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

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

data_cj1095
_database_code_depnum_ccdc_archive 'CCDC 1401422'
_audit_update_record             
;
2015-05-18 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C47 H42 N P'
_chemical_formula_weight         651.79

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   9.1571(6)
_cell_length_b                   41.566(3)
_cell_length_c                   9.5665(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.692(6)
_cell_angle_gamma                90.00
_cell_volume                     3552.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1384
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.983
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_process_details   'Sortav (Blessing)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex X8'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17730
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0575
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.93
_diffrn_reflns_theta_max         25.50
_reflns_number_total             6603
_reflns_number_gt                5065
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0167P)²+2.4894P] 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         6603
_refine_ls_number_parameters     444
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0482
_refine_ls_wR_factor_ref         0.0930
_refine_ls_wR_factor_gt          0.0843
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.27599(6) 0.123359(13) 0.47540(5) 0.01542(12) Uani 1 1 d . . .
N1 N 0.20106(17) 0.12519(4) 0.62400(15) 0.0160(4) Uani 1 1 d . . .
H1 H 0.1036 0.1273 0.6136 0.019 Uiso 1 1 calc R . .
C1 C 0.2940(2) 0.12335(5) 0.76473(18) 0.0144(4) Uani 1 1 d . . .
C2 C 0.2878(2) 0.09591(5) 0.84943(19) 0.0147(4) Uani 1 1 d . . .
C3 C 0.3692(2) 0.09567(5) 0.99058(19) 0.0156(4) Uani 1 1 d . . .
H3 H 0.3613 0.0776 1.0493 0.019 Uiso 1 1 calc R . .
C4 C 0.4615(2) 0.12107(5) 1.04815(19) 0.0152(4) Uani 1 1 d . . .
C5 C 0.4743(2) 0.14677(5) 0.95827(19) 0.0158(4) Uani 1 1 d . . .
H5 H 0.5439 0.1634 0.9931 0.019 Uiso 1 1 calc R . .
C6 C 0.3886(2) 0.14892(5) 0.81916(19) 0.0147(4) Uani 1 1 d . . .
C7 C 0.1878(2) 0.06790(5) 0.78303(19) 0.0164(4) Uani 1 1 d . . .
H7 H 0.1980 0.0668 0.6812 0.020 Uiso 1 1 calc R . .
C8 C 0.2374(2) 0.03500(5) 0.84680(19) 0.0163(4) Uani 1 1 d . . .
C9 C 0.1847(2) 0.02162(5) 0.9599(2) 0.0202(5) Uani 1 1 d . . .
H9 H 0.1157 0.0333 1.0014 0.024 Uiso 1 1 calc R . .
C10 C 0.2324(2) -0.00861(5) 1.0120(2) 0.0222(5) Uani 1 1 d . . .
H10 H 0.1959 -0.0175 1.0893 0.027 Uiso 1 1 calc R . .
C11 C 0.3321(2) -0.02589(5) 0.9531(2) 0.0222(5) Uani 1 1 d . . .
H11 H 0.3644 -0.0465 0.9898 0.027 Uiso 1 1 calc R . .
C12 C 0.3849(2) -0.01308(5) 0.8402(2) 0.0232(5) Uani 1 1 d . . .
H12 H 0.4536 -0.0249 0.7989 0.028 Uiso 1 1 calc R . .
C13 C 0.3373(2) 0.01707(5) 0.7878(2) 0.0214(5) Uani 1 1 d . . .
H13 H 0.3735 0.0257 0.7100 0.026 Uiso 1 1 calc R . .
C14 C 0.0221(2) 0.07445(5) 0.7751(2) 0.0174(4) Uani 1 1 d . . .
C15 C -0.0286(2) 0.09035(5) 0.8829(2) 0.0233(5) Uani 1 1 d . . .
H15 H 0.0414 0.0980 0.9645 0.028 Uiso 1 1 calc R . .
C16 C -0.1805(2) 0.09518(5) 0.8728(2) 0.0296(5) Uani 1 1 d . . .
H16 H -0.2135 0.1060 0.9478 0.036 Uiso 1 1 calc R . .
C17 C -0.2840(2) 0.08445(6) 0.7548(2) 0.0316(6) Uani 1 1 d . . .
H17 H -0.3880 0.0877 0.7483 0.038 Uiso 1 1 calc R . .
C18 C -0.2347(2) 0.06900(6) 0.6463(2) 0.0317(6) Uani 1 1 d . . .
H18 H -0.3052 0.0616 0.5645 0.038 Uiso 1 1 calc R . .
C19 C -0.0832(2) 0.06423(5) 0.6556(2) 0.0242(5) Uani 1 1 d . . .
H19 H -0.0507 0.0538 0.5793 0.029 Uiso 1 1 calc R . .
C20 C 0.3961(2) 0.17971(5) 0.73364(19) 0.0157(4) Uani 1 1 d . . .
H20 H 0.3505 0.1744 0.6314 0.019 Uiso 1 1 calc R . .
C21 C 0.5589(2) 0.18868(5) 0.73871(18) 0.0158(4) Uani 1 1 d . . .
C22 C 0.6462(2) 0.16690(5) 0.6827(2) 0.0204(5) Uani 1 1 d . . .
H22 H 0.6025 0.1474 0.6416 0.024 Uiso 1 1 calc R . .
C23 C 0.7953(2) 0.17301(5) 0.6855(2) 0.0238(5) Uani 1 1 d . . .
H23 H 0.8529 0.1578 0.6469 0.029 Uiso 1 1 calc R . .
C24 C 0.8603(2) 0.20134(5) 0.7444(2) 0.0226(5) Uani 1 1 d . . .
H24 H 0.9627 0.2057 0.7467 0.027 Uiso 1 1 calc R . .
C25 C 0.7747(2) 0.22325(5) 0.7996(2) 0.0227(5) Uani 1 1 d . . .
H25 H 0.8188 0.2428 0.8401 0.027 Uiso 1 1 calc R . .
C26 C 0.6251(2) 0.21710(5) 0.79684(19) 0.0191(4) Uani 1 1 d . . .
H26 H 0.5677 0.2325 0.8350 0.023 Uiso 1 1 calc R . .
C27 C 0.3034(2) 0.20724(5) 0.77454(19) 0.0165(4) Uani 1 1 d . . .
C28 C 0.2806(2) 0.21181(5) 0.9121(2) 0.0203(5) Uani 1 1 d . . .
H28 H 0.3206 0.1967 0.9852 0.024 Uiso 1 1 calc R . .
C29 C 0.2002(2) 0.23806(5) 0.9443(2) 0.0225(5) Uani 1 1 d . . .
H29 H 0.1872 0.2410 1.0394 0.027 Uiso 1 1 calc R . .
C30 C 0.1390(2) 0.25997(5) 0.8394(2) 0.0238(5) Uani 1 1 d . . .
H30 H 0.0841 0.2779 0.8617 0.029 Uiso 1 1 calc R . .
C31 C 0.1586(2) 0.25550(5) 0.7011(2) 0.0235(5) Uani 1 1 d . . .
H31 H 0.1158 0.2703 0.6279 0.028 Uiso 1 1 calc R . .
C32 C 0.2406(2) 0.22947(5) 0.6695(2) 0.0197(5) Uani 1 1 d . . .
H32 H 0.2541 0.2268 0.5746 0.024 Uiso 1 1 calc R . .
C33 C 0.5405(2) 0.12161(5) 1.20630(19) 0.0186(4) Uani 1 1 d . . .
H33 H 0.4813 0.1078 1.2590 0.022 Uiso 1 1 calc R . .
C34 C 0.5470(2) 0.15533(5) 1.2712(2) 0.0238(5) Uani 1 1 d . . .
H34A H 0.6147 0.1688 1.2301 0.036 Uiso 1 1 calc R . .
H34B H 0.5839 0.1540 1.3753 0.036 Uiso 1 1 calc R . .
H34C H 0.4466 0.1648 1.2499 0.036 Uiso 1 1 calc R . .
C35 C 0.6987(2) 0.10804(6) 1.2338(2) 0.0303(6) Uani 1 1 d . . .
H35A H 0.6958 0.0861 1.1959 0.045 Uiso 1 1 calc R . .
H35B H 0.7415 0.1077 1.3371 0.045 Uiso 1 1 calc R . .
H35C H 0.7607 0.1216 1.1860 0.045 Uiso 1 1 calc R . .
C36 C 0.1438(2) 0.14865(5) 0.35263(19) 0.0171(4) Uani 1 1 d . . .
C37 C 0.1346(2) 0.14634(5) 0.2048(2) 0.0217(5) Uani 1 1 d . . .
H37 H 0.1918 0.1305 0.1691 0.026 Uiso 1 1 calc R . .
C38 C 0.0429(2) 0.16687(6) 0.1104(2) 0.0255(5) Uani 1 1 d . . .
H38 H 0.0369 0.1650 0.0104 0.031 Uiso 1 1 calc R . .
C39 C -0.0400(2) 0.19020(6) 0.1615(2) 0.0283(5) Uani 1 1 d . . .
H39 H -0.1029 0.2043 0.0967 0.034 Uiso 1 1 calc R . .
C40 C -0.0308(2) 0.19283(5) 0.3069(2) 0.0257(5) Uani 1 1 d . . .
H40 H -0.0874 0.2089 0.3420 0.031 Uiso 1 1 calc R . .
C41 C 0.0601(2) 0.17232(5) 0.4021(2) 0.0197(5) Uani 1 1 d . . .
H41 H 0.0654 0.1744 0.5020 0.024 Uiso 1 1 calc R . .
C42 C 0.2182(2) 0.08346(5) 0.40248(19) 0.0178(4) Uani 1 1 d . . .
C43 C 0.3257(2) 0.05919(5) 0.4211(2) 0.0242(5) Uani 1 1 d . . .
H43 H 0.4276 0.0642 0.4608 0.029 Uiso 1 1 calc R . .
C44 C 0.2846(3) 0.02779(6) 0.3818(2) 0.0348(6) Uani 1 1 d . . .
H44 H 0.3583 0.0113 0.3946 0.042 Uiso 1 1 calc R . .
C45 C 0.1371(3) 0.02043(6) 0.3243(2) 0.0353(6) Uani 1 1 d . . .
H45 H 0.1092 -0.0012 0.2994 0.042 Uiso 1 1 calc R . .
C46 C 0.0303(3) 0.04412(6) 0.3026(2) 0.0317(6) Uani 1 1 d . . .
H46 H -0.0711 0.0390 0.2614 0.038 Uiso 1 1 calc R . .
C47 C 0.0703(2) 0.07546(5) 0.3408(2) 0.0254(5) Uani 1 1 d . . .
H47 H -0.0040 0.0918 0.3248 0.030 Uiso 1 1 calc R . .


_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
P1 N1 1.7106(15) . ?
P1 C36 1.823(2) . ?
P1 C42 1.832(2) . ?
N1 C1 1.428(2) . ?
C1 C6 1.397(3) . ?
C1 C2 1.407(3) . ?
C2 C3 1.392(3) . ?
C2 C7 1.530(3) . ?
C3 C4 1.388(3) . ?
C4 C5 1.392(3) . ?
C4 C33 1.527(2) . ?
C5 C6 1.391(2) . ?
C6 C20 1.529(3) . ?
C7 C8 1.525(3) . ?
C7 C14 1.528(3) . ?
C8 C13 1.392(3) . ?
C8 C9 1.394(3) . ?
C9 C10 1.387(3) . ?
C10 C11 1.376(3) . ?
C11 C12 1.383(3) . ?
C12 C13 1.384(3) . ?
C14 C15 1.388(3) . ?
C14 C19 1.390(3) . ?
C15 C16 1.388(3) . ?
C16 C17 1.379(3) . ?
C17 C18 1.378(3) . ?
C18 C19 1.385(3) . ?
C20 C27 1.526(3) . ?
C20 C21 1.527(3) . ?
C21 C26 1.387(3) . ?
C21 C22 1.391(3) . ?
C22 C23 1.383(3) . ?
C23 C24 1.382(3) . ?
C24 C25 1.381(3) . ?
C25 C26 1.388(3) . ?
C27 C28 1.390(3) . ?
C27 C32 1.393(3) . ?
C28 C29 1.388(3) . ?
C29 C30 1.380(3) . ?
C30 C31 1.386(3) . ?
C31 C32 1.388(3) . ?
C33 C35 1.523(3) . ?
C33 C34 1.529(3) . ?
C36 C41 1.393(3) . ?
C36 C37 1.401(3) . ?
C37 C38 1.384(3) . ?
C38 C39 1.385(3) . ?
C39 C40 1.380(3) . ?
C40 C41 1.384(3) . ?
C42 C47 1.393(3) . ?
C42 C43 1.393(3) . ?
C43 C44 1.387(3) . ?
C44 C45 1.376(3) . ?
C45 C46 1.372(3) . ?
C46 C47 1.381(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
N1 P1 C36 100.31(8) . . ?
N1 P1 C42 102.80(8) . . ?
C36 P1 C42 100.44(9) . . ?
C1 N1 P1 121.08(13) . . ?
C6 C1 C2 120.14(16) . . ?
C6 C1 N1 120.19(17) . . ?
C2 C1 N1 119.66(17) . . ?
C3 C2 C1 118.91(18) . . ?
C3 C2 C7 122.78(17) . . ?
C1 C2 C7 118.29(16) . . ?
C4 C3 C2 121.95(18) . . ?
C3 C4 C5 117.71(16) . . ?
C3 C4 C33 121.26(17) . . ?
C5 C4 C33 120.97(17) . . ?
C6 C5 C4 122.25(18) . . ?
C5 C6 C1 118.73(18) . . ?
C5 C6 C20 118.91(17) . . ?
C1 C6 C20 122.31(16) . . ?
C8 C7 C14 112.62(16) . . ?
C8 C7 C2 114.70(15) . . ?
C14 C7 C2 112.47(16) . . ?
C13 C8 C9 118.12(18) . . ?
C13 C8 C7 118.85(17) . . ?
C9 C8 C7 123.02(18) . . ?
C10 C9 C8 120.37(19) . . ?
C11 C10 C9 120.70(19) . . ?
C10 C11 C12 119.75(19) . . ?
C11 C12 C13 119.7(2) . . ?
C12 C13 C8 121.40(19) . . ?
C15 C14 C19 118.17(19) . . ?
C15 C14 C7 122.63(17) . . ?
C19 C14 C7 119.20(18) . . ?
C14 C15 C16 120.7(2) . . ?
C17 C16 C15 120.5(2) . . ?
C18 C17 C16 119.2(2) . . ?
C17 C18 C19 120.5(2) . . ?
C18 C19 C14 120.8(2) . . ?
C27 C20 C21 113.76(16) . . ?
C27 C20 C6 113.42(15) . . ?
C21 C20 C6 110.24(15) . . ?
C26 C21 C22 118.07(19) . . ?
C26 C21 C20 123.97(18) . . ?
C22 C21 C20 117.96(18) . . ?
C23 C22 C21 121.5(2) . . ?
C24 C23 C22 119.9(2) . . ?
C25 C24 C23 119.2(2) . . ?
C24 C25 C26 120.8(2) . . ?
C21 C26 C25 120.5(2) . . ?
C28 C27 C32 117.93(19) . . ?
C28 C27 C20 123.55(17) . . ?
C32 C27 C20 118.50(17) . . ?
C29 C28 C27 120.98(19) . . ?
C30 C29 C28 120.51(19) . . ?
C29 C30 C31 119.3(2) . . ?
C30 C31 C32 120.16(19) . . ?
C31 C32 C27 121.15(18) . . ?
C35 C33 C4 113.03(16) . . ?
C35 C33 C34 108.59(17) . . ?
C4 C33 C34 112.56(16) . . ?
C41 C36 C37 118.42(18) . . ?
C41 C36 P1 121.70(14) . . ?
C37 C36 P1 119.65(15) . . ?
C38 C37 C36 120.6(2) . . ?
C37 C38 C39 120.19(19) . . ?
C40 C39 C38 119.6(2) . . ?
C39 C40 C41 120.6(2) . . ?
C40 C41 C36 120.51(18) . . ?
C47 C42 C43 118.3(2) . . ?
C47 C42 P1 123.38(16) . . ?
C43 C42 P1 118.03(15) . . ?
C44 C43 C42 120.3(2) . . ?
C45 C44 C43 120.1(2) . . ?
C46 C45 C44 120.4(2) . . ?
C45 C46 C47 119.9(2) . . ?
C46 C47 C42 121.0(2) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.049
####################################################################### 
# 
# 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_cj1089
_database_code_depnum_ccdc_archive 'CCDC 1401423'
_audit_update_record             
;
2015-07-22 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C43 H52 N3 P'
_chemical_formula_weight         641.85

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)

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

_cell_length_a                   8.5767(6)
_cell_length_b                   18.5068(14)
_cell_length_c                   11.4751(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.692(7)
_cell_angle_gamma                90.00
_cell_volume                     1819.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             692
_exptl_absorpt_coefficient_mu    0.109
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.961
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_process_details   'Sortav (Blessing)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex X8'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8742
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0592
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.03
_diffrn_reflns_theta_max         25.50
_reflns_number_total             5873
_reflns_number_gt                5145
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0415P)²+0.0619P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(9)
_refine_ls_number_reflns         5873
_refine_ls_number_parameters     430
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0414
_refine_ls_wR_factor_ref         0.0949
_refine_ls_wR_factor_gt          0.0876
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.92102(7) 0.02936(3) 0.18220(6) 0.02153(16) Uani 1 1 d . . .
N1 N 0.9380(2) 0.11789(11) 0.14230(17) 0.0193(5) Uani 1 1 d . . .
H1 H 1.0304 0.1384 0.1403 0.023 Uiso 1 1 calc R . .
C5 C 0.6115(3) 0.25007(13) 0.1574(2) 0.0188(5) Uani 1 1 d . . .
H5 H 0.5752 0.2852 0.2101 0.023 Uiso 1 1 calc R . .
C7 C 0.8289(3) 0.22145(13) 0.3081(2) 0.0195(5) Uani 1 1 d . . .
H7 H 0.8781 0.1742 0.3307 0.023 Uiso 1 1 calc R . .
C3 C 0.5876(3) 0.18937(14) -0.0251(2) 0.0202(5) Uani 1 1 d . . .
H3 H 0.5325 0.1815 -0.0978 0.024 Uiso 1 1 calc R . .
C21 C 0.6564(3) 0.05450(12) -0.1545(2) 0.0196(6) Uani 1 1 d . . .
N3 N 0.9034(2) 0.02531(13) 0.32822(18) 0.0287(5) Uani 1 1 d . . .
C2 C 0.7210(3) 0.14810(12) 0.0027(2) 0.0182(5) Uani 1 1 d . . .
C1 C 0.7990(3) 0.15839(13) 0.1120(2) 0.0182(5) Uani 1 1 d . . .
N2 N 1.1127(2) 0.00601(11) 0.17176(19) 0.0258(5) Uani 1 1 d . . .
C38 C 1.1427(3) -0.07139(14) 0.1845(2) 0.0301(7) Uani 1 1 d . . .
H38A H 1.0756 -0.0908 0.2450 0.036 Uiso 1 1 calc R . .
H38B H 1.2527 -0.0783 0.2124 0.036 Uiso 1 1 calc R . .
C4 C 0.5328(3) 0.24167(14) 0.0506(2) 0.0194(5) Uani 1 1 d . . .
C20 C 0.7857(3) 0.09595(13) -0.0861(2) 0.0204(6) Uani 1 1 d . . .
H20 H 0.8471 0.0590 -0.0400 0.024 Uiso 1 1 calc R . .
C26 C 0.5673(3) 0.00521(14) -0.0935(2) 0.0273(6) Uani 1 1 d . . .
H26 H 0.5871 -0.0008 -0.0119 0.033 Uiso 1 1 calc R . .
C27 C 0.9008(3) 0.13324(14) -0.1637(2) 0.0209(6) Uani 1 1 d . . .
C33 C 0.3900(3) 0.28788(14) 0.0200(2) 0.0230(6) Uani 1 1 d . . .
H33 H 0.3858 0.3266 0.0805 0.028 Uiso 1 1 calc R . .
C8 C 0.7194(3) 0.24044(14) 0.4047(2) 0.0216(6) Uani 1 1 d . . .
C24 C 0.4206(3) -0.02708(14) -0.2691(3) 0.0303(7) Uani 1 1 d . . .
H24 H 0.3401 -0.0544 -0.3080 0.036 Uiso 1 1 calc R . .
C22 C 0.6258(3) 0.06129(14) -0.2736(2) 0.0256(6) Uani 1 1 d . . .
H22 H 0.6857 0.0940 -0.3170 0.031 Uiso 1 1 calc R . .
C6 C 0.7425(3) 0.20893(12) 0.1908(2) 0.0185(5) Uani 1 1 d . . .
C32 C 0.8668(3) 0.19798(15) -0.2206(2) 0.0258(6) Uani 1 1 d . . .
H32 H 0.7699 0.2211 -0.2091 0.031 Uiso 1 1 calc R . .
C14 C 0.9623(3) 0.27471(14) 0.2968(2) 0.0207(6) Uani 1 1 d . . .
C31 C 0.9715(3) 0.22947(16) -0.2938(2) 0.0316(7) Uani 1 1 d . . .
H31 H 0.9454 0.2734 -0.3328 0.038 Uiso 1 1 calc R . .
C28 C 1.0446(3) 0.10119(15) -0.1816(2) 0.0287(6) Uani 1 1 d . . .
H28 H 1.0707 0.0568 -0.1440 0.034 Uiso 1 1 calc R . .
C9 C 0.6105(3) 0.18865(15) 0.4365(2) 0.0295(6) Uani 1 1 d . . .
H9 H 0.6040 0.1440 0.3957 0.035 Uiso 1 1 calc R . .
C25 C 0.4510(3) -0.03488(15) -0.1503(2) 0.0298(7) Uani 1 1 d . . .
H25 H 0.3914 -0.0680 -0.1075 0.036 Uiso 1 1 calc R . .
C13 C 0.7254(3) 0.30488(15) 0.4652(2) 0.0286(6) Uani 1 1 d . . .
H13 H 0.7985 0.3408 0.4451 0.034 Uiso 1 1 calc R . .
C11 C 0.5213(3) 0.26570(18) 0.5862(2) 0.0358(7) Uani 1 1 d . . .
H11 H 0.4553 0.2741 0.6490 0.043 Uiso 1 1 calc R . .
C23 C 0.5085(3) 0.02086(16) -0.3304(2) 0.0304(6) Uani 1 1 d . . .
H23 H 0.4889 0.0263 -0.4121 0.036 Uiso 1 1 calc R . .
C34 C 0.2392(3) 0.24349(16) 0.0255(3) 0.0331(7) Uani 1 1 d . . .
H34A H 0.2412 0.2038 -0.0309 0.050 Uiso 1 1 calc R . .
H34B H 0.1491 0.2746 0.0066 0.050 Uiso 1 1 calc R . .
H34C H 0.2311 0.2237 0.1042 0.050 Uiso 1 1 calc R . .
C19 C 1.1073(3) 0.26120(15) 0.3529(2) 0.0290(6) Uani 1 1 d . . .
H19 H 1.1222 0.2184 0.3977 0.035 Uiso 1 1 calc R . .
C30 C 1.1138(3) 0.19696(16) -0.3101(3) 0.0340(7) Uani 1 1 d . . .
H30 H 1.1860 0.2185 -0.3599 0.041 Uiso 1 1 calc R . .
C18 C 1.2299(3) 0.30958(17) 0.3441(2) 0.0339(7) Uani 1 1 d . . .
H18 H 1.3284 0.2990 0.3816 0.041 Uiso 1 1 calc R . .
C15 C 0.9456(3) 0.33749(14) 0.2327(2) 0.0291(6) Uani 1 1 d . . .
H15 H 0.8489 0.3472 0.1920 0.035 Uiso 1 1 calc R . .
C17 C 1.2104(3) 0.37231(15) 0.2821(2) 0.0317(7) Uani 1 1 d . . .
H17 H 1.2941 0.4056 0.2774 0.038 Uiso 1 1 calc R . .
C36 C 1.2354(3) 0.04624(14) 0.1157(2) 0.0277(6) Uani 1 1 d . . .
H36A H 1.1879 0.0880 0.0733 0.033 Uiso 1 1 calc R . .
H36B H 1.2836 0.0146 0.0578 0.033 Uiso 1 1 calc R . .
C16 C 1.0664(3) 0.38661(15) 0.2261(3) 0.0331(7) Uani 1 1 d . . .
H16 H 1.0510 0.4302 0.1833 0.040 Uiso 1 1 calc R . .
C40 C 1.0173(3) 0.05463(16) 0.4147(2) 0.0343(7) Uani 1 1 d . . .
H40A H 0.9617 0.0874 0.4668 0.041 Uiso 1 1 calc R . .
H40B H 1.0932 0.0842 0.3732 0.041 Uiso 1 1 calc R . .
C37 C 1.3619(4) 0.0735(2) 0.2020(3) 0.0481(8) Uani 1 1 d . . .
H37A H 1.3173 0.1091 0.2542 0.072 Uiso 1 1 calc R . .
H37B H 1.4454 0.0962 0.1594 0.072 Uiso 1 1 calc R . .
H37C H 1.4047 0.0329 0.2480 0.072 Uiso 1 1 calc R . .
C10 C 0.5124(3) 0.20143(17) 0.5261(2) 0.0339(7) Uani 1 1 d . . .
H10 H 0.4386 0.1658 0.5464 0.041 Uiso 1 1 calc R . .
C29 C 1.1505(3) 0.13326(16) -0.2538(2) 0.0323(7) Uani 1 1 d . . .
H29 H 1.2487 0.1110 -0.2642 0.039 Uiso 1 1 calc R . .
C41 C 1.1072(4) 0.00047(18) 0.4895(3) 0.0499(9) Uani 1 1 d . . .
H41A H 1.0346 -0.0270 0.5358 0.075 Uiso 1 1 calc R . .
H41B H 1.1824 0.0259 0.5418 0.075 Uiso 1 1 calc R . .
H41C H 1.1630 -0.0327 0.4395 0.075 Uiso 1 1 calc R . .
C43 C 0.7747(5) -0.0868(2) 0.3914(4) 0.0687(12) Uani 1 1 d . . .
H43A H 0.7911 -0.1109 0.3169 0.103 Uiso 1 1 calc R . .
H43B H 0.6771 -0.1041 0.4228 0.103 Uiso 1 1 calc R . .
H43C H 0.8620 -0.0978 0.4467 0.103 Uiso 1 1 calc R . .
C39 C 1.1137(4) -0.11448(16) 0.0736(3) 0.0404(7) Uani 1 1 d . . .
H39A H 1.0034 -0.1107 0.0479 0.061 Uiso 1 1 calc R . .
H39B H 1.1402 -0.1653 0.0883 0.061 Uiso 1 1 calc R . .
H39C H 1.1788 -0.0954 0.0127 0.061 Uiso 1 1 calc R . .
C12 C 0.6264(3) 0.31796(18) 0.5550(2) 0.0371(7) Uani 1 1 d . . .
H12 H 0.6309 0.3629 0.5950 0.044 Uiso 1 1 calc R . .
C42 C 0.7653(4) -0.0086(2) 0.3730(3) 0.0544(10) Uani 1 1 d . . .
H42A H 0.6756 0.0014 0.3179 0.065 Uiso 1 1 calc R . .
H42B H 0.7430 0.0145 0.4481 0.065 Uiso 1 1 calc R . .
C35 C 0.3988(4) 0.32497(17) -0.0977(3) 0.0405(8) Uani 1 1 d . . .
H35A H 0.4953 0.3532 -0.0992 0.061 Uiso 1 1 calc R . .
H35B H 0.3088 0.3571 -0.1103 0.061 Uiso 1 1 calc R . .
H35C H 0.3980 0.2884 -0.1596 0.061 Uiso 1 1 calc R . .


_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
P1 N3 1.691(2) . ?
P1 N1 1.709(2) . ?
P1 N2 1.709(2) . ?
N1 C1 1.437(3) . ?
C5 C4 1.380(3) . ?
C5 C6 1.396(3) . ?
C7 C14 1.521(3) . ?
C7 C6 1.523(3) . ?
C7 C8 1.527(3) . ?
C3 C4 1.396(3) . ?
C3 C2 1.400(3) . ?
C21 C22 1.385(3) . ?
C21 C26 1.398(3) . ?
C21 C20 1.534(3) . ?
N3 C42 1.455(3) . ?
N3 C40 1.464(4) . ?
C2 C1 1.407(3) . ?
C2 C20 1.526(3) . ?
C1 C6 1.403(3) . ?
N2 C38 1.461(3) . ?
N2 C36 1.462(3) . ?
C38 C39 1.512(4) . ?
C4 C33 1.521(3) . ?
C20 C27 1.526(3) . ?
C26 C25 1.382(4) . ?
C27 C32 1.389(4) . ?
C27 C28 1.392(4) . ?
C33 C35 1.521(4) . ?
C33 C34 1.536(4) . ?
C8 C13 1.380(4) . ?
C8 C9 1.398(4) . ?
C24 C23 1.378(4) . ?
C24 C25 1.383(4) . ?
C22 C23 1.391(4) . ?
C32 C31 1.387(4) . ?
C14 C15 1.379(4) . ?
C14 C19 1.396(4) . ?
C31 C30 1.381(4) . ?
C28 C29 1.391(4) . ?
C9 C10 1.380(4) . ?
C13 C12 1.387(4) . ?
C11 C10 1.375(4) . ?
C11 C12 1.381(4) . ?
C19 C18 1.388(4) . ?
C30 C29 1.374(4) . ?
C18 C17 1.368(4) . ?
C15 C16 1.383(4) . ?
C17 C16 1.390(4) . ?
C36 C37 1.521(4) . ?
C40 C41 1.508(4) . ?
C43 C42 1.464(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 P1 N1 108.69(11) . . ?
N3 P1 N2 100.92(11) . . ?
N1 P1 N2 97.43(10) . . ?
C1 N1 P1 118.99(15) . . ?
C4 C5 C6 122.4(2) . . ?
C14 C7 C6 111.11(19) . . ?
C14 C7 C8 113.8(2) . . ?
C6 C7 C8 112.7(2) . . ?
C4 C3 C2 122.1(2) . . ?
C22 C21 C26 118.1(2) . . ?
C22 C21 C20 123.9(2) . . ?
C26 C21 C20 118.0(2) . . ?
C42 N3 C40 116.7(2) . . ?
C42 N3 P1 118.7(2) . . ?
C40 N3 P1 124.56(17) . . ?
C3 C2 C1 118.6(2) . . ?
C3 C2 C20 120.8(2) . . ?
C1 C2 C20 120.5(2) . . ?
C6 C1 C2 120.0(2) . . ?
C6 C1 N1 120.0(2) . . ?
C2 C1 N1 120.0(2) . . ?
C38 N2 C36 114.57(19) . . ?
C38 N2 P1 113.98(16) . . ?
C36 N2 P1 128.05(17) . . ?
N2 C38 C39 114.3(2) . . ?
C5 C4 C3 117.7(2) . . ?
C5 C4 C33 119.7(2) . . ?
C3 C4 C33 122.5(2) . . ?
C27 C20 C2 111.66(19) . . ?
C27 C20 C21 113.6(2) . . ?
C2 C20 C21 112.38(19) . . ?
C25 C26 C21 120.9(3) . . ?
C32 C27 C28 117.8(2) . . ?
C32 C27 C20 122.5(2) . . ?
C28 C27 C20 119.7(2) . . ?
C35 C33 C4 112.7(2) . . ?
C35 C33 C34 110.8(2) . . ?
C4 C33 C34 111.1(2) . . ?
C13 C8 C9 118.1(2) . . ?
C13 C8 C7 123.7(2) . . ?
C9 C8 C7 118.2(2) . . ?
C23 C24 C25 119.2(3) . . ?
C21 C22 C23 120.9(2) . . ?
C5 C6 C1 119.0(2) . . ?
C5 C6 C7 120.8(2) . . ?
C1 C6 C7 120.1(2) . . ?
C31 C32 C27 121.3(2) . . ?
C15 C14 C19 117.7(2) . . ?
C15 C14 C7 122.1(2) . . ?
C19 C14 C7 120.1(2) . . ?
C30 C31 C32 120.0(3) . . ?
C29 C28 C27 120.9(3) . . ?
C10 C9 C8 121.0(3) . . ?
C26 C25 C24 120.5(2) . . ?
C8 C13 C12 121.0(3) . . ?
C10 C11 C12 119.8(2) . . ?
C24 C23 C22 120.5(3) . . ?
C18 C19 C14 120.8(3) . . ?
C29 C30 C31 119.6(2) . . ?
C17 C18 C19 120.7(3) . . ?
C14 C15 C16 121.6(3) . . ?
C18 C17 C16 119.1(2) . . ?
N2 C36 C37 112.9(2) . . ?
C15 C16 C17 120.1(3) . . ?
N3 C40 C41 116.5(3) . . ?
C11 C10 C9 120.0(3) . . ?
C30 C29 C28 120.3(2) . . ?
C11 C12 C13 120.0(3) . . ?
N3 C42 C43 116.0(3) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.043
####################################################################### 
# 
# 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_cj1096
_database_code_depnum_ccdc_archive 'CCDC 1401424'
_audit_update_record             
;
2015-05-18 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C50 H59 K N3 P'
_chemical_formula_weight         772.07

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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   18.506(4)
_cell_length_b                   12.825(3)
_cell_length_c                   18.632(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.72(3)
_cell_angle_gamma                90.00
_cell_volume                     4382.0(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1656
_exptl_absorpt_coefficient_mu    0.194
_exptl_absorpt_correction_type   multi-scan'
_exptl_absorpt_correction_T_min  0.983
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_process_details   XDS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71080
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'Australian Synchrotron'
_diffrn_radiation_monochromator  ?
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            50871
_diffrn_reflns_av_R_equivalents  0.0735
_diffrn_reflns_av_sigmaI/netI    0.0434
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.91
_diffrn_reflns_theta_max         27.00
_reflns_number_total             9538
_reflns_number_gt                6850
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Blu-Ice (McPhillips, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CifTAB

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1277P)²+4.5364P] 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         9538
_refine_ls_number_parameters     468
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.1050
_refine_ls_R_factor_gt           0.0776
_refine_ls_wR_factor_ref         0.2331
_refine_ls_wR_factor_gt          0.2091
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.034
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.33591(5) 0.27156(5) 0.20368(4) 0.0458(2) Uani 1 1 d . . .
P1 P 0.21773(5) 0.29795(6) 0.05472(4) 0.0388(2) Uani 1 1 d . . .
N1 N 0.25748(14) 0.39151(18) 0.10648(13) 0.0341(5) Uani 1 1 d . . .
C1 C 0.28838(16) 0.4811(2) 0.08258(14) 0.0297(6) Uani 1 1 d . . .
N2 N 0.14481(17) 0.3584(2) 0.00649(15) 0.0477(7) Uani 1 1 d . . .
C2 C 0.28356(17) 0.5744(2) 0.12328(14) 0.0309(6) Uani 1 1 d . . .
N3 N 0.18991(19) 0.2248(2) 0.12549(16) 0.0495(7) Uani 1 1 d . . .
C3 C 0.31410(17) 0.6669(2) 0.10325(15) 0.0332(6) Uani 1 1 d . . .
H3 H 0.3096 0.7276 0.1315 0.040 Uiso 1 1 calc R . .
C4 C 0.35103(19) 0.6737(2) 0.04338(16) 0.0371(7) Uani 1 1 d . . .
C5 C 0.35867(18) 0.5825(2) 0.00476(15) 0.0354(6) Uani 1 1 d . . .
H5 H 0.3847 0.5849 -0.0358 0.043 Uiso 1 1 calc R . .
C6 C 0.32951(17) 0.4875(2) 0.02343(14) 0.0311(6) Uani 1 1 d . . .
C7 C 0.3813(3) 0.7764(2) 0.0194(2) 0.0606(12) Uani 1 1 d . . .
H7 H 0.4187 0.7597 -0.0129 0.073 Uiso 1 1 calc R . .
C8 C 0.4177(2) 0.8435(3) 0.0809(3) 0.0625(11) Uani 1 1 d . . .
H8A H 0.3805 0.8718 0.1084 0.094 Uiso 1 1 calc R . .
H8B H 0.4438 0.9010 0.0611 0.094 Uiso 1 1 calc R . .
H8C H 0.4522 0.8011 0.1130 0.094 Uiso 1 1 calc R . .
C9 C 0.3207(4) 0.8379(4) -0.0250(3) 0.0959(18) Uani 1 1 d U . .
H9A H 0.3012 0.7975 -0.0679 0.144 Uiso 1 1 calc R . .
H9B H 0.3403 0.9042 -0.0402 0.144 Uiso 1 1 calc R . .
H9C H 0.2817 0.8517 0.0044 0.144 Uiso 1 1 calc R . .
C10 C 0.24691(17) 0.5674(2) 0.19144(14) 0.0325(6) Uani 1 1 d . . .
H10 H 0.2014 0.5257 0.1782 0.039 Uiso 1 1 calc R . .
C11 C 0.22282(19) 0.6733(2) 0.21696(17) 0.0389(7) Uani 1 1 d . . .
C12 C 0.2547(2) 0.7204(2) 0.28056(18) 0.0474(8) Uani 1 1 d . . .
H12 H 0.2936 0.6864 0.3100 0.057 Uiso 1 1 calc R . .
C13 C 0.2302(3) 0.8170(3) 0.3015(2) 0.0601(10) Uani 1 1 d . . .
H13 H 0.2518 0.8477 0.3456 0.072 Uiso 1 1 calc R . .
C14 C 0.1749(3) 0.8684(3) 0.2588(3) 0.0662(11) Uani 1 1 d . . .
H14 H 0.1578 0.9336 0.2740 0.079 Uiso 1 1 calc R . .
C15 C 0.1445(2) 0.8250(3) 0.1941(3) 0.0651(11) Uani 1 1 d . . .
H15 H 0.1081 0.8617 0.1632 0.078 Uiso 1 1 calc R . .
C16 C 0.1673(2) 0.7277(3) 0.1741(2) 0.0526(9) Uani 1 1 d . . .
H16 H 0.1447 0.6971 0.1303 0.063 Uiso 1 1 calc R . .
C17 C 0.29351(17) 0.5068(2) 0.25126(15) 0.0331(6) Uani 1 1 d . . .
C18 C 0.2605(2) 0.4532(2) 0.30340(16) 0.0417(7) Uani 1 1 d . . .
H18 H 0.2091 0.4558 0.3021 0.050 Uiso 1 1 calc R . .
C19 C 0.3026(2) 0.3959(3) 0.35758(17) 0.0464(8) Uani 1 1 d . . .
H19 H 0.2796 0.3590 0.3924 0.056 Uiso 1 1 calc R . .
C20 C 0.3776(2) 0.3927(2) 0.36063(17) 0.0436(8) Uani 1 1 d . . .
H20 H 0.4061 0.3541 0.3976 0.052 Uiso 1 1 calc R . .
C21 C 0.41087(19) 0.4465(2) 0.30917(17) 0.0404(7) Uani 1 1 d . . .
H21 H 0.4624 0.4446 0.3109 0.048 Uiso 1 1 calc R . .
C22 C 0.36897(18) 0.5030(2) 0.25529(15) 0.0362(6) Uani 1 1 d . . .
H22 H 0.3923 0.5397 0.2205 0.043 Uiso 1 1 calc R . .
C23 C 0.34985(18) 0.3861(2) -0.01147(15) 0.0336(6) Uani 1 1 d . . .
H23 H 0.3044 0.3432 -0.0192 0.040 Uiso 1 1 calc R . .
C24 C 0.37384(19) 0.4011(2) -0.08595(15) 0.0356(7) Uani 1 1 d . . .
C25 C 0.3224(2) 0.4379(3) -0.14188(17) 0.0453(8) Uani 1 1 d . . .
H25 H 0.2740 0.4511 -0.1326 0.054 Uiso 1 1 calc R . .
C26 C 0.3404(2) 0.4554(3) -0.21062(17) 0.0523(9) Uani 1 1 d . . .
H26 H 0.3052 0.4831 -0.2474 0.063 Uiso 1 1 calc R . .
C27 C 0.4099(2) 0.4323(3) -0.22544(18) 0.0515(9) Uani 1 1 d . . .
H27 H 0.4225 0.4436 -0.2726 0.062 Uiso 1 1 calc R . .
C28 C 0.4606(2) 0.3928(2) -0.17139(19) 0.0479(9) Uani 1 1 d . . .
H28 H 0.5081 0.3754 -0.1816 0.057 Uiso 1 1 calc R . .
C29 C 0.4427(2) 0.3782(2) -0.10165(17) 0.0404(7) Uani 1 1 d . . .
H29 H 0.4784 0.3521 -0.0646 0.048 Uiso 1 1 calc R . .
C30 C 0.40398(18) 0.3254(2) 0.04108(15) 0.0348(6) Uani 1 1 d . . .
C31 C 0.45762(18) 0.3750(2) 0.08872(16) 0.0378(7) Uani 1 1 d . . .
H31 H 0.4605 0.4489 0.0882 0.045 Uiso 1 1 calc R . .
C32 C 0.5070(2) 0.3193(2) 0.13703(18) 0.0429(7) Uani 1 1 d . . .
H32 H 0.5428 0.3550 0.1692 0.051 Uiso 1 1 calc R . .
C33 C 0.5036(2) 0.2108(2) 0.13784(17) 0.0438(8) Uani 1 1 d . . .
H33 H 0.5374 0.1719 0.1702 0.053 Uiso 1 1 calc R . .
C34 C 0.4507(2) 0.1602(2) 0.09117(17) 0.0431(8) Uani 1 1 d . . .
H34 H 0.4482 0.0863 0.0916 0.052 Uiso 1 1 calc R . .
C35 C 0.4014(2) 0.2163(2) 0.04372(16) 0.0394(7) Uani 1 1 d . . .
H35 H 0.3650 0.1801 0.0124 0.047 Uiso 1 1 calc R . .
C36 C 0.1162(2) 0.3164(3) -0.0648(2) 0.0578(10) Uani 1 1 d . . .
H36A H 0.1454 0.2548 -0.0749 0.069 Uiso 1 1 calc R . .
H36B H 0.1218 0.3696 -0.1021 0.069 Uiso 1 1 calc R . .
C37 C 0.0360(3) 0.2847(5) -0.0708(3) 0.0883(17) Uani 1 1 d . . .
H37A H 0.0306 0.2275 -0.0371 0.132 Uiso 1 1 calc R . .
H37B H 0.0191 0.2617 -0.1204 0.132 Uiso 1 1 calc R . .
H37C H 0.0068 0.3444 -0.0589 0.132 Uiso 1 1 calc R . .
C38 C 0.1114(2) 0.4548(3) 0.02635(19) 0.0517(9) Uani 1 1 d . . .
H38A H 0.1328 0.4740 0.0761 0.062 Uiso 1 1 calc R . .
H38B H 0.0587 0.4424 0.0269 0.062 Uiso 1 1 calc R . .
C39 C 0.1204(3) 0.5455(3) -0.0235(2) 0.0647(11) Uani 1 1 d . . .
H39A H 0.1723 0.5558 -0.0269 0.097 Uiso 1 1 calc R . .
H39B H 0.1004 0.6088 -0.0041 0.097 Uiso 1 1 calc R . .
H39C H 0.0942 0.5309 -0.0717 0.097 Uiso 1 1 calc R . .
C40 C 0.1627(3) 0.1208(3) 0.1009(3) 0.0778(15) Uani 1 1 d . . .
H40A H 0.1273 0.1286 0.0564 0.093 Uiso 1 1 calc R . .
H40B H 0.1368 0.0891 0.1387 0.093 Uiso 1 1 calc R . .
C41 C 0.2245(4) 0.0481(4) 0.0854(3) 0.101(2) Uani 1 1 d . . .
H41A H 0.2469 0.0755 0.0445 0.151 Uiso 1 1 calc R . .
H41B H 0.2047 -0.0216 0.0734 0.151 Uiso 1 1 calc R . .
H41C H 0.2613 0.0440 0.1283 0.151 Uiso 1 1 calc R . .
C42 C 0.1394(3) 0.2760(3) 0.1701(2) 0.0590(10) Uani 1 1 d . . .
H42A H 0.0889 0.2701 0.1451 0.071 Uiso 1 1 calc R . .
H42B H 0.1516 0.3510 0.1751 0.071 Uiso 1 1 calc R . .
C43 C 0.1437(3) 0.2272(4) 0.2456(2) 0.0696(12) Uani 1 1 d . . .
H43A H 0.1292 0.1537 0.2410 0.104 Uiso 1 1 calc R . .
H43B H 0.1108 0.2644 0.2737 0.104 Uiso 1 1 calc R . .
H43C H 0.1938 0.2321 0.2703 0.104 Uiso 1 1 calc R . .
C44 C 0.0182(4) 0.5047(6) 0.2196(4) 0.115(2) Uiso 1 1 d D . .
H44A H -0.0271 0.5377 0.1973 0.173 Uiso 1 1 calc R . .
H44B H 0.0109 0.4292 0.2223 0.173 Uiso 1 1 calc R . .
H44C H 0.0572 0.5191 0.1902 0.173 Uiso 1 1 calc R . .
C45 C 0.0395(4) 0.5485(5) 0.2960(3) 0.1062(19) Uiso 1 1 d D . .
C46 C 0.0599(4) 0.6469(6) 0.3130(4) 0.124(2) Uiso 1 1 d D . .
H46 H 0.0586 0.6956 0.2744 0.148 Uiso 1 1 calc R . .
C47 C 0.0828(6) 0.6831(8) 0.3829(5) 0.158(3) Uiso 1 1 d D . .
H47 H 0.0953 0.7547 0.3893 0.190 Uiso 1 1 calc R . .
C48 C 0.0881(6) 0.6208(8) 0.4421(6) 0.165(4) Uiso 1 1 d D . .
H48 H 0.1054 0.6410 0.4904 0.198 Uiso 1 1 calc R . .
C49 C 0.0638(7) 0.5227(9) 0.4197(7) 0.202(5) Uiso 1 1 d D . .
H49 H 0.0603 0.4755 0.4584 0.243 Uiso 1 1 calc R . .
C50 C 0.0438(6) 0.4802(8) 0.3521(5) 0.163(4) Uiso 1 1 d D . .
H50 H 0.0337 0.4080 0.3452 0.196 Uiso 1 1 calc R . .


_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
K1 N1 2.654(3) . ?
K1 N3 2.954(3) . ?
K1 C22 3.154(3) . ?
K1 C27 3.157(3) 4_566 ?
K1 C21 3.176(3) . ?
K1 C17 3.270(3) . ?
K1 C20 3.310(3) . ?
K1 P1 3.3120(16) . ?
K1 C26 3.316(4) 4_566 ?
K1 C18 3.395(3) . ?
K1 C19 3.409(4) . ?
K1 C35 3.438(3) . ?
P1 N1 1.649(3) . ?
P1 N2 1.704(3) . ?
P1 N3 1.751(3) . ?
N1 C1 1.383(3) . ?
C1 C6 1.423(4) . ?
C1 C2 1.426(4) . ?
N2 C38 1.453(5) . ?
N2 C36 1.464(4) . ?
C2 C3 1.387(4) . ?
C2 C10 1.521(4) . ?
N3 C40 1.476(4) . ?
N3 C42 1.485(5) . ?
C3 C4 1.387(4) . ?
C4 C5 1.390(4) . ?
C4 C7 1.522(4) . ?
C5 C6 1.395(4) . ?
C6 C23 1.524(4) . ?
C7 C9 1.520(7) . ?
C7 C8 1.518(6) . ?
C10 C11 1.525(4) . ?
C10 C17 1.527(4) . ?
C11 C12 1.389(5) . ?
C11 C16 1.400(5) . ?
C12 C13 1.393(5) . ?
C13 C14 1.376(6) . ?
C14 C15 1.379(6) . ?
C15 C16 1.384(5) . ?
C17 C22 1.389(4) . ?
C17 C18 1.395(4) . ?
C18 C19 1.398(5) . ?
C19 C20 1.381(5) . ?
C20 C21 1.391(5) . ?
C21 C22 1.387(4) . ?
C23 C30 1.518(4) . ?
C23 C24 1.525(4) . ?
C24 C29 1.377(5) . ?
C24 C25 1.395(5) . ?
C25 C26 1.384(4) . ?
C26 C27 1.383(6) . ?
C26 K1 3.316(4) 4_565 ?
C27 C28 1.378(6) . ?
C27 K1 3.157(3) 4_565 ?
C28 C29 1.396(4) . ?
C30 C31 1.393(4) . ?
C30 C35 1.401(4) . ?
C31 C32 1.391(5) . ?
C32 C33 1.392(4) . ?
C33 C34 1.381(5) . ?
C34 C35 1.384(5) . ?
C36 C37 1.528(6) . ?
C38 C39 1.512(6) . ?
C40 C41 1.533(8) . ?
C42 C43 1.532(5) . ?
C44 C45 1.532(6) . ?
C45 C46 1.344(6) . ?
C45 C50 1.358(7) . ?
C46 C47 1.393(7) . ?
C47 C48 1.356(7) . ?
C48 C49 1.381(7) . ?
C49 C50 1.378(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 K1 N3 53.21(8) . . ?
N1 K1 C22 74.25(8) . . ?
N3 K1 C22 117.95(9) . . ?
N1 K1 C27 158.73(9) . 4_566 ?
N3 K1 C27 110.76(10) . 4_566 ?
C22 K1 C27 126.60(10) . 4_566 ?
N1 K1 C21 99.56(8) . . ?
N3 K1 C21 138.01(9) . . ?
C22 K1 C21 25.32(8) . . ?
C27 K1 C21 101.38(10) 4_566 . ?
N1 K1 C17 61.39(7) . . ?
N3 K1 C17 94.84(8) . . ?
C22 K1 C17 24.89(8) . . ?
C27 K1 C17 139.20(8) 4_566 . ?
C21 K1 C17 44.04(8) . . ?
N1 K1 C20 111.83(8) . . ?
N3 K1 C20 128.33(9) . . ?
C22 K1 C20 43.64(7) . . ?
C27 K1 C20 89.01(9) 4_566 . ?
C21 K1 C20 24.65(8) . . ?
C17 K1 C20 50.44(8) . . ?
N1 K1 P1 29.56(5) . . ?
N3 K1 P1 31.81(6) . . ?
C22 K1 P1 103.80(6) . . ?
C27 K1 P1 129.46(8) 4_566 . ?
C21 K1 P1 129.10(6) . . ?
C17 K1 P1 88.71(6) . . ?
C20 K1 P1 137.87(7) . . ?
N1 K1 C26 144.42(10) . 4_566 ?
N3 K1 C26 91.22(9) . 4_566 ?
C22 K1 C26 133.46(8) . 4_566 ?
C27 K1 C26 24.51(10) 4_566 4_566 ?
C21 K1 C26 109.97(9) . 4_566 ?
C17 K1 C26 132.13(8) . 4_566 ?
C20 K1 C26 89.93(8) . 4_566 ?
P1 K1 C26 117.66(7) . 4_566 ?
N1 K1 C18 75.43(8) . . ?
N3 K1 C18 89.63(9) . . ?
C22 K1 C18 42.64(8) . . ?
C27 K1 C18 121.76(8) 4_566 . ?
C21 K1 C18 49.75(9) . . ?
C17 K1 C18 24.08(7) . . ?
C20 K1 C18 42.11(9) . . ?
P1 K1 C18 96.60(6) . . ?
C26 K1 C18 108.94(8) 4_566 . ?
N1 K1 C19 99.14(8) . . ?
N3 K1 C19 104.68(9) . . ?
C22 K1 C19 49.68(8) . . ?
C27 K1 C19 98.78(9) 4_566 . ?
C21 K1 C19 42.46(9) . . ?
C17 K1 C19 42.54(7) . . ?
C20 K1 C19 23.66(9) . . ?
P1 K1 C19 118.92(7) . . ?
C26 K1 C19 90.07(8) 4_566 . ?
C18 K1 C19 23.72(8) . . ?
N1 K1 C35 75.65(8) . . ?
N3 K1 C35 86.33(9) . . ?
C22 K1 C35 112.44(7) . . ?
C27 K1 C35 90.49(8) 4_566 . ?
C21 K1 C35 120.44(9) . . ?
C17 K1 C35 123.40(7) . . ?
C20 K1 C35 142.69(9) . . ?
P1 K1 C35 64.19(7) . . ?
C26 K1 C35 104.34(8) 4_566 . ?
C18 K1 C35 146.56(7) . . ?
C19 K1 C35 161.83(8) . . ?
N1 P1 N2 103.72(14) . . ?
N1 P1 N3 95.90(13) . . ?
N2 P1 N3 110.41(16) . . ?
N1 P1 K1 52.55(9) . . ?
N2 P1 K1 151.11(10) . . ?
N3 P1 K1 62.75(11) . . ?
C1 N1 P1 125.9(2) . . ?
C1 N1 K1 119.28(19) . . ?
P1 N1 K1 97.90(11) . . ?
N1 C1 C6 125.8(2) . . ?
N1 C1 C2 117.9(2) . . ?
C6 C1 C2 116.2(2) . . ?
C38 N2 C36 115.4(3) . . ?
C38 N2 P1 125.9(2) . . ?
C36 N2 P1 118.4(3) . . ?
C3 C2 C1 121.2(2) . . ?
C3 C2 C10 121.2(2) . . ?
C1 C2 C10 117.5(2) . . ?
C40 N3 C42 111.0(3) . . ?
C40 N3 P1 111.9(2) . . ?
C42 N3 P1 117.1(2) . . ?
C40 N3 K1 126.0(3) . . ?
C42 N3 K1 103.7(2) . . ?
P1 N3 K1 85.44(12) . . ?
C4 C3 C2 122.2(2) . . ?
C3 C4 C5 117.3(3) . . ?
C3 C4 C7 122.1(3) . . ?
C5 C4 C7 120.6(3) . . ?
C4 C5 C6 122.4(3) . . ?
C5 C6 C1 120.6(2) . . ?
C5 C6 C23 120.9(2) . . ?
C1 C6 C23 118.0(2) . . ?
C9 C7 C8 109.7(3) . . ?
C9 C7 C4 109.6(4) . . ?
C8 C7 C4 114.3(3) . . ?
C2 C10 C11 113.0(2) . . ?
C2 C10 C17 111.6(2) . . ?
C11 C10 C17 112.7(2) . . ?
C12 C11 C16 117.7(3) . . ?
C12 C11 C10 123.0(3) . . ?
C16 C11 C10 119.3(3) . . ?
C11 C12 C13 120.5(4) . . ?
C14 C13 C12 120.7(4) . . ?
C13 C14 C15 119.7(3) . . ?
C16 C15 C14 119.8(4) . . ?
C15 C16 C11 121.5(4) . . ?
C22 C17 C18 118.4(3) . . ?
C22 C17 C10 121.5(3) . . ?
C18 C17 C10 120.1(3) . . ?
C22 C17 K1 72.90(16) . . ?
C18 C17 K1 82.97(18) . . ?
C10 C17 K1 113.84(16) . . ?
C17 C18 C19 120.6(3) . . ?
C17 C18 K1 72.95(18) . . ?
C19 C18 K1 78.7(2) . . ?
C20 C19 C18 120.3(3) . . ?
C20 C19 K1 74.16(19) . . ?
C18 C19 K1 77.57(19) . . ?
C19 C20 C21 119.5(3) . . ?
C19 C20 K1 82.2(2) . . ?
C21 C20 K1 72.29(18) . . ?
C22 C21 C20 120.1(3) . . ?
C22 C21 K1 76.46(18) . . ?
C20 C21 K1 83.05(19) . . ?
C21 C22 C17 121.2(3) . . ?
C21 C22 K1 78.22(18) . . ?
C17 C22 K1 82.21(17) . . ?
C30 C23 C6 110.0(2) . . ?
C30 C23 C24 113.8(3) . . ?
C6 C23 C24 113.5(2) . . ?
C29 C24 C25 118.1(3) . . ?
C29 C24 C23 123.9(3) . . ?
C25 C24 C23 118.0(3) . . ?
C26 C25 C24 121.4(4) . . ?
C25 C26 C27 119.7(4) . . ?
C25 C26 K1 108.0(2) . 4_565 ?
C27 C26 K1 71.33(19) . 4_565 ?
C28 C27 C26 119.6(3) . . ?
C28 C27 K1 102.5(2) . 4_565 ?
C26 C27 K1 84.2(2) . 4_565 ?
C27 C28 C29 120.4(4) . . ?
C24 C29 C28 120.7(3) . . ?
C31 C30 C35 117.3(3) . . ?
C31 C30 C23 121.9(2) . . ?
C35 C30 C23 120.8(3) . . ?
C31 C30 K1 81.21(17) . . ?
C35 C30 K1 75.80(17) . . ?
C23 C30 K1 112.09(18) . . ?
C32 C31 C30 121.8(3) . . ?
C33 C32 C31 119.6(3) . . ?
C34 C33 C32 119.4(3) . . ?
C33 C34 C35 120.6(3) . . ?
C33 C34 K1 82.34(19) . . ?
C35 C34 K1 76.58(18) . . ?
C34 C35 C30 121.2(3) . . ?
C34 C35 K1 80.36(18) . . ?
C30 C35 K1 80.94(17) . . ?
N2 C36 C37 113.2(4) . . ?
N2 C38 C39 114.4(3) . . ?
N3 C40 C41 112.1(4) . . ?
N3 C42 C43 112.0(4) . . ?
C46 C45 C50 116.0(8) . . ?
C46 C45 C44 126.4(7) . . ?
C50 C45 C44 117.4(7) . . ?
C45 C46 C47 125.1(9) . . ?
C48 C47 C46 122.9(10) . . ?
C47 C48 C49 107.8(11) . . ?
C50 C49 C48 132.3(13) . . ?
C45 C50 C49 115.5(10) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.964
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.077
####################################################################### 
# 
# 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_cj1080
_database_code_depnum_ccdc_archive 'CCDC 1401425'
_audit_update_record             
;
2015-05-18 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C47 H60 N3 P'
_chemical_formula_weight         697.95

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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   11.2534(6)
_cell_length_b                   12.2272(5)
_cell_length_c                   16.8486(9)
_cell_angle_alpha                70.230(4)
_cell_angle_beta                 73.735(4)
_cell_angle_gamma                76.194(4)
_cell_volume                     2067.62(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             756
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.988
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_process_details   'Sortav (Blessing)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex X8'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18998
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.07
_diffrn_reflns_theta_max         25.50
_reflns_number_total             7695
_reflns_number_gt                5990
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0371P)²+0.7930P] 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         7695
_refine_ls_number_parameters     470
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0424
_refine_ls_wR_factor_ref         0.1030
_refine_ls_wR_factor_gt          0.0920
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.72022(4) 0.75639(3) 0.65399(3) 0.01782(11) Uani 1 1 d . . .
N1 N 0.82973(13) 0.70727(11) 0.71737(8) 0.0187(3) Uani 1 1 d . . .
H1 H 0.9065 0.6767 0.6966 0.022 Uiso 1 1 calc R . .
N2 N 0.81755(13) 0.76939(11) 0.55522(8) 0.0204(3) Uani 1 1 d . . .
C41 C 0.96792(19) 0.66040(16) 0.45730(12) 0.0341(5) Uani 1 1 d . . .
H41A H 0.9005 0.6187 0.4625 0.051 Uiso 1 1 calc R . .
H41B H 1.0484 0.6075 0.4519 0.051 Uiso 1 1 calc R . .
H41C H 0.9702 0.7291 0.4060 0.051 Uiso 1 1 calc R . .
C13 C 0.92162(17) 0.33938(15) 0.98672(11) 0.0290(4) Uani 1 1 d . . .
H13 H 0.9940 0.3745 0.9744 0.035 Uiso 1 1 calc R . .
C2 C 0.76083(15) 0.82664(14) 0.81810(10) 0.0193(3) Uani 1 1 d . . .
C6 C 0.80276(15) 0.61361(13) 0.87410(10) 0.0189(3) Uani 1 1 d . . .
C8 C 0.83507(16) 0.38833(13) 0.93464(10) 0.0209(4) Uani 1 1 d . . .
N3 N 0.64580(13) 0.64283(12) 0.67018(9) 0.0245(3) Uani 1 1 d . . .
C22 C 0.65218(17) 1.13405(14) 0.67380(11) 0.0257(4) Uani 1 1 d . . .
H22 H 0.7299 1.1618 0.6468 0.031 Uiso 1 1 calc R . .
C39 C 0.94400(16) 0.70092(14) 0.53778(11) 0.0238(4) Uani 1 1 d . . .
H39 H 0.9474 0.6282 0.5879 0.029 Uiso 1 1 calc R . .
C3 C 0.72279(16) 0.83158(14) 0.90318(11) 0.0237(4) Uani 1 1 d . . .
H3 H 0.6952 0.9065 0.9131 0.028 Uiso 1 1 calc R . .
C36 C 0.78992(17) 0.88098(14) 0.48751(11) 0.0258(4) Uani 1 1 d . . .
H36 H 0.8536 0.8769 0.4332 0.031 Uiso 1 1 calc R . .
C27 C 0.86851(16) 1.00141(13) 0.75793(10) 0.0208(4) Uani 1 1 d . . .
C44 C 0.6394(2) 0.55176(17) 0.56015(12) 0.0387(5) Uani 1 1 d . . .
H44A H 0.5499 0.5470 0.5818 0.058 Uiso 1 1 calc R . .
H44B H 0.6811 0.4873 0.5349 0.058 Uiso 1 1 calc R . .
H44C H 0.6502 0.6273 0.5159 0.058 Uiso 1 1 calc R . .
C19 C 1.03485(17) 0.42964(14) 0.74444(11) 0.0253(4) Uani 1 1 d . . .
H19 H 0.9798 0.3909 0.7336 0.030 Uiso 1 1 calc R . .
C45 C 0.51336(16) 0.64889(15) 0.71860(11) 0.0255(4) Uani 1 1 d . . .
H45 H 0.4808 0.5824 0.7141 0.031 Uiso 1 1 calc R . .
C28 C 0.99517(16) 0.96880(14) 0.72657(11) 0.0240(4) Uani 1 1 d . . .
H28 H 1.0209 0.9125 0.6952 0.029 Uiso 1 1 calc R . .
C20 C 0.77395(15) 0.94107(13) 0.74512(10) 0.0196(4) Uani 1 1 d . . .
H20 H 0.8128 0.9181 0.6908 0.023 Uiso 1 1 calc R . .
C26 C 0.53577(16) 0.98323(15) 0.76906(11) 0.0244(4) Uani 1 1 d . . .
H26 H 0.5323 0.9066 0.8084 0.029 Uiso 1 1 calc R . .
C14 C 0.99076(16) 0.48966(13) 0.80670(10) 0.0205(4) Uani 1 1 d . . .
C25 C 0.42579(18) 1.05542(16) 0.75023(12) 0.0310(4) Uani 1 1 d . . .
H25 H 0.3478 1.0278 0.7765 0.037 Uiso 1 1 calc R . .
C23 C 0.54249(18) 1.20629(16) 0.65536(12) 0.0316(4) Uani 1 1 d . . .
H23 H 0.5454 1.2832 0.6162 0.038 Uiso 1 1 calc R . .
C5 C 0.76674(16) 0.62366(14) 0.95719(11) 0.0228(4) Uani 1 1 d . . .
H5 H 0.7717 0.5543 1.0045 0.027 Uiso 1 1 calc R . .
C40 C 1.04970(18) 0.76358(17) 0.53166(13) 0.0353(5) Uani 1 1 d . . .
H40A H 1.0541 0.8324 0.4804 0.053 Uiso 1 1 calc R . .
H40B H 1.1295 0.7096 0.5272 0.053 Uiso 1 1 calc R . .
H40C H 1.0335 0.7891 0.5835 0.053 Uiso 1 1 calc R . .
C38 C 0.8000(2) 0.98983(15) 0.50743(13) 0.0376(5) Uani 1 1 d . . .
H38A H 0.7324 1.0020 0.5564 0.056 Uiso 1 1 calc R . .
H38B H 0.7930 1.0584 0.4568 0.056 Uiso 1 1 calc R . .
H38C H 0.8812 0.9795 0.5220 0.056 Uiso 1 1 calc R . .
C42 C 0.69739(17) 0.54199(15) 0.63464(12) 0.0274(4) Uani 1 1 d . . .
H42 H 0.7887 0.5453 0.6099 0.033 Uiso 1 1 calc R . .
C32 C 0.83356(17) 1.08451(15) 0.80344(11) 0.0269(4) Uani 1 1 d . . .
H32 H 0.7472 1.1091 0.8249 0.032 Uiso 1 1 calc R . .
C7 C 0.85414(16) 0.49517(13) 0.85587(10) 0.0194(3) Uani 1 1 d . . .
H7 H 0.8055 0.4908 0.8159 0.023 Uiso 1 1 calc R . .
C46 C 0.50194(18) 0.62976(17) 0.81423(12) 0.0340(4) Uani 1 1 d . . .
H46A H 0.5521 0.5543 0.8382 0.051 Uiso 1 1 calc R . .
H46B H 0.4139 0.6291 0.8445 0.051 Uiso 1 1 calc R . .
H46C H 0.5325 0.6936 0.8216 0.051 Uiso 1 1 calc R . .
C47 C 0.43008(18) 0.76206(17) 0.67999(14) 0.0374(5) Uani 1 1 d . . .
H47A H 0.4581 0.8297 0.6839 0.056 Uiso 1 1 calc R . .
H47B H 0.3430 0.7591 0.7120 0.056 Uiso 1 1 calc R . .
H47C H 0.4357 0.7701 0.6192 0.056 Uiso 1 1 calc R . .
C18 C 1.15775(18) 0.42578(17) 0.69813(12) 0.0335(4) Uani 1 1 d . . .
H18 H 1.1862 0.3852 0.6555 0.040 Uiso 1 1 calc R . .
C33 C 0.6829(2) 0.74168(16) 1.06534(12) 0.0348(5) Uani 1 1 d . . .
H33 H 0.7014 0.6610 1.1053 0.042 Uiso 1 1 calc R . .
C21 C 0.65077(16) 1.02125(14) 0.73127(10) 0.0199(4) Uani 1 1 d . . .
C17 C 1.23932(18) 0.48056(17) 0.71359(13) 0.0370(5) Uani 1 1 d . . .
H17 H 1.3238 0.4776 0.6819 0.044 Uiso 1 1 calc R . .
C15 C 1.07402(16) 0.54489(14) 0.82124(11) 0.0258(4) Uani 1 1 d . . .
H15 H 1.0459 0.5867 0.8632 0.031 Uiso 1 1 calc R . .
C43 C 0.68804(19) 0.42215(15) 0.70190(13) 0.0343(5) Uani 1 1 d . . .
H43A H 0.7266 0.4165 0.7489 0.051 Uiso 1 1 calc R . .
H43B H 0.7319 0.3599 0.6749 0.051 Uiso 1 1 calc R . .
H43C H 0.5996 0.4131 0.7252 0.051 Uiso 1 1 calc R . .
C37 C 0.6624(2) 0.89398(18) 0.46905(14) 0.0441(5) Uani 1 1 d . . .
H37A H 0.6580 0.8254 0.4529 0.066 Uiso 1 1 calc R . .
H37B H 0.6493 0.9656 0.4215 0.066 Uiso 1 1 calc R . .
H37C H 0.5972 0.8993 0.5208 0.066 Uiso 1 1 calc R . .
C1 C 0.79659(15) 0.71592(13) 0.80312(10) 0.0179(3) Uani 1 1 d . . .
C31 C 0.92337(18) 1.13175(16) 0.81780(12) 0.0318(4) Uani 1 1 d . . .
H31 H 0.8982 1.1874 0.8497 0.038 Uiso 1 1 calc R . .
C4 C 0.72344(17) 0.73228(15) 0.97371(11) 0.0255(4) Uani 1 1 d . . .
C16 C 1.19707(18) 0.53971(16) 0.77542(13) 0.0339(4) Uani 1 1 d . . .
H16 H 1.2530 0.5771 0.7866 0.041 Uiso 1 1 calc R . .
C24 C 0.42891(18) 1.16729(16) 0.69347(12) 0.0330(5) Uani 1 1 d . . .
H24 H 0.3534 1.2169 0.6808 0.040 Uiso 1 1 calc R . .
C35 C 0.7536(2) 0.8202(3) 1.08010(15) 0.0625(8) Uani 1 1 d . . .
H35A H 0.8439 0.7956 1.0614 0.094 Uiso 1 1 calc R . .
H35B H 0.7334 0.8144 1.1417 0.094 Uiso 1 1 calc R . .
H35C H 0.7297 0.9018 1.0468 0.094 Uiso 1 1 calc R . .
C34 C 0.5432(2) 0.7838(3) 1.08940(15) 0.0634(8) Uani 1 1 d . . .
H34A H 0.5222 0.8633 1.0517 0.095 Uiso 1 1 calc R . .
H34B H 0.5199 0.7850 1.1497 0.095 Uiso 1 1 calc R . .
H34C H 0.4971 0.7303 1.0823 0.095 Uiso 1 1 calc R . .
C29 C 1.08515(17) 1.01677(16) 0.74011(11) 0.0285(4) Uani 1 1 d . . .
H29 H 1.1715 0.9936 0.7179 0.034 Uiso 1 1 calc R . .
C30 C 1.04900(18) 1.09824(16) 0.78593(12) 0.0309(4) Uani 1 1 d . . .
H30 H 1.1104 1.1311 0.7955 0.037 Uiso 1 1 calc R . .
C12 C 0.90389(19) 0.23928(16) 1.05690(12) 0.0349(5) Uani 1 1 d . . .
H12 H 0.9638 0.2066 1.0921 0.042 Uiso 1 1 calc R . .
C9 C 0.72971(17) 0.33599(15) 0.95497(11) 0.0274(4) Uani 1 1 d . . .
H9 H 0.6687 0.3690 0.9206 0.033 Uiso 1 1 calc R . .
C10 C 0.71178(19) 0.23630(16) 1.02469(12) 0.0355(5) Uani 1 1 d . . .
H10 H 0.6391 0.2014 1.0377 0.043 Uiso 1 1 calc R . .
C11 C 0.7995(2) 0.18799(16) 1.07503(12) 0.0367(5) Uani 1 1 d . . .
H11 H 0.7878 0.1191 1.1224 0.044 Uiso 1 1 calc R . .


_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
P1 N3 1.6954(14) . ?
P1 N2 1.6963(14) . ?
P1 N1 1.7234(14) . ?
N1 C1 1.4214(19) . ?
N2 C39 1.475(2) . ?
N2 C36 1.484(2) . ?
C41 C39 1.531(2) . ?
C13 C8 1.386(2) . ?
C13 C12 1.393(3) . ?
C2 C3 1.394(2) . ?
C2 C1 1.405(2) . ?
C2 C20 1.525(2) . ?
C6 C5 1.383(2) . ?
C6 C1 1.412(2) . ?
C6 C7 1.526(2) . ?
C8 C9 1.385(2) . ?
C8 C7 1.522(2) . ?
N3 C42 1.476(2) . ?
N3 C45 1.483(2) . ?
C22 C23 1.382(3) . ?
C22 C21 1.392(2) . ?
C39 C40 1.525(2) . ?
C3 C4 1.382(2) . ?
C36 C37 1.513(3) . ?
C36 C38 1.514(2) . ?
C27 C28 1.385(2) . ?
C27 C32 1.394(2) . ?
C27 C20 1.528(2) . ?
C44 C42 1.528(3) . ?
C19 C18 1.383(3) . ?
C19 C14 1.393(2) . ?
C45 C46 1.520(3) . ?
C45 C47 1.526(3) . ?
C28 C29 1.387(2) . ?
C20 C21 1.522(2) . ?
C26 C25 1.386(2) . ?
C26 C21 1.386(2) . ?
C14 C15 1.392(2) . ?
C14 C7 1.526(2) . ?
C25 C24 1.381(3) . ?
C23 C24 1.377(3) . ?
C5 C4 1.394(2) . ?
C42 C43 1.525(3) . ?
C32 C31 1.387(2) . ?
C18 C17 1.380(3) . ?
C33 C35 1.501(3) . ?
C33 C34 1.517(3) . ?
C33 C4 1.518(2) . ?
C17 C16 1.379(3) . ?
C15 C16 1.382(3) . ?
C31 C30 1.379(3) . ?
C29 C30 1.380(3) . ?
C12 C11 1.374(3) . ?
C9 C10 1.387(3) . ?
C10 C11 1.376(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
N3 P1 N2 104.43(7) . . ?
N3 P1 N1 108.11(7) . . ?
N2 P1 N1 99.54(7) . . ?
C1 N1 P1 120.31(11) . . ?
C39 N2 C36 116.18(13) . . ?
C39 N2 P1 125.46(11) . . ?
C36 N2 P1 115.53(11) . . ?
C8 C13 C12 120.85(17) . . ?
C3 C2 C1 118.73(14) . . ?
C3 C2 C20 118.74(14) . . ?
C1 C2 C20 122.26(14) . . ?
C5 C6 C1 119.58(14) . . ?
C5 C6 C7 122.12(14) . . ?
C1 C6 C7 118.26(13) . . ?
C9 C8 C13 118.22(16) . . ?
C9 C8 C7 119.79(15) . . ?
C13 C8 C7 121.98(15) . . ?
C42 N3 C45 116.27(13) . . ?
C42 N3 P1 125.94(12) . . ?
C45 N3 P1 117.61(10) . . ?
C23 C22 C21 121.17(17) . . ?
N2 C39 C40 114.09(13) . . ?
N2 C39 C41 111.97(14) . . ?
C40 C39 C41 110.16(15) . . ?
C4 C3 C2 122.91(15) . . ?
N2 C36 C37 111.40(15) . . ?
N2 C36 C38 113.93(14) . . ?
C37 C36 C38 109.76(16) . . ?
C28 C27 C32 118.07(15) . . ?
C28 C27 C20 118.99(14) . . ?
C32 C27 C20 122.87(15) . . ?
C18 C19 C14 120.82(16) . . ?
N3 C45 C46 111.97(14) . . ?
N3 C45 C47 112.95(15) . . ?
C46 C45 C47 111.10(15) . . ?
C27 C28 C29 121.27(16) . . ?
C21 C20 C2 114.87(14) . . ?
C21 C20 C27 113.78(12) . . ?
C2 C20 C27 108.60(13) . . ?
C25 C26 C21 120.96(17) . . ?
C15 C14 C19 118.12(16) . . ?
C15 C14 C7 121.76(14) . . ?
C19 C14 C7 120.11(15) . . ?
C24 C25 C26 120.35(18) . . ?
C24 C23 C22 120.27(17) . . ?
C6 C5 C4 122.11(15) . . ?
N3 C42 C43 114.14(15) . . ?
N3 C42 C44 111.83(15) . . ?
C43 C42 C44 110.23(14) . . ?
C31 C32 C27 120.78(17) . . ?
C8 C7 C6 114.78(13) . . ?
C8 C7 C14 111.74(13) . . ?
C6 C7 C14 111.32(13) . . ?
C17 C18 C19 120.36(17) . . ?
C35 C33 C34 109.56(17) . . ?
C35 C33 C4 112.50(17) . . ?
C34 C33 C4 111.82(16) . . ?
C26 C21 C22 117.89(16) . . ?
C26 C21 C20 122.26(15) . . ?
C22 C21 C20 119.67(15) . . ?
C16 C17 C18 119.41(18) . . ?
C16 C15 C14 120.81(16) . . ?
C2 C1 C6 119.16(14) . . ?
C2 C1 N1 120.35(14) . . ?
C6 C1 N1 120.46(13) . . ?
C30 C31 C32 120.25(16) . . ?
C3 C4 C5 117.30(15) . . ?
C3 C4 C33 121.21(15) . . ?
C5 C4 C33 121.46(15) . . ?
C17 C16 C15 120.48(17) . . ?
C23 C24 C25 119.36(17) . . ?
C30 C29 C28 119.93(17) . . ?
C31 C30 C29 119.70(17) . . ?
C11 C12 C13 119.84(18) . . ?
C8 C9 C10 121.11(17) . . ?
C11 C10 C9 119.89(18) . . ?
C12 C11 C10 120.07(17) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.506
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.041
####################################################################### 
# 
# 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_cj1159
_database_code_depnum_ccdc_archive 'CCDC 1401426'
_audit_update_record             
;
2015-05-18 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42.50 H45 N2 P'
_chemical_formula_weight         614.78

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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   9.931(2)
_cell_length_b                   11.495(2)
_cell_length_c                   16.176(3)
_cell_angle_alpha                92.84(3)
_cell_angle_beta                 107.41(3)
_cell_angle_gamma                90.52(3)
_cell_volume                     1759.2(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             658
_exptl_absorpt_coefficient_mu    0.110
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.993
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_process_details   XDS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71090
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'Australian Synchrotron'
_diffrn_radiation_monochromator  ?
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12551
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.10
_diffrn_reflns_theta_max         25.50
_reflns_number_total             6033
_reflns_number_gt                5396
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Blu-Ice (McPhillips, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CifTAB

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
 A molecule of toluene was located in the asymmetric unit. Its atoms were
 set at 50% occupancy, and its carbon atoms refined isotropically.
 The low value (92.2%) for completeness of data to theta = 25.5 deg. arises 
 from hardware constraints associated with the diffractometer used at the 
 Australian Synchrotron and is common for triclinic data sets on that instrument. 
 Its minimum crystal to detector distance is 72 mm and its
 goniometer only rotates about the phi axis.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0617P)²+2.6486P] 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         6033
_refine_ls_number_parameters     403
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0625
_refine_ls_wR_factor_ref         0.1558
_refine_ls_wR_factor_gt          0.1513
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.111
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.20336(7) 0.14223(6) 0.29956(4) 0.02159(18) Uani 1 1 d . . .
N1 N 0.1359(2) 0.24289(18) 0.24062(13) 0.0203(4) Uani 1 1 d . . .
C1 C 0.0139(2) 0.3015(2) 0.24379(15) 0.0189(5) Uani 1 1 d . . .
N2 N 0.3422(2) 0.10740(19) 0.26900(14) 0.0234(5) Uani 1 1 d . . .
C2 C 0.0254(3) 0.4025(2) 0.29857(15) 0.0190(5) Uani 1 1 d . . .
C3 C -0.0960(3) 0.4627(2) 0.29783(16) 0.0209(5) Uani 1 1 d . . .
H3 H -0.0883 0.5296 0.3360 0.025 Uiso 1 1 calc R . .
C4 C -0.2286(3) 0.4277(2) 0.24271(16) 0.0210(5) Uani 1 1 d . . .
C5 C -0.2365(3) 0.3307(2) 0.18648(16) 0.0208(5) Uani 1 1 d . . .
H5 H -0.3257 0.3065 0.1476 0.025 Uiso 1 1 calc R . .
C6 C -0.1178(3) 0.2678(2) 0.18531(15) 0.0196(5) Uani 1 1 d . . .
C7 C -0.1253(3) 0.1657(2) 0.12048(16) 0.0202(5) Uani 1 1 d . . .
H7 H -0.0341 0.1680 0.1062 0.024 Uiso 1 1 calc R . .
C8 C -0.1335(2) 0.0473(2) 0.15756(16) 0.0211(5) Uani 1 1 d . . .
C9 C -0.0900(3) -0.0509(2) 0.11973(17) 0.0279(6) Uani 1 1 d . . .
H9 H -0.0573 -0.0422 0.0708 0.033 Uiso 1 1 calc R . .
C10 C -0.0926(3) -0.1623(2) 0.15114(17) 0.0352(7) Uani 1 1 d . . .
H10 H -0.0557 -0.2274 0.1274 0.042 Uiso 1 1 calc R . .
C42 C -0.0940(3) 0.5416(2) -0.07282(17) 0.0259(14) Uiso 0.50 1 d PRD A -1
H42 H -0.1619 0.5678 -0.1229 0.031 Uiso 0.50 1 d PR B -1
C43 C 0.0385(3) 0.4948(2) -0.07622(17) 0.0290(15) Uiso 0.50 1 d PRD A -1
H43 H 0.0607 0.4941 -0.1294 0.035 Uiso 0.50 1 calc PR C -1
C44 C 0.1303(3) 0.4527(2) -0.00741(17) 0.031(2) Uiso 0.50 1 d PRD A -1
H44 H 0.2147 0.4239 -0.0161 0.038 Uiso 0.50 1 calc PR D -1
C11 C -0.1520(3) -0.1735(3) 0.2190(2) 0.0331(6) Uani 1 1 d . . .
H11 H -0.1628 -0.2485 0.2386 0.040 Uiso 1 1 calc R . .
C12 C -0.1950(3) -0.0770(3) 0.25743(19) 0.0320(6) Uani 1 1 d . . .
H12 H -0.2312 -0.0857 0.3050 0.038 Uiso 1 1 calc R . .
C13 C -0.1857(3) 0.0333(2) 0.22717(18) 0.0272(6) Uani 1 1 d . . .
H13 H -0.2153 0.0993 0.2543 0.033 Uiso 1 1 calc R . .
C14 C -0.2414(3) 0.1773(2) 0.03472(16) 0.0199(5) Uani 1 1 d . . .
C15 C -0.2090(3) 0.2310(2) -0.03247(17) 0.0254(6) Uani 1 1 d . . .
H15 H -0.1151 0.2580 -0.0247 0.030 Uiso 1 1 calc R . .
C16 C -0.3122(3) 0.2453(2) -0.11061(17) 0.0284(6) Uani 1 1 d . . .
H16 H -0.2884 0.2807 -0.1564 0.034 Uiso 1 1 calc R . .
C17 C -0.4502(3) 0.2082(2) -0.12217(17) 0.0280(6) Uani 1 1 d . . .
H17 H -0.5212 0.2194 -0.1753 0.034 Uiso 1 1 calc R . .
C18 C -0.4840(3) 0.1546(2) -0.05593(17) 0.0256(6) Uani 1 1 d . . .
H18 H -0.5783 0.1284 -0.0637 0.031 Uiso 1 1 calc R . .
C19 C -0.3799(3) 0.1391(2) 0.02197(16) 0.0223(5) Uani 1 1 d . . .
H19 H -0.4036 0.1019 0.0671 0.027 Uiso 1 1 calc R . .
C20 C -0.3592(3) 0.4945(2) 0.24479(18) 0.0261(6) Uani 1 1 d . . .
H20 H -0.3303 0.5785 0.2588 0.031 Uiso 1 1 calc R . .
C21 C -0.4162(3) 0.4532(3) 0.3163(2) 0.0349(7) Uani 1 1 d . . .
H21A H -0.4420 0.3701 0.3055 0.052 Uiso 1 1 calc R . .
H21B H -0.4997 0.4975 0.3170 0.052 Uiso 1 1 calc R . .
H21C H -0.3435 0.4653 0.3726 0.052 Uiso 1 1 calc R . .
C22 C -0.4764(3) 0.4865(3) 0.1586(2) 0.0355(7) Uani 1 1 d . . .
H22A H -0.5086 0.4051 0.1439 0.053 Uiso 1 1 calc R . .
H22B H -0.4405 0.5153 0.1130 0.053 Uiso 1 1 calc R . .
H22C H -0.5555 0.5338 0.1635 0.053 Uiso 1 1 calc R . .
C23 C 0.1724(3) 0.4451(2) 0.35382(15) 0.0197(5) Uani 1 1 d . . .
H23 H 0.2361 0.4305 0.3170 0.024 Uiso 1 1 calc R . .
C24 C 0.2317(3) 0.3765(2) 0.43446(15) 0.0193(5) Uani 1 1 d . . .
C25 C 0.1453(3) 0.3279(2) 0.47767(17) 0.0241(5) Uani 1 1 d . . .
H25 H 0.0459 0.3361 0.4563 0.029 Uiso 1 1 calc R . .
C26 C 0.2029(3) 0.2672(2) 0.55209(18) 0.0281(6) Uani 1 1 d . . .
H26 H 0.1428 0.2348 0.5814 0.034 Uiso 1 1 calc R . .
C27 C 0.3473(3) 0.2539(2) 0.58337(17) 0.0269(6) Uani 1 1 d . . .
H27 H 0.3864 0.2124 0.6341 0.032 Uiso 1 1 calc R . .
C28 C 0.4344(3) 0.3013(2) 0.54045(17) 0.0259(6) Uani 1 1 d . . .
H28 H 0.5336 0.2918 0.5615 0.031 Uiso 1 1 calc R . .
C29 C 0.3772(3) 0.3625(2) 0.46682(16) 0.0226(5) Uani 1 1 d . . .
H29 H 0.4378 0.3954 0.4380 0.027 Uiso 1 1 calc R . .
C30 C 0.1789(2) 0.5762(2) 0.37418(16) 0.0205(5) Uani 1 1 d . . .
C31 C 0.1720(3) 0.6251(2) 0.45275(17) 0.0239(5) Uani 1 1 d . . .
H31 H 0.1661 0.5761 0.4972 0.029 Uiso 1 1 calc R . .
C32 C 0.1735(3) 0.7456(2) 0.46715(18) 0.0277(6) Uani 1 1 d . . .
H32 H 0.1694 0.7782 0.5214 0.033 Uiso 1 1 calc R . .
C33 C 0.1809(3) 0.8181(2) 0.40289(19) 0.0299(6) Uani 1 1 d . . .
H33 H 0.1808 0.9003 0.4126 0.036 Uiso 1 1 calc R . .
C34 C 0.1884(3) 0.7699(2) 0.32438(18) 0.0295(6) Uani 1 1 d . . .
H34 H 0.1944 0.8191 0.2801 0.035 Uiso 1 1 calc R . .
C35 C 0.1874(3) 0.6503(2) 0.31035(17) 0.0260(6) Uani 1 1 d . . .
H35 H 0.1925 0.6180 0.2562 0.031 Uiso 1 1 calc R . .
C36 C 0.3800(3) 0.1608(3) 0.19824(18) 0.0292(6) Uani 1 1 d . . .
H36A H 0.4822 0.1516 0.2067 0.035 Uiso 1 1 calc R . .
H36B H 0.3618 0.2453 0.2004 0.035 Uiso 1 1 calc R . .
C37 C 0.2976(3) 0.1074(3) 0.11004(19) 0.0385(7) Uani 1 1 d . . .
H37A H 0.3115 0.0231 0.1085 0.058 Uiso 1 1 calc R . .
H37B H 0.3309 0.1419 0.0653 0.058 Uiso 1 1 calc R . .
H37C H 0.1970 0.1225 0.0992 0.058 Uiso 1 1 calc R . .
C38 C 0.4374(3) 0.0204(2) 0.31724(18) 0.0286(6) Uani 1 1 d . . .
H38A H 0.4651 -0.0332 0.2757 0.034 Uiso 1 1 calc R . .
H38B H 0.3866 -0.0261 0.3489 0.034 Uiso 1 1 calc R . .
C39 C 0.5691(3) 0.0755(3) 0.38131(19) 0.0351(7) Uani 1 1 d . . .
H39A H 0.6205 0.1208 0.3502 0.053 Uiso 1 1 calc R . .
H39B H 0.6295 0.0142 0.4115 0.053 Uiso 1 1 calc R . .
H39C H 0.5424 0.1270 0.4236 0.053 Uiso 1 1 calc R . .
C40 C -0.2464(6) 0.5833(6) 0.0175(4) 0.0417(14) Uiso 0.50 1 d PD A -1
H40A H -0.2776 0.6458 -0.0225 0.063 Uiso 0.50 1 calc PR A -1
H40B H -0.2374 0.6130 0.0768 0.063 Uiso 0.50 1 calc PR A -1
H40C H -0.3157 0.5186 0.0012 0.063 Uiso 0.50 1 calc PR A -1
C41 C -0.1090(8) 0.5423(9) 0.0130(5) 0.072(4) Uiso 0.50 1 d PD A -1
C45 C 0.1187(9) 0.4452(10) 0.0774(4) 0.086(4) Uiso 0.50 1 d PD A -1
H45 H 0.1870 0.4108 0.1235 0.103 Uiso 0.50 1 calc PR A -1
C46 C -0.0079(8) 0.4956(7) 0.0853(4) 0.059(2) Uiso 0.50 1 d PD A -1
H46 H -0.0254 0.4980 0.1400 0.071 Uiso 0.50 1 calc PR A -1


_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
P1 N1 1.561(2) . ?
P1 N2 1.645(2) . ?
N1 C1 1.405(3) . ?
C1 C6 1.403(4) . ?
C1 C2 1.408(4) . ?
N2 C36 1.467(3) . ?
N2 C38 1.468(3) . ?
C2 C3 1.393(3) . ?
C2 C23 1.528(3) . ?
C3 C4 1.393(4) . ?
C4 C5 1.390(4) . ?
C4 C20 1.522(3) . ?
C5 C6 1.392(3) . ?
C6 C7 1.521(3) . ?
C7 C8 1.525(3) . ?
C7 C14 1.528(3) . ?
C8 C13 1.389(4) . ?
C8 C9 1.391(4) . ?
C9 C10 1.404(4) . ?
C10 C11 1.403(4) . ?
C42 C41 1.439(5) . ?
C42 C43 1.4411 . ?
C43 C44 1.3260 . ?
C44 C45 1.418(6) . ?
C11 C12 1.377(4) . ?
C12 C13 1.394(4) . ?
C14 C19 1.392(4) . ?
C14 C15 1.392(3) . ?
C15 C16 1.387(4) . ?
C16 C17 1.386(4) . ?
C17 C18 1.385(4) . ?
C18 C19 1.391(4) . ?
C20 C22 1.523(4) . ?
C20 C21 1.526(4) . ?
C23 C24 1.523(3) . ?
C23 C30 1.524(3) . ?
C24 C25 1.388(3) . ?
C24 C29 1.395(3) . ?
C25 C26 1.394(4) . ?
C26 C27 1.383(4) . ?
C27 C28 1.384(4) . ?
C28 C29 1.387(4) . ?
C30 C31 1.385(4) . ?
C30 C35 1.391(4) . ?
C31 C32 1.392(4) . ?
C32 C33 1.382(4) . ?
C33 C34 1.383(4) . ?
C34 C35 1.382(4) . ?
C36 C37 1.513(4) . ?
C38 C39 1.514(4) . ?
C40 C41 1.469(6) . ?
C41 C46 1.426(6) . ?
C45 C46 1.426(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 P1 N2 104.19(11) . . ?
C1 N1 P1 124.82(17) . . ?
C6 C1 N1 120.1(2) . . ?
C6 C1 C2 119.5(2) . . ?
N1 C1 C2 120.0(2) . . ?
C36 N2 C38 117.6(2) . . ?
C36 N2 P1 124.06(17) . . ?
C38 N2 P1 118.26(18) . . ?
C3 C2 C1 119.3(2) . . ?
C3 C2 C23 122.4(2) . . ?
C1 C2 C23 118.3(2) . . ?
C2 C3 C4 121.9(2) . . ?
C5 C4 C3 117.8(2) . . ?
C5 C4 C20 121.8(2) . . ?
C3 C4 C20 120.4(2) . . ?
C4 C5 C6 122.1(2) . . ?
C5 C6 C1 119.3(2) . . ?
C5 C6 C7 122.0(2) . . ?
C1 C6 C7 118.6(2) . . ?
C6 C7 C8 113.5(2) . . ?
C6 C7 C14 112.94(19) . . ?
C8 C7 C14 111.6(2) . . ?
C13 C8 C9 118.4(2) . . ?
C13 C8 C7 122.3(2) . . ?
C9 C8 C7 119.3(2) . . ?
C8 C9 C10 122.4(2) . . ?
C11 C10 C9 117.3(2) . . ?
C41 C42 C43 112.4(3) . . ?
C44 C43 C42 122.1 . . ?
C43 C44 C45 128.3(3) . . ?
C12 C11 C10 120.8(3) . . ?
C11 C12 C13 120.5(3) . . ?
C8 C13 C12 120.4(3) . . ?
C19 C14 C15 118.5(2) . . ?
C19 C14 C7 122.4(2) . . ?
C15 C14 C7 119.0(2) . . ?
C16 C15 C14 120.7(2) . . ?
C17 C16 C15 120.2(2) . . ?
C18 C17 C16 119.7(2) . . ?
C17 C18 C19 119.9(2) . . ?
C18 C19 C14 120.9(2) . . ?
C4 C20 C22 113.5(2) . . ?
C4 C20 C21 110.6(2) . . ?
C22 C20 C21 109.5(2) . . ?
C24 C23 C30 112.7(2) . . ?
C24 C23 C2 113.4(2) . . ?
C30 C23 C2 111.94(19) . . ?
C25 C24 C29 118.6(2) . . ?
C25 C24 C23 121.9(2) . . ?
C29 C24 C23 119.5(2) . . ?
C24 C25 C26 120.6(2) . . ?
C27 C26 C25 120.2(2) . . ?
C26 C27 C28 119.7(2) . . ?
C27 C28 C29 120.1(2) . . ?
C28 C29 C24 120.8(2) . . ?
C31 C30 C35 118.4(2) . . ?
C31 C30 C23 122.7(2) . . ?
C35 C30 C23 118.8(2) . . ?
C30 C31 C32 120.5(2) . . ?
C33 C32 C31 120.4(3) . . ?
C32 C33 C34 119.4(3) . . ?
C35 C34 C33 120.1(3) . . ?
C34 C35 C30 121.1(3) . . ?
N2 C36 C37 112.4(2) . . ?
N2 C38 C39 112.4(2) . . ?
C46 C41 C42 123.8(4) . . ?
C46 C41 C40 122.3(5) . . ?
C42 C41 C40 113.6(5) . . ?
C44 C45 C46 111.8(5) . . ?
C41 C46 C45 121.5(5) . . ?

_diffrn_measured_fraction_theta_max 0.922
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.922
_refine_diff_density_max         1.711
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.058
####################################################################### 
# 
# 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_cj1087
_database_code_depnum_ccdc_archive 'CCDC 1401427'
_audit_update_record             
;
2015-07-22 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C47 H41 Cl3 N P Si'
_chemical_formula_weight         785.22

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'
Si Si 0.0817 0.0704 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

loop_
_symmetry_equiv_pos_as_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'

_cell_length_a                   10.0456(15)
_cell_length_b                   13.252(2)
_cell_length_c                   29.583(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3938.4(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1640
_exptl_absorpt_coefficient_mu    0.339
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.954
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_process_details   'Sortav (Blessing)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex X8'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13854
_diffrn_reflns_av_R_equivalents  0.1607
_diffrn_reflns_av_sigmaI/netI    0.2340
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.15
_diffrn_reflns_theta_max         25.50
_reflns_number_total             7047
_reflns_number_gt                4081
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.
 The high r-factors for the crystal structure arose from weak data above
 theta angles of 23 deg. Despite this, the gross molecular connectivity
 of the compound is unambiguous. 
 The number of restraints used during the final refinement is 6, which
 is related to a weak ISOR restraint being placed on atom C9.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1229P)²+0.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.21(15)
_refine_ls_number_reflns         7047
_refine_ls_number_parameters     480
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1549
_refine_ls_R_factor_gt           0.1039
_refine_ls_wR_factor_ref         0.2826
_refine_ls_wR_factor_gt          0.2410
_refine_ls_goodness_of_fit_ref   1.029
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.74960(19) 0.11439(19) 0.16279(8) 0.0333(6) Uani 1 1 d . . .
Cl3 Cl 0.4994(2) 0.08317(18) 0.23123(8) 0.0342(6) Uani 1 1 d . . .
P1 P 0.3491(2) -0.05327(19) 0.11789(9) 0.0280(6) Uani 1 1 d . . .
Si1 Si 0.5496(2) 0.0956(2) 0.16546(9) 0.0277(6) Uani 1 1 d . . .
Cl2 Cl 0.4673(2) 0.22869(18) 0.14560(9) 0.0357(6) Uani 1 1 d . . .
C27 C 0.6572(8) -0.2939(7) 0.1676(3) 0.026(2) Uani 1 1 d . . .
N1 N 0.5089(6) -0.0059(5) 0.1335(3) 0.0277(18) Uani 1 1 d . . .
C20 C 0.6567(8) -0.1804(7) 0.1697(3) 0.029(2) Uani 1 1 d . . .
H20 H 0.5637 -0.1599 0.1775 0.035 Uiso 1 1 calc R . .
C38 C 0.2790(8) -0.2163(7) 0.2362(3) 0.031(2) Uani 1 1 d . . .
H38 H 0.3016 -0.2148 0.2674 0.037 Uiso 1 1 calc R . .
C5 C 0.7434(8) -0.0616(7) 0.0378(3) 0.027(2) Uani 1 1 d . . .
H5 H 0.7635 -0.0367 0.0085 0.032 Uiso 1 1 calc R . .
C7 C 0.5461(8) 0.0563(6) 0.0388(3) 0.0223(19) Uani 1 1 d . . .
H7 H 0.4578 0.0510 0.0542 0.027 Uiso 1 1 calc R . .
C9 C 0.7171(8) 0.1993(6) 0.0541(3) 0.0221(19) Uani 1 1 d U . .
H9 H 0.7863 0.1522 0.0600 0.027 Uiso 1 1 calc R . .
C43 C 0.1887(8) 0.0798(8) 0.1712(4) 0.037(3) Uani 1 1 d . . .
H43 H 0.2173 0.0439 0.1972 0.045 Uiso 1 1 calc R . .
C28 C 0.7462(9) -0.3567(7) 0.1904(3) 0.028(2) Uani 1 1 d . . .
H28 H 0.8147 -0.3271 0.2081 0.034 Uiso 1 1 calc R . .
C37 C 0.3238(8) -0.1396(7) 0.2074(3) 0.031(2) Uani 1 1 d . . .
H37 H 0.3723 -0.0844 0.2196 0.038 Uiso 1 1 calc R . .
C1 C 0.6125(8) -0.0542(7) 0.1067(3) 0.024(2) Uani 1 1 d . . .
C32 C 0.5585(9) -0.3432(8) 0.1425(3) 0.033(2) Uani 1 1 d . . .
H32 H 0.4949 -0.3039 0.1266 0.040 Uiso 1 1 calc R . .
C19 C 0.6020(8) 0.0648(7) -0.0455(3) 0.025(2) Uani 1 1 d . . .
H19 H 0.6735 0.1096 -0.0394 0.030 Uiso 1 1 calc R . .
C36 C 0.2983(8) -0.1431(7) 0.1608(4) 0.031(2) Uani 1 1 d . . .
C13 C 0.4945(9) 0.2408(7) 0.0319(3) 0.030(2) Uani 1 1 d . . .
H13 H 0.4090 0.2199 0.0218 0.036 Uiso 1 1 calc R . .
C26 C 0.8763(9) -0.1112(7) 0.2016(3) 0.030(2) Uani 1 1 d . . .
H26 H 0.9149 -0.1136 0.1723 0.037 Uiso 1 1 calc R . .
C44 C 0.0986(8) 0.1613(8) 0.1755(4) 0.041(3) Uani 1 1 d . . .
H44 H 0.0655 0.1808 0.2042 0.049 Uiso 1 1 calc R . .
C42 C 0.2349(8) 0.0528(7) 0.1290(3) 0.027(2) Uani 1 1 d . . .
C33 C 0.9381(8) -0.1792(7) 0.0283(3) 0.031(2) Uani 1 1 d . . .
H33 H 0.9683 -0.2422 0.0438 0.037 Uiso 1 1 calc R . .
C46 C 0.1021(9) 0.1843(7) 0.0943(4) 0.033(2) Uani 1 1 d . . .
H46 H 0.0717 0.2189 0.0681 0.040 Uiso 1 1 calc R . .
C11 C 0.6443(10) 0.3721(7) 0.0469(4) 0.039(3) Uani 1 1 d . . .
H11 H 0.6651 0.4420 0.0487 0.047 Uiso 1 1 calc R . .
C31 C 0.5508(10) -0.4448(8) 0.1402(4) 0.043(3) Uani 1 1 d . . .
H31 H 0.4824 -0.4752 0.1227 0.052 Uiso 1 1 calc R . .
C2 C 0.6865(8) -0.1351(7) 0.1245(3) 0.028(2) Uani 1 1 d . . .
C39 C 0.2014(9) -0.2946(8) 0.2193(4) 0.041(3) Uani 1 1 d . . .
H39 H 0.1679 -0.3454 0.2389 0.049 Uiso 1 1 calc R . .
C14 C 0.5226(8) 0.0287(7) -0.0095(3) 0.027(2) Uani 1 1 d . . .
C25 C 0.9513(9) -0.0781(7) 0.2382(3) 0.035(2) Uani 1 1 d . . .
H25 H 1.0407 -0.0573 0.2336 0.042 Uiso 1 1 calc R . .
C6 C 0.6356(8) -0.0189(6) 0.0616(3) 0.024(2) Uani 1 1 d . . .
C16 C 0.3881(9) -0.0629(7) -0.0642(4) 0.038(3) Uani 1 1 d . . .
H16 H 0.3157 -0.1068 -0.0704 0.046 Uiso 1 1 calc R . .
C4 C 0.8200(8) -0.1375(7) 0.0552(3) 0.026(2) Uani 1 1 d . . .
C21 C 0.7458(8) -0.1406(7) 0.2078(3) 0.025(2) Uani 1 1 d . . .
C22 C 0.6937(9) -0.1371(8) 0.2517(3) 0.035(2) Uani 1 1 d . . .
H22 H 0.6046 -0.1581 0.2569 0.042 Uiso 1 1 calc R . .
C8 C 0.5881(8) 0.1652(7) 0.0428(3) 0.023(2) Uani 1 1 d . . .
C41 C 0.2210(10) -0.2227(8) 0.1447(4) 0.041(3) Uani 1 1 d . . .
H41 H 0.2003 -0.2260 0.1134 0.049 Uiso 1 1 calc R . .
C17 C 0.4694(10) -0.0272(8) -0.0996(4) 0.046(3) Uani 1 1 d . . .
H17 H 0.4518 -0.0454 -0.1301 0.055 Uiso 1 1 calc R . .
C45 C 0.0598(9) 0.2120(8) 0.1368(4) 0.036(2) Uani 1 1 d . . .
H45 H 0.0016 0.2682 0.1397 0.044 Uiso 1 1 calc R . .
C15 C 0.4149(8) -0.0335(7) -0.0206(3) 0.029(2) Uani 1 1 d . . .
H15 H 0.3580 -0.0563 0.0029 0.035 Uiso 1 1 calc R . .
C10 C 0.7415(9) 0.2995(7) 0.0566(3) 0.033(2) Uani 1 1 d . . .
H10 H 0.8279 0.3215 0.0652 0.040 Uiso 1 1 calc R . .
C3 C 0.7925(8) -0.1744(7) 0.0980(3) 0.025(2) Uani 1 1 d . . .
H3 H 0.8457 -0.2273 0.1099 0.031 Uiso 1 1 calc R . .
C12 C 0.5183(9) 0.3414(6) 0.0347(4) 0.034(2) Uani 1 1 d . . .
H12 H 0.4502 0.3892 0.0285 0.041 Uiso 1 1 calc R . .
C30 C 0.6404(9) -0.5051(9) 0.1629(3) 0.040(3) Uani 1 1 d . . .
H30 H 0.6347 -0.5766 0.1612 0.049 Uiso 1 1 calc R . .
C29 C 0.7381(10) -0.4591(7) 0.1879(3) 0.037(2) Uani 1 1 d . . .
H29 H 0.8009 -0.4993 0.2038 0.044 Uiso 1 1 calc R . .
C47 C 0.1919(8) 0.1032(7) 0.0908(4) 0.030(2) Uani 1 1 d . . .
H47 H 0.2233 0.0830 0.0619 0.036 Uiso 1 1 calc R . .
C18 C 0.5772(10) 0.0361(9) -0.0888(4) 0.045(3) Uani 1 1 d . . .
H18 H 0.6339 0.0593 -0.1123 0.053 Uiso 1 1 calc R . .
C34 C 0.8991(10) -0.2082(9) -0.0196(4) 0.048(3) Uani 1 1 d . . .
H34A H 0.8838 -0.1471 -0.0375 0.071 Uiso 1 1 calc R . .
H34B H 0.8175 -0.2487 -0.0189 0.071 Uiso 1 1 calc R . .
H34C H 0.9709 -0.2477 -0.0334 0.071 Uiso 1 1 calc R . .
C24 C 0.8990(8) -0.0749(8) 0.2802(4) 0.041(3) Uani 1 1 d . . .
H24 H 0.9526 -0.0527 0.3047 0.049 Uiso 1 1 calc R . .
C23 C 0.7711(10) -0.1030(8) 0.2881(3) 0.042(3) Uani 1 1 d . . .
H23 H 0.7347 -0.0996 0.3177 0.050 Uiso 1 1 calc R . .
C35 C 1.0554(9) -0.1055(9) 0.0288(4) 0.052(3) Uani 1 1 d . . .
H35A H 1.1287 -0.1334 0.0108 0.078 Uiso 1 1 calc R . .
H35B H 1.0852 -0.0951 0.0600 0.078 Uiso 1 1 calc R . .
H35C H 1.0274 -0.0409 0.0158 0.078 Uiso 1 1 calc R . .
C40 C 0.1738(10) -0.2975(10) 0.1735(4) 0.051(3) Uani 1 1 d . . .
H40 H 0.1219 -0.3512 0.1616 0.061 Uiso 1 1 calc R . .


_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
Cl1 Si1 2.026(3) . ?
Cl3 Si1 2.017(4) . ?
P1 N1 1.785(7) . ?
P1 C36 1.814(10) . ?
P1 C42 1.843(9) . ?
Si1 N1 1.693(8) . ?
Si1 Cl2 2.035(4) . ?
C27 C28 1.395(12) . ?
C27 C32 1.400(12) . ?
C27 C20 1.505(13) . ?
N1 C1 1.456(11) . ?
C20 C2 1.494(13) . ?
C20 C21 1.532(12) . ?
C38 C39 1.392(14) . ?
C38 C37 1.401(13) . ?
C5 C4 1.368(12) . ?
C5 C6 1.411(12) . ?
C7 C14 1.493(12) . ?
C7 C6 1.503(11) . ?
C7 C8 1.508(12) . ?
C9 C10 1.352(12) . ?
C9 C8 1.412(12) . ?
C43 C42 1.379(13) . ?
C43 C44 1.415(14) . ?
C28 C29 1.361(13) . ?
C37 C36 1.402(14) . ?
C1 C2 1.408(12) . ?
C1 C6 1.432(12) . ?
C32 C31 1.350(13) . ?
C19 C18 1.359(13) . ?
C19 C14 1.415(12) . ?
C36 C41 1.395(13) . ?
C13 C12 1.357(11) . ?
C13 C8 1.413(12) . ?
C26 C21 1.379(12) . ?
C26 C25 1.390(13) . ?
C44 C45 1.382(14) . ?
C42 C47 1.382(13) . ?
C33 C34 1.520(14) . ?
C33 C35 1.530(13) . ?
C33 C4 1.533(12) . ?
C46 C45 1.377(14) . ?
C46 C47 1.407(13) . ?
C11 C12 1.378(14) . ?
C11 C10 1.401(13) . ?
C31 C30 1.378(14) . ?
C2 C3 1.422(12) . ?
C39 C40 1.382(15) . ?
C14 C15 1.400(12) . ?
C25 C24 1.350(14) . ?
C16 C15 1.373(14) . ?
C16 C17 1.411(15) . ?
C4 C3 1.384(12) . ?
C21 C22 1.402(13) . ?
C22 C23 1.403(13) . ?
C41 C40 1.391(15) . ?
C17 C18 1.406(15) . ?
C30 C29 1.372(14) . ?
C24 C23 1.358(13) . ?

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 P1 C36 107.6(4) . . ?
N1 P1 C42 104.2(4) . . ?
C36 P1 C42 101.5(4) . . ?
N1 Si1 Cl3 114.4(3) . . ?
N1 Si1 Cl1 108.4(3) . . ?
Cl3 Si1 Cl1 107.21(15) . . ?
N1 Si1 Cl2 115.4(3) . . ?
Cl3 Si1 Cl2 104.34(15) . . ?
Cl1 Si1 Cl2 106.57(15) . . ?
C28 C27 C32 115.5(9) . . ?
C28 C27 C20 125.4(9) . . ?
C32 C27 C20 119.1(8) . . ?
C1 N1 Si1 118.7(5) . . ?
C1 N1 P1 110.3(5) . . ?
Si1 N1 P1 129.9(4) . . ?
C2 C20 C27 111.4(8) . . ?
C2 C20 C21 113.7(7) . . ?
C27 C20 C21 111.9(7) . . ?
C39 C38 C37 120.1(9) . . ?
C4 C5 C6 122.5(8) . . ?
C14 C7 C6 111.2(7) . . ?
C14 C7 C8 110.8(7) . . ?
C6 C7 C8 115.6(7) . . ?
C10 C9 C8 119.6(8) . . ?
C42 C43 C44 119.7(10) . . ?
C29 C28 C27 122.1(9) . . ?
C38 C37 C36 121.1(9) . . ?
C2 C1 C6 120.7(8) . . ?
C2 C1 N1 120.6(8) . . ?
C6 C1 N1 118.7(8) . . ?
C31 C32 C27 122.2(9) . . ?
C18 C19 C14 120.8(9) . . ?
C41 C36 C37 117.6(9) . . ?
C41 C36 P1 114.4(8) . . ?
C37 C36 P1 128.0(7) . . ?
C12 C13 C8 124.4(9) . . ?
C21 C26 C25 120.1(9) . . ?
C45 C44 C43 118.5(10) . . ?
C43 C42 C47 120.6(9) . . ?
C43 C42 P1 124.6(7) . . ?
C47 C42 P1 114.7(7) . . ?
C34 C33 C35 111.7(9) . . ?
C34 C33 C4 112.1(7) . . ?
C35 C33 C4 111.2(8) . . ?
C45 C46 C47 117.9(9) . . ?
C12 C11 C10 119.4(9) . . ?
C32 C31 C30 121.1(10) . . ?
C1 C2 C3 117.9(8) . . ?
C1 C2 C20 122.3(8) . . ?
C3 C2 C20 119.8(8) . . ?
C40 C39 C38 119.1(9) . . ?
C15 C14 C19 117.2(8) . . ?
C15 C14 C7 119.5(8) . . ?
C19 C14 C7 123.3(8) . . ?
C24 C25 C26 121.0(9) . . ?
C5 C6 C1 117.4(8) . . ?
C5 C6 C7 120.0(8) . . ?
C1 C6 C7 122.5(8) . . ?
C15 C16 C17 119.3(9) . . ?
C5 C4 C3 119.5(8) . . ?
C5 C4 C33 120.3(8) . . ?
C3 C4 C33 120.2(8) . . ?
C26 C21 C22 117.9(8) . . ?
C26 C21 C20 123.7(8) . . ?
C22 C21 C20 118.3(8) . . ?
C21 C22 C23 121.0(8) . . ?
C9 C8 C13 116.0(8) . . ?
C9 C8 C7 125.6(7) . . ?
C13 C8 C7 118.3(8) . . ?
C40 C41 C36 121.2(10) . . ?
C18 C17 C16 118.4(10) . . ?
C46 C45 C44 122.6(9) . . ?
C16 C15 C14 122.7(9) . . ?
C9 C10 C11 122.5(9) . . ?
C4 C3 C2 121.7(8) . . ?
C13 C12 C11 117.9(9) . . ?
C29 C30 C31 118.2(10) . . ?
C28 C29 C30 120.9(10) . . ?
C42 C47 C46 120.7(9) . . ?
C19 C18 C17 121.5(9) . . ?
C25 C24 C23 121.2(9) . . ?
C24 C23 C22 118.7(9) . . ?
C39 C40 C41 120.9(10) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.897
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.136
####################################################################### 
# 
# 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_cj1161
_database_code_depnum_ccdc_archive 'CCDC 1401428'
_audit_update_record             
;
2015-05-18 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C47 H42 Cl2 N P Si'
_chemical_formula_weight         750.78

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'
Si Si 0.0817 0.0704 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   P212121

loop_
_symmetry_equiv_pos_as_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'

_cell_length_a                   9.9729(4)
_cell_length_b                   13.3211(6)
_cell_length_c                   29.4129(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3907.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       colourless
_exptl_crystal_colour            block
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1576
_exptl_absorpt_coefficient_mu    0.273
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9475
_exptl_absorpt_correction_T_max  0.9865
_exptl_absorpt_process_details   'SCALE3 ABSPACK'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Gemini Ultra'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14488
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_sigmaI/netI    0.0608
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         2.91
_diffrn_reflns_theta_max         25.49
_reflns_number_total             6782
_reflns_number_gt                5927
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.
 One Cl and the H atom of the SiCl2H fragment of the molecule were found
 to be disordered over two sites. Both disordered Cl sets were refined
 anisotropically.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0559P)²+3.8418P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(9)
_refine_ls_number_reflns         6782
_refine_ls_number_parameters     482
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0520
_refine_ls_wR_factor_ref         0.1279
_refine_ls_wR_factor_gt          0.1201
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.163
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.66841(10) 0.55428(8) 0.11722(3) 0.0182(2) Uani 1 1 d . . .
Cl1 Cl 0.54407(12) 0.27447(8) 0.14949(4) 0.0326(3) Uani 1 1 d . A .
Si1 Si 0.46648(13) 0.41021(9) 0.16594(4) 0.0251(3) Uani 1 1 d D . .
Cl2 Cl 0.26916(13) 0.39457(12) 0.16778(5) 0.0254(5) Uani 0.743(4) 1 d P A 1
C7 C 0.4698(4) 0.4445(3) 0.03698(12) 0.0178(8) Uani 1 1 d . . .
H7 H 0.5588 0.4509 0.0523 0.021 Uiso 1 1 calc R . .
N1 N 0.5084(3) 0.5087(3) 0.13158(11) 0.0177(7) Uani 1 1 d . A .
C1 C 0.4029(4) 0.5555(3) 0.10404(13) 0.0164(8) Uani 1 1 d . . .
C42 C 0.7165(4) 0.6436(3) 0.16216(14) 0.0213(9) Uani 1 1 d . . .
C3 C 0.2240(4) 0.6752(3) 0.09590(13) 0.0177(8) Uani 1 1 d . . .
H3 H 0.1724 0.7287 0.1081 0.021 Uiso 1 1 calc R A .
C6 C 0.3800(4) 0.5222(3) 0.05952(13) 0.0176(9) Uani 1 1 d . A .
C47 C 0.6808(4) 0.6401(3) 0.20793(14) 0.0201(9) Uani 1 1 d . . .
H47 H 0.6285 0.5857 0.2190 0.024 Uiso 1 1 calc R . .
C9 C 0.5998(4) 0.5321(3) -0.02462(15) 0.0221(9) Uani 1 1 d . . .
H9 H 0.6559 0.5587 -0.0014 0.026 Uiso 1 1 calc R . .
C27 C 0.3577(4) 0.7936(3) 0.16833(13) 0.0199(9) Uani 1 1 d . A .
C41 C 0.8214(4) 0.4182(3) 0.17262(14) 0.0240(9) Uani 1 1 d . . .
H41 H 0.7885 0.4525 0.1986 0.029 Uiso 1 1 calc R . .
C33 C 0.0787(4) 0.6832(3) 0.02499(14) 0.0222(9) Uani 1 1 d . . .
H33 H 0.0467 0.7449 0.0410 0.027 Uiso 1 1 calc R A .
C21 C 0.2622(4) 0.6382(3) 0.20654(13) 0.0183(9) Uani 1 1 d . A .
C8 C 0.4950(4) 0.4701(3) -0.01282(13) 0.0180(9) Uani 1 1 d . . .
C5 C 0.2754(4) 0.5649(3) 0.03499(13) 0.0199(9) Uani 1 1 d . . .
H5 H 0.2588 0.5415 0.0050 0.024 Uiso 1 1 calc R A .
C20 C 0.3541(4) 0.6787(3) 0.16948(13) 0.0181(9) Uani 1 1 d . . .
H20 H 0.4468 0.6566 0.1778 0.022 Uiso 1 1 calc R A .
C14 C 0.4295(4) 0.3350(3) 0.04257(13) 0.0198(9) Uani 1 1 d . . .
C19 C 0.3036(4) 0.3033(3) 0.05584(14) 0.0237(10) Uani 1 1 d . . .
H19 H 0.2359 0.3515 0.0622 0.028 Uiso 1 1 calc R . .
C10 C 0.6253(5) 0.5565(4) -0.06926(16) 0.0297(11) Uani 1 1 d . . .
H10 H 0.7001 0.5973 -0.0768 0.036 Uiso 1 1 calc R . .
C36 C 0.7803(4) 0.4479(3) 0.12936(14) 0.0209(9) Uani 1 1 d . . .
C22 C 0.1294(4) 0.6161(4) 0.19956(15) 0.0320(11) Uani 1 1 d . . .
H22 H 0.0924 0.6235 0.1700 0.038 Uiso 1 1 calc R A .
C15 C 0.5266(4) 0.2626(3) 0.03280(14) 0.0252(10) Uani 1 1 d . . .
H15 H 0.6133 0.2829 0.0231 0.030 Uiso 1 1 calc R . .
C4 C 0.1941(4) 0.6401(3) 0.05230(13) 0.0183(9) Uani 1 1 d . A .
C38 C 0.9198(4) 0.3183(4) 0.09720(18) 0.0328(11) Uani 1 1 d . . .
H38 H 0.9535 0.2839 0.0713 0.039 Uiso 1 1 calc R . .
C39 C 0.9592(5) 0.2891(4) 0.13978(17) 0.0336(11) Uani 1 1 d . . .
H39 H 1.0200 0.2348 0.1433 0.040 Uiso 1 1 calc R . .
C13 C 0.4124(4) 0.4325(3) -0.04754(14) 0.0221(9) Uani 1 1 d . . .
H13 H 0.3405 0.3886 -0.0403 0.026 Uiso 1 1 calc R . .
C46 C 0.7205(5) 0.7145(3) 0.23720(15) 0.0277(10) Uani 1 1 d . . .
H46 H 0.6946 0.7113 0.2682 0.033 Uiso 1 1 calc R . .
C40 C 0.9105(4) 0.3386(4) 0.17787(16) 0.0304(11) Uani 1 1 d . . .
H40 H 0.9379 0.3183 0.2074 0.036 Uiso 1 1 calc R . .
C18 C 0.2750(5) 0.2014(3) 0.05999(15) 0.0260(10) Uani 1 1 d . . .
H18 H 0.1882 0.1803 0.0693 0.031 Uiso 1 1 calc R . .
C28 C 0.2714(5) 0.8540(3) 0.19335(14) 0.0280(10) Uani 1 1 d . . .
H28 H 0.2034 0.8244 0.2116 0.034 Uiso 1 1 calc R A .
C35 C 0.1198(5) 0.7136(4) -0.02289(15) 0.0341(11) Uani 1 1 d . A .
H35A H 0.1994 0.7566 -0.0214 0.051 Uiso 1 1 calc R . .
H35B H 0.0462 0.7503 -0.0374 0.051 Uiso 1 1 calc R . .
H35C H 0.1403 0.6533 -0.0407 0.051 Uiso 1 1 calc R . .
C32 C 0.4563(5) 0.8402(3) 0.14215(15) 0.0272(10) Uani 1 1 d . . .
H32 H 0.5163 0.8002 0.1248 0.033 Uiso 1 1 calc R A .
C16 C 0.4976(4) 0.1618(3) 0.03717(16) 0.0288(11) Uani 1 1 d . . .
H16 H 0.5648 0.1132 0.0309 0.035 Uiso 1 1 calc R . .
C17 C 0.3724(5) 0.1311(3) 0.05055(15) 0.0284(10) Uani 1 1 d . . .
H17 H 0.3529 0.0616 0.0533 0.034 Uiso 1 1 calc R . .
C37 C 0.8311(4) 0.3977(3) 0.09144(15) 0.0240(9) Uani 1 1 d . . .
C43 C 0.7940(4) 0.7238(3) 0.14693(15) 0.0289(10) Uani 1 1 d . . .
H43 H 0.8163 0.7303 0.1157 0.035 Uiso 1 1 calc R . .
C30 C 0.3821(5) 1.0027(4) 0.16571(17) 0.0344(11) Uani 1 1 d . . .
H30 H 0.3900 1.0737 0.1648 0.041 Uiso 1 1 calc R A .
C2 C 0.3263(4) 0.6348(3) 0.12194(12) 0.0167(8) Uani 1 1 d . A .
C31 C 0.4684(5) 0.9437(4) 0.14101(16) 0.0344(11) Uani 1 1 d . A .
H31 H 0.5365 0.9740 0.1231 0.041 Uiso 1 1 calc R . .
C11 C 0.5410(5) 0.5211(4) -0.10334(15) 0.0330(11) Uani 1 1 d . . .
H11 H 0.5561 0.5394 -0.1341 0.040 Uiso 1 1 calc R . .
C34 C -0.0373(5) 0.6093(4) 0.02335(19) 0.0377(12) Uani 1 1 d . A .
H34A H -0.0081 0.5473 0.0084 0.057 Uiso 1 1 calc R . .
H34B H -0.1118 0.6389 0.0062 0.057 Uiso 1 1 calc R . .
H34C H -0.0669 0.5941 0.0544 0.057 Uiso 1 1 calc R . .
C24 C 0.1007(5) 0.5706(4) 0.27798(15) 0.0299(11) Uani 1 1 d . . .
H24 H 0.0460 0.5468 0.3021 0.036 Uiso 1 1 calc R A .
C26 C 0.3129(5) 0.6267(4) 0.24982(14) 0.0318(11) Uani 1 1 d . . .
H26 H 0.4044 0.6422 0.2555 0.038 Uiso 1 1 calc R A .
C23 C 0.0480(5) 0.5832(4) 0.23487(15) 0.0336(11) Uani 1 1 d . A .
H23 H -0.0441 0.5693 0.2294 0.040 Uiso 1 1 calc R . .
C29 C 0.2846(5) 0.9585(4) 0.19168(16) 0.0333(11) Uani 1 1 d . A .
H29 H 0.2251 0.9994 0.2088 0.040 Uiso 1 1 calc R . .
C45 C 0.7978(5) 0.7942(4) 0.22223(17) 0.0372(12) Uani 1 1 d . . .
H45 H 0.8198 0.8466 0.2428 0.045 Uiso 1 1 calc R . .
C12 C 0.4356(5) 0.4592(4) -0.09210(15) 0.0298(11) Uani 1 1 d . . .
H12 H 0.3781 0.4347 -0.1153 0.036 Uiso 1 1 calc R . .
C25 C 0.2332(5) 0.5930(4) 0.28535(15) 0.0401(13) Uani 1 1 d . A .
H25 H 0.2705 0.5854 0.3149 0.048 Uiso 1 1 calc R . .
C44 C 0.8409(3) 0.7990(3) 0.18060(9) 0.0448(14) Uani 1 1 d . . .
H44 H 0.9019 0.8502 0.1718 0.054 Uiso 1 1 calc R . .
H37 H 0.8143 0.4258 0.0650 0.031(13) Uiso 1 1 d R . .
Cl2A Cl 0.4938(3) 0.4223(3) 0.23470(9) 0.0359(16) Uani 0.257(4) 1 d PRD A 2
H1 H 0.5198 0.4293 0.2084 0.043 Uiso 0.743(4) 1 d PRD A 1
H1A H 0.328(4) 0.394(17) 0.163(8) 0.043 Uiso 0.257(4) 1 d PD A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 N1 1.760(3) . ?
P1 C36 1.839(4) . ?
P1 C42 1.842(4) . ?
Cl1 Si1 2.0254(17) . ?
Si1 N1 1.707(4) . ?
Si1 Cl2 1.9796(18) . ?
Si1 Cl2A 2.047(2) . ?
C7 C6 1.520(6) . ?
C7 C14 1.522(6) . ?
C7 C8 1.525(5) . ?
N1 C1 1.466(5) . ?
C1 C6 1.401(6) . ?
C1 C2 1.406(6) . ?
C42 C43 1.393(6) . ?
C42 C47 1.393(6) . ?
C3 C2 1.385(6) . ?
C3 C4 1.397(6) . ?
C6 C5 1.391(6) . ?
C47 C46 1.371(6) . ?
C9 C10 1.376(6) . ?
C9 C8 1.377(6) . ?
C27 C28 1.389(6) . ?
C27 C32 1.395(6) . ?
C27 C20 1.532(6) . ?
C41 C40 1.392(6) . ?
C41 C36 1.394(6) . ?
C33 C4 1.516(6) . ?
C33 C34 1.520(6) . ?
C33 C35 1.522(6) . ?
C21 C22 1.372(6) . ?
C21 C26 1.379(6) . ?
C21 C20 1.523(6) . ?
C8 C13 1.404(6) . ?
C5 C4 1.385(6) . ?
C20 C2 1.541(5) . ?
C14 C19 1.381(6) . ?
C14 C15 1.396(6) . ?
C19 C18 1.393(6) . ?
C10 C11 1.390(7) . ?
C36 C37 1.395(6) . ?
C22 C23 1.390(6) . ?
C15 C16 1.380(6) . ?
C38 C39 1.369(7) . ?
C38 C37 1.390(7) . ?
C39 C40 1.387(7) . ?
C13 C12 1.378(6) . ?
C46 C45 1.384(7) . ?
C18 C17 1.377(6) . ?
C28 C29 1.399(7) . ?
C32 C31 1.384(7) . ?
C16 C17 1.371(6) . ?
C43 C44 1.484(5) . ?
C30 C29 1.369(7) . ?
C30 C31 1.373(7) . ?
C11 C12 1.376(7) . ?
C24 C25 1.372(7) . ?
C24 C23 1.383(7) . ?
C26 C25 1.388(6) . ?
C45 C44 1.299(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 P1 C36 103.73(18) . . ?
N1 P1 C42 106.69(17) . . ?
C36 P1 C42 101.57(19) . . ?
N1 Si1 Cl2 109.89(13) . . ?
N1 Si1 Cl1 116.80(13) . . ?
Cl2 Si1 Cl1 106.99(8) . . ?
N1 Si1 Cl2A 119.45(15) . . ?
Cl2 Si1 Cl2A 96.52(12) . . ?
Cl1 Si1 Cl2A 104.80(12) . . ?
C6 C7 C14 116.8(3) . . ?
C6 C7 C8 111.3(3) . . ?
C14 C7 C8 111.2(3) . . ?
C1 N1 Si1 118.6(3) . . ?
C1 N1 P1 111.8(2) . . ?
Si1 N1 P1 129.0(2) . . ?
C6 C1 C2 119.9(4) . . ?
C6 C1 N1 119.9(4) . . ?
C2 C1 N1 120.2(3) . . ?
C43 C42 C47 118.5(4) . . ?
C43 C42 P1 114.2(3) . . ?
C47 C42 P1 127.3(3) . . ?
C2 C3 C4 122.3(4) . . ?
C5 C6 C1 118.5(4) . . ?
C5 C6 C7 119.6(3) . . ?
C1 C6 C7 121.8(4) . . ?
C46 C47 C42 120.6(4) . . ?
C10 C9 C8 121.5(4) . . ?
C28 C27 C32 118.1(4) . . ?
C28 C27 C20 123.6(4) . . ?
C32 C27 C20 118.3(4) . . ?
C40 C41 C36 120.3(4) . . ?
C4 C33 C34 110.5(4) . . ?
C4 C33 C35 112.8(4) . . ?
C34 C33 C35 110.3(4) . . ?
C22 C21 C26 118.0(4) . . ?
C22 C21 C20 123.4(4) . . ?
C26 C21 C20 118.6(4) . . ?
C9 C8 C13 118.4(4) . . ?
C9 C8 C7 120.1(4) . . ?
C13 C8 C7 121.5(4) . . ?
C4 C5 C6 123.0(4) . . ?
C21 C20 C27 112.5(3) . . ?
C21 C20 C2 114.0(3) . . ?
C27 C20 C2 111.3(3) . . ?
C19 C14 C15 118.5(4) . . ?
C19 C14 C7 124.3(4) . . ?
C15 C14 C7 117.2(4) . . ?
C14 C19 C18 120.6(4) . . ?
C9 C10 C11 119.8(4) . . ?
C41 C36 C37 119.1(4) . . ?
C41 C36 P1 125.0(3) . . ?
C37 C36 P1 115.7(3) . . ?
C21 C22 C23 121.3(4) . . ?
C16 C15 C14 120.5(4) . . ?
C5 C4 C3 117.0(4) . . ?
C5 C4 C33 121.5(4) . . ?
C3 C4 C33 121.5(4) . . ?
C39 C38 C37 120.7(4) . . ?
C38 C39 C40 120.2(4) . . ?
C12 C13 C8 120.1(4) . . ?
C47 C46 C45 121.0(4) . . ?
C39 C40 C41 119.7(4) . . ?
C17 C18 C19 120.0(4) . . ?
C27 C28 C29 120.0(5) . . ?
C31 C32 C27 121.2(4) . . ?
C17 C16 C15 120.5(4) . . ?
C16 C17 C18 119.9(4) . . ?
C38 C37 C36 119.9(4) . . ?
C42 C43 C44 118.6(4) . . ?
C29 C30 C31 119.6(4) . . ?
C3 C2 C1 119.0(4) . . ?
C3 C2 C20 119.2(3) . . ?
C1 C2 C20 121.8(3) . . ?
C30 C31 C32 120.2(5) . . ?
C12 C11 C10 119.4(4) . . ?
C25 C24 C23 119.0(4) . . ?
C21 C26 C25 121.4(4) . . ?
C24 C23 C22 120.1(4) . . ?
C30 C29 C28 120.9(5) . . ?
C44 C45 C46 121.4(4) . . ?
C11 C12 C13 120.8(4) . . ?
C24 C25 C26 120.2(4) . . ?
C45 C44 C43 119.4(4) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.49
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.316
_refine_diff_density_min         -0.985
_refine_diff_density_rms         0.065
####################################################################### 
# 
# 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_cj1135
_database_code_depnum_ccdc_archive 'CCDC 1401429'
_audit_update_record             
;
2015-07-22 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C61 H55 Cl5 N P Si'
_chemical_formula_weight         1038.37

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   12.6871(18)
_cell_length_b                   13.720(3)
_cell_length_c                   16.385(2)
_cell_angle_alpha                72.602(15)
_cell_angle_beta                 83.732(11)
_cell_angle_gamma                80.682(15)
_cell_volume                     2680.1(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9836
_cell_measurement_theta_min      2.99
_cell_measurement_theta_max      25.50

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1084
_exptl_absorpt_coefficient_mu    0.363
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.931
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_process_details   XDS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71080
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'Australian Synchrotron'
_diffrn_radiation_monochromator  ?
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18171
_diffrn_reflns_av_R_equivalents  0.1050
_diffrn_reflns_av_sigmaI/netI    0.2140
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.99
_diffrn_reflns_theta_max         25.50
_reflns_number_total             9836
_reflns_number_gt                4043
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Blu-Ice (McPhillips, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CifTAB

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0798P)²+0.0000P] 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         9836
_refine_ls_number_parameters     624
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1918
_refine_ls_R_factor_gt           0.0798
_refine_ls_wR_factor_ref         0.2279
_refine_ls_wR_factor_gt          0.1622
_refine_ls_goodness_of_fit_ref   0.940
_refine_ls_restrained_S_all      0.940
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.41411(11) 0.48854(12) 0.19294(8) 0.0300(4) Uani 1 1 d . . .
Cl1 Cl 0.07112(10) 0.45475(12) 0.15232(8) 0.0347(4) Uani 1 1 d . . .
Si1 Si 0.23340(12) 0.45171(13) 0.12844(9) 0.0301(4) Uani 1 1 d . . .
N1 N 0.2744(3) 0.5045(4) 0.2029(2) 0.0261(11) Uani 1 1 d . . .
C1 C 0.2118(4) 0.5700(4) 0.2505(3) 0.0280(13) Uani 1 1 d . . .
C49 C 0.3399(4) 0.5835(5) -0.0210(3) 0.0349(15) Uani 1 1 d . . .
H49 H 0.3898 0.5891 0.0160 0.042 Uiso 1 1 calc R . .
C59 C 0.2375(5) 0.2328(5) 0.2000(3) 0.0370(15) Uani 1 1 d . . .
H59 H 0.1694 0.2486 0.2270 0.044 Uiso 1 1 calc R . .
C2 C 0.1888(4) 0.5304(4) 0.3397(3) 0.0262(13) Uani 1 1 d . . .
C20 C 0.1804(4) 0.7204(5) 0.1131(3) 0.0293(13) Uani 1 1 d . . .
H20 H 0.2365 0.6756 0.0881 0.035 Uiso 1 1 calc R . .
C5 C 0.1410(4) 0.7415(5) 0.2607(3) 0.0299(13) Uani 1 1 d . . .
H5 H 0.1210 0.8127 0.2332 0.036 Uiso 1 1 calc R . .
C47 C 0.4506(4) 0.2991(5) 0.3173(3) 0.0332(14) Uani 1 1 d . . .
H47 H 0.4017 0.2783 0.2879 0.040 Uiso 1 1 calc R . .
C41 C 0.4220(4) 0.6684(5) 0.2493(3) 0.0319(14) Uani 1 1 d . . .
H41 H 0.3685 0.6474 0.2936 0.038 Uiso 1 1 calc R . .
C22 C 0.3152(4) 0.8461(5) 0.0559(3) 0.0362(15) Uani 1 1 d . . .
H22 H 0.3693 0.7885 0.0608 0.043 Uiso 1 1 calc R . .
C29 C -0.1159(4) 0.7082(5) 0.0968(3) 0.0356(15) Uani 1 1 d . . .
H29 H -0.1799 0.7017 0.1329 0.043 Uiso 1 1 calc R . .
C15 C -0.0038(4) 0.4309(5) 0.3638(3) 0.0330(14) Uani 1 1 d . . .
H15 H -0.0112 0.5022 0.3597 0.040 Uiso 1 1 calc R . .
C21 C 0.2094(4) 0.8296(5) 0.0793(3) 0.0284(13) Uani 1 1 d . . .
C6 C 0.1805(4) 0.6754(5) 0.2104(3) 0.0282(13) Uani 1 1 d . . .
C14 C 0.0972(4) 0.3720(5) 0.3773(3) 0.0318(14) Uani 1 1 d . . .
C8 C 0.2243(4) 0.3884(4) 0.4789(3) 0.0290(13) Uani 1 1 d . . .
C48 C 0.2571(4) 0.5233(4) 0.0127(3) 0.0271(13) Uani 1 1 d . . .
C31 C -0.0251(5) 0.7319(5) -0.0429(4) 0.0397(16) Uani 1 1 d . . .
H31 H -0.0266 0.7416 -0.1027 0.048 Uiso 1 1 calc R . .
C55 C 0.3887(4) 0.2851(5) 0.1052(3) 0.0339(15) Uani 1 1 d . . .
H55 H 0.4256 0.3374 0.0669 0.041 Uiso 1 1 calc R . .
C42 C 0.4685(4) 0.4032(5) 0.2917(3) 0.0278(13) Uani 1 1 d . . .
C13 C 0.3279(4) 0.3984(5) 0.4964(3) 0.0354(15) Uani 1 1 d . . .
H13 H 0.3790 0.4202 0.4502 0.042 Uiso 1 1 calc R . .
C36 C 0.4575(4) 0.6078(5) 0.1912(3) 0.0309(14) Uani 1 1 d . . .
C43 C 0.5449(4) 0.4299(5) 0.3351(3) 0.0318(14) Uani 1 1 d . . .
H43 H 0.5608 0.4987 0.3187 0.038 Uiso 1 1 calc R . .
C45 C 0.5767(5) 0.2556(5) 0.4258(4) 0.0409(16) Uani 1 1 d . . .
H45 H 0.6135 0.2058 0.4710 0.049 Uiso 1 1 calc R . .
C54 C 0.2903(4) 0.3135(5) 0.1465(3) 0.0303(14) Uani 1 1 d . . .
C46 C 0.5025(5) 0.2268(5) 0.3841(3) 0.0396(15) Uani 1 1 d . . .
H46 H 0.4874 0.1576 0.4014 0.047 Uiso 1 1 calc R . .
C32 C 0.0695(4) 0.7292(5) -0.0078(3) 0.0342(14) Uani 1 1 d . . .
H32 H 0.1334 0.7362 -0.0439 0.041 Uiso 1 1 calc R . .
C16 C -0.0928(5) 0.3891(5) 0.3562(3) 0.0374(15) Uani 1 1 d . . .
H16 H -0.1600 0.4315 0.3469 0.045 Uiso 1 1 calc R . .
C28 C -0.0202(4) 0.7056(5) 0.1304(3) 0.0366(15) Uani 1 1 d . . .
H28 H -0.0185 0.6963 0.1901 0.044 Uiso 1 1 calc R . .
C4 C 0.1299(4) 0.7060(5) 0.3498(3) 0.0298(14) Uani 1 1 d . . .
C57 C 0.3808(5) 0.1060(5) 0.1733(4) 0.0489(18) Uani 1 1 d . . .
H57 H 0.4115 0.0359 0.1828 0.059 Uiso 1 1 calc R . .
C7 C 0.1970(4) 0.4148(5) 0.3848(3) 0.0303(14) Uani 1 1 d . . .
H7 H 0.2574 0.3801 0.3545 0.036 Uiso 1 1 calc R . .
C40 C 0.4651(4) 0.7566(5) 0.2410(4) 0.0377(15) Uani 1 1 d . . .
H40 H 0.4405 0.7958 0.2799 0.045 Uiso 1 1 calc R . .
C39 C 0.5439(5) 0.7902(5) 0.1770(4) 0.0422(16) Uani 1 1 d . . .
H39 H 0.5717 0.8522 0.1718 0.051 Uiso 1 1 calc R . .
C24 C 0.2659(5) 1.0276(6) 0.0179(4) 0.0484(17) Uani 1 1 d . . .
H24 H 0.2851 1.0952 -0.0027 0.058 Uiso 1 1 calc R . .
C11 C 0.2821(5) 0.3463(5) 0.6471(3) 0.0387(15) Uani 1 1 d . . .
H11 H 0.3010 0.3319 0.7045 0.046 Uiso 1 1 calc R . .
C37 C 0.5390(4) 0.6424(5) 0.1282(3) 0.0339(14) Uani 1 1 d . . .
H37 H 0.5657 0.6031 0.0896 0.041 Uiso 1 1 calc R . .
C33 C 0.1018(4) 0.7803(5) 0.4034(3) 0.0332(14) Uani 1 1 d . . .
H33 H 0.0755 0.7402 0.4616 0.040 Uiso 1 1 calc R . .
C23 C 0.3433(5) 0.9443(5) 0.0258(4) 0.0409(16) Uani 1 1 d . . .
H23 H 0.4162 0.9539 0.0107 0.049 Uiso 1 1 calc R . .
C19 C 0.1030(5) 0.2666(5) 0.3853(3) 0.0372(15) Uani 1 1 d . . .
H19 H 0.1695 0.2234 0.3964 0.045 Uiso 1 1 calc R . .
C17 C -0.0842(5) 0.2856(6) 0.3623(3) 0.0453(18) Uani 1 1 d . . .
H17 H -0.1451 0.2568 0.3561 0.054 Uiso 1 1 calc R . .
C44 C 0.5968(4) 0.3562(5) 0.4017(3) 0.0356(15) Uani 1 1 d . . .
H44 H 0.6469 0.3755 0.4310 0.043 Uiso 1 1 calc R . .
C9 C 0.1522(4) 0.3573(4) 0.5471(3) 0.0335(14) Uani 1 1 d . . .
H9 H 0.0820 0.3500 0.5371 0.040 Uiso 1 1 calc R . .
C26 C 0.1312(4) 0.9152(5) 0.0694(3) 0.0340(14) Uani 1 1 d . . .
H26 H 0.0582 0.9059 0.0832 0.041 Uiso 1 1 calc R . .
C30 C -0.1179(5) 0.7205(5) 0.0099(4) 0.0406(16) Uani 1 1 d . . .
H30 H -0.1833 0.7211 -0.0136 0.049 Uiso 1 1 calc R . .
C3 C 0.1506(4) 0.6003(5) 0.3869(3) 0.0331(14) Uani 1 1 d . . .
H3 H 0.1383 0.5741 0.4472 0.040 Uiso 1 1 calc R . .
C38 C 0.5811(4) 0.7317(5) 0.1210(4) 0.0423(16) Uani 1 1 d . . .
H38 H 0.6357 0.7530 0.0777 0.051 Uiso 1 1 calc R . .
C25 C 0.1590(5) 1.0143(5) 0.0396(4) 0.0442(16) Uani 1 1 d . . .
H25 H 0.1054 1.0725 0.0342 0.053 Uiso 1 1 calc R . .
C50 C 0.3497(4) 0.6349(5) -0.1079(3) 0.0356(15) Uani 1 1 d . . .
H50 H 0.4044 0.6778 -0.1285 0.043 Uiso 1 1 calc R . .
C18 C 0.0137(5) 0.2239(6) 0.3774(3) 0.0456(17) Uani 1 1 d . . .
H18 H 0.0199 0.1525 0.3824 0.055 Uiso 1 1 calc R . .
C27 C 0.0739(4) 0.7164(5) 0.0786(3) 0.0297(13) Uani 1 1 d . . .
C56 C 0.4330(5) 0.1826(5) 0.1192(4) 0.0432(17) Uani 1 1 d . . .
H56 H 0.4999 0.1656 0.0910 0.052 Uiso 1 1 calc R . .
C51 C 0.2832(4) 0.6257(5) -0.1645(3) 0.0366(15) Uani 1 1 d . . .
H51 H 0.2920 0.6603 -0.2239 0.044 Uiso 1 1 calc R . .
C34 C 0.2032(5) 0.8212(6) 0.4143(4) 0.0534(19) Uani 1 1 d . . .
H34A H 0.2317 0.8603 0.3581 0.080 Uiso 1 1 calc R . .
H34B H 0.2568 0.7631 0.4399 0.080 Uiso 1 1 calc R . .
H34C H 0.1859 0.8662 0.4517 0.080 Uiso 1 1 calc R . .
C53 C 0.1889(4) 0.5140(5) -0.0458(3) 0.0357(15) Uani 1 1 d . . .
H53 H 0.1327 0.4729 -0.0256 0.043 Uiso 1 1 calc R . .
C58 C 0.2826(5) 0.1309(5) 0.2142(4) 0.0473(17) Uani 1 1 d . . .
H58 H 0.2464 0.0778 0.2521 0.057 Uiso 1 1 calc R . .
C52 C 0.2024(4) 0.5645(5) -0.1331(3) 0.0350(15) Uani 1 1 d . . .
H52 H 0.1557 0.5569 -0.1716 0.042 Uiso 1 1 calc R . .
C10 C 0.1812(5) 0.3363(5) 0.6310(3) 0.0407(16) Uani 1 1 d . . .
H10 H 0.1304 0.3148 0.6775 0.049 Uiso 1 1 calc R . .
C35 C 0.0142(5) 0.8688(5) 0.3695(4) 0.0480(17) Uani 1 1 d . . .
H35A H 0.0381 0.9109 0.3129 0.072 Uiso 1 1 calc R . .
H35B H -0.0012 0.9115 0.4089 0.072 Uiso 1 1 calc R . .
H35C H -0.0506 0.8411 0.3648 0.072 Uiso 1 1 calc R . .
C12 C 0.3560(5) 0.3772(5) 0.5796(4) 0.0429(16) Uani 1 1 d . . .
H12 H 0.4262 0.3839 0.5904 0.051 Uiso 1 1 calc R . .
Cl4 Cl 0.80570(18) 0.91651(17) 0.19928(11) 0.0793(7) Uani 1 1 d . . .
Cl5 Cl 0.8391(3) 1.1026(2) 0.23646(15) 0.1379(12) Uani 1 1 d . . .
C60 C 0.7927(9) 1.0493(7) 0.1702(5) 0.115(4) Uani 1 1 d . . .
H60A H 0.8301 1.0731 0.1130 0.138 Uiso 1 1 calc R . .
H60B H 0.7158 1.0762 0.1642 0.138 Uiso 1 1 calc R . .
Cl3 Cl 0.69359(17) 0.96506(17) 0.48087(13) 0.0796(6) Uani 1 1 d . . .
Cl2 Cl 0.55054(18) 0.94353(19) 0.36249(15) 0.0898(7) Uani 1 1 d . . .
C61 C 0.6662(6) 0.8903(6) 0.4187(4) 0.066(2) Uani 1 1 d . . .
H61A H 0.6570 0.8204 0.4563 0.080 Uiso 1 1 calc R . .
H61B H 0.7279 0.8835 0.3774 0.080 Uiso 1 1 calc R . .


_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
P1 N1 1.746(4) . ?
P1 C36 1.800(6) . ?
P1 C42 1.821(5) . ?
Cl1 Si1 2.049(2) . ?
Si1 N1 1.753(4) . ?
Si1 C54 1.863(6) . ?
Si1 C48 1.873(5) . ?
N1 C1 1.449(6) . ?
C1 C6 1.408(7) . ?
C1 C2 1.414(7) . ?
C49 C50 1.388(7) . ?
C49 C48 1.405(7) . ?
C59 C58 1.382(8) . ?
C59 C54 1.406(8) . ?
C2 C3 1.401(7) . ?
C2 C7 1.528(8) . ?
C20 C21 1.524(8) . ?
C20 C6 1.529(7) . ?
C20 C27 1.535(7) . ?
C5 C4 1.393(7) . ?
C5 C6 1.400(7) . ?
C47 C46 1.382(8) . ?
C47 C42 1.411(8) . ?
C41 C40 1.370(8) . ?
C41 C36 1.435(7) . ?
C22 C23 1.381(8) . ?
C22 C21 1.390(7) . ?
C29 C28 1.378(7) . ?
C29 C30 1.386(7) . ?
C15 C16 1.379(7) . ?
C15 C14 1.401(7) . ?
C21 C26 1.391(8) . ?
C14 C19 1.402(8) . ?
C14 C7 1.510(7) . ?
C8 C9 1.374(7) . ?
C8 C13 1.411(7) . ?
C8 C7 1.540(7) . ?
C48 C53 1.405(7) . ?
C31 C32 1.378(7) . ?
C31 C30 1.384(7) . ?
C55 C56 1.388(8) . ?
C55 C54 1.408(7) . ?
C42 C43 1.415(7) . ?
C13 C12 1.381(7) . ?
C36 C37 1.411(7) . ?
C43 C44 1.387(7) . ?
C45 C44 1.375(8) . ?
C45 C46 1.391(8) . ?
C32 C27 1.379(7) . ?
C16 C17 1.381(9) . ?
C28 C27 1.389(7) . ?
C4 C3 1.387(8) . ?
C4 C33 1.513(7) . ?
C57 C56 1.367(9) . ?
C57 C58 1.392(8) . ?
C40 C39 1.394(7) . ?
C39 C38 1.391(8) . ?
C24 C23 1.365(8) . ?
C24 C25 1.391(8) . ?
C11 C10 1.371(8) . ?
C11 C12 1.381(7) . ?
C37 C38 1.383(8) . ?
C33 C35 1.521(8) . ?
C33 C34 1.530(8) . ?
C19 C18 1.391(8) . ?
C17 C18 1.387(8) . ?
C9 C10 1.395(7) . ?
C26 C25 1.390(8) . ?
C50 C51 1.365(7) . ?
C51 C52 1.387(8) . ?
C53 C52 1.396(7) . ?
Cl4 C60 1.725(9) . ?
Cl5 C60 1.677(8) . ?
Cl3 C61 1.739(7) . ?
Cl2 C61 1.755(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 P1 C36 108.1(2) . . ?
N1 P1 C42 110.4(2) . . ?
C36 P1 C42 100.7(3) . . ?
N1 Si1 C54 112.0(2) . . ?
N1 Si1 C48 116.2(2) . . ?
C54 Si1 C48 109.4(2) . . ?
N1 Si1 Cl1 105.38(14) . . ?
C54 Si1 Cl1 106.23(19) . . ?
C48 Si1 Cl1 106.90(17) . . ?
C1 N1 P1 123.0(3) . . ?
C1 N1 Si1 129.3(3) . . ?
P1 N1 Si1 106.4(2) . . ?
C6 C1 C2 119.1(5) . . ?
C6 C1 N1 120.7(4) . . ?
C2 C1 N1 120.0(5) . . ?
C50 C49 C48 120.7(5) . . ?
C58 C59 C54 121.4(5) . . ?
C3 C2 C1 118.3(5) . . ?
C3 C2 C7 119.3(4) . . ?
C1 C2 C7 122.3(5) . . ?
C21 C20 C6 114.4(4) . . ?
C21 C20 C27 109.6(5) . . ?
C6 C20 C27 112.4(4) . . ?
C4 C5 C6 122.0(5) . . ?
C46 C47 C42 121.6(5) . . ?
C40 C41 C36 120.3(5) . . ?
C23 C22 C21 121.6(6) . . ?
C28 C29 C30 119.3(5) . . ?
C16 C15 C14 122.4(6) . . ?
C22 C21 C26 118.1(6) . . ?
C22 C21 C20 120.7(5) . . ?
C26 C21 C20 121.2(5) . . ?
C5 C6 C1 119.5(5) . . ?
C5 C6 C20 117.7(5) . . ?
C1 C6 C20 122.6(5) . . ?
C15 C14 C19 116.4(5) . . ?
C15 C14 C7 124.2(6) . . ?
C19 C14 C7 119.4(5) . . ?
C9 C8 C13 117.9(5) . . ?
C9 C8 C7 123.3(5) . . ?
C13 C8 C7 118.7(4) . . ?
C53 C48 C49 117.0(5) . . ?
C53 C48 Si1 117.8(4) . . ?
C49 C48 Si1 125.2(4) . . ?
C32 C31 C30 119.2(5) . . ?
C56 C55 C54 121.6(6) . . ?
C47 C42 C43 117.2(5) . . ?
C47 C42 P1 118.6(4) . . ?
C43 C42 P1 123.0(5) . . ?
C12 C13 C8 121.1(5) . . ?
C37 C36 C41 116.7(5) . . ?
C37 C36 P1 116.1(4) . . ?
C41 C36 P1 127.1(4) . . ?
C44 C43 C42 120.4(6) . . ?
C44 C45 C46 120.0(6) . . ?
C59 C54 C55 116.7(5) . . ?
C59 C54 Si1 122.4(4) . . ?
C55 C54 Si1 120.9(4) . . ?
C47 C46 C45 119.8(6) . . ?
C31 C32 C27 121.6(5) . . ?
C15 C16 C17 119.9(6) . . ?
C29 C28 C27 121.2(5) . . ?
C3 C4 C5 117.1(5) . . ?
C3 C4 C33 121.8(5) . . ?
C5 C4 C33 121.1(5) . . ?
C56 C57 C58 119.8(6) . . ?
C14 C7 C2 111.6(5) . . ?
C14 C7 C8 111.4(4) . . ?
C2 C7 C8 112.2(4) . . ?
C41 C40 C39 121.8(6) . . ?
C38 C39 C40 119.0(6) . . ?
C23 C24 C25 120.6(7) . . ?
C10 C11 C12 119.6(5) . . ?
C38 C37 C36 122.0(5) . . ?
C4 C33 C35 114.6(4) . . ?
C4 C33 C34 109.4(5) . . ?
C35 C33 C34 110.7(5) . . ?
C24 C23 C22 119.6(6) . . ?
C18 C19 C14 121.5(6) . . ?
C16 C17 C18 119.7(6) . . ?
C45 C44 C43 121.0(5) . . ?
C8 C9 C10 120.7(5) . . ?
C25 C26 C21 120.6(5) . . ?
C31 C30 C29 120.4(5) . . ?
C4 C3 C2 123.2(5) . . ?
C37 C38 C39 120.1(6) . . ?
C26 C25 C24 119.5(6) . . ?
C51 C50 C49 122.0(6) . . ?
C17 C18 C19 120.0(6) . . ?
C32 C27 C28 118.3(5) . . ?
C32 C27 C20 119.2(5) . . ?
C28 C27 C20 122.4(4) . . ?
C57 C56 C55 120.3(6) . . ?
C50 C51 C52 118.3(5) . . ?
C52 C53 C48 120.9(5) . . ?
C59 C58 C57 120.2(6) . . ?
C51 C52 C53 121.0(5) . . ?
C11 C10 C9 120.8(5) . . ?
C13 C12 C11 119.9(6) . . ?
Cl5 C60 Cl4 116.9(5) . . ?
Cl3 C61 Cl2 112.3(4) . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.093
####################################################################### 
# 
# 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_cj1130
_database_code_depnum_ccdc_archive 'CCDC 1401430'
_audit_update_record             
;
2015-05-18 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C47 H43 N P Si0.50'
_chemical_formula_weight         666.34

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'
Si Si 0.0817 0.0704 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   21.116(4)
_cell_length_b                   9.7250(19)
_cell_length_c                   18.206(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.81(3)
_cell_angle_gamma                90.00
_cell_volume                     3704.0(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1414
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9877
_exptl_absorpt_correction_T_max  0.9938
_exptl_absorpt_process_details   XDS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'Australian Synchrotron'
_diffrn_radiation_monochromator  ?
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            32355
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_av_sigmaI/netI    0.0386
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.92
_diffrn_reflns_theta_max         27.95
_reflns_number_total             8787
_reflns_number_gt                7484
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Blu-Ice (McPhillips, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CifTAB

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.
 The asymmetric unit was found to contain protonated ligand (LH) and the
 complex, LSiH3, in a 50:50 ratio, sitting on the same site.  This gave rise
 to disorder of the PPh2 and one CHPh fragment of one CHPh2 substituent over
 two sites in a 50:50 ratio. This disorder was modelled and all non-hydrogen
 atoms of both disordered sets refined anisotropically. The amine proton of
 the protonated ligand (LH) was not placed in a calculated position. It was,
 however, added to the empirical formula of the asymmetric unit as 0.5 H, and
 its contribution to F(000) was adjusted for the final refinement. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0443P)²+2.6226P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8787
_refine_ls_number_parameters     646
_refine_ls_number_restraints     101
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0594
_refine_ls_wR_factor_ref         0.1449
_refine_ls_wR_factor_gt          0.1395
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_restrained_S_all      1.161
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.2401(2) 0.4688(6) 0.1661(3) 0.0233(6) Uani 0.50 1 d PD A 1
Si1 Si 0.30230(5) 0.63312(11) 0.04711(6) 0.0264(2) Uani 0.50 1 d PD A 1
N1 N 0.26160(7) 0.62217(15) 0.12213(8) 0.0240(3) Uani 1 1 d . . .
C3 C 0.29707(8) 0.90830(19) 0.25866(10) 0.0257(4) Uani 1 1 d . A .
H3 H 0.3300 0.9351 0.2968 0.031 Uiso 1 1 calc R . .
C23 C 0.3618(5) 0.696(2) 0.2332(5) 0.025(2) Uani 0.50 1 d PD A 1
H23 H 0.3498 0.6011 0.2154 0.029 Uiso 0.50 1 calc PR A 1
C14 C 0.08122(8) 0.81715(19) 0.11174(9) 0.0239(3) Uani 1 1 d . . .
C20 C 0.23407(9) 1.1220(2) 0.28608(10) 0.0274(4) Uani 1 1 d . A .
H20 H 0.2209 1.1956 0.2487 0.033 Uiso 1 1 calc R . .
C7 C 0.14623(8) 0.78278(18) 0.08874(9) 0.0227(3) Uani 1 1 d . A .
H7 H 0.1484 0.6802 0.0865 0.027 Uiso 1 1 calc R . .
C6 C 0.20003(8) 0.82730(18) 0.14876(9) 0.0218(3) Uani 1 1 d . . .
C4 C 0.24324(8) 0.99104(18) 0.24360(9) 0.0231(3) Uani 1 1 d . . .
C2 C 0.30447(8) 0.78707(18) 0.21966(10) 0.0244(3) Uani 1 1 d . . .
C5 C 0.19538(8) 0.94766(18) 0.18815(9) 0.0233(3) Uani 1 1 d . A .
H5 H 0.1582 1.0028 0.1770 0.028 Uiso 1 1 calc R . .
C15 C 0.04608(8) 0.9326(2) 0.08774(10) 0.0284(4) Uani 1 1 d . . .
H15 H 0.0613 0.9931 0.0531 0.034 Uiso 1 1 calc R . .
C24 C 0.42124(8) 0.7430(2) 0.20013(11) 0.0304(4) Uani 1 1 d D . .
C29 C 0.43657(9) 0.8792(2) 0.18801(12) 0.0335(4) Uani 1 1 d . A .
H29 H 0.4089 0.9504 0.1999 0.040 Uiso 1 1 calc R . .
C1 C 0.25552(8) 0.74593(18) 0.16401(9) 0.0223(3) Uani 1 1 d . A .
C36A C 0.1743(3) 0.4047(6) 0.1107(3) 0.0261(16) Uani 0.50 1 d PD A 2
C9 C 0.18276(11) 0.9609(3) 0.00065(13) 0.0414(5) Uani 1 1 d . A .
H9 H 0.1949 1.0205 0.0415 0.050 Uiso 1 1 calc R . .
C30A C 0.3800(4) 0.7025(8) 0.3308(3) 0.0260(15) Uani 0.50 1 d PD A 2
C8 C 0.15560(8) 0.8340(2) 0.01198(10) 0.0284(4) Uani 1 1 d . . .
C28 C 0.49212(10) 0.9126(3) 0.15855(12) 0.0400(5) Uani 1 1 d . . .
H28 H 0.5024 1.0062 0.1510 0.048 Uiso 1 1 calc R A .
C16 C -0.01153(9) 0.9609(2) 0.11397(11) 0.0350(4) Uani 1 1 d . . .
H16 H -0.0352 1.0407 0.0974 0.042 Uiso 1 1 calc R . .
C25 C 0.46211(9) 0.6408(2) 0.18083(13) 0.0380(5) Uani 1 1 d . A .
H25 H 0.4521 0.5471 0.1884 0.046 Uiso 1 1 calc R . .
C31 C 0.4346(4) 0.7731(8) 0.3533(4) 0.0345(18) Uani 0.50 1 d PD A 1
H31 H 0.4567 0.8367 0.3264 0.041 Uiso 0.50 1 calc PR A 1
C17 C -0.03429(9) 0.8735(3) 0.16389(12) 0.0397(5) Uani 1 1 d . . .
H17 H -0.0735 0.8933 0.1818 0.048 Uiso 1 1 calc R . .
C19 C 0.05712(9) 0.7293(2) 0.16177(12) 0.0353(4) Uani 1 1 d . . .
H19 H 0.0804 0.6490 0.1783 0.042 Uiso 1 1 calc R . .
C42 C 0.29518(17) 0.3453(4) 0.1325(2) 0.0251(9) Uani 0.50 1 d PD A 1
C39 C 0.0443(3) 0.3221(7) 0.0471(4) 0.038(2) Uani 0.50 1 d PD A 1
H39 H 0.0038 0.2914 0.0238 0.046 Uiso 0.50 1 calc PR A 1
C13 C 0.13769(11) 0.7506(3) -0.04927(11) 0.0427(5) Uani 1 1 d . A .
H13 H 0.1181 0.6643 -0.0428 0.051 Uiso 1 1 calc R . .
C18 C -0.00016(10) 0.7574(3) 0.18777(13) 0.0450(6) Uani 1 1 d . . .
H18 H -0.0159 0.6968 0.2220 0.054 Uiso 1 1 calc R . .
C22 C 0.17950(11) 1.1042(3) 0.33254(15) 0.0471(6) Uani 1 1 d . . .
H22A H 0.1919 1.0368 0.3719 0.071 Uiso 1 1 calc R A .
H22B H 0.1412 1.0717 0.3008 0.071 Uiso 1 1 calc R . .
H22C H 0.1704 1.1925 0.3547 0.071 Uiso 1 1 calc R . .
C26 C 0.51700(10) 0.6735(3) 0.15084(14) 0.0461(5) Uani 1 1 d . . .
H26 H 0.5441 0.6024 0.1375 0.055 Uiso 1 1 calc R A .
C35 C 0.3549(2) 0.5991(5) 0.3561(3) 0.0360(12) Uani 0.50 1 d PD A 1
H35 H 0.3222 0.5425 0.3312 0.043 Uiso 0.50 1 calc PR A 1
C37 C 0.1212(4) 0.3495(6) 0.1561(3) 0.0281(14) Uani 0.50 1 d PD A 1
H37 H 0.1330 0.3365 0.2079 0.034 Uiso 0.50 1 calc PR A 1
C27 C 0.53231(10) 0.8093(3) 0.14026(14) 0.0455(5) Uani 1 1 d . A .
H27 H 0.5704 0.8319 0.1204 0.055 Uiso 1 1 calc R . .
C21 C 0.29362(10) 1.1721(3) 0.33446(14) 0.0459(6) Uani 1 1 d . . .
H21A H 0.3043 1.1088 0.3762 0.069 Uiso 1 1 calc R A .
H21B H 0.2859 1.2641 0.3534 0.069 Uiso 1 1 calc R . .
H21C H 0.3292 1.1759 0.3052 0.069 Uiso 1 1 calc R . .
C12 C 0.14805(13) 0.7917(4) -0.12011(12) 0.0588(8) Uani 1 1 d . . .
H12 H 0.1360 0.7329 -0.1613 0.071 Uiso 1 1 calc R A .
C41 C 0.14471(19) 0.4322(4) 0.0390(2) 0.0286(9) Uani 0.50 1 d PD A 1
H41 H 0.1727 0.4766 0.0098 0.034 Uiso 0.50 1 calc PR A 1
C11 C 0.17551(13) 0.9163(4) -0.13035(14) 0.0640(9) Uani 1 1 d . A .
H11 H 0.1830 0.9441 -0.1784 0.077 Uiso 1 1 calc R . .
C10 C 0.19217(13) 1.0012(3) -0.07036(15) 0.0598(8) Uani 1 1 d . . .
H10 H 0.2104 1.0886 -0.0776 0.072 Uiso 1 1 calc R A .
C32 C 0.4505(3) 0.7623(7) 0.4297(4) 0.045(2) Uani 0.50 1 d PD A 1
H32 H 0.4834 0.8186 0.4548 0.054 Uiso 0.50 1 calc PR A 1
C38 C 0.0619(4) 0.3033(6) 0.1227(4) 0.0409(18) Uani 0.50 1 d PD A 1
H38 H 0.0336 0.2591 0.1515 0.049 Uiso 0.50 1 calc PR A 1
C47 C 0.35190(14) 0.3201(3) 0.17911(18) 0.0250(7) Uani 0.50 1 d PD A 1
H47 H 0.3584 0.3601 0.2272 0.030 Uiso 0.50 1 calc PR A 1
C40 C 0.0865(2) 0.3861(5) 0.0063(3) 0.0355(12) Uani 0.50 1 d PD A 1
H40 H 0.0747 0.3983 -0.0456 0.043 Uiso 0.50 1 calc PR A 1
C46 C 0.39902(15) 0.2374(4) 0.1563(2) 0.0316(8) Uani 0.50 1 d PD A 1
H46 H 0.4373 0.2202 0.1888 0.038 Uiso 0.50 1 calc PR A 1
C45 C 0.39017(18) 0.1799(4) 0.0861(2) 0.0362(9) Uani 0.50 1 d PD A 1
H45 H 0.4227 0.1244 0.0701 0.043 Uiso 0.50 1 calc PR A 1
C43 C 0.28633(16) 0.2863(3) 0.06226(19) 0.0324(8) Uani 0.50 1 d PD A 1
H43 H 0.2478 0.3025 0.0299 0.039 Uiso 0.50 1 calc PR A 1
C44 C 0.33355(18) 0.2038(4) 0.0393(2) 0.0401(10) Uani 0.50 1 d PD A 1
H44 H 0.3272 0.1634 -0.0087 0.048 Uiso 0.50 1 calc PR A 1
C47A C 0.34817(17) 0.4279(4) 0.0637(2) 0.0362(9) Uani 0.50 1 d PD A 2
H47A H 0.3493 0.5250 0.0587 0.043 Uiso 0.50 1 calc PR A 2
C43A C 0.30483(17) 0.2250(4) 0.11324(18) 0.0337(8) Uani 0.50 1 d PD A 2
H43A H 0.2761 0.1826 0.1421 0.040 Uiso 0.50 1 calc PR A 2
C46A C 0.38887(19) 0.3468(4) 0.0286(2) 0.0483(11) Uani 0.50 1 d PD A 2
H46A H 0.4174 0.3884 -0.0009 0.058 Uiso 0.50 1 calc PR A 2
C44A C 0.3459(2) 0.1449(4) 0.0781(2) 0.0411(10) Uani 0.50 1 d PD A 2
H44A H 0.3450 0.0477 0.0829 0.049 Uiso 0.50 1 calc PR A 2
C45A C 0.3880(2) 0.2046(4) 0.0363(2) 0.0496(12) Uani 0.50 1 d PD A 2
H45A H 0.4164 0.1490 0.0129 0.060 Uiso 0.50 1 calc PR A 2
C42A C 0.30557(17) 0.3677(4) 0.1063(2) 0.0260(9) Uani 0.50 1 d PD A 2
C33 C 0.4188(2) 0.6700(6) 0.4691(2) 0.0531(16) Uani 0.50 1 d PD A 1
H33 H 0.4299 0.6622 0.5212 0.064 Uiso 0.50 1 calc PR A 1
C34 C 0.3708(2) 0.5888(5) 0.4324(2) 0.0486(13) Uani 0.50 1 d PD A 1
H34 H 0.3487 0.5257 0.4596 0.058 Uiso 0.50 1 calc PR A 1
C33A C 0.3975(2) 0.7197(5) 0.4854(2) 0.0411(10) Uani 0.50 1 d PD A 2
H33A H 0.4034 0.7255 0.5380 0.049 Uiso 0.50 1 calc PR A 2
C34A C 0.3464(2) 0.6451(5) 0.4485(2) 0.0426(10) Uani 0.50 1 d PD A 2
H34A H 0.3173 0.5999 0.4759 0.051 Uiso 0.50 1 calc PR A 2
C35A C 0.3382(2) 0.6371(5) 0.3720(2) 0.0350(11) Uani 0.50 1 d PD A 2
H35A H 0.3033 0.5859 0.3472 0.042 Uiso 0.50 1 calc PR A 2
C32A C 0.4392(3) 0.7849(6) 0.4449(4) 0.0374(16) Uani 0.50 1 d PD A 2
H32A H 0.4741 0.8359 0.4697 0.045 Uiso 0.50 1 calc PR A 2
C30 C 0.3867(4) 0.6917(8) 0.3160(3) 0.0259(14) Uani 0.50 1 d PD A 1
C31A C 0.4307(4) 0.7766(8) 0.3680(4) 0.0293(16) Uani 0.50 1 d PD A 2
H31A H 0.4598 0.8219 0.3407 0.035 Uiso 0.50 1 calc PR A 2
C41A C 0.1624(2) 0.3771(5) 0.0362(2) 0.0365(11) Uani 0.50 1 d PD A 2
H41A H 0.1957 0.3863 0.0063 0.044 Uiso 0.50 1 calc PR A 2
C40A C 0.1017(2) 0.3354(5) 0.0042(3) 0.0417(14) Uani 0.50 1 d PD A 2
H40A H 0.0935 0.3166 -0.0475 0.050 Uiso 0.50 1 calc PR A 2
C38A C 0.0650(4) 0.3488(7) 0.1230(4) 0.0431(18) Uani 0.50 1 d PD A 2
H38A H 0.0317 0.3389 0.1529 0.052 Uiso 0.50 1 calc PR A 2
C37A C 0.1256(4) 0.3906(6) 0.1547(3) 0.0323(16) Uani 0.50 1 d PD A 2
H37A H 0.1338 0.4094 0.2063 0.039 Uiso 0.50 1 calc PR A 2
C36 C 0.1635(3) 0.4141(6) 0.1156(3) 0.0249(17) Uani 0.50 1 d PD A 1
C39A C 0.0534(3) 0.3218(8) 0.0478(5) 0.046(3) Uani 0.50 1 d PD A 2
H39A H 0.0120 0.2937 0.0260 0.055 Uiso 0.50 1 calc PR A 2
P1A P 0.2528(2) 0.4688(7) 0.1580(3) 0.0255(7) Uani 0.50 1 d PD A 2
C23A C 0.3681(4) 0.7048(18) 0.2458(4) 0.0224(18) Uani 0.50 1 d PD A 2
H23A H 0.3573 0.6074 0.2316 0.027 Uiso 0.50 1 calc PR A 2
H1A H 0.2695(18) 0.578(4) -0.0184(13) 0.028(11) Uiso 0.50 1 d PD B 1
H1B H 0.311(2) 0.7755(11) 0.044(3) 0.042(13) Uiso 0.50 1 d PD C 1
H1C H 0.3598(14) 0.560(5) 0.062(3) 0.058(16) Uiso 0.50 1 d PD D 1


_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
P1 N1 1.780(6) . ?
P1 C36 1.826(5) . ?
P1 C42 1.833(5) . ?
Si1 N1 1.7131(18) . ?
N1 C1 1.440(2) . ?
N1 P1A 1.649(7) . ?
C3 C4 1.389(2) . ?
C3 C2 1.396(3) . ?
C23 C2 1.492(18) . ?
C23 C30 1.529(7) . ?
C23 C24 1.534(6) . ?
C14 C15 1.384(3) . ?
C14 C19 1.394(3) . ?
C14 C7 1.526(2) . ?
C20 C21 1.514(3) . ?
C20 C4 1.516(2) . ?
C20 C22 1.529(3) . ?
C7 C8 1.522(2) . ?
C7 C6 1.528(2) . ?
C6 C5 1.383(2) . ?
C6 C1 1.410(2) . ?
C4 C5 1.393(2) . ?
C2 C1 1.404(2) . ?
C2 C23A 1.580(15) . ?
C15 C16 1.393(3) . ?
C24 C29 1.389(3) . ?
C24 C25 1.392(3) . ?
C24 C23A 1.531(6) . ?
C29 C28 1.393(3) . ?
C36A C41A 1.371(5) . ?
C36A C37A 1.394(6) . ?
C36A P1A 1.869(5) . ?
C9 C8 1.388(3) . ?
C9 C10 1.390(3) . ?
C30A C35A 1.388(6) . ?
C30A C31A 1.389(6) . ?
C30A C23A 1.534(7) . ?
C8 C13 1.389(3) . ?
C28 C27 1.385(3) . ?
C16 C17 1.378(3) . ?
C25 C26 1.384(3) . ?
C31 C30 1.386(6) . ?
C31 C32 1.391(6) . ?
C17 C18 1.378(3) . ?
C19 C18 1.385(3) . ?
C42 C43 1.392(5) . ?
C42 C47 1.392(4) . ?
C39 C40 1.384(6) . ?
C39 C38 1.388(6) . ?
C13 C12 1.396(3) . ?
C26 C27 1.379(4) . ?
C35 C34 1.387(5) . ?
C35 C30 1.389(6) . ?
C37 C36 1.384(6) . ?
C37 C38 1.390(6) . ?
C12 C11 1.367(5) . ?
C41 C40 1.367(5) . ?
C41 C36 1.409(5) . ?
C11 C10 1.376(5) . ?
C32 C33 1.378(6) . ?
C47 C46 1.386(4) . ?
C46 C45 1.383(5) . ?
C45 C44 1.391(4) . ?
C43 C44 1.388(4) . ?
C47A C46A 1.386(5) . ?
C47A C42A 1.394(5) . ?
C43A C44A 1.386(5) . ?
C43A C42A 1.393(5) . ?
C46A C45A 1.390(5) . ?
C44A C45A 1.374(5) . ?
C42A P1A 1.837(5) . ?
C33 C34 1.383(5) . ?
C33A C32A 1.379(5) . ?
C33A C34A 1.394(5) . ?
C34A C35A 1.382(5) . ?
C32A C31A 1.388(6) . ?
C41A C40A 1.395(5) . ?
C40A C39A 1.381(6) . ?
C38A C39A 1.383(6) . ?
C38A C37A 1.390(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 P1 C36 106.3(4) . . ?
N1 P1 C42 100.8(2) . . ?
C36 P1 C42 101.5(4) . . ?
C1 N1 P1A 121.6(2) . . ?
C1 N1 Si1 117.43(12) . . ?
P1A N1 Si1 117.85(17) . . ?
C1 N1 P1 114.58(19) . . ?
P1A N1 P1 9.9(2) . . ?
Si1 N1 P1 126.62(17) . . ?
C4 C3 C2 122.27(16) . . ?
C2 C23 C30 110.0(10) . . ?
C2 C23 C24 116.6(11) . . ?
C30 C23 C24 101.8(5) . . ?
C15 C14 C19 118.40(17) . . ?
C15 C14 C7 123.71(16) . . ?
C19 C14 C7 117.85(16) . . ?
C21 C20 C4 114.41(16) . . ?
C21 C20 C22 110.09(18) . . ?
C4 C20 C22 110.16(16) . . ?
C8 C7 C14 114.49(14) . . ?
C8 C7 C6 112.77(14) . . ?
C14 C7 C6 110.54(14) . . ?
C5 C6 C1 119.24(15) . . ?
C5 C6 C7 120.82(15) . . ?
C1 C6 C7 119.94(15) . . ?
C3 C4 C5 117.46(16) . . ?
C3 C4 C20 122.94(16) . . ?
C5 C4 C20 119.57(15) . . ?
C3 C2 C1 119.05(16) . . ?
C3 C2 C23 124.1(6) . . ?
C1 C2 C23 116.8(6) . . ?
C3 C2 C23A 115.1(5) . . ?
C1 C2 C23A 125.8(5) . . ?
C23 C2 C23A 9.3(9) . . ?
C6 C5 C4 122.43(16) . . ?
C14 C15 C16 120.50(18) . . ?
C29 C24 C25 118.35(18) . . ?
C29 C24 C23A 121.4(7) . . ?
C25 C24 C23A 119.3(7) . . ?
C29 C24 C23 124.5(8) . . ?
C25 C24 C23 117.1(8) . . ?
C23A C24 C23 9.8(7) . . ?
C24 C29 C28 120.7(2) . . ?
C2 C1 C6 119.53(16) . . ?
C2 C1 N1 120.70(15) . . ?
C6 C1 N1 119.77(15) . . ?
C41A C36A C37A 120.0(4) . . ?
C41A C36A P1A 123.5(5) . . ?
C37A C36A P1A 116.5(5) . . ?
C8 C9 C10 120.2(2) . . ?
C35A C30A C31A 118.6(4) . . ?
C35A C30A C23A 121.5(6) . . ?
C31A C30A C23A 119.7(6) . . ?
C9 C8 C13 118.2(2) . . ?
C9 C8 C7 122.38(18) . . ?
C13 C8 C7 119.38(19) . . ?
C27 C28 C29 119.9(2) . . ?
C17 C16 C15 120.24(19) . . ?
C26 C25 C24 121.1(2) . . ?
C30 C31 C32 120.6(5) . . ?
C18 C17 C16 119.94(19) . . ?
C18 C19 C14 121.1(2) . . ?
C43 C42 C47 119.0(3) . . ?
C43 C42 P1 124.4(3) . . ?
C47 C42 P1 116.4(3) . . ?
C40 C39 C38 119.1(5) . . ?
C8 C13 C12 121.0(3) . . ?
C17 C18 C19 119.8(2) . . ?
C27 C26 C25 120.0(2) . . ?
C34 C35 C30 120.4(4) . . ?
C36 C37 C38 121.5(5) . . ?
C26 C27 C28 119.9(2) . . ?
C11 C12 C13 120.2(3) . . ?
C40 C41 C36 120.4(4) . . ?
C12 C11 C10 119.4(2) . . ?
C11 C10 C9 121.1(3) . . ?
C33 C32 C31 120.0(5) . . ?
C39 C38 C37 119.7(5) . . ?
C46 C47 C42 120.9(3) . . ?
C41 C40 C39 121.4(5) . . ?
C45 C46 C47 119.9(3) . . ?
C46 C45 C44 119.8(3) . . ?
C44 C43 C42 120.2(3) . . ?
C43 C44 C45 120.3(3) . . ?
C46A C47A C42A 120.4(3) . . ?
C44A C43A C42A 120.2(3) . . ?
C47A C46A C45A 120.1(3) . . ?
C45A C44A C43A 120.7(3) . . ?
C44A C45A C46A 119.7(3) . . ?
C43A C42A C47A 119.0(3) . . ?
C43A C42A P1A 118.2(4) . . ?
C47A C42A P1A 122.8(3) . . ?
C32 C33 C34 119.8(4) . . ?
C33 C34 C35 120.2(4) . . ?
C32A C33A C34A 119.4(4) . . ?
C35A C34A C33A 119.8(4) . . ?
C34A C35A C30A 121.2(4) . . ?
C33A C32A C31A 120.5(4) . . ?
C31 C30 C35 119.0(5) . . ?
C31 C30 C23 126.7(7) . . ?
C35 C30 C23 114.3(7) . . ?
C32A C31A C30A 120.5(5) . . ?
C36A C41A C40A 120.3(4) . . ?
C39A C40A C41A 119.7(4) . . ?
C39A C38A C37A 119.7(4) . . ?
C38A C37A C36A 119.9(4) . . ?
C37 C36 C41 117.9(4) . . ?
C37 C36 P1 117.1(5) . . ?
C41 C36 P1 125.0(5) . . ?
C40A C39A C38A 120.4(5) . . ?
N1 P1A C42A 100.0(3) . . ?
N1 P1A C36A 105.1(4) . . ?
C42A P1A C36A 98.5(4) . . ?
C24 C23A C30A 121.3(6) . . ?
C24 C23A C2 111.7(8) . . ?
C30A C23A C2 109.1(8) . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        27.95
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.050
####################################################################### 
# 
# 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_cj1081
_database_code_depnum_ccdc_archive 'CCDC 1401431'
_audit_update_record             
;
2015-05-18 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C47 H41 Cl5 N P Si2'
_chemical_formula_weight         884.21

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'
Si Si 0.0817 0.0704 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   10.1240(8)
_cell_length_b                   20.1891(15)
_cell_length_c                   21.6338(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.815(7)
_cell_angle_gamma                90.00
_cell_volume                     4416.5(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1832
_exptl_absorpt_coefficient_mu    0.453
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.954
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_process_details   'Sortav (Blessing)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex X8'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22407
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_sigmaI/netI    0.0711
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.97
_diffrn_reflns_theta_max         25.50
_reflns_number_total             8219
_reflns_number_gt                5642
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0595P)²+4.5852P] 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         8219
_refine_ls_number_parameters     507
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0577
_refine_ls_wR_factor_ref         0.1466
_refine_ls_wR_factor_gt          0.1276
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.47970(9) 0.70133(4) 0.39450(4) 0.0245(2) Uani 1 1 d . . .
N1 N 0.6511(3) 0.69355(13) 0.40998(13) 0.0228(6) Uani 1 1 d . . .
C19 C 1.0216(4) 0.78305(19) 0.46922(19) 0.0347(9) Uani 1 1 d . . .
H19 H 1.0332 0.7779 0.4262 0.042 Uiso 1 1 calc R . .
C6 C 0.7933(3) 0.78951(16) 0.38259(16) 0.0239(8) Uani 1 1 d . . .
C5 C 0.8598(3) 0.82183(17) 0.33667(17) 0.0254(8) Uani 1 1 d . . .
H5 H 0.8883 0.8661 0.3440 0.031 Uiso 1 1 calc R . .
C8 C 0.7625(3) 0.89829(17) 0.44289(16) 0.0263(8) Uani 1 1 d . . .
C42 C 0.4274(3) 0.64904(17) 0.32728(18) 0.0292(8) Uani 1 1 d . . .
C15 C 0.8904(4) 0.81569(18) 0.55242(18) 0.0359(9) Uani 1 1 d . . .
H15 H 0.8097 0.8319 0.5672 0.043 Uiso 1 1 calc R . .
C14 C 0.9020(4) 0.80655(16) 0.48909(17) 0.0270(8) Uani 1 1 d . . .
C9 C 0.6350(4) 0.92433(19) 0.44015(19) 0.0350(9) Uani 1 1 d . . .
H9 H 0.5612 0.8952 0.4387 0.042 Uiso 1 1 calc R . .
C7 C 0.7827(3) 0.82298(17) 0.44538(17) 0.0262(8) Uani 1 1 d . . .
H7 H 0.7031 0.8038 0.4644 0.031 Uiso 1 1 calc R . .
C46 C 0.3796(4) 0.5387(2) 0.2890(2) 0.0453(11) Uani 1 1 d . . .
H46 H 0.3869 0.4921 0.2941 0.054 Uiso 1 1 calc R . .
C47 C 0.4330(4) 0.58037(18) 0.3344(2) 0.0352(9) Uani 1 1 d . . .
H47 H 0.4740 0.5620 0.3709 0.042 Uiso 1 1 calc R . .
C27 C 0.8841(4) 0.58231(17) 0.35290(17) 0.0285(8) Uani 1 1 d . . .
C4 C 0.8867(3) 0.79275(17) 0.28078(16) 0.0251(8) Uani 1 1 d . . .
C3 C 0.8533(3) 0.72616(17) 0.27369(17) 0.0267(8) Uani 1 1 d . . .
H3 H 0.8765 0.7039 0.2371 0.032 Uiso 1 1 calc R . .
C22 C 0.6645(4) 0.60494(18) 0.20554(18) 0.0349(9) Uani 1 1 d . . .
H22 H 0.5913 0.6281 0.2208 0.042 Uiso 1 1 calc R . .
C17 C 1.1114(4) 0.7767(2) 0.5742(2) 0.0429(10) Uani 1 1 d . . .
H17 H 1.1824 0.7662 0.6029 0.051 Uiso 1 1 calc R . .
C11 C 0.7196(4) 1.03535(19) 0.44218(19) 0.0395(10) Uani 1 1 d . . .
H11 H 0.7048 1.0818 0.4424 0.047 Uiso 1 1 calc R . .
C2 C 0.7877(3) 0.69117(16) 0.31778(16) 0.0229(8) Uani 1 1 d . . .
C36 C 0.4521(3) 0.78422(16) 0.36308(17) 0.0242(8) Uani 1 1 d . . .
C20 C 0.7747(3) 0.61586(16) 0.31205(17) 0.0260(8) Uani 1 1 d . . .
H20 H 0.6879 0.6031 0.3288 0.031 Uiso 1 1 calc R . .
C33 C 0.9565(4) 0.82924(19) 0.23036(19) 0.0358(9) Uani 1 1 d . . .
H33 H 0.9182 0.8120 0.1900 0.043 Uiso 1 1 calc R . .
C21 C 0.7744(4) 0.59169(16) 0.24514(17) 0.0280(8) Uani 1 1 d . . .
C10 C 0.6141(4) 0.9920(2) 0.4395(2) 0.0428(10) Uani 1 1 d . . .
H10 H 0.5263 1.0088 0.4372 0.051 Uiso 1 1 calc R . .
C12 C 0.8454(4) 1.01083(18) 0.44444(18) 0.0344(9) Uani 1 1 d . . .
H12 H 0.9184 1.0404 0.4455 0.041 Uiso 1 1 calc R . .
C34 C 1.1033(5) 0.8107(3) 0.2332(2) 0.0708(17) Uani 1 1 d . . .
H34A H 1.1466 0.8318 0.1988 0.106 Uiso 1 1 calc R . .
H34B H 1.1123 0.7625 0.2302 0.106 Uiso 1 1 calc R . .
H34C H 1.1449 0.8260 0.2725 0.106 Uiso 1 1 calc R . .
C35 C 0.9307(7) 0.9024(2) 0.2305(3) 0.088(2) Uani 1 1 d . . .
H35A H 0.8354 0.9104 0.2313 0.132 Uiso 1 1 calc R . .
H35B H 0.9649 0.9223 0.1932 0.132 Uiso 1 1 calc R . .
H35C H 0.9752 0.9224 0.2673 0.132 Uiso 1 1 calc R . .
C26 C 0.8793(4) 0.55706(18) 0.22171(18) 0.0347(9) Uani 1 1 d . . .
H26 H 0.9550 0.5471 0.2478 0.042 Uiso 1 1 calc R . .
C23 C 0.6608(5) 0.58473(19) 0.1442(2) 0.0432(11) Uani 1 1 d . . .
H23 H 0.5857 0.5947 0.1178 0.052 Uiso 1 1 calc R . .
C1 C 0.7479(3) 0.72433(16) 0.37055(16) 0.0215(7) Uani 1 1 d . . .
C25 C 0.8738(5) 0.53674(19) 0.1598(2) 0.0442(11) Uani 1 1 d . . .
H25 H 0.9462 0.5132 0.1442 0.053 Uiso 1 1 calc R . .
C18 C 1.1247(4) 0.7669(2) 0.51135(19) 0.0389(10) Uani 1 1 d . . .
H18 H 1.2045 0.7491 0.4970 0.047 Uiso 1 1 calc R . .
C13 C 0.8672(4) 0.94298(17) 0.44517(17) 0.0305(9) Uani 1 1 d . . .
H13 H 0.9554 0.9267 0.4473 0.037 Uiso 1 1 calc R . .
C24 C 0.7652(5) 0.55036(19) 0.1212(2) 0.0472(12) Uani 1 1 d . . .
H24 H 0.7622 0.5363 0.0792 0.057 Uiso 1 1 calc R . .
Cl1 Cl 0.61564(9) 0.55439(4) 0.47659(5) 0.0365(2) Uani 1 1 d . . .
Cl2 Cl 0.86484(8) 0.64989(4) 0.50901(4) 0.0310(2) Uani 1 1 d . . .
Si1 Si 0.67265(9) 0.65214(5) 0.47906(5) 0.0253(2) Uani 1 1 d . . .
Si2 Si 0.54150(11) 0.69171(6) 0.55746(5) 0.0365(3) Uani 1 1 d . . .
Cl4 Cl 0.37322(11) 0.63705(6) 0.56559(6) 0.0581(4) Uani 1 1 d . . .
Cl5 Cl 0.48678(9) 0.78868(5) 0.54717(5) 0.0410(3) Uani 1 1 d . . .
Cl3 Cl 0.64464(13) 0.68534(9) 0.64053(6) 0.0788(5) Uani 1 1 d . . .
C37 C 0.3550(3) 0.82185(17) 0.38999(18) 0.0275(8) Uani 1 1 d . . .
H37 H 0.3129 0.8049 0.4249 0.033 Uiso 1 1 calc R . .
C28 C 0.8604(4) 0.51969(18) 0.37683(18) 0.0350(9) Uani 1 1 d . . .
H28 H 0.7774 0.4988 0.3683 0.042 Uiso 1 1 calc R . .
C39 C 0.3810(4) 0.90922(18) 0.31666(19) 0.0352(9) Uani 1 1 d . . .
H39 H 0.3578 0.9519 0.3012 0.042 Uiso 1 1 calc R . .
C30 C 1.0776(5) 0.5166(2) 0.4251(2) 0.0451(11) Uani 1 1 d . . .
H30 H 1.1433 0.4944 0.4502 0.054 Uiso 1 1 calc R . .
C16 C 0.9954(5) 0.8015(2) 0.59459(19) 0.0427(10) Uani 1 1 d . . .
H16 H 0.9863 0.8090 0.6375 0.051 Uiso 1 1 calc R . .
C40 C 0.4775(4) 0.87239(18) 0.28886(18) 0.0332(9) Uani 1 1 d . . .
H40 H 0.5196 0.8899 0.2541 0.040 Uiso 1 1 calc R . .
C29 C 0.9571(4) 0.4876(2) 0.41309(19) 0.0426(10) Uani 1 1 d . . .
H29 H 0.9396 0.4451 0.4297 0.051 Uiso 1 1 calc R . .
C31 C 1.1040(4) 0.5779(2) 0.4008(2) 0.0437(11) Uani 1 1 d . . .
H31 H 1.1884 0.5977 0.4086 0.052 Uiso 1 1 calc R . .
C38 C 0.3187(4) 0.88359(18) 0.36682(19) 0.0331(9) Uani 1 1 d . . .
H38 H 0.2512 0.9082 0.3854 0.040 Uiso 1 1 calc R . .
C41 C 0.5128(3) 0.81042(17) 0.31140(17) 0.0277(8) Uani 1 1 d . . .
H41 H 0.5784 0.7854 0.2918 0.033 Uiso 1 1 calc R . .
C32 C 1.0067(4) 0.61117(19) 0.36486(18) 0.0352(9) Uani 1 1 d . . .
H32 H 1.0248 0.6537 0.3485 0.042 Uiso 1 1 calc R . .
C45 C 0.3156(4) 0.5641(2) 0.2362(2) 0.0525(12) Uani 1 1 d . . .
H45 H 0.2789 0.5352 0.2052 0.063 Uiso 1 1 calc R . .
C43 C 0.3612(4) 0.6741(2) 0.2744(2) 0.0421(10) Uani 1 1 d . . .
H43 H 0.3535 0.7207 0.2688 0.051 Uiso 1 1 calc R . .
C44 C 0.3059(5) 0.6313(2) 0.2292(2) 0.0535(12) Uani 1 1 d . . .
H44 H 0.2611 0.6491 0.1934 0.064 Uiso 1 1 calc R . .


_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
P1 N1 1.758(3) . ?
P1 C36 1.823(3) . ?
P1 C42 1.853(4) . ?
N1 C1 1.468(4) . ?
N1 Si1 1.717(3) . ?
C19 C14 1.389(5) . ?
C19 C18 1.390(5) . ?
C6 C5 1.390(5) . ?
C6 C1 1.414(5) . ?
C6 C7 1.526(5) . ?
C5 C4 1.383(5) . ?
C8 C13 1.391(5) . ?
C8 C9 1.393(5) . ?
C8 C7 1.535(5) . ?
C42 C43 1.393(5) . ?
C42 C47 1.396(5) . ?
C15 C14 1.393(5) . ?
C15 C16 1.396(6) . ?
C14 C7 1.533(5) . ?
C9 C10 1.382(5) . ?
C46 C47 1.383(6) . ?
C46 C45 1.383(6) . ?
C27 C32 1.385(5) . ?
C27 C28 1.391(5) . ?
C27 C20 1.539(5) . ?
C4 C3 1.393(5) . ?
C4 C33 1.519(5) . ?
C3 C2 1.383(5) . ?
C22 C23 1.387(6) . ?
C22 C21 1.396(5) . ?
C17 C16 1.370(6) . ?
C17 C18 1.386(6) . ?
C11 C12 1.365(6) . ?
C11 C10 1.380(6) . ?
C2 C1 1.400(5) . ?
C2 C20 1.531(5) . ?
C36 C37 1.392(5) . ?
C36 C41 1.405(5) . ?
C20 C21 1.527(5) . ?
C33 C35 1.500(6) . ?
C33 C34 1.531(6) . ?
C21 C26 1.388(5) . ?
C12 C13 1.388(5) . ?
C26 C25 1.399(6) . ?
C23 C24 1.377(6) . ?
C25 C24 1.376(6) . ?
Cl1 Si1 2.0561(13) . ?
Cl2 Si1 2.0209(13) . ?
Si1 Si2 2.3452(15) . ?
Si2 Cl3 2.0375(17) . ?
Si2 Cl5 2.0438(15) . ?
Si2 Cl4 2.0446(16) . ?
C37 C38 1.386(5) . ?
C28 C29 1.386(5) . ?
C39 C38 1.382(6) . ?
C39 C40 1.388(5) . ?
C30 C29 1.366(6) . ?
C30 C31 1.377(6) . ?
C40 C41 1.383(5) . ?
C31 C32 1.396(5) . ?
C45 C44 1.368(6) . ?
C43 C44 1.400(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 P1 C36 106.57(14) . . ?
N1 P1 C42 109.88(15) . . ?
C36 P1 C42 101.40(17) . . ?
C1 N1 Si1 130.7(2) . . ?
C1 N1 P1 122.1(2) . . ?
Si1 N1 P1 106.92(15) . . ?
C14 C19 C18 121.0(4) . . ?
C5 C6 C1 118.0(3) . . ?
C5 C6 C7 119.1(3) . . ?
C1 C6 C7 122.7(3) . . ?
C4 C5 C6 123.3(3) . . ?
C13 C8 C9 117.4(3) . . ?
C13 C8 C7 122.8(3) . . ?
C9 C8 C7 119.8(3) . . ?
C43 C42 C47 117.8(3) . . ?
C43 C42 P1 123.0(3) . . ?
C47 C42 P1 118.1(3) . . ?
C14 C15 C16 121.2(4) . . ?
C19 C14 C15 117.8(4) . . ?
C19 C14 C7 123.8(3) . . ?
C15 C14 C7 118.4(3) . . ?
C10 C9 C8 121.0(4) . . ?
C6 C7 C14 111.4(3) . . ?
C6 C7 C8 115.0(3) . . ?
C14 C7 C8 109.6(3) . . ?
C47 C46 C45 120.9(4) . . ?
C46 C47 C42 120.9(4) . . ?
C32 C27 C28 118.8(3) . . ?
C32 C27 C20 122.4(3) . . ?
C28 C27 C20 118.8(3) . . ?
C5 C4 C3 116.7(3) . . ?
C5 C4 C33 122.7(3) . . ?
C3 C4 C33 120.5(3) . . ?
C2 C3 C4 122.6(3) . . ?
C23 C22 C21 120.9(4) . . ?
C16 C17 C18 119.6(4) . . ?
C12 C11 C10 119.4(4) . . ?
C3 C2 C1 119.1(3) . . ?
C3 C2 C20 119.6(3) . . ?
C1 C2 C20 120.9(3) . . ?
C37 C36 C41 118.2(3) . . ?
C37 C36 P1 116.3(3) . . ?
C41 C36 P1 125.2(3) . . ?
C21 C20 C2 113.0(3) . . ?
C21 C20 C27 111.8(3) . . ?
C2 C20 C27 109.5(3) . . ?
C35 C33 C4 112.9(3) . . ?
C35 C33 C34 114.1(4) . . ?
C4 C33 C34 109.7(3) . . ?
C26 C21 C22 118.3(4) . . ?
C26 C21 C20 122.7(3) . . ?
C22 C21 C20 119.0(3) . . ?
C11 C10 C9 120.6(4) . . ?
C11 C12 C13 120.4(4) . . ?
C21 C26 C25 120.1(4) . . ?
C24 C23 C22 120.6(4) . . ?
C2 C1 C6 119.4(3) . . ?
C2 C1 N1 119.9(3) . . ?
C6 C1 N1 120.5(3) . . ?
C24 C25 C26 121.1(4) . . ?
C17 C18 C19 120.3(4) . . ?
C12 C13 C8 121.3(3) . . ?
C25 C24 C23 119.0(4) . . ?
N1 Si1 Cl2 111.65(11) . . ?
N1 Si1 Cl1 114.92(11) . . ?
Cl2 Si1 Cl1 104.56(5) . . ?
N1 Si1 Si2 114.30(10) . . ?
Cl2 Si1 Si2 110.25(6) . . ?
Cl1 Si1 Si2 100.23(6) . . ?
Cl3 Si2 Cl5 106.32(8) . . ?
Cl3 Si2 Cl4 106.45(8) . . ?
Cl5 Si2 Cl4 107.69(6) . . ?
Cl3 Si2 Si1 109.42(6) . . ?
Cl5 Si2 Si1 114.06(6) . . ?
Cl4 Si2 Si1 112.46(7) . . ?
C38 C37 C36 121.3(3) . . ?
C29 C28 C27 120.4(4) . . ?
C38 C39 C40 119.8(3) . . ?
C29 C30 C31 120.1(4) . . ?
C17 C16 C15 120.1(4) . . ?
C41 C40 C39 120.5(4) . . ?
C30 C29 C28 120.5(4) . . ?
C30 C31 C32 120.0(4) . . ?
C39 C38 C37 119.8(3) . . ?
C40 C41 C36 120.3(3) . . ?
C27 C32 C31 120.2(4) . . ?
C44 C45 C46 119.1(4) . . ?
C42 C43 C44 120.5(4) . . ?
C45 C44 C43 120.8(4) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.049
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.074
####################################################################### 
# 
# 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_cj1149
_database_code_depnum_ccdc_archive 'CCDC 1401432'
_audit_update_record             
;
2015-05-18 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C47 H46 N P Si2'
_chemical_formula_weight         712.00

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'
Si Si 0.0817 0.0704 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   13.977(3)
_cell_length_b                   9.827(2)
_cell_length_c                   29.607(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.56(3)
_cell_angle_gamma                90.00
_cell_volume                     3969.3(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       rod
_exptl_crystal_colour            colorless'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1512
_exptl_absorpt_coefficient_mu    0.163
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.990
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_process_details   XDS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71090
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'Australian Synchrotron'
_diffrn_radiation_monochromator  ?
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            29006
_diffrn_reflns_av_R_equivalents  0.0775
_diffrn_reflns_av_sigmaI/netI    0.0592
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         2.96
_diffrn_reflns_theta_max         25.50
_reflns_number_total             7305
_reflns_number_gt                6637
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Blu-Ice (McPhillips, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CifTAB

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0600P)²+3.3140P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7305
_refine_ls_number_parameters     482
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0488
_refine_ls_wR_factor_ref         0.1310
_refine_ls_wR_factor_gt          0.1280
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.25885(3) 0.50243(4) 0.138692(16) 0.01446(13) Uani 1 1 d . . .
Si1 Si 0.09283(4) 0.68857(5) 0.080323(18) 0.01860(14) Uani 1 1 d D . .
Si2 Si -0.05528(4) 0.58830(7) 0.08677(2) 0.03080(16) Uani 1 1 d D . .
N1 N 0.20181(11) 0.65549(15) 0.12075(5) 0.0140(3) Uani 1 1 d . . .
C8 C 0.06131(13) 0.74679(18) 0.20375(6) 0.0148(4) Uani 1 1 d . . .
C36 C 0.15726(13) 0.38075(18) 0.12991(6) 0.0158(4) Uani 1 1 d . . .
C11 C -0.13808(14) 0.8076(2) 0.19456(7) 0.0227(4) Uani 1 1 d . . .
H11 H -0.2055 0.8285 0.1917 0.027 Uiso 1 1 calc R . .
C7 C 0.16937(13) 0.70881(17) 0.21346(6) 0.0144(3) Uani 1 1 d . . .
H7 H 0.1727 0.6160 0.2000 0.017 Uiso 1 1 calc R . .
C30 C 0.45156(13) 0.81990(18) 0.08345(6) 0.0165(4) Uani 1 1 d . . .
C19 C 0.17947(14) 0.77578(19) 0.29771(6) 0.0188(4) Uani 1 1 d . . .
H19 H 0.1279 0.8392 0.2878 0.023 Uiso 1 1 calc R . .
C6 C 0.23523(13) 0.80012(17) 0.19116(6) 0.0141(3) Uani 1 1 d . . .
C26 C 0.19865(14) 0.8899(2) -0.03914(6) 0.0217(4) Uani 1 1 d . . .
H26 H 0.1828 0.8436 -0.0680 0.026 Uiso 1 1 calc R . .
C3 C 0.36819(13) 0.95523(19) 0.15536(6) 0.0176(4) Uani 1 1 d . . .
H3 H 0.4134 1.0081 0.1431 0.021 Uiso 1 1 calc R . .
C42 C 0.32111(13) 0.44383(18) 0.09342(7) 0.0186(4) Uani 1 1 d . . .
C14 C 0.21148(13) 0.69512(18) 0.26524(6) 0.0159(4) Uani 1 1 d . . .
C39 C 0.01200(15) 0.1822(2) 0.12378(7) 0.0242(4) Uani 1 1 d . . .
H39 H -0.0367 0.1137 0.1218 0.029 Uiso 1 1 calc R . .
C15 C 0.28653(14) 0.6017(2) 0.28073(7) 0.0222(4) Uani 1 1 d . . .
H15 H 0.3090 0.5461 0.2589 0.027 Uiso 1 1 calc R . .
C9 C 0.02633(14) 0.87724(19) 0.19212(7) 0.0201(4) Uani 1 1 d . . .
H9 H 0.0703 0.9465 0.1871 0.024 Uiso 1 1 calc R . .
C2 C 0.31941(13) 0.84810(18) 0.12915(6) 0.0153(4) Uani 1 1 d . . .
C12 C -0.10380(15) 0.6764(2) 0.20567(7) 0.0247(4) Uani 1 1 d . . .
H12 H -0.1480 0.6069 0.2103 0.030 Uiso 1 1 calc R . .
C31 C 0.49344(14) 0.91816(19) 0.05976(6) 0.0190(4) Uani 1 1 d . . .
H31 H 0.4535 0.9873 0.0429 0.023 Uiso 1 1 calc R . .
C13 C -0.00543(14) 0.64653(19) 0.21005(7) 0.0195(4) Uani 1 1 d . . .
H13 H 0.0171 0.5563 0.2175 0.023 Uiso 1 1 calc R . .
C37 C 0.12566(14) 0.33757(18) 0.16927(6) 0.0184(4) Uani 1 1 d . . .
H37 H 0.1541 0.3764 0.1985 0.022 Uiso 1 1 calc R . .
C23 C 0.34197(13) 0.81345(18) 0.08245(6) 0.0158(4) Uani 1 1 d . . .
H23 H 0.3233 0.7157 0.0769 0.019 Uiso 1 1 calc R . .
C25 C 0.25682(14) 0.8269(2) -0.00104(6) 0.0192(4) Uani 1 1 d . . .
H25 H 0.2817 0.7383 -0.0043 0.023 Uiso 1 1 calc R . .
C38 C 0.05375(14) 0.23931(19) 0.16633(7) 0.0218(4) Uani 1 1 d . . .
H38 H 0.0330 0.2111 0.1934 0.026 Uiso 1 1 calc R . .
C29 C 0.24504(15) 1.0227(2) 0.04548(7) 0.0237(4) Uani 1 1 d . . .
H29 H 0.2603 1.0691 0.0743 0.028 Uiso 1 1 calc R . .
C18 C 0.22246(15) 0.7641(2) 0.34457(7) 0.0249(4) Uani 1 1 d . . .
H18 H 0.2010 0.8207 0.3664 0.030 Uiso 1 1 calc R . .
C32 C 0.59347(14) 0.9155(2) 0.06069(6) 0.0237(4) Uani 1 1 d . . .
H32 H 0.6211 0.9822 0.0441 0.028 Uiso 1 1 calc R . .
C1 C 0.25175(12) 0.77007(17) 0.14697(6) 0.0134(3) Uani 1 1 d . . .
C24 C 0.27955(13) 0.89120(19) 0.04203(6) 0.0158(4) Uani 1 1 d . . .
C5 C 0.28553(14) 0.90826(18) 0.21600(6) 0.0169(4) Uani 1 1 d . . .
H5 H 0.2737 0.9291 0.2456 0.020 Uiso 1 1 calc R . .
C20 C 0.41311(14) 1.09625(19) 0.22864(6) 0.0211(4) Uani 1 1 d . . .
H20 H 0.4530 1.1441 0.2092 0.025 Uiso 1 1 calc R . .
C40 C 0.04101(15) 0.2245(2) 0.08423(7) 0.0247(4) Uani 1 1 d . . .
H40 H 0.0116 0.1861 0.0551 0.030 Uiso 1 1 calc R . .
C28 C 0.18822(16) 1.0864(2) 0.00690(7) 0.0268(4) Uani 1 1 d . . .
H28 H 0.1659 1.1768 0.0095 0.032 Uiso 1 1 calc R . .
C34 C 0.61209(15) 0.7187(2) 0.10940(7) 0.0283(5) Uani 1 1 d . . .
H34 H 0.6525 0.6504 0.1266 0.034 Uiso 1 1 calc R . .
C35 C 0.51217(15) 0.7207(2) 0.10816(7) 0.0236(4) Uani 1 1 d . . .
H35 H 0.4847 0.6530 0.1245 0.028 Uiso 1 1 calc R . .
C43 C 0.29477(15) 0.4722(2) 0.04618(7) 0.0235(4) Uani 1 1 d . . .
H43 H 0.2390 0.5274 0.0346 0.028 Uiso 1 1 calc R . .
C10 C -0.07295(15) 0.90754(19) 0.18770(7) 0.0227(4) Uani 1 1 d . . .
H10 H -0.0959 0.9973 0.1799 0.027 Uiso 1 1 calc R . .
C4 C 0.35263(14) 0.98692(18) 0.19888(6) 0.0178(4) Uani 1 1 d . . .
C33 C 0.65275(14) 0.8167(2) 0.08548(7) 0.0257(4) Uani 1 1 d . . .
H33 H 0.7210 0.8158 0.0862 0.031 Uiso 1 1 calc R . .
C22 C 0.35006(17) 1.2016(2) 0.24575(9) 0.0349(5) Uani 1 1 d . . .
H22A H 0.3070 1.1563 0.2631 0.052 Uiso 1 1 calc R . .
H22B H 0.3103 1.2499 0.2193 0.052 Uiso 1 1 calc R . .
H22C H 0.3922 1.2667 0.2659 0.052 Uiso 1 1 calc R . .
C44 C 0.34902(18) 0.4208(2) 0.01582(8) 0.0344(5) Uani 1 1 d . . .
H44 H 0.3307 0.4415 -0.0162 0.041 Uiso 1 1 calc R . .
C47 C 0.40264(15) 0.3617(2) 0.10946(8) 0.0299(5) Uani 1 1 d . . .
H47 H 0.4218 0.3414 0.1415 0.036 Uiso 1 1 calc R . .
C17 C 0.29657(15) 0.6701(2) 0.35933(7) 0.0293(5) Uani 1 1 d . . .
H17 H 0.3253 0.6613 0.3914 0.035 Uiso 1 1 calc R . .
C27 C 0.16371(14) 1.0196(2) -0.03528(7) 0.0233(4) Uani 1 1 d . . .
H27 H 0.1232 1.0628 -0.0613 0.028 Uiso 1 1 calc R . .
C41 C 0.11342(14) 0.32342(19) 0.08725(7) 0.0209(4) Uani 1 1 d . . .
H41 H 0.1332 0.3522 0.0600 0.025 Uiso 1 1 calc R . .
C16 C 0.32881(15) 0.5886(2) 0.32733(7) 0.0285(5) Uani 1 1 d . . .
H16 H 0.3797 0.5242 0.3374 0.034 Uiso 1 1 calc R . .
C46 C 0.45630(18) 0.3090(3) 0.07901(10) 0.0418(6) Uani 1 1 d . . .
H46 H 0.5112 0.2521 0.0903 0.050 Uiso 1 1 calc R . .
C45 C 0.42971(18) 0.3395(3) 0.03242(10) 0.0428(6) Uani 1 1 d . . .
H45 H 0.4669 0.3045 0.0117 0.051 Uiso 1 1 calc R . .
C21 C 0.48379(16) 1.0326(2) 0.26996(9) 0.0351(5) Uani 1 1 d . . .
H21A H 0.5282 1.1028 0.2861 0.053 Uiso 1 1 calc R . .
H21B H 0.5221 0.9611 0.2590 0.053 Uiso 1 1 calc R . .
H21C H 0.4464 0.9931 0.2912 0.053 Uiso 1 1 calc R . .
H1A H 0.0775(19) 0.8273(9) 0.0808(9) 0.041(7) Uiso 1 1 d D . .
H1B H 0.1024(19) 0.651(3) 0.0365(4) 0.038(7) Uiso 1 1 d D . .
H2B H -0.049(2) 0.4836(16) 0.1190(6) 0.055(9) Uiso 1 1 d D . .
H2C H -0.1166(17) 0.6918(19) 0.0964(8) 0.063(9) Uiso 1 1 d D . .
H2A H -0.091(2) 0.539(2) 0.0420(4) 0.082(11) Uiso 1 1 d 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
P1 N1 1.7310(15) . ?
P1 C36 1.8312(18) . ?
P1 C42 1.8418(19) . ?
Si1 N1 1.7509(16) . ?
Si1 Si2 2.3377(9) . ?
N1 C1 1.457(2) . ?
C8 C9 1.388(3) . ?
C8 C13 1.397(3) . ?
C8 C7 1.521(2) . ?
C36 C41 1.397(3) . ?
C36 C37 1.399(3) . ?
C11 C10 1.384(3) . ?
C11 C12 1.391(3) . ?
C7 C14 1.524(2) . ?
C7 C6 1.534(2) . ?
C30 C35 1.391(3) . ?
C30 C31 1.395(3) . ?
C30 C23 1.527(2) . ?
C19 C18 1.392(3) . ?
C19 C14 1.393(3) . ?
C6 C5 1.393(2) . ?
C6 C1 1.408(2) . ?
C26 C27 1.379(3) . ?
C26 C25 1.385(3) . ?
C3 C4 1.388(3) . ?
C3 C2 1.395(3) . ?
C42 C47 1.393(3) . ?
C42 C43 1.395(3) . ?
C14 C15 1.394(3) . ?
C39 C40 1.384(3) . ?
C39 C38 1.387(3) . ?
C15 C16 1.384(3) . ?
C9 C10 1.397(3) . ?
C2 C1 1.406(2) . ?
C2 C23 1.522(2) . ?
C12 C13 1.384(3) . ?
C31 C32 1.393(3) . ?
C37 C38 1.383(3) . ?
C23 C24 1.524(3) . ?
C25 C24 1.397(3) . ?
C29 C28 1.390(3) . ?
C29 C24 1.391(3) . ?
C18 C17 1.386(3) . ?
C32 C33 1.379(3) . ?
C5 C4 1.393(3) . ?
C20 C22 1.517(3) . ?
C20 C4 1.524(2) . ?
C20 C21 1.529(3) . ?
C40 C41 1.392(3) . ?
C28 C27 1.386(3) . ?
C34 C33 1.388(3) . ?
C34 C35 1.389(3) . ?
C43 C44 1.391(3) . ?
C44 C45 1.382(4) . ?
C47 C46 1.392(3) . ?
C17 C16 1.388(3) . ?
C46 C45 1.381(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 P1 C36 103.45(8) . . ?
N1 P1 C42 107.89(8) . . ?
C36 P1 C42 99.61(8) . . ?
N1 Si1 Si2 121.35(6) . . ?
C1 N1 P1 111.88(11) . . ?
C1 N1 Si1 117.75(11) . . ?
P1 N1 Si1 130.19(9) . . ?
C9 C8 C13 118.36(17) . . ?
C9 C8 C7 123.71(16) . . ?
C13 C8 C7 117.78(16) . . ?
C41 C36 C37 118.37(17) . . ?
C41 C36 P1 124.46(14) . . ?
C37 C36 P1 117.08(14) . . ?
C10 C11 C12 119.28(18) . . ?
C8 C7 C14 111.23(14) . . ?
C8 C7 C6 116.05(14) . . ?
C14 C7 C6 110.36(14) . . ?
C35 C30 C31 118.40(17) . . ?
C35 C30 C23 118.35(16) . . ?
C31 C30 C23 123.22(17) . . ?
C18 C19 C14 120.49(18) . . ?
C5 C6 C1 118.99(16) . . ?
C5 C6 C7 120.03(15) . . ?
C1 C6 C7 120.80(15) . . ?
C27 C26 C25 120.11(18) . . ?
C4 C3 C2 121.97(16) . . ?
C47 C42 C43 118.39(18) . . ?
C47 C42 P1 114.46(16) . . ?
C43 C42 P1 127.14(15) . . ?
C19 C14 C15 118.64(17) . . ?
C19 C14 C7 122.17(16) . . ?
C15 C14 C7 119.17(16) . . ?
C40 C39 C38 120.27(18) . . ?
C16 C15 C14 121.11(19) . . ?
C8 C9 C10 120.60(17) . . ?
C3 C2 C1 119.36(16) . . ?
C3 C2 C23 120.10(15) . . ?
C1 C2 C23 120.51(16) . . ?
C13 C12 C11 120.19(18) . . ?
C32 C31 C30 120.41(18) . . ?
C12 C13 C8 121.11(17) . . ?
C38 C37 C36 121.07(18) . . ?
C2 C23 C24 113.88(15) . . ?
C2 C23 C30 112.22(15) . . ?
C24 C23 C30 113.26(14) . . ?
C26 C25 C24 121.20(18) . . ?
C37 C38 C39 119.78(18) . . ?
C28 C29 C24 120.22(18) . . ?
C17 C18 C19 120.02(19) . . ?
C33 C32 C31 120.54(18) . . ?
C2 C1 C6 119.57(16) . . ?
C2 C1 N1 120.33(15) . . ?
C6 C1 N1 120.05(15) . . ?
C29 C24 C25 118.29(17) . . ?
C29 C24 C23 123.82(16) . . ?
C25 C24 C23 117.89(16) . . ?
C6 C5 C4 122.26(16) . . ?
C22 C20 C4 112.65(17) . . ?
C22 C20 C21 109.47(17) . . ?
C4 C20 C21 110.79(16) . . ?
C39 C40 C41 119.87(19) . . ?
C27 C28 C29 120.81(19) . . ?
C33 C34 C35 119.82(19) . . ?
C34 C35 C30 121.17(18) . . ?
C44 C43 C42 120.9(2) . . ?
C11 C10 C9 120.45(18) . . ?
C3 C4 C5 117.84(17) . . ?
C3 C4 C20 121.05(16) . . ?
C5 C4 C20 120.91(16) . . ?
C32 C33 C34 119.64(18) . . ?
C45 C44 C43 119.8(2) . . ?
C46 C47 C42 120.7(2) . . ?
C18 C17 C16 120.03(19) . . ?
C26 C27 C28 119.33(19) . . ?
C40 C41 C36 120.63(18) . . ?
C15 C16 C17 119.69(19) . . ?
C45 C46 C47 120.0(2) . . ?
C46 C45 C44 120.1(2) . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.068
####################################################################### 
# 
# 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_cj1160
_database_code_depnum_ccdc_archive 'CCDC 1401433'
_audit_update_record             
;
2015-05-18 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C54 H49 Cl9 N P Si5'
_chemical_formula_weight         1202.41

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'
Si Si 0.0817 0.0704 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.470(2)
_cell_length_b                   16.168(3)
_cell_length_c                   18.415(4)
_cell_angle_alpha                108.85(3)
_cell_angle_beta                 90.82(3)
_cell_angle_gamma                99.88(3)
_cell_volume                     2898.3(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1236
_exptl_absorpt_coefficient_mu    0.603
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.914
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_process_details   XDS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71090
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'Australian Synchrotron'
_diffrn_radiation_monochromator  ?
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18549
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_sigmaI/netI    0.0675
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.94
_diffrn_reflns_theta_max         25.00
_reflns_number_total             9364
_reflns_number_gt                7007
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Blu-Ice (McPhillips, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CifTAB

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
 A molecule of toluene of crystallisation was located in the asymmetric unit.
 the carbon atoms of this were refined anisotropically.
 The low value (91.8%) for completeness of data to theta = 25.0 deg. arises 
 from hardware constraints associated with the diffractometer used at the 
 Australian Synchrotron and is common for triclinic data sets on that instrument. 
 Its minimum crystal to detector distance is 72 mm and its
 goniometer only rotates about the phi axis.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0706P)²+1.0669P] 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         9364
_refine_ls_number_parameters     634
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0478
_refine_ls_wR_factor_ref         0.1311
_refine_ls_wR_factor_gt          0.1205
_refine_ls_goodness_of_fit_ref   1.029
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl8 Cl -0.19178(9) -0.01122(6) 0.07764(5) 0.0300(2) Uani 1 1 d . . .
P1 P -0.25985(9) 0.07511(6) 0.29363(5) 0.0222(2) Uani 1 1 d . . .
Cl9 Cl 0.10815(9) -0.03983(7) 0.09233(5) 0.0338(2) Uani 1 1 d . . .
Si1 Si -0.00480(9) 0.09670(7) 0.27240(5) 0.0212(2) Uani 1 1 d . . .
Cl2 Cl 0.10726(9) 0.05896(6) 0.45557(5) 0.0305(2) Uani 1 1 d . . .
Si2 Si 0.04491(10) 0.00454(7) 0.34170(5) 0.0239(2) Uani 1 1 d . . .
Cl3 Cl 0.20021(10) -0.04206(7) 0.28407(5) 0.0346(2) Uani 1 1 d . . .
Si3 Si -0.10032(11) -0.13201(7) 0.30785(6) 0.0271(2) Uani 1 1 d . . .
Si5 Si -0.05335(10) -0.02268(7) 0.15228(5) 0.0246(2) Uani 1 1 d . . .
Cl4 Cl -0.27308(10) -0.13477(7) 0.35744(5) 0.0355(2) Uani 1 1 d . . .
Cl6 Cl -0.32343(10) -0.20323(7) 0.13884(6) 0.0399(3) Uani 1 1 d . . .
Si4 Si -0.13092(10) -0.15804(7) 0.17503(5) 0.0273(2) Uani 1 1 d . . .
Cl5 Cl -0.00985(11) -0.22458(7) 0.33090(5) 0.0368(2) Uani 1 1 d . . .
Cl7 Cl -0.02905(12) -0.25168(7) 0.11589(6) 0.0438(3) Uani 1 1 d . . .
N1 N -0.1262(3) 0.15750(19) 0.29846(15) 0.0203(6) Uani 1 1 d . . .
C4 C -0.1791(3) 0.3907(2) 0.38753(19) 0.0220(7) Uani 1 1 d . . .
H4 H -0.1846 0.4312 0.4375 0.026 Uiso 1 1 calc R . .
C12 C 0.0657(3) 0.3252(2) 0.45991(18) 0.0210(7) Uani 1 1 d . . .
C37 C -0.3255(3) 0.0956(2) 0.3885(2) 0.0236(8) Uani 1 1 d . . .
C11 C -0.0830(3) 0.2983(2) 0.45227(18) 0.0203(7) Uani 1 1 d . . .
H11 H -0.1024 0.2328 0.4427 0.024 Uiso 1 1 calc R . .
C17 C 0.1314(4) 0.3888(2) 0.43108(19) 0.0242(8) Uani 1 1 d . . .
H17 H 0.0835 0.4191 0.4072 0.029 Uiso 1 1 calc R . .
C3 C -0.1380(3) 0.3117(2) 0.38090(18) 0.0199(7) Uani 1 1 d . . .
C13 C 0.1387(4) 0.2827(2) 0.49535(19) 0.0256(8) Uani 1 1 d . . .
H13 H 0.0954 0.2396 0.5160 0.031 Uiso 1 1 calc R . .
C24 C -0.1142(4) 0.2250(2) 0.16182(18) 0.0228(7) Uani 1 1 d . . .
H24 H -0.1281 0.1605 0.1569 0.027 Uiso 1 1 calc R . .
C1 C -0.1352(3) 0.2497(2) 0.30677(19) 0.0194(7) Uani 1 1 d . . .
C32 C 0.0855(4) 0.2031(3) 0.0886(2) 0.0293(8) Uani 1 1 d . . .
H32 H 0.0348 0.1502 0.0540 0.035 Uiso 1 1 calc R . .
C38 C -0.2461(4) 0.0957(2) 0.4505(2) 0.0263(8) Uani 1 1 d . . .
H38 H -0.1583 0.0890 0.4433 0.032 Uiso 1 1 calc R . .
C18 C -0.1489(3) 0.3407(2) 0.52476(18) 0.0200(7) Uani 1 1 d . . .
C19 C -0.0790(4) 0.3966(2) 0.5929(2) 0.0250(8) Uani 1 1 d . . .
H19 H 0.0129 0.4121 0.5942 0.030 Uiso 1 1 calc R . .
C7 C -0.1509(3) 0.2760(2) 0.24212(18) 0.0210(7) Uani 1 1 d . . .
C31 C 0.0295(4) 0.2543(2) 0.15217(19) 0.0231(8) Uani 1 1 d . . .
C25 C -0.1996(4) 0.2336(2) 0.09764(19) 0.0250(8) Uani 1 1 d . . .
C22 C -0.3466(4) 0.3521(3) 0.5904(2) 0.0279(8) Uani 1 1 d . . .
H22 H -0.4386 0.3371 0.5893 0.034 Uiso 1 1 calc R . .
C6 C -0.1908(3) 0.3563(2) 0.25194(19) 0.0225(7) Uani 1 1 d . . .
H6 H -0.2036 0.3732 0.2079 0.027 Uiso 1 1 calc R . .
C44 C -0.4344(4) 0.1728(3) 0.2555(2) 0.0257(8) Uani 1 1 d . . .
H44 H -0.3916 0.2229 0.2967 0.031 Uiso 1 1 calc R . .
C20 C -0.1422(4) 0.4300(3) 0.6592(2) 0.0289(8) Uani 1 1 d . . .
H20 H -0.0933 0.4683 0.7052 0.035 Uiso 1 1 calc R . .
C5 C -0.2128(3) 0.4130(2) 0.32371(19) 0.0221(7) Uani 1 1 d . . .
C36 C 0.1071(4) 0.3304(2) 0.2023(2) 0.0274(8) Uani 1 1 d . . .
H36 H 0.0713 0.3659 0.2460 0.033 Uiso 1 1 calc R . .
C8 C -0.2741(4) 0.4934(2) 0.3329(2) 0.0273(8) Uani 1 1 d . . .
H8 H -0.2447 0.5371 0.3852 0.033 Uiso 1 1 calc R . .
C14 C 0.2737(4) 0.3022(3) 0.5010(2) 0.0290(8) Uani 1 1 d . . .
H14 H 0.3221 0.2729 0.5258 0.035 Uiso 1 1 calc R . .
C48 C -0.4581(4) 0.0181(3) 0.1786(2) 0.0294(8) Uani 1 1 d . . .
H48 H -0.4311 -0.0376 0.1668 0.035 Uiso 1 1 calc R . .
C40 C -0.4234(4) 0.1107(3) 0.5321(2) 0.0332(9) Uani 1 1 d . . .
H40 H -0.4567 0.1167 0.5809 0.040 Uiso 1 1 calc R . .
C42 C -0.4558(4) 0.0994(3) 0.3995(2) 0.0278(8) Uani 1 1 d . . .
H42 H -0.5125 0.0966 0.3577 0.033 Uiso 1 1 calc R . .
C43 C -0.3913(3) 0.0922(2) 0.2382(2) 0.0250(8) Uani 1 1 d . . .
C41 C -0.5040(4) 0.1070(3) 0.4705(2) 0.0318(9) Uani 1 1 d . . .
H41 H -0.5932 0.1098 0.4770 0.038 Uiso 1 1 calc R . .
C45 C -0.5384(4) 0.1804(3) 0.2132(2) 0.0282(8) Uani 1 1 d . . .
H45 H -0.5664 0.2358 0.2248 0.034 Uiso 1 1 calc R . .
C15 C 0.3375(4) 0.3641(3) 0.4706(2) 0.0314(9) Uani 1 1 d . . .
H15 H 0.4298 0.3762 0.4730 0.038 Uiso 1 1 calc R . .
C35 C 0.2360(4) 0.3553(3) 0.1895(2) 0.0303(8) Uani 1 1 d . . .
H35 H 0.2877 0.4073 0.2247 0.036 Uiso 1 1 calc R . .
C10 C -0.2373(5) 0.5405(3) 0.2744(2) 0.0395(10) Uani 1 1 d . . .
H10A H -0.1425 0.5561 0.2758 0.059 Uiso 1 1 calc R . .
H10B H -0.2744 0.5947 0.2871 0.059 Uiso 1 1 calc R . .
H10C H -0.2715 0.5009 0.2228 0.059 Uiso 1 1 calc R . .
C47 C -0.5637(4) 0.0265(3) 0.1372(2) 0.0324(9) Uani 1 1 d . . .
H47 H -0.6095 -0.0237 0.0971 0.039 Uiso 1 1 calc R . .
C46 C -0.6025(4) 0.1073(3) 0.1536(2) 0.0323(9) Uani 1 1 d . . .
H46 H -0.6736 0.1130 0.1241 0.039 Uiso 1 1 calc R . .
C39 C -0.2935(4) 0.1056(2) 0.5220(2) 0.0287(8) Uani 1 1 d . . .
H39 H -0.2372 0.1088 0.5641 0.034 Uiso 1 1 calc R . .
C21 C -0.2752(4) 0.4076(3) 0.6583(2) 0.0299(8) Uani 1 1 d . . .
H21 H -0.3182 0.4299 0.7037 0.036 Uiso 1 1 calc R . .
C23 C -0.2835(4) 0.3187(2) 0.5245(2) 0.0250(8) Uani 1 1 d . . .
H23 H -0.3327 0.2804 0.4786 0.030 Uiso 1 1 calc R . .
C30 C -0.1613(4) 0.2970(3) 0.0622(2) 0.0350(9) Uani 1 1 d . . .
H30 H -0.0774 0.3335 0.0755 0.042 Uiso 1 1 calc R . .
C27 C -0.4047(4) 0.1905(3) 0.0215(2) 0.0376(10) Uani 1 1 d . . .
H27 H -0.4884 0.1538 0.0075 0.045 Uiso 1 1 calc R . .
C16 C 0.2671(4) 0.4084(3) 0.4369(2) 0.0285(8) Uani 1 1 d . . .
H16 H 0.3110 0.4524 0.4175 0.034 Uiso 1 1 calc R . .
C33 C 0.2135(4) 0.2286(3) 0.0755(2) 0.0332(9) Uani 1 1 d . . .
H33 H 0.2494 0.1934 0.0316 0.040 Uiso 1 1 calc R . .
C28 C -0.3655(4) 0.2546(3) -0.0126(2) 0.0432(11) Uani 1 1 d . . .
H28 H -0.4222 0.2620 -0.0498 0.052 Uiso 1 1 calc R . .
C26 C -0.3222(4) 0.1796(3) 0.0760(2) 0.0296(8) Uani 1 1 d . . .
H26 H -0.3495 0.1351 0.0987 0.035 Uiso 1 1 calc R . .
C34 C 0.2902(4) 0.3049(3) 0.1257(2) 0.0328(9) Uani 1 1 d . . .
H34 H 0.3782 0.3224 0.1166 0.039 Uiso 1 1 calc R . .
C9 C -0.4222(4) 0.4654(3) 0.3298(3) 0.0470(11) Uani 1 1 d . . .
H9A H -0.4537 0.4219 0.2792 0.070 Uiso 1 1 calc R . .
H9B H -0.4628 0.5177 0.3384 0.070 Uiso 1 1 calc R . .
H9C H -0.4446 0.4387 0.3699 0.070 Uiso 1 1 calc R . .
C29 C -0.2437(4) 0.3076(3) 0.0078(2) 0.0429(11) Uani 1 1 d . . .
H29 H -0.2164 0.3515 -0.0156 0.052 Uiso 1 1 calc R . .
Cl1 Cl 0.16745(8) 0.18038(6) 0.27979(5) 0.0259(2) Uani 1 1 d . . .
C49 C -0.2946(7) 0.3606(5) 0.8316(3) 0.0724(17) Uani 1 1 d . . .
C55 C -0.3463(9) 0.2699(5) 0.7730(4) 0.098(3) Uani 1 1 d . . .
H55A H -0.2948 0.2610 0.7280 0.147 Uiso 1 1 calc R . .
H55B H -0.4374 0.2663 0.7572 0.147 Uiso 1 1 calc R . .
H55C H -0.3400 0.2237 0.7960 0.147 Uiso 1 1 calc R . .
C50 C -0.1672(7) 0.3926(5) 0.8421(4) 0.0796(19) Uani 1 1 d . . .
H50 H -0.1119 0.3576 0.8106 0.095 Uiso 1 1 calc R . .
C54 C -0.3789(9) 0.4097(5) 0.8735(4) 0.086(2) Uani 1 1 d . . .
H54 H -0.4700 0.3885 0.8648 0.103 Uiso 1 1 calc R . .
C52 C -0.1903(11) 0.5234(5) 0.9427(5) 0.098(3) Uani 1 1 d . . .
H52 H -0.1546 0.5772 0.9825 0.117 Uiso 1 1 calc R . .
C51 C -0.1095(9) 0.4734(5) 0.8958(4) 0.085(2) Uani 1 1 d . . .
H51 H -0.0181 0.4936 0.9003 0.102 Uiso 1 1 calc R . .
C53 C -0.3277(12) 0.4933(6) 0.9306(5) 0.113(3) Uani 1 1 d . . .
H53 H -0.3845 0.5285 0.9603 0.135 Uiso 1 1 calc R . .


_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
Cl8 Si5 2.0550(15) . ?
P1 N1 1.738(3) . ?
P1 C43 1.812(4) . ?
P1 C37 1.836(4) . ?
P1 Si1 2.6841(15) . ?
Cl9 Si5 2.0425(15) . ?
Si1 N1 1.719(3) . ?
Si1 Cl1 2.0342(15) . ?
Si1 Si2 2.3655(15) . ?
Si1 Si5 2.3978(16) . ?
Cl2 Si2 2.0418(14) . ?
Si2 Cl3 2.0714(15) . ?
Si2 Si3 2.3466(17) . ?
Si3 Cl4 2.0381(16) . ?
Si3 Cl5 2.0502(16) . ?
Si3 Si4 2.3512(15) . ?
Si5 Si4 2.3701(16) . ?
Cl6 Si4 2.0450(16) . ?
Si4 Cl7 2.0342(17) . ?
N1 C1 1.468(5) . ?
C4 C3 1.386(5) . ?
C4 C5 1.393(5) . ?
C12 C17 1.390(5) . ?
C12 C13 1.392(5) . ?
C12 C11 1.534(5) . ?
C37 C42 1.391(5) . ?
C37 C38 1.402(5) . ?
C11 C3 1.520(5) . ?
C11 C18 1.525(5) . ?
C17 C16 1.396(5) . ?
C3 C1 1.414(5) . ?
C13 C14 1.390(5) . ?
C24 C25 1.528(5) . ?
C24 C31 1.529(5) . ?
C24 C7 1.534(5) . ?
C1 C7 1.404(5) . ?
C32 C33 1.381(6) . ?
C32 C31 1.400(5) . ?
C38 C39 1.385(5) . ?
C18 C23 1.393(5) . ?
C18 C19 1.393(5) . ?
C19 C20 1.393(5) . ?
C7 C6 1.389(5) . ?
C31 C36 1.388(5) . ?
C25 C30 1.392(6) . ?
C25 C26 1.395(5) . ?
C22 C23 1.387(5) . ?
C22 C21 1.396(5) . ?
C6 C5 1.393(5) . ?
C44 C45 1.375(5) . ?
C44 C43 1.394(5) . ?
C20 C21 1.376(6) . ?
C5 C8 1.509(5) . ?
C36 C35 1.387(5) . ?
C8 C10 1.526(6) . ?
C8 C9 1.533(6) . ?
C14 C15 1.380(6) . ?
C48 C47 1.384(6) . ?
C48 C43 1.402(5) . ?
C40 C41 1.384(6) . ?
C40 C39 1.389(6) . ?
C42 C41 1.384(5) . ?
C45 C46 1.385(5) . ?
C15 C16 1.378(6) . ?
C35 C34 1.386(6) . ?
C47 C46 1.375(6) . ?
C30 C29 1.383(6) . ?
C27 C28 1.384(6) . ?
C27 C26 1.388(6) . ?
C33 C34 1.388(6) . ?
C28 C29 1.380(6) . ?
C49 C50 1.333(9) . ?
C49 C54 1.366(9) . ?
C49 C55 1.515(10) . ?
C50 C51 1.389(10) . ?
C54 C53 1.427(12) . ?
C52 C51 1.384(12) . ?
C52 C53 1.427(13) . ?

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 P1 C43 107.51(16) . . ?
N1 P1 C37 109.84(15) . . ?
C43 P1 C37 101.39(17) . . ?
N1 P1 Si1 38.80(10) . . ?
C43 P1 Si1 128.72(12) . . ?
C37 P1 Si1 123.77(12) . . ?
N1 Si1 Cl1 109.53(11) . . ?
N1 Si1 Si2 120.79(11) . . ?
Cl1 Si1 Si2 103.09(6) . . ?
N1 Si1 Si5 114.11(11) . . ?
Cl1 Si1 Si5 114.26(6) . . ?
Si2 Si1 Si5 94.17(5) . . ?
N1 Si1 P1 39.32(10) . . ?
Cl1 Si1 P1 148.75(6) . . ?
Si2 Si1 P1 95.82(5) . . ?
Si5 Si1 P1 88.54(6) . . ?
Cl2 Si2 Cl3 106.70(6) . . ?
Cl2 Si2 Si3 115.22(7) . . ?
Cl3 Si2 Si3 97.63(6) . . ?
Cl2 Si2 Si1 119.96(6) . . ?
Cl3 Si2 Si1 100.29(6) . . ?
Si3 Si2 Si1 112.83(6) . . ?
Cl4 Si3 Cl5 107.69(7) . . ?
Cl4 Si3 Si2 117.78(7) . . ?
Cl5 Si3 Si2 109.26(6) . . ?
Cl4 Si3 Si4 111.28(6) . . ?
Cl5 Si3 Si4 112.12(6) . . ?
Si2 Si3 Si4 98.60(6) . . ?
Cl9 Si5 Cl8 105.96(6) . . ?
Cl9 Si5 Si4 106.80(6) . . ?
Cl8 Si5 Si4 105.81(6) . . ?
Cl9 Si5 Si1 111.72(6) . . ?
Cl8 Si5 Si1 116.19(6) . . ?
Si4 Si5 Si1 109.80(6) . . ?
Cl7 Si4 Cl6 108.39(7) . . ?
Cl7 Si4 Si3 110.08(7) . . ?
Cl6 Si4 Si3 110.14(7) . . ?
Cl7 Si4 Si5 109.33(7) . . ?
Cl6 Si4 Si5 110.92(7) . . ?
Si3 Si4 Si5 107.99(6) . . ?
C1 N1 Si1 133.1(2) . . ?
C1 N1 P1 123.8(2) . . ?
Si1 N1 P1 101.88(16) . . ?
C3 C4 C5 122.5(3) . . ?
C17 C12 C13 118.3(3) . . ?
C17 C12 C11 122.8(3) . . ?
C13 C12 C11 118.9(3) . . ?
C42 C37 C38 118.0(3) . . ?
C42 C37 P1 122.6(3) . . ?
C38 C37 P1 118.9(3) . . ?
C3 C11 C18 113.4(3) . . ?
C3 C11 C12 110.0(3) . . ?
C18 C11 C12 114.4(3) . . ?
C12 C17 C16 120.6(3) . . ?
C4 C3 C1 118.9(3) . . ?
C4 C3 C11 119.4(3) . . ?
C1 C3 C11 121.3(3) . . ?
C14 C13 C12 121.1(4) . . ?
C25 C24 C31 110.6(3) . . ?
C25 C24 C7 112.4(3) . . ?
C31 C24 C7 111.1(3) . . ?
C7 C1 C3 119.0(3) . . ?
C7 C1 N1 121.2(3) . . ?
C3 C1 N1 119.7(3) . . ?
C33 C32 C31 120.9(4) . . ?
C39 C38 C37 121.1(4) . . ?
C23 C18 C19 118.5(3) . . ?
C23 C18 C11 118.9(3) . . ?
C19 C18 C11 122.5(3) . . ?
C20 C19 C18 120.8(3) . . ?
C6 C7 C1 118.8(3) . . ?
C6 C7 C24 117.6(3) . . ?
C1 C7 C24 123.3(3) . . ?
C36 C31 C32 118.0(3) . . ?
C36 C31 C24 123.4(3) . . ?
C32 C31 C24 118.5(3) . . ?
C30 C25 C26 118.5(3) . . ?
C30 C25 C24 121.9(3) . . ?
C26 C25 C24 119.6(3) . . ?
C23 C22 C21 120.1(4) . . ?
C7 C6 C5 122.7(3) . . ?
C45 C44 C43 120.4(3) . . ?
C21 C20 C19 120.2(3) . . ?
C4 C5 C6 116.8(3) . . ?
C4 C5 C8 120.9(3) . . ?
C6 C5 C8 122.3(3) . . ?
C35 C36 C31 121.0(3) . . ?
C5 C8 C10 114.6(3) . . ?
C5 C8 C9 108.8(3) . . ?
C10 C8 C9 110.4(3) . . ?
C15 C14 C13 119.8(3) . . ?
C47 C48 C43 119.8(4) . . ?
C41 C40 C39 119.5(4) . . ?
C41 C42 C37 120.9(4) . . ?
C44 C43 C48 119.1(3) . . ?
C44 C43 P1 123.3(3) . . ?
C48 C43 P1 117.5(3) . . ?
C40 C41 C42 120.5(4) . . ?
C44 C45 C46 120.1(4) . . ?
C16 C15 C14 119.9(4) . . ?
C36 C35 C34 120.6(4) . . ?
C46 C47 C48 120.3(4) . . ?
C47 C46 C45 120.3(4) . . ?
C38 C39 C40 119.9(4) . . ?
C20 C21 C22 119.6(3) . . ?
C22 C23 C18 120.7(3) . . ?
C29 C30 C25 120.9(4) . . ?
C28 C27 C26 120.3(4) . . ?
C15 C16 C17 120.2(4) . . ?
C32 C33 C34 120.7(4) . . ?
C29 C28 C27 119.7(4) . . ?
C27 C26 C25 120.4(4) . . ?
C35 C34 C33 118.8(4) . . ?
C28 C29 C30 120.2(4) . . ?
C50 C49 C54 120.0(8) . . ?
C50 C49 C55 120.0(7) . . ?
C54 C49 C55 119.9(7) . . ?
C49 C50 C51 124.7(8) . . ?
C49 C54 C53 118.9(8) . . ?
C51 C52 C53 119.4(8) . . ?
C52 C51 C50 117.5(8) . . ?
C54 C53 C52 119.4(8) . . ?

_diffrn_measured_fraction_theta_max 0.918
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.918
_refine_diff_density_max         0.809
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.075
####################################################################### 
# 
# 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_cj1162
_database_code_depnum_ccdc_archive 'CCDC 1401434'
_audit_update_record             
;
2015-05-18 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C101 H90 Cl8 N2 P2 Si5'
_chemical_formula_weight         1817.74

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'
Si Si 0.0817 0.0704 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   17.441(4)
_cell_length_b                   23.780(5)
_cell_length_c                   23.866(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.20(3)
_cell_angle_gamma                90.00
_cell_volume                     9883(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       colourless
_exptl_crystal_colour            plate
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3784
_exptl_absorpt_coefficient_mu    0.366
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.963
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_process_details   XDS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71090
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'Australian Synchrotron'
_diffrn_radiation_monochromator  ?
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            39379
_diffrn_reflns_av_R_equivalents  0.1434
_diffrn_reflns_av_sigmaI/netI    0.1102
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.93
_diffrn_reflns_theta_max         20.96
_reflns_number_total             10481
_reflns_number_gt                5890
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Blu-Ice (McPhillips, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CifTAB

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
 Two molecules of toluene of crystallisation in the asymmteric unit were
 refined with their atomic positions set at 50% occupancy and their
 carbon atoms set as isotropic.
 The methyl and methine groups of one isopropyl substituent were found
 to be disordered over two sites. This disorder was modelled and the carbon
 atoms of the major disordered set refined anisotropically, while those of
 the minor set were refined isotropically.
 The low value of theta max for the diffraction data (20.96 deg.) and
 associated Level A cifcheck alert, arose from the data above that angle
 being to weak to observe. Hence, the software used to integrate the diffraction
 data at the Australian Synchrotron discarded these data.
 This resulted in the poor quality of the crystal structure. Although the
 metrical parameters for the compound should not be considered as
 accurate, the gross molecular connectivity of the compound is unambiguous.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1330P)²+52.7850P] 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         10481
_refine_ls_number_parameters     1072
_refine_ls_number_restraints     63
_refine_ls_R_factor_all          0.1680
_refine_ls_R_factor_gt           0.1007
_refine_ls_wR_factor_ref         0.3063
_refine_ls_wR_factor_gt          0.2647
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.054
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl5 Cl 0.43641(17) 0.12570(16) 0.44067(13) 0.0689(10) Uani 1 1 d . . .
Cl1 Cl 0.15824(18) 0.25185(15) 0.28583(13) 0.0668(9) Uani 1 1 d . . .
Cl4 Cl 0.52866(17) 0.25733(16) 0.39679(13) 0.0700(10) Uani 1 1 d . . .
Cl6 Cl 0.45507(17) 0.07028(15) 0.31659(13) 0.0658(9) Uani 1 1 d . . .
P2 P 0.43717(17) 0.20175(15) 0.22283(13) 0.0541(9) Uani 1 1 d . . .
Cl2 Cl 0.31946(18) 0.33174(15) 0.27098(13) 0.0687(10) Uani 1 1 d . . .
Cl7 Cl 0.23081(18) 0.07395(15) 0.38489(14) 0.0693(10) Uani 1 1 d . . .
Cl3 Cl 0.36380(18) 0.33812(16) 0.40612(13) 0.0730(10) Uani 1 1 d . . .
Cl8 Cl 0.25548(18) 0.11365(17) 0.25633(13) 0.0730(11) Uani 1 1 d . . .
P1 P 0.24958(17) 0.21043(15) 0.46353(13) 0.0555(9) Uani 1 1 d . . .
Si1 Si 0.22908(18) 0.22873(16) 0.35276(14) 0.0548(9) Uani 1 1 d . . .
Si5 Si 0.27654(18) 0.13735(16) 0.33879(14) 0.0567(10) Uani 1 1 d . . .
Si3 Si 0.45676(18) 0.22844(17) 0.33257(13) 0.0572(10) Uani 1 1 d . . .
Si2 Si 0.34224(19) 0.28309(16) 0.34082(14) 0.0582(9) Uani 1 1 d . . .
Si4 Si 0.41075(18) 0.13889(16) 0.35641(14) 0.0573(10) Uani 1 1 d . . .
N2 N 0.5028(5) 0.2320(4) 0.2703(4) 0.055(3) Uani 1 1 d . . .
N1 N 0.1813(5) 0.2363(4) 0.4141(4) 0.051(3) Uani 1 1 d . . .
C6 C 0.0419(6) 0.2230(5) 0.4236(5) 0.053(3) Uani 1 1 d . . .
C4 C -0.0344(5) 0.3015(6) 0.4613(4) 0.061(4) Uani 1 1 d D . .
C7 C 0.0418(6) 0.1649(5) 0.3979(5) 0.051(3) Uani 1 1 d . . .
H7 H 0.0932 0.1477 0.4071 0.061 Uiso 1 1 calc R . .
C3 C 0.0260(7) 0.3350(6) 0.4577(5) 0.058(3) Uani 1 1 d . . .
H3 H 0.0211 0.3730 0.4691 0.070 Uiso 1 1 calc R . .
C5 C -0.0268(7) 0.2449(6) 0.4421(5) 0.059(3) Uani 1 1 d . . .
H5 H -0.0704 0.2210 0.4420 0.070 Uiso 1 1 calc R . .
C1 C 0.1062(6) 0.2595(6) 0.4252(4) 0.049(3) Uani 1 1 d . . .
C89 C 0.4124(7) 0.2497(6) 0.1643(4) 0.058(3) Uani 1 1 d . . .
C93 C 0.4410(7) 0.3022(6) 0.0823(5) 0.066(4) Uani 1 1 d . . .
H93 H 0.4779 0.3191 0.0599 0.079 Uiso 1 1 calc R . .
C88 C 0.4396(7) 0.0947(6) 0.1800(5) 0.060(3) Uani 1 1 d . . .
H88 H 0.3966 0.0899 0.2023 0.072 Uiso 1 1 calc R . .
C94 C 0.4644(7) 0.2728(6) 0.1300(5) 0.062(4) Uani 1 1 d . . .
H94 H 0.5178 0.2685 0.1392 0.075 Uiso 1 1 calc R . .
C91 C 0.3104(8) 0.2839(7) 0.1010(5) 0.077(4) Uani 1 1 d . . .
H91 H 0.2571 0.2878 0.0915 0.092 Uiso 1 1 calc R . .
C92 C 0.3633(8) 0.3070(6) 0.0671(5) 0.071(4) Uani 1 1 d . . .
H92 H 0.3469 0.3260 0.0336 0.085 Uiso 1 1 calc R . .
C37 C 0.3516(7) 0.2707(6) 0.5283(5) 0.069(4) Uani 1 1 d . . .
H37 H 0.3861 0.2543 0.5036 0.082 Uiso 1 1 calc R . .
C90 C 0.3355(7) 0.2547(6) 0.1497(5) 0.068(4) Uani 1 1 d . . .
H90 H 0.2990 0.2382 0.1728 0.081 Uiso 1 1 calc R . .
C14 C 0.0282(6) 0.1650(6) 0.3333(5) 0.058(3) Uani 1 1 d . . .
C44 C 0.1276(8) 0.1207(7) 0.5782(5) 0.071(4) Uani 1 1 d . . .
H44 H 0.0831 0.1242 0.5992 0.085 Uiso 1 1 calc R . .
C36 C 0.2734(6) 0.2620(6) 0.5191(5) 0.059(3) Uani 1 1 d . . .
C41 C 0.2240(7) 0.2850(6) 0.5562(5) 0.062(4) Uani 1 1 d . . .
H41 H 0.1702 0.2795 0.5500 0.074 Uiso 1 1 calc R . .
C83 C 0.4797(6) 0.1455(6) 0.1830(4) 0.052(3) Uani 1 1 d . . .
C87 C 0.4597(7) 0.0528(6) 0.1470(5) 0.066(4) Uani 1 1 d . . .
H87 H 0.4306 0.0190 0.1459 0.079 Uiso 1 1 calc R . .
C86 C 0.5219(8) 0.0578(6) 0.1147(5) 0.065(4) Uani 1 1 d . . .
H86 H 0.5361 0.0276 0.0913 0.078 Uiso 1 1 calc R . .
C71 C 0.6600(7) 0.1628(7) 0.3483(5) 0.069(4) Uani 1 1 d . . .
C8 C -0.0188(8) 0.1269(6) 0.4221(5) 0.062(4) Uani 1 1 d . . .
C40 C 0.2507(8) 0.3145(6) 0.6005(6) 0.073(4) Uani 1 1 d . . .
H40 H 0.2153 0.3289 0.6258 0.088 Uiso 1 1 calc R . .
C85 C 0.5629(7) 0.1066(7) 0.1164(5) 0.070(4) Uani 1 1 d . . .
H85 H 0.6063 0.1100 0.0943 0.084 Uiso 1 1 calc R . .
C20 C -0.1137(5) 0.3178(5) 0.4782(4) 0.070(4) Uani 1 1 d D . .
H20 H -0.1433 0.2826 0.4846 0.084 Uiso 1 1 calc R . .
C84 C 0.5429(6) 0.1510(6) 0.1496(5) 0.058(3) Uani 1 1 d . . .
H84 H 0.5715 0.1850 0.1498 0.069 Uiso 1 1 calc R . .
C45 C 0.1732(8) 0.0761(7) 0.5863(6) 0.082(4) Uani 1 1 d . . .
H45 H 0.1617 0.0491 0.6139 0.099 Uiso 1 1 calc R . .
C55 C 0.5068(9) 0.4001(6) 0.2132(6) 0.072(4) Uani 1 1 d . . .
C34 C 0.1329(10) 0.4972(7) 0.5046(6) 0.084(4) Uani 1 1 d . . .
H34 H 0.0967 0.5271 0.5049 0.100 Uiso 1 1 calc R . .
C19 C -0.0156(7) 0.2070(7) 0.3062(6) 0.074(4) Uani 1 1 d . . .
H19 H -0.0367 0.2370 0.3265 0.088 Uiso 1 1 calc R . .
C15 C 0.0571(6) 0.1212(6) 0.3024(5) 0.063(4) Uani 1 1 d . . .
H15 H 0.0869 0.0926 0.3209 0.076 Uiso 1 1 calc R . .
C35 C 0.1208(9) 0.4530(6) 0.4670(6) 0.070(4) Uani 1 1 d . . .
H35 H 0.0777 0.4539 0.4409 0.084 Uiso 1 1 calc R . .
C53 C 0.5827(7) 0.3128(7) 0.2460(5) 0.068(4) Uani 1 1 d . . .
C48 C 0.5775(7) 0.2553(7) 0.2590(5) 0.063(4) Uani 1 1 d . B .
C33 C 0.1961(10) 0.4982(7) 0.5410(7) 0.082(4) Uani 1 1 d . . .
H33 H 0.2046 0.5283 0.5668 0.098 Uiso 1 1 calc R . .
C30 C 0.1705(8) 0.4081(6) 0.4671(5) 0.060(3) Uani 1 1 d . . .
C13 C -0.0936(7) 0.1238(6) 0.4001(6) 0.073(4) Uani 1 1 d . . .
H13 H -0.1079 0.1444 0.3670 0.087 Uiso 1 1 calc R . .
C42 C 0.2096(7) 0.1563(6) 0.5080(5) 0.061(4) Uani 1 1 d . . .
C43 C 0.1441(7) 0.1622(6) 0.5395(5) 0.067(4) Uani 1 1 d . . .
H43 H 0.1117 0.1941 0.5344 0.081 Uiso 1 1 calc R . .
C2 C 0.0977(7) 0.3176(6) 0.4376(5) 0.060(3) Uani 1 1 d . . .
C23 C 0.1575(8) 0.3602(5) 0.4249(5) 0.063(4) Uani 1 1 d . . .
H23 H 0.2073 0.3395 0.4238 0.075 Uiso 1 1 calc R . .
C50 C 0.7111(8) 0.2423(8) 0.2407(6) 0.082(5) Uani 1 1 d . A .
H50 H 0.7545 0.2182 0.2403 0.099 Uiso 1 1 calc R . .
C75 C 0.6462(8) 0.1223(8) 0.4402(6) 0.087(5) Uani 1 1 d . . .
H75 H 0.6274 0.0929 0.4626 0.104 Uiso 1 1 calc R . .
C39 C 0.3284(8) 0.3249(7) 0.6108(6) 0.088(5) Uani 1 1 d . . .
H39 H 0.3464 0.3462 0.6425 0.105 Uiso 1 1 calc R . .
C76 C 0.6332(7) 0.1207(7) 0.3824(6) 0.078(4) Uani 1 1 d . . .
H76 H 0.6053 0.0901 0.3658 0.094 Uiso 1 1 calc R . .
C61 C 0.5402(10) 0.3872(8) 0.3145(6) 0.085(5) Uani 1 1 d . . .
C72 C 0.7016(8) 0.2062(8) 0.3732(6) 0.088(5) Uani 1 1 d . . .
H72 H 0.7203 0.2360 0.3512 0.106 Uiso 1 1 calc R . .
C70 C 0.6411(7) 0.1598(7) 0.2861(5) 0.068(4) Uani 1 1 d . B .
H70 H 0.5873 0.1455 0.2812 0.082 Uiso 1 1 calc R . .
C24 C 0.1411(8) 0.3860(6) 0.3662(6) 0.072(4) Uani 1 1 d . . .
C60 C 0.4415(9) 0.3982(6) 0.1794(6) 0.074(4) Uani 1 1 d . B .
H60 H 0.4080 0.3669 0.1819 0.089 Uiso 1 1 calc R . .
C31 C 0.2360(8) 0.4091(6) 0.5019(6) 0.069(4) Uani 1 1 d . . .
H31 H 0.2730 0.3799 0.5006 0.082 Uiso 1 1 calc R . .
C47 C 0.2547(7) 0.1083(6) 0.5164(5) 0.067(4) Uani 1 1 d . . .
H47 H 0.2984 0.1034 0.4949 0.080 Uiso 1 1 calc R . .
C25 C 0.1959(9) 0.4209(6) 0.3441(6) 0.077(4) Uani 1 1 d . . .
H25 H 0.2427 0.4280 0.3653 0.093 Uiso 1 1 calc R . .
C49 C 0.6411(7) 0.2200(7) 0.2591(5) 0.072(4) Uani 1 1 d . . .
C17 C 0.0017(8) 0.1624(8) 0.2172(6) 0.082(5) Uani 1 1 d . . .
H17 H -0.0051 0.1628 0.1774 0.099 Uiso 1 1 calc R . .
C73 C 0.7161(8) 0.2054(8) 0.4330(7) 0.095(5) Uani 1 1 d . . .
H73 H 0.7478 0.2336 0.4505 0.113 Uiso 1 1 calc R . .
C9 C -0.0002(9) 0.0937(7) 0.4677(6) 0.077(4) Uani 1 1 d . . .
H9 H 0.0513 0.0930 0.4829 0.093 Uiso 1 1 calc R . .
C21 C -0.1541(7) 0.3498(7) 0.4305(5) 0.101(6) Uani 1 1 d D . .
H21A H -0.1270 0.3852 0.4245 0.151 Uiso 1 1 calc R . .
H21B H -0.2070 0.3578 0.4398 0.151 Uiso 1 1 calc R . .
H21C H -0.1545 0.3270 0.3962 0.151 Uiso 1 1 calc R . .
C22 C -0.1072(7) 0.3503(6) 0.5327(5) 0.080(4) Uani 1 1 d D . .
H22A H -0.0768 0.3844 0.5278 0.121 Uiso 1 1 calc R . .
H22B H -0.0820 0.3269 0.5621 0.121 Uiso 1 1 calc R . .
H22C H -0.1586 0.3608 0.5437 0.121 Uiso 1 1 calc R . .
C38 C 0.3802(8) 0.3029(7) 0.5728(6) 0.093(5) Uani 1 1 d . . .
H38 H 0.4337 0.3101 0.5778 0.111 Uiso 1 1 calc R . .
C32 C 0.2469(10) 0.4542(8) 0.5391(6) 0.083(4) Uani 1 1 d . . .
H32 H 0.2913 0.4544 0.5641 0.100 Uiso 1 1 calc R . .
C51 C 0.7189(6) 0.2961(8) 0.2239(5) 0.085(5) Uani 1 1 d D . .
C52 C 0.6545(9) 0.3303(7) 0.2283(6) 0.085(5) Uani 1 1 d . A .
H52 H 0.6596 0.3688 0.2184 0.102 Uiso 1 1 calc R . .
C10 C -0.0556(14) 0.0610(7) 0.4921(7) 0.102(6) Uani 1 1 d . . .
H10 H -0.0421 0.0389 0.5243 0.123 Uiso 1 1 calc R . .
C58 C 0.4702(15) 0.4850(7) 0.1379(7) 0.101(6) Uani 1 1 d . B .
H58 H 0.4579 0.5136 0.1112 0.121 Uiso 1 1 calc R . .
C27 C 0.1160(11) 0.4342(8) 0.2624(6) 0.089(5) Uani 1 1 d . . .
H27 H 0.1078 0.4505 0.2263 0.107 Uiso 1 1 calc R . .
C16 C 0.0424(8) 0.1189(7) 0.2438(6) 0.077(4) Uani 1 1 d . . .
H16 H 0.0601 0.0880 0.2228 0.092 Uiso 1 1 calc R . .
C77 C 0.6920(7) 0.1157(8) 0.2605(6) 0.078(4) Uani 1 1 d . . .
C12 C -0.1479(10) 0.0918(8) 0.4248(9) 0.096(5) Uani 1 1 d . . .
H12 H -0.1995 0.0915 0.4096 0.116 Uiso 1 1 calc R . .
C82 C 0.6594(9) 0.0707(8) 0.2304(6) 0.085(5) Uani 1 1 d . B .
H82 H 0.6051 0.0681 0.2253 0.102 Uiso 1 1 calc R . .
C46 C 0.2379(8) 0.0683(7) 0.5547(6) 0.082(4) Uani 1 1 d . . .
H46 H 0.2693 0.0359 0.5599 0.098 Uiso 1 1 calc R . .
C18 C -0.0276(7) 0.2032(8) 0.2464(6) 0.083(5) Uani 1 1 d . . .
H18 H -0.0579 0.2311 0.2273 0.100 Uiso 1 1 calc R . .
C26 C 0.1831(10) 0.4458(6) 0.2913(7) 0.084(5) Uani 1 1 d . . .
H26 H 0.2202 0.4699 0.2762 0.100 Uiso 1 1 calc R . .
C74 C 0.6852(9) 0.1652(9) 0.4647(6) 0.096(5) Uani 1 1 d . . .
H74 H 0.6912 0.1672 0.5044 0.115 Uiso 1 1 calc R . .
C59 C 0.4219(11) 0.4417(7) 0.1403(6) 0.093(5) Uani 1 1 d . . .
H59 H 0.3762 0.4400 0.1168 0.112 Uiso 1 1 calc R B .
C11 C -0.1280(14) 0.0609(8) 0.4702(10) 0.110(7) Uani 1 1 d . . .
H11 H -0.1656 0.0386 0.4871 0.131 Uiso 1 1 calc R . .
C29 C 0.0746(9) 0.3762(7) 0.3327(6) 0.084(4) Uani 1 1 d . . .
H29 H 0.0372 0.3511 0.3459 0.101 Uiso 1 1 calc R . .
C57 C 0.5359(12) 0.4911(8) 0.1712(8) 0.096(6) Uani 1 1 d . . .
H57 H 0.5677 0.5234 0.1690 0.115 Uiso 1 1 calc R B .
C56 C 0.5534(9) 0.4480(7) 0.2079(6) 0.085(5) Uani 1 1 d . B .
H56 H 0.5994 0.4506 0.2310 0.102 Uiso 1 1 calc R . .
C78 C 0.7719(8) 0.1174(8) 0.2691(6) 0.093(5) Uani 1 1 d . B .
H78 H 0.7957 0.1461 0.2916 0.111 Uiso 1 1 calc R . .
C81 C 0.7057(11) 0.0289(8) 0.2075(6) 0.101(6) Uani 1 1 d . . .
H81 H 0.6825 -0.0018 0.1875 0.122 Uiso 1 1 calc R B .
C28 C 0.0606(12) 0.4017(8) 0.2808(7) 0.104(6) Uani 1 1 d . . .
H28 H 0.0137 0.3962 0.2593 0.125 Uiso 1 1 calc R . .
C66 C 0.4853(11) 0.4253(9) 0.3302(8) 0.110(6) Uani 1 1 d . B .
H66 H 0.4390 0.4302 0.3078 0.133 Uiso 1 1 calc R . .
C79 C 0.8170(9) 0.0761(11) 0.2440(8) 0.109(6) Uani 1 1 d . . .
H79 H 0.8714 0.0784 0.2478 0.131 Uiso 1 1 calc R B .
C67A C 0.8025(7) 0.3060(10) 0.2095(10) 0.070(10) Uiso 0.50 1 d PD A 2
H67A H 0.8342 0.2721 0.2019 0.084 Uiso 0.50 1 calc PR A 2
C63 C 0.6235(13) 0.4149(12) 0.3938(8) 0.132(9) Uani 1 1 d . . .
H63 H 0.6689 0.4099 0.4171 0.159 Uiso 1 1 calc R B .
C69A C 0.8354(17) 0.3481(18) 0.2532(19) 0.15(2) Uiso 0.50 1 d PD A 2
H69A H 0.8028 0.3816 0.2531 0.219 Uiso 0.50 1 calc PR A 2
H69B H 0.8875 0.3588 0.2439 0.219 Uiso 0.50 1 calc PR A 2
H69C H 0.8370 0.3307 0.2905 0.219 Uiso 0.50 1 calc PR A 2
C62 C 0.6091(10) 0.3830(8) 0.3446(7) 0.104(6) Uani 1 1 d . B .
H62 H 0.6475 0.3584 0.3322 0.124 Uiso 1 1 calc R . .
C80 C 0.7824(11) 0.0325(10) 0.2139(7) 0.108(6) Uani 1 1 d . B .
H80 H 0.8133 0.0047 0.1976 0.130 Uiso 1 1 calc R . .
C64 C 0.5662(16) 0.4553(12) 0.4069(9) 0.146(9) Uani 1 1 d . B .
H64 H 0.5769 0.4818 0.4361 0.175 Uiso 1 1 calc R . .
C65 C 0.4989(12) 0.4562(10) 0.3789(8) 0.134(8) Uani 1 1 d . . .
H65 H 0.4587 0.4785 0.3924 0.161 Uiso 1 1 calc R B .
C68A C 0.8007(13) 0.3531(11) 0.1660(11) 0.076(8) Uiso 0.50 1 d PD A 2
H68A H 0.7865 0.3885 0.1838 0.114 Uiso 0.50 1 calc PR A 2
H68B H 0.7629 0.3442 0.1354 0.114 Uiso 0.50 1 calc PR A 2
H68C H 0.8516 0.3570 0.1510 0.114 Uiso 0.50 1 calc PR A 2
C96 C 0.1769(6) 0.1098(5) 0.0890(7) 0.037(5) Uiso 0.50 1 d PD . .
C95 C 0.2175(9) 0.0567(7) 0.1114(9) 0.053(6) Uiso 0.50 1 d PD . .
H95A H 0.2694 0.0664 0.1261 0.079 Uiso 0.50 1 calc PR . .
H95B H 0.2207 0.0293 0.0809 0.079 Uiso 0.50 1 calc PR . .
H95C H 0.1885 0.0405 0.1414 0.079 Uiso 0.50 1 calc PR . .
C101 C 0.1643(9) 0.1553(7) 0.1235(5) 0.067(7) Uiso 0.50 1 d PD . .
H101 H 0.1811 0.1538 0.1620 0.080 Uiso 0.50 1 calc PR . .
C100 C 0.1273(10) 0.2030(6) 0.1022(7) 0.069(7) Uiso 0.50 1 d PD . .
H100 H 0.1188 0.2341 0.1261 0.083 Uiso 0.50 1 calc PR . .
C99 C 0.1027(9) 0.2054(6) 0.0459(7) 0.052(6) Uiso 0.50 1 d PD . .
H99 H 0.0772 0.2380 0.0312 0.062 Uiso 0.50 1 calc PR . .
C108 C 0.0964(11) 0.4552(7) 0.0817(8) 0.077(8) Uiso 0.50 1 d PD . .
H108 H 0.1171 0.4900 0.0702 0.092 Uiso 0.50 1 calc PR . .
C104 C 0.1148(13) 0.3650(8) 0.1265(9) 0.113(12) Uiso 0.50 1 d PD . .
H104 H 0.1480 0.3386 0.1453 0.135 Uiso 0.50 1 calc PR . .
C103 C 0.1425(9) 0.4159(8) 0.1092(8) 0.113(11) Uiso 0.50 1 d PD . .
C106 C -0.0103(10) 0.3919(11) 0.0881(10) 0.108(11) Uiso 0.50 1 d PD . .
H106 H -0.0631 0.3835 0.0807 0.129 Uiso 0.50 1 calc PR . .
C107 C 0.0185(11) 0.4431(10) 0.0711(9) 0.120(12) Uiso 0.50 1 d PD . .
H107 H -0.0145 0.4698 0.0524 0.144 Uiso 0.50 1 calc PR . .
C105 C 0.0368(14) 0.3526(9) 0.1157(10) 0.164(18) Uiso 0.50 1 d PD . .
H105 H 0.0164 0.3177 0.1272 0.197 Uiso 0.50 1 calc PR . .
C97 C 0.1524(11) 0.1122(7) 0.0326(7) 0.134(14) Uiso 0.50 1 d PD . .
H97 H 0.1609 0.0811 0.0087 0.161 Uiso 0.50 1 calc PR . .
C98 C 0.1154(12) 0.1601(8) 0.0113(6) 0.118(12) Uiso 0.50 1 d PD . .
H98 H 0.0988 0.1616 -0.0273 0.141 Uiso 0.50 1 calc PR . .
C102 C 0.2254(10) 0.4291(14) 0.1206(13) 0.18(2) Uiso 0.50 1 d PD . .
H10A H 0.2310 0.4581 0.1497 0.267 Uiso 0.50 1 calc PR . .
H10B H 0.2471 0.4429 0.0861 0.267 Uiso 0.50 1 calc PR . .
H10C H 0.2528 0.3951 0.1333 0.267 Uiso 0.50 1 calc PR . .
C68 C 0.8222(12) 0.3080(15) 0.1598(10) 0.088(8) Uani 0.50 1 d PDU A 1
H68D H 0.8747 0.3219 0.1567 0.132 Uiso 0.50 1 calc PR A 1
H68E H 0.7905 0.3196 0.1266 0.132 Uiso 0.50 1 calc PR A 1
H68F H 0.8229 0.2669 0.1623 0.132 Uiso 0.50 1 calc PR A 1
C67 C 0.7889(10) 0.3324(11) 0.2122(7) 0.076(7) Uani 0.50 1 d PDU A 1
H67 H 0.7730 0.3723 0.2055 0.091 Uiso 0.50 1 calc PR A 1
C69 C 0.8432(9) 0.3283(15) 0.2646(9) 0.059(7) Uani 0.50 1 d PDU A 1
H69D H 0.8311 0.2944 0.2858 0.089 Uiso 0.50 1 calc PR A 1
H69E H 0.8369 0.3615 0.2882 0.089 Uiso 0.50 1 calc PR A 1
H69F H 0.8964 0.3262 0.2535 0.089 Uiso 0.50 1 calc PR A 1
C54 C 0.5223(8) 0.3565(6) 0.2572(6) 0.070(4) Uiso 1 1 d . B 1
H54 H 0.4731 0.3356 0.2609 0.084 Uiso 1 1 calc R B 1


_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
Cl5 Si4 2.060(4) . ?
Cl1 Si1 2.040(4) . ?
Cl4 Si3 2.044(4) . ?
Cl6 Si4 2.060(5) . ?
P2 N2 1.721(9) . ?
P2 C83 1.823(13) . ?
P2 C89 1.835(13) . ?
P2 Si3 2.698(4) . ?
Cl2 Si2 2.050(5) . ?
Cl7 Si5 2.054(5) . ?
Cl3 Si2 2.054(5) . ?
Cl8 Si5 2.060(5) . ?
P1 N1 1.740(9) . ?
P1 C42 1.832(13) . ?
P1 C36 1.837(13) . ?
P1 Si1 2.683(5) . ?
Si1 N1 1.735(9) . ?
Si1 Si5 2.356(5) . ?
Si1 Si2 2.390(5) . ?
Si5 Si4 2.355(4) . ?
Si3 N2 1.731(9) . ?
Si3 Si4 2.357(5) . ?
Si3 Si2 2.400(5) . ?
N2 C48 1.455(15) . ?
N1 C1 1.459(14) . ?
C6 C5 1.401(16) . ?
C6 C1 1.415(16) . ?
C6 C7 1.512(16) . ?
C4 C3 1.326(16) . ?
C4 C5 1.431(17) . ?
C4 C20 1.514(7) . ?
C7 C8 1.530(16) . ?
C7 C14 1.545(16) . ?
C3 C2 1.426(16) . ?
C1 C2 1.423(17) . ?
C89 C90 1.371(16) . ?
C89 C94 1.372(16) . ?
C93 C94 1.376(17) . ?
C93 C92 1.387(17) . ?
C88 C87 1.330(17) . ?
C88 C83 1.395(17) . ?
C91 C92 1.375(17) . ?
C91 C90 1.404(17) . ?
C37 C38 1.379(18) . ?
C37 C36 1.385(16) . ?
C14 C15 1.387(17) . ?
C14 C19 1.394(18) . ?
C44 C45 1.333(19) . ?
C44 C43 1.393(18) . ?
C36 C41 1.382(16) . ?
C41 C40 1.331(17) . ?
C83 C84 1.401(15) . ?
C87 C86 1.371(17) . ?
C86 C85 1.363(18) . ?
C71 C72 1.377(19) . ?
C71 C76 1.388(19) . ?
C71 C70 1.504(17) . ?
C8 C9 1.368(18) . ?
C8 C13 1.381(18) . ?
C40 C39 1.386(18) . ?
C85 C84 1.377(18) . ?
C20 C21 1.510(8) . ?
C20 C22 1.512(7) . ?
C45 C46 1.404(19) . ?
C55 C60 1.360(19) . ?
C55 C56 1.41(2) . ?
C55 C54 1.490(19) . ?
C34 C33 1.37(2) . ?
C34 C35 1.390(19) . ?
C19 C18 1.432(18) . ?
C15 C16 1.410(17) . ?
C35 C30 1.375(18) . ?
C53 C48 1.406(19) . ?
C53 C52 1.406(18) . ?
C53 C54 1.514(19) . ?
C48 C49 1.392(19) . ?
C33 C32 1.38(2) . ?
C30 C31 1.374(18) . ?
C30 C23 1.529(17) . ?
C13 C12 1.37(2) . ?
C42 C47 1.393(17) . ?
C42 C43 1.409(16) . ?
C2 C23 1.498(17) . ?
C23 C24 1.543(18) . ?
C50 C51 1.35(2) . ?
C50 C49 1.423(18) . ?
C75 C74 1.34(2) . ?
C75 C76 1.385(18) . ?
C39 C38 1.417(18) . ?
C61 C62 1.37(2) . ?
C61 C66 1.38(2) . ?
C61 C54 1.57(2) . ?
C72 C73 1.44(2) . ?
C70 C77 1.524(19) . ?
C70 C49 1.57(2) . ?
C24 C29 1.390(19) . ?
C24 C25 1.391(19) . ?
C60 C59 1.42(2) . ?
C31 C32 1.399(19) . ?
C47 C46 1.362(18) . ?
C25 C26 1.400(19) . ?
C17 C18 1.31(2) . ?
C17 C16 1.39(2) . ?
C73 C74 1.35(2) . ?
C9 C10 1.39(2) . ?
C51 C52 1.39(2) . ?
C51 C67 1.535(8) . ?
C51 C67A 1.535(8) . ?
C10 C11 1.34(3) . ?
C58 C59 1.33(2) . ?
C58 C57 1.36(2) . ?
C27 C28 1.33(2) . ?
C27 C26 1.35(2) . ?
C77 C82 1.39(2) . ?
C77 C78 1.398(19) . ?
C12 C11 1.34(3) . ?
C82 C81 1.41(2) . ?
C29 C28 1.39(2) . ?
C57 C56 1.37(2) . ?
C78 C79 1.41(2) . ?
C81 C80 1.34(2) . ?
C66 C65 1.38(2) . ?
C79 C80 1.38(3) . ?
C67A C68A 1.525(8) . ?
C67A C69A 1.534(8) . ?
C63 C62 1.41(2) . ?
C63 C64 1.43(3) . ?
C64 C65 1.32(3) . ?
C96 C101 1.385(7) . ?
C96 C97 1.390(7) . ?
C96 C95 1.529(8) . ?
C101 C100 1.388(7) . ?
C100 C99 1.389(7) . ?
C99 C98 1.384(7) . ?
C108 C103 1.376(7) . ?
C108 C107 1.398(7) . ?
C104 C103 1.375(7) . ?
C104 C105 1.401(7) . ?
C103 C102 1.490(6) . ?
C106 C105 1.384(7) . ?
C106 C107 1.387(7) . ?
C97 C98 1.391(7) . ?
C68 C67 1.524(8) . ?
C67 C69 1.529(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 P2 C83 112.0(5) . . ?
N2 P2 C89 111.1(5) . . ?
C83 P2 C89 98.3(5) . . ?
N2 P2 Si3 38.7(3) . . ?
C83 P2 Si3 130.3(4) . . ?
C89 P2 Si3 127.2(4) . . ?
N1 P1 C42 111.9(5) . . ?
N1 P1 C36 111.8(5) . . ?
C42 P1 C36 97.4(6) . . ?
N1 P1 Si1 39.4(3) . . ?
C42 P1 Si1 130.6(4) . . ?
C36 P1 Si1 128.0(4) . . ?
N1 Si1 Cl1 109.6(4) . . ?
N1 Si1 Si5 113.9(4) . . ?
Cl1 Si1 Si5 109.9(2) . . ?
N1 Si1 Si2 118.9(3) . . ?
Cl1 Si1 Si2 103.24(19) . . ?
Si5 Si1 Si2 100.55(17) . . ?
N1 Si1 P1 39.5(3) . . ?
Cl1 Si1 P1 148.97(19) . . ?
Si5 Si1 P1 87.78(16) . . ?
Si2 Si1 P1 98.03(16) . . ?
Cl7 Si5 Cl8 104.9(2) . . ?
Cl7 Si5 Si4 109.1(2) . . ?
Cl8 Si5 Si4 107.29(18) . . ?
Cl7 Si5 Si1 116.83(19) . . ?
Cl8 Si5 Si1 110.0(2) . . ?
Si4 Si5 Si1 108.30(19) . . ?
N2 Si3 Cl4 109.5(3) . . ?
N2 Si3 Si4 115.6(4) . . ?
Cl4 Si3 Si4 109.00(19) . . ?
N2 Si3 Si2 118.2(4) . . ?
Cl4 Si3 Si2 103.6(2) . . ?
Si4 Si3 Si2 99.98(17) . . ?
N2 Si3 P2 38.5(3) . . ?
Cl4 Si3 P2 147.78(18) . . ?
Si4 Si3 P2 89.73(16) . . ?
Si2 Si3 P2 98.41(16) . . ?
Cl2 Si2 Cl3 106.0(2) . . ?
Cl2 Si2 Si1 106.17(19) . . ?
Cl3 Si2 Si1 111.82(19) . . ?
Cl2 Si2 Si3 111.30(19) . . ?
Cl3 Si2 Si3 106.8(2) . . ?
Si1 Si2 Si3 114.4(2) . . ?
Cl5 Si4 Cl6 105.3(2) . . ?
Cl5 Si4 Si5 109.36(18) . . ?
Cl6 Si4 Si5 107.5(2) . . ?
Cl5 Si4 Si3 108.4(2) . . ?
Cl6 Si4 Si3 117.56(19) . . ?
Si5 Si4 Si3 108.63(19) . . ?
C48 N2 P2 127.4(7) . . ?
C48 N2 Si3 129.8(8) . . ?
P2 N2 Si3 102.8(5) . . ?
C1 N1 Si1 132.1(7) . . ?
C1 N1 P1 126.7(7) . . ?
Si1 N1 P1 101.1(5) . . ?
C5 C6 C1 117.0(11) . . ?
C5 C6 C7 119.0(10) . . ?
C1 C6 C7 123.6(11) . . ?
C3 C4 C5 117.2(9) . . ?
C3 C4 C20 127.2(11) . . ?
C5 C4 C20 115.4(11) . . ?
C6 C7 C8 111.8(10) . . ?
C6 C7 C14 113.6(10) . . ?
C8 C7 C14 107.9(9) . . ?
C4 C3 C2 124.2(12) . . ?
C6 C5 C4 123.1(11) . . ?
C6 C1 C2 120.6(11) . . ?
C6 C1 N1 118.8(11) . . ?
C2 C1 N1 120.6(10) . . ?
C90 C89 C94 118.9(12) . . ?
C90 C89 P2 115.6(9) . . ?
C94 C89 P2 124.7(10) . . ?
C94 C93 C92 119.9(12) . . ?
C87 C88 C83 122.1(12) . . ?
C89 C94 C93 121.4(12) . . ?
C92 C91 C90 119.8(12) . . ?
C91 C92 C93 119.4(12) . . ?
C38 C37 C36 121.0(12) . . ?
C89 C90 C91 120.6(12) . . ?
C15 C14 C19 119.7(12) . . ?
C15 C14 C7 119.3(11) . . ?
C19 C14 C7 120.9(12) . . ?
C45 C44 C43 121.0(13) . . ?
C41 C36 C37 118.9(12) . . ?
C41 C36 P1 127.0(9) . . ?
C37 C36 P1 113.3(9) . . ?
C40 C41 C36 120.9(12) . . ?
C88 C83 C84 117.4(11) . . ?
C88 C83 P2 116.4(9) . . ?
C84 C83 P2 125.7(11) . . ?
C88 C87 C86 120.8(13) . . ?
C85 C86 C87 119.2(13) . . ?
C72 C71 C76 118.3(13) . . ?
C72 C71 C70 122.8(14) . . ?
C76 C71 C70 118.8(13) . . ?
C9 C8 C13 116.8(13) . . ?
C9 C8 C7 120.2(13) . . ?
C13 C8 C7 123.0(13) . . ?
C41 C40 C39 122.0(13) . . ?
C86 C85 C84 121.3(12) . . ?
C21 C20 C22 113.7(11) . . ?
C21 C20 C4 108.8(7) . . ?
C22 C20 C4 109.6(7) . . ?
C85 C84 C83 119.3(12) . . ?
C44 C45 C46 121.2(14) . . ?
C60 C55 C56 116.2(14) . . ?
C60 C55 C54 120.6(13) . . ?
C56 C55 C54 122.9(14) . . ?
C33 C34 C35 120.8(16) . . ?
C14 C19 C18 117.6(14) . . ?
C14 C15 C16 120.4(13) . . ?
C30 C35 C34 120.9(14) . . ?
C48 C53 C52 115.1(14) . . ?
C48 C53 C54 125.0(11) . . ?
C52 C53 C54 119.4(15) . . ?
C49 C48 C53 121.6(12) . . ?
C49 C48 N2 119.5(13) . . ?
C53 C48 N2 118.8(12) . . ?
C34 C33 C32 117.7(14) . . ?
C31 C30 C35 119.4(13) . . ?
C31 C30 C23 119.8(13) . . ?
C35 C30 C23 120.4(12) . . ?
C12 C13 C8 121.7(16) . . ?
C47 C42 C43 118.2(12) . . ?
C47 C42 P1 115.4(9) . . ?
C43 C42 P1 125.8(12) . . ?
C44 C43 C42 119.1(13) . . ?
C1 C2 C3 117.1(11) . . ?
C1 C2 C23 122.3(11) . . ?
C3 C2 C23 120.3(12) . . ?
C2 C23 C30 116.8(11) . . ?
C2 C23 C24 110.9(11) . . ?
C30 C23 C24 108.4(11) . . ?
C51 C50 C49 123.1(14) . . ?
C74 C75 C76 120.4(16) . . ?
C40 C39 C38 118.2(13) . . ?
C75 C76 C71 121.5(14) . . ?
C62 C61 C66 120.4(17) . . ?
C62 C61 C54 123.4(17) . . ?
C66 C61 C54 115.7(14) . . ?
C71 C72 C73 118.6(15) . . ?
C71 C70 C77 109.2(11) . . ?
C71 C70 C49 110.9(12) . . ?
C77 C70 C49 116.7(11) . . ?
C29 C24 C25 116.9(14) . . ?
C29 C24 C23 124.2(13) . . ?
C25 C24 C23 118.9(13) . . ?
C55 C60 C59 121.9(16) . . ?
C30 C31 C32 118.4(14) . . ?
C46 C47 C42 121.8(12) . . ?
C24 C25 C26 120.9(15) . . ?
C48 C49 C50 118.3(15) . . ?
C48 C49 C70 122.2(11) . . ?
C50 C49 C70 119.0(14) . . ?
C18 C17 C16 120.7(14) . . ?
C74 C73 C72 120.8(15) . . ?
C8 C9 C10 121.0(16) . . ?
C37 C38 C39 118.8(13) . . ?
C33 C32 C31 122.6(15) . . ?
C50 C51 C52 115.9(10) . . ?
C50 C51 C67 132.9(15) . . ?
C52 C51 C67 109.8(16) . . ?
C50 C51 C67A 108.9(14) . . ?
C52 C51 C67A 134.9(15) . . ?
C67 C51 C67A 25.4(12) . . ?
C51 C52 C53 125.7(14) . . ?
C11 C10 C9 119.9(18) . . ?
C59 C58 C57 124.8(18) . . ?
C28 C27 C26 125.1(16) . . ?
C17 C16 C15 119.0(14) . . ?
C82 C77 C78 118.2(15) . . ?
C82 C77 C70 120.4(12) . . ?
C78 C77 C70 121.3(16) . . ?
C11 C12 C13 119.8(18) . . ?
C77 C82 C81 121.0(15) . . ?
C47 C46 C45 118.5(14) . . ?
C17 C18 C19 122.4(15) . . ?
C27 C26 C25 117.6(15) . . ?
C75 C74 C73 120.3(15) . . ?
C58 C59 C60 117.4(18) . . ?
C10 C11 C12 120.8(18) . . ?
C28 C29 C24 122.5(15) . . ?
C58 C57 C56 116.2(16) . . ?
C57 C56 C55 123.6(16) . . ?
C77 C78 C79 119.5(17) . . ?
C80 C81 C82 120.0(18) . . ?
C27 C28 C29 116.9(17) . . ?
C65 C66 C61 119.0(19) . . ?
C80 C79 C78 120.4(16) . . ?
C68A C67A C69A 89(3) . . ?
C68A C67A C51 106.4(8) . . ?
C69A C67A C51 105.8(8) . . ?
C62 C63 C64 116.7(19) . . ?
C61 C62 C63 121(2) . . ?
C81 C80 C79 120.7(17) . . ?
C65 C64 C63 121(2) . . ?
C64 C65 C66 122(2) . . ?
C101 C96 C97 119.6(6) . . ?
C101 C96 C95 121.5(14) . . ?
C97 C96 C95 118.9(14) . . ?
C96 C101 C100 120.4(6) . . ?
C101 C100 C99 120.0(6) . . ?
C98 C99 C100 119.6(6) . . ?
C103 C108 C107 118.9(6) . . ?
C103 C104 C105 118.9(6) . . ?
C104 C103 C108 122.3(5) . . ?
C104 C103 C102 119.1(7) . . ?
C108 C103 C102 118.6(7) . . ?
C105 C106 C107 121.1(6) . . ?
C106 C107 C108 119.4(6) . . ?
C106 C105 C104 119.3(6) . . ?
C96 C97 C98 119.9(6) . . ?
C99 C98 C97 120.4(6) . . ?
C68 C67 C69 114(2) . . ?
C68 C67 C51 106.3(8) . . ?
C69 C67 C51 106.1(7) . . ?
C55 C54 C53 116.9(12) . . ?
C55 C54 C61 108.1(12) . . ?
C53 C54 C61 111.5(12) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        20.96
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.759
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.083
