.3449(5) 0.068(4) Uani 1 d . . 
H39A H 0.4303(28) 0.5525(66) 0.3643(10) 0.102 Uiso 1 calc R . 
H39B H 0.4683(8) 0.5603(72) 0.3195(19) 0.102 Uiso 1 calc R . 
H39C H 0.4219(24) 0.6709(13) 0.3335(27) 0.102 Uiso 1 calc R . 
C40 C 0.5773(5) 1.1409(9) 0.3158(3) 0.028(2) Uani 1 d . . 
H40A H 0.6089(5) 1.1999(9) 0.3335(3) 0.033 Uiso 1 calc R . 
C41 C 0.6170(6) 1.0970(10) 0.2760(4) 0.042(3) Uani 1 d . . 
H41A H 0.6614(6) 1.0576(10) 0.2884(4) 0.050 Uiso 1 calc R . 
H41B H 0.5880(6) 1.0366(10) 0.2579(4) 0.050 Uiso 1 calc R . 
C42 C 0.6333(7) 1.2041(10) 0.2451(4) 0.048(3) Uani 1 d . . 
H42A H 0.6672(7) 1.2591(10) 0.2624(4) 0.058 Uiso 1 calc R . 
H42B H 0.6556(7) 1.1723(10) 0.2193(4) 0.058 Uiso 1 calc R . 
C43 C 0.5671(7) 1.2759(11) 0.2272(4) 0.051(3) Uani 1 d . . 
H43A H 0.5804(7) 1.3465(11) 0.2098(4) 0.061 Uiso 1 calc R . 
H43B H 0.5355(7) 1.2242(11) 0.2067(4) 0.061 Uiso 1 calc R . 
C44 C 0.5281(7) 1.3192(11) 0.2670(4) 0.050(3) Uani 1 d . . 
H44A H 0.4844(7) 1.3613(11) 0.2549(4) 0.060 Uiso 1 calc R . 
H44B H 0.5580(7) 1.3776(11) 0.2855(4) 0.060 Uiso 1 calc R . 
C45 C 0.5095(6) 1.2121(10) 0.2974(4) 0.042(3) Uani 1 d . . 
H45A H 0.4762(6) 1.1571(10) 0.2797(4) 0.050 Uiso 1 calc R . 
H45B H 0.4865(6) 1.2435(10) 0.3230(4) 0.050 Uiso 1 calc R . 
C46 C 0.5081(5) 1.0877(8) 0.3972(4) 0.030(2) Uani 1 d . . 
H46A H 0.4643(5) 1.1201(8) 0.3800(4) 0.036 Uiso 1 calc R . 
C47 C 0.4859(6) 0.9954(9) 0.4327(4) 0.036(3) Uani 1 d . . 
H47A H 0.4605(6) 0.9269(9) 0.4169(4) 0.044 Uiso 1 calc R . 
H47B H 0.5281(6) 0.9632(9) 0.4510(4) 0.044 Uiso 1 calc R . 
C48 C 0.4378(7) 1.0588(11) 0.4640(4) 0.036(3) Uani 1 d . . 
H48A H 0.3944(7) 1.0873(11) 0.4458(4) 0.043 Uiso 1 calc R . 
H48B H 0.4243(7) 1.0006(11) 0.4866(4) 0.043 Uiso 1 calc R . 
C49 C 0.4770(7) 1.1683(11) 0.4884(4) 0.037(3) Uani 1 d . . 
H49A H 0.4451(7) 1.2098(11) 0.5072(4) 0.045 Uiso 1 calc R . 
H49B H 0.5177(7) 1.1382(11) 0.5088(4) 0.045 Uiso 1 calc R . 
C50 C 0.5024(6) 1.2587(9) 0.4554(4) 0.036(3) Uani 1 d . . 
H50A H 0.5306(6) 1.3221(9) 0.4724(4) 0.043 Uiso 1 calc R . 
H50B H 0.4615(6) 1.2980(9) 0.4381(4) 0.043 Uiso 1 calc R . 
C51 C 0.5476(6) 1.1958(8) 0.4222(4) 0.034(2) Uani 1 d . . 
H51A H 0.5599(6) 1.2554(8) 0.3997(4) 0.041 Uiso 1 calc R . 
H51B H 0.5918(6) 1.1663(8) 0.4391(4) 0.041 Uiso 1 calc R . 
C52 C 0.3938(6) 0.1512(8) 0.1412(4) 0.033(3) Uani 1 d . . 
H52A H 0.4007(6) 0.1676(8) 0.1741(4) 0.040 Uiso 1 calc R . 
H52B H 0.4395(6) 0.1408(8) 0.1294(4) 0.040 Uiso 1 calc R . 
C53 C 0.5046(6) 0.8974(9) 0.3246(4) 0.034(3) Uani 1 d . . 
H53A H 0.4594(6) 0.8853(9) 0.3369(4) 0.041 Uiso 1 calc R . 
H53B H 0.4965(6) 0.9119(9) 0.2917(4) 0.041 Uiso 1 calc R . 
F1 F 0.1128(6) 0.5330(10) 0.1342(3) 0.108(4) Uani 1 d . . 
F2 F 0.1818(5) 0.5342(8) 0.0761(4) 0.098(3) Uani 1 d . . 
F3 F 0.0652(5) 0.7153(9) 0.1072(3) 0.091(3) Uani 1 d . . 
F4 F 0.1823(5) 0.6933(8) 0.1245(3) 0.085(3) Uani 1 d . . 
F5 F 0.0627(5) 0.5535(8) 0.0602(4) 0.097(3) Uani 1 d . . 
F6 F 0.1353(6) 0.7128(8) 0.0515(3) 0.077(3) Uani 1 d . . 
F7 F 0.2851(9) 0.7774(15) 0.3307(6) 0.179(7) Uani 1 d . . 
F8 F 0.3338(6) 0.8062(9) 0.4000(5) 0.123(5) Uani 1 d . . 
F9 F 0.2170(6) 0.7859(11) 0.3837(6) 0.144(5) Uani 1 d . . 
F10 F 0.3331(6) 0.9626(11) 0.3532(5) 0.142(5) Uani 1 d . . 
F11 F 0.2151(6) 0.9352(11) 0.3343(4) 0.129(4) Uani 1 d . . 
F12 F 0.2654(8) 0.9657(10) 0.4061(5) 0.121(5) 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 
Rh1 0.0288(5) 0.0228(3) 0.0332(5) 0.0009(4) 0.0006(4) 0.0003(3) 
Rh2 0.0281(5) 0.0241(3) 0.0345(5) -0.0009(4) 0.0021(4) -0.0002(3) 
P1 0.030(2) 0.0243(13) 0.033(2) 0.0073(12) 0.0061(13) 0.0035(11) 
P2 0.0281(15) 0.0209(13) 0.028(2) 0.0018(12) 0.0030(12) -0.0005(11) 
P3 0.031(2) 0.0343(15) 0.038(2) -0.0126(14) 0.0061(14) -0.0017(12) 
P4 0.0273(15) 0.0251(13) 0.027(2) -0.0017(13) 0.0046(12) 0.0005(11) 
P5 0.039(2) 0.033(2) 0.038(2) -0.0023(14) 0.004(2) -0.0017(13) 
P6 0.041(3) 0.046(2) 0.080(4) 0.000(2) -0.001(2) -0.001(2) 
C1 0.011(6) 0.046(7) 0.079(11) 0.036(7) 0.005(6) -0.006(5) 
C2 0.048(9) 0.024(6) 0.103(15) -0.002(8) -0.035(9) -0.007(6) 
C3 0.058(10) 0.068(9) 0.058(10) -0.040(8) -0.008(8) 0.000(7) 
C4 0.050(9) 0.089(10) 0.034(8) 0.003(7) -0.011(7) 0.021(8) 
C5 0.028(7) 0.048(7) 0.055(9) 0.002(7) -0.008(6) 0.003(5) 
C6 0.024(7) 0.033(7) 0.077(11) 0.004(7) -0.018(7) 0.001(5) 
C7 0.073(14) 0.102(14) 0.201(26) 0.023(16) 0.046(15) 0.009(11) 
C8 0.050(8) 0.039(6) 0.048(8) 0.022(6) 0.013(6) -0.001(5) 
C9 0.063(9) 0.094(10) 0.080(11) 0.030(9) 0.048(8) 0.033(8) 
C10 0.075(10) 0.120(13) 0.051(9) 0.040(9) -0.023(8) -0.015(9) 
C11 0.048(7) 0.034(6) 0.039(7) 0.010(5) 0.018(6) 0.012(5) 
C12 0.058(8) 0.042(6) 0.084(11) -0.032(7) 0.026(8) -0.005(6) 
C13 0.047(7) 0.068(8) 0.072(9) 0.010(8) 0.017(7) 0.025(7) 
C14 0.033(5) 0.028(5) 0.033(6) 0.008(5) -0.007(5) 0.001(4) 
C15 0.033(6) 0.047(6) 0.044(7) -0.001(5) 0.005(5) -0.011(5) 
C16 0.079(9) 0.036(6) 0.061(9) -0.022(6) 0.000(7) -0.005(6) 
C17 0.078(9) 0.047(7) 0.036(8) -0.016(6) 0.009(7) -0.003(6) 
C18 0.059(8) 0.055(7) 0.038(7) -0.022(6) 0.012(6) 0.001(6) 
C19 0.045(7) 0.048(7) 0.040(7) 0.001(6) 0.006(6) 0.008(5) 
C20 0.028(5) 0.026(5) 0.034(6) 0.005(5) -0.001(5) -0.012(4) 
C21 0.035(6) 0.029(5) 0.028(6) -0.001(4) 0.006(5) -0.004(4) 
C22 0.045(6) 0.031(5) 0.038(7) 0.006(5) 0.010(5) 0.001(5) 
C23 0.048(8) 0.045(7) 0.054(9) 0.004(6) 0.005(7) 0.000(6) 
C24 0.037(7) 0.039(7) 0.062(10) -0.011(6) 0.005(7) 0.005(5) 
C25 0.029(6) 0.030(5) 0.042(7) -0.001(5) 0.007(5) 0.006(4) 
C27 0.034(8) 0.065(9) 0.037(9) 0.005(7) -0.011(7) 0.009(7) 
C28 0.021(6) 0.043(7) 0.054(9) 0.015(6) -0.008(6) -0.010(5) 
C29 0.031(7) 0.037(6) 0.061(9) -0.005(7) -0.013(6) -0.006(5) 
C30 0.035(7) 0.070(8) 0.054(9) -0.010(8) -0.019(7) 0.008(6) 
C31 0.056(9) 0.061(8) 0.043(8) 0.019(7) -0.007(7) -0.005(6) 
C32 0.046(8) 0.025(6) 0.055(9) 0.015(6) 0.005(7) 0.005(5) 
C33 0.048(8) 0.098(11) 0.035(8) -0.016(8) 0.003(6) 0.017(7) 
C34 0.037(7) 0.095(10) 0.073(11) -0.054(9) 0.022(7) -0.004(7) 
C35 0.086(13) 0.180(19) 0.075(13) -0.054(13) 0.025(11) 0.050(13) 
C36 0.165(20) 0.296(29) 0.072(14) -0.123(17) -0.062(13) 0.169(20) 
C37 0.052(7) 0.031(6) 0.071(9) -0.004(6) 0.024(7) 0.001(5) 
C38 0.070(9) 0.034(6) 0.082(11) 0.022(7) 0.029(8) 0.001(6) 
C39 0.048(7) 0.065(8) 0.096(11) -0.032(8) 0.024(7) -0.034(7) 
C40 0.029(5) 0.032(5) 0.024(5) 0.008(5) 0.011(4) -0.005(4) 
C41 0.054(7) 0.044(6) 0.031(6) 0.008(5) 0.019(5) 0.014(5) 
C42 0.060(8) 0.048(7) 0.042(8) -0.008(6) 0.024(7) 0.002(6) 
C43 0.056(8) 0.059(7) 0.037(8) 0.020(6) 0.000(6) -0.005(6) 
C44 0.059(7) 0.060(7) 0.033(7) 0.011(6) 0.012(6) 0.022(6) 
C45 0.045(6) 0.047(6) 0.033(7) 0.002(5) 0.008(5) 0.015(5) 
C46 0.029(5) 0.027(5) 0.034(6) 0.000(5) 0.006(5) 0.002(4) 
C47 0.047(7) 0.029(5) 0.034(7) 0.003(5) 0.011(5) -0.009(5) 
C48 0.046(8) 0.033(6) 0.034(7) -0.004(5) 0.025(6) -0.005(5) 
C49 0.059(8) 0.040(6) 0.015(6) -0.010(5) 0.015(6) 0.003(5) 
C50 0.049(7) 0.028(5) 0.030(7) -0.008(5) 0.004(5) 0.003(5) 
C51 0.045(6) 0.023(5) 0.035(6) -0.001(4) 0.010(5) -0.009(4) 
C52 0.032(7) 0.028(5) 0.039(7) 0.007(5) 0.003(6) -0.002(4) 
C53 0.031(7) 0.041(6) 0.029(7) -0.011(5) -0.001(5) -0.012(5) 
F1 0.119(9) 0.128(8) 0.072(7) 0.056(6) -0.014(6) -0.041(7) 
F2 0.101(8) 0.090(7) 0.104(8) -0.012(6) 0.010(6) 0.063(6) 
F3 0.072(6) 0.118(7) 0.084(7) -0.024(6) 0.019(5) 0.034(5) 
F4 0.071(6) 0.105(6) 0.075(6) -0.017(5) -0.006(5) -0.037(5) 
F5 0.093(7) 0.084(6) 0.103(8) -0.021(6) -0.036(6) -0.015(5) 
F6 0.110(8) 0.062(5) 0.064(6) 0.012(5) 0.029(6) 0.010(5) 
F7 0.168(14) 0.196(15) 0.170(14) -0.082(12) 0.001(11) 0.080(11) 
F8 0.114(8) 0.075(6) 0.160(11) 0.017(7) -0.069(8) 0.012(6) 
F9 0.105(9) 0.114(9) 0.210(16) 0.026(9) 0.000(10) -0.064(7) 
F10 0.098(9) 0.153(10) 0.177(13) 0.077(9) 0.028(8) -0.024(7) 
F11 0.099(8) 0.140(9) 0.137(11) 0.021(8) -0.034(8) 0.033(7) 
F12 0.144(11) 0.082(7) 0.138(11) -0.043(7) 0.017(9) 0.015(7) 
  
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. 
planes) 
 are estimated using the full covariance matrix.  The cell esds are 
taken 
 into account individually in the estimation of esds in distances, 
angles 
 and torsion angles; correlations between esds in cell parameters are 
only 
 used when they are defined by crystal symmetry.  An approximate 
(isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. 
planes. 
; 
  
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Rh1 P2 2.217(3) . ? 
Rh1 P1 2.235(3) . ? 
Rh1 C5 2.265(12) . ? 
Rh1 C2 2.291(13) . ? 
Rh1 C6 2.302(13) . ? 
Rh1 C4 2.332(13) . ? 
Rh1 C3 2.327(13) . ? 
Rh1 C1 2.392(14) . ? 
Rh2 P4 2.223(3) . ? 
Rh2 P3 2.234(3) . ? 
Rh2 C29 2.268(12) . ? 
Rh2 C32 2.305(12) . ? 
Rh2 C31 2.316(13) . ? 
Rh2 C30 2.318(14) . ? 
Rh2 C28 2.349(12) . ? 
Rh2 C27 2.38(2) . ? 
P1 C8 1.850(11) . ? 
P1 C11 1.857(11) . ? 
P1 C52 1.850(10) . ? 
P1 P2 2.643(4) . ? 
P2 C20 1.849(10) . ? 
P2 C14 1.850(11) . ? 
P2 C52 1.846(11) . ? 
P3 C53 1.795(12) . ? 
P3 C34 1.832(13) . ? 
P3 C37 1.858(12) . ? 
P3 P4 2.638(4) . ? 
P4 C46 1.835(10) . ? 
P4 C53 1.840(10) . ? 
P4 C40 1.841(10) . ? 
P5 F2 1.573(9) . ? 
P5 F4 1.570(9) . ? 
P5 F5 1.578(9) . ? 
P5 F6 1.578(10) . ? 
P5 F3 1.587(9) . ? 
P5 F1 1.598(10) . ? 
P6 F7 1.514(14) . ? 
P6 F8 1.545(10) . ? 
P6 F12 1.550(13) . ? 
P6 F11 1.558(10) . ? 
P6 F10 1.560(11) . ? 
P6 F9 1.557(12) . ? 
C1 C6 1.42(2) . ? 
C1 C2 1.47(2) . ? 
C1 C7 1.47(3) . ? 
C2 C3 1.40(2) . ? 
C3 C4 1.38(2) . ? 
C4 C5 1.38(2) . ? 
C5 C6 1.36(2) . ? 
C8 C9 1.50(2) . ? 
C8 C10 1.56(2) . ? 
C11 C12 1.516(15) . ? 
C11 C13 1.522(14) . ? 
C14 C19 1.51(2) . ? 
C14 C15 1.541(13) . ? 
C15 C16 1.52(2) . ? 
C16 C17 1.51(2) . ? 
C17 C18 1.50(2) . ? 
C18 C19 1.53(2) . ? 
C20 C25 1.529(14) . ? 
C20 C21 1.543(13) . ? 
C21 C22 1.521(14) . ? 
C22 C23 1.54(2) . ? 
C23 C24 1.526(13) . ? 
C24 C25 1.54(2) . ? 
C27 C28 1.40(2) . ? 
C27 C32 1.38(2) . ? 
C27 C33 1.51(2) . ? 
C28 C29 1.43(2) . ? 
C29 C30 1.41(2) . ? 
C30 C31 1.37(2) . ? 
C31 C32 1.40(2) . ? 
C34 C35 1.42(2) . ? 
C34 C36 1.42(2) . ? 
C37 C38 1.50(2) . ? 
C37 C39 1.54(2) . ? 
C40 C41 1.531(14) . ? 
C40 C45 1.534(13) . ? 
C41 C42 1.53(2) . ? 
C42 C43 1.51(2) . ? 
C43 C44 1.52(2) . ? 
C44 C45 1.53(2) . ? 
C46 C51 1.529(13) . ? 
C46 C47 1.536(14) . ? 
C47 C48 1.526(15) . ? 
C48 C49 1.532(12) . ? 
C49 C50 1.50(2) . ? 
C50 C51 1.526(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 
P2 Rh1 P1 72.82(11) . . ? 
P2 Rh1 C5 103.3(3) . . ? 
P1 Rh1 C5 174.2(4) . . ? 
P2 Rh1 C2 176.3(4) . . ? 
P1 Rh1 C2 110.7(3) . . ? 
C5 Rh1 C2 73.3(5) . . ? 
P2 Rh1 C6 113.7(3) . . ? 
P1 Rh1 C6 150.7(4) . . ? 
C5 Rh1 C6 34.7(5) . . ? 
C2 Rh1 C6 62.7(5) . . ? 
P2 Rh1 C4 116.2(4) . . ? 
P1 Rh1 C4 142.7(4) . . ? 
C5 Rh1 C4 35.0(5) . . ? 
C2 Rh1 C4 61.8(6) . . ? 
C6 Rh1 C4 62.5(6) . . ? 
P2 Rh1 C3 144.6(5) . . ? 
P1 Rh1 C3 117.9(4) . . ? 
C5 Rh1 C3 62.8(5) . . ? 
C2 Rh1 C3 35.2(6) . . ? 
C6 Rh1 C3 74.4(5) . . ? 
C4 Rh1 C3 34.4(5) . . ? 
P2 Rh1 C1 140.6(4) . . ? 
P1 Rh1 C1 122.3(3) . . ? 
C5 Rh1 C1 63.4(5) . . ? 
C2 Rh1 C1 36.6(6) . . ? 
C6 Rh1 C1 35.1(4) . . ? 
C4 Rh1 C1 75.2(6) . . ? 
C3 Rh1 C1 65.3(6) . . ? 
P4 Rh2 P3 72.57(11) . . ? 
P4 Rh2 C29 103.6(3) . . ? 
P3 Rh2 C29 175.1(4) . . ? 
P4 Rh2 C32 177.5(4) . . ? 
P3 Rh2 C32 109.1(3) . . ? 
C29 Rh2 C32 74.6(5) . . ? 
P4 Rh2 C31 142.3(4) . . ? 
P3 Rh2 C31 118.5(3) . . ? 
C29 Rh2 C31 62.6(5) . . ? 
C32 Rh2 C31 35.3(5) . . ? 
P4 Rh2 C30 114.2(3) . . ? 
P3 Rh2 C30 142.7(4) . . ? 
C29 Rh2 C30 35.7(5) . . ? 
C32 Rh2 C30 63.3(5) . . ? 
C31 Rh2 C30 34.5(5) . . ? 
P4 Rh2 C28 116.6(3) . . ? 
P3 Rh2 C28 148.4(4) . . ? 
C29 Rh2 C28 36.0(5) . . ? 
C32 Rh2 C28 63.0(5) . . ? 
C31 Rh2 C28 74.0(5) . . ? 
C30 Rh2 C28 64.3(5) . . ? 
P4 Rh2 C27 146.5(4) . . ? 
P3 Rh2 C27 122.6(4) . . ? 
C29 Rh2 C27 62.4(5) . . ? 
C32 Rh2 C27 34.3(5) . . ? 
C31 Rh2 C27 61.4(5) . . ? 
C30 Rh2 C27 73.3(5) . . ? 
C28 Rh2 C27 34.5(5) . . ? 
C8 P1 C11 103.1(5) . . ? 
C8 P1 C52 110.5(6) . . ? 
C11 P1 C52 105.7(5) . . ? 
C8 P1 Rh1 122.6(4) . . ? 
C11 P1 Rh1 116.3(4) . . ? 
C52 P1 Rh1 97.6(3) . . ? 
C8 P1 P2 131.5(4) . . ? 
C11 P1 P2 122.0(4) . . ? 
C52 P1 P2 44.3(3) . . ? 
Rh1 P1 P2 53.27(8) . . ? 
C20 P2 C14 105.0(5) . . ? 
C20 P2 C52 106.7(5) . . ? 
C14 P2 C52 108.6(5) . . ? 
C20 P2 Rh1 119.1(3) . . ? 
C14 P2 Rh1 118.1(3) . . ? 
C52 P2 Rh1 98.3(3) . . ? 
C20 P2 P1 125.3(3) . . ? 
C14 P2 P1 126.5(4) . . ? 
C52 P2 P1 44.4(3) . . ? 
Rh1 P2 P1 53.91(8) . . ? 
C53 P3 C34 109.3(7) . . ? 
C53 P3 C37 105.8(5) . . ? 
C34 P3 C37 103.8(7) . . ? 
C53 P3 Rh2 97.6(3) . . ? 
C34 P3 Rh2 123.1(4) . . ? 
C37 P3 Rh2 115.8(4) . . ? 
C53 P3 P4 44.1(3) . . ? 
C34 P3 P4 130.3(6) . . ? 
C37 P3 P4 122.1(4) . . ? 
Rh2 P3 P4 53.52(9) . . ? 
C46 P4 C53 107.2(5) . . ? 
C46 P4 C40 104.4(4) . . ? 
C53 P4 C40 109.3(5) . . ? 
C46 P4 Rh2 118.6(4) . . ? 
C53 P4 Rh2 96.7(4) . . ? 
C40 P4 Rh2 119.6(3) . . ? 
C46 P4 P3 125.0(3) . . ? 
C53 P4 P3 42.8(4) . . ? 
C40 P4 P3 127.0(4) . . ? 
Rh2 P4 P3 53.91(9) . . ? 
F2 P5 F4 90.5(6) . . ? 
F2 P5 F5 90.8(6) . . ? 
F4 P5 F5 178.6(7) . . ? 
F2 P5 F6 89.2(6) . . ? 
F4 P5 F6 89.9(6) . . ? 
F5 P5 F6 90.3(6) . . ? 
F2 P5 F3 178.0(6) . . ? 
F4 P5 F3 89.1(5) . . ? 
F5 P5 F3 89.5(6) . . ? 
F6 P5 F3 88.9(5) . . ? 
F2 P5 F1 90.8(6) . . ? 
F4 P5 F1 88.7(6) . . ? 
F5 P5 F1 91.2(6) . . ? 
F6 P5 F1 178.6(7) . . ? 
F3 P5 F1 91.2(7) . . ? 
F7 P6 F8 89.1(8) . . ? 
F7 P6 F12 178.3(10) . . ? 
F8 P6 F12 89.5(8) . . ? 
F7 P6 F11 89.9(8) . . ? 
F8 P6 F11 178.5(7) . . ? 
F12 P6 F11 91.4(8) . . ? 
F7 P6 F10 95.1(11) . . ? 
F8 P6 F10 89.3(7) . . ? 
F12 P6 F10 86.0(8) . . ? 
F11 P6 F10 92.0(7) . . ? 
F7 P6 F9 87.7(10) . . ? 
F8 P6 F9 90.6(7) . . ? 
F12 P6 F9 91.3(9) . . ? 
F11 P6 F9 88.2(8) . . ? 
F10 P6 F9 177.2(9) . . ? 
C6 C1 C2 111.4(14) . . ? 
C6 C1 C7 128.2(17) . . ? 
C2 C1 C7 120.0(14) . . ? 
C6 C1 Rh1 69.0(8) . . ? 
C2 C1 Rh1 67.9(8) . . ? 
C7 C1 Rh1 136.8(14) . . ? 
C3 C2 C1 125.1(12) . . ? 
C3 C2 Rh1 73.8(8) . . ? 
C1 C2 Rh1 75.4(8) . . ? 
C4 C3 C2 117.7(13) . . ? 
C4 C3 Rh1 73.0(7) . . ? 
C2 C3 Rh1 71.0(8) . . ? 
C5 C4 C3 119.9(15) . . ? 
C5 C4 Rh1 69.8(8) . . ? 
C3 C4 Rh1 72.6(8) . . ? 
C6 C5 C4 122.1(14) . . ? 
C6 C5 Rh1 74.2(8) . . ? 
C4 C5 Rh1 75.2(8) . . ? 
C5 C6 C1 123.7(15) . . ? 
C5 C6 Rh1 71.2(8) . . ? 
C1 C6 Rh1 75.9(8) . . ? 
C9 C8 C10 108.2(12) . . ? 
C9 C8 P1 112.8(8) . . ? 
C10 C8 P1 113.1(8) . . ? 
C12 C11 C13 111.1(10) . . ? 
C12 C11 P1 110.8(8) . . ? 
C13 C11 P1 115.3(9) . . ? 
C19 C14 C15 110.2(9) . . ? 
C19 C14 P2 111.3(7) . . ? 
C15 C14 P2 113.9(7) . . ? 
C16 C15 C14 108.7(9) . . ? 
C15 C16 C17 111.7(10) . . ? 
C18 C17 C16 109.4(11) . . ? 
C17 C18 C19 111.0(10) . . ? 
C14 C19 C18 110.8(10) . . ? 
C25 C20 C21 110.4(9) . . ? 
C25 C20 P2 112.5(6) . . ? 
C21 C20 P2 111.2(7) . . ? 
C22 C21 C20 110.5(8) . . ? 
C21 C22 C23 111.6(9) . . ? 
C24 C23 C22 110.6(10) . . ? 
C23 C24 C25 111.4(10) . . ? 
C20 C25 C24 110.7(8) . . ? 
C28 C27 C32 121.7(15) . . ? 
C28 C27 C33 116.5(15) . . ? 
C32 C27 C33 121.8(14) . . ? 
C28 C27 Rh2 71.5(8) . . ? 
C32 C27 Rh2 69.8(9) . . ? 
C33 C27 Rh2 130.9(10) . . ? 
C27 C28 C29 116.6(13) . . ? 
C27 C28 Rh2 74.1(8) . . ? 
C29 C28 Rh2 68.9(7) . . ? 
C30 C29 C28 122.1(12) . . ? 
C30 C29 Rh2 74.1(7) . . ? 
C28 C29 Rh2 75.1(7) . . ? 
C31 C30 C29 117.8(14) . . ? 
C31 C30 Rh2 72.7(7) . . ? 
C29 C30 Rh2 70.2(8) . . ? 
C30 C31 C32 122.1(13) . . ? 
C30 C31 Rh2 72.8(7) . . ? 
C32 C31 Rh2 72.0(8) . . ? 
C31 C32 C27 119.1(13) . . ? 
C31 C32 Rh2 72.8(7) . . ? 
C27 C32 Rh2 75.9(8) . . ? 
C35 C34 C36 112.9(17) . . ? 
C35 C34 P3 115.7(10) . . ? 
C36 C34 P3 117.9(10) . . ? 
C38 C37 C39 111.6(10) . . ? 
C38 C37 P3 111.0(8) . . ? 
C39 C37 P3 113.8(10) . . ? 
C41 C40 C45 110.5(8) . . ? 
C41 C40 P4 112.6(7) . . ? 
C45 C40 P4 113.7(7) . . ? 
C42 C41 C40 111.4(9) . . ? 
C43 C42 C41 112.5(10) . . ? 
C44 C43 C42 110.2(10) . . ? 
C43 C44 C45 112.0(10) . . ? 
C44 C45 C40 110.5(9) . . ? 
C51 C46 C47 109.5(9) . . ? 
C51 C46 P4 111.8(7) . . ? 
C47 C46 P4 112.5(6) . . ? 
C48 C47 C46 109.8(8) . . ? 
C49 C48 C47 110.1(9) . . ? 
C50 C49 C48 112.3(9) . . ? 
C49 C50 C51 111.3(8) . . ? 
C46 C51 C50 111.8(8) . . ? 
P2 C52 P1 91.3(5) . . ? 
P3 C53 P4 93.1(5) . . ? 
  
_refine_diff_density_max    1.406 
_refine_diff_density_min   -0.404 
_refine_diff_density_rms    0.092 


data_mm2wb 

_publ_author_name
;
  Justin Wolf,a Matthias Manger,a Ulrich Schmidt,a Guido Fries,
  a Dietmar Barth,a Birgit Weberndrfer,a David A. Vicic,
  b William D. Jonesb and Helmut Werner
;

_publ_author_address
;
        Prof. Dr. Helmut Werner
        Institut f\"ur Anorganische Chemie
        Universit\"at W\"urzburg
        Am Hubland
        D-97074 W\"urzburg
        Deutschland
;

_publ_contact_author
;
        Prof. Dr. Helmut Werner
        Institut f\"ur Anorganische Chemie
        Universit\"at W\"urzburg
        Am Hubland
        D-97074 W\"urzburg
        Deutschland
;
_publ_contact_author_phone        '049 931 888 5261'
_publ_contact_author_fax          '049 931 888 4605'
_publ_contact_author_email        helmut.werner@mail.uni-wuerzburg.de
_publ_requested_journal           'J. Chem. Soc., Dalton Trans.'
_publ_requested_coeditor_name     ?

_publ_contact_letter
;
  Please consider this CIF submission for publication in 
  "J. Chem. Soc., Dalton Trans."
;


_publ_section_title
;
  A new synthetic route to ligands of the general composition
  R2PCH2ER'2 (E = P, As) and some rhodium complexes derived thereof 
;

_publ_section_abstract
;
 Symmetrical and unsymmetrical bis(phosphino)methanes R2PCH2PR'2 (8-16)
 as well as the arsino(phosphino) analogues R'2AsCH2PR2 (21-25) with 
bulky
 alkyl, cycloalkyl or aryl groups R and R' were prepared from the 
stannylated
 phosphines R2PCH2SnR''3 (3-5, 6, 7) via metalation with MeLi or PhLi in
 the presence of TMEDA and subsequent treatment with R'2PCl or R'2AsCl,
 respectively. Compound 25 (R' = Cy, R = Men) is the first
 arsino(phosphino)methane which has been structurally characterized. The
 bis(phosphino)methanes R2PCH2PR2 (R = Pri 17, Cy 18) and R2PCH2PR'2
 (12, 19, 20) were also obtained by thermal reaction of R2PCH2SnPh3 and
 the corresponding chlorophosphine R2PCl or R'2PCl in the absence of 
solvent.
 The bis(cyclooctene) derivative [RhCl(C8H14)2]2 26 reacted with excess
 Pri2PCH2PPri2 to give [Rh(k2-Pri2PCH2PPri2)2]Cl 27, while treatment of 
26
 with Ph2PCH2PPri2 yielded the chloro-bridged dimer [{RhCl(k2-
Ph2PCH2PPri2)}2] 28. The reaction of the cationic species 
[Rh(C8H14)2(acetone)2]PF6 29 with Cy2PCH2PPri2 in benzene or toluene 
afforded the half-sandwich-type complexes
 [(h6-C6H6)Rh(k2-Cy2PCH2PPri2)]PF6 30, [(h6-C6H5CH3)Rh(k2-
Cy2PCH2PPri2)]PF6
 31, of which the latter was characterized by X-ray crystallography.

 Ditertiary phosphines containing two phosphorus atoms which are linked
 together by a chain of CH2 moieties are of major interest as mono- and
 bidentate ligands in transition-metal chemistry.1 Since the 
coordination
 mode of these phosphines and therefore the reactivity of the complexes
 obtained thereof are strongly dependent on both the substituents at
 phosphorus and the length of the carbon bridging unit, a great variety
 of diphosphine ligands have been prepared.2 Despite the large number
 of publications on their coordination chemistry,1 only a few synthetic
 routes allowing the unrestricted variation of structural features are
 established for the preparation of ligands of the general composition
 R2P(CH2)nPR'2.2,3
 In the course of our continuous studies concerning the coordination
 capabilities of bifunctional (possibly hemilabile) phosphines,4 we
 recently set out to prepare sterically hindered donor systems in which
 one PR2 unit is connected to an AsR2 or SbR2 fragment only by one 
methylene
 bridge.5,6 In order to introduce different elements of group 15 as well
 as a variety of different organic substituents, we were particularly
 interested to develop a general methodology for bis(phosphino)methanes
 as well as their P/As and P/Sb analogues. Here we describe the 
preparation
 of a series of symmetrical and unsymmetrical compounds of the
 type R2PCH2ER'2 (E = P, As) from the stannylated iodomethanes 
ICH2SnR''3
 as starting materials, the molecular structure of one representative,
 and illustrate with a few examples how the bis(phosphino)methanes 
behave
 as ligands for rhodium(I) as the metal centre. Some preliminary results
 of these studies were already communicated.7
;

_publ_section_exptl_prep
;
 Crystals were grown from iPrOH at cooling from 40_C to 0_C.
;

_publ_section_exptl_refinement
;
Due to measurement on an area detector system no standards are reported.
Reflections were collected only to theta = 48 deg. Because of the long 
c-axis
problems with overlapping reflections on the IP occured when measuring
up to higher theta range.
;

_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C33 H62 As P' 
_chemical_formula_weight          564.72 
_chemical_melting_point           67_C 
_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' 
 'P'  'P'   0.1023   0.0942 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'As'  'As'  -0.0300   2.0070 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            trigonal
_symmetry_space_group_name_H-M    P3121 
_symmetry_Int_Tables_number       152
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-y, x-y, z+1/3' 
 'y, x, -z' 
 '-x+y, -x, z+2/3' 
 'x-y, -y, -z+2/3' 
 '-x, -x+y, -z+1/3' 
 
_cell_length_a                    10.0640(4) 
_cell_length_b                    10.0640(4) 
_cell_length_c                    57.716(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 120.00 
_cell_volume                      5062.5(4) 
_cell_formula_units_Z             6 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used     5000 
_cell_measurement_theta_min       2.34 
_cell_measurement_theta_max       24.1 
 
_exptl_crystal_description        prism 
_exptl_crystal_colour             colourless 
_exptl_crystal_size_max           0.25 
_exptl_crystal_size_mid           0.25 
_exptl_crystal_size_min           0.1 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.111 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1848 
_exptl_absorpt_coefficient_mu     1.071 
_exptl_absorpt_correction_type    none 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       173(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            'Mo K\a' 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device        'IPDS (STOE)' 
_diffrn_measurement_method        'PSI scans' 
_diffrn_standards_number          0
_diffrn_standards_interval_count  0 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         0 
_diffrn_reflns_number             10185 
_diffrn_reflns_av_R_equivalents   0.0430 
_diffrn_reflns_av_sigmaI/netI     0.0853 
_diffrn_reflns_limit_h_min        -11 
_diffrn_reflns_limit_h_max        5 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        11 
_diffrn_reflns_limit_l_min        -58 
_diffrn_reflns_limit_l_max        66 
_diffrn_reflns_theta_min          2.34 
_diffrn_reflns_theta_max          24.17 
_reflns_number_total              5402 
_reflns_number_gt                 3469 
_reflns_observed_criterion        >2sigma(I) 

 
_computing_data_collection        'IPDS (STOE)'
_computing_cell_refinement        'IPDS (STOE)'
_computing_data_reduction         'IPDS (STOE)'
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_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^)+(0.0377P)^2^+0.0000P] 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     refxyz 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    -0.039(13) 
_refine_ls_number_reflns          4857 
_refine_ls_number_parameters      322 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0729 
_refine_ls_R_factor_gt            0.0418 
_refine_ls_wR_factor_all          0.0955 
_refine_ls_wR_factor_ref          0.0854 
_refine_ls_goodness_of_fit_all    0.927 
_refine_ls_goodness_of_fit_ref    1.016 
_refine_ls_restrained_S_all       0.898 
_refine_ls_restrained_S_obs       1.016 
_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 
As As 0.39726(6) 0.44638(6) 0.042792(9) 0.04812(15) Uani 1 d . . 
P P 0.57262(13) 0.53887(15) 0.08952(2) 0.0432(3) Uani 1 d . . 
C1 C 0.3811(5) 0.4662(5) 0.07677(7) 0.0433(11) Uani 1 d . . 
H1A H 0.3440(5) 0.5367(5) 0.07998(7) 0.052 Uiso 1 calc R . 
H1B H 0.3095(5) 0.3672(5) 0.08341(7) 0.052 Uiso 1 calc R . 
C10 C 0.5484(5) 0.5608(5) 0.12159(8) 0.0450(12) Uani 1 d . . 
H10 H 0.5879(5) 0.5029(5) 0.12993(8) 0.054 Uiso 1 calc R . 
C11 C 0.6490(5) 0.7319(5) 0.12868(8) 0.0500(13) Uani 1 d . . 
H11 H 0.6144(5) 0.7901(5) 0.11931(8) 0.060 Uiso 1 calc R . 
C12 C 0.6196(6) 0.7543(6) 0.15414(9) 0.0653(14) Uani 1 d . . 
H12A H 0.6606(6) 0.7053(6) 0.16399(9) 0.078 Uiso 1 calc R . 
H12B H 0.6745(6) 0.8632(6) 0.15766(9) 0.078 Uiso 1 calc R . 
C13 C 0.4510(6) 0.6896(7) 0.15985(10) 0.069(2) Uani 1 d . . 
H13A H 0.4401(6) 0.7061(7) 0.17613(10) 0.083 Uiso 1 calc R . 
H13B H 0.4105(6) 0.7427(7) 0.15083(10) 0.083 Uiso 1 calc R . 
C14 C 0.3609(6) 0.5201(6) 0.15455(9) 0.0610(14) Uani 1 d . . 
H14 H 0.4037(6) 0.4686(6) 0.16378(9) 0.073 Uiso 1 calc R . 
C15 C 0.3799(5) 0.4949(6) 0.12891(8) 0.0502(12) Uani 1 d . . 
H15A H 0.3346(5) 0.5424(6) 0.11963(8) 0.060 Uiso 1 calc R . 
H15B H 0.3242(5) 0.3857(6) 0.12569(8) 0.060 Uiso 1 calc R . 
C16 C 0.8203(5) 0.7992(5) 0.12358(9) 0.0546(13) Uani 1 d . . 
H16 H 0.8285(5) 0.7765(5) 0.10730(9) 0.066 Uiso 1 calc R . 
C17 C 0.8964(6) 0.7272(7) 0.13791(10) 0.082(2) Uani 1 d . . 
H17A H 0.8903(43) 0.7461(42) 0.15407(11) 0.122 Uiso 1 calc R . 
H17B H 1.0021(14) 0.7717(35) 0.1335(5) 0.122 Uiso 1 calc R . 
H17C H 0.8445(31) 0.6185(10) 0.1352(6) 0.122 Uiso 1 calc R . 
C18 C 0.9114(7) 0.9748(6) 0.12612(12) 0.088(2) Uani 1 d . . 
H18A H 1.0154(14) 1.0126(8) 0.1212(7) 0.132 Uiso 1 calc R . 
H18B H 0.9106(42) 1.0019(6) 0.1420(2) 0.132 Uiso 1 calc R . 
H18C H 0.8653(30) 1.0194(7) 0.1167(6) 0.132 Uiso 1 calc R . 
C19 C 0.1899(7) 0.4476(8) 0.16045(10) 0.087(2) Uani 1 d . . 
H19A H 0.1375(11) 0.3412(14) 0.1562(7) 0.131 Uiso 1 calc R . 
H19B H 0.1468(13) 0.4996(33) 0.1521(6) 0.131 Uiso 1 calc R . 
H19C H 0.1783(7) 0.4569(44) 0.17679(15) 0.131 Uiso 1 calc R . 
C20 C 0.5832(5) 0.3587(5) 0.08800(8) 0.0439(11) Uani 1 d . . 
H20 H 0.5629(5) 0.3266(5) 0.07175(8) 0.053 Uiso 1 calc R . 
C21 C 0.7451(5) 0.3833(5) 0.09305(9) 0.0514(13) Uani 1 d . . 
H21 H 0.7638(5) 0.4036(5) 0.10968(9) 0.062 Uiso 1 calc R . 
C22 C 0.7430(6) 0.2316(6) 0.08807(10) 0.065(2) Uani 1 d . . 
H22A H 0.7277(6) 0.2103(6) 0.07160(10) 0.079 Uiso 1 calc R . 
H22B H 0.8420(6) 0.2439(6) 0.09215(10) 0.079 Uiso 1 calc R . 
C23 C 0.6182(6) 0.0952(6) 0.10132(10) 0.068(2) Uani 1 d . . 
H23A H 0.6195(6) 0.0029(6) 0.09689(10) 0.082 Uiso 1 calc R . 
H23B H 0.6391(6) 0.1109(6) 0.11780(10) 0.082 Uiso 1 calc R . 
C24 C 0.4604(5) 0.0739(5) 0.09647(9) 0.0555(13) Uani 1 d . . 
H24 H 0.4371(5) 0.0501(5) 0.07999(9) 0.067 Uiso 1 calc R . 
C25 C 0.4615(5) 0.2225(5) 0.10180(8) 0.0518(13) Uani 1 d . . 
H25A H 0.4804(5) 0.2446(5) 0.11822(8) 0.062 Uiso 1 calc R . 
H25B H 0.3613(5) 0.2093(5) 0.09831(8) 0.062 Uiso 1 calc R . 
C26 C 0.8762(5) 0.5210(6) 0.08018(9) 0.0558(13) Uani 1 d . . 
H26 H 0.8700(5) 0.6118(6) 0.08461(9) 0.067 Uiso 1 calc R . 
C27 C 0.8639(6) 0.5100(6) 0.05401(9) 0.0677(15) Uani 1 d . . 
H27A H 0.8704(37) 0.4226(22) 0.04889(10) 0.102 Uiso 1 calc R . 
H27B H 0.9462(22) 0.6015(17) 0.04728(10) 0.102 Uiso 1 calc R . 
H27C H 0.7674(16) 0.4989(37) 0.04927(10) 0.102 Uiso 1 calc R . 
C28 C 1.0337(6) 0.5494(6) 0.08829(11) 0.079(2) Uani 1 d . . 
H28A H 1.0384(16) 0.5544(43) 0.10491(11) 0.118 Uiso 1 calc R . 
H28B H 1.1128(6) 0.6445(22) 0.0820(5) 0.118 Uiso 1 calc R . 
H28C H 1.0483(19) 0.4670(23) 0.0831(6) 0.118 Uiso 1 calc R . 
C29 C 0.3375(7) -0.0593(6) 0.11078(10) 0.079(2) Uani 1 d . . 
H29A H 0.2383(8) -0.0732(29) 0.1071(5) 0.118 Uiso 1 calc R . 
H29B H 0.3579(26) -0.0366(20) 0.12698(10) 0.118 Uiso 1 calc R . 
H29C H 0.3392(30) -0.1516(11) 0.1072(5) 0.118 Uiso 1 calc R . 
C30 C 0.3375(5) 0.5974(5) 0.03366(8) 0.0452(12) Uani 1 d . . 
H30 H 0.2457(5) 0.5765(5) 0.04243(8) 0.054 Uiso 1 calc R . 
C31 C 0.4666(6) 0.7598(5) 0.03975(8) 0.0534(12) Uani 1 d . . 
H31A H 0.4868(6) 0.7658(5) 0.05626(8) 0.064 Uiso 1 calc R . 
H31B H 0.5596(6) 0.7804(5) 0.03169(8) 0.064 Uiso 1 calc R . 
C32 C 0.4245(6) 0.8818(6) 0.03304(9) 0.0610(14) Uani 1 d . . 
H32A H 0.3380(6) 0.8680(6) 0.04228(9) 0.073 Uiso 1 calc R . 
H32B H 0.5106(6) 0.9831(6) 0.03626(9) 0.073 Uiso 1 calc R . 
C33 C 0.3836(6) 0.8696(6) 0.00746(9) 0.0666(15) Uani 1 d . . 
H33A H 0.4741(6) 0.8960(6) -0.00175(9) 0.080 Uiso 1 calc R . 
H33B H 0.3502(6) 0.9424(6) 0.00384(9) 0.080 Uiso 1 calc R . 
C34 C 0.2570(6) 0.7085(5) 0.00110(9) 0.0627(15) Uani 1 d . . 
H34A H 0.2383(6) 0.7033(5) -0.01545(9) 0.075 Uiso 1 calc R . 
H34B H 0.1630(6) 0.6865(5) 0.00898(9) 0.075 Uiso 1 calc R . 
C35 C 0.3004(5) 0.5879(5) 0.00783(8) 0.0512(12) Uani 1 d . . 
H35A H 0.2159(5) 0.4864(5) 0.00422(8) 0.061 Uiso 1 calc R . 
H35B H 0.3888(5) 0.6040(5) -0.00112(8) 0.061 Uiso 1 calc R . 
C40 C 0.2057(5) 0.2528(5) 0.03703(8) 0.0440(11) Uani 1 d . . 
H40 H 0.1937(5) 0.2448(5) 0.02016(8) 0.053 Uiso 1 calc R . 
C41 C 0.0560(5) 0.2356(5) 0.04642(10) 0.061(2) Uani 1 d . . 
H41A H 0.0417(5) 0.3168(5) 0.04011(10) 0.073 Uiso 1 calc R . 
H41B H 0.0637(5) 0.2474(5) 0.06313(10) 0.073 Uiso 1 calc R . 
C42 C -0.0851(6) 0.0793(6) 0.04039(11) 0.066(2) Uani 1 d . . 
H42A H -0.1757(6) 0.0714(6) 0.04763(11) 0.080 Uiso 1 calc R . 
H42B H -0.1008(6) 0.0716(6) 0.02375(11) 0.080 Uiso 1 calc R . 
C43 C -0.0620(6) -0.0514(6) 0.04878(12) 0.077(2) Uani 1 d . . 
H43A H -0.0554(6) -0.0491(6) 0.06555(12) 0.092 Uiso 1 calc R . 
H43B H -0.1493(6) -0.1489(6) 0.04423(12) 0.092 Uiso 1 calc R . 
C44 C 0.0828(6) -0.0368(6) 0.03858(12) 0.081(2) Uani 1 d . . 
H44A H 0.0722(6) -0.0478(6) 0.02188(12) 0.097 Uiso 1 calc R . 
H44B H 0.0974(6) -0.1188(6) 0.04450(12) 0.097 Uiso 1 calc R . 
C45 C 0.2228(6) 0.1168(5) 0.04442(10) 0.0568(13) Uani 1 d . . 
H45A H 0.3120(6) 0.1236(5) 0.03682(10) 0.068 Uiso 1 calc R . 
H45B H 0.2403(6) 0.1221(5) 0.06101(10) 0.068 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 
As 0.0489(3) 0.0562(3) 0.0453(3) -0.0040(3) -0.0013(3) 0.0308(3) 
P 0.0431(7) 0.0459(7) 0.0425(8) -0.0011(6) -0.0009(6) 0.0236(6) 
C1 0.044(3) 0.062(3) 0.030(2) -0.010(2) -0.005(2) 0.031(2) 
C10 0.052(3) 0.051(3) 0.038(3) -0.007(2) -0.007(2) 0.029(2) 
C11 0.056(3) 0.049(3) 0.049(3) -0.005(2) -0.007(2) 0.029(2) 
C12 0.075(4) 0.068(3) 0.056(4) -0.014(3) -0.002(3) 0.039(3) 
C13 0.081(4) 0.087(4) 0.048(4) -0.010(3) 0.004(3) 0.048(4) 
C14 0.069(4) 0.070(4) 0.047(3) 0.004(3) 0.009(3) 0.037(3) 
C15 0.047(3) 0.061(3) 0.043(3) 0.002(2) 0.010(2) 0.027(2) 
C16 0.049(3) 0.051(3) 0.057(3) -0.010(3) -0.009(3) 0.020(3) 
C17 0.071(4) 0.097(5) 0.083(4) -0.020(4) -0.025(3) 0.047(3) 
C18 0.063(4) 0.058(4) 0.123(6) -0.019(4) -0.004(4) 0.015(3) 
C19 0.069(4) 0.115(5) 0.062(4) 0.001(4) 0.027(3) 0.035(4) 
C20 0.046(3) 0.043(3) 0.041(3) -0.003(2) -0.004(2) 0.022(2) 
C21 0.054(3) 0.054(3) 0.055(3) -0.007(2) -0.008(2) 0.034(3) 
C22 0.068(4) 0.065(3) 0.077(4) -0.005(3) -0.009(3) 0.043(3) 
C23 0.076(4) 0.052(3) 0.083(4) 0.001(3) -0.007(3) 0.037(3) 
C24 0.055(3) 0.043(3) 0.065(4) -0.004(3) -0.004(3) 0.022(2) 
C25 0.049(3) 0.046(3) 0.056(3) 0.001(3) 0.003(3) 0.020(2) 
C26 0.037(3) 0.052(3) 0.077(4) -0.010(3) -0.002(2) 0.021(2) 
C27 0.062(3) 0.065(3) 0.077(4) 0.001(3) 0.016(3) 0.032(3) 
C28 0.054(4) 0.086(4) 0.101(5) -0.029(3) -0.003(3) 0.038(3) 
C29 0.084(4) 0.053(4) 0.086(5) 0.005(3) -0.004(4) 0.024(3) 
C30 0.044(3) 0.046(3) 0.049(3) 0.004(2) -0.002(2) 0.025(2) 
C31 0.062(3) 0.049(3) 0.050(3) -0.003(2) -0.007(3) 0.028(3) 
C32 0.060(3) 0.043(3) 0.069(4) 0.003(3) -0.005(3) 0.017(3) 
C33 0.071(4) 0.051(3) 0.065(4) 0.012(3) -0.005(3) 0.021(3) 
C34 0.060(3) 0.052(3) 0.063(4) 0.014(3) -0.007(3) 0.018(3) 
C35 0.049(3) 0.050(3) 0.046(3) 0.006(2) -0.003(2) 0.018(3) 
C40 0.042(3) 0.041(3) 0.042(3) -0.008(2) -0.003(2) 0.016(2) 
C41 0.050(3) 0.063(4) 0.073(4) -0.011(3) -0.004(3) 0.030(3) 
C42 0.052(3) 0.068(4) 0.082(4) -0.020(3) -0.012(3) 0.033(3) 
C43 0.057(4) 0.064(4) 0.102(5) 0.002(3) 0.004(3) 0.024(3) 
C44 0.071(4) 0.052(3) 0.121(6) -0.005(3) -0.006(4) 0.031(3) 
C45 0.064(3) 0.040(3) 0.072(4) -0.003(3) -0.002(3) 0.031(3) 
 
_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 
As C30 1.965(4) . ? 
As C40 1.966(4) . ? 
As C1 1.986(4) . ? 
As P 3.1004(13) . ? 
P C1 1.839(4) . ? 
P C20 1.870(5) . ? 
P C10 1.894(4) . ? 
C10 C15 1.539(6) . ? 
C10 C11 1.554(6) . ? 
C11 C16 1.533(6) . ? 
C11 C12 1.538(7) . ? 
C12 C13 1.519(7) . ? 
C13 C14 1.509(7) . ? 
C14 C15 1.530(6) . ? 
C14 C19 1.534(7) . ? 
C16 C17 1.533(7) . ? 
C16 C18 1.538(7) . ? 
C20 C25 1.528(6) . ? 
C20 C21 1.549(6) . ? 
C21 C22 1.543(6) . ? 
C21 C26 1.544(7) . ? 
C22 C23 1.524(7) . ? 
C23 C24 1.518(7) . ? 
C24 C25 1.522(6) . ? 
C24 C29 1.534(7) . ? 
C26 C27 1.515(7) . ? 
C26 C28 1.537(6) . ? 
C30 C35 1.529(6) . ? 
C30 C31 1.536(6) . ? 
C31 C32 1.535(7) . ? 
C32 C33 1.521(7) . ? 
C33 C34 1.523(7) . ? 
C34 C35 1.532(6) . ? 
C40 C45 1.523(6) . ? 
C40 C41 1.527(6) . ? 
C41 C42 1.542(6) . ? 
C42 C43 1.524(7) . ? 
C43 C44 1.510(8) . ? 
C44 C45 1.520(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 
C30 As C40 101.2(2) . . ? 
C30 As C1 96.6(2) . . ? 
C40 As C1 100.2(2) . . ? 
C30 As P 110.45(14) . . ? 
C40 As P 124.98(14) . . ? 
C1 As P 34.30(12) . . ? 
C1 P C20 98.7(2) . . ? 
C1 P C10 105.5(2) . . ? 
C20 P C10 103.4(2) . . ? 
C1 P As 37.48(13) . . ? 
C20 P As 88.15(15) . . ? 
C10 P As 142.93(15) . . ? 
P C1 As 108.2(2) . . ? 
C15 C10 C11 111.9(4) . . ? 
C15 C10 P 113.3(3) . . ? 
C11 C10 P 109.6(3) . . ? 
C16 C11 C12 112.0(4) . . ? 
C16 C11 C10 113.9(4) . . ? 
C12 C11 C10 110.3(4) . . ? 
C13 C12 C11 113.6(4) . . ? 
C14 C13 C12 110.6(4) . . ? 
C13 C14 C15 109.2(4) . . ? 
C13 C14 C19 112.9(4) . . ? 
C15 C14 C19 109.8(4) . . ? 
C14 C15 C10 113.3(4) . . ? 
C11 C16 C17 113.9(4) . . ? 
C11 C16 C18 112.5(4) . . ? 
C17 C16 C18 109.9(4) . . ? 
C25 C20 C21 110.6(4) . . ? 
C25 C20 P 115.9(3) . . ? 
C21 C20 P 113.7(3) . . ? 
C22 C21 C26 112.4(4) . . ? 
C22 C21 C20 108.3(4) . . ? 
C26 C21 C20 114.3(4) . . ? 
C23 C22 C21 113.3(4) . . ? 
C24 C23 C22 111.5(4) . . ? 
C23 C24 C25 109.3(4) . . ? 
C23 C24 C29 110.7(4) . . ? 
C25 C24 C29 110.9(4) . . ? 
C24 C25 C20 112.6(4) . . ? 
C27 C26 C28 110.9(4) . . ? 
C27 C26 C21 114.3(4) . . ? 
C28 C26 C21 111.1(4) . . ? 
C35 C30 C31 109.9(4) . . ? 
C35 C30 As 111.9(3) . . ? 
C31 C30 As 109.8(3) . . ? 
C32 C31 C30 111.6(4) . . ? 
C33 C32 C31 110.6(4) . . ? 
C32 C33 C34 111.6(4) . . ? 
C33 C34 C35 111.3(4) . . ? 
C30 C35 C34 110.8(4) . . ? 
C45 C40 C41 110.3(4) . . ? 
C45 C40 As 110.4(3) . . ? 
C41 C40 As 118.4(3) . . ? 
C40 C41 C42 112.9(4) . . ? 
C43 C42 C41 110.4(4) . . ? 
C44 C43 C42 110.4(5) . . ? 
C43 C44 C45 111.8(5) . . ? 
C44 C45 C40 112.9(4) . . ? 
 
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
 C30 As P C1 70.8(3) . . . . ? 
 C40 As P C1 -50.1(3) . . . . ? 
 C1 As P C1 0.000(1) . . . . ? 
 C30 As P C20 177.8(2) . . . . ? 
 C40 As P C20 56.9(2) . . . . ? 
 C1 As P C20 107.0(3) . . . . ? 
 C30 As P C10 67.8(3) . . . . ? 
 C40 As P C10 -53.1(3) . . . . ? 
 C1 As P C10 -3.0(3) . . . . ? 
 C20 P C1 As -75.3(2) . . . . ? 
 C10 P C1 As 178.1(2) . . . . ? 
 As P C1 As 0.0 . . . . ? 
 C30 As C1 P -117.0(2) . . . . ? 
 C40 As C1 P 140.3(2) . . . . ? 
 P As C1 P 0.0 . . . . ? 
 C1 P C10 C15 7.6(4) . . . . ? 
 C20 P C10 C15 -95.6(3) . . . . ? 
 As P C10 C15 9.5(5) . . . . ? 
 C1 P C10 C11 -118.2(3) . . . . ? 
 C20 P C10 C11 138.6(3) . . . . ? 
 As P C10 C11 -116.3(3) . . . . ? 
 C15 C10 C11 C16 175.2(4) . . . . ? 
 P C10 C11 C16 -58.2(5) . . . . ? 
 C15 C10 C11 C12 48.2(5) . . . . ? 
 P C10 C11 C12 174.8(3) . . . . ? 
 C16 C11 C12 C13 179.8(4) . . . . ? 
 C10 C11 C12 C13 -52.2(6) . . . . ? 
 C11 C12 C13 C14 58.4(6) . . . . ? 
 C12 C13 C14 C15 -58.6(6) . . . . ? 
 C12 C13 C14 C19 178.8(5) . . . . ? 
 C13 C14 C15 C10 57.0(5) . . . . ? 
 C19 C14 C15 C10 -178.6(4) . . . . ? 
 C11 C10 C15 C14 -52.4(5) . . . . ? 
 P C10 C15 C14 -177.0(3) . . . . ? 
 C12 C11 C16 C17 60.3(5) . . . . ? 
 C10 C11 C16 C17 -65.8(6) . . . . ? 
 C12 C11 C16 C18 -65.5(6) . . . . ? 
 C10 C11 C16 C18 168.4(5) . . . . ? 
 C1 P C20 C25 -61.5(4) . . . . ? 
 C10 P C20 C25 46.9(4) . . . . ? 
 As P C20 C25 -97.5(3) . . . . ? 
 C1 P C20 C21 168.7(3) . . . . ? 
 C10 P C20 C21 -83.0(4) . . . . ? 
 As P C20 C21 132.6(3) . . . . ? 
 C25 C20 C21 C22 55.0(5) . . . . ? 
 P C20 C21 C22 -172.6(4) . . . . ? 
 C25 C20 C21 C26 -178.9(4) . . . . ? 
 P C20 C21 C26 -46.4(5) . . . . ? 
 C26 C21 C22 C23 177.8(4) . . . . ? 
 C20 C21 C22 C23 -54.9(6) . . . . ? 
 C21 C22 C23 C24 56.2(6) . . . . ? 
 C22 C23 C24 C25 -55.0(6) . . . . ? 
 C22 C23 C24 C29 -177.4(4) . . . . ? 
 C23 C24 C25 C20 57.3(5) . . . . ? 
 C29 C24 C25 C20 179.6(4) . . . . ? 
 C21 C20 C25 C24 -58.5(5) . . . . ? 
 P C20 C25 C24 170.2(3) . . . . ? 
 C22 C21 C26 C27 63.5(5) . . . . ? 
 C20 C21 C26 C27 -60.4(5) . . . . ? 
 C22 C21 C26 C28 -62.8(6) . . . . ? 
 C20 C21 C26 C28 173.2(4) . . . . ? 
 C40 As C30 C35 -64.8(3) . . . . ? 
 C1 As C30 C35 -166.7(3) . . . . ? 
 P As C30 C35 161.0(3) . . . . ? 
 C40 As C30 C31 172.9(3) . . . . ? 
 C1 As C30 C31 71.1(3) . . . . ? 
 P As C30 C31 38.7(3) . . . . ? 
 C35 C30 C31 C32 56.9(5) . . . . ? 
 As C30 C31 C32 -179.7(3) . . . . ? 
 C30 C31 C32 C33 -55.8(6) . . . . ? 
 C31 C32 C33 C34 54.8(6) . . . . ? 
 C32 C33 C34 C35 -55.6(6) . . . . ? 
 C31 C30 C35 C34 -56.8(5) . . . . ? 
 As C30 C35 C34 -179.0(3) . . . . ? 
 C33 C34 C35 C30 56.6(6) . . . . ? 
 C30 As C40 C45 -176.6(3) . . . . ? 
 C1 As C40 C45 -77.7(4) . . . . ? 
 P As C40 C45 -51.7(4) . . . . ? 
 C30 As C40 C41 -48.2(4) . . . . ? 
 C1 As C40 C41 50.7(4) . . . . ? 
 P As C40 C41 76.7(4) . . . . ? 
 C45 C40 C41 C42 -52.3(6) . . . . ? 
 As C40 C41 C42 179.3(4) . . . . ? 
 C40 C41 C42 C43 55.3(7) . . . . ? 
 C41 C42 C43 C44 -56.5(7) . . . . ? 
 C42 C43 C44 C45 57.1(7) . . . . ? 
 C43 C44 C45 C40 -55.5(7) . . . . ? 
 C41 C40 C45 C44 52.1(6) . . . . ? 
 As C40 C45 C44 -175.3(4) . . . . ? 
 
_refine_diff_density_max    0.373 
_refine_diff_density_min   -0.410 
_refine_diff_density_rms    0.056