# Copyright The Royal Society of Chemistry, 1998.

data_4a

_audit_creation_method            SHELXL
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_formula_moiety          ?
_chemical_formula_structural      ?
_chemical_formula_analytical      ?
_chemical_formula_sum             'C52 H44 B2 Cl9 O4 P2 Rh'
_chemical_formula_weight          1238.39
_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'
 'B'  'B'   0.0013   0.0007
 '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'
 'Rh'  'Rh'  -1.1178   0.9187
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting            triclinic
_symmetry_space_group_name_H-M    P-1

loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'

_cell_length_a                    11.2003(6)
_cell_length_b                    13.5606(7)
_cell_length_c                    19.0819(10)
_cell_angle_alpha                 83.5510(10)
_cell_angle_beta                  83.0640(10)
_cell_angle_gamma                 79.3730(10)
_cell_volume                      2815.6(3)
_cell_formula_units_Z             2
_cell_measurement_temperature     160(2)
_cell_measurement_reflns_used     18178
_cell_measurement_theta_min       1.79
_cell_measurement_theta_max       25.51

_exptl_crystal_description        Block
_exptl_crystal_colour             Colourless
_exptl_crystal_size_max           0.62
_exptl_crystal_size_mid           0.20
_exptl_crystal_size_min           0.18
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.461
_exptl_crystal_density_method     ?
_exptl_crystal_F_000              1252
_exptl_absorpt_coefficient_mu     0.830
_exptl_absorpt_correction_type    empirical
_exptl_absorpt_correction_T_min   0.422
_exptl_absorpt_correction_T_max   0.502

_exptl_special_details
;
 ?
;

_diffrn_ambient_temperature       160(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 CCD diffractometer'
_diffrn_measurement_method        '\w rotation with narrow frames'
_diffrn_standards_number          0
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             24661
_diffrn_reflns_av_R_equivalents   0.0385
_diffrn_reflns_av_sigmaI/netI     0.0325
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        12
_diffrn_reflns_limit_k_min        -16
_diffrn_reflns_limit_k_max        16
_diffrn_reflns_limit_l_min        -22
_diffrn_reflns_limit_l_max        22
_diffrn_reflns_theta_min          1.08
_diffrn_reflns_theta_max          25.53
_reflns_number_total              9306
_reflns_number_observed           8469
_reflns_observed_criterion        >2sigma(I)

_computing_data_collection        'Siemens SMART'
_computing_cell_refinement        'local programs'
_computing_data_reduction         'Siemens SAINT'
_computing_structure_solution     'Siemens SHELXTL'
_computing_structure_refinement   'Siemens SHELXTL'
_computing_molecular_graphics     'Siemens SHELXTL'
_computing_publication_material   'SHELXTL and local programs'

_refine_special_details
;
 Refinement on F^2^ for ALL reflections except for 3 with very
negative F^2^
 or flagged by the user for potential systematic errors. 
Weighted R-factors
 wR and all goodnesses of fit S are based on F^2^, conventional
R-factors R
 are based on F, with F set to zero for negative F^2^. The
observed criterion
 of F^2^ > 2sigma(F^2^) is used only for calculating
_R_factor_obs etc. and is
 not relevant to the choice of reflections for refinement. 
R-factors based
 on F^2^ are statistically about twice as large as those based on
F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme
 'calc w=1/[\s^2^(Fo^2^)+(0.0372P)^2^+5.1991P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      heavy
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     ?
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.0018(2)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_number_reflns          9303
_refine_ls_number_parameters      644
_refine_ls_number_restraints      4
_refine_ls_R_factor_all           0.0452
_refine_ls_R_factor_obs           0.0402
_refine_ls_wR_factor_all          0.1022
_refine_ls_wR_factor_obs          0.0978
_refine_ls_goodness_of_fit_all    1.054
_refine_ls_goodness_of_fit_obs    1.062
_refine_ls_restrained_S_all       1.058
_refine_ls_restrained_S_obs       1.064
_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
Rh1 Rh 0.58706(2) 0.69135(2) 0.720735(12) 0.02455(9) Uani 1 d . .
B1 B 0.6868(3) 0.5802(3) 0.6723(2) 0.0289(8) Uani 1 d . .
O1 O 0.7285(2) 0.5809(2) 0.60006(12) 0.0334(5) Uani 1 d . .
O2 O 0.7404(2) 0.4893(2) 0.70797(12) 0.0322(5) Uani 1 d . .
C1 C 0.8068(3) 0.4899(2) 0.5920(2) 0.0325(7) Uani 1 d . .
C2 C 0.8139(3) 0.4351(2) 0.6571(2) 0.0308(7) Uani 1 d . .
C3 C 0.8867(3) 0.3426(3) 0.6659(2) 0.0386(8) Uani 1 d . .
H3 H 0.8918(3) 0.3055(3) 0.7111(2) 0.046 Uiso 1 d R .
C4 C 0.9542(3) 0.3070(3) 0.6050(2) 0.0445(9) Uani 1 d . .
H4 H 1.0055(3) 0.2429(3) 0.6083(2) 0.053 Uiso 1 d R .
C5 C 0.9471(3) 0.3617(3) 0.5398(2) 0.0476(10) Uani 1 d . .
H5 H 0.9960(3) 0.3352(3) 0.4997(2) 0.057 Uiso 1 d R .
C6 C 0.8719(4) 0.4550(3) 0.5312(2) 0.0459(9) Uani 1 d . .
H6 H 0.8651(4) 0.4921(3) 0.4861(2) 0.055 Uiso 1 d R .
B2 B 0.4577(4) 0.6229(3) 0.6930(2) 0.0309(8) Uani 1 d . .
O3 O 0.4639(2) 0.5295(2) 0.66640(12) 0.0374(6) Uani 1 d . .
O4 O 0.3352(2) 0.6681(2) 0.70591(13) 0.0382(6) Uani 1 d . .
C7 C 0.3447(4) 0.5161(3) 0.6670(2) 0.0438(9) Uani 1 d . .
C8 C 0.2670(4) 0.5988(3) 0.6904(2) 0.0460(10) Uani 1 d . .
C9 C 0.1424(4) 0.6051(4) 0.6986(3) 0.0693(14) Uani 1 d . .
H9 H 0.0892(4) 0.6629(4) 0.7147(3) 0.083 Uiso 1 d R .
C10 C 0.0994(5) 0.5216(6) 0.6816(3) 0.089(2) Uani 1 d . .
H10 H 0.0140(5) 0.5221(6) 0.6857(3) 0.107 Uiso 1 d R .
C11 C 0.1774(6) 0.4382(5) 0.6586(3) 0.083(2) Uani 1 d . .
H11 H 0.1441(6) 0.3825(5) 0.6483(3) 0.100 Uiso 1 d R .
C12 C 0.3032(5) 0.4323(4) 0.6505(2) 0.0625(13) Uani 1 d . .
H12 H 0.3570(5) 0.3743(4) 0.6350(2) 0.075 Uiso 1 d R .
Cl1 Cl 0.68850(7) 0.80407(6) 0.77425(4) 0.0324(2) Uani 1 d . .
P1 P 0.56979(7) 0.59537(6) 0.82995(4) 0.0270(2) Uani 1 d . .
C13 C 0.4788(3) 0.6829(2) 0.8899(2) 0.0305(7) Uani 1 d . .
C14 C 0.3786(3) 0.7482(3) 0.8644(2) 0.0373(8) Uani 1 d . .
H14 H 0.3596(3) 0.7449(3) 0.8176(2) 0.045 Uiso 1 d R .
C15 C 0.3079(3) 0.8184(3) 0.9063(2) 0.0435(9) Uani 1 d . .
H15 H 0.2392(3) 0.8618(3) 0.8888(2) 0.052 Uiso 1 d R .
C16 C 0.3364(4) 0.8250(3) 0.9738(2) 0.0479(10) Uani 1 d . .
H16 H 0.2880(4) 0.8733(3) 1.0026(2) 0.057 Uiso 1 d R .
C17 C 0.4354(4) 0.7614(3) 0.9994(2) 0.0475(10) Uani 1 d . .
H17 H 0.4547(4) 0.7657(3) 1.0460(2) 0.057 Uiso 1 d R .
C18 C 0.5076(3) 0.6904(3) 0.9578(2) 0.0375(8) Uani 1 d . .
H18 H 0.5763(3) 0.6475(3) 0.9758(2) 0.045 Uiso 1 d R .
C19 C 0.7064(3) 0.5390(2) 0.8725(2) 0.0305(7) Uani 1 d . .
C20 C 0.8190(3) 0.5636(3) 0.8453(2) 0.0367(8) Uani 1 d . .
H20 H 0.8247(3) 0.6100(3) 0.8044(2) 0.044 Uiso 1 d R .
C21 C 0.9231(4) 0.5200(3) 0.8777(2) 0.0491(10) Uani 1 d . .
H21 H 0.9997(4) 0.5382(3) 0.8597(2) 0.059 Uiso 1 d R .
C22 C 0.9152(4) 0.4513(3) 0.9368(2) 0.0485(10) Uani 1 d . .
H22 H 0.9870(4) 0.4204(3) 0.9580(2) 0.058 Uiso 1 d R .
C23 C 0.8039(4) 0.4268(3) 0.9639(2) 0.0458(9) Uani 1 d . .
H23 H 0.7986(4) 0.3805(3) 1.0050(2) 0.055 Uiso 1 d R .
C24 C 0.6998(3) 0.4698(3) 0.9319(2) 0.0391(8) Uani 1 d . .
H24 H 0.6233(3) 0.4516(3) 0.9501(2) 0.047 Uiso 1 d R .
C25 C 0.4850(3) 0.4908(2) 0.8365(2) 0.0299(7) Uani 1 d . .
C26 C 0.3606(3) 0.5033(3) 0.8579(2) 0.0397(8) Uani 1 d . .
H26 H 0.3187(3) 0.5659(3) 0.8733(2) 0.048 Uiso 1 d R .
C27 C 0.2971(4) 0.4248(3) 0.8571(2) 0.0513(10) Uani 1 d . .
H27 H 0.2119(4) 0.4347(3) 0.8716(2) 0.062 Uiso 1 d R .
C28 C 0.3559(4) 0.3337(3) 0.8356(2) 0.0470(10) Uani 1 d . .
H28 H 0.3116(4) 0.2804(3) 0.8348(2) 0.056 Uiso 1 d R .
C29 C 0.4790(4) 0.3200(3) 0.8147(2) 0.0437(9) Uani 1 d . .
H29 H 0.5207(4) 0.2569(3) 0.8001(2) 0.052 Uiso 1 d R .
C30 C 0.5434(3) 0.3979(3) 0.8149(2) 0.0387(8) Uani 1 d . .
H30 H 0.6284(3) 0.3880(3) 0.7999(2) 0.046 Uiso 1 d R .
C31 C 0.4704(3) 0.7771(2) 0.5539(2) 0.0317(7) Uani 1 d . .
P2 P 0.56873(7) 0.80077(6) 0.61795(4) 0.0271(2) Uani 1 d . .
C32 C 0.4979(4) 0.6875(3) 0.5217(2) 0.0409(8) Uani 1 d . .
H32 H 0.5683(4) 0.6399(3) 0.5326(2) 0.049 Uiso 1 d R .
C33 C 0.4238(4) 0.6674(3) 0.4737(2) 0.0493(10) Uani 1 d . .
H33 H 0.4434(4) 0.6061(3) 0.4518(2) 0.059 Uiso 1 d R .
C34 C 0.3228(4) 0.7359(3) 0.4575(2) 0.0489(10) Uani 1 d . .
H34 H 0.2715(4) 0.7217(3) 0.4251(2) 0.059 Uiso 1 d R .
C35 C 0.2943(4) 0.8253(3) 0.4888(2) 0.0486(10) Uani 1 d . .
H35 H 0.2250(4) 0.8733(3) 0.4767(2) 0.058 Uiso 1 d R .
C36 C 0.3673(3) 0.8459(3) 0.5370(2) 0.0393(8) Uani 1 d . .
H36 H 0.3459(3) 0.9071(3) 0.5590(2) 0.047 Uiso 1 d R .
C37 C 0.7053(3) 0.8305(2) 0.5640(2) 0.0296(7) Uani 1 d . .
C38 C 0.7002(3) 0.8700(3) 0.4932(2) 0.0379(8) Uani 1 d . .
H38 H 0.6278(3) 0.8735(3) 0.4710(2) 0.045 Uiso 1 d R .
C39 C 0.8014(3) 0.9029(3) 0.4552(2) 0.0418(9) Uani 1 d . .
H39 H 0.7974(3) 0.9300(3) 0.4073(2) 0.050 Uiso 1 d R .
C40 C 0.9069(3) 0.8974(3) 0.4868(2) 0.0431(9) Uani 1 d . .
H40 H 0.9751(3) 0.9216(3) 0.4608(2) 0.052 Uiso 1 d R .
C41 C 0.9136(3) 0.8561(3) 0.5560(2) 0.0443(9) Uani 1 d . .
H41 H 0.9875(3) 0.8501(3) 0.5772(2) 0.053 Uiso 1 d R .
C42 C 0.8131(3) 0.8221(3) 0.5946(2) 0.0375(8) Uani 1 d . .
H42 H 0.8182(3) 0.7937(3) 0.6422(2) 0.045 Uiso 1 d R .
C43 C 0.4945(3) 0.9206(2) 0.6508(2) 0.0294(7) Uani 1 d . .
C44 C 0.5475(3) 1.0070(3) 0.6383(2) 0.0373(8) Uani 1 d . .
H44 H 0.6225(3) 1.0063(3) 0.6091(2) 0.045 Uiso 1 d R .
C45 C 0.4906(4) 1.0944(3) 0.6686(2) 0.0466(9) Uani 1 d . .
H45 H 0.5272(4) 1.1530(3) 0.6605(2) 0.056 Uiso 1 d R .
C46 C 0.3828(4) 1.0964(3) 0.7112(2) 0.0507(10) Uani 1 d . .
H46 H 0.3431(4) 1.1568(3) 0.7307(2) 0.061 Uiso 1 d R .
C47 C 0.3297(4) 1.0112(3) 0.7246(2) 0.0469(9) Uani 1 d . .
H47 H 0.2556(4) 1.0123(3) 0.7548(2) 0.056 Uiso 1 d R .
C48 C 0.3846(3) 0.9239(3) 0.6948(2) 0.0373(8) Uani 1 d . .
H48 H 0.3475(3) 0.8655(3) 0.7042(2) 0.045 Uiso 1 d R .
C49 C 0.8516(5) 0.7990(4) 0.9231(3) 0.080(2) Uani 1 d . .
H49A H 0.8258(5) 0.8727(4) 0.9239(3) 0.096 Uiso 1 d R .
H49B H 0.8120(5) 0.7776(4) 0.8851(3) 0.096 Uiso 1 d R .
Cl2 Cl 1.01029(14) 0.77062(13) 0.90341(10) 0.1001(5) Uani 1 d . .
Cl3 Cl 0.80060(12) 0.73937(12) 1.00326(7) 0.0804(4) Uani 1 d . .
C50 C 0.9173(5) 0.9609(4) 0.7387(3) 0.0714(14) Uani 1 d . .
H50A H 0.9147(5) 0.9725(4) 0.7892(3) 0.086 Uiso 1 d R .
H50B H 0.8577(5) 0.9165(4) 0.7353(3) 0.086 Uiso 1 d R .
Cl4 Cl 0.8750(2) 1.07607(12) 0.68968(9) 0.1146(6) Uani 1 d . .
Cl5 Cl 1.06193(14) 0.9008(2) 0.71013(9) 0.1060(6) Uani 1 d . .
C51 C 0.5298(4) 0.9840(3) 0.8782(3) 0.0566(11) Uani 1 d . .
H51A H 0.5125(4) 0.9609(3) 0.8337(3) 0.068 Uiso 1 d R .
H51B H 0.5468(4) 0.9243(3) 0.9127(3) 0.068 Uiso 1 d R .
Cl6 Cl 0.65881(11) 1.04310(8) 0.86234(7) 0.0634(3) Uani 1 d . .
Cl7 Cl 0.40148(10) 1.06609(8) 0.91260(6) 0.0599(3) Uani 1 d . .
C52 C 0.9775(6) 0.1841(4) 0.8860(4) 0.128(3) Uani 1 d D .
Cl8 Cl 1.0011(3) 0.0575(2) 0.9075(2) 0.1384(12) Uani 0.870(5) d
PD .
Cl9 Cl 1.0698(2) 0.2248(2) 0.81573(11) 0.1224(10) Uani 0.878(5) d
PD .
Cl10 Cl 0.8403(8) 0.2132(7) 0.8552(4) 0.125(4) Uani 0.250(5) d PD
.

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 0.02571(14) 0.02361(14) 0.02494(15) -0.00026(10) -0.00401(10)
-0.00610(10)
B1 0.029(2) 0.027(2) 0.032(2) -0.0015(15) -0.0049(15) -0.0077(15)
O1 0.0383(13) 0.0288(12) 0.0300(12) 0.0006(9) 0.0022(10)
-0.0034(10)
O2 0.0371(13) 0.0293(12) 0.0293(12) -0.0038(9) -0.0038(10)
-0.0025(10)
C1 0.031(2) 0.030(2) 0.037(2) -0.0052(14) 0.0014(14) -0.0076(14)
C2 0.028(2) 0.030(2) 0.037(2) -0.0080(14) -0.0054(14) -0.0069(13)
C3 0.037(2) 0.031(2) 0.050(2) -0.007(2) -0.013(2) -0.0051(15)
C4 0.035(2) 0.032(2) 0.069(3) -0.017(2) -0.006(2) -0.003(2)
C5 0.040(2) 0.043(2) 0.060(3) -0.019(2) 0.013(2) -0.010(2)
C6 0.051(2) 0.042(2) 0.044(2) -0.008(2) 0.011(2) -0.015(2)
B2 0.036(2) 0.031(2) 0.025(2) 0.0030(15) -0.004(2) -0.008(2)
O3 0.0446(14) 0.0383(13) 0.0346(13) -0.0041(10) -0.0059(11)
-0.0196(11)
O4 0.0289(12) 0.0463(14) 0.0419(14) -0.0019(11) -0.0077(10)
-0.0116(11)
C7 0.055(2) 0.060(2) 0.028(2) 0.001(2) -0.009(2) -0.037(2)
C8 0.043(2) 0.066(3) 0.036(2) 0.003(2) -0.009(2) -0.029(2)
C9 0.044(2) 0.110(4) 0.063(3) -0.006(3) -0.008(2) -0.035(3)
C10 0.063(3) 0.164(6) 0.063(3) -0.004(4) -0.012(3) -0.077(4)
C11 0.098(4) 0.131(5) 0.048(3) -0.009(3) -0.008(3) -0.088(4)
C12 0.086(3) 0.077(3) 0.040(2) -0.007(2) -0.004(2) -0.053(3)
Cl1 0.0400(4) 0.0305(4) 0.0303(4) -0.0015(3) -0.0080(3)
-0.0133(3)
P1 0.0281(4) 0.0264(4) 0.0268(4) 0.0011(3) -0.0037(3) -0.0075(3)
C13 0.033(2) 0.029(2) 0.030(2) -0.0004(13) 0.0006(14) -0.0105(14)
C14 0.038(2) 0.039(2) 0.035(2) -0.003(2) -0.0021(15) -0.009(2)
C15 0.039(2) 0.037(2) 0.051(2) -0.005(2) 0.003(2) -0.003(2)
C16 0.059(2) 0.038(2) 0.046(2) -0.009(2) 0.012(2) -0.011(2)
C17 0.072(3) 0.045(2) 0.030(2) -0.006(2) 0.002(2) -0.022(2)
C18 0.047(2) 0.034(2) 0.033(2) -0.0007(15) -0.004(2) -0.012(2)
C19 0.034(2) 0.028(2) 0.030(2) -0.0028(13) -0.0058(14)
-0.0057(14)
C20 0.034(2) 0.037(2) 0.040(2) 0.002(2) -0.0074(15) -0.0071(15)
C21 0.035(2) 0.052(2) 0.061(3) 0.001(2) -0.012(2) -0.007(2)
C22 0.045(2) 0.046(2) 0.053(2) 0.001(2) -0.022(2) 0.002(2)
C23 0.054(2) 0.042(2) 0.038(2) 0.008(2) -0.015(2) -0.001(2)
C24 0.041(2) 0.039(2) 0.037(2) 0.003(2) -0.007(2) -0.009(2)
C25 0.034(2) 0.029(2) 0.027(2) 0.0029(13) -0.0067(13) -0.0099(14)
C26 0.034(2) 0.036(2) 0.050(2) 0.000(2) -0.001(2) -0.010(2)
C27 0.037(2) 0.046(2) 0.073(3) 0.003(2) -0.006(2) -0.017(2)
C28 0.055(2) 0.043(2) 0.050(2) 0.005(2) -0.014(2) -0.026(2)
C29 0.060(2) 0.029(2) 0.043(2) -0.002(2) -0.005(2) -0.013(2)
C30 0.042(2) 0.034(2) 0.040(2) 0.003(2) -0.002(2) -0.011(2)
C31 0.033(2) 0.036(2) 0.028(2) 0.0059(14) -0.0074(14) -0.0115(14)
P2 0.0284(4) 0.0260(4) 0.0272(4) 0.0008(3) -0.0053(3) -0.0056(3)
C32 0.048(2) 0.038(2) 0.039(2) -0.003(2) -0.015(2) -0.006(2)
C33 0.060(3) 0.048(2) 0.046(2) -0.007(2) -0.016(2) -0.017(2)
C34 0.051(2) 0.062(3) 0.043(2) 0.002(2) -0.020(2) -0.028(2)
C35 0.038(2) 0.062(3) 0.047(2) 0.007(2) -0.018(2) -0.009(2)
C36 0.036(2) 0.042(2) 0.040(2) 0.001(2) -0.010(2) -0.007(2)
C37 0.035(2) 0.025(2) 0.029(2) -0.0016(13) -0.0025(13)
-0.0053(13)
C38 0.037(2) 0.037(2) 0.036(2) 0.0047(15) -0.0029(15) -0.001(2)
C39 0.046(2) 0.038(2) 0.034(2) 0.004(2) 0.007(2) -0.001(2)
C40 0.043(2) 0.036(2) 0.048(2) -0.009(2) 0.014(2) -0.010(2)
C41 0.037(2) 0.057(2) 0.042(2) -0.013(2) 0.002(2) -0.015(2)
C42 0.036(2) 0.047(2) 0.031(2) -0.005(2) -0.0025(15) -0.011(2)
C43 0.033(2) 0.026(2) 0.029(2) 0.0025(13) -0.0092(13) -0.0025(13)
C44 0.042(2) 0.034(2) 0.035(2) -0.0022(15) -0.004(2) -0.006(2)
C45 0.058(2) 0.033(2) 0.050(2) -0.006(2) -0.005(2) -0.011(2)
C46 0.061(3) 0.038(2) 0.050(2) -0.014(2) -0.005(2) 0.003(2)
C47 0.043(2) 0.050(2) 0.042(2) -0.005(2) 0.004(2) 0.001(2)
C48 0.035(2) 0.038(2) 0.038(2) 0.003(2) -0.0031(15) -0.006(2)
C49 0.082(4) 0.081(4) 0.080(4) 0.014(3) -0.042(3) -0.013(3)
Cl2 0.0750(9) 0.1101(12) 0.1116(12) 0.0275(10) -0.0015(8)
-0.0341(9)
Cl3 0.0627(7) 0.0982(10) 0.0730(8) -0.0052(7) -0.0051(6)
0.0024(7)
C50 0.088(4) 0.070(3) 0.063(3) -0.010(2) 0.016(3) -0.045(3)
Cl4 0.169(2) 0.0782(10) 0.0877(11) 0.0090(8) 0.0308(11)
-0.0371(11)
Cl5 0.0660(9) 0.174(2) 0.0856(11) -0.0379(11) -0.0069(7)
-0.0253(10)
C51 0.053(2) 0.041(2) 0.075(3) -0.012(2) -0.001(2) -0.004(2)
Cl6 0.0582(6) 0.0520(6) 0.0824(8) -0.0228(6) 0.0040(6) -0.0126(5)
Cl7 0.0590(6) 0.0414(5) 0.0741(8) -0.0087(5) 0.0070(5) -0.0026(5)
C52 0.121(6) 0.108(6) 0.153(8) -0.017(5) 0.004(6) -0.020(5)
Cl8 0.155(2) 0.091(2) 0.169(3) 0.0012(15) -0.031(2) -0.0177(14)
Cl9 0.0896(14) 0.189(3) 0.0926(15) 0.0269(14) -0.0308(11)
-0.0451(14)
Cl10 0.137(7) 0.131(7) 0.105(6) -0.009(5) 0.011(5) -0.036(5)

_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 B1 1.954(4) . ?
Rh1 B2 2.008(4) . ?
Rh1 P2 2.3285(8) . ?
Rh1 P1 2.3369(8) . ?
Rh1 Cl1 2.4375(8) . ?
B1 O1 1.400(4) . ?
B1 O2 1.407(4) . ?
O1 C1 1.387(4) . ?
O2 C2 1.381(4) . ?
C1 C6 1.376(5) . ?
C1 C2 1.377(5) . ?
C2 C3 1.370(5) . ?
C3 C4 1.390(5) . ?
C4 C5 1.377(6) . ?
C5 C6 1.390(5) . ?
B2 O4 1.400(5) . ?
B2 O3 1.404(4) . ?
O3 C7 1.378(4) . ?
O4 C8 1.391(4) . ?
C7 C8 1.369(6) . ?
C7 C12 1.385(5) . ?
C8 C9 1.372(6) . ?
C9 C10 1.393(8) . ?
C10 C11 1.374(9) . ?
C11 C12 1.387(7) . ?
P1 C19 1.820(3) . ?
P1 C13 1.826(3) . ?
P1 C25 1.833(3) . ?
C13 C18 1.392(5) . ?
C13 C14 1.396(5) . ?
C14 C15 1.382(5) . ?
C15 C16 1.380(6) . ?
C16 C17 1.377(6) . ?
C17 C18 1.393(5) . ?
C19 C20 1.388(5) . ?
C19 C24 1.394(5) . ?
C20 C21 1.389(5) . ?
C21 C22 1.385(6) . ?
C22 C23 1.376(6) . ?
C23 C24 1.383(5) . ?
C25 C30 1.389(5) . ?
C25 C26 1.389(5) . ?
C26 C27 1.388(5) . ?
C27 C28 1.370(6) . ?
C28 C29 1.373(6) . ?
C29 C30 1.385(5) . ?
C31 C32 1.390(5) . ?
C31 C36 1.391(5) . ?
C31 P2 1.831(3) . ?
P2 C37 1.821(3) . ?
P2 C43 1.825(3) . ?
C32 C33 1.388(5) . ?
C33 C34 1.368(6) . ?
C34 C35 1.379(6) . ?
C35 C36 1.384(5) . ?
C37 C42 1.385(5) . ?
C37 C38 1.399(5) . ?
C38 C39 1.387(5) . ?
C39 C40 1.376(6) . ?
C40 C41 1.379(5) . ?
C41 C42 1.392(5) . ?
C43 C44 1.393(5) . ?
C43 C48 1.400(5) . ?
C44 C45 1.389(5) . ?
C45 C46 1.369(6) . ?
C46 C47 1.379(6) . ?
C47 C48 1.379(5) . ?
C49 Cl3 1.732(6) . ?
C49 Cl2 1.752(6) . ?
C50 Cl5 1.728(5) . ?
C50 Cl4 1.745(5) . ?
C51 Cl7 1.755(4) . ?
C51 Cl6 1.757(4) . ?
C52 Cl10 1.674(5) . ?
C52 Cl9 1.697(5) . ?
C52 Cl8 1.699(5) . ?

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
B1 Rh1 B2 78.9(2) . . ?
B1 Rh1 P2 94.45(11) . . ?
B2 Rh1 P2 89.12(10) . . ?
B1 Rh1 P1 93.90(11) . . ?
B2 Rh1 P1 86.68(10) . . ?
P2 Rh1 P1 169.75(3) . . ?
B1 Rh1 Cl1 118.89(11) . . ?
B2 Rh1 Cl1 162.07(11) . . ?
P2 Rh1 Cl1 91.77(3) . . ?
P1 Rh1 Cl1 89.38(3) . . ?
O1 B1 O2 109.1(3) . . ?
O1 B1 Rh1 127.1(2) . . ?
O2 B1 Rh1 123.4(2) . . ?
C1 O1 B1 106.2(3) . . ?
C2 O2 B1 106.3(3) . . ?
C6 C1 C2 122.2(3) . . ?
C6 C1 O1 128.6(3) . . ?
C2 C1 O1 109.2(3) . . ?
C3 C2 C1 122.4(3) . . ?
C3 C2 O2 128.3(3) . . ?
C1 C2 O2 109.2(3) . . ?
C2 C3 C4 116.0(4) . . ?
C5 C4 C3 121.7(3) . . ?
C4 C5 C6 122.0(4) . . ?
C1 C6 C5 115.7(4) . . ?
O4 B2 O3 109.3(3) . . ?
O4 B2 Rh1 118.5(3) . . ?
O3 B2 Rh1 131.9(3) . . ?
C7 O3 B2 106.0(3) . . ?
C8 O4 B2 105.9(3) . . ?
C8 C7 O3 109.7(3) . . ?
C8 C7 C12 122.3(4) . . ?
O3 C7 C12 128.0(4) . . ?
C7 C8 C9 122.5(4) . . ?
C7 C8 O4 109.0(3) . . ?
C9 C8 O4 128.4(4) . . ?
C8 C9 C10 115.7(5) . . ?
C11 C10 C9 121.8(5) . . ?
C10 C11 C12 122.2(5) . . ?
C7 C12 C11 115.5(5) . . ?
C19 P1 C13 106.40(15) . . ?
C19 P1 C25 102.91(15) . . ?
C13 P1 C25 104.32(15) . . ?
C19 P1 Rh1 119.85(11) . . ?
C13 P1 Rh1 104.46(11) . . ?
C25 P1 Rh1 117.49(11) . . ?
C18 C13 C14 119.0(3) . . ?
C18 C13 P1 123.3(3) . . ?
C14 C13 P1 117.6(3) . . ?
C15 C14 C13 120.6(3) . . ?
C16 C15 C14 120.2(4) . . ?
C17 C16 C15 119.8(4) . . ?
C16 C17 C18 120.7(4) . . ?
C13 C18 C17 119.7(4) . . ?
C20 C19 C24 119.2(3) . . ?
C20 C19 P1 120.3(3) . . ?
C24 C19 P1 120.5(3) . . ?
C19 C20 C21 120.1(3) . . ?
C22 C21 C20 120.2(4) . . ?
C23 C22 C21 120.0(3) . . ?
C22 C23 C24 120.2(3) . . ?
C23 C24 C19 120.4(3) . . ?
C30 C25 C26 118.3(3) . . ?
C30 C25 P1 119.9(3) . . ?
C26 C25 P1 121.7(3) . . ?
C27 C26 C25 120.3(3) . . ?
C28 C27 C26 120.8(4) . . ?
C27 C28 C29 119.5(3) . . ?
C28 C29 C30 120.3(4) . . ?
C29 C30 C25 120.8(3) . . ?
C32 C31 C36 118.6(3) . . ?
C32 C31 P2 119.5(3) . . ?
C36 C31 P2 121.8(3) . . ?
C37 P2 C43 104.06(15) . . ?
C37 P2 C31 104.48(15) . . ?
C43 P2 C31 104.90(15) . . ?
C37 P2 Rh1 119.84(11) . . ?
C43 P2 Rh1 103.48(10) . . ?
C31 P2 Rh1 118.22(11) . . ?
C33 C32 C31 120.5(4) . . ?
C34 C33 C32 120.2(4) . . ?
C33 C34 C35 120.0(4) . . ?
C34 C35 C36 120.3(4) . . ?
C35 C36 C31 120.3(4) . . ?
C42 C37 C38 119.3(3) . . ?
C42 C37 P2 119.8(3) . . ?
C38 C37 P2 120.7(3) . . ?
C39 C38 C37 120.0(3) . . ?
C40 C39 C38 120.4(3) . . ?
C39 C40 C41 120.0(3) . . ?
C40 C41 C42 120.3(4) . . ?
C37 C42 C41 120.1(3) . . ?
C44 C43 C48 118.7(3) . . ?
C44 C43 P2 122.5(3) . . ?
C48 C43 P2 118.6(2) . . ?
C45 C44 C43 120.0(3) . . ?
C46 C45 C44 120.5(4) . . ?
C45 C46 C47 120.1(4) . . ?
C46 C47 C48 120.1(4) . . ?
C47 C48 C43 120.5(3) . . ?
Cl3 C49 Cl2 112.9(3) . . ?
Cl5 C50 Cl4 112.5(3) . . ?
Cl7 C51 Cl6 111.1(2) . . ?
Cl10 C52 Cl9 101.9(4) . . ?
Cl10 C52 Cl8 106.0(5) . . ?
Cl9 C52 Cl8 115.3(4) . . ?

_refine_diff_density_max    1.001
_refine_diff_density_min   -0.746
_refine_diff_density_rms    0.067

#===END

data_4d


_audit_creation_method            SHELXL
_chemical_name_systematic
;
 Bis(3-Me-boryl)bis(triphenylphosphine)Rhodium(III)Chloride
;
_chemical_name_common             ?
_chemical_formula_moiety          ?
_chemical_formula_structural
'Rh (CH3 C6 H3 O2 B)2 (P(C6 H5)3)2 Cl (C H2 Cl 2)3 (C6 H 14)0.5'
_chemical_formula_analytical      ?
_chemical_formula_sum             'C56 H55 B2 Cl7 O4 P2 Rh'
_chemical_formula_weight          1226.62
_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'
 'B'  'B'   0.0013   0.0007
 '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'
 'Rh'  'Rh'  -1.1178   0.9187
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting            'triclinic'
_symmetry_space_group_name_H-M    'P -1'

loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'

_cell_length_a                    10.939(4)
_cell_length_b                    13.843(6)
_cell_length_c                    19.916(7)
_cell_angle_alpha                 80.34(3)
_cell_angle_beta                  81.99(3)
_cell_angle_gamma                 77.63(3)
_cell_volume                      2887.3(20)
_cell_formula_units_Z             2
_cell_measurement_temperature     173(2)
_cell_measurement_reflns_used     216
_cell_measurement_theta_min       5
_cell_measurement_theta_max       50

_exptl_crystal_description        plate
_exptl_crystal_colour             ?
_exptl_crystal_size_max           0.5
_exptl_crystal_size_mid           0.2
_exptl_crystal_size_min           0.05
_exptl_crystal_density_meas       'not measured'
_exptl_crystal_density_diffrn     1.411
_exptl_crystal_density_method     ?
_exptl_crystal_F_000              1254
_exptl_absorpt_coefficient_mu     0.719
_exptl_absorpt_correction_type
'Empirical, pseudo-azimuthal scan, (Siemens, 1995a)'
_exptl_absorpt_correction_T_min   0.288
_exptl_absorpt_correction_T_max   0.526

_exptl_special_details
;
 ?
;

#================================================================
# 7. EXPERIMENTAL DATA

_diffrn_ambient_temperature       173(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 Area Detector'
_diffrn_measurement_method        '\w rotation with narrow frames'
_diffrn_reflns_theta_full       ?
_diffrn_detector_area_resol_mean  60
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         none
_diffrn_reflns_number             17737
_diffrn_reflns_av_R_equivalents   0.0883
_diffrn_reflns_av_sigmaI/netI     0.2838
_diffrn_reflns_limit_h_min        -14
_diffrn_reflns_limit_h_max        13
_diffrn_reflns_limit_k_min        -17
_diffrn_reflns_limit_k_max        7
_diffrn_reflns_limit_l_min        -25
_diffrn_reflns_limit_l_max        24
_diffrn_reflns_theta_min          1.72
_diffrn_reflns_theta_max          27.51
_reflns_number_total              12337
_reflns_number_observed           4356
_reflns_observed_criterion        >2sigma(I)


_computing_data_collection        'SMART (Siemens, 1995b)'
_computing_cell_refinement        'SAINT (Siemens, 1995b)'
_computing_data_reduction         'SAINT (Siemens, 1995b)'
_computing_structure_solution     'SHELXTL (Siemens, 1995a)'
_computing_structure_refinement   'SHELXTL (Siemens, 1995a)'
_computing_molecular_graphics     'SHELXTL (Siemens, 1995a)'
_computing_publication_material   'SHELXTL (Siemens, 1995a)'


#================================================================

# 8. REFINEMENT DATA

_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^)+(0.1355P)^2^+8.18P] where P=(Max(Fo^2^)+2Fc^2^)/3'
_refine_ls_hydrogen_treatment     'see text'
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        none
_refine_ls_number_reflns          12337
_refine_ls_number_parameters      642
_refine_ls_number_restraints      24
_refine_ls_R_factor_all           0.2386
_refine_ls_R_factor_obs           0.1083
_refine_ls_wR_factor_all          0.3042
_refine_ls_wR_factor_obs          0.2459
_refine_ls_goodness_of_fit_all    0.899
_refine_ls_goodness_of_fit_obs    1.248
_refine_ls_restrained_S_all       0.904
_refine_ls_restrained_S_obs       1.256
_refine_ls_shift/esd_max          -0.063
_refine_ls_shift/esd_mean         0.004
_refine_diff_density_max   2.625
_refine_diff_density_min   -1.841
_refine_diff_density_rms          0.184
#================================================================

# 9. ATOMIC COORDINATES AND THERMAL PARAMETERS

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 0.57522(8) 0.69362(7) 0.72845(4) 0.0308(3) Uani 1 d . .
P1 P 0.5558(2) 0.8049(2) 0.62712(13) 0.0304(7) Uani 1 d . .
P2 P 0.5617(3) 0.5943(2) 0.83561(13) 0.0303(7) Uani 1 d . .
B1 B 0.4303(11) 0.6375(11) 0.7067(6) 0.031(3) Uani 1 d . .
B2 B 0.6694(10) 0.5861(9) 0.6829(6) 0.027(3) Uani 1 d U .
O1 O 0.4302(6) 0.5546(6) 0.6757(4) 0.042(2) Uani 1 d . .
O2 O 0.3095(6) 0.6885(6) 0.7234(3) 0.036(2) Uani 1 d . .
O3 O 0.7251(7) 0.4900(6) 0.7168(3) 0.037(2) Uani 1 d . .
O4 O 0.7131(7) 0.5850(6) 0.6127(3) 0.033(2) Uani 1 d . .
Cl1 Cl 0.6888(3) 0.7998(2) 0.77342(13) 0.0402(8) Uani 1 d . .
C11 C 0.4851(10) 0.9226(10) 0.6549(5) 0.038(3) Uani 1 d . .
C12 C 0.3921(10) 0.9207(9) 0.7018(5) 0.037(3) Uani 1 d U .
H12 H 0.3653(10) 0.8598(9) 0.7203(5) 0.044 Uiso 1 calc R .
C13 C 0.3268(12) 1.0171(11) 0.7266(6) 0.057(4) Uani 1 d . .
H13 H 0.2519(12) 1.0196(11) 0.7573(6) 0.069 Uiso 1 calc R .
C14 C 0.3782(13) 1.1057(10) 0.7038(7) 0.058(4) Uani 1 d . .
H14 H 0.3421(13) 1.1666(10) 0.7211(7) 0.070 Uiso 1 calc R .
C15 C 0.4841(12) 1.0983(11) 0.6550(6) 0.052(4) Uani 1 d . .
H15 H 0.5192(12) 1.1558(11) 0.6378(6) 0.062 Uiso 1 calc R .
C16 C 0.5361(11) 1.0119(10) 0.6323(6) 0.041(3) Uani 1 d . .
H16 H 0.6092(11) 1.0091(10) 0.6002(6) 0.050 Uiso 1 calc R .
C21 C 0.4451(10) 0.7900(9) 0.5693(5) 0.033(3) Uani 1 d . .
C22 C 0.3428(10) 0.8641(10) 0.5545(5) 0.043(3) Uani 1 d . .
H22 H 0.3277(10) 0.9235(10) 0.5748(5) 0.052 Uiso 1 calc R .
C23 C 0.2608(10) 0.8525(10) 0.5097(6) 0.044(3) Uani 1 d . .
H23 H 0.1918(10) 0.9047(10) 0.4983(6) 0.053 Uiso 1 calc R .
C24 C 0.2809(11) 0.7654(11) 0.4825(6) 0.046(3) Uani 1 d . .
H24 H 0.2245(11) 0.7555(11) 0.4532(6) 0.055 Uiso 1 calc R .
C25 C 0.3817(12) 0.6937(11) 0.4978(6) 0.052(3) Uani 1 d . .
H25 H 0.3953(12) 0.6337(11) 0.4783(6) 0.062 Uiso 1 calc R .
C26 C 0.4661(11) 0.7033(10) 0.5405(5) 0.040(3) Uani 1 d . .
H26 H 0.5368(11) 0.6516(10) 0.5499(5) 0.048 Uiso 1 calc R .
C31 C 0.6972(10) 0.8254(8) 0.5700(5) 0.031(3) Uani 1 d . .
C32 C 0.6916(10) 0.8585(8) 0.5012(5) 0.033(3) Uani 1 d . .
H32 H 0.6147(10) 0.8680(8) 0.4817(5) 0.039 Uiso 1 calc R .
C33 C 0.8015(10) 0.8782(9) 0.4600(6) 0.040(3) Uani 1 d . .
H33 H 0.7993(10) 0.8990(9) 0.4122(6) 0.048 Uiso 1 calc R .
C34 C 0.9102(10) 0.8678(9) 0.4880(6) 0.042(3) Uani 1 d . .
H34 H 0.9823(10) 0.8848(9) 0.4599(6) 0.050 Uiso 1 calc R .
C35 C 0.9183(10) 0.8337(10) 0.5551(6) 0.048(4) Uani 1 d . .
H35 H 0.9964(10) 0.8239(10) 0.5734(6) 0.057 Uiso 1 calc R .
C36 C 0.8078(10) 0.8121(10) 0.5991(6) 0.047(3) Uani 1 d . .
H36 H 0.8113(10) 0.7894(10) 0.6466(6) 0.056 Uiso 1 calc R .
C41 C 0.7046(10) 0.5230(8) 0.8698(5) 0.034(3) Uani 1 d . .
C42 C 0.8211(10) 0.5499(9) 0.8448(6) 0.043(3) Uani 1 d U .
H42 H 0.8252(10) 0.6047(9) 0.8093(6) 0.052 Uiso 1 calc R .
C43 C 0.9302(12) 0.4965(11) 0.8718(7) 0.069(5) Uani 1 d . .
H43 H 1.0082(12) 0.5161(11) 0.8548(7) 0.082 Uiso 1 calc R .
C44 C 0.9281(11) 0.4190(12) 0.9206(6) 0.065(4) Uani 1 d . .
H44 H 1.0039(11) 0.3829(12) 0.9381(6) 0.078 Uiso 1 calc R .
C45 C 0.8103(11) 0.3897(11) 0.9470(6) 0.058(4) Uani 1 d . .
H45 H 0.8070(11) 0.3352(11) 0.9828(6) 0.069 Uiso 1 calc R .
C46 C 0.7043(10) 0.4408(10) 0.9202(6) 0.045(3) Uani 1 d . .
H46 H 0.6271(10) 0.4196(10) 0.9364(6) 0.053 Uiso 1 calc R .
C51 C 0.4558(10) 0.5044(9) 0.8482(5) 0.034(3) Uani 1 d . .
C52 C 0.4900(12) 0.4217(10) 0.8147(6) 0.050(3) Uani 1 d . .
H52 H 0.5676(12) 0.4127(10) 0.7863(6) 0.060 Uiso 1 calc R .
C53 C 0.4129(13) 0.3496(11) 0.8214(6) 0.062(4) Uani 1 d . .
H53 H 0.4367(13) 0.2931(11) 0.7978(6) 0.074 Uiso 1 calc R .
C54 C 0.2992(13) 0.3660(11) 0.8647(7) 0.059(4) Uani 1 d . .
H54 H 0.2450(13) 0.3193(11) 0.8703(7) 0.071 Uiso 1 calc R .
C55 C 0.2649(11) 0.4462(11) 0.8985(7) 0.060(4) Uani 1 d . .
H55 H 0.1868(11) 0.4556(11) 0.9265(7) 0.072 Uiso 1 calc R .
C56 C 0.3439(10) 0.5162(10) 0.8926(6) 0.047(3) Uani 1 d . .
H56 H 0.3216(10) 0.5705(10) 0.9183(6) 0.056 Uiso 1 calc R .
C61 C 0.4881(11) 0.6828(9) 0.8954(5) 0.042(3) Uani 1 d . .
C62 C 0.4800(12) 0.7536(11) 0.9974(6) 0.052(4) Uani 1 d . .
H62 H 0.5127(12) 0.7534(11) 1.0392(6) 0.063 Uiso 1 calc R .
C63 C 0.5389(11) 0.6832(10) 0.9552(5) 0.043(3) Uani 1 d . .
H63A H 0.6124(11) 0.6363(10) 0.9671(5) 0.051 Uiso 1 calc R .
C64 C 0.3725(13) 0.8256(9) 0.9796(6) 0.050(3) Uani 1 d . .
H64 H 0.3335(13) 0.8760(9) 1.0071(6) 0.060 Uiso 1 calc R .
C65 C 0.3270(11) 0.8175(10) 0.9181(7) 0.054(4) Uani 1 d . .
H65 H 0.2537(11) 0.8631(10) 0.9043(7) 0.065 Uiso 1 calc R .
C66 C 0.3885(9) 0.7415(9) 0.8749(5) 0.029(2) Uani 1 d U .
H66 H 0.3566(9) 0.7359(9) 0.8340(5) 0.035 Uiso 1 calc R .
C71 C 0.3006(10) 0.5586(9) 0.6739(5) 0.034(3) Uani 1 d . .
C72 C 0.2304(10) 0.6345(10) 0.7029(5) 0.037(3) Uani 1 d . .
C73 C 0.0983(10) 0.6539(11) 0.7096(6) 0.055(4) Uani 1 d . .
H73 H 0.0475(10) 0.7081(11) 0.7304(6) 0.066 Uiso 1 calc R .
C74 C 0.0488(12) 0.5845(14) 0.6823(6) 0.067(5) Uani 1 d . .
H74 H -0.0402(12) 0.5920(14) 0.6858(6) 0.081 Uiso 1 calc R .
C75 C 0.1176(11) 0.5100(11) 0.6523(6) 0.048(3) Uani 1 d . .
H75 H 0.0765(11) 0.4697(11) 0.6324(6) 0.057 Uiso 1 calc R .
C76 C 0.2497(11) 0.4882(11) 0.6487(6) 0.047(3) Uani 1 d . .
C77 C 0.3311(13) 0.4045(12) 0.6199(9) 0.077(5) Uani 1 d . .
H77A H 0.3973(58) 0.3739(47) 0.6497(27) 0.116 Uiso 1 calc R .
H77B H 0.3696(74) 0.4281(17) 0.5743(22) 0.116 Uiso 1 calc R .
H77C H 0.2814(23) 0.3549(37) 0.6161(50) 0.116 Uiso 1 calc R .
C81 C 0.8044(10) 0.4374(9) 0.6683(6) 0.037(3) Uani 1 d . .
C82 C 0.7923(10) 0.4973(9) 0.6035(5) 0.032(3) Uani 1 d . .
C83 C 0.8617(11) 0.4652(11) 0.5464(6) 0.048(3) Uani 1 d . .
H83 H 0.8554(11) 0.5039(11) 0.5024(6) 0.058 Uiso 1 calc R .
C84 C 0.9438(12) 0.3711(10) 0.5559(6) 0.049(3) Uani 1 d . .
H84 H 0.9943(12) 0.3465(10) 0.5173(6) 0.059 Uiso 1 calc R .
C85 C 0.9531(10) 0.3137(11) 0.6198(7) 0.049(3) Uani 1 d . .
H85 H 1.0099(10) 0.2512(11) 0.6243(7) 0.059 Uiso 1 calc R .
C86 C 0.8804(12) 0.3469(11) 0.6767(7) 0.051(4) Uani 1 d . .
C87 C 0.8939(17) 0.2892(13) 0.7506(8) 0.099(6) Uani 1 d . .
H87A H 0.8115(26) 0.2978(76) 0.7778(20) 0.149 Uiso 1 calc R .
H87B H 0.9526(89) 0.3156(62) 0.7721(24) 0.149 Uiso 1 calc R .
H87C H 0.9261(110) 0.2180(19) 0.7481(9) 0.149 Uiso 1 calc R .
Cl6 Cl 0.0533(5) 0.9387(5) 0.6975(3) 0.145(2) Uani 1 d . .
Cl4 Cl 0.3365(5) 0.9414(6) 1.1466(3) 0.153(3) Uani 1 d . .
Cl7 Cl -0.1701(5) 1.0802(5) 0.6699(3) 0.130(2) Uani 1 d . .
Cl5 Cl 0.5998(4) 0.9271(4) 1.1015(3) 0.105(2) Uani 1 d . .
C97 C 0.4600(15) 1.0026(14) 1.1308(10) 0.112(7) Uani 1 d . .
H97A H 0.4719(15) 1.0258(14) 1.1734(10) 0.135 Uiso 1 calc R .
H97B H 0.4399(15) 1.0622(14) 1.0961(10) 0.135 Uiso 1 calc R .
C98 C -0.1003(18) 0.9684(14) 0.7194(11) 0.132(8) Uani 1 d . .
H98A H -0.1158(18) 0.9766(14) 0.7684(11) 0.158 Uiso 1 calc R .
H98B H -0.1402(18) 0.9133(14) 0.7131(11) 0.158 Uiso 1 calc R .
Cl9 Cl 0.0357(5) 0.7461(6) 0.8853(3) 0.140(2) Uani 1 d . .
Cl8 Cl -0.1789(6) 0.7950(6) 0.9802(3) 0.159(3) Uani 1 d . .
C99 C -0.1210(20) 0.7762(26) 0.9066(12) 0.219(18) Uani 1 d . .
H99A H -0.1524(20) 0.8373(26) 0.8753(12) 0.263 Uiso 1 calc R .
H99B H -0.1577(20) 0.7222(26) 0.8954(12) 0.263 Uiso 1 calc R .
C101 C 0.0352(15) 0.9785(32) 1.0190(21) 0.189(17) Uani 1 d . .
C100 C -0.0170(24) 0.9288(29) 1.1037(18) 0.221(17) 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 0.0291(5) 0.0430(7) 0.0241(4) 0.0111(4) -0.0035(3) -0.0270(4)
P1 0.0282(14) 0.042(2) 0.0236(14) 0.0121(13) -0.0053(11)
-0.0242(15)
P2 0.0308(15) 0.039(2) 0.0247(14) 0.0094(13) -0.0051(11)
-0.0230(15)
B1 0.028(7) 0.038(9) 0.028(6) -0.009(6) -0.001(5) -0.005(6)
B2 0.020(4) 0.029(5) 0.030(4) 0.008(4) -0.013(3) -0.007(4)
O1 0.031(4) 0.051(6) 0.040(4) 0.012(4) 0.003(3) -0.017(4)
O2 0.028(4) 0.046(5) 0.037(4) 0.002(4) -0.007(3) -0.019(4)
O3 0.039(4) 0.037(5) 0.029(4) 0.007(4) 0.002(3) -0.008(4)
O4 0.041(4) 0.038(5) 0.020(4) 0.009(3) 0.000(3) -0.014(4)
Cl1 0.047(2) 0.049(2) 0.0314(15) 0.0116(13) -0.0085(12) -0.036(2)
C11 0.029(6) 0.061(9) 0.031(6) -0.004(6) -0.027(5) -0.009(6)
C12 0.046(4) 0.040(5) 0.031(4) 0.017(4) -0.020(4) -0.028(4)
C13 0.052(8) 0.059(11) 0.054(8) 0.012(7) 0.013(6) -0.022(8)
C14 0.072(9) 0.032(9) 0.067(9) -0.027(7) 0.006(8) 0.004(8)
C15 0.068(9) 0.045(10) 0.051(8) 0.000(7) -0.001(7) -0.040(8)
C16 0.050(7) 0.046(9) 0.035(6) 0.008(6) -0.013(5) -0.029(7)
C21 0.030(6) 0.044(8) 0.030(6) 0.013(5) -0.008(5) -0.027(6)
C22 0.039(6) 0.063(10) 0.031(6) 0.011(6) -0.007(5) -0.029(7)
C23 0.024(6) 0.059(10) 0.048(7) 0.013(7) -0.014(5) -0.014(6)
C24 0.035(7) 0.073(11) 0.040(7) -0.001(7) -0.006(5) -0.036(7)
C25 0.060(8) 0.049(10) 0.053(8) -0.001(7) -0.008(7) -0.030(8)
C26 0.043(7) 0.041(9) 0.038(7) 0.007(6) -0.015(5) -0.015(6)
C31 0.039(6) 0.031(7) 0.025(5) 0.001(5) 0.006(5) -0.019(6)
C32 0.034(6) 0.039(8) 0.024(5) 0.010(5) -0.004(4) -0.016(6)
C33 0.039(6) 0.037(8) 0.038(6) 0.013(5) 0.006(5) -0.016(6)
C34 0.038(7) 0.043(8) 0.048(7) -0.004(6) 0.009(5) -0.023(6)
C35 0.029(6) 0.082(11) 0.037(7) 0.006(6) -0.002(5) -0.032(7)
C36 0.039(6) 0.078(11) 0.028(6) 0.009(6) 0.000(5) -0.036(7)
C41 0.036(6) 0.036(8) 0.031(6) 0.011(5) -0.005(5) -0.021(6)
C42 0.038(4) 0.046(5) 0.044(5) 0.013(4) -0.002(4) -0.020(4)
C43 0.044(7) 0.082(12) 0.071(9) 0.048(8) -0.004(7) -0.039(8)
C44 0.039(7) 0.100(13) 0.053(8) 0.028(8) -0.033(6) -0.017(8)
C45 0.044(7) 0.082(11) 0.042(7) 0.039(7) -0.012(6) -0.032(8)
C46 0.028(6) 0.063(10) 0.040(7) 0.012(6) 0.004(5) -0.024(6)
C51 0.030(6) 0.039(8) 0.035(6) 0.015(5) -0.010(5) -0.020(6)
C52 0.052(8) 0.047(9) 0.050(8) 0.011(7) 0.010(6) -0.031(7)
C53 0.080(10) 0.074(11) 0.040(7) 0.012(7) -0.003(7) -0.053(9)
C54 0.061(9) 0.060(11) 0.066(9) 0.030(8) -0.033(7) -0.049(8)
C55 0.031(7) 0.060(11) 0.087(11) 0.028(8) -0.008(7) -0.030(7)
C56 0.033(6) 0.066(10) 0.048(7) 0.011(6) -0.008(5) -0.037(7)
C61 0.050(7) 0.053(9) 0.031(6) -0.003(6) 0.014(5) -0.043(7)
C62 0.060(8) 0.058(10) 0.040(7) 0.006(7) 0.000(6) -0.026(8)
C63 0.048(7) 0.056(9) 0.033(6) 0.005(6) -0.003(5) -0.039(7)
C64 0.073(9) 0.025(8) 0.046(8) 0.005(6) 0.015(7) -0.020(7)
C65 0.036(7) 0.056(10) 0.063(9) 0.008(7) -0.004(6) -0.006(7)
C66 0.026(4) 0.042(5) 0.029(4) 0.005(4) -0.016(3) -0.025(4)
C71 0.032(6) 0.037(8) 0.034(6) 0.019(5) -0.013(5) -0.025(6)
C72 0.040(6) 0.056(9) 0.024(6) 0.003(6) -0.008(5) -0.034(7)
C73 0.027(6) 0.084(12) 0.060(8) -0.013(8) 0.001(6) -0.028(7)
C74 0.040(7) 0.127(16) 0.048(8) -0.005(9) -0.001(6) -0.052(9)
C75 0.039(7) 0.064(11) 0.050(8) 0.000(7) -0.011(6) -0.034(7)
C76 0.038(7) 0.065(10) 0.045(7) -0.002(7) -0.005(5) -0.026(7)
C77 0.063(9) 0.066(12) 0.115(13) -0.031(10) 0.000(9) -0.032(9)
C81 0.032(6) 0.031(8) 0.053(8) 0.000(6) -0.012(5) -0.017(6)
C82 0.027(6) 0.038(8) 0.033(6) -0.004(5) 0.001(5) -0.018(6)
C83 0.049(7) 0.058(10) 0.040(7) -0.003(7) 0.003(6) -0.025(8)
C84 0.052(8) 0.053(10) 0.053(8) -0.016(7) 0.006(6) -0.033(8)
C85 0.029(6) 0.059(10) 0.062(9) -0.006(7) -0.012(6) -0.012(7)
C86 0.057(8) 0.046(10) 0.054(8) -0.005(7) 0.009(7) -0.029(8)
C87 0.134(16) 0.079(14) 0.068(11) 0.023(9) -0.010(11) -0.009(12)
Cl6 0.111(4) 0.154(6) 0.171(6) 0.014(5) -0.015(4) -0.057(4)
Cl4 0.125(4) 0.212(7) 0.157(5) -0.087(5) 0.063(4) -0.111(5)
Cl7 0.115(4) 0.164(6) 0.097(4) 0.040(4) -0.006(3) -0.047(4)
Cl5 0.098(3) 0.089(4) 0.131(4) -0.032(3) 0.028(3) -0.041(3)
C97 0.093(13) 0.101(17) 0.154(18) -0.052(14) 0.041(13) -0.054(13)
C98 0.123(16) 0.087(16) 0.166(20) 0.034(13) 0.044(15) -0.059(14)
Cl9 0.101(4) 0.217(8) 0.108(4) -0.028(4) 0.008(3) -0.053(5)
Cl8 0.118(4) 0.225(8) 0.109(4) 0.022(5) 0.018(4) -0.033(5)
C99 0.113(17) 0.407(51) 0.128(21) -0.143(27) -0.065(15) 0.083(24)
C101 0.032(14) 0.277(43) 0.283(44) -0.139(37) 0.020(19)
-0.034(22)
C100 0.111(20) 0.315(48) 0.260(37) -0.162(37) -0.018(22)
0.000(25)

#================================================================

# 10. MOLECULAR GEOMETRY

_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 B2 1.906(13) . ?
Rh1 B1 2.034(12) . ?
Rh1 P1 2.329(3) . ?
Rh1 P2 2.341(3) . ?
Rh1 Cl1 2.458(3) . ?
P1 C11 1.790(13) . ?
P1 C31 1.831(10) . ?
P1 C21 1.847(10) . ?
P2 C41 1.815(11) . ?
P2 C61 1.835(12) . ?
P2 C51 1.841(11) . ?
B1 O2 1.383(14) . ?
B1 O1 1.391(15) . ?
B2 O4 1.414(13) . ?
B2 O3 1.437(13) . ?
O1 C71 1.412(11) . ?
O2 C72 1.397(12) . ?
O3 C81 1.396(13) . ?
O4 C82 1.355(13) . ?
C11 C12 1.284(14) . ?
C11 C16 1.44(2) . ?
C12 C13 1.50(2) . ?
C13 C14 1.44(2) . ?
C14 C15 1.40(2) . ?
C15 C16 1.33(2) . ?
C21 C26 1.38(2) . ?
C21 C22 1.37(2) . ?
C22 C23 1.400(14) . ?
C23 C24 1.37(2) . ?
C24 C25 1.35(2) . ?
C25 C26 1.379(15) . ?
C31 C36 1.377(14) . ?
C31 C32 1.377(13) . ?
C32 C33 1.408(13) . ?
C33 C34 1.353(15) . ?
C34 C35 1.349(15) . ?
C35 C36 1.445(14) . ?
C41 C46 1.386(15) . ?
C41 C42 1.405(13) . ?
C42 C43 1.39(2) . ?
C43 C44 1.32(2) . ?
C44 C45 1.44(2) . ?
C45 C46 1.350(15) . ?
C51 C52 1.38(2) . ?
C51 C56 1.403(15) . ?
C52 C53 1.42(2) . ?
C53 C54 1.41(2) . ?
C54 C55 1.35(2) . ?
C55 C56 1.41(2) . ?
C61 C66 1.28(2) . ?
C61 C63 1.383(15) . ?
C62 C63 1.39(2) . ?
C62 C64 1.41(2) . ?
C64 C65 1.42(2) . ?
C65 C66 1.46(2) . ?
C71 C72 1.33(2) . ?
C71 C76 1.41(2) . ?
C72 C73 1.404(15) . ?
C73 C74 1.41(2) . ?
C74 C75 1.32(2) . ?
C75 C76 1.41(2) . ?
C76 C77 1.45(2) . ?
C81 C86 1.35(2) . ?
C81 C82 1.418(15) . ?
C82 C83 1.361(15) . ?
C83 C84 1.42(2) . ?
C84 C85 1.39(2) . ?
C85 C86 1.38(2) . ?
C86 C87 1.56(2) . ?
Cl6 C98 1.66(2) . ?
Cl4 C97 1.71(2) . ?
Cl7 C98 1.77(2) . ?
Cl5 C97 1.74(2) . ?
Cl9 C99 1.69(2) . ?
Cl8 C99 1.56(2) . ?
C101 C101 1.15(6) 2_577 ?
C101 C100 1.78(5) . ?

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
B2 Rh1 B1 80.9(5) . . ?
B2 Rh1 P1 93.4(3) . . ?
B1 Rh1 P1 88.4(4) . . ?
B2 Rh1 P2 93.8(3) . . ?
B1 Rh1 P2 87.2(4) . . ?
P1 Rh1 P2 170.81(11) . . ?
B2 Rh1 Cl1 118.9(3) . . ?
B1 Rh1 Cl1 160.2(4) . . ?
P1 Rh1 Cl1 91.07(10) . . ?
P2 Rh1 Cl1 90.34(10) . . ?
C11 P1 C31 106.1(5) . . ?
C11 P1 C21 102.7(5) . . ?
C31 P1 C21 104.3(5) . . ?
C11 P1 Rh1 104.2(4) . . ?
C31 P1 Rh1 119.6(4) . . ?
C21 P1 Rh1 118.0(3) . . ?
C41 P2 C61 106.6(5) . . ?
C41 P2 C51 104.2(5) . . ?
C61 P2 C51 103.8(5) . . ?
C41 P2 Rh1 119.5(3) . . ?
C61 P2 Rh1 104.5(4) . . ?
C51 P2 Rh1 116.8(3) . . ?
O2 B1 O1 111.7(10) . . ?
O2 B1 Rh1 117.4(9) . . ?
O1 B1 Rh1 130.9(8) . . ?
O4 B2 O3 105.2(9) . . ?
O4 B2 Rh1 129.6(8) . . ?
O3 B2 Rh1 124.8(8) . . ?
B1 O1 C71 102.7(9) . . ?
B1 O2 C72 105.2(9) . . ?
C81 O3 B2 108.5(8) . . ?
C82 O4 B2 110.4(8) . . ?
C12 C11 C16 121.3(12) . . ?
C12 C11 P1 115.3(10) . . ?
C16 C11 P1 123.1(9) . . ?
C11 C12 C13 118.2(11) . . ?
C14 C13 C12 119.7(11) . . ?
C15 C14 C13 117.1(12) . . ?
C16 C15 C14 121.1(12) . . ?
C15 C16 C11 122.2(11) . . ?
C26 C21 C22 119.8(10) . . ?
C26 C21 P1 119.2(9) . . ?
C22 C21 P1 121.0(10) . . ?
C21 C22 C23 120.4(12) . . ?
C24 C23 C22 119.4(11) . . ?
C25 C24 C23 119.1(11) . . ?
C24 C25 C26 123.1(13) . . ?
C21 C26 C25 118.1(11) . . ?
C36 C31 C32 121.1(9) . . ?
C36 C31 P1 117.6(7) . . ?
C32 C31 P1 121.1(8) . . ?
C31 C32 C33 119.0(10) . . ?
C34 C33 C32 120.6(10) . . ?
C35 C34 C33 121.3(10) . . ?
C34 C35 C36 119.8(10) . . ?
C31 C36 C35 118.1(10) . . ?
C46 C41 C42 117.6(10) . . ?
C46 C41 P2 122.3(8) . . ?
C42 C41 P2 120.1(8) . . ?
C43 C42 C41 120.2(10) . . ?
C44 C43 C42 121.5(11) . . ?
C43 C44 C45 119.5(11) . . ?
C46 C45 C44 119.1(10) . . ?
C45 C46 C41 122.1(10) . . ?
C52 C51 C56 119.4(11) . . ?
C52 C51 P2 118.8(8) . . ?
C56 C51 P2 121.7(10) . . ?
C51 C52 C53 122.1(11) . . ?
C54 C53 C52 116.7(14) . . ?
C55 C54 C53 121.9(12) . . ?
C54 C55 C56 120.8(12) . . ?
C51 C56 C55 119.0(13) . . ?
C66 C61 C63 125.9(12) . . ?
C66 C61 P2 112.6(9) . . ?
C63 C61 P2 121.5(10) . . ?
C63 C62 C64 121.5(12) . . ?
C61 C63 C62 118.6(12) . . ?
C65 C64 C62 115.4(12) . . ?
C64 C65 C66 122.5(11) . . ?
C61 C66 C65 116.2(10) . . ?
C72 C71 C76 123.3(10) . . ?
C72 C71 O1 111.4(9) . . ?
C76 C71 O1 125.2(12) . . ?
C71 C72 O2 108.9(9) . . ?
C71 C72 C73 123.1(11) . . ?
O2 C72 C73 128.0(12) . . ?
C72 C73 C74 112.9(13) . . ?
C75 C74 C73 124.4(12) . . ?
C74 C75 C76 122.3(12) . . ?
C71 C76 C75 113.8(13) . . ?
C71 C76 C77 120.8(11) . . ?
C75 C76 C77 125.3(12) . . ?
C86 C81 O3 129.7(11) . . ?
C86 C81 C82 123.0(12) . . ?
O3 C81 C82 107.3(10) . . ?
O4 C82 C83 131.2(11) . . ?
O4 C82 C81 108.6(9) . . ?
C83 C82 C81 120.1(12) . . ?
C82 C83 C84 116.5(12) . . ?
C85 C84 C83 122.2(12) . . ?
C86 C85 C84 120.3(13) . . ?
C81 C86 C85 117.8(13) . . ?
C81 C86 C87 119.3(12) . . ?
C85 C86 C87 122.5(13) . . ?
Cl4 C97 Cl5 112.4(10) . . ?
Cl6 C98 Cl7 112.0(9) . . ?
Cl8 C99 Cl9 122.3(12) . . ?
C101 C101 C100 121.4(33) 2_577 . ?

#===END

data_12

_audit_creation_method            SHELXL
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_formula_moiety          ?
_chemical_formula_structural      ?
_chemical_formula_analytical      ?
_chemical_formula_sum
 'C24 H38 B2 Cl O4 P2 Rh'
_chemical_formula_weight          612.46
_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'
 'B'  'B'   0.0013   0.0007
 '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'
 '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    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                    13.9618(14)
_cell_length_b                    10.4578(11)
_cell_length_c                    19.219(2)
_cell_angle_alpha                 90.00
_cell_angle_beta                  92.337(3)
_cell_angle_gamma                 90.00
_cell_volume                      2803.8(5)
_cell_formula_units_Z             4
_cell_measurement_temperature     160(2)
_cell_measurement_reflns_used     11682
_cell_measurement_theta_min       1.77
_cell_measurement_theta_max       28.31

_exptl_crystal_description        Block
_exptl_crystal_colour             Colourless
_exptl_crystal_size_max           0.38
_exptl_crystal_size_mid           0.24
_exptl_crystal_size_min           0.24
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.451
_exptl_crystal_density_method     ?
_exptl_crystal_F_000              1264
_exptl_absorpt_coefficient_mu     0.846
_exptl_absorpt_correction_type    empirical
_exptl_absorpt_correction_T_min   0.739
_exptl_absorpt_correction_T_max   0.862

_exptl_special_details
;
 ?
;

_diffrn_ambient_temperature       160(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 CCD diffractometer'
_diffrn_measurement_method        '\w rotation with narrow frames'
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             16886
_diffrn_reflns_av_R_equivalents   0.0258
_diffrn_reflns_av_sigmaI/netI     0.0330
_diffrn_reflns_limit_h_min        -17
_diffrn_reflns_limit_h_max        18
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        10
_diffrn_reflns_limit_l_min        -20
_diffrn_reflns_limit_l_max        25
_diffrn_reflns_theta_min          1.77
_diffrn_reflns_theta_max          28.38
_reflns_number_total              6439
_reflns_number_observed           5463
_reflns_observed_criterion        >2sigma(I)

_computing_data_collection        'Siemens SMART'
_computing_cell_refinement        'local programs'
_computing_data_reduction         'Siemens SAINT'
_computing_structure_solution     'SHELXS-96 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-96 (Sheldrick, 1996)'
_computing_molecular_graphics     ?
_computing_publication_material   ?

_refine_special_details
;
 Refinement of F^2^ against ALL reflections.  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^)+(0.0242P)^2^+1.7283P] 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        0.00133(12)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_number_reflns          6439
_refine_ls_number_parameters      314
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0393
_refine_ls_R_factor_obs           0.0289
_refine_ls_wR_factor_all          0.0646
_refine_ls_wR_factor_obs          0.0607
_refine_ls_goodness_of_fit_all    1.042
_refine_ls_goodness_of_fit_obs    1.067
_refine_ls_restrained_S_all       1.042
_refine_ls_restrained_S_obs       1.067
_refine_ls_shift/esd_max          0.002
_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
Rh1 Rh -0.503546(11) 0.953357(16) 0.737426(8) 0.01917(6) Uani 1 d
. .
Cl1 Cl -0.53520(4) 0.79713(5) 0.82681(3) 0.02946(13) Uani 1 d . .
B1 B -0.39500(17) 0.9764(2) 0.67603(13) 0.0220(5) Uani 1 d . .
O1 O -0.31271(10) 1.05167(14) 0.68982(7) 0.0237(3) Uani 1 d . .
O2 O -0.38373(10) 0.90861(14) 0.61357(7) 0.0226(3) Uani 1 d . .
C1 C -0.25286(15) 1.0294(2) 0.63555(11) 0.0222(4) Uani 1 d . .
C2 C -0.29536(14) 0.94250(19) 0.58975(11) 0.0214(4) Uani 1 d . .
C3 C -0.25198(15) 0.9015(2) 0.53083(11) 0.0258(5) Uani 1 d . .
H3 H -0.2817 0.8415 0.4997 0.031 Uiso 1 calc R .
C4 C -0.16186(16) 0.9530(2) 0.51938(12) 0.0314(5) Uani 1 d . .
H4 H -0.1292 0.9282 0.4791 0.038 Uiso 1 calc R .
C5 C -0.11908(16) 1.0395(2) 0.56532(13) 0.0318(5) Uani 1 d . .
H5 H -0.0575 1.0723 0.5559 0.038 Uiso 1 calc R .
C6 C -0.16375(15) 1.0798(2) 0.62492(12) 0.0281(5) Uani 1 d . .
H6 H -0.1342 1.1390 0.6566 0.034 Uiso 1 calc R .
B2 B -0.54074(17) 1.1021(2) 0.67728(12) 0.0216(5) Uani 1 d . .
O3 O -0.50037(10) 1.16040(14) 0.61881(8) 0.0241(3) Uani 1 d . .
O4 O -0.62893(10) 1.16374(14) 0.68899(7) 0.0250(3) Uani 1 d . .
C7 C -0.56373(15) 1.2535(2) 0.59560(11) 0.0212(4) Uani 1 d . .
C8 C -0.64211(15) 1.2544(2) 0.63721(11) 0.0225(4) Uani 1 d . .
C9 C -0.71972(16) 1.3328(2) 0.62348(12) 0.0292(5) Uani 1 d . .
H9 H -0.7742 1.3318 0.6515 0.035 Uiso 1 calc R .
C10 C -0.71409(16) 1.4139(2) 0.56604(12) 0.0281(5) Uani 1 d . .
H10 H -0.7660 1.4700 0.5549 0.034 Uiso 1 calc R .
C11 C -0.63516(17) 1.4146(2) 0.52513(12) 0.0281(5) Uani 1 d . .
H11 H -0.6338 1.4713 0.4865 0.034 Uiso 1 calc R .
C12 C -0.55771(16) 1.3341(2) 0.53927(11) 0.0265(5) Uani 1 d . .
H12 H -0.5031 1.3345 0.5114 0.032 Uiso 1 calc R .
P1 P -0.59008(4) 0.81955(5) 0.66065(3) 0.02224(12) Uani 1 d . .
C13 C -0.60264(16) 0.8648(2) 0.56894(11) 0.0258(5) Uani 1 d . .
H13A H -0.6237 0.9551 0.5664 0.031 Uiso 1 calc R .
H13B H -0.5385 0.8604 0.5489 0.031 Uiso 1 calc R .
C14 C -0.67201(17) 0.7852(2) 0.52300(12) 0.0304(5) Uani 1 d . .
H14A H -0.6582 0.6941 0.5300 0.046 Uiso 1 calc R .
H14B H -0.6643 0.8074 0.4740 0.046 Uiso 1 calc R .
H14C H -0.7380 0.8030 0.5356 0.046 Uiso 1 calc R .
C15 C -0.71355(16) 0.7982(2) 0.68675(13) 0.0347(6) Uani 1 d . .
H15A H -0.7452 0.7350 0.6551 0.042 Uiso 1 calc R .
H15B H -0.7120 0.7614 0.7342 0.042 Uiso 1 calc R .
C16 C -0.77448(19) 0.9183(3) 0.68656(17) 0.0495(7) Uani 1 d . .
H16A H -0.7455 0.9807 0.7191 0.074 Uiso 1 calc R .
H16B H -0.8391 0.8969 0.7009 0.074 Uiso 1 calc R .
H16C H -0.7782 0.9548 0.6396 0.074 Uiso 1 calc R .
C17 C -0.55078(18) 0.6526(2) 0.66350(13) 0.0349(6) Uani 1 d . .
H17A H -0.5712 0.6147 0.7077 0.042 Uiso 1 calc R .
H17B H -0.5849 0.6062 0.6251 0.042 Uiso 1 calc R .
C18 C -0.44577(19) 0.6293(3) 0.65812(14) 0.0421(6) Uani 1 d . .
H18A H -0.4236 0.6689 0.6154 0.063 Uiso 1 calc R .
H18B H -0.4336 0.5371 0.6568 0.063 Uiso 1 calc R .
H18C H -0.4112 0.6668 0.6986 0.063 Uiso 1 calc R .
P2 P -0.43792(4) 1.07999(6) 0.82656(3) 0.02589(13) Uani 1 d . .
C19 C -0.35885(19) 0.9940(3) 0.88839(13) 0.0413(6) Uani 1 d . .
H19A H -0.3326 1.0550 0.9237 0.050 Uiso 1 calc R .
H19B H -0.3968 0.9293 0.9129 0.050 Uiso 1 calc R .
C20 C -0.27630(19) 0.9277(3) 0.85426(16) 0.0487(7) Uani 1 d . .
H20A H -0.2367 0.9915 0.8316 0.073 Uiso 1 calc R .
H20B H -0.3016 0.8668 0.8194 0.073 Uiso 1 calc R .
H20C H -0.2373 0.8819 0.8897 0.073 Uiso 1 calc R .
C21 C -0.54135(19) 1.1255(3) 0.87760(14) 0.0405(6) Uani 1 d . .
H21A H -0.5858 1.1762 0.8470 0.049 Uiso 1 calc R .
H21B H -0.5754 1.0463 0.8901 0.049 Uiso 1 calc R .
C22 C -0.5213(3) 1.2014(3) 0.94382(17) 0.0692(11) Uani 1 d . .
H22A H -0.4967 1.2861 0.9320 0.104 Uiso 1 calc R .
H22B H -0.4735 1.1563 0.9734 0.104 Uiso 1 calc R .
H22C H -0.5807 1.2109 0.9688 0.104 Uiso 1 calc R .
C23 C -0.37336(17) 1.2288(2) 0.81313(12) 0.0336(5) Uani 1 d . .
H23A H -0.3607 1.2698 0.8590 0.040 Uiso 1 calc R .
H23B H -0.3105 1.2078 0.7940 0.040 Uiso 1 calc R .
C24 C -0.4230(2) 1.3244(3) 0.76558(15) 0.0526(8) Uani 1 d . .
H24A H -0.4870 1.3424 0.7823 0.079 Uiso 1 calc R .
H24B H -0.4288 1.2893 0.7183 0.079 Uiso 1 calc R .
H24C H -0.3856 1.4036 0.7652 0.079 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
Rh1 0.01750(9) 0.02183(9) 0.01808(9) 0.00000(6) -0.00040(6)
0.00058(6)
Cl1 0.0276(3) 0.0336(3) 0.0272(3) 0.0082(2) 0.0014(2) 0.0006(2)
B1 0.0197(12) 0.0227(13) 0.0231(12) 0.0007(9) -0.0035(9)
0.0020(9)
O1 0.0201(7) 0.0267(8) 0.0244(8) -0.0038(6) 0.0006(6) -0.0017(6)
O2 0.0185(7) 0.0255(8) 0.0240(8) -0.0025(6) 0.0031(6) -0.0017(6)
C1 0.0205(10) 0.0227(11) 0.0233(11) 0.0021(8) -0.0007(8)
0.0009(8)
C2 0.0173(10) 0.0215(11) 0.0252(11) 0.0045(8) 0.0001(8) 0.0010(8)
C3 0.0260(11) 0.0279(12) 0.0235(11) -0.0003(9) 0.0001(9)
0.0050(9)
C4 0.0274(12) 0.0390(14) 0.0283(12) 0.0085(10) 0.0083(9)
0.0078(10)
C5 0.0206(11) 0.0379(14) 0.0373(13) 0.0122(11) 0.0039(9)
0.0007(10)
C6 0.0227(11) 0.0281(12) 0.0333(12) 0.0053(10) -0.0029(9)
-0.0039(9)
B2 0.0187(11) 0.0251(13) 0.0208(12) -0.0039(10) -0.0008(9)
0.0000(9)
O3 0.0213(7) 0.0250(8) 0.0261(8) 0.0022(6) 0.0033(6) 0.0031(6)
O4 0.0236(8) 0.0283(8) 0.0235(8) 0.0061(6) 0.0052(6) 0.0052(6)
C7 0.0216(10) 0.0204(11) 0.0213(10) -0.0020(8) -0.0008(8)
0.0012(8)
C8 0.0244(11) 0.0228(11) 0.0203(10) 0.0016(8) 0.0007(8) 0.0006(8)
C9 0.0249(11) 0.0327(13) 0.0303(12) 0.0018(10) 0.0048(9)
0.0063(9)
C10 0.0304(12) 0.0247(12) 0.0289(12) 0.0004(9) -0.0015(9)
0.0062(9)
C11 0.0384(13) 0.0219(11) 0.0237(11) 0.0018(9) 0.0007(9)
0.0019(9)
C12 0.0302(12) 0.0251(12) 0.0247(11) 0.0001(9) 0.0076(9)
0.0005(9)
P1 0.0219(3) 0.0217(3) 0.0228(3) -0.0003(2) -0.0023(2) -0.0008(2)
C13 0.0268(12) 0.0260(12) 0.0243(11) 0.0001(9) -0.0024(9)
-0.0005(9)
C14 0.0310(12) 0.0297(13) 0.0297(12) -0.0028(10) -0.0080(10)
-0.0009(10)
C15 0.0284(12) 0.0400(15) 0.0358(13) -0.0028(11) 0.0025(10)
-0.0123(10)
C16 0.0266(13) 0.0589(19) 0.0635(19) -0.0033(15) 0.0093(13)
-0.0016(12)
C17 0.0444(15) 0.0234(12) 0.0358(13) -0.0030(10) -0.0096(11)
0.0025(10)
C18 0.0530(17) 0.0323(14) 0.0412(15) 0.0037(12) 0.0031(12)
0.0114(12)
P2 0.0260(3) 0.0309(3) 0.0205(3) -0.0035(2) -0.0019(2) -0.0014(2)
C19 0.0395(15) 0.0525(17) 0.0307(13) 0.0043(12) -0.0146(11)
-0.0071(12)
C20 0.0319(14) 0.0507(18) 0.0624(19) 0.0122(14) -0.0125(13)
0.0029(12)
C21 0.0402(15) 0.0444(16) 0.0377(14) -0.0113(12) 0.0118(11)
-0.0052(12)
C22 0.078(2) 0.076(2) 0.056(2) -0.0369(18) 0.0313(18) -0.0253(19)
C23 0.0345(13) 0.0380(14) 0.0285(12) -0.0099(10) 0.0024(10)
-0.0134(11)
C24 0.068(2) 0.0355(16) 0.0526(18) 0.0016(13) -0.0161(15)
-0.0172(14)

_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 B1 1.973(2) . ?
Rh1 B2 1.994(2) . ?
Rh1 P2 2.3238(6) . ?
Rh1 P1 2.3345(6) . ?
Rh1 Cl1 2.4243(6) . ?
B1 O2 1.409(3) . ?
B1 O1 1.409(3) . ?
O1 C1 1.382(2) . ?
O2 C2 1.380(2) . ?
C1 C6 1.374(3) . ?
C1 C2 1.382(3) . ?
C2 C3 1.374(3) . ?
C3 C4 1.395(3) . ?
C4 C5 1.382(3) . ?
C5 C6 1.392(3) . ?
B2 O3 1.416(3) . ?
B2 O4 1.416(3) . ?
O3 C7 1.378(2) . ?
O4 C8 1.381(2) . ?
C7 C12 1.377(3) . ?
C7 C8 1.381(3) . ?
C8 C9 1.376(3) . ?
C9 C10 1.397(3) . ?
C10 C11 1.380(3) . ?
C11 C12 1.389(3) . ?
P1 C13 1.827(2) . ?
P1 C15 1.829(2) . ?
P1 C17 1.830(2) . ?
C13 C14 1.530(3) . ?
C15 C16 1.517(4) . ?
C17 C18 1.494(3) . ?
P2 C23 1.822(2) . ?
P2 C19 1.826(3) . ?
P2 C21 1.841(2) . ?
C19 C20 1.517(4) . ?
C21 C22 1.516(4) . ?
C23 C24 1.504(4) . ?

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
B1 Rh1 B2 75.29(10) . . ?
B1 Rh1 P2 94.69(7) . . ?
B2 Rh1 P2 93.92(7) . . ?
B1 Rh1 P1 94.91(7) . . ?
B2 Rh1 P1 89.16(7) . . ?
P2 Rh1 P1 170.37(2) . . ?
B1 Rh1 Cl1 132.29(7) . . ?
B2 Rh1 Cl1 152.34(7) . . ?
P2 Rh1 Cl1 86.53(2) . . ?
P1 Rh1 Cl1 86.52(2) . . ?
O2 B1 O1 108.84(18) . . ?
O2 B1 Rh1 124.28(16) . . ?
O1 B1 Rh1 126.60(16) . . ?
C1 O1 B1 106.11(16) . . ?
C2 O2 B1 106.61(16) . . ?
C6 C1 C2 121.7(2) . . ?
C6 C1 O1 128.8(2) . . ?
C2 C1 O1 109.52(17) . . ?
C3 C2 O2 128.6(2) . . ?
C3 C2 C1 122.5(2) . . ?
O2 C2 C1 108.90(18) . . ?
C2 C3 C4 116.1(2) . . ?
C5 C4 C3 121.4(2) . . ?
C4 C5 C6 121.8(2) . . ?
C1 C6 C5 116.4(2) . . ?
O3 B2 O4 107.86(18) . . ?
O3 B2 Rh1 133.91(16) . . ?
O4 B2 Rh1 118.08(16) . . ?
C7 O3 B2 106.88(16) . . ?
C8 O4 B2 106.81(16) . . ?
C12 C7 O3 128.90(19) . . ?
C12 C7 C8 121.77(19) . . ?
O3 C7 C8 109.30(17) . . ?
C9 C8 O4 128.90(19) . . ?
C9 C8 C7 121.9(2) . . ?
O4 C8 C7 109.11(18) . . ?
C8 C9 C10 116.4(2) . . ?
C11 C10 C9 121.7(2) . . ?
C10 C11 C12 121.2(2) . . ?
C7 C12 C11 116.9(2) . . ?
C13 P1 C15 104.00(11) . . ?
C13 P1 C17 107.05(11) . . ?
C15 P1 C17 99.21(12) . . ?
C13 P1 Rh1 118.77(7) . . ?
C15 P1 Rh1 111.67(8) . . ?
C17 P1 Rh1 113.95(8) . . ?
C14 C13 P1 116.69(16) . . ?
C16 C15 P1 115.65(18) . . ?
C18 C17 P1 116.59(18) . . ?
C23 P2 C19 102.92(12) . . ?
C23 P2 C21 104.94(12) . . ?
C19 P2 C21 104.32(13) . . ?
C23 P2 Rh1 124.39(8) . . ?
C19 P2 Rh1 114.13(9) . . ?
C21 P2 Rh1 104.24(9) . . ?
C20 C19 P2 113.18(18) . . ?
C22 C21 P2 117.4(2) . . ?
C24 C23 P2 115.78(18) . . ?

_refine_diff_density_max    0.560
_refine_diff_density_min   -0.658
_refine_diff_density_rms    0.067

#===END

data_13

_audit_creation_method            SHELXL
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_formula_moiety          ?
_chemical_formula_structural      ?
_chemical_formula_analytical      ?
_chemical_formula_sum             'C24 H38 B2 Cl Ir O4 P2'
_chemical_formula_weight          701.75
_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'
 'B'  'B'   0.0013   0.0007
 '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'
 'Ir'  'Ir'  -1.4442   7.9887
 '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                    13.970(2)
_cell_length_b                    10.5507(15)
_cell_length_c                    19.155(3)
_cell_angle_alpha                 90.00
_cell_angle_beta                  92.819(3)
_cell_angle_gamma                 90.00
_cell_volume                      2819.9(7)
_cell_formula_units_Z             4
_cell_measurement_temperature     160(2)
_cell_measurement_reflns_used     9423
_cell_measurement_theta_min       2.13
_cell_measurement_theta_max       28.38

_exptl_crystal_description        Block
_exptl_crystal_colour             'Pale yellow'
_exptl_crystal_size_max           0.50
_exptl_crystal_size_mid           0.44
_exptl_crystal_size_min           0.12
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.653
_exptl_crystal_density_method     ?
_exptl_crystal_F_000              1392
_exptl_absorpt_coefficient_mu     4.970
_exptl_absorpt_correction_type    empirical
_exptl_absorpt_correction_T_min   0.148
_exptl_absorpt_correction_T_max   0.408

_exptl_special_details
;
 ?
;

_diffrn_ambient_temperature       160(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 CCD diffractometer'
_diffrn_measurement_method        '\w rotation with narrow frames'
_diffrn_standards_number          0
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             17064
_diffrn_reflns_av_R_equivalents   0.0644
_diffrn_reflns_av_sigmaI/netI     0.0523
_diffrn_reflns_limit_h_min        -16
_diffrn_reflns_limit_h_max        17
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -24
_diffrn_reflns_limit_l_max        22
_diffrn_reflns_theta_min          1.76
_diffrn_reflns_theta_max          28.51
_reflns_number_total              6382
_reflns_number_observed           5081
_reflns_observed_criterion        >2sigma(I)

_computing_data_collection        'Siemens SMART'
_computing_cell_refinement        'local programs'
_computing_data_reduction         'Siemens SAINT'
_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^)+(0.0336P)^2^+11.7717P] 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        0.00012(8)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_number_reflns          6381
_refine_ls_number_parameters      314
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0568
_refine_ls_R_factor_obs           0.0381
_refine_ls_wR_factor_all          0.0982
_refine_ls_wR_factor_obs          0.0854
_refine_ls_goodness_of_fit_all    1.067
_refine_ls_goodness_of_fit_obs    1.048
_refine_ls_restrained_S_all       1.069
_refine_ls_restrained_S_obs       1.048
_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
Ir1 Ir -0.001808(14) 0.04625(2) 0.238732(11) 0.02746(8) Uani 1 d
. .
Cl1 Cl -0.03467(11) 0.1986(2) 0.32898(8) 0.0412(4) Uani 1 d . .
B1 B 0.1068(4) 0.0252(6) 0.1763(3) 0.0282(13) Uani 1 d . .
O1 O 0.1905(3) -0.0496(4) 0.1892(2) 0.0308(8) Uani 1 d . .
O2 O 0.1185(3) 0.0933(4) 0.1137(2) 0.0291(8) Uani 1 d . .
C1 C 0.2488(4) -0.0274(5) 0.1349(3) 0.0293(12) Uani 1 d . .
C2 C 0.2049(4) 0.0584(5) 0.0894(3) 0.0276(11) Uani 1 d . .
C3 C 0.2480(4) 0.1007(6) 0.0303(3) 0.0335(12) Uani 1 d . .
H3 H 0.2183(4) 0.1618(6) -0.0001(3) 0.040 Uiso 1 calc R .
C4 C 0.3385(4) 0.0482(7) 0.0175(3) 0.0413(15) Uani 1 d . .
H4 H 0.3702(4) 0.0728(7) -0.0231(3) 0.050 Uiso 1 calc R .
C5 C 0.3815(4) -0.0382(6) 0.0632(3) 0.0399(15) Uani 1 d . .
H5 H 0.4427(4) -0.0712(6) 0.0535(3) 0.048 Uiso 1 calc R .
C6 C 0.3375(4) -0.0780(6) 0.1229(3) 0.0387(14) Uani 1 d . .
H6 H 0.3672(4) -0.1377(6) 0.1541(3) 0.046 Uiso 1 calc R .
B2 B -0.0419(4) -0.1022(6) 0.1789(3) 0.0275(13) Uani 1 d . .
O3 O -0.1298(3) -0.1658(4) 0.1891(2) 0.0323(9) Uani 1 d . .
O4 O 0.0001(3) -0.1610(4) 0.1209(2) 0.0335(9) Uani 1 d . .
C7 C -0.1414(4) -0.2557(5) 0.1375(3) 0.0287(11) Uani 1 d . .
C8 C -0.0626(4) -0.2537(5) 0.0967(3) 0.0284(11) Uani 1 d . .
C9 C -0.0549(4) -0.3337(6) 0.0403(3) 0.0345(13) Uani 1 d . .
H9 H -0.0001(4) -0.3334(6) 0.0129(3) 0.041 Uiso 1 calc R .
C10 C -0.1321(4) -0.4152(6) 0.0256(3) 0.0358(13) Uani 1 d . .
H10 H -0.1302(4) -0.4715(6) -0.0131(3) 0.043 Uiso 1 calc R .
C11 C -0.2111(4) -0.4157(6) 0.0660(3) 0.0367(14) Uani 1 d . .
H11 H -0.2622(4) -0.4726(6) 0.0547(3) 0.044 Uiso 1 calc R .
C12 C -0.2177(4) -0.3355(6) 0.1225(3) 0.0386(14) Uani 1 d . .
H12 H -0.2725(4) -0.3353(6) 0.1499(3) 0.046 Uiso 1 calc R .
P1 P -0.08845(10) 0.18099(15) 0.16247(8) 0.0313(3) Uani 1 d . .
C13 C -0.2108(5) 0.2039(7) 0.1885(4) 0.046(2) Uani 1 d . .
H13A H -0.2086(5) 0.2407(7) 0.2361(4) 0.055 Uiso 1 calc R .
H13B H -0.2425(5) 0.2664(7) 0.1566(4) 0.055 Uiso 1 calc R .
C14 C -0.2720(5) 0.0849(9) 0.1886(5) 0.063(2) Uani 1 d . .
H14A H -0.3376(12) 0.1072(11) 0.1999(31) 0.094 Uiso 1 calc R .
H14B H -0.2452(25) 0.0254(25) 0.2236(22) 0.094 Uiso 1 calc R .
H14C H -0.2728(35) 0.0453(32) 0.1423(10) 0.094 Uiso 1 calc R .
C15 C -0.0490(5) 0.3474(6) 0.1650(4) 0.053(2) Uani 1 d . .
H15A H -0.0834(5) 0.3929(6) 0.1262(4) 0.063 Uiso 1 calc R .
H15B H -0.0694(5) 0.3853(6) 0.2091(4) 0.063 Uiso 1 calc R .
C16 C 0.0543(6) 0.3718(7) 0.1601(4) 0.059(2) Uani 1 d . .
H16A H 0.0654(7) 0.4634(8) 0.1577(30) 0.089 Uiso 1 calc R .
H16B H 0.0769(10) 0.3313(46) 0.1179(16) 0.089 Uiso 1 calc R .
H16C H 0.0892(7) 0.3369(47) 0.2014(15) 0.089 Uiso 1 calc R .
C17 C -0.1026(4) 0.1346(6) 0.0713(3) 0.0356(13) Uani 1 d . .
H17A H -0.0388(4) 0.1381(6) 0.0510(3) 0.043 Uiso 1 calc R .
H17B H -0.1240(4) 0.0452(6) 0.0694(3) 0.043 Uiso 1 calc R .
C18 C -0.1720(4) 0.2125(6) 0.0249(3) 0.0385(14) Uani 1 d . .
H18A H -0.1671(23) 0.1866(30) -0.0240(4) 0.058 Uiso 1 calc R .
H18B H -0.1561(20) 0.3026(7) 0.0296(18) 0.058 Uiso 1 calc R .
H18C H -0.2376(5) 0.1984(33) 0.0390(15) 0.058 Uiso 1 calc R .
P2 P 0.06556(13) -0.0793(2) 0.32761(8) 0.0427(4) Uani 1 d . .
C19 C 0.1428(6) 0.0088(10) 0.3899(4) 0.070(2) Uani 1 d . .
H19A H 0.1033(6) 0.0720(10) 0.4137(4) 0.084 Uiso 1 calc R .
H19B H 0.1692(6) -0.0507(10) 0.4259(4) 0.084 Uiso 1 calc R .
C20 C 0.2247(5) 0.0765(8) 0.3579(5) 0.062(2) Uani 1 d . .
H20A H 0.2628(25) 0.1212(46) 0.3945(7) 0.093 Uiso 1 calc R .
H20B H 0.1994(5) 0.1377(40) 0.3232(23) 0.093 Uiso 1 calc R .
H20C H 0.2652(24) 0.0147(10) 0.3351(26) 0.093 Uiso 1 calc R .
C21 C -0.0405(6) -0.1245(8) 0.3807(4) 0.064(2) Uani 1 d . .
H21A H -0.0738(6) -0.0459(8) 0.3939(4) 0.077 Uiso 1 calc R .
H21B H -0.0859(6) -0.1746(8) 0.3505(4) 0.077 Uiso 1 calc R .
C22 C -0.0166(8) -0.1986(11) 0.4455(5) 0.102(4) Uani 1 d . .
H22A H -0.0741(17) -0.2078(72) 0.4723(24) 0.152 Uiso 1 calc R .
H22B H 0.0331(45) -0.1541(42) 0.4738(22) 0.152 Uiso 1 calc R .
H22C H 0.0069(59) -0.2826(31) 0.4328(5) 0.152 Uiso 1 calc R .
C23 C 0.1268(5) -0.2262(8) 0.3120(4) 0.057(2) Uani 1 d . .
H23A H 0.1884(5) -0.2054(8) 0.2911(4) 0.068 Uiso 1 calc R .
H23B H 0.1425(5) -0.2662(8) 0.3579(4) 0.068 Uiso 1 calc R .
C24 C 0.0784(8) -0.3201(9) 0.2678(5) 0.089(3) Uani 1 d . .
H24A H 0.0178(27) -0.3440(53) 0.2879(21) 0.133 Uiso 1 calc R .
H24B H 0.1192(25) -0.3953(31) 0.2646(33) 0.133 Uiso 1 calc R .
H24C H 0.0655(49) -0.2847(27) 0.2210(12) 0.133 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
Ir1 0.02568(12) 0.03390(13) 0.02283(12) -0.00084(9) 0.00129(7)
-0.00462(9)
Cl1 0.0365(8) 0.0538(9) 0.0338(8) -0.0142(7) 0.0056(6) -0.0080(7)
B1 0.022(3) 0.036(4) 0.026(3) 0.002(3) 0.001(2) 0.000(2)
O1 0.024(2) 0.038(2) 0.030(2) 0.005(2) -0.0011(15) 0.001(2)
O2 0.022(2) 0.035(2) 0.030(2) 0.004(2) 0.0015(15) 0.002(2)
C1 0.021(3) 0.033(3) 0.034(3) -0.005(2) -0.003(2) -0.001(2)
C2 0.023(3) 0.031(3) 0.029(3) -0.004(2) 0.000(2) -0.002(2)
C3 0.033(3) 0.037(3) 0.030(3) -0.002(2) 0.000(2) -0.002(2)
C4 0.032(3) 0.057(4) 0.035(3) -0.014(3) 0.007(2) -0.013(3)
C5 0.021(3) 0.052(4) 0.047(4) -0.012(3) 0.005(2) 0.001(3)
C6 0.027(3) 0.039(3) 0.049(4) -0.009(3) -0.008(3) 0.000(2)
B2 0.026(3) 0.029(3) 0.027(3) 0.001(3) 0.002(2) -0.004(2)
O3 0.028(2) 0.040(2) 0.030(2) -0.007(2) 0.010(2) -0.010(2)
O4 0.029(2) 0.042(2) 0.030(2) -0.005(2) 0.007(2) -0.007(2)
C7 0.028(3) 0.032(3) 0.027(3) 0.000(2) 0.004(2) 0.001(2)
C8 0.030(3) 0.032(3) 0.023(3) 0.001(2) 0.001(2) -0.003(2)
C9 0.038(3) 0.036(3) 0.031(3) -0.002(2) 0.010(2) -0.001(2)
C10 0.044(3) 0.035(3) 0.029(3) -0.001(2) 0.004(2) -0.001(3)
C11 0.038(3) 0.031(3) 0.041(3) 0.000(3) -0.003(3) -0.009(2)
C12 0.032(3) 0.045(4) 0.039(3) -0.004(3) 0.009(2) -0.011(3)
P1 0.0283(7) 0.0340(8) 0.0314(8) -0.0030(6) -0.0007(6) -0.0012(6)
C13 0.042(4) 0.059(4) 0.038(4) -0.001(3) 0.006(3) 0.012(3)
C14 0.033(4) 0.079(6) 0.078(6) 0.006(5) 0.020(3) 0.005(4)
C15 0.064(5) 0.036(4) 0.055(4) 0.006(3) -0.019(4) -0.005(3)
C16 0.072(5) 0.046(4) 0.059(5) -0.001(4) -0.003(4) -0.022(4)
C17 0.031(3) 0.041(3) 0.034(3) 0.000(3) -0.003(2) 0.003(3)
C18 0.035(3) 0.041(4) 0.038(3) 0.001(3) -0.007(2) 0.000(3)
P2 0.0486(10) 0.0521(10) 0.0267(8) 0.0084(7) -0.0060(7)
-0.0083(8)
C19 0.069(6) 0.087(6) 0.051(5) -0.009(4) -0.023(4) 0.016(5)
C20 0.035(4) 0.065(5) 0.084(6) -0.010(4) -0.016(4) 0.002(3)
C21 0.073(5) 0.057(5) 0.062(5) 0.004(4) 0.008(4) 0.014(4)
C22 0.108(8) 0.117(9) 0.084(7) 0.053(7) 0.046(6) 0.035(7)
C23 0.050(4) 0.078(6) 0.043(4) 0.025(4) 0.011(3) 0.025(4)
C24 0.127(9) 0.065(6) 0.070(6) -0.001(5) -0.033(6) 0.044(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
Ir1 B1 1.991(6) . ?
Ir1 B2 2.004(6) . ?
Ir1 P2 2.320(2) . ?
Ir1 P1 2.334(2) . ?
Ir1 Cl1 2.421(2) . ?
B1 O2 1.414(7) . ?
B1 O1 1.422(7) . ?
O1 C1 1.373(7) . ?
O2 C2 1.365(6) . ?
C1 C2 1.379(8) . ?
C1 C6 1.379(8) . ?
C2 C3 1.381(8) . ?
C3 C4 1.413(9) . ?
C4 C5 1.380(9) . ?
C5 C6 1.390(9) . ?
B2 O3 1.421(7) . ?
B2 O4 1.424(8) . ?
O3 C7 1.374(7) . ?
O4 C8 1.378(6) . ?
C7 C12 1.377(8) . ?
C7 C8 1.380(8) . ?
C8 C9 1.381(8) . ?
C9 C10 1.397(8) . ?
C10 C11 1.378(9) . ?
C11 C12 1.381(9) . ?
P1 C17 1.816(6) . ?
P1 C13 1.820(7) . ?
P1 C15 1.840(7) . ?
C13 C14 1.519(11) . ?
C15 C16 1.472(10) . ?
C17 C18 1.523(8) . ?
P2 C23 1.803(8) . ?
P2 C19 1.824(8) . ?
P2 C21 1.898(9) . ?
C19 C20 1.505(12) . ?
C21 C22 1.490(12) . ?
C23 C24 1.449(12) . ?

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
B1 Ir1 B2 76.6(3) . . ?
B1 Ir1 P2 94.8(2) . . ?
B2 Ir1 P2 93.8(2) . . ?
B1 Ir1 P1 94.5(2) . . ?
B2 Ir1 P1 89.8(2) . . ?
P2 Ir1 P1 170.56(6) . . ?
B1 Ir1 Cl1 132.9(2) . . ?
B2 Ir1 Cl1 150.4(2) . . ?
P2 Ir1 Cl1 86.53(6) . . ?
P1 Ir1 Cl1 86.09(6) . . ?
O2 B1 O1 107.6(5) . . ?
O2 B1 Ir1 125.2(4) . . ?
O1 B1 Ir1 126.9(4) . . ?
C1 O1 B1 106.6(4) . . ?
C2 O2 B1 107.0(4) . . ?
O1 C1 C2 109.3(5) . . ?
O1 C1 C6 129.1(5) . . ?
C2 C1 C6 121.6(6) . . ?
O2 C2 C1 109.5(5) . . ?
O2 C2 C3 128.3(5) . . ?
C1 C2 C3 122.1(5) . . ?
C2 C3 C4 116.4(6) . . ?
C5 C4 C3 121.0(6) . . ?
C4 C5 C6 121.6(6) . . ?
C1 C6 C5 117.2(6) . . ?
O3 B2 O4 107.1(5) . . ?
O3 B2 Ir1 120.6(4) . . ?
O4 B2 Ir1 132.2(4) . . ?
C7 O3 B2 107.4(4) . . ?
C8 O4 B2 106.9(4) . . ?
O3 C7 C12 129.4(5) . . ?
O3 C7 C8 109.1(5) . . ?
C12 C7 C8 121.5(5) . . ?
O4 C8 C7 109.5(5) . . ?
O4 C8 C9 128.6(5) . . ?
C7 C8 C9 121.9(5) . . ?
C8 C9 C10 116.5(5) . . ?
C11 C10 C9 121.3(6) . . ?
C10 C11 C12 121.6(6) . . ?
C7 C12 C11 117.2(6) . . ?
C17 P1 C13 103.9(3) . . ?
C17 P1 C15 107.5(3) . . ?
C13 P1 C15 98.7(4) . . ?
C17 P1 Ir1 117.8(2) . . ?
C13 P1 Ir1 112.0(2) . . ?
C15 P1 Ir1 114.8(2) . . ?
C14 C13 P1 115.3(5) . . ?
C16 C15 P1 117.3(6) . . ?
C18 C17 P1 116.9(4) . . ?
C23 P2 C19 106.1(4) . . ?
C23 P2 C21 105.2(4) . . ?
C19 P2 C21 103.3(4) . . ?
C23 P2 Ir1 123.2(2) . . ?
C19 P2 Ir1 113.2(3) . . ?
C21 P2 Ir1 103.7(3) . . ?
C20 C19 P2 114.3(6) . . ?
C22 C21 P2 115.4(6) . . ?
C24 C23 P2 118.2(6) . . ?

_refine_diff_density_max    1.436
_refine_diff_density_min   -1.678
_refine_diff_density_rms    0.150

#===END