# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cb27ck
_database_code_depnum_ccdc_archive 'CCDC 1037662'
_audit_update_record             
;
2014-12-04 deposited with the CCDC.
2015-03-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C9 H26 P3 Rh)2'
_chemical_formula_sum            'C18 H52 P6 Rh2'
_chemical_formula_weight         660.23

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'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.6621(2)
_cell_length_b                   12.0824(2)
_cell_length_c                   13.1972(2)
_cell_angle_alpha                90
_cell_angle_beta                 108.536(2)
_cell_angle_gamma                90
_cell_volume                     1460.74(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    21745
_cell_measurement_theta_min      2.7870
_cell_measurement_theta_max      30.6700

_exptl_crystal_description       'fragment of rhombohedron'
_exptl_crystal_colour            'clear intense orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_F_000             680
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.27
_exptl_absorpt_coefficient_mu    1.462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.990
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET)
 (compiled Dec 19 2012,11:08:27)
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 The collected data cover nominally a full sphere of the reciprocal space.
 A combination of 19 sets of ω scans were used; each set at different \j,
 2θ or κ angles and each scan 0.7 deg in ω.
 Each frame was exposured for 10s. Nominal crystal to detector distance 45 mm.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction, Xcalibur, EOS'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 16.1419
_diffrn_reflns_number            46335
_diffrn_reflns_av_unetI/netI     0.0123
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.300
_diffrn_reflns_theta_max         28.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3890
_reflns_number_gt                3700
_reflns_threshold_expression     'I > 2σ(I)'

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET)
(compiled Dec 19 2012,11:08:27)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET)
(compiled Dec 19 2012,11:08:27)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET)
(compiled Dec 19 2012,11:08:27)
;
_computing_structure_solution    
;
 SIR-92 (A. Altomare, G. Cascarano, C. Giacovazzo and A. Guagliardi,
 J. Appl. Crystallogr. 1993, 26, 343-350.)
;
_computing_structure_refinement  
;
 SHELXL-2013 (G. M. Sheldrick, Acta Cryst. (2008). A64, 122-122)'
;
_computing_molecular_graphics    
;
 Diamond 3.2i, K. Brandenburg, Crystal Impact GbR, Bonn, Germany.
;
_computing_publication_material  
;
 WinGX v2013.2 (L. J. Farrugia, J. Appl. Cryst. 2012, 45, 849-854.)
;


_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0181P)²+1.8164P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3890
_refine_ls_number_parameters     126
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0214
_refine_ls_R_factor_gt           0.0200
_refine_ls_wR_factor_ref         0.0473
_refine_ls_wR_factor_gt          0.0466
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.82953(17) 0.06905(14) 0.52312(13) 0.0136(3) Uani 1 1 d . . . . .
H1A H 0.7415 0.0703 0.5461 0.016 Uiso 1 1 calc R U . . .
H1B H 0.8270 0.1342 0.4771 0.016 Uiso 1 1 calc R U . . .
C2 C 0.64322(18) -0.10043(16) 0.39329(14) 0.0206(3) Uani 1 1 d . . . . .
H2A H 0.5967 -0.1021 0.4493 0.031 Uiso 1 1 calc R U . . .
H2B H 0.6394 -0.1744 0.3621 0.031 Uiso 1 1 calc R U . . .
H2C H 0.5915 -0.0479 0.3375 0.031 Uiso 1 1 calc R U . . .
C3 C 0.88764(19) -0.16297(14) 0.55663(14) 0.0171(3) Uani 1 1 d . . . . .
H3A H 0.9907 -0.1538 0.5987 0.026 Uiso 1 1 calc R U . . .
H3B H 0.8727 -0.2366 0.5238 0.026 Uiso 1 1 calc R U . . .
H3C H 0.8272 -0.1551 0.6034 0.026 Uiso 1 1 calc R U . . .
C4 C 1.3069(2) -0.10606(16) 0.78983(15) 0.0223(4) Uani 1 1 d . . . . .
H4A H 1.3693 -0.1316 0.8600 0.033 Uiso 1 1 calc R U . . .
H4B H 1.3678 -0.0846 0.7462 0.033 Uiso 1 1 calc R U . . .
H4C H 1.2408 -0.1659 0.7541 0.033 Uiso 1 1 calc R U . . .
C5 C 1.1290(2) -0.04930(18) 0.90766(16) 0.0271(4) Uani 1 1 d . . . . .
H5A H 1.0582 -0.1071 0.8740 0.041 Uiso 1 1 calc R U . . .
H5B H 1.0813 0.0075 0.9379 0.041 Uiso 1 1 calc R U . . .
H5C H 1.2101 -0.0819 0.9647 0.041 Uiso 1 1 calc R U . . .
C6 C 1.3445(2) 0.10193(17) 0.89251(16) 0.0263(4) Uani 1 1 d . . . . .
H6A H 1.3010 0.1663 0.9159 0.039 Uiso 1 1 calc R U . . .
H6B H 1.4081 0.1269 0.8521 0.039 Uiso 1 1 calc R U . . .
H6C H 1.4020 0.0597 0.9551 0.039 Uiso 1 1 calc R U . . .
C7 C 0.97524(19) 0.22949(15) 0.87287(14) 0.0190(3) Uani 1 1 d . . . . .
H7A H 0.9012 0.2704 0.8940 0.029 Uiso 1 1 calc R U . . .
H7B H 1.0477 0.2814 0.8628 0.029 Uiso 1 1 calc R U . . .
H7C H 1.0236 0.1761 0.9289 0.029 Uiso 1 1 calc R U . . .
C8 C 0.74551(19) 0.07945(16) 0.78254(15) 0.0209(4) Uani 1 1 d . . . . .
H8A H 0.6864 0.1314 0.8084 0.031 Uiso 1 1 calc R U . . .
H8B H 0.7911 0.0256 0.8387 0.031 Uiso 1 1 calc R U . . .
H8C H 0.6830 0.0406 0.7193 0.031 Uiso 1 1 calc R U . . .
C9 C 0.7799(2) 0.27040(16) 0.67082(15) 0.0237(4) Uani 1 1 d . . . . .
H9A H 0.7123 0.2422 0.6037 0.035 Uiso 1 1 calc R U . . .
H9B H 0.8453 0.3250 0.6552 0.035 Uiso 1 1 calc R U . . .
H9C H 0.7243 0.3054 0.7127 0.035 Uiso 1 1 calc R U . . .
P1 P 0.83575(4) -0.05686(3) 0.45159(3) 0.01144(8) Uani 1 1 d . . . . .
P2 P 1.19929(4) 0.01380(4) 0.80704(3) 0.01328(8) Uani 1 1 d . . . . .
P3 P 0.88767(4) 0.15560(4) 0.74728(3) 0.01258(8) Uani 1 1 d . . . . .
Rh1 Rh 1.02456(2) 0.07142(2) 0.66032(2) 0.01047(4) Uani 1 1 d . . . . .


_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
C1 P1 1.8015(16) . ?
C1 Rh1 2.1589(16) . ?
C2 P1 1.8492(17) . ?
C3 P1 1.8370(17) . ?
C4 P2 1.8383(18) . ?
C5 P2 1.838(2) . ?
C6 P2 1.8354(19) . ?
C7 P3 1.8353(17) . ?
C8 P3 1.8320(18) . ?
C9 P3 1.8327(18) . ?
P1 Rh1 2.3025(4) 3_756 ?
P2 Rh1 2.2374(4) . ?
P3 Rh1 2.2507(4) . ?
Rh1 P1 2.3025(4) 3_756 ?

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
P1 C1 Rh1 106.56(7) . . ?
C1 P1 C3 103.92(8) . . ?
C1 P1 C2 105.17(8) . . ?
C3 P1 C2 96.45(8) . . ?
C1 P1 Rh1 121.65(6) . 3_756 ?
C3 P1 Rh1 110.84(6) . 3_756 ?
C2 P1 Rh1 115.38(6) . 3_756 ?
C6 P2 C5 100.51(10) . . ?
C6 P2 C4 100.44(9) . . ?
C5 P2 C4 96.64(9) . . ?
C6 P2 Rh1 124.78(7) . . ?
C5 P2 Rh1 113.82(7) . . ?
C4 P2 Rh1 116.04(6) . . ?
C8 P3 C9 100.32(9) . . ?
C8 P3 C7 100.52(8) . . ?
C9 P3 C7 98.47(9) . . ?
C8 P3 Rh1 120.81(6) . . ?
C9 P3 Rh1 112.61(6) . . ?
C7 P3 Rh1 120.23(6) . . ?
C1 Rh1 P2 159.88(5) . . ?
C1 Rh1 P3 86.33(4) . . ?
P2 Rh1 P3 95.934(15) . . ?
C1 Rh1 P1 89.68(4) . 3_756 ?
P2 Rh1 P1 95.532(15) . 3_756 ?
P3 Rh1 P1 157.061(16) . 3_756 ?

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
Rh1 C1 P1 C3 45.84(9) . . . . ?
Rh1 C1 P1 C2 146.62(8) . . . . ?
Rh1 C1 P1 Rh1 -79.84(8) . . . 3_756 ?

_refine_diff_density_max         2.283
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.072

_shelxl_version_number           2013-4

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cb33ck
_database_code_depnum_ccdc_archive 'CCDC 1037663'
_audit_update_record             
;
2014-12-04 deposited with the CCDC.
2015-03-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C17 H37 B N2 P3 Rh'
_chemical_formula_sum            'C17 H37 B N2 P3 Rh'
_chemical_formula_weight         476.11

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/n'
_space_group_name_Hall           '-P 2yac'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z-1/2'

_cell_length_a                   6.66500(10)
_cell_length_b                   13.9554(2)
_cell_length_c                   12.2545(2)
_cell_angle_alpha                90
_cell_angle_beta                 91.4030(10)
_cell_angle_gamma                90
_cell_volume                     1139.48(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    102(2)
_cell_measurement_reflns_used    39289
_cell_measurement_theta_min      3.31
_cell_measurement_theta_max      30.60

_exptl_crystal_description       'fragment of rhombohedral'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_F_000             496
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    0.963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.846
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
 (compiled Feb  1 2013,16:14:44)
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 The collected data cover nominally a full sphere of the reciprocal space.
 A combination of 37 sets of ω scans were used; each set at different \j,
 2θ or κ angles and each scan 0.8 deg in ω.
 Each frame was exposured for 10s. Nominal crystal to detector distance 45 mm.
;

_diffrn_ambient_temperature      102(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction, Xcalibur, EOS'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 16.1419
_diffrn_reflns_number            105629
_diffrn_reflns_av_unetI/netI     0.0119
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.212
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3327
_reflns_number_gt                3136
_reflns_threshold_expression     'I > 2σ(I)'

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
;

_computing_data_collection       
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
 (compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
 (compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
 (compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    
;
 SIR-92 (A. Altomare, G. Cascarano, C. Giacovazzo and A. Guagliardi,
 J. Appl. Crystallogr. 1993, 26, 343-350.)
;
_computing_structure_refinement  
;
 SHELXL-2013 (G. M. Sheldrick, Acta Cryst. (2008). A64, 122-122)'
;
_computing_molecular_graphics    
;
 Diamond 3.2i, K. Brandenburg, Crystal Impact GbR, Bonn, Germany.
;
_computing_publication_material  
;
 WinGX v2013.2 (L. J. Farrugia, J. Appl. Cryst. 2012, 45, 849-854.)
;

_refine_special_details          
;
 The ASU contains half a molecule of [(Me3P)3Rh-Bdmab] situated on a 
 two-fold rotation axis causing disorder of a Me3P moiety. During the 
 refinement similarity restraints on the P-C distances and the 
 C-P-C angles (SADI) were employed.

 All H atoms were placed in idealised positions and refined using a riding
 model, with a common U restrained to be 1.2 (1.5 for methyl groups) times 
 the equivalent isotropic displacement parameter of the parent atom.
 Methyl groups were treated as a rigid bodies and allowed to rotate about
 the E-CH3 bond.


 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0334P)²+1.4491P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3327
_refine_ls_number_parameters     131
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0277
_refine_ls_wR_factor_ref         0.0729
_refine_ls_wR_factor_gt          0.0714
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.100
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6591(3) -0.04308(12) 0.27822(14) 0.0163(3) Uani 1 1 d . . . . .
C2 C 0.5664(3) -0.12858(13) 0.30589(15) 0.0203(3) Uani 1 1 d . . . . .
H2 H 0.4434 -0.1288 0.3435 0.024 Uiso 1 1 calc R U . . .
C3 C 0.6596(3) -0.21442(13) 0.27678(15) 0.0228(4) Uani 1 1 d . . . . .
H3 H 0.5979 -0.2737 0.2940 0.027 Uiso 1 1 calc R U . . .
C4 C 0.4299(3) 0.07498(14) 0.35907(17) 0.0248(4) Uani 1 1 d . . . . .
H4A H 0.3164 0.0345 0.3362 0.037 Uiso 1 1 calc R U . . .
H4B H 0.3949 0.1425 0.3474 0.037 Uiso 1 1 calc R U . . .
H4C H 0.4612 0.0642 0.4367 0.037 Uiso 1 1 calc R U . . .
C5 C 0.7434(4) 0.29994(15) -0.03322(16) 0.0285(4) Uani 1 1 d . . . . .
H5A H 0.8774 0.2713 -0.0365 0.043 Uiso 1 1 calc R U . . .
H5B H 0.7561 0.3693 -0.0224 0.043 Uiso 1 1 calc R U . . .
H5C H 0.6692 0.2873 -0.1017 0.043 Uiso 1 1 calc R U . . .
C6 C 0.3583(3) 0.30031(15) 0.06185(18) 0.0286(4) Uani 1 1 d . . . . .
H6A H 0.3020 0.2815 -0.0096 0.043 Uiso 1 1 calc R U . . .
H6B H 0.3688 0.3703 0.0655 0.043 Uiso 1 1 calc R U . . .
H6C H 0.2705 0.2775 0.1194 0.043 Uiso 1 1 calc R U . . .
C7 C 0.5596(3) 0.12887(13) 0.02161(16) 0.0237(4) Uani 1 1 d . . . . .
H7A H 0.4752 0.0917 0.0704 0.036 Uiso 1 1 calc R U . . .
H7B H 0.6873 0.0954 0.0121 0.036 Uiso 1 1 calc R U . . .
H7C H 0.4906 0.1362 -0.0494 0.036 Uiso 1 1 calc R U . . .
C8 C 0.9900(5) 0.4697(3) 0.1953(4) 0.0537(15) Uani 0.5 1 d D . P . .
H8A H 1.0085 0.5384 0.2086 0.080 Uiso 0.5 1 calc R U P . .
H8B H 0.9906 0.4572 0.1166 0.080 Uiso 0.5 1 calc R U P . .
H8C H 1.0994 0.4339 0.2314 0.080 Uiso 0.5 1 calc R U P . .
C9 C 0.5905(7) 0.5073(3) 0.1630(3) 0.0378(11) Uani 0.5 1 d D . P . .
H9A H 0.4513 0.5028 0.1866 0.057 Uiso 0.5 1 calc R U P . .
H9B H 0.5984 0.4859 0.0871 0.057 Uiso 0.5 1 calc R U P . .
H9C H 0.6361 0.5739 0.1688 0.057 Uiso 0.5 1 calc R U P . .
C10 C 0.7555(6) 0.5087(3) 0.3700(3) 0.0355(10) Uani 0.5 1 d D . P . .
H10A H 0.7825 0.5748 0.3477 0.053 Uiso 0.5 1 calc R U P . .
H10B H 0.8615 0.4871 0.4211 0.053 Uiso 0.5 1 calc R U P . .
H10C H 0.6256 0.5058 0.4056 0.053 Uiso 0.5 1 calc R U P . .
B1 B 0.7500 0.11649(19) 0.2500 0.0166(5) Uani 1 2 d S T P . .
N1 N 0.6030(2) 0.05109(11) 0.29558(12) 0.0180(3) Uani 1 1 d . . . . .
P1 P 0.60782(8) 0.24736(3) 0.08102(4) 0.01874(10) Uani 1 1 d . . . . .
P2 P 0.7500 0.43131(5) 0.2500 0.02746(16) Uani 1 2 d DS T P . .
Rh1 Rh 0.7500 0.26511(2) 0.2500 0.01679(7) Uani 1 2 d S T P . .


_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
C1 N1 1.384(2) . ?
C1 C2 1.389(2) . ?
C1 C1 1.410(3) 2_655 ?
C2 C3 1.400(3) . ?
C3 C3 1.386(4) 2_655 ?
C4 N1 1.446(2) . ?
C5 P1 1.838(2) . ?
C6 P1 1.830(2) . ?
C7 P1 1.8318(19) . ?
C8 P2 1.829(3) . ?
C9 P2 1.826(3) . ?
C10 P2 1.824(3) . ?
B1 N1 1.460(2) 2_655 ?
B1 N1 1.460(2) . ?
B1 Rh1 2.074(3) . ?
P1 Rh1 2.2697(5) . ?
P2 C10 1.824(3) 2_655 ?
P2 C9 1.826(3) 2_655 ?
P2 C8 1.829(3) 2_655 ?
P2 Rh1 2.3194(7) . ?
Rh1 P1 2.2697(5) 2_655 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 130.90(16) . . ?
N1 C1 C1 108.29(9) . 2_655 ?
C2 C1 C1 120.81(10) . 2_655 ?
C1 C2 C3 118.05(17) . . ?
C3 C3 C2 121.13(11) 2_655 . ?
N1 B1 N1 102.6(2) 2_655 . ?
N1 B1 Rh1 128.69(10) 2_655 . ?
N1 B1 Rh1 128.69(10) . . ?
C1 N1 C4 121.56(15) . . ?
C1 N1 B1 110.40(15) . . ?
C4 N1 B1 127.83(15) . . ?
C6 P1 C7 99.42(10) . . ?
C6 P1 C5 101.74(11) . . ?
C7 P1 C5 98.19(9) . . ?
C6 P1 Rh1 115.52(7) . . ?
C7 P1 Rh1 121.76(7) . . ?
C5 P1 Rh1 116.69(7) . . ?
C10 P2 C10 107.4(3) . 2_655 ?
C10 P2 C9 35.49(18) . 2_655 ?
C10 P2 C9 97.28(13) 2_655 2_655 ?
C10 P2 C9 97.28(13) . . ?
C10 P2 C9 35.49(18) 2_655 . ?
C9 P2 C9 109.0(3) 2_655 . ?
C10 P2 C8 96.97(13) . . ?
C10 P2 C8 62.11(16) 2_655 . ?
C9 P2 C8 62.75(15) 2_655 . ?
C9 P2 C8 96.79(13) . . ?
C10 P2 C8 62.11(16) . 2_655 ?
C10 P2 C8 96.97(13) 2_655 2_655 ?
C9 P2 C8 96.79(13) 2_655 2_655 ?
C9 P2 C8 62.75(15) . 2_655 ?
C8 P2 C8 146.0(3) . 2_655 ?
C10 P2 Rh1 126.31(14) . . ?
C10 P2 Rh1 126.31(14) 2_655 . ?
C9 P2 Rh1 125.48(14) 2_655 . ?
C9 P2 Rh1 125.48(14) . . ?
C8 P2 Rh1 107.01(16) . . ?
C8 P2 Rh1 107.01(16) 2_655 . ?
B1 Rh1 P1 83.732(12) . . ?
B1 Rh1 P1 83.731(12) . 2_655 ?
P1 Rh1 P1 167.46(2) . 2_655 ?
B1 Rh1 P2 180.0 . . ?
P1 Rh1 P2 96.268(12) . . ?
P1 Rh1 P2 96.269(12) 2_655 . ?

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
N1 C1 C2 C3 179.73(18) . . . . ?
C1 C1 C2 C3 0.4(3) 2_655 . . . ?
C1 C2 C3 C3 0.9(3) . . . 2_655 ?
C2 C1 N1 C4 5.4(3) . . . . ?
C1 C1 N1 C4 -175.20(18) 2_655 . . . ?
C2 C1 N1 B1 -179.39(16) . . . . ?
C1 C1 N1 B1 0.0(2) 2_655 . . . ?
N1 B1 N1 C1 0.01(9) 2_655 . . . ?
Rh1 B1 N1 C1 -179.99(9) . . . . ?
N1 B1 N1 C4 174.8(2) 2_655 . . . ?
Rh1 B1 N1 C4 -5.2(2) . . . . ?

_refine_diff_density_max         1.322
_refine_diff_density_min         -1.120
_refine_diff_density_rms         0.084

_shelxl_version_number           2013-4

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cb37ck
_database_code_depnum_ccdc_archive 'CCDC 1037664'
_audit_update_record             
;
2014-12-04 deposited with the CCDC.
2015-03-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H48 B O2 P4 Rh'
_chemical_formula_sum            'C18 H48 B O2 P4 Rh'
_chemical_formula_weight         534.16

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'
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.2105(6)
_cell_length_b                   12.2896(12)
_cell_length_c                   12.3812(11)
_cell_angle_alpha                90.471(8)
_cell_angle_beta                 98.184(6)
_cell_angle_gamma                90.520(8)
_cell_volume                     1387.1(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    22157
_cell_measurement_theta_min      2.75
_cell_measurement_theta_max      30.57

_exptl_crystal_description       'fragment of rod'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_F_000             564
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_absorpt_coefficient_mu    0.856
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.958
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET)
 (compiled Dec 19 2012,11:08:27)
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 The collected data cover nominally a full sphere of the reciprocal space.
 A combination of 423 sets of ω scans were used; each set at different \j,
 2θ or κ angles and each scan 0.8 deg in ω.
 Each frame was exposured for 10s. Nominal crystal to detector distance 45 mm.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction, Xcalibur, EOS'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 16.1419
_diffrn_reflns_number            25564
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.234
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             25564
_reflns_number_gt                21727
_reflns_threshold_expression     'I > 2σ(I)'


_computing_data_collection       
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
 (compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
 (compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
 (compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    
;
 SIR-92 (A. Altomare, G. Cascarano, C. Giacovazzo and A. Guagliardi,
 J. Appl. Crystallogr. 1993, 26, 343-350.)
;
_computing_structure_refinement  
;
 SHELXL-2013 (G. M. Sheldrick, Acta Cryst. (2008). A64, 122-122)'
;
_computing_molecular_graphics    
;
 Diamond 3.2i, K. Brandenburg, Crystal Impact GbR, Bonn, Germany.
;
_computing_publication_material  
;
 WinGX v2013.2 (L. J. Farrugia, J. Appl. Cryst. 2012, 45, 849-854.)
;


_refine_special_details          
;
 The crystal is non-merohedrally twinned by 180 rotation about the 
 reciprocal [0 1 0] axis. The two components were indexed separately
 and integrated taking both components into account (HKLF5-file).
 The refinement was performed against these data of both components; the
 structure solution was performed on one data set containing only the data
 of the main component (Rint = 0.0801). The twin factor refined to 0.4123(7).
 

 All H atoms were placed in idealised positions and refined using a riding
 model, with a common U restrained to be 1.2 (1.5 for methyl groups) times
 the equivalent isotropic displacement parameter of the parent atom.
 Methyl groups were treated as a rigid bodies and allowed to rotate about
 the E-CH3 bond.

 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0557P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         25564
_refine_ls_number_parameters     252
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0380
_refine_ls_wR_factor_ref         0.0911
_refine_ls_wR_factor_gt          0.0878
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.006
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6825(3) 0.2100(3) 1.0447(2) 0.0157(6) Uani 1 1 d . . . . .
C2 C 0.5875(3) 0.3122(3) 1.0193(2) 0.0160(6) Uani 1 1 d . . . . .
C3 C 0.8346(3) 0.2375(3) 1.1082(2) 0.0214(7) Uani 1 1 d . . . . .
H3A H 0.8973 0.1734 1.1100 0.032 Uiso 1 1 calc R U . . .
H3B H 0.8242 0.2596 1.1829 0.032 Uiso 1 1 calc R U . . .
H3C H 0.8794 0.2973 1.0721 0.032 Uiso 1 1 calc R U . . .
C4 C 0.6107(4) 0.1183(3) 1.0996(3) 0.0234(7) Uani 1 1 d . . . . .
H4A H 0.5201 0.0953 1.0534 0.035 Uiso 1 1 calc R U . . .
H4B H 0.5877 0.1436 1.1704 0.035 Uiso 1 1 calc R U . . .
H4C H 0.6779 0.0567 1.1104 0.035 Uiso 1 1 calc R U . . .
C5 C 0.6273(4) 0.4069(3) 1.0986(2) 0.0212(7) Uani 1 1 d . . . . .
H5A H 0.7294 0.4291 1.0968 0.032 Uiso 1 1 calc R U . . .
H5B H 0.6155 0.3842 1.1726 0.032 Uiso 1 1 calc R U . . .
H5C H 0.5625 0.4682 1.0773 0.032 Uiso 1 1 calc R U . . .
C6 C 0.4226(3) 0.2881(3) 1.0096(3) 0.0245(7) Uani 1 1 d . . . . .
H6A H 0.3678 0.3524 0.9817 0.037 Uiso 1 1 calc R U . . .
H6B H 0.3973 0.2700 1.0816 0.037 Uiso 1 1 calc R U . . .
H6C H 0.3973 0.2266 0.9594 0.037 Uiso 1 1 calc R U . . .
C7 C 0.9594(3) 0.2585(3) 0.4873(2) 0.0217(7) Uani 1 1 d . . . . .
H7A H 0.9562 0.2692 0.4087 0.033 Uiso 1 1 calc R U . . .
H7B H 1.0106 0.1907 0.5085 0.033 Uiso 1 1 calc R U . . .
H7C H 1.0116 0.3198 0.5270 0.033 Uiso 1 1 calc R U . . .
C8 C 0.6913(4) 0.3636(3) 0.4384(3) 0.0242(8) Uani 1 1 d . . . . .
H8A H 0.7243 0.4326 0.4742 0.036 Uiso 1 1 calc R U . . .
H8B H 0.5841 0.3585 0.4306 0.036 Uiso 1 1 calc R U . . .
H8C H 0.7228 0.3603 0.3660 0.036 Uiso 1 1 calc R U . . .
C9 C 0.7058(3) 0.1364(3) 0.4272(3) 0.0228(7) Uani 1 1 d . . . . .
H9A H 0.5986 0.1313 0.4197 0.034 Uiso 1 1 calc R U . . .
H9B H 0.7484 0.0683 0.4568 0.034 Uiso 1 1 calc R U . . .
H9C H 0.7357 0.1493 0.3554 0.034 Uiso 1 1 calc R U . . .
C10 C 0.9633(4) 0.4830(3) 0.6654(3) 0.0224(7) Uani 1 1 d . . . . .
H10A H 0.9207 0.4892 0.5886 0.034 Uiso 1 1 calc R U . . .
H10B H 1.0516 0.4383 0.6711 0.034 Uiso 1 1 calc R U . . .
H10C H 0.9892 0.5557 0.6958 0.034 Uiso 1 1 calc R U . . .
C11 C 0.6997(4) 0.5313(3) 0.7376(3) 0.0325(8) Uani 1 1 d . . . . .
H11A H 0.6285 0.5168 0.7876 0.049 Uiso 1 1 calc R U . . .
H11B H 0.6481 0.5385 0.6632 0.049 Uiso 1 1 calc R U . . .
H11C H 0.7533 0.5990 0.7596 0.049 Uiso 1 1 calc R U . . .
C12 C 0.9328(4) 0.4468(3) 0.8768(3) 0.0338(9) Uani 1 1 d . . . . .
H12A H 0.9658 0.5229 0.8810 0.051 Uiso 1 1 calc R U . . .
H12B H 1.0182 0.3991 0.8885 0.051 Uiso 1 1 calc R U . . .
H12C H 0.8702 0.4332 0.9331 0.051 Uiso 1 1 calc R U . . .
C13 C 0.3823(3) 0.1870(3) 0.5305(3) 0.0253(8) Uani 1 1 d . . . . .
H13A H 0.2769 0.1823 0.5342 0.038 Uiso 1 1 calc R U . . .
H13B H 0.4168 0.1164 0.5077 0.038 Uiso 1 1 calc R U . . .
H13C H 0.4007 0.2425 0.4776 0.038 Uiso 1 1 calc R U . . .
C14 C 0.4033(3) 0.1138(3) 0.7398(3) 0.0218(7) Uani 1 1 d . . . . .
H14A H 0.4372 0.1217 0.8182 0.033 Uiso 1 1 calc R U . . .
H14B H 0.4351 0.0436 0.7139 0.033 Uiso 1 1 calc R U . . .
H14C H 0.2960 0.1173 0.7264 0.033 Uiso 1 1 calc R U . . .
C015 C 0.3651(3) 0.3361(3) 0.6972(3) 0.0245(7) Uani 1 1 d . . . . .
H01A H 0.2625 0.3115 0.6872 0.037 Uiso 1 1 calc R U . . .
H01B H 0.3762 0.3967 0.6480 0.037 Uiso 1 1 calc R U . . .
H01C H 0.3941 0.3602 0.7729 0.037 Uiso 1 1 calc R U . . .
C16 C 0.7671(4) -0.0245(3) 0.7955(3) 0.0258(7) Uani 1 1 d . . . . .
H16A H 0.6971 -0.0518 0.7340 0.039 Uiso 1 1 calc R U . . .
H16B H 0.7144 -0.0047 0.8561 0.039 Uiso 1 1 calc R U . . .
H16C H 0.8385 -0.0812 0.8191 0.039 Uiso 1 1 calc R U . . .
C17 C 1.0132(3) 0.1117(3) 0.8676(2) 0.0236(7) Uani 1 1 d . . . . .
H17A H 0.9740 0.1402 0.9315 0.035 Uiso 1 1 calc R U . . .
H17B H 1.0872 0.1624 0.8473 0.035 Uiso 1 1 calc R U . . .
H17C H 1.0582 0.0408 0.8849 0.035 Uiso 1 1 calc R U . . .
C18 C 0.9680(4) 0.0242(3) 0.6586(3) 0.0238(8) Uani 1 1 d . . . . .
H18A H 1.0150 -0.0396 0.6948 0.036 Uiso 1 1 calc R U . . .
H18B H 1.0434 0.0732 0.6373 0.036 Uiso 1 1 calc R U . . .
H18C H 0.9015 0.0009 0.5934 0.036 Uiso 1 1 calc R U . . .
B1 B 0.6828(3) 0.2543(3) 0.8633(2) 0.0107(5) Uani 1 1 d . . . . .
P1 P 0.77130(7) 0.25060(8) 0.52067(5) 0.01364(14) Uani 1 1 d . . . . .
P2 P 0.82877(8) 0.41893(7) 0.74216(6) 0.01481(16) Uani 1 1 d . . . . .
P3 P 0.48146(7) 0.22433(6) 0.66642(6) 0.01452(17) Uani 1 1 d . . . . .
P4 P 0.86324(8) 0.09594(7) 0.75293(6) 0.01426(16) Uani 1 1 d . . . . .
Rh1 Rh 0.72964(2) 0.24843(2) 0.70190(2) 0.00963(6) Uani 1 1 d . . . . .
O1 O 0.7057(2) 0.17164(19) 0.93747(15) 0.0164(4) Uani 1 1 d . . . . .
O2 O 0.6197(2) 0.34210(18) 0.91205(15) 0.0150(4) Uani 1 1 d . . . . .


_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
C1 O1 1.449(3) . ?
C1 C4 1.516(5) . ?
C1 C3 1.539(4) . ?
C1 C2 1.546(4) . ?
C2 O2 1.451(3) . ?
C2 C5 1.524(4) . ?
C2 C6 1.532(4) . ?
C7 P1 1.839(3) . ?
C8 P1 1.827(3) . ?
C9 P1 1.853(3) . ?
C10 P2 1.840(4) . ?
C11 P2 1.827(4) . ?
C12 P2 1.829(3) . ?
C13 P3 1.849(3) . ?
C14 P3 1.838(4) . ?
C015 P3 1.820(3) . ?
C16 P4 1.837(4) . ?
C17 P4 1.842(3) . ?
C18 P4 1.842(3) . ?
B1 O1 1.372(4) . ?
B1 O2 1.403(4) . ?
B1 Rh1 2.104(3) . ?
P1 Rh1 2.3299(7) . ?
P2 Rh1 2.3002(9) . ?
P3 Rh1 2.2816(7) . ?
P4 Rh1 2.2946(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C4 107.7(3) . . ?
O1 C1 C3 107.0(2) . . ?
C4 C1 C3 110.4(2) . . ?
O1 C1 C2 103.2(2) . . ?
C4 C1 C2 115.4(3) . . ?
C3 C1 C2 112.4(3) . . ?
O2 C2 C5 109.4(3) . . ?
O2 C2 C6 107.8(2) . . ?
C5 C2 C6 109.5(3) . . ?
O2 C2 C1 102.4(2) . . ?
C5 C2 C1 114.3(2) . . ?
C6 C2 C1 113.1(3) . . ?
O1 B1 O2 108.7(2) . . ?
O1 B1 Rh1 125.6(2) . . ?
O2 B1 Rh1 125.7(2) . . ?
C8 P1 C7 99.04(17) . . ?
C8 P1 C9 99.06(15) . . ?
C7 P1 C9 97.33(16) . . ?
C8 P1 Rh1 116.26(12) . . ?
C7 P1 Rh1 120.44(9) . . ?
C9 P1 Rh1 120.31(12) . . ?
C11 P2 C12 98.6(2) . . ?
C11 P2 C10 98.18(18) . . ?
C12 P2 C10 95.29(16) . . ?
C11 P2 Rh1 116.56(13) . . ?
C12 P2 Rh1 119.75(13) . . ?
C10 P2 Rh1 123.33(12) . . ?
C015 P3 C14 100.00(17) . . ?
C015 P3 C13 98.06(15) . . ?
C14 P3 C13 95.62(16) . . ?
C015 P3 Rh1 118.21(11) . . ?
C14 P3 Rh1 116.43(10) . . ?
C13 P3 Rh1 123.69(11) . . ?
C16 P4 C17 101.08(16) . . ?
C16 P4 C18 96.62(18) . . ?
C17 P4 C18 97.44(15) . . ?
C16 P4 Rh1 118.66(11) . . ?
C17 P4 Rh1 116.76(12) . . ?
C18 P4 Rh1 121.88(11) . . ?
B1 Rh1 P3 81.42(7) . . ?
B1 Rh1 P4 86.34(10) . . ?
P3 Rh1 P4 115.98(3) . . ?
B1 Rh1 P2 84.11(11) . . ?
P3 Rh1 P2 120.36(3) . . ?
P4 Rh1 P2 120.37(3) . . ?
B1 Rh1 P1 176.48(9) . . ?
P3 Rh1 P1 96.58(2) . . ?
P4 Rh1 P1 97.15(3) . . ?
P2 Rh1 P1 94.46(3) . . ?
B1 O1 C1 110.2(2) . . ?
B1 O2 C2 110.2(2) . . ?

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
O1 C1 C2 O2 -22.3(3) . . . . ?
C4 C1 C2 O2 -139.5(2) . . . . ?
C3 C1 C2 O2 92.7(3) . . . . ?
O1 C1 C2 C5 -140.4(3) . . . . ?
C4 C1 C2 C5 102.4(3) . . . . ?
C3 C1 C2 C5 -25.4(4) . . . . ?
O1 C1 C2 C6 93.4(3) . . . . ?
C4 C1 C2 C6 -23.8(4) . . . . ?
C3 C1 C2 C6 -151.6(2) . . . . ?
O2 B1 O1 C1 -10.4(3) . . . . ?
Rh1 B1 O1 C1 171.08(19) . . . . ?
C4 C1 O1 B1 143.1(2) . . . . ?
C3 C1 O1 B1 -98.2(3) . . . . ?
C2 C1 O1 B1 20.6(3) . . . . ?
O1 B1 O2 C2 -5.4(3) . . . . ?
Rh1 B1 O2 C2 173.11(18) . . . . ?
C5 C2 O2 B1 139.0(2) . . . . ?
C6 C2 O2 B1 -102.0(3) . . . . ?
C1 C2 O2 B1 17.4(3) . . . . ?

_refine_diff_density_max         1.539
_refine_diff_density_min         -2.467
_refine_diff_density_rms         0.112

_shelxl_version_number           2013-4

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cb38ck
_database_code_depnum_ccdc_archive 'CCDC 1037665'
_audit_update_record             
;
2014-12-04 deposited with the CCDC.
2015-03-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H45 B N2 P3 Rh, C7 H8, 1/2 (C5 H12)'
_chemical_formula_sum            'C38.50 H59 B N2 P3 Rh'
_chemical_formula_weight         756.50

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.91850(10)
_cell_length_b                   11.7946(2)
_cell_length_c                   18.9805(2)
_cell_angle_alpha                72.3240(10)
_cell_angle_beta                 80.4470(10)
_cell_angle_gamma                67.9810(10)
_cell_volume                     1957.87(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    57983
_cell_measurement_theta_min      2.80
_cell_measurement_theta_max      29.55

_exptl_crystal_description       'fragment of prism'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_F_000             798
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.27
_exptl_absorpt_coefficient_mu    0.587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.977
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
 (compiled Feb  1 2013,16:14:44)
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 The collected data cover nominally a full sphere of the reciprocal space.
 A combination of 48 sets of ω scans were used; each set at different \j,
 2θ or κ angles and each scan 0.8 deg in ω.
 Each frame was exposured for 10s. Nominal crystal to detector distance 45 mm.
;



_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction, Xcalibur, EOS'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 16.1419
_diffrn_reflns_number            249085
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.219
_diffrn_reflns_theta_max         30.857
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             11747
_reflns_number_gt                10306
_reflns_threshold_expression     'I > 2σ(I)'


_computing_data_collection       
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
 (compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
 (compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
 (compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    
;
 SIR-92 (A. Altomare, G. Cascarano, C. Giacovazzo and A. Guagliardi,
 J. Appl. Crystallogr. 1993, 26, 343-350.)
;
_computing_structure_refinement  
;
 SHELXL-2014/7 (G. M. Sheldrick, Acta Cryst. (2008). A64, 112-122)'
;
_computing_molecular_graphics    
;
 Diamond 3.2i, K. Brandenburg, Crystal Impact GbR, Bonn, Germany.
;
_computing_publication_material  
;
 WinGX v2014.1 (L. J. Farrugia, J. Appl. Cryst. 2012, 45, 849-854.)
;


_refine_special_details          
;
 The structure contains one molecule of n-pentane and two molecules of 
 toluene in the ASU.

   1) The n-pentane molecule is disordered on an inversion centre; 
      all C-C distances were restraint to 1.54 Ang (DFIX). 
      The SOF refined to ca. 1/2 and was fixed to 1/2.

   2) The disordered PhMe molecule was refined employing geometrical restraints:
      - the phenyl moiety was refined as regular hexagon (AFIX 66)
      - the H3C-C(ipso) distance was restraint to 1.54 Ang (DFIX).
      - the two H3C-C(ortho) distance were restraint to equivalence (SADI).
      - all ADP were restraint to approximate isotropic behaviour (ISOR).



 All H atoms were placed in idealised positions and refined using a riding
 model, with a common U restrained to be 1.2 (1.5 for methyl groups) times
 the equivalent isotropic displacement parameter of the parent atom.
 Methyl groups, besides those of solvent molecules, were treated as a rigid
 bodies and allowed to rotate about the E-CH3 bond.



 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0361P)²+2.7091P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11747
_refine_ls_number_parameters     482
_refine_ls_number_restraints     92
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0423
_refine_ls_wR_factor_ref         0.1040
_refine_ls_wR_factor_gt          0.0979
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_restrained_S_all      1.153
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2755(2) 0.15981(19) 0.67928(12) 0.0218(4) Uani 1 1 d . . . . .
C2 C 0.2062(2) 0.1396(2) 0.62895(14) 0.0272(4) Uani 1 1 d . . . . .
H2 H 0.1996 0.1898 0.5791 0.033 Uiso 1 1 calc R U . . .
C3 C 0.1464(3) 0.0431(2) 0.65374(16) 0.0332(5) Uani 1 1 d . . . . .
H3 H 0.0976 0.0282 0.6202 0.040 Uiso 1 1 calc R U . . .
C4 C 0.1569(3) -0.0310(2) 0.72598(16) 0.0346(5) Uani 1 1 d . . . . .
H4 H 0.1158 -0.0962 0.7411 0.042 Uiso 1 1 calc R U . . .
C5 C 0.2267(3) -0.0118(2) 0.77716(15) 0.0299(5) Uani 1 1 d . . . . .
H5 H 0.2345 -0.0633 0.8267 0.036 Uiso 1 1 calc R U . . .
C6 C 0.2844(2) 0.0851(2) 0.75322(12) 0.0231(4) Uani 1 1 d . . . . .
C7 C 0.3388(3) 0.3462(2) 0.60307(12) 0.0264(4) Uani 1 1 d . . . . .
H7A H 0.3694 0.4107 0.6128 0.032 Uiso 1 1 calc R U . . .
H7B H 0.2370 0.3884 0.5883 0.032 Uiso 1 1 calc R U . . .
C8 C 0.4337(2) 0.3027(2) 0.53801(12) 0.0242(4) Uani 1 1 d . . . . .
C9 C 0.4474(3) 0.3941(2) 0.47296(13) 0.0262(4) Uani 1 1 d . . . . .
H9 H 0.3985 0.4814 0.4708 0.031 Uiso 1 1 calc R U . . .
C10 C 0.5309(3) 0.3600(2) 0.41150(13) 0.0296(5) Uani 1 1 d . . . . .
H10 H 0.5392 0.4236 0.3678 0.036 Uiso 1 1 calc R U . . .
C11 C 0.6025(3) 0.2324(2) 0.41399(14) 0.0318(5) Uani 1 1 d . . . . .
H11 H 0.6596 0.2085 0.3720 0.038 Uiso 1 1 calc R U . . .
C12 C 0.5901(3) 0.1408(2) 0.47798(14) 0.0315(5) Uani 1 1 d . . . . .
H12 H 0.6387 0.0537 0.4799 0.038 Uiso 1 1 calc R U . . .
C13 C 0.5066(3) 0.1758(2) 0.53970(13) 0.0282(4) Uani 1 1 d . . . . .
H13 H 0.4994 0.1120 0.5835 0.034 Uiso 1 1 calc R U . . .
C14 C 0.3669(3) 0.0794(2) 0.87070(12) 0.0279(4) Uani 1 1 d . . . . .
H14A H 0.2717 0.0757 0.8950 0.033 Uiso 1 1 calc R U . . .
H14B H 0.3915 0.1387 0.8893 0.033 Uiso 1 1 calc R U . . .
C15 C 0.4810(2) -0.0511(2) 0.89413(12) 0.0238(4) Uani 1 1 d . . . . .
C16 C 0.5878(3) -0.1038(2) 0.84456(13) 0.0286(4) Uani 1 1 d . . . . .
H16 H 0.5857 -0.0603 0.7934 0.034 Uiso 1 1 calc R U . . .
C17 C 0.6981(3) -0.2198(2) 0.86884(14) 0.0310(5) Uani 1 1 d . . . . .
H17 H 0.7716 -0.2539 0.8344 0.037 Uiso 1 1 calc R U . . .
C18 C 0.7010(3) -0.2853(2) 0.94290(14) 0.0294(5) Uani 1 1 d . . . . .
H18 H 0.7764 -0.3643 0.9594 0.035 Uiso 1 1 calc R U . . .
C19 C 0.5934(3) -0.2353(2) 0.99307(13) 0.0280(4) Uani 1 1 d . . . . .
H19 H 0.5942 -0.2804 1.0439 0.034 Uiso 1 1 calc R U . . .
C20 C 0.4843(2) -0.1189(2) 0.96862(12) 0.0254(4) Uani 1 1 d . . . . .
H20 H 0.4108 -0.0851 1.0032 0.031 Uiso 1 1 calc R U . . .
C21 C 0.1088(3) 0.4664(3) 0.88203(14) 0.0371(5) Uani 1 1 d . . . . .
H21A H 0.1505 0.5054 0.9076 0.056 Uiso 1 1 calc R U . . .
H21B H 0.1230 0.3786 0.9105 0.056 Uiso 1 1 calc R U . . .
H21C H 0.0044 0.5142 0.8775 0.056 Uiso 1 1 calc R U . . .
C22 C 0.1407(3) 0.6382(2) 0.74434(17) 0.0412(6) Uani 1 1 d . . . . .
H22A H 0.0354 0.6765 0.7538 0.062 Uiso 1 1 calc R U . . .
H22B H 0.1635 0.6513 0.6909 0.062 Uiso 1 1 calc R U . . .
H22C H 0.1916 0.6780 0.7640 0.062 Uiso 1 1 calc R U . . .
C23 C 0.0704(3) 0.4284(3) 0.75171(17) 0.0376(6) Uani 1 1 d . . . . .
H23A H -0.0290 0.4843 0.7607 0.056 Uiso 1 1 calc R U . . .
H23B H 0.0788 0.3400 0.7757 0.056 Uiso 1 1 calc R U . . .
H23C H 0.0923 0.4395 0.6983 0.056 Uiso 1 1 calc R U . . .
C24 C 0.3893(4) 0.5788(3) 0.89639(17) 0.0437(7) Uani 1 1 d . . . . .
H24A H 0.4362 0.6291 0.9092 0.066 Uiso 1 1 calc R U . . .
H24B H 0.3681 0.5188 0.9414 0.066 Uiso 1 1 calc R U . . .
H24C H 0.2983 0.6354 0.8729 0.066 Uiso 1 1 calc R U . . .
C25 C 0.6706(3) 0.4141(3) 0.88890(16) 0.0401(6) Uani 1 1 d . . . . .
H25A H 0.7568 0.3762 0.8589 0.060 Uiso 1 1 calc R U . . .
H25B H 0.6531 0.3477 0.9311 0.060 Uiso 1 1 calc R U . . .
H25C H 0.6869 0.4772 0.9070 0.060 Uiso 1 1 calc R U . . .
C26 C 0.5599(4) 0.6221(3) 0.76749(16) 0.0518(8) Uani 1 1 d . . . . .
H26A H 0.5961 0.6623 0.7948 0.078 Uiso 1 1 calc R U . . .
H26B H 0.4738 0.6846 0.7417 0.078 Uiso 1 1 calc R U . . .
H26C H 0.6360 0.5896 0.7312 0.078 Uiso 1 1 calc R U . . .
C27 C 0.7780(3) 0.1274(3) 0.82511(18) 0.0460(7) Uani 1 1 d . . . . .
H27A H 0.8773 0.0870 0.8062 0.069 Uiso 1 1 calc R U . . .
H27B H 0.7309 0.0637 0.8459 0.069 Uiso 1 1 calc R U . . .
H27C H 0.7815 0.1653 0.8638 0.069 Uiso 1 1 calc R U . . .
C28 C 0.7084(3) 0.1581(3) 0.68265(18) 0.0458(7) Uani 1 1 d . . . . .
H28A H 0.8134 0.1135 0.6766 0.069 Uiso 1 1 calc R U . . .
H28B H 0.6720 0.2149 0.6348 0.069 Uiso 1 1 calc R U . . .
H28C H 0.6583 0.0963 0.7006 0.069 Uiso 1 1 calc R U . . .
C29 C 0.7998(3) 0.3366(4) 0.70593(18) 0.0496(8) Uani 1 1 d . . . . .
H29A H 0.8131 0.3784 0.7403 0.074 Uiso 1 1 calc R U . . .
H29B H 0.7596 0.4005 0.6607 0.074 Uiso 1 1 calc R U . . .
H29C H 0.8940 0.2767 0.6935 0.074 Uiso 1 1 calc R U . . .
B1 B 0.3822(2) 0.2423(2) 0.74345(13) 0.0189(4) Uani 1 1 d . . . . .
N1 N 0.34132(19) 0.24889(16) 0.67159(10) 0.0212(3) Uani 1 1 d . . . . .
N2 N 0.3512(2) 0.13061(17) 0.79180(10) 0.0227(3) Uani 1 1 d . . . . .
P1 P 0.19933(6) 0.46844(5) 0.78974(3) 0.02343(11) Uani 1 1 d . . . . .
P2 P 0.51137(8) 0.49132(6) 0.83208(3) 0.03073(13) Uani 1 1 d . . . . .
P3 P 0.67398(7) 0.25084(7) 0.74950(4) 0.03269(14) Uani 1 1 d . . . . .
Rh1 Rh 0.44293(2) 0.36533(2) 0.78027(2) 0.02326(5) Uani 1 1 d . . . . .
C30 C -0.0534(8) 0.2251(7) 0.0493(4) 0.0532(17) Uani 0.5 1 d D . P A 3
H30A H -0.0119 0.2926 0.0380 0.080 Uiso 0.5 1 calc R U P A 3
H30B H -0.1558 0.2622 0.0370 0.080 Uiso 0.5 1 calc R U P A 3
H30C H -0.0467 0.1810 0.1021 0.080 Uiso 0.5 1 calc R U P A 3
C31 C 0.0317(7) 0.1305(6) 0.0034(4) 0.0519(17) Uani 0.5 1 d D . P A 3
H31A H 0.1354 0.0955 0.0152 0.062 Uiso 0.5 1 calc R U P A 3
H31B H 0.0265 0.1765 -0.0498 0.062 Uiso 0.5 1 calc R U P A 3
C32 C -0.0240(6) 0.0201(5) 0.0167(3) 0.046(2) Uani 0.5 1 d D . P A 3
H32A H -0.1264 0.0558 0.0026 0.056 Uiso 0.5 1 calc R U P A 3
H32B H -0.0243 -0.0220 0.0704 0.056 Uiso 0.5 1 calc R U P A 3
C33 C 0.0612(9) -0.0817(7) -0.0246(6) 0.069(3) Uani 0.5 1 d D . P A 3
H33A H 0.0663 -0.0382 -0.0780 0.083 Uiso 0.5 1 calc R U P A 3
H33B H 0.1622 -0.1198 -0.0084 0.083 Uiso 0.5 1 calc R U P A 3
C34 C 0.0057(11) -0.1906(9) -0.0166(7) 0.076(3) Uani 0.5 1 d D . P A 3
H34A H 0.0709 -0.2475 -0.0459 0.114 Uiso 0.5 1 calc R U P A 3
H34B H 0.0036 -0.2379 0.0356 0.114 Uiso 0.5 1 calc R U P A 3
H34C H -0.0927 -0.1559 -0.0343 0.114 Uiso 0.5 1 calc R U P A 3
C35 C 0.0039(5) 0.2487(4) 0.4545(3) 0.054(2) Uani 0.438(5) 1 d DG U P B 1
C36 C 0.0329(6) 0.1400(5) 0.4316(4) 0.059(2) Uani 0.438(5) 1 d DG U P B 1
H36 H -0.0333 0.0950 0.4456 0.071 Uiso 0.438(5) 1 calc R U P B 1
C37 C 0.1589(7) 0.0973(6) 0.3882(4) 0.118(5) Uani 0.438(5) 1 d G U P B 1
H37 H 0.1787 0.0231 0.3726 0.142 Uiso 0.438(5) 1 calc R U P B 1
C38 C 0.2558(6) 0.1632(7) 0.3676(4) 0.053(2) Uani 0.438(5) 1 d G U P B 1
H38 H 0.3419 0.1340 0.3380 0.064 Uiso 0.438(5) 1 calc R U P B 1
C39 C 0.2268(5) 0.2718(6) 0.3905(3) 0.072(3) Uani 0.438(5) 1 d G U P B 1
H39 H 0.2930 0.3169 0.3765 0.087 Uiso 0.438(5) 1 calc R U P B 1
C40 C 0.1008(5) 0.3146(4) 0.4339(3) 0.0394(16) Uani 0.438(5) 1 d DG U P B 1
H40 H 0.0809 0.3888 0.4495 0.047 Uiso 0.438(5) 1 calc R U P B 1
C41 C -0.1330(7) 0.2938(7) 0.5042(4) 0.057(2) Uani 0.438(5) 1 d D U P B 1
H41A H -0.1368 0.3711 0.5150 0.086 Uiso 0.438(5) 1 calc R U P B 1
H41B H -0.2198 0.3116 0.4788 0.086 Uiso 0.438(5) 1 calc R U P B 1
H41C H -0.1297 0.2276 0.5506 0.086 Uiso 0.438(5) 1 calc R U P B 1
C35A C 0.1381(4) 0.2145(3) 0.4093(2) 0.0402(12) Uani 0.562(5) 1 d DG U P B 2
C36A C 0.1604(4) 0.3193(4) 0.4173(2) 0.0512(16) Uani 0.562(5) 1 d DG U P B 2
H36A H 0.2447 0.3387 0.3944 0.061 Uiso 0.562(5) 1 calc R U P B 2
C37A C 0.0594(5) 0.3957(4) 0.4589(3) 0.073(2) Uani 0.562(5) 1 d G U P B 2
H37A H 0.0747 0.4674 0.4645 0.088 Uiso 0.562(5) 1 calc R U P B 2
C38A C -0.0639(5) 0.3674(5) 0.4925(2) 0.075(2) Uani 0.562(5) 1 d G U P B 2
H38A H -0.1329 0.4196 0.5209 0.090 Uiso 0.562(5) 1 calc R U P B 2
C39A C -0.0862(4) 0.2626(6) 0.4844(3) 0.073(2) Uani 0.562(5) 1 d G U P B 2
H39A H -0.1705 0.2432 0.5073 0.087 Uiso 0.562(5) 1 calc R U P B 2
C40A C 0.0147(5) 0.1862(5) 0.4428(3) 0.085(3) Uani 0.562(5) 1 d DG U P B 2
H40A H -0.0005 0.1145 0.4372 0.102 Uiso 0.562(5) 1 calc R U P B 2
C41A C 0.2412(10) 0.1389(8) 0.3565(6) 0.106(4) Uani 0.562(5) 1 d D U P B 2
H41D H 0.2107 0.0685 0.3572 0.159 Uiso 0.562(5) 1 calc R U P B 2
H41E H 0.2378 0.1946 0.3061 0.159 Uiso 0.562(5) 1 calc R U P B 2
H41F H 0.3408 0.1052 0.3726 0.159 Uiso 0.562(5) 1 calc R U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.386(3) . ?
C1 N1 1.393(3) . ?
C1 C6 1.409(3) . ?
C2 C3 1.399(3) . ?
C3 C4 1.380(4) . ?
C4 C5 1.396(4) . ?
C5 C6 1.389(3) . ?
C6 N2 1.389(3) . ?
C7 N1 1.447(3) . ?
C7 C8 1.520(3) . ?
C8 C13 1.389(3) . ?
C8 C9 1.397(3) . ?
C9 C10 1.387(3) . ?
C10 C11 1.392(3) . ?
C11 C12 1.382(4) . ?
C12 C13 1.394(3) . ?
C14 N2 1.446(3) . ?
C14 C15 1.514(3) . ?
C15 C16 1.387(3) . ?
C15 C20 1.396(3) . ?
C16 C17 1.394(3) . ?
C17 C18 1.382(4) . ?
C18 C19 1.387(3) . ?
C19 C20 1.392(3) . ?
C21 P1 1.829(3) . ?
C22 P1 1.826(3) . ?
C23 P1 1.829(2) . ?
C24 P2 1.833(3) . ?
C25 P2 1.838(3) . ?
C26 P2 1.824(3) . ?
C27 P3 1.827(3) . ?
C28 P3 1.828(3) . ?
C29 P3 1.833(3) . ?
B1 N1 1.458(3) . ?
B1 N2 1.466(3) . ?
B1 Rh1 2.090(2) . ?
P1 Rh1 2.2659(6) . ?
P2 Rh1 2.3455(6) . ?
P3 Rh1 2.2651(7) . ?
C30 C31 1.535(2) . ?
C31 C32 1.536(2) . ?
C32 C33 1.536(2) . ?
C33 C34 1.536(2) . ?
C35 C36 1.3900 . ?
C35 C40 1.3900 . ?
C35 C41 1.535(2) . ?
C36 C37 1.3900 . ?
C37 C38 1.3900 . ?
C38 C39 1.3900 . ?
C39 C40 1.3900 . ?
C35A C36A 1.3900 . ?
C35A C40A 1.3900 . ?
C35A C41A 1.537(2) . ?
C36A C37A 1.3900 . ?
C37A C38A 1.3900 . ?
C38A C39A 1.3900 . ?
C39A C40A 1.3900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 N1 131.1(2) . . ?
C2 C1 C6 120.5(2) . . ?
N1 C1 C6 108.32(18) . . ?
C1 C2 C3 118.1(2) . . ?
C4 C3 C2 121.2(2) . . ?
C3 C4 C5 121.2(2) . . ?
C6 C5 C4 117.8(2) . . ?
C5 C6 N2 130.7(2) . . ?
C5 C6 C1 121.1(2) . . ?
N2 C6 C1 108.15(18) . . ?
N1 C7 C8 116.40(18) . . ?
C13 C8 C9 118.1(2) . . ?
C13 C8 C7 123.1(2) . . ?
C9 C8 C7 118.73(19) . . ?
C10 C9 C8 121.3(2) . . ?
C9 C10 C11 119.8(2) . . ?
C12 C11 C10 119.5(2) . . ?
C11 C12 C13 120.3(2) . . ?
C8 C13 C12 120.9(2) . . ?
N2 C14 C15 115.36(19) . . ?
C16 C15 C20 118.3(2) . . ?
C16 C15 C14 122.2(2) . . ?
C20 C15 C14 119.4(2) . . ?
C15 C16 C17 120.8(2) . . ?
C18 C17 C16 120.2(2) . . ?
C17 C18 C19 119.7(2) . . ?
C18 C19 C20 119.8(2) . . ?
C19 C20 C15 121.1(2) . . ?
N1 B1 N2 102.51(17) . . ?
N1 B1 Rh1 132.40(16) . . ?
N2 B1 Rh1 124.61(16) . . ?
C1 N1 C7 121.23(18) . . ?
C1 N1 B1 110.19(17) . . ?
C7 N1 B1 127.54(18) . . ?
C6 N2 C14 121.56(19) . . ?
C6 N2 B1 110.36(18) . . ?
C14 N2 B1 127.65(18) . . ?
C22 P1 C21 101.62(14) . . ?
C22 P1 C23 98.59(14) . . ?
C21 P1 C23 97.64(13) . . ?
C22 P1 Rh1 114.65(10) . . ?
C21 P1 Rh1 118.61(9) . . ?
C23 P1 Rh1 121.89(8) . . ?
C26 P2 C24 98.09(16) . . ?
C26 P2 C25 100.45(15) . . ?
C24 P2 C25 96.95(14) . . ?
C26 P2 Rh1 116.70(9) . . ?
C24 P2 Rh1 122.33(10) . . ?
C25 P2 Rh1 117.97(10) . . ?
C27 P3 C28 99.26(15) . . ?
C27 P3 C29 102.06(16) . . ?
C28 P3 C29 97.50(14) . . ?
C27 P3 Rh1 116.30(10) . . ?
C28 P3 Rh1 120.27(9) . . ?
C29 P3 Rh1 117.83(12) . . ?
B1 Rh1 P3 85.37(6) . . ?
B1 Rh1 P1 83.58(6) . . ?
P3 Rh1 P1 167.10(2) . . ?
B1 Rh1 P2 174.95(7) . . ?
P3 Rh1 P2 94.87(2) . . ?
P1 Rh1 P2 96.73(2) . . ?
C30 C31 C32 114.1(5) . . ?
C31 C32 C33 116.7(4) . . ?
C34 C33 C32 118.9(7) . . ?
C36 C35 C40 120.0 . . ?
C36 C35 C41 120.06(8) . . ?
C40 C35 C41 119.92(8) . . ?
C35 C36 C37 120.0 . . ?
C36 C37 C38 120.0 . . ?
C39 C38 C37 120.0 . . ?
C38 C39 C40 120.0 . . ?
C39 C40 C35 120.0 . . ?
C36A C35A C40A 120.0 . . ?
C36A C35A C41A 119.69(9) . . ?
C40A C35A C41A 119.99(9) . . ?
C35A C36A C37A 120.0 . . ?
C38A C37A C36A 120.0 . . ?
C37A C38A C39A 120.0 . . ?
C40A C39A C38A 120.0 . . ?
C39A C40A C35A 120.0 . . ?

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
N1 C1 C2 C3 -178.3(2) . . . . ?
C6 C1 C2 C3 -0.2(3) . . . . ?
C1 C2 C3 C4 -0.6(3) . . . . ?
C2 C3 C4 C5 0.5(4) . . . . ?
C3 C4 C5 C6 0.5(4) . . . . ?
C4 C5 C6 N2 175.8(2) . . . . ?
C4 C5 C6 C1 -1.3(3) . . . . ?
C2 C1 C6 C5 1.2(3) . . . . ?
N1 C1 C6 C5 179.7(2) . . . . ?
C2 C1 C6 N2 -176.53(19) . . . . ?
N1 C1 C6 N2 2.0(2) . . . . ?
N1 C7 C8 C13 7.4(3) . . . . ?
N1 C7 C8 C9 -173.4(2) . . . . ?
C13 C8 C9 C10 0.1(3) . . . . ?
C7 C8 C9 C10 -179.1(2) . . . . ?
C8 C9 C10 C11 0.2(4) . . . . ?
C9 C10 C11 C12 -0.2(4) . . . . ?
C10 C11 C12 C13 -0.1(4) . . . . ?
C9 C8 C13 C12 -0.5(3) . . . . ?
C7 C8 C13 C12 178.8(2) . . . . ?
C11 C12 C13 C8 0.5(4) . . . . ?
N2 C14 C15 C16 16.1(3) . . . . ?
N2 C14 C15 C20 -167.1(2) . . . . ?
C20 C15 C16 C17 -1.9(3) . . . . ?
C14 C15 C16 C17 174.9(2) . . . . ?
C15 C16 C17 C18 1.2(4) . . . . ?
C16 C17 C18 C19 0.1(4) . . . . ?
C17 C18 C19 C20 -0.7(3) . . . . ?
C18 C19 C20 C15 0.0(3) . . . . ?
C16 C15 C20 C19 1.3(3) . . . . ?
C14 C15 C20 C19 -175.6(2) . . . . ?
C2 C1 N1 C7 3.4(3) . . . . ?
C6 C1 N1 C7 -174.95(18) . . . . ?
C2 C1 N1 B1 172.5(2) . . . . ?
C6 C1 N1 B1 -5.8(2) . . . . ?
C8 C7 N1 C1 -71.5(3) . . . . ?
C8 C7 N1 B1 121.4(2) . . . . ?
N2 B1 N1 C1 7.0(2) . . . . ?
Rh1 B1 N1 C1 -165.15(16) . . . . ?
N2 B1 N1 C7 175.23(19) . . . . ?
Rh1 B1 N1 C7 3.1(3) . . . . ?
C5 C6 N2 C14 -1.9(4) . . . . ?
C1 C6 N2 C14 175.48(19) . . . . ?
C5 C6 N2 B1 -174.9(2) . . . . ?
C1 C6 N2 B1 2.5(2) . . . . ?
C15 C14 N2 C6 73.5(3) . . . . ?
C15 C14 N2 B1 -114.9(2) . . . . ?
N1 B1 N2 C6 -5.7(2) . . . . ?
Rh1 B1 N2 C6 167.20(15) . . . . ?
N1 B1 N2 C14 -178.1(2) . . . . ?
Rh1 B1 N2 C14 -5.2(3) . . . . ?
C30 C31 C32 C33 -177.0(7) . . . . ?
C31 C32 C33 C34 -176.9(9) . . . . ?
C40 C35 C36 C37 0.0 . . . . ?
C41 C35 C36 C37 -178.3(6) . . . . ?
C35 C36 C37 C38 0.0 . . . . ?
C36 C37 C38 C39 0.0 . . . . ?
C37 C38 C39 C40 0.0 . . . . ?
C38 C39 C40 C35 0.0 . . . . ?
C36 C35 C40 C39 0.0 . . . . ?
C41 C35 C40 C39 178.3(6) . . . . ?
C40A C35A C36A C37A 0.0 . . . . ?
C41A C35A C36A C37A 173.5(6) . . . . ?
C35A C36A C37A C38A 0.0 . . . . ?
C36A C37A C38A C39A 0.0 . . . . ?
C37A C38A C39A C40A 0.0 . . . . ?
C38A C39A C40A C35A 0.0 . . . . ?
C36A C35A C40A C39A 0.0 . . . . ?
C41A C35A C40A C39A -173.4(6) . . . . ?

_refine_diff_density_max         1.430
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.084

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cb39ck
_database_code_depnum_ccdc_archive 'CCDC 1037666'
_audit_update_record             
;
2014-12-04 deposited with the CCDC.
2015-03-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H46 B N2 P4 Rh'
_chemical_formula_sum            'C20 H46 B N2 P4 Rh'
_chemical_formula_weight         552.19

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'
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.2189(4)
_cell_length_b                   19.0437(7)
_cell_length_c                   15.9428(6)
_cell_angle_alpha                90
_cell_angle_beta                 94.531(4)
_cell_angle_gamma                90
_cell_volume                     2790.20(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    175(2)
_cell_measurement_reflns_used    41883
_cell_measurement_theta_min      2.68
_cell_measurement_theta_max      30.33

_exptl_crystal_description       rhombohedral
_exptl_crystal_colour            'clear very pale'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_F_000             1160
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    0.851
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.47
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
 (compiled Aug 13 2014,18:06:01)
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 The crystal was obtained by in situ crystallisation from a saturated solution
 of [(Me3P)3Rh-Bdmab] in PMe3. The light yellow solution (approx. 0.2 ul,
 1.5 mm height) was placed in a thin-walled glass tube of 0.5 mm outer diameter
 and flame-sealed. In this capillary microcrystals had formed, presumably due
 to evaporation of PMe3 during the preparation procedure. By repeated careful
 warming (with the finger tips and/or warm water) and cooling (ice water, 
 evaporation of acetone) the microcrystals were converted into 2
 well-developed individual crystals (ca. 0.1x0.1x0.1 mm3).
 At this point it was decided to proceed with these two crystals together,
 as attempts to separate them (by careful shaking) were unsuccessful and
 to dissolve and recrystallise appeared not very promising. The capillary
 was immersed in the nitrogen gas stream on the diffractometer and cooled to
 -40 C within 30 min and after 15 min at this temperature to -80 C within
 30 min. At this point the two crystals had developed to two adjacent
 individual rhombohedral crystals of ca. 0.18x0.20x0.24 and 0.09x0.10x0.11 mm3
 size, whilst the solution had completely discoloured. In order to fix
 the crystals inside  the capillary the temperature was lowered to -98 C 
 (175 K), below the melting point of PMe3 that solidified to a polycrystalline
 block that embedded the crystals. In this form the larger of the two crystals
 was centred in the beam and the data collection was commenced.


 The collected data cover nominally a full sphere of the reciprocal space.
 A combination of 32 sets of ω scans were used; each set at different \j,
 2θ or κ angles and each scan 0.8 deg in ω.
 Each frame was exposured for 15s. Nominal crystal to detector distance 43 mm.
;



_diffrn_ambient_temperature      175(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction, Xcalibur, EOS'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 16.1419
_diffrn_reflns_number            201179
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_av_R_equivalents  0.0879
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.139
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8105
_reflns_number_gt                6997
_reflns_threshold_expression     'I > 2σ(I)'


_reflns_special_details          
;
 The diffraction pattern shows at higher diffraction angles (d <= 1.5) well
 resolved reflections that were indexed using two orientation
 matrices. This is in agreement with the two crystals observed. At this 
 diffraction higher angle only a negligible number of overlapping reflections
 were observed and the orientation matrices were used for integration. 
 However, at lower diffraction angles (d > 1.5) a considerable number of
 reflections showing characteristics of a powder pattern were
 observed originating presumably from the polycrystalline PMe3. 
 The diffraction data for both crystals were separately integrated to 
 two datasets. For solution and refinement of the structure only the dataset 
 with the better I/sigma(I) ratio was used. As a consequence of 
 the presence of polycrystalline PMe3 7 low angle reflections of high
 Fo/Fc ratio have been omitted in the refinement.
 
 All H atoms were placed in idealised positions and refined using a riding
 model, with a common U restrained to be 1.2 (1.5 for methyl groups) times
 the equivalent isotropic displacement parameter of the parent atom.
 Methyl groups were treated as a rigid bodies and allowed to rotate about
 the E-CH3 bond.

 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.

 Reflections were merged by SHELXL according to the crystal class for the 
 calculation of statistics and refinement.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    
;
 SIR-92 (A. Altomare, G. Cascarano, C. Giacovazzo, A. Guagliardi, M. C. Burla,
         G. Polidori and M. Camalli, J. Appl. Crystallogr., 1994, 27, 435.)
;
_computing_structure_refinement  
;
 SHELXL-2014/7 (G. M. Sheldrick, Acta Cryst. (2008), A64, 112-122)'
;
_computing_molecular_graphics    
;
 K. Brandenburg, 1999, Diamond 3.2i, Crystal Impact GbR, Bonn, Germany.
;
_computing_publication_material  
;
 WinGX v2014.1 (L. J. Farrugia, J. Appl. Cryst., 2012, 45, 849-854.)
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0288P)²+3.4069P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         8105
_refine_ls_number_parameters     267
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0415
_refine_ls_wR_factor_ref         0.0876
_refine_ls_wR_factor_gt          0.0844
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_restrained_S_all      1.141
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.9515(3) 0.16043(16) 0.56331(17) 0.0308(6) Uani 1 1 d . . . . .
C2 C 1.0226(3) 0.1607(2) 0.4900(2) 0.0437(8) Uani 1 1 d . . . . .
H2 H 1.0131 0.1226 0.4515 0.052 Uiso 1 1 calc R U . . .
C3 C 1.1091(4) 0.2193(2) 0.4745(2) 0.0552(11) Uani 1 1 d . . . . .
H3 H 1.1589 0.2208 0.4246 0.066 Uiso 1 1 calc R U . . .
C4 C 1.1233(4) 0.2746(2) 0.5300(3) 0.0529(10) Uani 1 1 d . . . . .
H4 H 1.1834 0.3133 0.5177 0.063 Uiso 1 1 calc R U . . .
C5 C 1.0514(3) 0.27534(17) 0.6041(2) 0.0421(8) Uani 1 1 d . . . . .
H5 H 1.0601 0.3139 0.6420 0.051 Uiso 1 1 calc R U . . .
C6 C 0.9665(3) 0.21712(16) 0.61991(19) 0.0327(6) Uani 1 1 d . . . . .
C7 C 0.8263(3) 0.04642(16) 0.55149(18) 0.0371(7) Uani 1 1 d . . . . .
H7A H 0.7856 0.0569 0.4942 0.056 Uiso 1 1 calc R U . . .
H7B H 0.7550 0.0199 0.5812 0.056 Uiso 1 1 calc R U . . .
H7C H 0.9151 0.0185 0.5491 0.056 Uiso 1 1 calc R U . . .
C8 C 0.8843(4) 0.25229(18) 0.7564(2) 0.0506(9) Uani 1 1 d . . . . .
H8A H 0.9842 0.2624 0.7787 0.076 Uiso 1 1 calc R U . . .
H8B H 0.8299 0.2323 0.8011 0.076 Uiso 1 1 calc R U . . .
H8C H 0.8372 0.2958 0.7359 0.076 Uiso 1 1 calc R U . . .
C9 C 0.4827(4) 0.11878(19) 0.55521(19) 0.0423(7) Uani 1 1 d . . . . .
H9A H 0.4045 0.1476 0.5279 0.063 Uiso 1 1 calc R U . . .
H9B H 0.4564 0.0690 0.5498 0.063 Uiso 1 1 calc R U . . .
H9C H 0.5730 0.1273 0.5283 0.063 Uiso 1 1 calc R U . . .
C10 C 0.5313(4) 0.23667(16) 0.6527(2) 0.0462(8) Uani 1 1 d . . . . .
H10A H 0.4462 0.2554 0.6193 0.069 Uiso 1 1 calc R U . . .
H10B H 0.6190 0.2456 0.6235 0.069 Uiso 1 1 calc R U . . .
H10C H 0.5405 0.2597 0.7079 0.069 Uiso 1 1 calc R U . . .
C11 C 0.3188(3) 0.1420(2) 0.6940(2) 0.0496(9) Uani 1 1 d . . . . .
H11A H 0.3103 0.1706 0.7445 0.074 Uiso 1 1 calc R U . . .
H11B H 0.2885 0.0937 0.7050 0.074 Uiso 1 1 calc R U . . .
H11C H 0.2564 0.1616 0.6472 0.074 Uiso 1 1 calc R U . . .
C12 C 0.4087(4) -0.0420(2) 0.6586(2) 0.0523(9) Uani 1 1 d . . . . .
H12A H 0.4459 -0.0379 0.6029 0.078 Uiso 1 1 calc R U . . .
H12B H 0.3317 -0.0072 0.6640 0.078 Uiso 1 1 calc R U . . .
H12C H 0.3693 -0.0893 0.6654 0.078 Uiso 1 1 calc R U . . .
C13 C 0.4650(5) -0.0637(2) 0.8281(2) 0.0650(12) Uani 1 1 d . . . . .
H13A H 0.4246 -0.1097 0.8116 0.097 Uiso 1 1 calc R U . . .
H13B H 0.3861 -0.0323 0.8419 0.097 Uiso 1 1 calc R U . . .
H13C H 0.5347 -0.0690 0.8773 0.097 Uiso 1 1 calc R U . . .
C14 C 0.6645(4) -0.10313(17) 0.7130(3) 0.0569(10) Uani 1 1 d . . . . .
H14A H 0.7451 -0.1102 0.7560 0.085 Uiso 1 1 calc R U . . .
H14B H 0.7033 -0.0955 0.6583 0.085 Uiso 1 1 calc R U . . .
H14C H 0.6019 -0.1448 0.7102 0.085 Uiso 1 1 calc R U . . .
C15 C 0.8857(4) -0.02452(18) 0.8946(2) 0.0474(8) Uani 1 1 d . . . . .
H15A H 0.9843 -0.0421 0.9095 0.071 Uiso 1 1 calc R U . . .
H15B H 0.8217 -0.0639 0.8774 0.071 Uiso 1 1 calc R U . . .
H15C H 0.8491 -0.0012 0.9435 0.071 Uiso 1 1 calc R U . . .
C16 C 1.0041(4) -0.0105(2) 0.7384(2) 0.0489(9) Uani 1 1 d . . . . .
H16A H 1.0370 0.0210 0.6951 0.073 Uiso 1 1 calc R U . . .
H16B H 0.9478 -0.0492 0.7114 0.073 Uiso 1 1 calc R U . . .
H16C H 1.0888 -0.0295 0.7719 0.073 Uiso 1 1 calc R U . . .
C17 C 1.0301(3) 0.0978(2) 0.8530(2) 0.0460(8) Uani 1 1 d . . . . .
H17A H 1.1140 0.0703 0.8758 0.069 Uiso 1 1 calc R U . . .
H17B H 0.9914 0.1251 0.8983 0.069 Uiso 1 1 calc R U . . .
H17C H 1.0603 0.1298 0.8095 0.069 Uiso 1 1 calc R U . . .
C18 C 0.5394(6) 0.2272(2) 0.8801(3) 0.0744(15) Uani 1 1 d . . . . .
H18A H 0.5138 0.2398 0.9366 0.112 Uiso 1 1 calc R U . . .
H18B H 0.4535 0.2318 0.8402 0.112 Uiso 1 1 calc R U . . .
H18C H 0.6162 0.2586 0.8633 0.112 Uiso 1 1 calc R U . . .
C19 C 0.7294(4) 0.1423(3) 0.9750(2) 0.0726(14) Uani 1 1 d . . . . .
H19A H 0.8126 0.1718 0.9635 0.109 Uiso 1 1 calc R U . . .
H19B H 0.7639 0.0953 0.9918 0.109 Uiso 1 1 calc R U . . .
H19C H 0.6785 0.1632 1.0206 0.109 Uiso 1 1 calc R U . . .
C20 C 0.4506(4) 0.0994(2) 0.9320(2) 0.0517(9) Uani 1 1 d . . . . .
H20A H 0.4759 0.0525 0.9538 0.078 Uiso 1 1 calc R U . . .
H20B H 0.3656 0.0961 0.8912 0.078 Uiso 1 1 calc R U . . .
H20C H 0.4280 0.1301 0.9785 0.078 Uiso 1 1 calc R U . . .
B1 B 0.8131(3) 0.13467(15) 0.67687(18) 0.0240(5) Uani 1 1 d . . . . .
P1 P 0.50904(7) 0.14208(4) 0.66677(4) 0.02780(14) Uani 1 1 d . . . . .
P2 P 0.55805(8) -0.02627(4) 0.74040(4) 0.02829(14) Uani 1 1 d . . . . .
P3 P 0.88931(8) 0.03864(4) 0.80723(4) 0.02914(15) Uani 1 1 d . . . . .
P4 P 0.60488(8) 0.13588(4) 0.88022(4) 0.02820(14) Uani 1 1 d . . . . .
Rh1 Rh 0.67270(2) 0.08314(2) 0.75507(2) 0.01826(5) Uani 1 1 d . . . . .
N1 N 0.8603(2) 0.11148(12) 0.59583(14) 0.0275(5) Uani 1 1 d . . . . .
N2 N 0.8865(3) 0.20266(12) 0.68790(15) 0.0311(5) Uani 1 1 d . . . . .


_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
C1 N1 1.383(3) . ?
C1 C2 1.385(4) . ?
C1 C6 1.407(4) . ?
C2 C3 1.406(5) . ?
C3 C4 1.375(6) . ?
C4 C5 1.400(5) . ?
C5 C6 1.392(4) . ?
C6 N2 1.386(4) . ?
C7 N1 1.448(4) . ?
C8 N2 1.446(4) . ?
C9 P1 1.831(3) . ?
C10 P1 1.829(3) . ?
C11 P1 1.839(3) . ?
C12 P2 1.845(3) . ?
C13 P2 1.840(4) . ?
C14 P2 1.834(4) . ?
C15 P3 1.843(3) . ?
C16 P3 1.840(3) . ?
C17 P3 1.827(3) . ?
C18 P4 1.841(4) . ?
C19 P4 1.829(4) . ?
C20 P4 1.836(3) . ?
B1 N1 1.464(4) . ?
B1 N2 1.465(4) . ?
B1 Rh1 2.109(3) . ?
P1 Rh1 2.2765(7) . ?
P2 Rh1 2.3396(7) . ?
P3 Rh1 2.2660(7) . ?
P4 Rh1 2.3616(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
N1 C1 C2 131.4(3) . . ?
N1 C1 C6 108.0(2) . . ?
C2 C1 C6 120.6(3) . . ?
C1 C2 C3 117.7(4) . . ?
C4 C3 C2 121.5(3) . . ?
C3 C4 C5 121.5(3) . . ?
C6 C5 C4 117.1(3) . . ?
N2 C6 C5 129.9(3) . . ?
N2 C6 C1 108.5(2) . . ?
C5 C6 C1 121.5(3) . . ?
N1 B1 N2 101.9(2) . . ?
N1 B1 Rh1 128.36(19) . . ?
N2 B1 Rh1 129.8(2) . . ?
C10 P1 C9 97.32(16) . . ?
C10 P1 C11 98.50(17) . . ?
C9 P1 C11 99.99(17) . . ?
C10 P1 Rh1 119.09(12) . . ?
C9 P1 Rh1 120.80(11) . . ?
C11 P1 Rh1 116.81(11) . . ?
C14 P2 C13 99.3(2) . . ?
C14 P2 C12 94.90(18) . . ?
C13 P2 C12 96.2(2) . . ?
C14 P2 Rh1 119.25(13) . . ?
C13 P2 Rh1 120.20(13) . . ?
C12 P2 Rh1 121.43(13) . . ?
C17 P3 C16 97.37(17) . . ?
C17 P3 C15 98.94(17) . . ?
C16 P3 C15 99.48(17) . . ?
C17 P3 Rh1 119.56(12) . . ?
C16 P3 Rh1 120.21(11) . . ?
C15 P3 Rh1 116.96(12) . . ?
C19 P4 C20 96.43(19) . . ?
C19 P4 C18 97.0(2) . . ?
C20 P4 C18 95.3(2) . . ?
C19 P4 Rh1 122.40(13) . . ?
C20 P4 Rh1 119.00(13) . . ?
C18 P4 Rh1 120.62(13) . . ?
B1 Rh1 P3 80.02(8) . . ?
B1 Rh1 P1 79.20(8) . . ?
P3 Rh1 P1 158.92(3) . . ?
B1 Rh1 P2 130.45(8) . . ?
P3 Rh1 P2 94.69(3) . . ?
P1 Rh1 P2 96.04(3) . . ?
B1 Rh1 P4 121.15(8) . . ?
P3 Rh1 P4 97.67(3) . . ?
P1 Rh1 P4 96.08(3) . . ?
P2 Rh1 P4 108.40(3) . . ?
C1 N1 C7 120.5(2) . . ?
C1 N1 B1 111.1(2) . . ?
C7 N1 B1 128.4(2) . . ?
C6 N2 C8 120.1(2) . . ?
C6 N2 B1 110.5(2) . . ?
C8 N2 B1 129.4(2) . . ?

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
N1 C1 C2 C3 180.0(3) . . . . ?
C6 C1 C2 C3 -0.1(4) . . . . ?
C1 C2 C3 C4 0.0(5) . . . . ?
C2 C3 C4 C5 -0.5(5) . . . . ?
C3 C4 C5 C6 0.9(5) . . . . ?
C4 C5 C6 N2 178.5(3) . . . . ?
C4 C5 C6 C1 -1.0(4) . . . . ?
N1 C1 C6 N2 1.0(3) . . . . ?
C2 C1 C6 N2 -179.0(3) . . . . ?
N1 C1 C6 C5 -179.5(3) . . . . ?
C2 C1 C6 C5 0.6(4) . . . . ?
C2 C1 N1 C7 0.9(5) . . . . ?
C6 C1 N1 C7 -179.0(2) . . . . ?
C2 C1 N1 B1 179.2(3) . . . . ?
C6 C1 N1 B1 -0.7(3) . . . . ?
N2 B1 N1 C1 0.2(3) . . . . ?
Rh1 B1 N1 C1 179.2(2) . . . . ?
N2 B1 N1 C7 178.4(3) . . . . ?
Rh1 B1 N1 C7 -2.6(4) . . . . ?
C5 C6 N2 C8 -0.2(5) . . . . ?
C1 C6 N2 C8 179.3(3) . . . . ?
C5 C6 N2 B1 179.6(3) . . . . ?
C1 C6 N2 B1 -0.9(3) . . . . ?
N1 B1 N2 C6 0.4(3) . . . . ?
Rh1 B1 N2 C6 -178.6(2) . . . . ?
N1 B1 N2 C8 -179.7(3) . . . . ?
Rh1 B1 N2 C8 1.2(5) . . . . ?

_refine_diff_density_max         0.618
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.089

