# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1449234'
_audit_update_record             
;
2016-01-22 deposited with the CCDC.
2016-02-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H92 Cl6 Fe3 N4 O2 P4'
_chemical_formula_sum            'C46 H92 Cl6 Fe3 N4 O2 P4'
_chemical_formula_weight         1237.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Fe Fe 0.3463 0.8444 '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      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   23.440(3)
_cell_length_b                   23.440(3)
_cell_length_c                   32.519(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     15473(5)
_cell_formula_units_Z            9
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2881
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      22.73

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_F_000             5868
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    0.983
_shelx_estimated_absorpt_T_min   0.828
_shelx_estimated_absorpt_T_max   0.925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5734
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  triumph
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            59437
_diffrn_reflns_av_unetI/netI     0.1613
_diffrn_reflns_av_R_equivalents  0.2125
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_theta_min         1.605
_diffrn_reflns_theta_max         28.062
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8314
_reflns_number_gt                4173
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0766P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_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         8314
_refine_ls_number_parameters     283
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1912
_refine_ls_R_factor_gt           0.0897
_refine_ls_wR_factor_ref         0.1960
_refine_ls_wR_factor_gt          0.1603
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.000
_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 0.5783(3) 0.0365(3) 0.18430(17) 0.0283(13) Uani 1 1 d . . . . .
C2 C 0.4818(3) 0.0140(3) 0.15494(19) 0.0366(15) Uani 1 1 d . . . . .
H2 H 0.4473 -0.0004 0.1353 0.044 Uiso 1 1 calc R U . . .
C3 C 0.4839(3) 0.0411(3) 0.19132(19) 0.0348(15) Uani 1 1 d . . . . .
H3 H 0.4514 0.0495 0.2026 0.042 Uiso 1 1 calc R U . . .
C4 C 0.5807(4) 0.0426(4) 0.0690(2) 0.061(2) Uani 1 1 d . . . . .
C5 C 0.6252(4) 0.1120(5) 0.0888(3) 0.0841(17) Uani 1 1 d . . . . .
H5A H 0.6371 0.1462 0.0679 0.126 Uiso 1 1 calc R U . . .
H5B H 0.6653 0.1144 0.0998 0.126 Uiso 1 1 calc R U . . .
H5C H 0.6010 0.1187 0.1111 0.126 Uiso 1 1 calc R U . . .
C6 C 0.6180(4) 0.0322(5) 0.0350(3) 0.0841(17) Uani 1 1 d . . . . .
H6A H 0.5917 -0.0126 0.0241 0.126 Uiso 1 1 calc R U . . .
H6B H 0.6597 0.0384 0.0457 0.126 Uiso 1 1 calc R U . . .
H6C H 0.6268 0.0641 0.0129 0.126 Uiso 1 1 calc R U . . .
C7 C 0.5209(4) 0.0429(5) 0.0515(3) 0.0841(17) Uani 1 1 d . . . . .
H7A H 0.5350 0.0772 0.0304 0.126 Uiso 1 1 calc R U . . .
H7B H 0.4980 0.0517 0.0736 0.126 Uiso 1 1 calc R U . . .
H7C H 0.4912 -0.0001 0.0392 0.126 Uiso 1 1 calc R U . . .
C8 C 0.4960(4) -0.1024(4) 0.1005(3) 0.064(2) Uani 1 1 d . . . . .
C9 C 0.4292(13) -0.1215(11) 0.0895(11) 0.081(3) Uani 0.5 1 d . . P A 1
H9A H 0.4294 -0.0964 0.0653 0.122 Uiso 0.5 1 calc R U P A 1
H9B H 0.4080 -0.1123 0.1125 0.122 Uiso 0.5 1 calc R U P A 1
H9C H 0.4047 -0.1687 0.0832 0.122 Uiso 0.5 1 calc R U P A 1
C10 C 0.4780(9) -0.1352(9) 0.1460(7) 0.081(3) Uani 0.5 1 d . . P A 1
H10A H 0.4558 -0.1163 0.1618 0.122 Uiso 0.5 1 calc R U P A 1
H10B H 0.5186 -0.1262 0.1602 0.122 Uiso 0.5 1 calc R U P A 1
H10C H 0.4488 -0.1829 0.1435 0.122 Uiso 0.5 1 calc R U P A 1
C11 C 0.5162(9) -0.1432(9) 0.0756(7) 0.081(3) Uani 0.5 1 d . . P A 1
H11A H 0.4769 -0.1820 0.0649 0.122 Uiso 0.5 1 calc R U P A 1
H11B H 0.5409 -0.1574 0.0931 0.122 Uiso 0.5 1 calc R U P A 1
H11C H 0.5441 -0.1169 0.0527 0.122 Uiso 0.5 1 calc R U P A 1
C9B C 0.4281(14) -0.1039(11) 0.0899(11) 0.081(3) Uani 0.5 1 d . . P A 2
H9D H 0.3921 -0.1497 0.0888 0.122 Uiso 0.5 1 calc R U P A 2
H9E H 0.4322 -0.0829 0.0632 0.122 Uiso 0.5 1 calc R U P A 2
H9F H 0.4188 -0.0801 0.1112 0.122 Uiso 0.5 1 calc R U P A 2
C10B C 0.5003(9) -0.1436(9) 0.1326(7) 0.081(3) Uani 0.5 1 d . . P A 2
H10D H 0.4961 -0.1276 0.1596 0.122 Uiso 0.5 1 calc R U P A 2
H10E H 0.5430 -0.1416 0.1308 0.122 Uiso 0.5 1 calc R U P A 2
H10F H 0.4648 -0.1892 0.1289 0.122 Uiso 0.5 1 calc R U P A 2
C11B C 0.5152(9) -0.1180(9) 0.0542(6) 0.081(3) Uani 0.5 1 d . . P A 2
H11D H 0.5583 -0.1154 0.0555 0.122 Uiso 0.5 1 calc R U P A 2
H11E H 0.5170 -0.0856 0.0345 0.122 Uiso 0.5 1 calc R U P A 2
H11F H 0.4817 -0.1624 0.0455 0.122 Uiso 0.5 1 calc R U P A 2
C12 C 0.5190(3) 0.0379(3) 0.29527(19) 0.0484(19) Uani 1 1 d . . . . .
C13 C 0.5147(4) -0.0273(4) 0.2890(3) 0.0916(18) Uani 1 1 d . . . . .
H13A H 0.5590 -0.0216 0.2899 0.137 Uiso 1 1 calc R U . . .
H13B H 0.4946 -0.0453 0.2622 0.137 Uiso 1 1 calc R U . . .
H13C H 0.4877 -0.0576 0.3108 0.137 Uiso 1 1 calc R U . . .
C14 C 0.4497(4) 0.0253(4) 0.2951(3) 0.0916(18) Uani 1 1 d . . . . .
H14A H 0.4296 0.0080 0.2682 0.137 Uiso 1 1 calc R U . . .
H14B H 0.4500 0.0667 0.3004 0.137 Uiso 1 1 calc R U . . .
H14C H 0.4241 -0.0068 0.3165 0.137 Uiso 1 1 calc R U . . .
C15 C 0.5489(4) 0.0681(4) 0.3367(3) 0.0916(18) Uani 1 1 d . . . . .
H15A H 0.5943 0.0765 0.3380 0.137 Uiso 1 1 calc R U . . .
H15B H 0.5229 0.0377 0.3587 0.137 Uiso 1 1 calc R U . . .
H15C H 0.5490 0.1097 0.3400 0.137 Uiso 1 1 calc R U . . .
C16 C 0.5828(3) 0.1742(3) 0.25151(19) 0.0350(15) Uani 1 1 d . . . . .
C17 C 0.5184(3) 0.1758(4) 0.2551(2) 0.055(2) Uani 1 1 d . . . . .
H17A H 0.5266 0.2200 0.2484 0.082 Uiso 1 1 calc R U . . .
H17B H 0.5015 0.1644 0.2832 0.082 Uiso 1 1 calc R U . . .
H17C H 0.4858 0.1438 0.2359 0.082 Uiso 1 1 calc R U . . .
C18 C 0.6313(4) 0.2177(4) 0.2852(2) 0.064(2) Uani 1 1 d . . . . .
H18A H 0.6740 0.2205 0.2808 0.096 Uiso 1 1 calc R U . . .
H18B H 0.6140 0.1983 0.3122 0.096 Uiso 1 1 calc R U . . .
H18C H 0.6368 0.2619 0.2839 0.096 Uiso 1 1 calc R U . . .
C19 C 0.6132(3) 0.2022(3) 0.2095(2) 0.0509(19) Uani 1 1 d . . . . .
H19A H 0.5820 0.1760 0.1878 0.076 Uiso 1 1 calc R U . . .
H19B H 0.6539 0.2006 0.2062 0.076 Uiso 1 1 calc R U . . .
H19C H 0.6231 0.2480 0.2075 0.076 Uiso 1 1 calc R U . . .
C20 C 0.8542(3) 0.1132(4) 0.2536(2) 0.0475(18) Uani 1 1 d . . . . .
H20A H 0.8102 0.1047 0.2625 0.057 Uiso 1 1 calc R U . . .
H20B H 0.8879 0.1570 0.2639 0.057 Uiso 1 1 calc R U . . .
C21 C 0.8671(5) 0.0609(4) 0.2694(3) 0.076(3) Uani 1 1 d . . . . .
H21A H 0.9039 0.0798 0.2894 0.092 Uiso 1 1 calc R U . . .
H21B H 0.8274 0.0258 0.2833 0.092 Uiso 1 1 calc R U . . .
C22 C 0.8840(7) 0.0344(5) 0.2339(3) 0.120(4) Uani 1 1 d D . . . .
H22A H 0.8619 -0.0142 0.2357 0.144 Uiso 1 1 calc R U . . .
H22B H 0.9322 0.0523 0.2327 0.144 Uiso 1 1 calc R U . . .
C23 C 0.8614(4) 0.0544(4) 0.1973(2) 0.061(2) Uani 1 1 d D . . . .
H23A H 0.8931 0.0656 0.1744 0.073 Uiso 1 1 calc R U . . .
H23B H 0.8178 0.0183 0.1882 0.073 Uiso 1 1 calc R U . . .
N1 N 0.5397(2) 0.0106(2) 0.15071(14) 0.0318(12) Uani 1 1 d . . . . .
N2 N 0.5434(2) 0.0549(2) 0.20965(13) 0.0272(11) Uani 1 1 d . . . . .
P1 P 0.56844(8) -0.01876(9) 0.11040(5) 0.0425(5) Uani 1 1 d . . . . .
P2 P 0.58067(7) 0.09328(7) 0.25636(5) 0.0277(4) Uani 1 1 d . . . . .
Cl1 Cl 0.67283(9) -0.01641(8) 0.24614(5) 0.0504(5) Uani 1 1 d . . . . .
Cl2 Cl 0.75193(7) 0.16600(7) 0.21557(5) 0.0355(4) Uani 1 1 d . . . . .
Cl3 Cl 0.74080(7) 0.06127(7) 0.14133(5) 0.0357(4) Uani 1 1 d . . . . .
Fe1 Fe 0.67339(4) 0.05482(4) 0.19915(3) 0.0342(2) Uani 1 1 d . . . . .
Fe2 Fe 0.8333 0.1667 0.1667 0.0280(3) Uani 1 2 d S . P . .
O1 O 0.8570(2) 0.11086(19) 0.20919(13) 0.0394(10) 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 1.354(7) . ?
C1 N2 1.374(7) . ?
C1 Fe1 2.103(6) . ?
C2 C3 1.332(8) . ?
C2 N1 1.405(7) . ?
C2 H2 0.9500 . ?
C3 N2 1.399(7) . ?
C3 H3 0.9500 . ?
C4 C6 1.501(10) . ?
C4 C7 1.515(10) . ?
C4 C5 1.566(12) . ?
C4 P1 1.885(8) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.44(3) . ?
C8 C10B 1.46(2) . ?
C8 C11 1.499(18) . ?
C8 C9B 1.61(3) . ?
C8 C10 1.62(2) . ?
C8 C11B 1.66(2) . ?
C8 P1 1.871(8) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C9B H9D 0.9800 . ?
C9B H9E 0.9800 . ?
C9B H9F 0.9800 . ?
C10B H10D 0.9800 . ?
C10B H10E 0.9800 . ?
C10B H10F 0.9800 . ?
C11B H11D 0.9800 . ?
C11B H11E 0.9800 . ?
C11B H11F 0.9800 . ?
C12 C13 1.492(11) . ?
C12 C14 1.500(11) . ?
C12 C15 1.520(10) . ?
C12 P2 1.871(6) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C19 1.530(9) . ?
C16 C17 1.532(8) . ?
C16 C18 1.540(9) . ?
C16 P2 1.880(6) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 O1 1.447(7) . ?
C20 C21 1.493(10) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.457(11) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.473(7) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 O1 1.431(7) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
N1 P1 1.763(5) . ?
N2 P2 1.759(5) . ?
Cl1 Fe1 2.2587(19) . ?
Cl2 Fe1 2.3807(17) . ?
Cl2 Fe2 2.4781(14) . ?
Cl3 Fe1 2.4118(18) . ?
Cl3 Fe2 2.4755(14) . ?
Fe2 O1 2.158(4) 13_655 ?
Fe2 O1 2.158(4) . ?
Fe2 Cl3 2.4756(14) 13_655 ?
Fe2 Cl2 2.4780(14) 13_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 N2 104.8(5) . . ?
N1 C1 Fe1 132.8(4) . . ?
N2 C1 Fe1 122.3(4) . . ?
C3 C2 N1 108.0(5) . . ?
C3 C2 H2 126.0 . . ?
N1 C2 H2 126.0 . . ?
C2 C3 N2 106.4(5) . . ?
C2 C3 H3 126.8 . . ?
N2 C3 H3 126.8 . . ?
C6 C4 C7 109.8(6) . . ?
C6 C4 C5 109.4(7) . . ?
C7 C4 C5 106.7(7) . . ?
C6 C4 P1 106.4(6) . . ?
C7 C4 P1 118.9(6) . . ?
C5 C4 P1 105.4(5) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 C11 108.0(12) . . ?
C10B C8 C9B 122.3(15) . . ?
C9 C8 C10 95.5(16) . . ?
C11 C8 C10 106.2(11) . . ?
C10B C8 C11B 112.6(10) . . ?
C9B C8 C11B 100.0(14) . . ?
C9 C8 P1 130.1(9) . . ?
C10B C8 P1 104.1(8) . . ?
C11 C8 P1 110.5(9) . . ?
C9B C8 P1 115.4(9) . . ?
C10 C8 P1 103.0(7) . . ?
C11B C8 P1 100.5(8) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C8 C9B H9D 109.5 . . ?
C8 C9B H9E 109.5 . . ?
H9D C9B H9E 109.5 . . ?
C8 C9B H9F 109.5 . . ?
H9D C9B H9F 109.5 . . ?
H9E C9B H9F 109.5 . . ?
C8 C10B H10D 109.5 . . ?
C8 C10B H10E 109.5 . . ?
H10D C10B H10E 109.5 . . ?
C8 C10B H10F 109.5 . . ?
H10D C10B H10F 109.5 . . ?
H10E C10B H10F 109.5 . . ?
C8 C11B H11D 109.5 . . ?
C8 C11B H11E 109.5 . . ?
H11D C11B H11E 109.5 . . ?
C8 C11B H11F 109.5 . . ?
H11D C11B H11F 109.5 . . ?
H11E C11B H11F 109.5 . . ?
C13 C12 C14 106.7(6) . . ?
C13 C12 C15 112.2(7) . . ?
C14 C12 C15 107.3(7) . . ?
C13 C12 P2 104.6(5) . . ?
C14 C12 P2 121.2(5) . . ?
C15 C12 P2 105.0(4) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C19 C16 C17 108.1(5) . . ?
C19 C16 C18 108.7(6) . . ?
C17 C16 C18 110.0(5) . . ?
C19 C16 P2 106.2(4) . . ?
C17 C16 P2 119.3(4) . . ?
C18 C16 P2 104.2(4) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O1 C20 C21 106.4(5) . . ?
O1 C20 H20A 110.5 . . ?
C21 C20 H20A 110.5 . . ?
O1 C20 H20B 110.5 . . ?
C21 C20 H20B 110.5 . . ?
H20A C20 H20B 108.6 . . ?
C22 C21 C20 106.6(6) . . ?
C22 C21 H21A 110.4 . . ?
C20 C21 H21A 110.4 . . ?
C22 C21 H21B 110.4 . . ?
C20 C21 H21B 110.4 . . ?
H21A C21 H21B 108.6 . . ?
C21 C22 C23 106.8(7) . . ?
C21 C22 H22A 110.4 . . ?
C23 C22 H22A 110.4 . . ?
C21 C22 H22B 110.4 . . ?
C23 C22 H22B 110.4 . . ?
H22A C22 H22B 108.6 . . ?
O1 C23 C22 106.1(6) . . ?
O1 C23 H23A 110.5 . . ?
C22 C23 H23A 110.5 . . ?
O1 C23 H23B 110.5 . . ?
C22 C23 H23B 110.5 . . ?
H23A C23 H23B 108.7 . . ?
C1 N1 C2 110.1(5) . . ?
C1 N1 P1 118.3(4) . . ?
C2 N1 P1 131.6(4) . . ?
C1 N2 C3 110.7(4) . . ?
C1 N2 P2 117.2(4) . . ?
C3 N2 P2 132.0(4) . . ?
N1 P1 C8 102.3(3) . . ?
N1 P1 C4 100.1(3) . . ?
C8 P1 C4 112.9(4) . . ?
N2 P2 C12 102.5(2) . . ?
N2 P2 C16 101.5(2) . . ?
C12 P2 C16 112.3(3) . . ?
Fe1 Cl2 Fe2 91.98(5) . . ?
Fe1 Cl3 Fe2 91.30(5) . . ?
C1 Fe1 Cl1 112.98(16) . . ?
C1 Fe1 Cl2 115.81(15) . . ?
Cl1 Fe1 Cl2 111.90(7) . . ?
C1 Fe1 Cl3 115.31(16) . . ?
Cl1 Fe1 Cl3 109.59(6) . . ?
Cl2 Fe1 Cl3 88.99(6) . . ?
O1 Fe2 O1 180.0 13_655 . ?
O1 Fe2 Cl3 91.66(11) 13_655 . ?
O1 Fe2 Cl3 88.33(11) . . ?
O1 Fe2 Cl3 88.33(11) 13_655 13_655 ?
O1 Fe2 Cl3 91.67(11) . 13_655 ?
Cl3 Fe2 Cl3 180.0 . 13_655 ?
O1 Fe2 Cl2 90.89(11) 13_655 13_655 ?
O1 Fe2 Cl2 89.11(11) . 13_655 ?
Cl3 Fe2 Cl2 94.61(5) . 13_655 ?
Cl3 Fe2 Cl2 85.40(5) 13_655 13_655 ?
O1 Fe2 Cl2 89.11(11) 13_655 . ?
O1 Fe2 Cl2 90.89(11) . . ?
Cl3 Fe2 Cl2 85.39(5) . . ?
Cl3 Fe2 Cl2 94.60(5) 13_655 . ?
Cl2 Fe2 Cl2 180.0 13_655 . ?
C23 O1 C20 109.4(5) . . ?
C23 O1 Fe2 123.1(4) . . ?
C20 O1 Fe2 125.8(3) . . ?

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 C2 C3 N2 0.3(7) . . . . ?
O1 C20 C21 C22 5.9(10) . . . . ?
C20 C21 C22 C23 -17.4(12) . . . . ?
C21 C22 C23 O1 22.5(11) . . . . ?
N2 C1 N1 C2 1.1(6) . . . . ?
Fe1 C1 N1 C2 -175.2(4) . . . . ?
N2 C1 N1 P1 179.7(4) . . . . ?
Fe1 C1 N1 P1 3.5(8) . . . . ?
C3 C2 N1 C1 -0.9(7) . . . . ?
C3 C2 N1 P1 -179.3(5) . . . . ?
N1 C1 N2 C3 -0.9(6) . . . . ?
Fe1 C1 N2 C3 175.9(4) . . . . ?
N1 C1 N2 P2 -178.2(4) . . . . ?
Fe1 C1 N2 P2 -1.5(6) . . . . ?
C2 C3 N2 C1 0.3(7) . . . . ?
C2 C3 N2 P2 177.2(4) . . . . ?
C1 N1 P1 C8 130.7(5) . . . . ?
C2 N1 P1 C8 -51.0(6) . . . . ?
C1 N1 P1 C4 -113.0(5) . . . . ?
C2 N1 P1 C4 65.3(6) . . . . ?
C9 C8 P1 N1 57.8(19) . . . . ?
C10B C8 P1 N1 -80.4(8) . . . . ?
C11 C8 P1 N1 -164.1(10) . . . . ?
C9B C8 P1 N1 56.4(15) . . . . ?
C10 C8 P1 N1 -51.0(8) . . . . ?
C11B C8 P1 N1 162.9(7) . . . . ?
C9 C8 P1 C4 -48.9(19) . . . . ?
C10B C8 P1 C4 172.9(8) . . . . ?
C11 C8 P1 C4 89.2(10) . . . . ?
C9B C8 P1 C4 -50.3(15) . . . . ?
C10 C8 P1 C4 -157.7(7) . . . . ?
C11B C8 P1 C4 56.2(8) . . . . ?
C6 C4 P1 N1 169.0(5) . . . . ?
C7 C4 P1 N1 -66.6(7) . . . . ?
C5 C4 P1 N1 52.9(5) . . . . ?
C6 C4 P1 C8 -83.0(6) . . . . ?
C7 C4 P1 C8 41.5(7) . . . . ?
C5 C4 P1 C8 161.0(5) . . . . ?
C1 N2 P2 C12 -122.3(5) . . . . ?
C3 N2 P2 C12 61.1(6) . . . . ?
C1 N2 P2 C16 121.6(4) . . . . ?
C3 N2 P2 C16 -55.1(6) . . . . ?
C13 C12 P2 N2 61.0(6) . . . . ?
C14 C12 P2 N2 -59.2(7) . . . . ?
C15 C12 P2 N2 179.3(6) . . . . ?
C13 C12 P2 C16 169.2(5) . . . . ?
C14 C12 P2 C16 48.9(7) . . . . ?
C15 C12 P2 C16 -72.5(6) . . . . ?
C19 C16 P2 N2 -50.2(4) . . . . ?
C17 C16 P2 N2 72.1(5) . . . . ?
C18 C16 P2 N2 -164.8(4) . . . . ?
C19 C16 P2 C12 -158.9(4) . . . . ?
C17 C16 P2 C12 -36.6(6) . . . . ?
C18 C16 P2 C12 86.4(5) . . . . ?
C22 C23 O1 C20 -19.1(9) . . . . ?
C22 C23 O1 Fe2 175.2(6) . . . . ?
C21 C20 O1 C23 8.3(8) . . . . ?
C21 C20 O1 Fe2 173.5(5) . . . . ?

_refine_diff_density_max         0.666
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.091

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.000 0.500 603.0 90.5
2 0.333 0.667 0.167 594.6 90.0
3 0.667 0.333 0.833 594.6 89.9
_platon_squeeze_details          
;
The residual electron density was assigned to half a molecule of 
the tetrahydrofuran solvent [270/18= 15 e per asymmetric unit; half a
molecule of C4H8O1 would give 20 e]. 
;


_shelxl_version_number           2013-4

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
####################################################################### 
# 
# 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_pbpa140106
_database_code_depnum_ccdc_archive 'CCDC 1449235'
_audit_update_record             
;
2016-01-22 deposited with the CCDC.
2016-02-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H76 N4 P4 Rh, 2(C H2 Cl2), Cl'
_chemical_formula_sum            'C40 H80 Cl5 N4 P4 Rh'
_chemical_formula_weight         1021.12

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_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                   14.6459(12)
_cell_length_b                   15.1086(13)
_cell_length_c                   15.8170(13)
_cell_angle_alpha                88.107(2)
_cell_angle_beta                 64.451(2)
_cell_angle_gamma                72.376(2)
_cell_volume                     2990.1(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    8217
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      27.95

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.134
_exptl_crystal_F_000             1076
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    0.643
_shelx_estimated_absorpt_T_min   0.856
_shelx_estimated_absorpt_T_max   0.950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6784
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            40535
_diffrn_reflns_av_unetI/netI     0.0771
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.436
_diffrn_reflns_theta_max         28.206
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             14544
_reflns_number_gt                9039
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1220P)²] 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         14544
_refine_ls_number_parameters     483
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1111
_refine_ls_R_factor_gt           0.0699
_refine_ls_wR_factor_ref         0.2111
_refine_ls_wR_factor_gt          0.1933
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.000
_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 0.3374(3) 0.5248(3) 0.5470(3) 0.0276(9) Uani 1 1 d . . . . .
C2 C 0.2236(4) 0.5042(3) 0.4921(3) 0.0327(10) Uani 1 1 d . . . . .
H2 H 0.1982 0.4880 0.4507 0.039 Uiso 1 1 calc R U . . .
C3 C 0.1653(4) 0.5419(4) 0.5815(3) 0.0340(11) Uani 1 1 d . . . . .
H3 H 0.0900 0.5573 0.6159 0.041 Uiso 1 1 calc R U . . .
C4 C 0.4622(4) 0.5155(4) 0.2866(3) 0.0368(11) Uani 1 1 d . . . . .
C5 C 0.4700(7) 0.6075(5) 0.3106(5) 0.076(2) Uani 1 1 d . . . . .
H5A H 0.4813 0.6436 0.2564 0.114 Uiso 1 1 calc R U . . .
H5B H 0.5302 0.5964 0.3263 0.114 Uiso 1 1 calc R U . . .
H5C H 0.4037 0.6426 0.3649 0.114 Uiso 1 1 calc R U . . .
C6 C 0.5631(5) 0.4624(6) 0.1971(4) 0.074(2) Uani 1 1 d . . . . .
H6A H 0.5772 0.5043 0.1477 0.111 Uiso 1 1 calc R U . . .
H6B H 0.5518 0.4086 0.1750 0.111 Uiso 1 1 calc R U . . .
H6C H 0.6242 0.4407 0.2117 0.111 Uiso 1 1 calc R U . . .
C7 C 0.3666(4) 0.5297(5) 0.2669(4) 0.0506(15) Uani 1 1 d . . . . .
H7A H 0.3013 0.5640 0.3224 0.076 Uiso 1 1 calc R U . . .
H7B H 0.3625 0.4688 0.2525 0.076 Uiso 1 1 calc R U . . .
H7C H 0.3741 0.5657 0.2129 0.076 Uiso 1 1 calc R U . . .
C8 C 0.4748(4) 0.3226(4) 0.3686(4) 0.0420(13) Uani 1 1 d . . . . .
C9 C 0.5889(5) 0.2664(5) 0.3099(7) 0.097(3) Uani 1 1 d . . . . .
H9A H 0.5964 0.1997 0.3101 0.145 Uiso 1 1 calc R U . . .
H9B H 0.6335 0.2801 0.3360 0.145 Uiso 1 1 calc R U . . .
H9C H 0.6116 0.2826 0.2451 0.145 Uiso 1 1 calc R U . . .
C10 C 0.4015(5) 0.3061(4) 0.3317(4) 0.0467(13) Uani 1 1 d . . . . .
H10A H 0.4188 0.3279 0.2693 0.070 Uiso 1 1 calc R U . . .
H10B H 0.3273 0.3406 0.3750 0.070 Uiso 1 1 calc R U . . .
H10C H 0.4108 0.2392 0.3269 0.070 Uiso 1 1 calc R U . . .
C11 C 0.4390(8) 0.2896(5) 0.4698(6) 0.085(3) Uani 1 1 d . . . . .
H11A H 0.4457 0.2232 0.4654 0.127 Uiso 1 1 calc R U . . .
H11B H 0.3645 0.3262 0.5100 0.127 Uiso 1 1 calc R U . . .
H11C H 0.4845 0.2989 0.4972 0.127 Uiso 1 1 calc R U . . .
C12 C 0.1284(4) 0.5374(5) 0.8105(4) 0.0556(17) Uani 1 1 d . . . . .
C13 C 0.2142(7) 0.4462(7) 0.7974(8) 0.125(5) Uani 1 1 d . . . . .
H13A H 0.1851 0.4074 0.8462 0.187 Uiso 1 1 calc R U . . .
H13B H 0.2738 0.4585 0.8023 0.187 Uiso 1 1 calc R U . . .
H13C H 0.2396 0.4134 0.7351 0.187 Uiso 1 1 calc R U . . .
C14 C 0.0368(5) 0.5183(5) 0.8050(5) 0.0630(18) Uani 1 1 d . . . . .
H14A H 0.0633 0.4763 0.7477 0.095 Uiso 1 1 calc R U . . .
H14B H -0.0139 0.5772 0.8032 0.095 Uiso 1 1 calc R U . . .
H14C H 0.0010 0.4888 0.8604 0.095 Uiso 1 1 calc R U . . .
C15 C 0.0891(8) 0.5869(9) 0.9100(5) 0.140(5) Uani 1 1 d . . . . .
H15A H 0.0193 0.6345 0.9284 0.210 Uiso 1 1 calc R U . . .
H15B H 0.1405 0.6166 0.9089 0.210 Uiso 1 1 calc R U . . .
H15C H 0.0828 0.5408 0.9555 0.210 Uiso 1 1 calc R U . . .
C16 C 0.1076(4) 0.7294(4) 0.7271(4) 0.0540(16) Uani 1 1 d . . . . .
C17 C -0.0043(4) 0.7360(5) 0.7412(5) 0.0642(18) Uani 1 1 d . . . . .
H17A H -0.0462 0.7255 0.8061 0.096 Uiso 1 1 calc R U . . .
H17B H 0.0009 0.6886 0.6971 0.096 Uiso 1 1 calc R U . . .
H17C H -0.0393 0.7983 0.7295 0.096 Uiso 1 1 calc R U . . .
C18 C 0.1626(6) 0.7622(5) 0.6305(6) 0.079(2) Uani 1 1 d . . . . .
H18A H 0.1184 0.8248 0.6282 0.119 Uiso 1 1 calc R U . . .
H18B H 0.1717 0.7186 0.5807 0.119 Uiso 1 1 calc R U . . .
H18C H 0.2326 0.7642 0.6208 0.119 Uiso 1 1 calc R U . . .
C19 C 0.0985(7) 0.7933(6) 0.8048(8) 0.125(4) Uani 1 1 d . . . . .
H19A H 0.0520 0.8564 0.8072 0.187 Uiso 1 1 calc R U . . .
H19B H 0.1695 0.7955 0.7916 0.187 Uiso 1 1 calc R U . . .
H19C H 0.0680 0.7692 0.8655 0.187 Uiso 1 1 calc R U . . .
C20 C 0.6078(4) -0.0611(3) -0.1370(3) 0.0297(10) Uani 1 1 d . . . . .
C21 C 0.7165(4) -0.2065(4) -0.2160(3) 0.0353(11) Uani 1 1 d . . . . .
H21 H 0.7514 -0.2722 -0.2279 0.042 Uiso 1 1 calc R U . . .
C22 C 0.7282(4) -0.1439(4) -0.2780(3) 0.0385(12) Uani 1 1 d . . . . .
H22 H 0.7743 -0.1579 -0.3436 0.046 Uiso 1 1 calc R U . . .
C23 C 0.6820(4) -0.2115(4) 0.0263(4) 0.0471(14) Uani 1 1 d . . . . .
C24 C 0.7444(6) -0.1426(6) 0.0017(6) 0.088(3) Uani 1 1 d . . . . .
H24A H 0.6979 -0.0819 0.0386 0.132 Uiso 1 1 calc R U . . .
H24B H 0.7701 -0.1355 -0.0657 0.132 Uiso 1 1 calc R U . . .
H24C H 0.8055 -0.1661 0.0163 0.132 Uiso 1 1 calc R U . . .
C25 C 0.6324(6) -0.2145(8) 0.1320(5) 0.117(4) Uani 1 1 d . . . . .
H25A H 0.6008 -0.2650 0.1470 0.176 Uiso 1 1 calc R U . . .
H25B H 0.5768 -0.1548 0.1631 0.176 Uiso 1 1 calc R U . . .
H25C H 0.6876 -0.2258 0.1541 0.176 Uiso 1 1 calc R U . . .
C26 C 0.7596(5) -0.3080(5) -0.0244(5) 0.0680(19) Uani 1 1 d . . . . .
H26A H 0.8210 -0.3237 -0.0100 0.102 Uiso 1 1 calc R U . . .
H26B H 0.7843 -0.3072 -0.0926 0.102 Uiso 1 1 calc R U . . .
H26C H 0.7231 -0.3550 -0.0030 0.102 Uiso 1 1 calc R U . . .
C27 C 0.4970(4) -0.2413(4) -0.0060(3) 0.0388(12) Uani 1 1 d . . . . .
C28 C 0.4386(9) -0.2572(8) 0.0959(5) 0.138(5) Uani 1 1 d . . . . .
H28A H 0.4118 -0.1988 0.1368 0.207 Uiso 1 1 calc R U . . .
H28B H 0.4877 -0.3053 0.1133 0.207 Uiso 1 1 calc R U . . .
H28C H 0.3784 -0.2779 0.1035 0.207 Uiso 1 1 calc R U . . .
C29 C 0.5629(6) -0.3359(5) -0.0620(5) 0.072(2) Uani 1 1 d . . . . .
H29A H 0.5155 -0.3687 -0.0642 0.108 Uiso 1 1 calc R U . . .
H29B H 0.6061 -0.3724 -0.0319 0.108 Uiso 1 1 calc R U . . .
H29C H 0.6101 -0.3281 -0.1263 0.108 Uiso 1 1 calc R U . . .
C30 C 0.4212(6) -0.1923(5) -0.0451(6) 0.078(2) Uani 1 1 d . . . . .
H30A H 0.4615 -0.1818 -0.1104 0.117 Uiso 1 1 calc R U . . .
H30B H 0.3747 -0.1321 -0.0071 0.117 Uiso 1 1 calc R U . . .
H30C H 0.3775 -0.2309 -0.0436 0.117 Uiso 1 1 calc R U . . .
C31 C 0.7971(12) 0.0514(7) -0.3319(8) 0.156(4) Uani 1 1 d . . . . .
C32 C 0.7832(11) 0.1512(8) -0.3687(12) 0.212(5) Uani 1 1 d . . . . .
H32A H 0.7167 0.1961 -0.3227 0.318 Uiso 1 1 calc R U . . .
H32B H 0.7806 0.1476 -0.4293 0.318 Uiso 1 1 calc R U . . .
H32C H 0.8437 0.1714 -0.3767 0.318 Uiso 1 1 calc R U . . .
C33 C 0.8151(11) 0.0567(9) -0.2505(13) 0.212(5) Uani 1 1 d . . . . .
H33A H 0.8039 0.0029 -0.2159 0.318 Uiso 1 1 calc R U . . .
H33B H 0.7651 0.1146 -0.2096 0.318 Uiso 1 1 calc R U . . .
H33C H 0.8886 0.0561 -0.2702 0.318 Uiso 1 1 calc R U . . .
C34 C 0.8846(11) -0.0267(9) -0.3967(12) 0.212(5) Uani 1 1 d . . . . .
H34A H 0.8755 -0.0330 -0.4538 0.318 Uiso 1 1 calc R U . . .
H34B H 0.8848 -0.0843 -0.3664 0.318 Uiso 1 1 calc R U . . .
H34C H 0.9525 -0.0154 -0.4136 0.318 Uiso 1 1 calc R U . . .
C35 C 0.6145(12) 0.0301(7) -0.3757(7) 0.156(4) Uani 1 1 d . . . . .
C36 C 0.5231(16) 0.0007(9) -0.3295(10) 0.239(7) Uani 1 1 d . . . . .
H36A H 0.4946 -0.0055 -0.3740 0.359 Uiso 1 1 calc R U . . .
H36B H 0.4685 0.0471 -0.2761 0.359 Uiso 1 1 calc R U . . .
H36C H 0.5432 -0.0597 -0.3065 0.359 Uiso 1 1 calc R U . . .
C37 C 0.6900(15) -0.0395(8) -0.4585(9) 0.239(7) Uani 1 1 d . . . . .
H37A H 0.6901 -0.1024 -0.4410 0.359 Uiso 1 1 calc R U . . .
H37B H 0.7620 -0.0353 -0.4802 0.359 Uiso 1 1 calc R U . . .
H37C H 0.6680 -0.0271 -0.5092 0.359 Uiso 1 1 calc R U . . .
C38 C 0.5728(15) 0.1258(8) -0.4070(9) 0.239(7) Uani 1 1 d . . . . .
H38A H 0.6047 0.1210 -0.4760 0.359 Uiso 1 1 calc R U . . .
H38B H 0.5924 0.1728 -0.3832 0.359 Uiso 1 1 calc R U . . .
H38C H 0.4949 0.1444 -0.3816 0.359 Uiso 1 1 calc R U . . .
C39 C 0.9589(6) 0.6527(5) 0.4600(5) 0.0637(18) Uani 1 1 d . . . . .
H39A H 0.9277 0.6208 0.5159 0.076 Uiso 1 1 calc R U . . .
H39B H 1.0198 0.6053 0.4098 0.076 Uiso 1 1 calc R U . . .
C40 C 0.1580(7) 0.6087(6) 0.1667(5) 0.085(2) Uani 1 1 d . . . . .
H40A H 0.0892 0.6206 0.1638 0.102 Uiso 1 1 calc R U . . .
H40B H 0.1681 0.5537 0.2014 0.102 Uiso 1 1 calc R U . . .
N1 N 0.3288(3) 0.4933(3) 0.4714(2) 0.0270(8) Uani 1 1 d . . . . .
N2 N 0.2346(3) 0.5551(3) 0.6167(2) 0.0283(8) Uani 1 1 d . . . . .
N3 N 0.6412(3) -0.1536(3) -0.1294(2) 0.0298(8) Uani 1 1 d . . . . .
N4 N 0.6619(3) -0.0536(3) -0.2315(2) 0.0323(9) Uani 1 1 d . . . . .
P1 P 0.46087(9) 0.44818(8) 0.38842(8) 0.0257(2) Uani 1 1 d . . . . .
P2 P 0.20166(10) 0.61028(11) 0.72605(8) 0.0383(3) Uani 1 1 d . . . . .
P3 P 0.57256(9) -0.15967(9) -0.00906(8) 0.0282(3) Uani 1 1 d . . . . .
P4 P 0.64758(16) 0.05242(11) -0.28024(10) 0.0594(5) Uani 1 1 d . . . . .
Cl1 Cl 0.13522(10) 0.43589(9) 0.31918(9) 0.0381(3) Uani 1 1 d . . . . .
Cl2 Cl 0.86171(19) 0.70702(17) 0.4204(2) 0.1018(8) Uani 1 1 d . . . . .
Cl3 Cl 1.00342(19) 0.73691(16) 0.48932(16) 0.0901(6) Uani 1 1 d . . . . .
Cl4 Cl 0.15245(19) 0.70327(18) 0.22666(17) 0.0986(7) Uani 1 1 d . . . . .
Cl5 Cl 0.2624(2) 0.58328(17) 0.05114(15) 0.1059(8) Uani 1 1 d . . . . .
Rh1 Rh 0.5000 0.5000 0.5000 0.02369(13) Uani 1 2 d S . P . .
Rh2 Rh 0.5000 0.0000 0.0000 0.02719(14) Uani 1 2 d S . 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 1.369(5) . ?
C1 N2 1.369(5) . ?
C1 Rh1 2.077(4) . ?
C2 C3 1.331(6) . ?
C2 N1 1.386(5) . ?
C2 H2 0.9500 . ?
C3 N2 1.413(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.504(8) . ?
C4 C7 1.515(7) . ?
C4 C6 1.543(8) . ?
C4 P1 1.873(5) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.493(8) . ?
C8 C10 1.505(6) . ?
C8 C11 1.571(9) . ?
C8 P1 1.867(5) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C14 1.492(8) . ?
C12 C13 1.506(11) . ?
C12 C15 1.550(9) . ?
C12 P2 1.879(6) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C19 1.522(9) . ?
C16 C17 1.526(8) . ?
C16 C18 1.536(10) . ?
C16 P2 1.902(6) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 N3 1.353(6) . ?
C20 N4 1.378(5) . ?
C20 Rh2 2.082(4) . ?
C21 C22 1.333(7) . ?
C21 N3 1.403(6) . ?
C21 H21 0.9500 . ?
C22 N4 1.411(6) . ?
C22 H22 0.9500 . ?
C23 C25 1.513(8) . ?
C23 C24 1.520(10) . ?
C23 C26 1.534(9) . ?
C23 P3 1.866(5) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C30 1.493(9) . ?
C27 C29 1.507(8) . ?
C27 C28 1.516(8) . ?
C27 P3 1.877(5) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C33 1.43(2) . ?
C31 C34 1.455(15) . ?
C31 C32 1.584(16) . ?
C31 P4 1.975(16) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C36 1.42(2) . ?
C35 C37 1.478(15) . ?
C35 C38 1.545(15) . ?
C35 P4 1.841(16) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 Cl3 1.749(7) . ?
C39 Cl2 1.766(7) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 Cl4 1.703(8) . ?
C40 Cl5 1.763(8) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
N1 P1 1.732(4) . ?
N2 P2 1.746(4) . ?
N3 P3 1.743(4) . ?
N4 P4 1.749(4) . ?
P1 Rh1 2.3003(10) . ?
P3 Rh2 2.3041(12) . ?
Rh1 C1 2.077(4) 2_666 ?
Rh1 P1 2.3003(10) 2_666 ?
Rh2 C20 2.083(4) 2_655 ?
Rh2 P3 2.3041(12) 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 N2 104.4(3) . . ?
N1 C1 Rh1 104.7(3) . . ?
N2 C1 Rh1 150.8(3) . . ?
C3 C2 N1 106.2(4) . . ?
C3 C2 H2 126.9 . . ?
N1 C2 H2 126.9 . . ?
C2 C3 N2 108.4(4) . . ?
C2 C3 H3 125.8 . . ?
N2 C3 H3 125.8 . . ?
C5 C4 C7 111.1(5) . . ?
C5 C4 C6 110.0(6) . . ?
C7 C4 C6 107.7(4) . . ?
C5 C4 P1 104.6(3) . . ?
C7 C4 P1 115.3(4) . . ?
C6 C4 P1 108.2(4) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 C10 112.4(5) . . ?
C9 C8 C11 107.9(6) . . ?
C10 C8 C11 106.1(5) . . ?
C9 C8 P1 110.8(4) . . ?
C10 C8 P1 114.6(4) . . ?
C11 C8 P1 104.3(4) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C14 C12 C13 109.3(7) . . ?
C14 C12 C15 108.7(5) . . ?
C13 C12 C15 108.1(7) . . ?
C14 C12 P2 120.9(4) . . ?
C13 C12 P2 104.0(4) . . ?
C15 C12 P2 105.1(5) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C19 C16 C17 109.2(6) . . ?
C19 C16 C18 110.1(7) . . ?
C17 C16 C18 106.8(5) . . ?
C19 C16 P2 106.2(5) . . ?
C17 C16 P2 118.3(5) . . ?
C18 C16 P2 106.2(4) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N3 C20 N4 104.7(4) . . ?
N3 C20 Rh2 104.8(3) . . ?
N4 C20 Rh2 150.5(4) . . ?
C22 C21 N3 104.4(4) . . ?
C22 C21 H21 127.8 . . ?
N3 C21 H21 127.8 . . ?
C21 C22 N4 109.9(4) . . ?
C21 C22 H22 125.0 . . ?
N4 C22 H22 125.0 . . ?
C25 C23 C24 109.5(7) . . ?
C25 C23 C26 110.2(6) . . ?
C24 C23 C26 108.2(5) . . ?
C25 C23 P3 108.4(4) . . ?
C24 C23 P3 104.3(4) . . ?
C26 C23 P3 115.9(4) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C30 C27 C29 108.4(5) . . ?
C30 C27 C28 111.7(7) . . ?
C29 C27 C28 107.3(6) . . ?
C30 C27 P3 105.6(4) . . ?
C29 C27 P3 116.1(4) . . ?
C28 C27 P3 107.8(4) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C33 C31 C34 106.6(16) . . ?
C33 C31 C32 107.5(12) . . ?
C34 C31 C32 117.0(10) . . ?
C33 C31 P4 104.2(8) . . ?
C34 C31 P4 121.2(10) . . ?
C32 C31 P4 99.0(9) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C36 C35 C37 106.4(13) . . ?
C36 C35 C38 104.6(14) . . ?
C37 C35 C38 110.7(10) . . ?
C36 C35 P4 103.9(8) . . ?
C37 C35 P4 122.4(12) . . ?
C38 C35 P4 107.2(8) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C35 C38 H38A 109.5 . . ?
C35 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C35 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
Cl3 C39 Cl2 109.6(4) . . ?
Cl3 C39 H39A 109.8 . . ?
Cl2 C39 H39A 109.8 . . ?
Cl3 C39 H39B 109.8 . . ?
Cl2 C39 H39B 109.8 . . ?
H39A C39 H39B 108.2 . . ?
Cl4 C40 Cl5 112.4(4) . . ?
Cl4 C40 H40A 109.1 . . ?
Cl5 C40 H40A 109.1 . . ?
Cl4 C40 H40B 109.1 . . ?
Cl5 C40 H40B 109.1 . . ?
H40A C40 H40B 107.9 . . ?
C1 N1 C2 111.8(4) . . ?
C1 N1 P1 102.6(3) . . ?
C2 N1 P1 145.4(3) . . ?
C1 N2 C3 109.2(3) . . ?
C1 N2 P2 122.2(3) . . ?
C3 N2 P2 128.4(3) . . ?
C20 N3 C21 112.8(4) . . ?
C20 N3 P3 103.2(3) . . ?
C21 N3 P3 144.0(3) . . ?
C20 N4 C22 108.2(4) . . ?
C20 N4 P4 123.6(3) . . ?
C22 N4 P4 128.2(3) . . ?
N1 P1 C8 101.8(2) . . ?
N1 P1 C4 102.2(2) . . ?
C8 P1 C4 114.0(2) . . ?
N1 P1 Rh1 85.28(11) . . ?
C8 P1 Rh1 121.46(16) . . ?
C4 P1 Rh1 121.04(16) . . ?
N2 P2 C12 102.2(2) . . ?
N2 P2 C16 101.4(2) . . ?
C12 P2 C16 111.8(3) . . ?
N3 P3 C23 103.2(2) . . ?
N3 P3 C27 102.7(2) . . ?
C23 P3 C27 113.1(3) . . ?
N3 P3 Rh2 84.72(14) . . ?
C23 P3 Rh2 120.9(2) . . ?
C27 P3 Rh2 122.06(18) . . ?
N4 P4 C35 103.2(4) . . ?
N4 P4 C31 98.5(4) . . ?
C35 P4 C31 110.7(6) . . ?
C1 Rh1 C1 180.0 . 2_666 ?
C1 Rh1 P1 112.74(11) . 2_666 ?
C1 Rh1 P1 67.26(11) 2_666 2_666 ?
C1 Rh1 P1 67.26(11) . . ?
C1 Rh1 P1 112.74(11) 2_666 . ?
P1 Rh1 P1 180.0 2_666 . ?
C20 Rh2 C20 180.0 . 2_655 ?
C20 Rh2 P3 67.31(13) . . ?
C20 Rh2 P3 112.69(13) 2_655 . ?
C20 Rh2 P3 112.69(13) . 2_655 ?
C20 Rh2 P3 67.31(13) 2_655 2_655 ?
P3 Rh2 P3 180.0 . 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 C2 C3 N2 0.3(6) . . . . ?
N3 C21 C22 N4 0.0(6) . . . . ?
N2 C1 N1 C2 0.6(5) . . . . ?
Rh1 C1 N1 C2 179.3(3) . . . . ?
N2 C1 N1 P1 -175.8(3) . . . . ?
Rh1 C1 N1 P1 2.9(3) . . . . ?
C3 C2 N1 C1 -0.6(6) . . . . ?
C3 C2 N1 P1 173.3(5) . . . . ?
N1 C1 N2 C3 -0.4(5) . . . . ?
Rh1 C1 N2 C3 -177.9(6) . . . . ?
N1 C1 N2 P2 -175.1(3) . . . . ?
Rh1 C1 N2 P2 7.4(9) . . . . ?
C2 C3 N2 C1 0.0(6) . . . . ?
C2 C3 N2 P2 174.3(4) . . . . ?
N4 C20 N3 C21 0.8(5) . . . . ?
Rh2 C20 N3 C21 -179.2(3) . . . . ?
N4 C20 N3 P3 179.2(3) . . . . ?
Rh2 C20 N3 P3 -0.7(3) . . . . ?
C22 C21 N3 C20 -0.5(5) . . . . ?
C22 C21 N3 P3 -177.9(4) . . . . ?
N3 C20 N4 C22 -0.7(5) . . . . ?
Rh2 C20 N4 C22 179.2(6) . . . . ?
N3 C20 N4 P4 179.9(3) . . . . ?
Rh2 C20 N4 P4 -0.2(9) . . . . ?
C21 C22 N4 C20 0.5(6) . . . . ?
C21 C22 N4 P4 179.8(4) . . . . ?
C1 N1 P1 C8 118.6(3) . . . . ?
C2 N1 P1 C8 -55.5(6) . . . . ?
C1 N1 P1 C4 -123.3(3) . . . . ?
C2 N1 P1 C4 62.5(6) . . . . ?
C1 N1 P1 Rh1 -2.5(3) . . . . ?
C2 N1 P1 Rh1 -176.7(6) . . . . ?
C9 C8 P1 N1 -171.0(5) . . . . ?
C10 C8 P1 N1 60.6(5) . . . . ?
C11 C8 P1 N1 -55.1(4) . . . . ?
C9 C8 P1 C4 79.8(5) . . . . ?
C10 C8 P1 C4 -48.7(5) . . . . ?
C11 C8 P1 C4 -164.3(4) . . . . ?
C9 C8 P1 Rh1 -79.3(5) . . . . ?
C10 C8 P1 Rh1 152.2(4) . . . . ?
C11 C8 P1 Rh1 36.6(5) . . . . ?
C5 C4 P1 N1 80.9(4) . . . . ?
C7 C4 P1 N1 -41.4(4) . . . . ?
C6 C4 P1 N1 -161.9(4) . . . . ?
C5 C4 P1 C8 -170.2(4) . . . . ?
C7 C4 P1 C8 67.6(5) . . . . ?
C6 C4 P1 C8 -53.0(5) . . . . ?
C5 C4 P1 Rh1 -11.0(5) . . . . ?
C7 C4 P1 Rh1 -133.2(4) . . . . ?
C6 C4 P1 Rh1 106.2(4) . . . . ?
C1 N2 P2 C12 -125.9(4) . . . . ?
C3 N2 P2 C12 60.4(5) . . . . ?
C1 N2 P2 C16 118.5(4) . . . . ?
C3 N2 P2 C16 -55.2(5) . . . . ?
C14 C12 P2 N2 -52.7(6) . . . . ?
C13 C12 P2 N2 70.4(6) . . . . ?
C15 C12 P2 N2 -176.0(5) . . . . ?
C14 C12 P2 C16 55.1(6) . . . . ?
C13 C12 P2 C16 178.2(6) . . . . ?
C15 C12 P2 C16 -68.2(6) . . . . ?
C20 N3 P3 C23 -119.8(3) . . . . ?
C21 N3 P3 C23 57.7(6) . . . . ?
C20 N3 P3 C27 122.4(3) . . . . ?
C21 N3 P3 C27 -60.1(6) . . . . ?
C20 N3 P3 Rh2 0.7(3) . . . . ?
C21 N3 P3 Rh2 178.2(6) . . . . ?
C25 C23 P3 N3 176.3(6) . . . . ?
C24 C23 P3 N3 59.7(5) . . . . ?
C26 C23 P3 N3 -59.2(5) . . . . ?
C25 C23 P3 C27 -73.6(6) . . . . ?
C24 C23 P3 C27 169.9(4) . . . . ?
C26 C23 P3 C27 51.0(5) . . . . ?
C25 C23 P3 Rh2 84.5(6) . . . . ?
C24 C23 P3 Rh2 -32.1(5) . . . . ?
C26 C23 P3 Rh2 -150.9(4) . . . . ?
C30 C27 P3 N3 -64.0(5) . . . . ?
C29 C27 P3 N3 56.2(5) . . . . ?
C28 C27 P3 N3 176.5(6) . . . . ?
C30 C27 P3 C23 -174.5(4) . . . . ?
C29 C27 P3 C23 -54.4(5) . . . . ?
C28 C27 P3 C23 66.0(7) . . . . ?
C30 C27 P3 Rh2 27.7(5) . . . . ?
C29 C27 P3 Rh2 147.9(4) . . . . ?
C28 C27 P3 Rh2 -91.8(6) . . . . ?
C20 N4 P4 C35 -126.6(5) . . . . ?
C22 N4 P4 C35 54.2(6) . . . . ?
C20 N4 P4 C31 119.7(5) . . . . ?
C22 N4 P4 C31 -59.6(6) . . . . ?
C36 C35 P4 N4 55.7(9) . . . . ?
C37 C35 P4 N4 -64.5(12) . . . . ?
C38 C35 P4 N4 166.1(10) . . . . ?
C36 C35 P4 C31 160.3(8) . . . . ?
C37 C35 P4 C31 40.1(12) . . . . ?
C38 C35 P4 C31 -89.3(11) . . . . ?

_refine_diff_density_max         1.543
_refine_diff_density_min         -1.248
_refine_diff_density_rms         0.120

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.000 0.000 543.0 58.5
_platon_squeeze_details          
;
 The residual electron density was assigned to a molecule of
 the pentane solvent [59/2 = 29 e per asymmetric unit; one molecule
 of C5H12 would give 42e].
;

_shelxl_version_number           2013-4

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
####################################################################### 
# 
# 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_pbpa140918
_database_code_depnum_ccdc_archive 'CCDC 1449236'
_audit_update_record             
;
2016-01-22 deposited with the CCDC.
2016-02-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C37 H38 B3 F15 N2 O3 P2, C7 H8'
_chemical_formula_sum            'C44 H46 B3 F15 N2 O3 P2'
_chemical_formula_weight         1030.20

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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                   11.9249(6)
_cell_length_b                   36.9050(17)
_cell_length_c                   13.6692(7)
_cell_angle_alpha                90
_cell_angle_beta                 102.6380(10)
_cell_angle_gamma                90
_cell_volume                     5869.9(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9982
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      26.83

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_F_000             2112
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    0.156
_shelx_estimated_absorpt_T_min   0.940
_shelx_estimated_absorpt_T_max   0.962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6731
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  triumph
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            58026
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.623
_diffrn_reflns_theta_max         28.047
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             14178
_reflns_number_gt                9041
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1067P)²+3.5135P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_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         14178
_refine_ls_number_parameters     591
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1126
_refine_ls_R_factor_gt           0.0748
_refine_ls_wR_factor_ref         0.2152
_refine_ls_wR_factor_gt          0.1998
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.000
_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 0.6089(2) 0.10860(7) 0.0481(2) 0.0269(5) Uani 1 1 d . . . . .
C2 C 0.5890(3) 0.10302(9) 0.2072(2) 0.0393(7) Uani 1 1 d . . . . .
H2 H 0.6026 0.0959 0.2756 0.047 Uiso 1 1 calc R U . . .
C3 C 0.5034(3) 0.12381(9) 0.1597(2) 0.0392(7) Uani 1 1 d . . . . .
H3 H 0.4449 0.1342 0.1881 0.047 Uiso 1 1 calc R U . . .
C4 C 0.8755(3) 0.09806(10) 0.2655(3) 0.0473(8) Uani 1 1 d . . . . .
C5 C 0.8441(4) 0.10575(15) 0.3643(4) 0.0910(10) Uani 1 1 d . . . . .
H5A H 0.8404 0.0829 0.4001 0.137 Uiso 1 1 calc R U . . .
H5B H 0.7692 0.1178 0.3523 0.137 Uiso 1 1 calc R U . . .
H5C H 0.9025 0.1215 0.4047 0.137 Uiso 1 1 calc R U . . .
C6 C 0.9941(4) 0.08181(16) 0.2839(4) 0.0910(10) Uani 1 1 d . . . . .
H6A H 1.0494 0.0986 0.3239 0.137 Uiso 1 1 calc R U . . .
H6B H 1.0152 0.0773 0.2196 0.137 Uiso 1 1 calc R U . . .
H6C H 0.9949 0.0589 0.3203 0.137 Uiso 1 1 calc R U . . .
C7 C 0.8688(4) 0.13557(15) 0.2125(4) 0.0910(10) Uani 1 1 d . . . . .
H7A H 0.7923 0.1460 0.2077 0.137 Uiso 1 1 calc R U . . .
H7B H 0.8830 0.1325 0.1450 0.137 Uiso 1 1 calc R U . . .
H7C H 0.9269 0.1518 0.2513 0.137 Uiso 1 1 calc R U . . .
C8 C 0.7363(3) 0.02639(8) 0.2285(2) 0.0417(7) Uani 1 1 d . . . . .
C9 C 0.8492(6) 0.00701(16) 0.2775(5) 0.0608(9) Uani 0.65 1 d . . P A 1
H9A H 0.8859 0.0198 0.3390 0.091 Uiso 0.65 1 calc R U P A 1
H9B H 0.9009 0.0069 0.2308 0.091 Uiso 0.65 1 calc R U P A 1
H9C H 0.8324 -0.0180 0.2939 0.091 Uiso 0.65 1 calc R U P A 1
C10 C 0.6618(6) 0.02893(16) 0.3049(5) 0.0608(9) Uani 0.65 1 d . . P A 1
H10A H 0.5828 0.0349 0.2707 0.091 Uiso 0.65 1 calc R U P A 1
H10B H 0.6917 0.0479 0.3537 0.091 Uiso 0.65 1 calc R U P A 1
H10C H 0.6626 0.0057 0.3395 0.091 Uiso 0.65 1 calc R U P A 1
C11 C 0.6752(6) 0.00379(16) 0.1388(5) 0.0608(9) Uani 0.65 1 d . . P A 1
H11A H 0.6603 -0.0206 0.1616 0.091 Uiso 0.65 1 calc R U P A 1
H11B H 0.7239 0.0021 0.0898 0.091 Uiso 0.65 1 calc R U P A 1
H11C H 0.6022 0.0154 0.1076 0.091 Uiso 0.65 1 calc R U P A 1
C9B C 0.8200(11) -0.0038(3) 0.2175(10) 0.0608(9) Uani 0.35 1 d . . P A 2
H9D H 0.8983 0.0034 0.2502 0.091 Uiso 0.35 1 calc R U P A 2
H9E H 0.8162 -0.0083 0.1462 0.091 Uiso 0.35 1 calc R U P A 2
H9F H 0.7994 -0.0260 0.2490 0.091 Uiso 0.35 1 calc R U P A 2
C10B C 0.7248(12) 0.0272(3) 0.3388(10) 0.0608(9) Uani 0.35 1 d . . P A 2
H10D H 0.6709 0.0463 0.3475 0.091 Uiso 0.35 1 calc R U P A 2
H10E H 0.8001 0.0320 0.3825 0.091 Uiso 0.35 1 calc R U P A 2
H10F H 0.6961 0.0037 0.3564 0.091 Uiso 0.35 1 calc R U P A 2
C11B C 0.6176(11) 0.0145(3) 0.1622(10) 0.0608(9) Uani 0.35 1 d . . P A 2
H11D H 0.6212 0.0154 0.0913 0.091 Uiso 0.35 1 calc R U P A 2
H11E H 0.5574 0.0310 0.1740 0.091 Uiso 0.35 1 calc R U P A 2
H11F H 0.6000 -0.0102 0.1799 0.091 Uiso 0.35 1 calc R U P A 2
C12 C 0.2819(2) 0.12782(9) -0.0410(2) 0.0385(7) Uani 1 1 d . . . . .
C13 C 0.3074(3) 0.08987(9) -0.0767(3) 0.0539(9) Uani 1 1 d . . . . .
H13A H 0.3586 0.0770 -0.0218 0.081 Uiso 1 1 calc R U . . .
H13B H 0.3444 0.0920 -0.1337 0.081 Uiso 1 1 calc R U . . .
H13C H 0.2353 0.0764 -0.0972 0.081 Uiso 1 1 calc R U . . .
C14 C 0.2287(3) 0.12379(13) 0.0491(3) 0.0656(11) Uani 1 1 d . . . . .
H14A H 0.2172 0.1478 0.0758 0.098 Uiso 1 1 calc R U . . .
H14B H 0.2799 0.1095 0.1008 0.098 Uiso 1 1 calc R U . . .
H14C H 0.1545 0.1114 0.0291 0.098 Uiso 1 1 calc R U . . .
C15 C 0.1956(3) 0.14598(11) -0.1265(3) 0.0557(9) Uani 1 1 d . . . . .
H15A H 0.1266 0.1309 -0.1449 0.084 Uiso 1 1 calc R U . . .
H15B H 0.2303 0.1489 -0.1846 0.084 Uiso 1 1 calc R U . . .
H15C H 0.1745 0.1698 -0.1044 0.084 Uiso 1 1 calc R U . . .
C16 C 0.4199(3) 0.19887(8) 0.0331(3) 0.0444(8) Uani 1 1 d . . . . .
C17 C 0.3682(4) 0.22458(10) -0.0553(4) 0.0692(12) Uani 1 1 d . . . . .
H17A H 0.2902 0.2166 -0.0865 0.104 Uiso 1 1 calc R U . . .
H17B H 0.4161 0.2240 -0.1050 0.104 Uiso 1 1 calc R U . . .
H17C H 0.3655 0.2493 -0.0300 0.104 Uiso 1 1 calc R U . . .
C18 C 0.5450(3) 0.20932(11) 0.0706(4) 0.0655(11) Uani 1 1 d . . . . .
H18A H 0.5495 0.2338 0.0988 0.098 Uiso 1 1 calc R U . . .
H18B H 0.5843 0.2087 0.0147 0.098 Uiso 1 1 calc R U . . .
H18C H 0.5819 0.1922 0.1225 0.098 Uiso 1 1 calc R U . . .
C19 C 0.3496(5) 0.20415(11) 0.1105(4) 0.0839(16) Uani 1 1 d . . . . .
H19A H 0.2696 0.1974 0.0820 0.126 Uiso 1 1 calc R U . . .
H19B H 0.3530 0.2296 0.1311 0.126 Uiso 1 1 calc R U . . .
H19C H 0.3802 0.1889 0.1688 0.126 Uiso 1 1 calc R U . . .
C20 C 0.4307(2) 0.13587(8) -0.2966(2) 0.0300(6) Uani 1 1 d . . . . .
C21 C 0.3741(3) 0.10430(8) -0.3337(2) 0.0367(7) Uani 1 1 d . . . . .
C22 C 0.2719(3) 0.10418(9) -0.4048(2) 0.0441(8) Uani 1 1 d . . . . .
C23 C 0.2230(3) 0.13622(10) -0.4426(2) 0.0437(8) Uani 1 1 d . . . . .
C24 C 0.2763(3) 0.16790(9) -0.4096(2) 0.0415(7) Uani 1 1 d . . . . .
C25 C 0.3777(2) 0.16760(8) -0.3375(2) 0.0342(6) Uani 1 1 d . . . . .
C26 C 0.7789(2) 0.20422(8) -0.1103(2) 0.0323(6) Uani 1 1 d . . . . .
C27 C 0.7286(2) 0.23783(8) -0.1375(2) 0.0371(7) Uani 1 1 d . . . . .
C28 C 0.7905(3) 0.26984(8) -0.1299(2) 0.0419(7) Uani 1 1 d . . . . .
C29 C 0.9069(3) 0.26878(9) -0.0962(2) 0.0430(8) Uani 1 1 d . . . . .
C30 C 0.9616(3) 0.23632(9) -0.0702(3) 0.0431(8) Uani 1 1 d . . . . .
C31 C 0.8968(3) 0.20497(9) -0.0763(2) 0.0390(7) Uani 1 1 d . . . . .
C32 C 0.7365(2) 0.07243(8) -0.0683(2) 0.0319(6) Uani 1 1 d . . . . .
C33 C 0.8538(3) 0.07156(9) -0.0683(2) 0.0425(7) Uani 1 1 d . . . . .
C34 C 0.9072(3) 0.04056(11) -0.0894(3) 0.0566(10) Uani 1 1 d . . . . .
C35 C 0.8493(4) 0.00981(11) -0.1122(3) 0.0611(11) Uani 1 1 d . . . . .
C36 C 0.7334(4) 0.00886(9) -0.1139(3) 0.0557(10) Uani 1 1 d . . . . .
C37 C 0.6808(3) 0.03987(9) -0.0913(2) 0.0425(7) Uani 1 1 d . . . . .
C38 C 0.5680(8) 0.1746(3) 0.4913(6) 0.184(5) Uani 1 1 d . . . . .
H38A H 0.5466 0.1816 0.5539 0.275 Uiso 1 1 calc R U . . .
H38B H 0.5668 0.1960 0.4486 0.275 Uiso 1 1 calc R U . . .
H38C H 0.6454 0.1641 0.5065 0.275 Uiso 1 1 calc R U . . .
C39 C 0.4862(5) 0.1477(2) 0.4389(4) 0.0980(8) Uani 1 1 d . . . . .
C40 C 0.5072(5) 0.11187(19) 0.4478(4) 0.0980(8) Uani 1 1 d . . . . .
H40 H 0.5776 0.1038 0.4888 0.118 Uiso 1 1 calc R U . . .
C41 C 0.4305(5) 0.0869(2) 0.3998(4) 0.0980(8) Uani 1 1 d . . . . .
H41 H 0.4487 0.0618 0.4065 0.118 Uiso 1 1 calc R U . . .
C42 C 0.3287(5) 0.09759(19) 0.3427(4) 0.0980(8) Uani 1 1 d . . . . .
H42 H 0.2751 0.0800 0.3099 0.118 Uiso 1 1 calc R U . . .
C43 C 0.3016(5) 0.13480(18) 0.3318(4) 0.0980(8) Uani 1 1 d . . . . .
H43 H 0.2301 0.1424 0.2915 0.118 Uiso 1 1 calc R U . . .
C44 C 0.3781(5) 0.15979(19) 0.3792(4) 0.0980(8) Uani 1 1 d . . . . .
H44 H 0.3605 0.1849 0.3730 0.118 Uiso 1 1 calc R U . . .
B1 B 0.6611(3) 0.10871(8) -0.0557(2) 0.0279(6) Uani 1 1 d . . . . .
B2 B 0.5422(3) 0.13599(9) -0.2080(2) 0.0295(6) Uani 1 1 d . . . . .
B3 B 0.7052(3) 0.16812(9) -0.1205(2) 0.0287(6) Uani 1 1 d . . . . .
N1 N 0.65540(19) 0.09356(6) 0.13882(17) 0.0311(5) Uani 1 1 d . . . . .
N2 N 0.51437(18) 0.12763(6) 0.06157(17) 0.0283(5) Uani 1 1 d . . . . .
F1 F 0.41702(18) 0.07203(5) -0.30147(15) 0.0547(5) Uani 1 1 d . . . . .
F2 F 0.2210(2) 0.07258(6) -0.43860(18) 0.0698(7) Uani 1 1 d . . . . .
F3 F 0.12469(17) 0.13623(7) -0.51193(16) 0.0662(6) Uani 1 1 d . . . . .
F4 F 0.23079(17) 0.19955(6) -0.44834(16) 0.0600(6) Uani 1 1 d . . . . .
F5 F 0.42349(16) 0.20004(5) -0.30734(15) 0.0512(5) Uani 1 1 d . . . . .
F6 F 0.61352(15) 0.24057(5) -0.17066(17) 0.0543(5) Uani 1 1 d . . . . .
F7 F 0.7373(2) 0.30136(5) -0.1562(2) 0.0679(7) Uani 1 1 d . . . . .
F8 F 0.96871(19) 0.29962(6) -0.08915(18) 0.0633(6) Uani 1 1 d . . . . .
F9 F 1.07580(16) 0.23506(6) -0.03881(18) 0.0647(6) Uani 1 1 d . . . . .
F10 F 0.95393(15) 0.17420(5) -0.05005(18) 0.0604(6) Uani 1 1 d . . . . .
F11 F 0.91965(16) 0.10085(6) -0.0448(2) 0.0651(6) Uani 1 1 d . . . . .
F12 F 1.0213(2) 0.04139(8) -0.0890(2) 0.0907(9) Uani 1 1 d . . . . .
F13 F 0.9013(3) -0.02078(7) -0.1355(2) 0.0970(10) Uani 1 1 d . . . . .
F14 F 0.6723(3) -0.02235(6) -0.1359(2) 0.0867(8) Uani 1 1 d . . . . .
F15 F 0.56763(17) 0.03725(5) -0.08984(17) 0.0560(5) Uani 1 1 d . . . . .
P1 P 0.78512(6) 0.06780(2) 0.16955(5) 0.02840(17) Uani 1 1 d . . . . .
P2 P 0.42023(6) 0.15381(2) -0.03159(6) 0.02915(17) Uani 1 1 d . . . . .
O1 O 0.56316(15) 0.10859(5) -0.14436(14) 0.0286(4) Uani 1 1 d . . . . .
O2 O 0.61600(17) 0.16512(6) -0.20324(15) 0.0389(5) Uani 1 1 d . . . . .
O3 O 0.72896(15) 0.14230(5) -0.05001(14) 0.0307(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 N1 1.361(3) . ?
C1 N2 1.374(3) . ?
C1 B1 1.670(4) . ?
C2 C3 1.328(4) . ?
C2 N1 1.395(4) . ?
C2 H2 0.9500 . ?
C3 N2 1.383(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.505(6) . ?
C4 C6 1.506(6) . ?
C4 C7 1.557(7) . ?
C4 P1 1.874(3) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C10 1.514(8) . ?
C8 C9B 1.526(12) . ?
C8 C11 1.529(7) . ?
C8 C9 1.542(7) . ?
C8 C10B 1.544(13) . ?
C8 C11B 1.566(13) . ?
C8 P1 1.879(3) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C9B H9D 0.9800 . ?
C9B H9E 0.9800 . ?
C9B H9F 0.9800 . ?
C10B H10D 0.9800 . ?
C10B H10E 0.9800 . ?
C10B H10F 0.9800 . ?
C11B H11D 0.9800 . ?
C11B H11E 0.9800 . ?
C11B H11F 0.9800 . ?
C12 C14 1.512(5) . ?
C12 C15 1.532(4) . ?
C12 C13 1.535(5) . ?
C12 P2 1.888(3) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C19 1.500(5) . ?
C16 C18 1.516(5) . ?
C16 C17 1.553(5) . ?
C16 P2 1.884(3) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.386(4) . ?
C20 C25 1.388(4) . ?
C20 B2 1.590(4) . ?
C21 F1 1.333(3) . ?
C21 C22 1.382(4) . ?
C22 F2 1.349(4) . ?
C22 C23 1.369(5) . ?
C23 F3 1.337(3) . ?
C23 C24 1.360(5) . ?
C24 F4 1.347(4) . ?
C24 C25 1.383(4) . ?
C25 F5 1.342(3) . ?
C26 C31 1.381(4) . ?
C26 C27 1.393(4) . ?
C26 B3 1.586(4) . ?
C27 F6 1.351(3) . ?
C27 C28 1.385(4) . ?
C28 F7 1.336(4) . ?
C28 C29 1.364(5) . ?
C29 F8 1.348(3) . ?
C29 C30 1.373(5) . ?
C30 F9 1.337(3) . ?
C30 C31 1.383(4) . ?
C31 F10 1.332(4) . ?
C32 C37 1.376(4) . ?
C32 C33 1.399(4) . ?
C32 B1 1.643(4) . ?
C33 F11 1.334(4) . ?
C33 C34 1.370(5) . ?
C34 C35 1.329(6) . ?
C34 F12 1.359(4) . ?
C35 F13 1.358(4) . ?
C35 C36 1.378(6) . ?
C36 F14 1.361(5) . ?
C36 C37 1.372(5) . ?
C37 F15 1.358(4) . ?
C38 C39 1.464(9) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C40 1.347(9) . ?
C39 C44 1.437(8) . ?
C40 C41 1.362(8) . ?
C40 H40 0.9500 . ?
C41 C42 1.351(8) . ?
C41 H41 0.9500 . ?
C42 C43 1.411(8) . ?
C42 H42 0.9500 . ?
C43 C44 1.358(8) . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
B1 O3 1.473(4) . ?
B1 O1 1.488(3) . ?
B2 O1 1.321(4) . ?
B2 O2 1.382(4) . ?
B3 O3 1.341(4) . ?
B3 O2 1.377(4) . ?
N1 P1 1.786(2) . ?
N2 P2 1.786(2) . ?

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 N2 105.6(2) . . ?
N1 C1 B1 128.5(2) . . ?
N2 C1 B1 125.6(2) . . ?
C3 C2 N1 107.8(3) . . ?
C3 C2 H2 126.1 . . ?
N1 C2 H2 126.1 . . ?
C2 C3 N2 107.9(3) . . ?
C2 C3 H3 126.0 . . ?
N2 C3 H3 126.0 . . ?
C5 C4 C6 109.5(4) . . ?
C5 C4 C7 104.6(4) . . ?
C6 C4 C7 112.5(4) . . ?
C5 C4 P1 121.5(3) . . ?
C6 C4 P1 104.8(3) . . ?
C7 C4 P1 103.9(2) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C10 C8 C11 109.8(4) . . ?
C10 C8 C9 108.5(4) . . ?
C11 C8 C9 108.2(4) . . ?
C9B C8 C10B 108.1(7) . . ?
C9B C8 C11B 105.5(7) . . ?
C10B C8 C11B 108.0(7) . . ?
C10 C8 P1 121.9(3) . . ?
C9B C8 P1 106.3(5) . . ?
C11 C8 P1 103.8(3) . . ?
C9 C8 P1 103.9(3) . . ?
C10B C8 P1 120.4(5) . . ?
C11B C8 P1 107.8(4) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C8 C9B H9D 109.5 . . ?
C8 C9B H9E 109.5 . . ?
H9D C9B H9E 109.5 . . ?
C8 C9B H9F 109.5 . . ?
H9D C9B H9F 109.5 . . ?
H9E C9B H9F 109.5 . . ?
C8 C10B H10D 109.5 . . ?
C8 C10B H10E 109.5 . . ?
H10D C10B H10E 109.5 . . ?
C8 C10B H10F 109.5 . . ?
H10D C10B H10F 109.5 . . ?
H10E C10B H10F 109.5 . . ?
C8 C11B H11D 109.5 . . ?
C8 C11B H11E 109.5 . . ?
H11D C11B H11E 109.5 . . ?
C8 C11B H11F 109.5 . . ?
H11D C11B H11F 109.5 . . ?
H11E C11B H11F 109.5 . . ?
C14 C12 C15 109.4(3) . . ?
C14 C12 C13 108.4(3) . . ?
C15 C12 C13 107.7(3) . . ?
C14 C12 P2 120.7(2) . . ?
C15 C12 P2 105.1(2) . . ?
C13 C12 P2 104.8(2) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C19 C16 C18 112.9(4) . . ?
C19 C16 C17 106.3(3) . . ?
C18 C16 C17 107.6(3) . . ?
C19 C16 P2 120.3(3) . . ?
C18 C16 P2 106.3(2) . . ?
C17 C16 P2 102.5(3) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 C25 114.8(2) . . ?
C21 C20 B2 122.7(3) . . ?
C25 C20 B2 122.3(3) . . ?
F1 C21 C22 116.4(3) . . ?
F1 C21 C20 120.6(3) . . ?
C22 C21 C20 123.0(3) . . ?
F2 C22 C23 119.7(3) . . ?
F2 C22 C21 120.3(3) . . ?
C23 C22 C21 120.0(3) . . ?
F3 C23 C24 120.6(3) . . ?
F3 C23 C22 120.2(3) . . ?
C24 C23 C22 119.2(3) . . ?
F4 C24 C23 119.8(3) . . ?
F4 C24 C25 120.1(3) . . ?
C23 C24 C25 120.1(3) . . ?
F5 C25 C24 116.4(3) . . ?
F5 C25 C20 120.7(2) . . ?
C24 C25 C20 122.9(3) . . ?
C31 C26 C27 114.8(3) . . ?
C31 C26 B3 123.4(3) . . ?
C27 C26 B3 121.7(2) . . ?
F6 C27 C28 116.6(3) . . ?
F6 C27 C26 120.2(3) . . ?
C28 C27 C26 123.2(3) . . ?
F7 C28 C29 120.2(3) . . ?
F7 C28 C27 120.6(3) . . ?
C29 C28 C27 119.2(3) . . ?
F8 C29 C28 120.0(3) . . ?
F8 C29 C30 119.8(3) . . ?
C28 C29 C30 120.2(3) . . ?
F9 C30 C29 120.4(3) . . ?
F9 C30 C31 120.4(3) . . ?
C29 C30 C31 119.2(3) . . ?
F10 C31 C26 119.8(3) . . ?
F10 C31 C30 116.8(3) . . ?
C26 C31 C30 123.4(3) . . ?
C37 C32 C33 114.4(3) . . ?
C37 C32 B1 119.2(2) . . ?
C33 C32 B1 126.1(3) . . ?
F11 C33 C34 116.8(3) . . ?
F11 C33 C32 121.2(3) . . ?
C34 C33 C32 122.0(3) . . ?
C35 C34 F12 119.2(3) . . ?
C35 C34 C33 121.4(4) . . ?
F12 C34 C33 119.4(4) . . ?
C34 C35 F13 121.6(4) . . ?
C34 C35 C36 119.6(3) . . ?
F13 C35 C36 118.8(4) . . ?
F14 C36 C37 120.4(4) . . ?
F14 C36 C35 120.8(3) . . ?
C37 C36 C35 118.7(4) . . ?
F15 C37 C36 116.6(3) . . ?
F15 C37 C32 119.4(3) . . ?
C36 C37 C32 124.0(3) . . ?
C39 C38 H38A 109.5 . . ?
C39 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C39 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C40 C39 C44 118.8(7) . . ?
C40 C39 C38 122.0(8) . . ?
C44 C39 C38 119.1(8) . . ?
C39 C40 C41 122.0(7) . . ?
C39 C40 H40 119.0 . . ?
C41 C40 H40 119.0 . . ?
C42 C41 C40 120.2(7) . . ?
C42 C41 H41 119.9 . . ?
C40 C41 H41 119.9 . . ?
C41 C42 C43 120.1(7) . . ?
C41 C42 H42 119.9 . . ?
C43 C42 H42 119.9 . . ?
C44 C43 C42 119.7(7) . . ?
C44 C43 H43 120.1 . . ?
C42 C43 H43 120.1 . . ?
C43 C44 C39 119.1(7) . . ?
C43 C44 H44 120.5 . . ?
C39 C44 H44 120.5 . . ?
O3 B1 O1 111.7(2) . . ?
O3 B1 C32 112.6(2) . . ?
O1 B1 C32 105.2(2) . . ?
O3 B1 C1 105.0(2) . . ?
O1 B1 C1 108.6(2) . . ?
C32 B1 C1 113.7(2) . . ?
O1 B2 O2 122.5(2) . . ?
O1 B2 C20 120.4(3) . . ?
O2 B2 C20 117.1(2) . . ?
O3 B3 O2 122.5(3) . . ?
O3 B3 C26 120.5(2) . . ?
O2 B3 C26 117.0(2) . . ?
C1 N1 C2 109.3(2) . . ?
C1 N1 P1 126.20(19) . . ?
C2 N1 P1 124.39(19) . . ?
C1 N2 C3 109.4(2) . . ?
C1 N2 P2 125.92(19) . . ?
C3 N2 P2 124.65(19) . . ?
N1 P1 C4 100.58(14) . . ?
N1 P1 C8 101.53(13) . . ?
C4 P1 C8 111.68(15) . . ?
N2 P2 C16 102.03(14) . . ?
N2 P2 C12 100.21(12) . . ?
C16 P2 C12 112.92(14) . . ?
B2 O1 B1 122.4(2) . . ?
B3 O2 B2 118.1(2) . . ?
B3 O3 B1 122.2(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
N1 C2 C3 N2 0.2(4) . . . . ?
C25 C20 C21 F1 179.1(3) . . . . ?
B2 C20 C21 F1 -5.5(5) . . . . ?
C25 C20 C21 C22 -1.0(5) . . . . ?
B2 C20 C21 C22 174.4(3) . . . . ?
F1 C21 C22 F2 -0.5(5) . . . . ?
C20 C21 C22 F2 179.6(3) . . . . ?
F1 C21 C22 C23 -179.2(3) . . . . ?
C20 C21 C22 C23 0.9(5) . . . . ?
F2 C22 C23 F3 0.7(5) . . . . ?
C21 C22 C23 F3 179.4(3) . . . . ?
F2 C22 C23 C24 -178.6(3) . . . . ?
C21 C22 C23 C24 0.1(5) . . . . ?
F3 C23 C24 F4 -1.2(5) . . . . ?
C22 C23 C24 F4 178.1(3) . . . . ?
F3 C23 C24 C25 179.7(3) . . . . ?
C22 C23 C24 C25 -1.0(5) . . . . ?
F4 C24 C25 F5 2.3(5) . . . . ?
C23 C24 C25 F5 -178.6(3) . . . . ?
F4 C24 C25 C20 -178.1(3) . . . . ?
C23 C24 C25 C20 0.9(5) . . . . ?
C21 C20 C25 F5 179.6(3) . . . . ?
B2 C20 C25 F5 4.2(4) . . . . ?
C21 C20 C25 C24 0.0(4) . . . . ?
B2 C20 C25 C24 -175.3(3) . . . . ?
C31 C26 C27 F6 -179.1(3) . . . . ?
B3 C26 C27 F6 2.2(5) . . . . ?
C31 C26 C27 C28 -1.1(5) . . . . ?
B3 C26 C27 C28 -179.8(3) . . . . ?
F6 C27 C28 F7 -1.3(5) . . . . ?
C26 C27 C28 F7 -179.4(3) . . . . ?
F6 C27 C28 C29 179.6(3) . . . . ?
C26 C27 C28 C29 1.5(5) . . . . ?
F7 C28 C29 F8 0.2(5) . . . . ?
C27 C28 C29 F8 179.4(3) . . . . ?
F7 C28 C29 C30 -179.3(3) . . . . ?
C27 C28 C29 C30 -0.1(5) . . . . ?
F8 C29 C30 F9 -0.6(5) . . . . ?
C28 C29 C30 F9 178.9(3) . . . . ?
F8 C29 C30 C31 179.0(3) . . . . ?
C28 C29 C30 C31 -1.5(5) . . . . ?
C27 C26 C31 F10 -178.8(3) . . . . ?
B3 C26 C31 F10 -0.1(5) . . . . ?
C27 C26 C31 C30 -0.6(5) . . . . ?
B3 C26 C31 C30 178.0(3) . . . . ?
F9 C30 C31 F10 -0.3(5) . . . . ?
C29 C30 C31 F10 -179.8(3) . . . . ?
F9 C30 C31 C26 -178.5(3) . . . . ?
C29 C30 C31 C26 2.0(5) . . . . ?
C37 C32 C33 F11 -178.3(3) . . . . ?
B1 C32 C33 F11 8.7(5) . . . . ?
C37 C32 C33 C34 -0.1(5) . . . . ?
B1 C32 C33 C34 -173.2(3) . . . . ?
F11 C33 C34 C35 179.0(4) . . . . ?
C32 C33 C34 C35 0.8(6) . . . . ?
F11 C33 C34 F12 -2.3(5) . . . . ?
C32 C33 C34 F12 179.5(3) . . . . ?
F12 C34 C35 F13 -0.3(6) . . . . ?
C33 C34 C35 F13 178.4(4) . . . . ?
F12 C34 C35 C36 -179.2(4) . . . . ?
C33 C34 C35 C36 -0.5(6) . . . . ?
C34 C35 C36 F14 -179.3(4) . . . . ?
F13 C35 C36 F14 1.7(6) . . . . ?
C34 C35 C36 C37 -0.3(6) . . . . ?
F13 C35 C36 C37 -179.3(3) . . . . ?
F14 C36 C37 F15 1.7(5) . . . . ?
C35 C36 C37 F15 -177.3(3) . . . . ?
F14 C36 C37 C32 -180.0(3) . . . . ?
C35 C36 C37 C32 1.0(6) . . . . ?
C33 C32 C37 F15 177.5(3) . . . . ?
B1 C32 C37 F15 -8.9(4) . . . . ?
C33 C32 C37 C36 -0.8(5) . . . . ?
B1 C32 C37 C36 172.8(3) . . . . ?
C44 C39 C40 C41 1.9(8) . . . . ?
C38 C39 C40 C41 179.4(5) . . . . ?
C39 C40 C41 C42 -1.4(8) . . . . ?
C40 C41 C42 C43 0.6(7) . . . . ?
C41 C42 C43 C44 -0.3(7) . . . . ?
C42 C43 C44 C39 0.7(7) . . . . ?
C40 C39 C44 C43 -1.5(7) . . . . ?
C38 C39 C44 C43 -179.1(5) . . . . ?
C37 C32 B1 O3 -169.2(3) . . . . ?
C33 C32 B1 O3 3.5(4) . . . . ?
C37 C32 B1 O1 -47.3(3) . . . . ?
C33 C32 B1 O1 125.5(3) . . . . ?
C37 C32 B1 C1 71.4(3) . . . . ?
C33 C32 B1 C1 -115.8(3) . . . . ?
N1 C1 B1 O3 -91.8(3) . . . . ?
N2 C1 B1 O3 80.4(3) . . . . ?
N1 C1 B1 O1 148.5(3) . . . . ?
N2 C1 B1 O1 -39.3(3) . . . . ?
N1 C1 B1 C32 31.7(4) . . . . ?
N2 C1 B1 C32 -156.1(2) . . . . ?
C21 C20 B2 O1 -23.0(4) . . . . ?
C25 C20 B2 O1 152.0(3) . . . . ?
C21 C20 B2 O2 155.0(3) . . . . ?
C25 C20 B2 O2 -30.0(4) . . . . ?
C31 C26 B3 O3 40.5(4) . . . . ?
C27 C26 B3 O3 -140.9(3) . . . . ?
C31 C26 B3 O2 -140.6(3) . . . . ?
C27 C26 B3 O2 38.0(4) . . . . ?
N2 C1 N1 C2 0.6(3) . . . . ?
B1 C1 N1 C2 174.0(3) . . . . ?
N2 C1 N1 P1 -176.15(18) . . . . ?
B1 C1 N1 P1 -2.7(4) . . . . ?
C3 C2 N1 C1 -0.5(4) . . . . ?
C3 C2 N1 P1 176.3(2) . . . . ?
N1 C1 N2 C3 -0.5(3) . . . . ?
B1 C1 N2 C3 -174.2(3) . . . . ?
N1 C1 N2 P2 178.80(18) . . . . ?
B1 C1 N2 P2 5.1(4) . . . . ?
C2 C3 N2 C1 0.2(4) . . . . ?
C2 C3 N2 P2 -179.1(2) . . . . ?
C1 N1 P1 C4 115.7(2) . . . . ?
C2 N1 P1 C4 -60.6(3) . . . . ?
C1 N1 P1 C8 -129.4(2) . . . . ?
C2 N1 P1 C8 54.3(3) . . . . ?
C5 C4 P1 N1 64.7(4) . . . . ?
C6 C4 P1 N1 -170.8(3) . . . . ?
C7 C4 P1 N1 -52.5(3) . . . . ?
C5 C4 P1 C8 -42.3(4) . . . . ?
C6 C4 P1 C8 82.2(3) . . . . ?
C7 C4 P1 C8 -159.5(3) . . . . ?
C10 C8 P1 N1 -45.3(4) . . . . ?
C9B C8 P1 N1 156.4(5) . . . . ?
C11 C8 P1 N1 79.0(3) . . . . ?
C9 C8 P1 N1 -167.9(3) . . . . ?
C10B C8 P1 N1 -80.6(6) . . . . ?
C11B C8 P1 N1 43.7(6) . . . . ?
C10 C8 P1 C4 61.2(4) . . . . ?
C9B C8 P1 C4 -97.2(6) . . . . ?
C11 C8 P1 C4 -174.6(3) . . . . ?
C9 C8 P1 C4 -61.5(4) . . . . ?
C10B C8 P1 C4 25.9(6) . . . . ?
C11B C8 P1 C4 150.1(6) . . . . ?
C1 N2 P2 C16 -127.1(2) . . . . ?
C3 N2 P2 C16 52.1(3) . . . . ?
C1 N2 P2 C12 116.6(2) . . . . ?
C3 N2 P2 C12 -64.2(3) . . . . ?
C19 C16 P2 N2 -77.9(4) . . . . ?
C18 C16 P2 N2 51.8(3) . . . . ?
C17 C16 P2 N2 164.6(2) . . . . ?
C19 C16 P2 C12 28.7(4) . . . . ?
C18 C16 P2 C12 158.5(3) . . . . ?
C17 C16 P2 C12 -88.8(3) . . . . ?
C14 C12 P2 N2 60.7(3) . . . . ?
C15 C12 P2 N2 -175.2(2) . . . . ?
C13 C12 P2 N2 -61.8(2) . . . . ?
C14 C12 P2 C16 -47.1(3) . . . . ?
C15 C12 P2 C16 77.0(3) . . . . ?
C13 C12 P2 C16 -169.6(2) . . . . ?
O2 B2 O1 B1 6.9(4) . . . . ?
C20 B2 O1 B1 -175.1(2) . . . . ?
O3 B1 O1 B2 -0.5(3) . . . . ?
C32 B1 O1 B2 -123.0(3) . . . . ?
C1 B1 O1 B2 115.0(3) . . . . ?
O3 B3 O2 B2 6.4(4) . . . . ?
C26 B3 O2 B2 -172.5(3) . . . . ?
O1 B2 O2 B3 -9.9(4) . . . . ?
C20 B2 O2 B3 172.1(3) . . . . ?
O2 B3 O3 B1 -0.1(4) . . . . ?
C26 B3 O3 B1 178.8(2) . . . . ?
O1 B1 O3 B3 -2.9(3) . . . . ?
C32 B1 O3 B3 115.3(3) . . . . ?
C1 B1 O3 B3 -120.5(3) . . . . ?

_refine_diff_density_max         0.861
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.065

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.007 0.000 0.500 730.5 197.7
2 -0.089 0.500 0.000 730.4 197.7
_platon_squeeze_details          
;
The residual electron density was assigned to two molecules of 
the toluene solvent [395/4 = 99 e per asymmetric unit; two  
molecules of C7H8 would give 100 e]. 
;

_shelxl_version_number           2013-4

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
####################################################################### 
# 
# 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_pbpa140925_02
_database_code_depnum_ccdc_archive 'CCDC 1449237'
_audit_update_record             
;
2016-01-22 deposited with the CCDC.
2016-02-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H40 N4 O2 P2 Rh2'
_chemical_formula_sum            'C24 H40 N4 O2 P2 Rh2'
_chemical_formula_weight         684.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_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+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   15.9082(5)
_cell_length_b                   14.5038(3)
_cell_length_c                   25.3341(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5845.3(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    52490
_cell_measurement_theta_min      0.998
_cell_measurement_theta_max      27.485

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_F_000             2784
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    1.265
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.78113
_exptl_absorpt_correction_T_max  0.87136
_exptl_absorpt_process_details   'MULscanABS in PLATON (Spek, 2003)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            34869
_diffrn_reflns_av_unetI/netI     0.1029
_diffrn_reflns_av_R_equivalents  0.1222
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.608
_diffrn_reflns_theta_max         27.451
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             6627
_reflns_number_gt                4786
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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       'Collect (Nonius B.V., 1998)'
_computing_cell_refinement       'Denzo (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo (Nonius B.V., 1998)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'PLATON 98 (Spek, 1998)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0653P)²+43.4863P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_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         6627
_refine_ls_number_parameters     295
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1534
_refine_ls_R_factor_gt           0.1022
_refine_ls_wR_factor_ref         0.2130
_refine_ls_wR_factor_gt          0.1914
_refine_ls_goodness_of_fit_ref   1.289
_refine_ls_restrained_S_all      1.289
_refine_ls_shift/su_max          0.000
_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 0.9339(6) 0.3462(7) 0.3323(4) 0.031(2) Uani 1 1 d . . . . .
C2 C 1.0196(7) 0.2239(8) 0.3263(5) 0.044(3) Uani 1 1 d . . . . .
H2 H 1.0575 0.1789 0.3131 0.053 Uiso 1 1 calc R U . . .
C3 C 0.9865(7) 0.2280(7) 0.3750(5) 0.041(3) Uani 1 1 d . . . . .
H3 H 0.9971 0.1851 0.4025 0.049 Uiso 1 1 calc R U . . .
C4 C 1.0727(7) 0.3937(8) 0.2174(5) 0.044(3) Uani 1 1 d . . . . .
C5 C 1.1044(8) 0.4603(10) 0.2588(7) 0.080(3) Uani 1 1 d . . . . .
H5A H 1.1173 0.4265 0.2913 0.120 Uiso 1 1 calc R U . . .
H5B H 1.0612 0.5067 0.2660 0.120 Uiso 1 1 calc R U . . .
H5C H 1.1554 0.4908 0.2459 0.120 Uiso 1 1 calc R U . . .
C6 C 1.0570(9) 0.4460(10) 0.1643(7) 0.080(3) Uani 1 1 d . . . . .
H6A H 1.0095 0.4884 0.1685 0.120 Uiso 1 1 calc R U . . .
H6B H 1.0442 0.4014 0.1363 0.120 Uiso 1 1 calc R U . . .
H6C H 1.1074 0.4810 0.1547 0.120 Uiso 1 1 calc R U . . .
C7 C 1.1390(8) 0.3187(10) 0.2079(7) 0.080(3) Uani 1 1 d . . . . .
H7A H 1.1944 0.3474 0.2042 0.120 Uiso 1 1 calc R U . . .
H7B H 1.1252 0.2848 0.1756 0.120 Uiso 1 1 calc R U . . .
H7C H 1.1396 0.2761 0.2379 0.120 Uiso 1 1 calc R U . . .
C8 C 0.9196(7) 0.2661(7) 0.1971(4) 0.033(2) Uani 1 1 d . . . . .
C9 C 0.8767(11) 0.3138(10) 0.1511(6) 0.086(6) Uani 1 1 d . . . . .
H9A H 0.9192 0.3417 0.1282 0.129 Uiso 1 1 calc R U . . .
H9B H 0.8391 0.3619 0.1646 0.129 Uiso 1 1 calc R U . . .
H9C H 0.8440 0.2686 0.1310 0.129 Uiso 1 1 calc R U . . .
C10 C 0.9774(8) 0.1912(8) 0.1765(5) 0.054(3) Uani 1 1 d . . . . .
H10A H 1.0113 0.2156 0.1474 0.081 Uiso 1 1 calc R U . . .
H10B H 0.9437 0.1391 0.1639 0.081 Uiso 1 1 calc R U . . .
H10C H 1.0146 0.1704 0.2050 0.081 Uiso 1 1 calc R U . . .
C11 C 0.8505(8) 0.2195(9) 0.2307(6) 0.061(4) Uani 1 1 d . . . . .
H11A H 0.8180 0.1772 0.2085 0.092 Uiso 1 1 calc R U . . .
H11B H 0.8130 0.2668 0.2452 0.092 Uiso 1 1 calc R U . . .
H11C H 0.8766 0.1850 0.2596 0.092 Uiso 1 1 calc R U . . .
C12 C 0.8167(6) 0.4658(6) 0.3960(4) 0.026(2) Uani 1 1 d . . . . .
C13 C 0.7395(6) 0.5948(7) 0.4046(4) 0.032(2) Uani 1 1 d . . . . .
H13 H 0.7056 0.6425 0.4190 0.039 Uiso 1 1 calc R U . . .
C14 C 0.7699(6) 0.5875(6) 0.3540(4) 0.029(2) Uani 1 1 d . . . . .
H14 H 0.7597 0.6306 0.3266 0.035 Uiso 1 1 calc R U . . .
C15 C 0.6804(7) 0.4209(10) 0.5115(5) 0.054(3) Uani 1 1 d . . . . .
C16 C 0.6509(9) 0.3484(10) 0.4724(7) 0.077(5) Uani 1 1 d . . . . .
H16A H 0.5949 0.3267 0.4825 0.115 Uiso 1 1 calc R U . . .
H16B H 0.6903 0.2965 0.4725 0.115 Uiso 1 1 calc R U . . .
H16C H 0.6486 0.3754 0.4370 0.115 Uiso 1 1 calc R U . . .
C17 C 0.6918(10) 0.3774(14) 0.5663(6) 0.096(6) Uani 1 1 d . . . . .
H17A H 0.7029 0.4259 0.5922 0.144 Uiso 1 1 calc R U . . .
H17B H 0.7393 0.3343 0.5654 0.144 Uiso 1 1 calc R U . . .
H17C H 0.6405 0.3441 0.5761 0.144 Uiso 1 1 calc R U . . .
C18 C 0.6157(8) 0.4998(12) 0.5127(7) 0.084(5) Uani 1 1 d . . . . .
H18A H 0.6105 0.5266 0.4774 0.126 Uiso 1 1 calc R U . . .
H18B H 0.6345 0.5473 0.5376 0.126 Uiso 1 1 calc R U . . .
H18C H 0.5611 0.4756 0.5240 0.126 Uiso 1 1 calc R U . . .
C19 C 0.8384(7) 0.5401(8) 0.5339(4) 0.041(3) Uani 1 1 d . . . . .
C20 C 0.8828(9) 0.4834(10) 0.5771(5) 0.063(2) Uani 1 1 d . . . . .
H20A H 0.9175 0.5243 0.5988 0.095 Uiso 1 1 calc R U . . .
H20B H 0.9186 0.4366 0.5605 0.095 Uiso 1 1 calc R U . . .
H20C H 0.8407 0.4531 0.5993 0.095 Uiso 1 1 calc R U . . .
C21 C 0.7816(9) 0.6133(10) 0.5582(5) 0.063(2) Uani 1 1 d . . . . .
H21A H 0.7429 0.5842 0.5832 0.095 Uiso 1 1 calc R U . . .
H21B H 0.7493 0.6438 0.5302 0.095 Uiso 1 1 calc R U . . .
H21C H 0.8161 0.6591 0.5767 0.095 Uiso 1 1 calc R U . . .
C22 C 0.9067(9) 0.5877(10) 0.5006(5) 0.063(2) Uani 1 1 d . . . . .
H22A H 0.8801 0.6235 0.4723 0.095 Uiso 1 1 calc R U . . .
H22B H 0.9437 0.5410 0.4851 0.095 Uiso 1 1 calc R U . . .
H22C H 0.9397 0.6290 0.5231 0.095 Uiso 1 1 calc R U . . .
C23 C 0.8443(6) 0.5240(7) 0.2326(4) 0.033(2) Uani 1 1 d . . . . .
C24 C 0.9019(6) 0.2788(8) 0.4930(4) 0.036(3) Uani 1 1 d . . . . .
N1 N 0.9871(5) 0.2990(5) 0.2993(3) 0.0305(19) Uani 1 1 d . . . . .
N2 N 0.9334(5) 0.3058(5) 0.3791(3) 0.0292(19) Uani 1 1 d . . . . .
N3 N 0.7698(5) 0.5162(5) 0.4302(3) 0.0274(18) Uani 1 1 d . . . . .
N4 N 0.8182(5) 0.5067(5) 0.3488(3) 0.0276(19) Uani 1 1 d . . . . .
O1 O 0.8189(5) 0.5651(6) 0.1963(3) 0.055(2) Uani 1 1 d . . . . .
O2 O 0.9258(6) 0.2321(7) 0.5266(4) 0.071(3) Uani 1 1 d . . . . .
P1 P 0.96840(15) 0.35432(16) 0.24015(10) 0.0238(5) Uani 1 1 d . . . . .
P2 P 0.78604(16) 0.4572(2) 0.48838(10) 0.0317(6) Uani 1 1 d . . . . .
Rh1 Rh 0.88333(5) 0.44944(5) 0.28558(3) 0.0234(2) Uani 1 1 d . . . . .
Rh2 Rh 0.86644(5) 0.35986(5) 0.44164(3) 0.0270(2) 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 N2 1.323(12) . ?
C1 N1 1.372(12) . ?
C1 Rh1 2.071(10) . ?
C2 C3 1.342(15) . ?
C2 N1 1.385(13) . ?
C2 H2 0.9500 . ?
C3 N2 1.413(12) . ?
C3 H3 0.9500 . ?
C4 C5 1.513(19) . ?
C4 C7 1.533(17) . ?
C4 C6 1.57(2) . ?
C4 P1 1.847(11) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C10 1.516(14) . ?
C8 C9 1.516(16) . ?
C8 C11 1.546(15) . ?
C8 P1 1.853(10) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 N4 1.335(12) . ?
C12 N3 1.357(11) . ?
C12 Rh2 2.080(9) . ?
C13 C14 1.374(14) . ?
C13 N3 1.397(12) . ?
C13 H13 0.9500 . ?
C14 N4 1.408(11) . ?
C14 H14 0.9500 . ?
C15 C16 1.518(19) . ?
C15 C17 1.535(19) . ?
C15 C18 1.54(2) . ?
C15 P2 1.856(12) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C21 1.524(16) . ?
C19 C22 1.540(18) . ?
C19 C20 1.540(17) . ?
C19 P2 1.862(11) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 O1 1.166(12) . ?
C23 Rh1 1.833(10) . ?
C24 O2 1.152(12) . ?
C24 Rh2 1.842(11) . ?
N1 P1 1.727(8) . ?
N2 Rh2 2.065(8) . ?
N3 P2 1.724(8) . ?
N4 Rh1 2.080(8) . ?
P1 Rh1 2.249(3) . ?
P2 Rh2 2.243(3) . ?

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
N2 C1 N1 109.1(8) . . ?
N2 C1 Rh1 146.1(8) . . ?
N1 C1 Rh1 104.7(6) . . ?
C3 C2 N1 105.8(9) . . ?
C3 C2 H2 127.1 . . ?
N1 C2 H2 127.1 . . ?
C2 C3 N2 109.7(9) . . ?
C2 C3 H3 125.2 . . ?
N2 C3 H3 125.2 . . ?
C5 C4 C7 109.4(11) . . ?
C5 C4 C6 109.9(11) . . ?
C7 C4 C6 108.6(11) . . ?
C5 C4 P1 106.3(8) . . ?
C7 C4 P1 116.6(8) . . ?
C6 C4 P1 106.0(8) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C10 C8 C9 109.6(10) . . ?
C10 C8 C11 107.9(9) . . ?
C9 C8 C11 107.6(12) . . ?
C10 C8 P1 116.3(8) . . ?
C9 C8 P1 109.0(8) . . ?
C11 C8 P1 106.0(7) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N4 C12 N3 110.0(8) . . ?
N4 C12 Rh2 145.1(7) . . ?
N3 C12 Rh2 104.6(6) . . ?
C14 C13 N3 104.4(8) . . ?
C14 C13 H13 127.8 . . ?
N3 C13 H13 127.8 . . ?
C13 C14 N4 110.2(9) . . ?
C13 C14 H14 124.9 . . ?
N4 C14 H14 124.9 . . ?
C16 C15 C17 110.0(13) . . ?
C16 C15 C18 108.8(12) . . ?
C17 C15 C18 111.5(13) . . ?
C16 C15 P2 105.7(9) . . ?
C17 C15 P2 107.1(9) . . ?
C18 C15 P2 113.6(10) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C21 C19 C22 109.1(11) . . ?
C21 C19 C20 111.0(10) . . ?
C22 C19 C20 107.7(10) . . ?
C21 C19 P2 115.8(8) . . ?
C22 C19 P2 105.4(8) . . ?
C20 C19 P2 107.5(8) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O1 C23 Rh1 174.5(10) . . ?
O2 C24 Rh2 176.3(10) . . ?
C1 N1 C2 108.8(8) . . ?
C1 N1 P1 100.9(6) . . ?
C2 N1 P1 149.1(8) . . ?
C1 N2 C3 106.6(8) . . ?
C1 N2 Rh2 121.5(6) . . ?
C3 N2 Rh2 131.9(7) . . ?
C12 N3 C13 109.5(8) . . ?
C12 N3 P2 101.3(6) . . ?
C13 N3 P2 148.5(7) . . ?
C12 N4 C14 106.0(8) . . ?
C12 N4 Rh1 121.4(6) . . ?
C14 N4 Rh1 132.6(6) . . ?
N1 P1 C4 105.1(5) . . ?
N1 P1 C8 105.2(4) . . ?
C4 P1 C8 114.0(5) . . ?
N1 P1 Rh1 86.8(3) . . ?
C4 P1 Rh1 120.7(4) . . ?
C8 P1 Rh1 118.2(4) . . ?
N3 P2 C15 105.9(5) . . ?
N3 P2 C19 106.1(5) . . ?
C15 P2 C19 113.1(6) . . ?
N3 P2 Rh2 86.9(3) . . ?
C15 P2 Rh2 120.2(5) . . ?
C19 P2 Rh2 118.6(4) . . ?
C23 Rh1 C1 167.6(4) . . ?
C23 Rh1 N4 99.2(4) . . ?
C1 Rh1 N4 92.4(3) . . ?
C23 Rh1 P1 101.0(3) . . ?
C1 Rh1 P1 67.3(3) . . ?
N4 Rh1 P1 159.8(2) . . ?
C24 Rh2 N2 98.2(4) . . ?
C24 Rh2 C12 168.8(4) . . ?
N2 Rh2 C12 92.8(3) . . ?
C24 Rh2 P2 101.7(4) . . ?
N2 Rh2 P2 159.8(2) . . ?
C12 Rh2 P2 67.2(3) . . ?

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 C2 C3 N2 -0.4(13) . . . . ?
N3 C13 C14 N4 -0.5(11) . . . . ?
N2 C1 N1 C2 1.8(12) . . . . ?
Rh1 C1 N1 C2 -175.8(7) . . . . ?
N2 C1 N1 P1 173.3(7) . . . . ?
Rh1 C1 N1 P1 -4.2(7) . . . . ?
C3 C2 N1 C1 -0.8(13) . . . . ?
C3 C2 N1 P1 -164.5(12) . . . . ?
N1 C1 N2 C3 -1.9(11) . . . . ?
Rh1 C1 N2 C3 173.8(11) . . . . ?
N1 C1 N2 Rh2 176.4(6) . . . . ?
Rh1 C1 N2 Rh2 -7.9(17) . . . . ?
C2 C3 N2 C1 1.5(13) . . . . ?
C2 C3 N2 Rh2 -176.7(8) . . . . ?
N4 C12 N3 C13 -0.7(11) . . . . ?
Rh2 C12 N3 C13 174.4(6) . . . . ?
N4 C12 N3 P2 -174.2(7) . . . . ?
Rh2 C12 N3 P2 1.0(6) . . . . ?
C14 C13 N3 C12 0.7(10) . . . . ?
C14 C13 N3 P2 168.4(10) . . . . ?
N3 C12 N4 C14 0.4(10) . . . . ?
Rh2 C12 N4 C14 -171.4(10) . . . . ?
N3 C12 N4 Rh1 -179.5(6) . . . . ?
Rh2 C12 N4 Rh1 8.7(16) . . . . ?
C13 C14 N4 C12 0.1(11) . . . . ?
C13 C14 N4 Rh1 180.0(7) . . . . ?
C1 N1 P1 C4 124.8(7) . . . . ?
C2 N1 P1 C4 -71.0(16) . . . . ?
C1 N1 P1 C8 -114.6(7) . . . . ?
C2 N1 P1 C8 49.6(16) . . . . ?
C1 N1 P1 Rh1 3.8(6) . . . . ?
C2 N1 P1 Rh1 168.0(16) . . . . ?
C5 C4 P1 N1 -62.0(10) . . . . ?
C7 C4 P1 N1 60.2(12) . . . . ?
C6 C4 P1 N1 -178.8(8) . . . . ?
C5 C4 P1 C8 -176.6(9) . . . . ?
C7 C4 P1 C8 -54.4(12) . . . . ?
C6 C4 P1 C8 66.5(9) . . . . ?
C5 C4 P1 Rh1 33.4(11) . . . . ?
C7 C4 P1 Rh1 155.6(9) . . . . ?
C6 C4 P1 Rh1 -83.5(9) . . . . ?
C10 C8 P1 N1 -72.8(9) . . . . ?
C9 C8 P1 N1 162.7(9) . . . . ?
C11 C8 P1 N1 47.1(9) . . . . ?
C10 C8 P1 C4 41.8(10) . . . . ?
C9 C8 P1 C4 -82.8(11) . . . . ?
C11 C8 P1 C4 161.7(8) . . . . ?
C10 C8 P1 Rh1 -167.5(7) . . . . ?
C9 C8 P1 Rh1 68.0(10) . . . . ?
C11 C8 P1 Rh1 -47.5(9) . . . . ?
C12 N3 P2 C15 -121.5(7) . . . . ?
C13 N3 P2 C15 70.4(14) . . . . ?
C12 N3 P2 C19 118.0(7) . . . . ?
C13 N3 P2 C19 -50.1(14) . . . . ?
C12 N3 P2 Rh2 -0.9(6) . . . . ?
C13 N3 P2 Rh2 -169.0(13) . . . . ?
C16 C15 P2 N3 68.8(10) . . . . ?
C17 C15 P2 N3 -174.0(10) . . . . ?
C18 C15 P2 N3 -50.4(12) . . . . ?
C16 C15 P2 C19 -175.5(9) . . . . ?
C17 C15 P2 C19 -58.2(12) . . . . ?
C18 C15 P2 C19 65.3(12) . . . . ?
C16 C15 P2 Rh2 -27.1(11) . . . . ?
C17 C15 P2 Rh2 90.2(11) . . . . ?
C18 C15 P2 Rh2 -146.3(9) . . . . ?
C21 C19 P2 N3 76.0(10) . . . . ?
C22 C19 P2 N3 -44.7(9) . . . . ?
C20 C19 P2 N3 -159.4(8) . . . . ?
C21 C19 P2 C15 -39.7(11) . . . . ?
C22 C19 P2 C15 -160.4(8) . . . . ?
C20 C19 P2 C15 84.9(9) . . . . ?
C21 C19 P2 Rh2 171.3(8) . . . . ?
C22 C19 P2 Rh2 50.7(9) . . . . ?
C20 C19 P2 Rh2 -64.0(9) . . . . ?

_refine_diff_density_max         0.794
_refine_diff_density_min         -0.871
_refine_diff_density_rms         0.231

_shelxl_version_number           2013-4

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
####################################################################### 
# 
# 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_pbpa141006
_database_code_depnum_ccdc_archive 'CCDC 1449238'
_audit_update_record             
;
2016-01-22 deposited with the CCDC.
2016-02-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H38 N2 P2 Se'
_chemical_formula_sum            'C19 H38 N2 P2 Se'
_chemical_formula_weight         435.41

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_H-M_alt        'C m c 21'
_space_group_name_Hall           'C 2c -2'

_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+1/2'
'-x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   14.2413(17)
_cell_length_b                   9.0598(11)
_cell_length_c                   17.831(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2300.6(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1855
_cell_measurement_theta_min      2.66
_cell_measurement_theta_max      27.93

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_F_000             920
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    1.775
_shelx_estimated_absorpt_T_min   0.764
_shelx_estimated_absorpt_T_max   0.932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6223
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  triumph
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5810
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.284
_diffrn_reflns_theta_max         27.996
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.771
_diffrn_reflns_point_group_measured_fraction_full 0.812
_reflns_number_total             2220
_reflns_number_gt                1792
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.495
_reflns_Friedel_fraction_max     0.528
_reflns_Friedel_fraction_full    0.610

_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0677P)²+4.2459P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_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_abs_structure_details 
;
 Flack x determined using 567 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.425(9)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2220
_refine_ls_number_parameters     127
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0499
_refine_ls_wR_factor_ref         0.1285
_refine_ls_wR_factor_gt          0.1166
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.000
_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 1.0000 0.1572(8) 0.3312(5) 0.0255(17) Uani 1 2 d S T P . .
C2 C 1.0000 0.2601(9) 0.4446(5) 0.040(2) Uani 1 2 d S T P . .
H2 H 1.0000 0.2712 0.4976 0.048 Uiso 1 2 calc R U P . .
C3 C 1.0000 0.3698(9) 0.3952(6) 0.039(2) Uani 1 2 d S T P . .
H3 H 1.0000 0.4722 0.4065 0.047 Uiso 1 2 calc R U P . .
C4 C 1.1100(4) -0.0544(7) 0.4999(4) 0.0336(14) Uani 1 1 d . . . . .
C5 C 1.1189(6) -0.2114(9) 0.5312(6) 0.072(3) Uani 1 1 d . . . . .
H5A H 1.1818 -0.2251 0.5524 0.108 Uiso 1 1 calc R U . . .
H5B H 1.1087 -0.2830 0.4908 0.108 Uiso 1 1 calc R U . . .
H5C H 1.0717 -0.2264 0.5706 0.108 Uiso 1 1 calc R U . . .
C6 C 1.1228(6) 0.0566(10) 0.5624(5) 0.059(2) Uani 1 1 d . . . . .
H6A H 1.1828 0.0386 0.5876 0.088 Uiso 1 1 calc R U . . .
H6B H 1.0714 0.0466 0.5985 0.088 Uiso 1 1 calc R U . . .
H6C H 1.1225 0.1566 0.5414 0.088 Uiso 1 1 calc R U . . .
C7 C 1.1882(5) -0.0325(10) 0.4423(6) 0.057(2) Uani 1 1 d . . . . .
H7A H 1.1815 0.0646 0.4187 0.086 Uiso 1 1 calc R U . . .
H7B H 1.1840 -0.1095 0.4038 0.086 Uiso 1 1 calc R U . . .
H7C H 1.2493 -0.0386 0.4673 0.086 Uiso 1 1 calc R U . . .
C8 C 0.8903(4) 0.5109(6) 0.2421(4) 0.0308(15) Uani 1 1 d . . . . .
C9 C 0.8112(4) 0.3962(7) 0.2466(6) 0.0497(19) Uani 1 1 d . . . . .
H9A H 0.8140 0.3455 0.2951 0.074 Uiso 1 1 calc R U . . .
H9B H 0.8188 0.3241 0.2061 0.074 Uiso 1 1 calc R U . . .
H9C H 0.7504 0.4458 0.2414 0.074 Uiso 1 1 calc R U . . .
C10 C 0.8776(5) 0.6211(8) 0.3061(5) 0.052(2) Uani 1 1 d . . . . .
H10A H 0.8157 0.6678 0.3020 0.078 Uiso 1 1 calc R U . . .
H10B H 0.9266 0.6968 0.3031 0.078 Uiso 1 1 calc R U . . .
H10C H 0.8823 0.5693 0.3542 0.078 Uiso 1 1 calc R U . . .
C11 C 0.8811(6) 0.5923(10) 0.1669(6) 0.063(3) Uani 1 1 d . . . . .
H11A H 0.8170 0.6301 0.1615 0.094 Uiso 1 1 calc R U . . .
H11B H 0.8949 0.5240 0.1258 0.094 Uiso 1 1 calc R U . . .
H11C H 0.9256 0.6748 0.1655 0.094 Uiso 1 1 calc R U . . .
N1 N 1.0000 0.1250(7) 0.4059(4) 0.0285(16) Uani 1 2 d S T P . .
N2 N 1.0000 0.3077(6) 0.3234(4) 0.0257(15) Uani 1 2 d S T P . .
P1 P 1.0000 -0.0565(2) 0.44110(12) 0.0257(5) Uani 1 2 d S T P . .
P2 P 1.0000 0.39675(19) 0.23475(11) 0.0223(5) Uani 1 2 d S T P . .
Se1 Se 1.0000 0.02342(9) 0.25369(7) 0.0754(6) 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 1.364(11) . ?
C1 N2 1.370(9) . ?
C1 Se1 1.839(8) . ?
C2 C3 1.329(13) . ?
C2 N1 1.405(10) . ?
C2 H2 0.9500 . ?
C3 N2 1.398(12) . ?
C3 H3 0.9500 . ?
C4 C6 1.512(11) . ?
C4 C7 1.528(11) . ?
C4 C5 1.533(9) . ?
C4 P1 1.885(7) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C10 1.526(10) . ?
C8 C9 1.534(8) . ?
C8 C11 1.536(11) . ?
C8 P2 1.878(5) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
N1 P1 1.760(7) . ?
N2 P2 1.775(7) . ?
P1 C4 1.885(7) 3_755 ?
P2 C8 1.878(5) 3_755 ?

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 N2 108.2(6) . . ?
N1 C1 Se1 126.4(5) . . ?
N2 C1 Se1 125.4(6) . . ?
C3 C2 N1 109.0(8) . . ?
C3 C2 H2 125.5 . . ?
N1 C2 H2 125.5 . . ?
C2 C3 N2 107.9(8) . . ?
C2 C3 H3 126.1 . . ?
N2 C3 H3 126.1 . . ?
C6 C4 C7 108.7(6) . . ?
C6 C4 C5 109.8(7) . . ?
C7 C4 C5 107.8(6) . . ?
C6 C4 P1 121.1(5) . . ?
C7 C4 P1 103.5(5) . . ?
C5 C4 P1 105.2(5) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C10 C8 C9 108.5(6) . . ?
C10 C8 C11 109.2(6) . . ?
C9 C8 C11 107.9(7) . . ?
C10 C8 P2 120.7(5) . . ?
C9 C8 P2 104.0(4) . . ?
C11 C8 P2 105.9(5) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C1 N1 C2 107.1(6) . . ?
C1 N1 P1 123.2(5) . . ?
C2 N1 P1 129.7(6) . . ?
C1 N2 C3 107.9(7) . . ?
C1 N2 P2 122.9(6) . . ?
C3 N2 P2 129.2(6) . . ?
N1 P1 C4 100.9(2) . . ?
N1 P1 C4 100.9(2) . 3_755 ?
C4 P1 C4 112.4(4) . 3_755 ?
N2 P2 C8 100.8(3) . 3_755 ?
N2 P2 C8 100.8(3) . . ?
C8 P2 C8 112.6(3) 3_755 . ?

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 C2 C3 N2 0.000(2) . . . . ?
N2 C1 N1 C2 0.000(2) . . . . ?
Se1 C1 N1 C2 180.000(2) . . . . ?
N2 C1 N1 P1 180.000(1) . . . . ?
Se1 C1 N1 P1 0.000(1) . . . . ?
C3 C2 N1 C1 0.000(2) . . . . ?
C3 C2 N1 P1 180.000(2) . . . . ?
N1 C1 N2 C3 0.000(2) . . . . ?
Se1 C1 N2 C3 180.000(2) . . . . ?
N1 C1 N2 P2 180.000(1) . . . . ?
Se1 C1 N2 P2 0.000(1) . . . . ?
C2 C3 N2 C1 0.000(2) . . . . ?
C2 C3 N2 P2 180.000(2) . . . . ?
C1 N1 P1 C4 122.2(2) . . . . ?
C2 N1 P1 C4 -57.8(2) . . . . ?
C1 N1 P1 C4 -122.2(2) . . . 3_755 ?
C2 N1 P1 C4 57.8(2) . . . 3_755 ?
C6 C4 P1 N1 57.1(7) . . . . ?
C7 C4 P1 N1 -64.9(5) . . . . ?
C5 C4 P1 N1 -177.9(6) . . . . ?
C6 C4 P1 C4 -49.5(7) . . . 3_755 ?
C7 C4 P1 C4 -171.6(3) . . . 3_755 ?
C5 C4 P1 C4 75.4(7) . . . 3_755 ?
C1 N2 P2 C8 -122.13(19) . . . 3_755 ?
C3 N2 P2 C8 57.87(19) . . . 3_755 ?
C1 N2 P2 C8 122.13(19) . . . . ?
C3 N2 P2 C8 -57.87(19) . . . . ?
C10 C8 P2 N2 56.7(6) . . . . ?
C9 C8 P2 N2 -65.2(6) . . . . ?
C11 C8 P2 N2 -178.9(5) . . . . ?
C10 C8 P2 C8 -50.0(8) . . . 3_755 ?
C9 C8 P2 C8 -171.9(4) . . . 3_755 ?
C11 C8 P2 C8 74.5(7) . . . 3_755 ?

_refine_diff_density_max         0.819
_refine_diff_density_min         -0.987
_refine_diff_density_rms         0.093

_shelxl_version_number           2013-4

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
####################################################################### 
# 
# 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_pbpa141118
_database_code_depnum_ccdc_archive 'CCDC 1449239'
_audit_update_record             
;
2016-01-22 deposited with the CCDC.
2016-02-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C37 H38 B F15 N2 P2, C4 H8 O'
_chemical_formula_sum            'C41 H46 B F15 N2 O P2'
_chemical_formula_weight         940.55

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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                   12.3210(5)
_cell_length_b                   22.2071(10)
_cell_length_c                   16.3727(7)
_cell_angle_alpha                90
_cell_angle_beta                 105.5780(10)
_cell_angle_gamma                90
_cell_volume                     4315.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    7601
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      27.16

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_F_000             1936
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    0.201
_shelx_estimated_absorpt_T_min   0.920
_shelx_estimated_absorpt_T_max   0.965
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6904
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            41879
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.584
_diffrn_reflns_theta_max         28.006
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             10387
_reflns_number_gt                7069
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0462P)²+2.3984P] 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         10387
_refine_ls_number_parameters     571
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0499
_refine_ls_wR_factor_ref         0.1179
_refine_ls_wR_factor_gt          0.1028
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.019
_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 0.64078(16) 0.81146(8) 0.77159(12) 0.0198(4) Uani 1 1 d . . . . .
C2 C 0.66314(17) 0.71098(9) 0.78786(13) 0.0275(4) Uani 1 1 d . . . . .
H2 H 0.6464 0.6692 0.7863 0.033 Uiso 1 1 calc R U . . .
C3 C 0.76422(18) 0.73521(9) 0.81645(14) 0.0301(5) Uani 1 1 d . . . . .
H3 H 0.8328 0.7140 0.8385 0.036 Uiso 1 1 calc R U . . .
C4 C 0.44884(19) 0.67445(9) 0.64026(13) 0.0308(5) Uani 1 1 d . . . . .
C5 C 0.5356(2) 0.69190(10) 0.59202(15) 0.0386(6) Uani 1 1 d . . . . .
H5A H 0.6118 0.6878 0.6298 0.058 Uiso 1 1 calc R U . . .
H5B H 0.5230 0.7337 0.5726 0.058 Uiso 1 1 calc R U . . .
H5C H 0.5272 0.6653 0.5430 0.058 Uiso 1 1 calc R U . . .
C6 C 0.3314(2) 0.67551(12) 0.57597(15) 0.0457(6) Uani 1 1 d . . . . .
H6A H 0.3304 0.6474 0.5296 0.069 Uiso 1 1 calc R U . . .
H6B H 0.3150 0.7163 0.5531 0.069 Uiso 1 1 calc R U . . .
H6C H 0.2742 0.6635 0.6044 0.069 Uiso 1 1 calc R U . . .
C7 C 0.4728(2) 0.60971(10) 0.67369(15) 0.0389(6) Uani 1 1 d . . . . .
H7A H 0.4644 0.5820 0.6258 0.058 Uiso 1 1 calc R U . . .
H7B H 0.4194 0.5987 0.7060 0.058 Uiso 1 1 calc R U . . .
H7C H 0.5498 0.6072 0.7105 0.058 Uiso 1 1 calc R U . . .
C8 C 0.39812(19) 0.70728(10) 0.80989(14) 0.0317(5) Uani 1 1 d . . . . .
C9 C 0.2825(2) 0.67729(12) 0.77547(17) 0.0456(6) Uani 1 1 d . . . . .
H9A H 0.2918 0.6388 0.7487 0.068 Uiso 1 1 calc R U . . .
H9B H 0.2335 0.7038 0.7335 0.068 Uiso 1 1 calc R U . . .
H9C H 0.2484 0.6701 0.8222 0.068 Uiso 1 1 calc R U . . .
C10 C 0.4770(2) 0.66434(12) 0.87088(15) 0.0465(6) Uani 1 1 d . . . . .
H10A H 0.5493 0.6844 0.8954 0.070 Uiso 1 1 calc R U . . .
H10B H 0.4893 0.6282 0.8401 0.070 Uiso 1 1 calc R U . . .
H10C H 0.4431 0.6528 0.9163 0.070 Uiso 1 1 calc R U . . .
C11 C 0.3812(3) 0.76348(12) 0.85972(18) 0.0557(8) Uani 1 1 d . . . . .
H11A H 0.3474 0.7518 0.9051 0.084 Uiso 1 1 calc R U . . .
H11B H 0.3311 0.7918 0.8214 0.084 Uiso 1 1 calc R U . . .
H11C H 0.4542 0.7828 0.8844 0.084 Uiso 1 1 calc R U . . .
C12 C 0.98079(19) 0.82892(12) 0.80960(17) 0.0437(6) Uani 1 1 d . . . . .
C13 C 1.0018(3) 0.76447(14) 0.7863(2) 0.0642(8) Uani 1 1 d . . . . .
H13A H 0.9338 0.7486 0.7463 0.096 Uiso 1 1 calc R U . . .
H13B H 1.0207 0.7396 0.8376 0.096 Uiso 1 1 calc R U . . .
H13C H 1.0645 0.7637 0.7600 0.096 Uiso 1 1 calc R U . . .
C14 C 1.0894(2) 0.85589(16) 0.8673(2) 0.0700(9) Uani 1 1 d . . . . .
H14A H 1.1148 0.8312 0.9186 0.105 Uiso 1 1 calc R U . . .
H14B H 1.0746 0.8970 0.8832 0.105 Uiso 1 1 calc R U . . .
H14C H 1.1480 0.8566 0.8370 0.105 Uiso 1 1 calc R U . . .
C15 C 0.9497(2) 0.86584(17) 0.7279(2) 0.0700(10) Uani 1 1 d . . . . .
H15A H 1.0133 0.8663 0.7026 0.105 Uiso 1 1 calc R U . . .
H15B H 0.9317 0.9072 0.7407 0.105 Uiso 1 1 calc R U . . .
H15C H 0.8840 0.8478 0.6879 0.105 Uiso 1 1 calc R U . . .
C16 C 0.9041(2) 0.80955(12) 0.97345(16) 0.0448(6) Uani 1 1 d . . . . .
C17 C 0.7940(2) 0.79881(13) 0.99855(17) 0.0477(6) Uani 1 1 d . . . . .
H17A H 0.7512 0.7664 0.9637 0.071 Uiso 1 1 calc R U . . .
H17B H 0.7490 0.8358 0.9895 0.071 Uiso 1 1 calc R U . . .
H17C H 0.8117 0.7874 1.0585 0.071 Uiso 1 1 calc R U . . .
C18 C 0.9763(2) 0.75185(14) 0.99171(18) 0.0574(8) Uani 1 1 d . . . . .
H18A H 0.9948 0.7427 1.0525 0.086 Uiso 1 1 calc R U . . .
H18B H 1.0460 0.7580 0.9748 0.086 Uiso 1 1 calc R U . . .
H18C H 0.9340 0.7182 0.9595 0.086 Uiso 1 1 calc R U . . .
C19 C 0.9681(3) 0.86036(16) 1.0311(2) 0.0729(10) Uani 1 1 d . . . . .
H19A H 0.9842 0.8478 1.0905 0.109 Uiso 1 1 calc R U . . .
H19B H 0.9216 0.8969 1.0224 0.109 Uiso 1 1 calc R U . . .
H19C H 1.0390 0.8686 1.0168 0.109 Uiso 1 1 calc R U . . .
C20 C 0.64678(18) 0.92564(8) 0.82460(13) 0.0254(4) Uani 1 1 d . . . . .
C21 C 0.6140(2) 0.91747(9) 0.89829(14) 0.0353(5) Uani 1 1 d . . . . .
C22 C 0.6490(3) 0.95147(11) 0.97065(16) 0.0511(7) Uani 1 1 d . . . . .
C23 C 0.7259(3) 0.99669(11) 0.97314(17) 0.0519(7) Uani 1 1 d . . . . .
C24 C 0.7639(2) 1.00656(10) 0.90370(17) 0.0413(6) Uani 1 1 d . . . . .
C25 C 0.72502(19) 0.97178(9) 0.83229(14) 0.0316(5) Uani 1 1 d . . . . .
C26 C 0.63633(17) 0.90387(9) 0.65815(13) 0.0243(4) Uani 1 1 d . . . . .
C27 C 0.68351(17) 0.86903(9) 0.60676(13) 0.0268(4) Uani 1 1 d . . . . .
C28 C 0.71199(19) 0.89007(10) 0.53585(14) 0.0331(5) Uani 1 1 d . . . . .
C29 C 0.6905(2) 0.94897(11) 0.51174(15) 0.0382(5) Uani 1 1 d . . . . .
C30 C 0.6404(2) 0.98560(10) 0.55838(15) 0.0363(5) Uani 1 1 d . . . . .
C31 C 0.61357(18) 0.96270(9) 0.62838(14) 0.0299(5) Uani 1 1 d . . . . .
C32 C 0.45454(17) 0.88844(9) 0.70545(13) 0.0247(4) Uani 1 1 d . . . . .
C33 C 0.38193(19) 0.92318(9) 0.73845(15) 0.0326(5) Uani 1 1 d . . . . .
C34 C 0.2678(2) 0.92836(11) 0.70142(17) 0.0410(6) Uani 1 1 d . . . . .
C35 C 0.21919(19) 0.90081(12) 0.62605(17) 0.0430(6) Uani 1 1 d . . . . .
C36 C 0.28625(19) 0.86805(11) 0.58790(14) 0.0352(5) Uani 1 1 d . . . . .
C37 C 0.39965(17) 0.86337(9) 0.62766(13) 0.0268(4) Uani 1 1 d . . . . .
C38 C 0.8934(3) 0.59826(15) 0.7455(2) 0.0745(10) Uani 1 1 d . . . . .
H38A H 0.8867 0.6336 0.7077 0.089 Uiso 1 1 calc R U . . .
H38B H 0.8289 0.5710 0.7219 0.089 Uiso 1 1 calc R U . . .
C39 C 0.9998(4) 0.5668(2) 0.7521(3) 0.0995(14) Uani 1 1 d . . . . .
H39A H 1.0531 0.5931 0.7330 0.119 Uiso 1 1 calc R U . . .
H39B H 0.9870 0.5299 0.7169 0.119 Uiso 1 1 calc R U . . .
C40 C 1.0447(3) 0.5515(2) 0.8431(3) 0.1042(15) Uani 1 1 d . . . . .
H40A H 1.1205 0.5692 0.8663 0.125 Uiso 1 1 calc R U . . .
H40B H 1.0497 0.5073 0.8512 0.125 Uiso 1 1 calc R U . . .
C41 C 0.9615(4) 0.57829(17) 0.8859(2) 0.0909(13) Uani 1 1 d . . . . .
H41A H 0.9158 0.5462 0.9025 0.109 Uiso 1 1 calc R U . . .
H41B H 1.0013 0.6009 0.9374 0.109 Uiso 1 1 calc R U . . .
N1 N 0.58539(13) 0.75703(7) 0.76044(10) 0.0213(3) Uani 1 1 d . . . . .
N2 N 0.75226(13) 0.79735(7) 0.80855(11) 0.0247(4) Uani 1 1 d . . . . .
B1 B 0.59423(19) 0.88166(9) 0.74150(14) 0.0223(4) Uani 1 1 d . . . . .
F1 F 0.54117(13) 0.87228(6) 0.90119(8) 0.0476(4) Uani 1 1 d . . . . .
F2 F 0.6102(2) 0.94114(8) 1.03844(10) 0.0887(7) Uani 1 1 d . . . . .
F3 F 0.76237(19) 1.03059(8) 1.04329(10) 0.0818(6) Uani 1 1 d . . . . .
F4 F 0.84078(14) 1.04995(7) 0.90513(11) 0.0603(4) Uani 1 1 d . . . . .
F5 F 0.77394(11) 0.98410(6) 0.76953(9) 0.0428(3) Uani 1 1 d . . . . .
F6 F 0.70345(11) 0.80956(5) 0.62356(8) 0.0352(3) Uani 1 1 d . . . . .
F7 F 0.75998(13) 0.85343(6) 0.49023(9) 0.0490(4) Uani 1 1 d . . . . .
F8 F 0.71711(15) 0.97055(7) 0.44274(10) 0.0607(5) Uani 1 1 d . . . . .
F9 F 0.61826(14) 1.04347(6) 0.53547(10) 0.0547(4) Uani 1 1 d . . . . .
F10 F 0.56168(11) 1.00117(5) 0.67007(9) 0.0388(3) Uani 1 1 d . . . . .
F11 F 0.41933(12) 0.95643(6) 0.80945(10) 0.0506(4) Uani 1 1 d . . . . .
F12 F 0.20383(13) 0.96200(8) 0.73903(12) 0.0666(5) Uani 1 1 d . . . . .
F13 F 0.10835(12) 0.90655(9) 0.58923(11) 0.0673(5) Uani 1 1 d . . . . .
F14 F 0.24147(12) 0.84045(7) 0.51335(9) 0.0525(4) Uani 1 1 d . . . . .
F15 F 0.45860(10) 0.82981(5) 0.58523(7) 0.0318(3) Uani 1 1 d . . . . .
P1 P 0.43910(4) 0.73820(2) 0.71540(3) 0.02235(11) Uani 1 1 d . . . . .
P2 P 0.86651(5) 0.84517(3) 0.86363(4) 0.03353(14) Uani 1 1 d . . . . .
O1 O 0.8936(3) 0.61653(13) 0.82699(17) 0.1133(11) 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 1.376(2) . ?
C1 N2 1.380(2) . ?
C1 B1 1.688(3) . ?
C2 C3 1.322(3) . ?
C2 N1 1.391(2) . ?
C2 H2 0.9500 . ?
C3 N2 1.390(3) . ?
C3 H3 0.9500 . ?
C4 C7 1.538(3) . ?
C4 C5 1.540(3) . ?
C4 C6 1.544(3) . ?
C4 P1 1.900(2) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C10 1.526(3) . ?
C8 C11 1.536(3) . ?
C8 C9 1.536(3) . ?
C8 P1 1.881(2) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.521(4) . ?
C12 C15 1.528(4) . ?
C12 C14 1.538(4) . ?
C12 P2 1.888(3) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.537(4) . ?
C16 C18 1.543(4) . ?
C16 C19 1.544(4) . ?
C16 P2 1.904(3) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.383(3) . ?
C20 C25 1.389(3) . ?
C20 B1 1.659(3) . ?
C21 F1 1.356(2) . ?
C21 C22 1.373(3) . ?
C22 F2 1.341(3) . ?
C22 C23 1.373(4) . ?
C23 F3 1.346(3) . ?
C23 C24 1.358(4) . ?
C24 F4 1.347(3) . ?
C24 C25 1.376(3) . ?
C25 F5 1.352(3) . ?
C26 C27 1.381(3) . ?
C26 C31 1.396(3) . ?
C26 B1 1.660(3) . ?
C27 F6 1.358(2) . ?
C27 C28 1.381(3) . ?
C28 F7 1.344(2) . ?
C28 C29 1.371(3) . ?
C29 F8 1.347(2) . ?
C29 C30 1.371(3) . ?
C30 F9 1.346(2) . ?
C30 C31 1.373(3) . ?
C31 F10 1.356(2) . ?
C32 C37 1.388(3) . ?
C32 C33 1.395(3) . ?
C32 B1 1.670(3) . ?
C33 F11 1.350(3) . ?
C33 C34 1.378(3) . ?
C34 F12 1.349(3) . ?
C34 C35 1.363(4) . ?
C35 F13 1.343(3) . ?
C35 C36 1.371(3) . ?
C36 F14 1.345(3) . ?
C36 C37 1.378(3) . ?
C37 F15 1.355(2) . ?
C38 O1 1.394(4) . ?
C38 C39 1.464(5) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.483(6) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 C41 1.511(6) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 O1 1.385(4) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
N1 P1 1.8037(16) . ?
N2 P2 1.8003(17) . ?

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 N2 104.98(15) . . ?
N1 C1 B1 130.92(17) . . ?
N2 C1 B1 123.90(16) . . ?
C3 C2 N1 108.48(17) . . ?
C3 C2 H2 125.8 . . ?
N1 C2 H2 125.8 . . ?
C2 C3 N2 107.75(18) . . ?
C2 C3 H3 126.1 . . ?
N2 C3 H3 126.1 . . ?
C7 C4 C5 108.94(19) . . ?
C7 C4 C6 108.16(18) . . ?
C5 C4 C6 107.41(19) . . ?
C7 C4 P1 120.35(15) . . ?
C5 C4 P1 108.53(14) . . ?
C6 C4 P1 102.67(16) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C10 C8 C11 108.3(2) . . ?
C10 C8 C9 109.53(19) . . ?
C11 C8 C9 107.6(2) . . ?
C10 C8 P1 120.10(17) . . ?
C11 C8 P1 104.18(15) . . ?
C9 C8 P1 106.48(16) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 C15 107.8(3) . . ?
C13 C12 C14 110.0(2) . . ?
C15 C12 C14 107.6(2) . . ?
C13 C12 P2 119.73(18) . . ?
C15 C12 P2 105.33(18) . . ?
C14 C12 P2 105.8(2) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 C18 108.9(2) . . ?
C17 C16 C19 107.0(2) . . ?
C18 C16 C19 108.4(2) . . ?
C17 C16 P2 107.99(17) . . ?
C18 C16 P2 120.61(19) . . ?
C19 C16 P2 103.2(2) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 C25 112.07(19) . . ?
C21 C20 B1 119.81(18) . . ?
C25 C20 B1 128.11(19) . . ?
F1 C21 C22 115.8(2) . . ?
F1 C21 C20 118.60(18) . . ?
C22 C21 C20 125.6(2) . . ?
F2 C22 C21 121.4(2) . . ?
F2 C22 C23 119.8(2) . . ?
C21 C22 C23 118.8(2) . . ?
F3 C23 C24 120.9(2) . . ?
F3 C23 C22 120.3(3) . . ?
C24 C23 C22 118.9(2) . . ?
F4 C24 C23 120.0(2) . . ?
F4 C24 C25 119.9(2) . . ?
C23 C24 C25 120.1(2) . . ?
F5 C25 C24 114.09(19) . . ?
F5 C25 C20 121.39(19) . . ?
C24 C25 C20 124.5(2) . . ?
C27 C26 C31 112.92(18) . . ?
C27 C26 B1 127.59(17) . . ?
C31 C26 B1 119.16(17) . . ?
F6 C27 C26 120.29(17) . . ?
F6 C27 C28 115.22(18) . . ?
C26 C27 C28 124.48(19) . . ?
F7 C28 C29 119.82(19) . . ?
F7 C28 C27 120.8(2) . . ?
C29 C28 C27 119.4(2) . . ?
F8 C29 C30 120.3(2) . . ?
F8 C29 C28 120.6(2) . . ?
C30 C29 C28 119.1(2) . . ?
F9 C30 C29 119.9(2) . . ?
F9 C30 C31 120.7(2) . . ?
C29 C30 C31 119.4(2) . . ?
F10 C31 C30 116.01(18) . . ?
F10 C31 C26 119.43(18) . . ?
C30 C31 C26 124.6(2) . . ?
C37 C32 C33 111.84(19) . . ?
C37 C32 B1 119.35(17) . . ?
C33 C32 B1 128.33(19) . . ?
F11 C33 C34 113.9(2) . . ?
F11 C33 C32 122.0(2) . . ?
C34 C33 C32 124.1(2) . . ?
F12 C34 C35 119.6(2) . . ?
F12 C34 C33 119.8(2) . . ?
C35 C34 C33 120.6(2) . . ?
F13 C35 C34 120.7(2) . . ?
F13 C35 C36 120.7(2) . . ?
C34 C35 C36 118.6(2) . . ?
F14 C36 C35 120.3(2) . . ?
F14 C36 C37 120.8(2) . . ?
C35 C36 C37 118.9(2) . . ?
F15 C37 C36 114.48(19) . . ?
F15 C37 C32 119.65(18) . . ?
C36 C37 C32 125.9(2) . . ?
O1 C38 C39 107.3(3) . . ?
O1 C38 H38A 110.3 . . ?
C39 C38 H38A 110.3 . . ?
O1 C38 H38B 110.3 . . ?
C39 C38 H38B 110.3 . . ?
H38A C38 H38B 108.5 . . ?
C38 C39 C40 105.5(3) . . ?
C38 C39 H39A 110.6 . . ?
C40 C39 H39A 110.6 . . ?
C38 C39 H39B 110.6 . . ?
C40 C39 H39B 110.6 . . ?
H39A C39 H39B 108.8 . . ?
C39 C40 C41 105.1(3) . . ?
C39 C40 H40A 110.7 . . ?
C41 C40 H40A 110.7 . . ?
C39 C40 H40B 110.7 . . ?
C41 C40 H40B 110.7 . . ?
H40A C40 H40B 108.8 . . ?
O1 C41 C40 106.0(3) . . ?
O1 C41 H41A 110.5 . . ?
C40 C41 H41A 110.5 . . ?
O1 C41 H41B 110.5 . . ?
C40 C41 H41B 110.5 . . ?
H41A C41 H41B 108.7 . . ?
C1 N1 C2 109.21(16) . . ?
C1 N1 P1 131.56(13) . . ?
C2 N1 P1 119.18(13) . . ?
C1 N2 C3 109.53(16) . . ?
C1 N2 P2 129.64(13) . . ?
C3 N2 P2 119.33(14) . . ?
C20 B1 C26 111.11(16) . . ?
C20 B1 C32 112.03(16) . . ?
C26 B1 C32 101.70(15) . . ?
C20 B1 C1 106.09(15) . . ?
C26 B1 C1 110.95(16) . . ?
C32 B1 C1 115.06(15) . . ?
N1 P1 C8 101.99(9) . . ?
N1 P1 C4 101.97(9) . . ?
C8 P1 C4 109.75(9) . . ?
N2 P2 C12 103.52(10) . . ?
N2 P2 C16 100.78(9) . . ?
C12 P2 C16 109.89(12) . . ?
C41 O1 C38 109.5(3) . . ?

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 C2 C3 N2 0.6(2) . . . . ?
C25 C20 C21 F1 -177.4(2) . . . . ?
B1 C20 C21 F1 1.6(3) . . . . ?
C25 C20 C21 C22 2.5(4) . . . . ?
B1 C20 C21 C22 -178.5(2) . . . . ?
F1 C21 C22 F2 -1.9(4) . . . . ?
C20 C21 C22 F2 178.2(3) . . . . ?
F1 C21 C22 C23 177.8(3) . . . . ?
C20 C21 C22 C23 -2.1(5) . . . . ?
F2 C22 C23 F3 0.0(5) . . . . ?
C21 C22 C23 F3 -179.6(3) . . . . ?
F2 C22 C23 C24 -179.8(3) . . . . ?
C21 C22 C23 C24 0.6(5) . . . . ?
F3 C23 C24 F4 1.4(4) . . . . ?
C22 C23 C24 F4 -178.8(3) . . . . ?
F3 C23 C24 C25 -179.5(3) . . . . ?
C22 C23 C24 C25 0.3(4) . . . . ?
F4 C24 C25 F5 2.5(3) . . . . ?
C23 C24 C25 F5 -176.6(2) . . . . ?
F4 C24 C25 C20 179.4(2) . . . . ?
C23 C24 C25 C20 0.2(4) . . . . ?
C21 C20 C25 F5 175.1(2) . . . . ?
B1 C20 C25 F5 -3.8(3) . . . . ?
C21 C20 C25 C24 -1.5(3) . . . . ?
B1 C20 C25 C24 179.5(2) . . . . ?
C31 C26 C27 F6 -175.38(18) . . . . ?
B1 C26 C27 F6 -2.1(3) . . . . ?
C31 C26 C27 C28 3.6(3) . . . . ?
B1 C26 C27 C28 176.9(2) . . . . ?
F6 C27 C28 F7 -2.5(3) . . . . ?
C26 C27 C28 F7 178.5(2) . . . . ?
F6 C27 C28 C29 177.2(2) . . . . ?
C26 C27 C28 C29 -1.8(4) . . . . ?
F7 C28 C29 F8 -0.1(4) . . . . ?
C27 C28 C29 F8 -179.8(2) . . . . ?
F7 C28 C29 C30 179.3(2) . . . . ?
C27 C28 C29 C30 -0.4(4) . . . . ?
F8 C29 C30 F9 -0.4(4) . . . . ?
C28 C29 C30 F9 -179.8(2) . . . . ?
F8 C29 C30 C31 179.8(2) . . . . ?
C28 C29 C30 C31 0.4(4) . . . . ?
F9 C30 C31 F10 1.8(3) . . . . ?
C29 C30 C31 F10 -178.4(2) . . . . ?
F9 C30 C31 C26 -178.1(2) . . . . ?
C29 C30 C31 C26 1.7(4) . . . . ?
C27 C26 C31 F10 176.58(18) . . . . ?
B1 C26 C31 F10 2.6(3) . . . . ?
C27 C26 C31 C30 -3.6(3) . . . . ?
B1 C26 C31 C30 -177.5(2) . . . . ?
C37 C32 C33 F11 -173.55(19) . . . . ?
B1 C32 C33 F11 -1.7(3) . . . . ?
C37 C32 C33 C34 4.5(3) . . . . ?
B1 C32 C33 C34 176.4(2) . . . . ?
F11 C33 C34 F12 -3.3(3) . . . . ?
C32 C33 C34 F12 178.5(2) . . . . ?
F11 C33 C34 C35 175.3(2) . . . . ?
C32 C33 C34 C35 -2.9(4) . . . . ?
F12 C34 C35 F13 -0.4(4) . . . . ?
C33 C34 C35 F13 -179.0(2) . . . . ?
F12 C34 C35 C36 178.4(2) . . . . ?
C33 C34 C35 C36 -0.2(4) . . . . ?
F13 C35 C36 F14 -0.9(3) . . . . ?
C34 C35 C36 F14 -179.7(2) . . . . ?
F13 C35 C36 C37 179.9(2) . . . . ?
C34 C35 C36 C37 1.0(3) . . . . ?
F14 C36 C37 F15 0.4(3) . . . . ?
C35 C36 C37 F15 179.62(19) . . . . ?
F14 C36 C37 C32 -178.19(19) . . . . ?
C35 C36 C37 C32 1.1(3) . . . . ?
C33 C32 C37 F15 177.87(17) . . . . ?
B1 C32 C37 F15 5.2(3) . . . . ?
C33 C32 C37 C36 -3.6(3) . . . . ?
B1 C32 C37 C36 -176.34(19) . . . . ?
O1 C38 C39 C40 17.1(5) . . . . ?
C38 C39 C40 C41 -2.5(5) . . . . ?
C39 C40 C41 O1 -12.9(5) . . . . ?
N2 C1 N1 C2 -1.8(2) . . . . ?
B1 C1 N1 C2 173.02(19) . . . . ?
N2 C1 N1 P1 -179.36(14) . . . . ?
B1 C1 N1 P1 -4.5(3) . . . . ?
C3 C2 N1 C1 0.8(2) . . . . ?
C3 C2 N1 P1 178.65(15) . . . . ?
N1 C1 N2 C3 2.2(2) . . . . ?
B1 C1 N2 C3 -173.08(17) . . . . ?
N1 C1 N2 P2 -163.44(14) . . . . ?
B1 C1 N2 P2 21.2(3) . . . . ?
C2 C3 N2 C1 -1.8(2) . . . . ?
C2 C3 N2 P2 165.54(15) . . . . ?
C21 C20 B1 C26 174.71(19) . . . . ?
C25 C20 B1 C26 -6.4(3) . . . . ?
C21 C20 B1 C32 61.7(2) . . . . ?
C25 C20 B1 C32 -119.4(2) . . . . ?
C21 C20 B1 C1 -64.6(2) . . . . ?
C25 C20 B1 C1 114.2(2) . . . . ?
C27 C26 B1 C20 129.9(2) . . . . ?
C31 C26 B1 C20 -57.1(2) . . . . ?
C27 C26 B1 C32 -110.7(2) . . . . ?
C31 C26 B1 C32 62.3(2) . . . . ?
C27 C26 B1 C1 12.2(3) . . . . ?
C31 C26 B1 C1 -174.88(18) . . . . ?
C37 C32 B1 C20 168.45(17) . . . . ?
C33 C32 B1 C20 -2.9(3) . . . . ?
C37 C32 B1 C26 49.7(2) . . . . ?
C33 C32 B1 C26 -121.6(2) . . . . ?
C37 C32 B1 C1 -70.3(2) . . . . ?
C33 C32 B1 C1 118.4(2) . . . . ?
N1 C1 B1 C20 135.2(2) . . . . ?
N2 C1 B1 C20 -50.8(2) . . . . ?
N1 C1 B1 C26 -104.0(2) . . . . ?
N2 C1 B1 C26 70.0(2) . . . . ?
N1 C1 B1 C32 10.7(3) . . . . ?
N2 C1 B1 C32 -175.28(17) . . . . ?
C1 N1 P1 C8 -114.79(18) . . . . ?
C2 N1 P1 C8 67.89(17) . . . . ?
C1 N1 P1 C4 131.75(17) . . . . ?
C2 N1 P1 C4 -45.58(17) . . . . ?
C10 C8 P1 N1 -43.11(19) . . . . ?
C11 C8 P1 N1 78.26(18) . . . . ?
C9 C8 P1 N1 -168.17(15) . . . . ?
C10 C8 P1 C4 64.4(2) . . . . ?
C11 C8 P1 C4 -174.18(17) . . . . ?
C9 C8 P1 C4 -60.62(18) . . . . ?
C1 N2 P2 C12 -128.74(18) . . . . ?
C3 N2 P2 C12 66.76(18) . . . . ?
C1 N2 P2 C16 117.55(18) . . . . ?
C3 N2 P2 C16 -46.94(18) . . . . ?
C13 C12 P2 N2 -41.4(2) . . . . ?
C15 C12 P2 N2 80.0(2) . . . . ?
C14 C12 P2 N2 -166.22(19) . . . . ?
C13 C12 P2 C16 65.6(2) . . . . ?
C15 C12 P2 C16 -173.03(19) . . . . ?
C14 C12 P2 C16 -59.3(2) . . . . ?
C40 C41 O1 C38 24.6(5) . . . . ?
C39 C38 O1 C41 -26.7(5) . . . . ?

_refine_diff_density_max         0.399
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.050

_shelxl_version_number           2013-4



_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
