data_2009src0117

#Dr. M. A. Beckett 

_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C36 H30 I N P2'
_chemical_formula_weight          665.45
 
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'
 'I'  'I'  -0.4742   1.8119
 '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                    29.6827(6)
_cell_length_b                    10.1604(2)
_cell_length_c                    20.2114(4)
_cell_angle_alpha                 90.00
_cell_angle_beta                  91.3370(10)
_cell_angle_gamma                 90.00
_cell_volume                      6093.9(2)
_cell_formula_units_Z             8
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     14269
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Slab
_exptl_crystal_colour             Colourless
_exptl_crystal_size_max           0.18
_exptl_crystal_size_mid           0.10
_exptl_crystal_size_min           0.05
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.451
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              2688
_exptl_absorpt_coefficient_mu     1.182
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.8154
_exptl_absorpt_correction_T_max   0.9433
_exptl_absorpt_process_details       'SADABS 2007/2 (Sheldrick, G.M., 2007)'

_exptl_special_details
;
SADABS was used to perform the Absorption correction
Parameter refinement on 49041 reflections reduced R(int) from 0.1282 to 0.0578
Ratio of minimum to maximum apparent transmission: 0.905943
The given Tmin and Tmax were generated using the SHELX SIZE command
;

_diffrn_ambient_temperature           120(2)
_diffrn_radiation_wavelength           0.71073
_diffrn_radiation_type                      MoK\a
_diffrn_radiation_source                  'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator    '10cm confocal mirrors'
_diffrn_measurement_device_type   
'Bruker-Nonius APEX II CCD camera on κ-goniostat'
_diffrn_measurement_method          'φ & ω scans'
_diffrn_detector_area_resol_mean   '4096x4096pixels / 62x62mm'
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             52122
_diffrn_reflns_av_R_equivalents   0.0539
_diffrn_reflns_av_sigmaI/netI     0.0501
_diffrn_reflns_limit_h_min        -38
_diffrn_reflns_limit_h_max        38
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -26
_diffrn_reflns_limit_l_max        26
_diffrn_reflns_theta_min          2.91
_diffrn_reflns_theta_max          27.48
_reflns_number_total              13900
_reflns_number_gt                 11771
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997a)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997b)' 
_computing_molecular_graphics     'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material   'WinGX (Farrugia, 1999)'
 
_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)+(0.0000P)²+23.1366P] 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          13900
_refine_ls_number_parameters      721
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0613
_refine_ls_R_factor_gt            0.0483
_refine_ls_wR_factor_ref          0.1045
_refine_ls_wR_factor_gt           0.0966
_refine_ls_goodness_of_fit_ref    1.111
_refine_ls_restrained_S_all       1.111
_refine_ls_shift/su_max           0.002
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
I1 I 0.369635(8) -0.03183(2) 0.279022(13) 0.02336(7) Uani 1 1 d . . .
I2 I 0.132635(8) 0.79725(2) 0.522407(13) 0.02426(7) Uani 1 1 d . . .
C1 C 0.44904(12) 0.1172(4) -0.13846(17) 0.0166(7) Uani 1 1 d . . .
C2 C 0.48299(12) 0.0265(4) -0.15317(19) 0.0220(8) Uani 1 1 d . . .
H2 H 0.4791 -0.0644 -0.1438 0.026 Uiso 1 1 calc R . .
C3 C 0.52246(13) 0.0712(5) -0.1817(2) 0.0296(9) Uani 1 1 d . . .
H3 H 0.5458 0.0108 -0.1914 0.036 Uiso 1 1 calc R . .
C4 C 0.52758(14) 0.2024(5) -0.1958(2) 0.0313(10) Uani 1 1 d . . .
H4 H 0.5543 0.2320 -0.2161 0.038 Uiso 1 1 calc R . .
C5 C 0.49427(14) 0.2922(4) -0.1807(2) 0.0287(9) Uani 1 1 d . . .
H5 H 0.4985 0.3830 -0.1898 0.034 Uiso 1 1 calc R . .
C6 C 0.45437(12) 0.2496(4) -0.15225(18) 0.0205(8) Uani 1 1 d . . .
H6 H 0.4312 0.3107 -0.1425 0.025 Uiso 1 1 calc R . .
C7 C 0.40561(12) -0.0902(3) -0.06631(18) 0.0168(7) Uani 1 1 d . . .
C8 C 0.43838(12) -0.0866(4) -0.01529(19) 0.0211(8) Uani 1 1 d . . .
H8 H 0.4550 -0.0082 -0.0071 0.025 Uiso 1 1 calc R . .
C9 C 0.44652(14) -0.1973(4) 0.0233(2) 0.0279(9) Uani 1 1 d . . .
H9 H 0.4687 -0.1946 0.0579 0.033 Uiso 1 1 calc R . .
C10 C 0.42216(15) -0.3126(4) 0.0115(2) 0.0320(10) Uani 1 1 d . . .
H10 H 0.4276 -0.3880 0.0383 0.038 Uiso 1 1 calc R . .
C11 C 0.39005(16) -0.3173(4) -0.0393(2) 0.0367(11) Uani 1 1 d . . .
H11 H 0.3736 -0.3961 -0.0474 0.044 Uiso 1 1 calc R . .
C12 C 0.38185(14) -0.2067(4) -0.0786(2) 0.0275(9) Uani 1 1 d . . .
H12 H 0.3601 -0.2106 -0.1138 0.033 Uiso 1 1 calc R . .
C13 C 0.36500(12) 0.0223(4) -0.18820(18) 0.0176(7) Uani 1 1 d . . .
C14 C 0.38140(15) -0.0762(4) -0.2293(2) 0.0321(10) Uani 1 1 d . . .
H14 H 0.4059 -0.1298 -0.2147 0.039 Uiso 1 1 calc R . .
C15 C 0.36180(17) -0.0955(4) -0.2915(2) 0.0379(11) Uani 1 1 d . . .
H15 H 0.3733 -0.1615 -0.3198 0.045 Uiso 1 1 calc R . .
C16 C 0.32557(14) -0.0191(4) -0.3126(2) 0.0278(9) Uani 1 1 d . . .
H16 H 0.3121 -0.0332 -0.3551 0.033 Uiso 1 1 calc R . .
C17 C 0.30910(13) 0.0775(4) -0.27161(19) 0.0231(8) Uani 1 1 d . . .
H17 H 0.2842 0.1299 -0.2859 0.028 Uiso 1 1 calc R . .
C18 C 0.32898(12) 0.0983(4) -0.20930(18) 0.0198(8) Uani 1 1 d . . .
H18 H 0.3177 0.1651 -0.1813 0.024 Uiso 1 1 calc R . .
C21 C 0.31812(12) 0.0474(4) 0.02718(18) 0.0189(7) Uani 1 1 d . . .
C22 C 0.27423(14) 0.0241(4) 0.00151(19) 0.0272(9) Uani 1 1 d . . .
H22 H 0.2602 0.0869 -0.0270 0.033 Uiso 1 1 calc R . .
C23 C 0.25146(15) -0.0907(4) 0.0180(2) 0.0299(9) Uani 1 1 d . . .
H23 H 0.2219 -0.1061 0.0007 0.036 Uiso 1 1 calc R . .
C24 C 0.27177(15) -0.1817(4) 0.0593(2) 0.0271(9) Uani 1 1 d . . .
H24 H 0.2565 -0.2609 0.0696 0.033 Uiso 1 1 calc R . .
C25 C 0.31401(15) -0.1585(4) 0.0855(2) 0.0358(11) Uani 1 1 d . . .
H25 H 0.3273 -0.2206 0.1152 0.043 Uiso 1 1 calc R . .
C26 C 0.33761(14) -0.0455(4) 0.0693(2) 0.0313(10) Uani 1 1 d . . .
H26 H 0.3671 -0.0317 0.0870 0.038 Uiso 1 1 calc R . .
C27 C 0.39002(12) 0.2361(4) 0.05878(17) 0.0180(7) Uani 1 1 d . . .
C28 C 0.43080(14) 0.2866(4) 0.0371(2) 0.0253(8) Uani 1 1 d . . .
H28 H 0.4365 0.2919 -0.0089 0.030 Uiso 1 1 calc R . .
C29 C 0.46323(15) 0.3293(4) 0.0834(2) 0.0308(9) Uani 1 1 d . . .
H29 H 0.4910 0.3643 0.0688 0.037 Uiso 1 1 calc R . .
C30 C 0.45520(15) 0.3209(4) 0.1501(2) 0.0301(9) Uani 1 1 d . . .
H30 H 0.4775 0.3498 0.1814 0.036 Uiso 1 1 calc R . .
C31 C 0.41511(15) 0.2708(4) 0.1716(2) 0.0305(9) Uani 1 1 d . . .
H31 H 0.4099 0.2654 0.2177 0.037 Uiso 1 1 calc R . .
C32 C 0.38215(14) 0.2280(4) 0.12689(19) 0.0278(9) Uani 1 1 d . . .
H32 H 0.3545 0.1936 0.1422 0.033 Uiso 1 1 calc R . .
C33 C 0.30720(12) 0.3182(3) -0.01112(17) 0.0162(7) Uani 1 1 d . . .
C34 C 0.30652(13) 0.3962(4) -0.0675(2) 0.0220(8) Uani 1 1 d . . .
H34 H 0.3277 0.3817 -0.1012 0.026 Uiso 1 1 calc R . .
C35 C 0.27452(14) 0.4961(4) -0.0745(2) 0.0264(9) Uani 1 1 d . . .
H35 H 0.2742 0.5499 -0.1129 0.032 Uiso 1 1 calc R . .
C36 C 0.24337(14) 0.5172(4) -0.0259(2) 0.0289(9) Uani 1 1 d . . .
H36 H 0.2212 0.5839 -0.0316 0.035 Uiso 1 1 calc R . .
C37 C 0.24440(13) 0.4413(4) 0.0312(2) 0.0284(9) Uani 1 1 d . . .
H37 H 0.2234 0.4576 0.0649 0.034 Uiso 1 1 calc R . .
C38 C 0.27615(12) 0.3414(4) 0.03915(19) 0.0212(8) Uani 1 1 d . . .
H38 H 0.2768 0.2892 0.0782 0.025 Uiso 1 1 calc R . .
N1 N 0.36970(10) 0.1700(3) -0.07309(14) 0.0184(6) Uani 1 1 d . . .
P1 P 0.39496(3) 0.05850(9) -0.11203(4) 0.01427(18) Uani 1 1 d . . .
P2 P 0.34805(3) 0.18839(9) -0.00264(4) 0.01560(18) Uani 1 1 d . . .
C41 C 0.18730(11) 0.2625(3) 0.25464(17) 0.0145(7) Uani 1 1 d . . .
C42 C 0.17620(13) 0.2292(4) 0.18920(19) 0.0203(8) Uani 1 1 d . . .
H42 H 0.1505 0.2672 0.1678 0.024 Uiso 1 1 calc R . .
C43 C 0.20287(14) 0.1400(4) 0.1553(2) 0.0267(9) Uani 1 1 d . . .
H43 H 0.1955 0.1183 0.1107 0.032 Uiso 1 1 calc R . .
C44 C 0.24003(13) 0.0829(4) 0.1866(2) 0.0240(8) Uani 1 1 d . . .
H44 H 0.2580 0.0221 0.1632 0.029 Uiso 1 1 calc R . .
C45 C 0.25116(12) 0.1138(4) 0.2517(2) 0.0220(8) Uani 1 1 d . . .
H45 H 0.2765 0.0738 0.2731 0.026 Uiso 1 1 calc R . .
C46 C 0.22500(12) 0.2037(4) 0.28578(18) 0.0186(7) Uani 1 1 d . . .
H46 H 0.2327 0.2254 0.3303 0.022 Uiso 1 1 calc R . .
C47 C 0.15111(11) 0.3477(4) 0.38024(17) 0.0160(7) Uani 1 1 d . . .
C48 C 0.14568(13) 0.2155(4) 0.39693(19) 0.0213(8) Uani 1 1 d . . .
H48 H 0.1494 0.1495 0.3642 0.026 Uiso 1 1 calc R . .
C49 C 0.13478(13) 0.1795(4) 0.46110(19) 0.0243(8) Uani 1 1 d . . .
H49 H 0.1314 0.0893 0.4724 0.029 Uiso 1 1 calc R . .
C50 C 0.12895(13) 0.2764(4) 0.50829(19) 0.0249(8) Uani 1 1 d . . .
H50 H 0.1216 0.2521 0.5521 0.030 Uiso 1 1 calc R . .
C51 C 0.13368(13) 0.4089(4) 0.49246(19) 0.0220(8) Uani 1 1 d . . .
H51 H 0.1291 0.4744 0.5251 0.026 Uiso 1 1 calc R . .
C52 C 0.14509(12) 0.4449(4) 0.42891(18) 0.0183(7) Uani 1 1 d . . .
H52 H 0.1489 0.5352 0.4181 0.022 Uiso 1 1 calc R . .
C53 C 0.19486(11) 0.5331(3) 0.28942(18) 0.0175(7) Uani 1 1 d . . .
C54 C 0.22588(12) 0.5664(4) 0.3396(2) 0.0218(8) Uani 1 1 d . . .
H54 H 0.2267 0.5176 0.3797 0.026 Uiso 1 1 calc R . .
C55 C 0.25540(13) 0.6702(4) 0.3312(2) 0.0270(9) Uani 1 1 d . . .
H55 H 0.2761 0.6934 0.3658 0.032 Uiso 1 1 calc R . .
C56 C 0.25474(14) 0.7405(4) 0.2723(2) 0.0301(10) Uani 1 1 d . . .
H56 H 0.2753 0.8110 0.2664 0.036 Uiso 1 1 calc R . .
C57 C 0.22425(14) 0.7084(4) 0.2223(2) 0.0267(9) Uani 1 1 d . . .
H57 H 0.2235 0.7581 0.1825 0.032 Uiso 1 1 calc R . .
C58 C 0.19470(12) 0.6039(4) 0.22984(19) 0.0189(7) Uani 1 1 d . . .
H58 H 0.1744 0.5805 0.1947 0.023 Uiso 1 1 calc R . .
C61 C 0.03503(12) 0.4829(4) 0.33008(18) 0.0180(7) Uani 1 1 d . . .
C62 C 0.03190(12) 0.3542(4) 0.35411(19) 0.0204(8) Uani 1 1 d . . .
H62 H 0.0501 0.2865 0.3364 0.024 Uiso 1 1 calc R . .
C63 C 0.00190(13) 0.3261(4) 0.40412(19) 0.0251(8) Uani 1 1 d . . .
H63 H -0.0006 0.2386 0.4202 0.030 Uiso 1 1 calc R . .
C64 C -0.02413(14) 0.4245(5) 0.4305(2) 0.0291(9) Uani 1 1 d . . .
H64 H -0.0445 0.4045 0.4646 0.035 Uiso 1 1 calc R . .
C65 C -0.02069(14) 0.5522(4) 0.4075(2) 0.0269(9) Uani 1 1 d . . .
H65 H -0.0387 0.6194 0.4260 0.032 Uiso 1 1 calc R . .
C66 C 0.00901(13) 0.5831(4) 0.3575(2) 0.0242(8) Uani 1 1 d . . .
H66 H 0.0116 0.6711 0.3421 0.029 Uiso 1 1 calc R . .
C67 C 0.03590(12) 0.4853(3) 0.18693(17) 0.0160(7) Uani 1 1 d . . .
C68 C 0.05620(13) 0.4409(4) 0.13041(19) 0.0224(8) Uani 1 1 d . . .
H68 H 0.0880 0.4297 0.1299 0.027 Uiso 1 1 calc R . .
C69 C 0.02988(14) 0.4124(4) 0.0739(2) 0.0265(9) Uani 1 1 d . . .
H69 H 0.0438 0.3811 0.0351 0.032 Uiso 1 1 calc R . .
C70 C -0.01626(14) 0.4298(4) 0.0745(2) 0.0262(9) Uani 1 1 d . . .
H70 H -0.0343 0.4084 0.0365 0.031 Uiso 1 1 calc R . .
C71 C -0.03612(13) 0.4789(4) 0.1309(2) 0.0286(9) Uani 1 1 d . . .
H71 H -0.0677 0.4937 0.1309 0.034 Uiso 1 1 calc R . .
C72 C -0.01038(12) 0.5063(4) 0.18714(19) 0.0217(8) Uani 1 1 d . . .
H72 H -0.0242 0.5393 0.2257 0.026 Uiso 1 1 calc R . .
C73 C 0.08879(12) 0.6811(3) 0.26314(18) 0.0157(7) Uani 1 1 d . . .
C74 C 0.09200(12) 0.7526(4) 0.20413(19) 0.0211(8) Uani 1 1 d . . .
H74 H 0.0786 0.7201 0.1643 0.025 Uiso 1 1 calc R . .
C75 C 0.11520(13) 0.8723(4) 0.2046(2) 0.0243(8) Uani 1 1 d . . .
H75 H 0.1167 0.9228 0.1651 0.029 Uiso 1 1 calc R . .
C76 C 0.13587(13) 0.9175(4) 0.2620(2) 0.0244(8) Uani 1 1 d . . .
H76 H 0.1525 0.9973 0.2614 0.029 Uiso 1 1 calc R . .
C77 C 0.13264(12) 0.8477(4) 0.3206(2) 0.0210(8) Uani 1 1 d . . .
H77 H 0.1470 0.8797 0.3598 0.025 Uiso 1 1 calc R . .
C78 C 0.10834(12) 0.7309(4) 0.32183(19) 0.0198(8) Uani 1 1 d . . .
H78 H 0.1050 0.6849 0.3623 0.024 Uiso 1 1 calc R . .
N41 N 0.11134(10) 0.4116(3) 0.25563(14) 0.0159(6) Uani 1 1 d . . .
P41 P 0.15782(3) 0.39312(9) 0.29476(4) 0.01339(17) Uani 1 1 d . . .
P42 P 0.07035(3) 0.51324(9) 0.26050(4) 0.01424(18) Uani 1 1 d . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
C1 C6 1.383(5) . ?
C1 C2 1.403(5) . ?
C1 P1 1.805(4) . ?
C2 C3 1.394(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.372(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.384(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.397(5) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C12 1.398(5) . ?
C7 C8 1.402(5) . ?
C7 P1 1.795(4) . ?
C8 C9 1.387(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.394(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.385(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.394(6) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C18 1.379(5) . ?
C13 C14 1.395(5) . ?
C13 P1 1.798(4) . ?
C14 C15 1.387(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.385(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.381(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.394(5) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C21 C26 1.388(5) . ?
C21 C22 1.411(5) . ?
C21 P2 1.797(4) . ?
C22 C23 1.392(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.375(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.370(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.389(6) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28 1.395(5) . ?
C27 C32 1.404(5) . ?
C27 P2 1.804(4) . ?
C28 C29 1.396(6) . ?
C28 H28 0.9500 . ?
C29 C30 1.378(6) . ?
C29 H29 0.9500 . ?
C30 C31 1.374(6) . ?
C30 H30 0.9500 . ?
C31 C32 1.386(6) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C34 1.388(5) . ?
C33 C38 1.408(5) . ?
C33 P2 1.797(4) . ?
C34 C35 1.395(5) . ?
C34 H34 0.9500 . ?
C35 C36 1.382(6) . ?
C35 H35 0.9500 . ?
C36 C37 1.387(6) . ?
C36 H36 0.9500 . ?
C37 C38 1.392(5) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
N1 P1 1.579(3) . ?
N1 P2 1.587(3) . ?
C41 C42 1.397(5) . ?
C41 C46 1.405(5) . ?
C41 P41 1.793(4) . ?
C42 C43 1.393(5) . ?
C42 H42 0.9500 . ?
C43 C44 1.385(6) . ?
C43 H43 0.9500 . ?
C44 C45 1.387(6) . ?
C44 H44 0.9500 . ?
C45 C46 1.391(5) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C47 C48 1.395(5) . ?
C47 C52 1.408(5) . ?
C47 P41 1.804(4) . ?
C48 C49 1.393(5) . ?
C48 H48 0.9500 . ?
C49 C50 1.385(6) . ?
C49 H49 0.9500 . ?
C50 C51 1.391(5) . ?
C50 H50 0.9500 . ?
C51 C52 1.385(5) . ?
C51 H51 0.9500 . ?
C52 H52 0.9500 . ?
C53 C54 1.396(5) . ?
C53 C58 1.403(5) . ?
C53 P41 1.802(4) . ?
C54 C55 1.384(5) . ?
C54 H54 0.9500 . ?
C55 C56 1.388(6) . ?
C55 H55 0.9500 . ?
C56 C57 1.380(6) . ?
C56 H56 0.9500 . ?
C57 C58 1.387(5) . ?
C57 H57 0.9500 . ?
C58 H58 0.9500 . ?
C61 C62 1.398(5) . ?
C61 C66 1.400(5) . ?
C61 P42 1.800(4) . ?
C62 C63 1.392(5) . ?
C62 H62 0.9500 . ?
C63 C64 1.378(6) . ?
C63 H63 0.9500 . ?
C64 C65 1.383(6) . ?
C64 H64 0.9500 . ?
C65 C66 1.393(5) . ?
C65 H65 0.9500 . ?
C66 H66 0.9500 . ?
C67 C68 1.380(5) . ?
C67 C72 1.390(5) . ?
C67 P42 1.807(4) . ?
C68 C69 1.398(5) . ?
C68 H68 0.9500 . ?
C69 C70 1.381(6) . ?
C69 H69 0.9500 . ?
C70 C71 1.388(6) . ?
C70 H70 0.9500 . ?
C71 C72 1.383(6) . ?
C71 H71 0.9500 . ?
C72 H72 0.9500 . ?
C73 C74 1.402(5) . ?
C73 C78 1.403(5) . ?
C73 P42 1.792(4) . ?
C74 C75 1.397(5) . ?
C74 H74 0.9500 . ?
C75 C76 1.378(6) . ?
C75 H75 0.9500 . ?
C76 C77 1.385(6) . ?
C76 H76 0.9500 . ?
C77 C78 1.389(5) . ?
C77 H77 0.9500 . ?
C78 H78 0.9500 . ?
N41 P41 1.585(3) . ?
N41 P42 1.601(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
C6 C1 C2 120.7(3) . . ?
C6 C1 P1 119.2(3) . . ?
C2 C1 P1 119.6(3) . . ?
C3 C2 C1 119.2(4) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C4 C3 C2 120.1(4) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 120.7(4) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C4 C5 C6 120.2(4) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C1 C6 C5 119.1(4) . . ?
C1 C6 H6 120.5 . . ?
C5 C6 H6 120.5 . . ?
C12 C7 C8 119.4(3) . . ?
C12 C7 P1 122.7(3) . . ?
C8 C7 P1 117.9(3) . . ?
C9 C8 C7 120.1(4) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C8 C9 C10 120.1(4) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
C11 C10 C9 120.1(4) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C10 C11 C12 120.2(4) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C11 C12 C7 120.1(4) . . ?
C11 C12 H12 120.0 . . ?
C7 C12 H12 120.0 . . ?
C18 C13 C14 119.8(3) . . ?
C18 C13 P1 121.0(3) . . ?
C14 C13 P1 119.0(3) . . ?
C15 C14 C13 119.8(4) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C16 C15 C14 120.3(4) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C17 C16 C15 119.8(4) . . ?
C17 C16 H16 120.1 . . ?
C15 C16 H16 120.1 . . ?
C16 C17 C18 120.0(4) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C13 C18 C17 120.2(4) . . ?
C13 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
C26 C21 C22 118.7(4) . . ?
C26 C21 P2 123.0(3) . . ?
C22 C21 P2 118.0(3) . . ?
C23 C22 C21 120.1(4) . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C24 C23 C22 120.0(4) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C25 C24 C23 120.2(4) . . ?
C25 C24 H24 119.9 . . ?
C23 C24 H24 119.9 . . ?
C24 C25 C26 120.8(4) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 H25 119.6 . . ?
C21 C26 C25 120.1(4) . . ?
C21 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
C28 C27 C32 119.7(4) . . ?
C28 C27 P2 118.2(3) . . ?
C32 C27 P2 122.1(3) . . ?
C27 C28 C29 119.6(4) . . ?
C27 C28 H28 120.2 . . ?
C29 C28 H28 120.2 . . ?
C30 C29 C28 120.3(4) . . ?
C30 C29 H29 119.9 . . ?
C28 C29 H29 119.9 . . ?
C31 C30 C29 120.2(4) . . ?
C31 C30 H30 119.9 . . ?
C29 C30 H30 119.9 . . ?
C30 C31 C32 121.0(4) . . ?
C30 C31 H31 119.5 . . ?
C32 C31 H31 119.5 . . ?
C31 C32 C27 119.3(4) . . ?
C31 C32 H32 120.4 . . ?
C27 C32 H32 120.4 . . ?
C34 C33 C38 120.0(3) . . ?
C34 C33 P2 119.6(3) . . ?
C38 C33 P2 120.4(3) . . ?
C33 C34 C35 119.7(4) . . ?
C33 C34 H34 120.1 . . ?
C35 C34 H34 120.1 . . ?
C36 C35 C34 120.4(4) . . ?
C36 C35 H35 119.8 . . ?
C34 C35 H35 119.8 . . ?
C35 C36 C37 120.2(4) . . ?
C35 C36 H36 119.9 . . ?
C37 C36 H36 119.9 . . ?
C36 C37 C38 120.2(4) . . ?
C36 C37 H37 119.9 . . ?
C38 C37 H37 119.9 . . ?
C37 C38 C33 119.4(4) . . ?
C37 C38 H38 120.3 . . ?
C33 C38 H38 120.3 . . ?
P1 N1 P2 137.6(2) . . ?
N1 P1 C7 115.30(16) . . ?
N1 P1 C13 110.04(17) . . ?
C7 P1 C13 110.25(17) . . ?
N1 P1 C1 110.25(17) . . ?
C7 P1 C1 106.47(17) . . ?
C13 P1 C1 103.87(17) . . ?
N1 P2 C33 106.68(16) . . ?
N1 P2 C21 114.89(17) . . ?
C33 P2 C21 106.23(17) . . ?
N1 P2 C27 111.18(17) . . ?
C33 P2 C27 108.79(16) . . ?
C21 P2 C27 108.80(17) . . ?
C42 C41 C46 119.2(3) . . ?
C42 C41 P41 120.1(3) . . ?
C46 C41 P41 120.3(3) . . ?
C43 C42 C41 119.9(3) . . ?
C43 C42 H42 120.0 . . ?
C41 C42 H42 120.0 . . ?
C44 C43 C42 120.3(4) . . ?
C44 C43 H43 119.9 . . ?
C42 C43 H43 119.9 . . ?
C43 C44 C45 120.5(4) . . ?
C43 C44 H44 119.8 . . ?
C45 C44 H44 119.8 . . ?
C44 C45 C46 119.7(3) . . ?
C44 C45 H45 120.2 . . ?
C46 C45 H45 120.2 . . ?
C45 C46 C41 120.4(3) . . ?
C45 C46 H46 119.8 . . ?
C41 C46 H46 119.8 . . ?
C48 C47 C52 119.3(3) . . ?
C48 C47 P41 119.6(3) . . ?
C52 C47 P41 120.5(3) . . ?
C49 C48 C47 120.6(4) . . ?
C49 C48 H48 119.7 . . ?
C47 C48 H48 119.7 . . ?
C50 C49 C48 119.3(4) . . ?
C50 C49 H49 120.3 . . ?
C48 C49 H49 120.3 . . ?
C49 C50 C51 121.0(4) . . ?
C49 C50 H50 119.5 . . ?
C51 C50 H50 119.5 . . ?
C52 C51 C50 119.8(4) . . ?
C52 C51 H51 120.1 . . ?
C50 C51 H51 120.1 . . ?
C51 C52 C47 120.0(3) . . ?
C51 C52 H52 120.0 . . ?
C47 C52 H52 120.0 . . ?
C54 C53 C58 119.2(3) . . ?
C54 C53 P41 122.7(3) . . ?
C58 C53 P41 117.8(3) . . ?
C55 C54 C53 120.3(4) . . ?
C55 C54 H54 119.9 . . ?
C53 C54 H54 119.9 . . ?
C54 C55 C56 120.1(4) . . ?
C54 C55 H55 120.0 . . ?
C56 C55 H55 120.0 . . ?
C57 C56 C55 120.2(4) . . ?
C57 C56 H56 119.9 . . ?
C55 C56 H56 119.9 . . ?
C56 C57 C58 120.4(4) . . ?
C56 C57 H57 119.8 . . ?
C58 C57 H57 119.8 . . ?
C57 C58 C53 119.8(4) . . ?
C57 C58 H58 120.1 . . ?
C53 C58 H58 120.1 . . ?
C62 C61 C66 120.1(3) . . ?
C62 C61 P42 118.4(3) . . ?
C66 C61 P42 121.4(3) . . ?
C63 C62 C61 119.5(4) . . ?
C63 C62 H62 120.2 . . ?
C61 C62 H62 120.2 . . ?
C64 C63 C62 120.3(4) . . ?
C64 C63 H63 119.8 . . ?
C62 C63 H63 119.8 . . ?
C63 C64 C65 120.3(4) . . ?
C63 C64 H64 119.8 . . ?
C65 C64 H64 119.8 . . ?
C64 C65 C66 120.6(4) . . ?
C64 C65 H65 119.7 . . ?
C66 C65 H65 119.7 . . ?
C65 C66 C61 119.2(4) . . ?
C65 C66 H66 120.4 . . ?
C61 C66 H66 120.4 . . ?
C68 C67 C72 120.2(3) . . ?
C68 C67 P42 118.9(3) . . ?
C72 C67 P42 120.9(3) . . ?
C67 C68 C69 119.8(4) . . ?
C67 C68 H68 120.1 . . ?
C69 C68 H68 120.1 . . ?
C70 C69 C68 120.1(4) . . ?
C70 C69 H69 119.9 . . ?
C68 C69 H69 119.9 . . ?
C69 C70 C71 119.5(4) . . ?
C69 C70 H70 120.2 . . ?
C71 C70 H70 120.2 . . ?
C72 C71 C70 120.7(4) . . ?
C72 C71 H71 119.7 . . ?
C70 C71 H71 119.7 . . ?
C71 C72 C67 119.6(4) . . ?
C71 C72 H72 120.2 . . ?
C67 C72 H72 120.2 . . ?
C74 C73 C78 119.8(3) . . ?
C74 C73 P42 119.7(3) . . ?
C78 C73 P42 119.2(3) . . ?
C75 C74 C73 119.3(4) . . ?
C75 C74 H74 120.4 . . ?
C73 C74 H74 120.4 . . ?
C76 C75 C74 120.3(4) . . ?
C76 C75 H75 119.8 . . ?
C74 C75 H75 119.8 . . ?
C75 C76 C77 120.7(4) . . ?
C75 C76 H76 119.6 . . ?
C77 C76 H76 119.6 . . ?
C76 C77 C78 120.0(4) . . ?
C76 C77 H77 120.0 . . ?
C78 C77 H77 120.0 . . ?
C77 C78 C73 119.8(3) . . ?
C77 C78 H78 120.1 . . ?
C73 C78 H78 120.1 . . ?
P41 N41 P42 134.4(2) . . ?
N41 P41 C41 106.87(16) . . ?
N41 P41 C53 113.68(16) . . ?
C41 P41 C53 104.59(16) . . ?
N41 P41 C47 113.20(16) . . ?
C41 P41 C47 108.04(16) . . ?
C53 P41 C47 109.91(17) . . ?
N41 P42 C73 112.57(16) . . ?
N41 P42 C61 113.26(16) . . ?
C73 P42 C61 108.84(17) . . ?
N41 P42 C67 105.34(16) . . ?
C73 P42 C67 109.91(16) . . ?
C61 P42 C67 106.69(17) . . ?
 
_diffrn_measured_fraction_theta_max    0.995
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.995
_refine_diff_density_max    0.637
_refine_diff_density_min   -0.593
_refine_diff_density_rms    0.116
