# Electronic Supplementary Material (ESI) for Chemical Science
# This journal is © The Royal Society of Chemistry 2013
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
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# fide research purposes only. It may contain copyright material
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data_ch121_[PN(C6H10)]4
_audit_creation_method SHELXL-97
#==============================================================================
# CHEMICAL DATA
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C24 H40 N4 P4, 2(C H2 Cl2)'
_chemical_formula_sum 'C26 H44 Cl4 N4 P4'
_chemical_formula_weight 678.33
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
#==============================================================================
# CRYSTAL DATA
_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M 'P -1'
_symmetry_space_group_name_Hall '-P 1'
_symmetry_Int_Tables_number 2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 11.5705(5)
_cell_length_b 12.2221(3)
_cell_length_c 13.6923(3)
_cell_angle_alpha 111.4080(10)
_cell_angle_beta 105.6400(10)
_cell_angle_gamma 97.4310(10)
_cell_volume 1679.02(9)
_cell_formula_units_Z 2
_cell_measurement_temperature 173(2)
_cell_measurement_reflns_used 9574
_cell_measurement_theta_min 5.544
_cell_measurement_theta_max 58.578
_exptl_crystal_description block
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.16
_exptl_crystal_size_min 0.10
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.342
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 712
_exptl_absorpt_coefficient_mu 0.567
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.8951
_exptl_absorpt_correction_T_max 0.9455
_exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)'
#==============================================================================
# EXPERIMENTAL DATA
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 173(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker Apex Kappa II-CCD-diffractometer'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 46693
_diffrn_reflns_av_R_equivalents 0.0507
_diffrn_reflns_av_sigmaI/netI 0.0422
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_theta_min 1.85
_diffrn_reflns_theta_max 29.00
_reflns_number_total 8903
_reflns_number_gt 6414
_reflns_threshold_expression >2\s(I)
_computing_data_collection 'Bruker Apex V7.51A'
_computing_cell_refinement 'Bruker Apex V7.51A'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material SHELXL-97
#==============================================================================
# REFINEMENT DATA
_refine_special_details
;
All H atoms
were positioned geometrically and refined using a riding model, with C---H =
0.98 (methyl groups), 0.99\%A (methylene groups), 1.00\%A (methine groups) or
0.95 \%A (aryl CH) and with U~iso~(H) = 1.5 times U~eq~(C)
(methyl groups) or with U~iso~(H) = 1.2 times U~eq~(C)
(methylene groups, aryl CH, methine groups). Torsion angles of all methyl
groups were allowed to refine.
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0563P)^2^+0.6250P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 8903
_refine_ls_number_parameters 380
_refine_ls_number_restraints 3
_refine_ls_R_factor_all 0.0687
_refine_ls_R_factor_gt 0.0427
_refine_ls_wR_factor_ref 0.1184
_refine_ls_wR_factor_gt 0.1035
_refine_ls_goodness_of_fit_ref 1.014
_refine_ls_restrained_S_all 1.014
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
#==============================================================================
# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_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 0.15782(4) 0.42057(4) 0.40488(4) 0.02551(11) Uani 1 1 d . . .
P2 P -0.03155(4) 0.24571(4) 0.20753(4) 0.02541(11) Uani 1 1 d . . .
P3 P 0.14974(5) 0.16567(4) 0.11541(4) 0.02618(11) Uani 1 1 d . . .
P4 P 0.33956(4) 0.34031(4) 0.31260(4) 0.02632(11) Uani 1 1 d . . .
N1 N 0.02540(14) 0.39752(14) 0.29828(13) 0.0254(3) Uani 1 1 d . . .
N2 N 0.01935(14) 0.22046(14) 0.09679(13) 0.0258(3) Uani 1 1 d . . .
N3 N 0.27785(14) 0.28488(14) 0.16926(13) 0.0264(3) Uani 1 1 d . . .
N4 N 0.28505(14) 0.46287(14) 0.37114(13) 0.0257(3) Uani 1 1 d . . .
C1 C 0.15513(18) 0.56707(18) 0.50669(16) 0.0301(4) Uani 1 1 d . . .
H1A H 0.1105 0.5500 0.5540 0.036 Uiso 1 1 calc R . .
H1B H 0.2419 0.6106 0.5559 0.036 Uiso 1 1 calc R . .
C2 C 0.09822(18) 0.65323(17) 0.46527(16) 0.0297(4) Uani 1 1 d . . .
C3 C 0.02647(17) 0.62079(17) 0.35989(16) 0.0281(4) Uani 1 1 d . . .
C4 C -0.00993(19) 0.49496(17) 0.26763(16) 0.0297(4) Uani 1 1 d . . .
H4A H -0.1012 0.4717 0.2312 0.036 Uiso 1 1 calc R . .
H4B H 0.0268 0.4987 0.2111 0.036 Uiso 1 1 calc R . .
C5 C 0.1298(2) 0.78007(19) 0.55525(18) 0.0412(5) Uani 1 1 d . . .
H5A H 0.0951 0.8329 0.5225 0.062 Uiso 1 1 calc R . .
H5B H 0.2201 0.8113 0.5894 0.062 Uiso 1 1 calc R . .
H5C H 0.0945 0.7785 0.6124 0.062 Uiso 1 1 calc R . .
C6 C -0.0299(2) 0.70643(19) 0.31802(19) 0.0369(5) Uani 1 1 d . . .
H6A H -0.1148 0.6993 0.3192 0.055 Uiso 1 1 calc R . .
H6B H -0.0314 0.6858 0.2414 0.055 Uiso 1 1 calc R . .
H6C H 0.0198 0.7900 0.3661 0.055 Uiso 1 1 calc R . .
C7 C -0.19351(18) 0.23940(18) 0.13793(17) 0.0316(4) Uani 1 1 d . . .
H7A H -0.2427 0.1547 0.1094 0.038 Uiso 1 1 calc R . .
H7B H -0.2235 0.2906 0.1957 0.038 Uiso 1 1 calc R . .
C8 C -0.22384(18) 0.27761(18) 0.04294(17) 0.0321(4) Uani 1 1 d . . .
C9 C -0.14374(19) 0.29729(18) -0.00662(16) 0.0323(4) Uani 1 1 d . . .
C10 C -0.01526(18) 0.27735(18) 0.01912(16) 0.0304(4) Uani 1 1 d . . .
H10A H -0.0062 0.2263 -0.0522 0.037 Uiso 1 1 calc R . .
H10B H 0.0451 0.3571 0.0502 0.037 Uiso 1 1 calc R . .
C11 C -0.3540(2) 0.2940(2) 0.0119(2) 0.0458(6) Uani 1 1 d . . .
H11A H -0.3729 0.3085 -0.0559 0.069 Uiso 1 1 calc R . .
H11B H -0.3603 0.3636 0.0731 0.069 Uiso 1 1 calc R . .
H11C H -0.4132 0.2205 -0.0018 0.069 Uiso 1 1 calc R . .
C12 C -0.1697(2) 0.3461(2) -0.09490(19) 0.0447(5) Uani 1 1 d . . .
H12A H -0.2498 0.3668 -0.1043 0.067 Uiso 1 1 calc R . .
H12B H -0.1721 0.2842 -0.1658 0.067 Uiso 1 1 calc R . .
H12C H -0.1039 0.4189 -0.0718 0.067 Uiso 1 1 calc R . .
C13 C 0.1510(2) 0.09396(17) -0.02717(17) 0.0329(4) Uani 1 1 d . . .
H13A H 0.1924 0.0273 -0.0311 0.040 Uiso 1 1 calc R . .
H13B H 0.0636 0.0557 -0.0771 0.040 Uiso 1 1 calc R . .
C14 C 0.21049(18) 0.16820(18) -0.07658(16) 0.0304(4) Uani 1 1 d . . .
C15 C 0.27678(18) 0.28274(18) -0.01707(16) 0.0297(4) Uani 1 1 d . . .
C16 C 0.30745(19) 0.35360(17) 0.10665(16) 0.0308(4) Uani 1 1 d . . .
H16A H 0.3974 0.3937 0.1401 0.037 Uiso 1 1 calc R . .
H16B H 0.2629 0.4186 0.1176 0.037 Uiso 1 1 calc R . .
C17 C 0.1883(2) 0.0968(2) -0.19884(18) 0.0430(5) Uani 1 1 d . . .
H17A H 0.1020 0.0860 -0.2426 0.064 Uiso 1 1 calc R . .
H17B H 0.2048 0.0171 -0.2108 0.064 Uiso 1 1 calc R . .
H17C H 0.2439 0.1409 -0.2226 0.064 Uiso 1 1 calc R . .
C18 C 0.3317(2) 0.3592(2) -0.06674(18) 0.0406(5) Uani 1 1 d . . .
H18A H 0.3350 0.3061 -0.1390 0.061 Uiso 1 1 calc R . .
H18B H 0.4158 0.4068 -0.0162 0.061 Uiso 1 1 calc R . .
H18C H 0.2799 0.4142 -0.0772 0.061 Uiso 1 1 calc R . .
C19 C 0.49804(18) 0.42130(19) 0.34119(17) 0.0324(4) Uani 1 1 d . . .
H19A H 0.5497 0.4298 0.4154 0.039 Uiso 1 1 calc R . .
H19B H 0.5297 0.3688 0.2856 0.039 Uiso 1 1 calc R . .
C20 C 0.52019(18) 0.54568(19) 0.34049(16) 0.0320(4) Uani 1 1 d . . .
C21 C 0.44002(18) 0.61448(19) 0.35131(16) 0.0321(4) Uani 1 1 d . . .
C22 C 0.31571(18) 0.57849(18) 0.36162(18) 0.0318(4) Uani 1 1 d . . .
H22A H 0.3110 0.6442 0.4281 0.038 Uiso 1 1 calc R . .
H22B H 0.2506 0.5747 0.2956 0.038 Uiso 1 1 calc R . .
C23 C 0.6424(2) 0.5849(2) 0.3282(2) 0.0432(5) Uani 1 1 d . . .
H23A H 0.6476 0.6622 0.3211 0.065 Uiso 1 1 calc R . .
H23B H 0.6486 0.5229 0.2613 0.065 Uiso 1 1 calc R . .
H23C H 0.7106 0.5951 0.3941 0.065 Uiso 1 1 calc R . .
C24 C 0.4632(2) 0.7403(2) 0.3538(2) 0.0462(6) Uani 1 1 d . . .
H24A H 0.5344 0.7947 0.4203 0.069 Uiso 1 1 calc R . .
H24B H 0.3896 0.7713 0.3561 0.069 Uiso 1 1 calc R . .
H24C H 0.4808 0.7365 0.2867 0.069 Uiso 1 1 calc R . .
C25 C 0.1808(3) 1.0910(2) 0.3820(2) 0.0532(6) Uani 1 1 d . . .
H25A H 0.2600 1.1493 0.4015 0.064 Uiso 0.918(2) 1 calc PR A 1
H25B H 0.1121 1.1220 0.3499 0.064 Uiso 0.918(2) 1 calc PR A 1
H25C H 0.2418 1.1688 0.4065 0.064 Uiso 0.082(2) 1 d PR A 2
H25D H 0.1077 1.0828 0.3197 0.064 Uiso 0.082(2) 1 d PR A 2
Cl1A Cl 0.17582(11) 0.94863(7) 0.28220(9) 0.0651(3) Uani 0.918(2) 1 d P A 1
Cl2A Cl 0.16786(13) 1.08051(13) 0.50318(11) 0.0708(4) Uani 0.918(2) 1 d P A 1
Cl1B Cl 0.2440(13) 0.9703(9) 0.3399(11) 0.0651(3) Uani 0.082(2) 1 d P A 2
Cl2B Cl 0.1246(18) 1.0670(18) 0.4799(16) 0.0708(4) Uani 0.082(2) 1 d P A 2
C26A C 0.4257(8) 0.038(5) 0.213(2) 0.0698(10) Uani 0.579(16) 1 d PD B 1
H26A H 0.3623 -0.0385 0.1607 0.084 Uiso 0.579(16) 1 calc PR B 1
H26B H 0.3823 0.0991 0.2458 0.084 Uiso 0.579(16) 1 calc PR B 1
Cl3A Cl 0.5038(8) 0.0891(9) 0.1400(7) 0.105(2) Uani 0.579(16) 1 d PD B 1
Cl4A Cl 0.5248(4) 0.0139(9) 0.3192(8) 0.135(2) Uani 0.579(16) 1 d PD B 1
C26B C 0.4183(11) 0.037(7) 0.215(3) 0.0698(10) Uani 0.421(16) 1 d PD B 2
H26C H 0.3730 -0.0494 0.1825 0.084 Uiso 0.421(16) 1 calc PR B 2
H26D H 0.3561 0.0857 0.2178 0.084 Uiso 0.421(16) 1 calc PR B 2
Cl3B Cl 0.4946(12) 0.0588(12) 0.1282(10) 0.109(3) Uani 0.421(16) 1 d PD B 2
Cl4B Cl 0.5146(4) 0.0768(12) 0.3510(4) 0.114(2) Uani 0.421(16) 1 d PD B 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.0264(2) 0.0279(2) 0.0218(2) 0.01052(19) 0.00819(19) 0.00542(19)
P2 0.0254(2) 0.0235(2) 0.0262(2) 0.01019(19) 0.00916(19) 0.00261(18)
P3 0.0282(2) 0.0213(2) 0.0277(2) 0.00930(19) 0.0097(2) 0.00467(18)
P4 0.0250(2) 0.0284(2) 0.0251(2) 0.0114(2) 0.00744(19) 0.00701(19)
N1 0.0258(8) 0.0243(8) 0.0236(7) 0.0092(6) 0.0074(6) 0.0037(6)
N2 0.0267(8) 0.0243(8) 0.0239(8) 0.0089(6) 0.0081(6) 0.0034(6)
N3 0.0268(8) 0.0251(8) 0.0254(8) 0.0102(6) 0.0081(6) 0.0032(6)
N4 0.0254(8) 0.0263(8) 0.0241(8) 0.0095(6) 0.0089(6) 0.0050(6)
C1 0.0276(10) 0.0358(10) 0.0224(9) 0.0080(8) 0.0087(8) 0.0053(8)
C2 0.0302(10) 0.0275(9) 0.0284(10) 0.0077(8) 0.0129(8) 0.0034(8)
C3 0.0268(9) 0.0257(9) 0.0315(10) 0.0105(8) 0.0125(8) 0.0052(7)
C4 0.0326(10) 0.0259(9) 0.0282(10) 0.0112(8) 0.0071(8) 0.0072(8)
C5 0.0516(14) 0.0312(11) 0.0326(11) 0.0064(9) 0.0136(10) 0.0059(10)
C6 0.0407(12) 0.0302(10) 0.0395(12) 0.0153(9) 0.0129(9) 0.0078(9)
C7 0.0256(9) 0.0277(10) 0.0360(11) 0.0090(8) 0.0106(8) 0.0019(7)
C8 0.0286(10) 0.0256(9) 0.0302(10) 0.0045(8) 0.0036(8) 0.0042(8)
C9 0.0352(11) 0.0293(10) 0.0268(10) 0.0098(8) 0.0049(8) 0.0083(8)
C10 0.0331(10) 0.0322(10) 0.0261(9) 0.0136(8) 0.0094(8) 0.0063(8)
C11 0.0331(11) 0.0483(14) 0.0521(14) 0.0190(12) 0.0102(10) 0.0141(10)
C12 0.0519(14) 0.0493(14) 0.0378(12) 0.0225(11) 0.0125(11) 0.0223(11)
C13 0.0380(11) 0.0225(9) 0.0318(10) 0.0041(8) 0.0136(9) 0.0052(8)
C14 0.0296(10) 0.0345(10) 0.0262(9) 0.0097(8) 0.0114(8) 0.0101(8)
C15 0.0273(9) 0.0345(10) 0.0272(9) 0.0140(8) 0.0087(8) 0.0065(8)
C16 0.0339(10) 0.0279(10) 0.0266(9) 0.0109(8) 0.0087(8) -0.0001(8)
C17 0.0510(14) 0.0418(12) 0.0291(11) 0.0073(9) 0.0154(10) 0.0078(10)
C18 0.0379(12) 0.0497(13) 0.0338(11) 0.0209(10) 0.0111(9) 0.0025(10)
C19 0.0244(9) 0.0398(11) 0.0294(10) 0.0120(9) 0.0076(8) 0.0079(8)
C20 0.0262(9) 0.0388(11) 0.0237(9) 0.0097(8) 0.0059(8) 0.0003(8)
C21 0.0292(10) 0.0337(10) 0.0263(10) 0.0106(8) 0.0055(8) -0.0008(8)
C22 0.0308(10) 0.0282(10) 0.0352(11) 0.0125(8) 0.0120(8) 0.0048(8)
C23 0.0311(11) 0.0561(14) 0.0423(13) 0.0229(11) 0.0129(10) 0.0029(10)
C24 0.0404(12) 0.0389(12) 0.0561(15) 0.0217(11) 0.0136(11) 0.0002(10)
C25 0.0684(17) 0.0372(13) 0.0617(16) 0.0243(12) 0.0296(14) 0.0122(12)
Cl1A 0.0804(7) 0.0485(4) 0.0629(6) 0.0150(4) 0.0353(6) 0.0068(4)
Cl2A 0.0986(10) 0.0521(5) 0.0598(7) 0.0182(5) 0.0398(7) 0.0015(6)
Cl1B 0.0804(7) 0.0485(4) 0.0629(6) 0.0150(4) 0.0353(6) 0.0068(4)
Cl2B 0.0986(10) 0.0521(5) 0.0598(7) 0.0182(5) 0.0398(7) 0.0015(6)
C26A 0.067(2) 0.0593(19) 0.093(3) 0.0321(19) 0.040(3) 0.022(3)
Cl3A 0.127(4) 0.092(4) 0.160(4) 0.065(3) 0.115(4) 0.050(3)
Cl4A 0.0864(16) 0.151(4) 0.215(4) 0.139(4) 0.037(2) 0.029(2)
C26B 0.067(2) 0.0593(19) 0.093(3) 0.0321(19) 0.040(3) 0.022(3)
Cl3B 0.120(4) 0.084(5) 0.134(4) 0.040(3) 0.078(3) 0.010(3)
Cl4B 0.0724(17) 0.146(5) 0.104(3) 0.055(3) -0.0056(17) 0.028(2)
#==============================================================================
# MOLECULAR GEOMETRY
_geom_special_details
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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 1.7146(16) . ?
P1 N4 1.7297(16) . ?
P1 C1 1.835(2) . ?
P2 N2 1.7111(16) . ?
P2 N1 1.7262(16) . ?
P2 C7 1.836(2) . ?
P3 N3 1.7122(16) . ?
P3 N2 1.7228(17) . ?
P3 C13 1.830(2) . ?
P4 N4 1.7101(16) . ?
P4 N3 1.7232(16) . ?
P4 C19 1.832(2) . ?
N1 C4 1.470(2) . ?
N2 C10 1.469(2) . ?
N3 C16 1.472(2) . ?
N4 C22 1.473(2) . ?
C1 C2 1.509(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.334(3) . ?
C2 C5 1.507(3) . ?
C3 C6 1.504(3) . ?
C3 C4 1.505(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.507(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.333(3) . ?
C8 C11 1.511(3) . ?
C9 C10 1.506(3) . ?
C9 C12 1.511(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.514(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.328(3) . ?
C14 C17 1.508(3) . ?
C15 C16 1.507(3) . ?
C15 C18 1.511(3) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.513(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.332(3) . ?
C20 C23 1.507(3) . ?
C21 C22 1.508(3) . ?
C21 C24 1.513(3) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 Cl1B 1.711(11) . ?
C25 Cl2B 1.74(2) . ?
C25 Cl2A 1.753(3) . ?
C25 Cl1A 1.759(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 H25C 0.9900 . ?
C25 H25D 0.9900 . ?
C26A Cl3A 1.733(8) . ?
C26A Cl4A 1.737(15) . ?
C26A H26A 0.9900 . ?
C26A H26B 0.9900 . ?
C26B Cl3B 1.734(9) . ?
C26B Cl4B 1.737(15) . ?
C26B H26C 0.9900 . ?
C26B H26D 0.9900 . ?
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 N4 108.77(8) . . ?
N1 P1 C1 98.72(8) . . ?
N4 P1 C1 101.29(8) . . ?
N2 P2 N1 108.65(8) . . ?
N2 P2 C7 98.58(9) . . ?
N1 P2 C7 101.44(8) . . ?
N3 P3 N2 108.49(8) . . ?
N3 P3 C13 98.79(8) . . ?
N2 P3 C13 102.46(9) . . ?
N4 P4 N3 109.07(8) . . ?
N4 P4 C19 98.59(9) . . ?
N3 P4 C19 101.79(9) . . ?
C4 N1 P1 123.24(12) . . ?
C4 N1 P2 122.71(12) . . ?
P1 N1 P2 111.10(9) . . ?
C10 N2 P2 122.85(13) . . ?
C10 N2 P3 122.94(13) . . ?
P2 N2 P3 110.96(9) . . ?
C16 N3 P3 123.14(12) . . ?
C16 N3 P4 123.02(12) . . ?
P3 N3 P4 111.39(9) . . ?
C22 N4 P4 123.60(13) . . ?
C22 N4 P1 122.77(13) . . ?
P4 N4 P1 111.06(9) . . ?
C2 C1 P1 119.17(13) . . ?
C2 C1 H1A 107.5 . . ?
P1 C1 H1A 107.5 . . ?
C2 C1 H1B 107.5 . . ?
P1 C1 H1B 107.5 . . ?
H1A C1 H1B 107.0 . . ?
C3 C2 C5 123.09(19) . . ?
C3 C2 C1 123.67(17) . . ?
C5 C2 C1 113.24(17) . . ?
C2 C3 C6 123.89(18) . . ?
C2 C3 C4 125.15(18) . . ?
C6 C3 C4 110.96(17) . . ?
N1 C4 C3 117.43(16) . . ?
N1 C4 H4A 107.9 . . ?
C3 C4 H4A 107.9 . . ?
N1 C4 H4B 107.9 . . ?
C3 C4 H4B 107.9 . . ?
H4A C4 H4B 107.2 . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 P2 119.17(14) . . ?
C8 C7 H7A 107.5 . . ?
P2 C7 H7A 107.5 . . ?
C8 C7 H7B 107.5 . . ?
P2 C7 H7B 107.5 . . ?
H7A C7 H7B 107.0 . . ?
C9 C8 C7 123.70(18) . . ?
C9 C8 C11 123.7(2) . . ?
C7 C8 C11 112.58(19) . . ?
C8 C9 C10 125.14(18) . . ?
C8 C9 C12 123.9(2) . . ?
C10 C9 C12 110.92(18) . . ?
N2 C10 C9 117.04(16) . . ?
N2 C10 H10A 108.0 . . ?
C9 C10 H10A 108.0 . . ?
N2 C10 H10B 108.0 . . ?
C9 C10 H10B 108.0 . . ?
H10A C10 H10B 107.3 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 P3 120.51(14) . . ?
C14 C13 H13A 107.2 . . ?
P3 C13 H13A 107.2 . . ?
C14 C13 H13B 107.2 . . ?
P3 C13 H13B 107.2 . . ?
H13A C13 H13B 106.8 . . ?
C15 C14 C17 124.41(19) . . ?
C15 C14 C13 123.05(18) . . ?
C17 C14 C13 112.53(17) . . ?
C14 C15 C16 125.53(18) . . ?
C14 C15 C18 123.39(19) . . ?
C16 C15 C18 111.09(17) . . ?
N3 C16 C15 116.88(16) . . ?
N3 C16 H16A 108.1 . . ?
C15 C16 H16A 108.1 . . ?
N3 C16 H16B 108.1 . . ?
C15 C16 H16B 108.1 . . ?
H16A C16 H16B 107.3 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 P4 118.96(14) . . ?
C20 C19 H19A 107.6 . . ?
P4 C19 H19A 107.6 . . ?
C20 C19 H19B 107.6 . . ?
P4 C19 H19B 107.6 . . ?
H19A C19 H19B 107.0 . . ?
C21 C20 C23 123.3(2) . . ?
C21 C20 C19 123.15(18) . . ?
C23 C20 C19 113.52(19) . . ?
C20 C21 C22 125.35(19) . . ?
C20 C21 C24 123.39(19) . . ?
C22 C21 C24 111.26(19) . . ?
N4 C22 C21 117.48(17) . . ?
N4 C22 H22A 107.9 . . ?
C21 C22 H22A 107.9 . . ?
N4 C22 H22B 107.9 . . ?
C21 C22 H22B 107.9 . . ?
H22A C22 H22B 107.2 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Cl1B C25 Cl2B 102.0(8) . . ?
Cl1B C25 Cl2A 97.3(4) . . ?
Cl2B C25 Cl2A 15.9(6) . . ?
Cl1B C25 Cl1A 29.3(5) . . ?
Cl2B C25 Cl1A 108.1(7) . . ?
Cl2A C25 Cl1A 111.12(14) . . ?
Cl1B C25 H25A 91.5 . . ?
Cl2B C25 H25A 123.9 . . ?
Cl2A C25 H25A 109.4 . . ?
Cl1A C25 H25A 109.4 . . ?
Cl1B C25 H25B 138.5 . . ?
Cl2B C25 H25B 96.8 . . ?
Cl2A C25 H25B 109.4 . . ?
Cl1A C25 H25B 109.4 . . ?
H25A C25 H25B 108.0 . . ?
Cl1B C25 H25C 111.1 . . ?
Cl2B C25 H25C 118.0 . . ?
Cl2A C25 H25C 106.9 . . ?
Cl1A C25 H25C 126.4 . . ?
H25A C25 H25C 19.7 . . ?
H25B C25 H25C 91.3 . . ?
Cl1B C25 H25D 109.8 . . ?
Cl2B C25 H25D 106.6 . . ?
Cl2A C25 H25D 122.3 . . ?
Cl1A C25 H25D 80.7 . . ?
H25A C25 H25D 119.3 . . ?
H25B C25 H25D 28.7 . . ?
H25C C25 H25D 108.9 . . ?
Cl3A C26A Cl4A 112.3(7) . . ?
Cl3A C26A H26A 109.1 . . ?
Cl4A C26A H26A 109.1 . . ?
Cl3A C26A H26B 109.1 . . ?
Cl4A C26A H26B 109.1 . . ?
H26A C26A H26B 107.9 . . ?
Cl3B C26B Cl4B 114.5(8) . . ?
Cl3B C26B H26C 108.6 . . ?
Cl4B C26B H26C 108.6 . . ?
Cl3B C26B H26D 108.6 . . ?
Cl4B C26B H26D 108.6 . . ?
H26C C26B H26D 107.6 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N4 P1 N1 C4 -64.94(16) . . . . ?
C1 P1 N1 C4 40.21(16) . . . . ?
N4 P1 N1 P2 96.07(10) . . . . ?
C1 P1 N1 P2 -158.78(9) . . . . ?
N2 P2 N1 C4 64.37(16) . . . . ?
C7 P2 N1 C4 -38.86(16) . . . . ?
N2 P2 N1 P1 -96.76(10) . . . . ?
C7 P2 N1 P1 160.01(9) . . . . ?
N1 P2 N2 C10 -63.21(16) . . . . ?
C7 P2 N2 C10 42.01(16) . . . . ?
N1 P2 N2 P3 96.90(10) . . . . ?
C7 P2 N2 P3 -157.88(9) . . . . ?
N3 P3 N2 C10 63.47(16) . . . . ?
C13 P3 N2 C10 -40.36(16) . . . . ?
N3 P3 N2 P2 -96.62(9) . . . . ?
C13 P3 N2 P2 159.55(9) . . . . ?
N2 P3 N3 C16 -66.57(16) . . . . ?
C13 P3 N3 C16 39.80(17) . . . . ?
N2 P3 N3 P4 96.12(10) . . . . ?
C13 P3 N3 P4 -157.50(10) . . . . ?
N4 P4 N3 C16 66.10(17) . . . . ?
C19 P4 N3 C16 -37.41(17) . . . . ?
N4 P4 N3 P3 -96.62(10) . . . . ?
C19 P4 N3 P3 159.87(10) . . . . ?
N3 P4 N4 C22 -66.13(16) . . . . ?
C19 P4 N4 C22 39.58(16) . . . . ?
N3 P4 N4 P1 96.07(9) . . . . ?
C19 P4 N4 P1 -158.22(10) . . . . ?
N1 P1 N4 C22 66.34(16) . . . . ?
C1 P1 N4 C22 -37.02(16) . . . . ?
N1 P1 N4 P4 -96.04(10) . . . . ?
C1 P1 N4 P4 160.60(9) . . . . ?
N1 P1 C1 C2 -30.46(16) . . . . ?
N4 P1 C1 C2 80.80(16) . . . . ?
P1 C1 C2 C3 14.6(3) . . . . ?
P1 C1 C2 C5 -165.85(15) . . . . ?
C5 C2 C3 C6 0.8(3) . . . . ?
C1 C2 C3 C6 -179.64(18) . . . . ?
C5 C2 C3 C4 -178.65(19) . . . . ?
C1 C2 C3 C4 0.9(3) . . . . ?
P1 N1 C4 C3 -32.4(2) . . . . ?
P2 N1 C4 C3 168.73(13) . . . . ?
C2 C3 C4 N1 6.7(3) . . . . ?
C6 C3 C4 N1 -172.80(17) . . . . ?
N2 P2 C7 C8 -29.72(17) . . . . ?
N1 P2 C7 C8 81.41(16) . . . . ?
P2 C7 C8 C9 11.4(3) . . . . ?
P2 C7 C8 C11 -167.25(15) . . . . ?
C7 C8 C9 C10 3.9(3) . . . . ?
C11 C8 C9 C10 -177.5(2) . . . . ?
C7 C8 C9 C12 -174.4(2) . . . . ?
C11 C8 C9 C12 4.1(3) . . . . ?
P2 N2 C10 C9 -34.6(2) . . . . ?
P3 N2 C10 C9 167.62(13) . . . . ?
C8 C9 C10 N2 6.4(3) . . . . ?
C12 C9 C10 N2 -175.05(17) . . . . ?
N3 P3 C13 C14 -25.62(18) . . . . ?
N2 P3 C13 C14 85.65(17) . . . . ?
P3 C13 C14 C15 8.4(3) . . . . ?
P3 C13 C14 C17 -172.92(16) . . . . ?
C17 C14 C15 C16 -175.7(2) . . . . ?
C13 C14 C15 C16 2.8(3) . . . . ?
C17 C14 C15 C18 4.3(3) . . . . ?
C13 C14 C15 C18 -177.19(19) . . . . ?
P3 N3 C16 C15 -35.9(2) . . . . ?
P4 N3 C16 C15 163.36(14) . . . . ?
C14 C15 C16 N3 9.8(3) . . . . ?
C18 C15 C16 N3 -170.15(17) . . . . ?
N4 P4 C19 C20 -33.21(17) . . . . ?
N3 P4 C19 C20 78.45(17) . . . . ?
P4 C19 C20 C21 19.4(3) . . . . ?
P4 C19 C20 C23 -161.49(15) . . . . ?
C23 C20 C21 C22 178.74(19) . . . . ?
C19 C20 C21 C22 -2.2(3) . . . . ?
C23 C20 C21 C24 -0.8(3) . . . . ?
C19 C20 C21 C24 178.28(19) . . . . ?
P4 N4 C22 C21 -30.0(2) . . . . ?
P1 N4 C22 C21 169.78(13) . . . . ?
C20 C21 C22 N4 6.1(3) . . . . ?
C24 C21 C22 N4 -174.37(17) . . . . ?
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full 29.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max 0.400
_refine_diff_density_min -0.343
_refine_diff_density_rms 0.059
_database_code_depnum_ccdc_archive 'CCDC 956156'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_ch124_[PN(C6H10)]4
_audit_update_record
;
2013-03-25 # Formatted by publCIF
;
_audit_creation_method SHELXL-97
#==============================================================================
# CHEMICAL DATA
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C24 H40 N4 P4, C H2 Cl2'
_chemical_formula_sum 'C25 H42 Cl2 N4 P4'
_chemical_formula_weight 593.41
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
#==============================================================================
# CRYSTAL DATA
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'C 2/c'
_symmetry_space_group_name_Hall '-C 2yc'
_symmetry_Int_Tables_number 15
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 18.4786(14)
_cell_length_b 10.3968(7)
_cell_length_c 16.6760(12)
_cell_angle_alpha 90.00
_cell_angle_beta 109.266(3)
_cell_angle_gamma 90.00
_cell_volume 3024.3(4)
_cell_formula_units_Z 4
_cell_measurement_temperature 173(2)
_cell_measurement_reflns_used 791
_cell_measurement_theta_min 5.175
_cell_measurement_theta_max 36.585
_exptl_crystal_description block
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.09
_exptl_crystal_size_mid 0.06
_exptl_crystal_size_min 0.04
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.303
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1256
_exptl_absorpt_coefficient_mu 0.448
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.9608
_exptl_absorpt_correction_T_max 0.9823
_exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)'
#==============================================================================
# EXPERIMENTAL DATA
_exptl_special_details ?
_diffrn_ambient_temperature 173(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker Apex Kappa II-CCD-diffractometer'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 11916
_diffrn_reflns_av_R_equivalents 0.1125
_diffrn_reflns_av_sigmaI/netI 0.1359
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_theta_min 2.28
_diffrn_reflns_theta_max 25.09
_reflns_number_total 2669
_reflns_number_gt 1440
_reflns_threshold_expression >2\s(I)
_computing_data_collection 'Bruker Apex V7.51A'
_computing_cell_refinement 'Bruker Apex V7.51A'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material SHELXL-97
#==============================================================================
# REFINEMENT DATA
_refine_special_details
;
All H atoms
were positioned geometrically and refined using a riding model, with C---H =
0.98 (methyl groups), 0.99\%A (methylene groups), 1.00\%A (methine groups) or
0.95 \%A (aryl CH) and with U~iso~(H) = 1.5 times U~eq~(C)
(methyl groups) or with U~iso~(H) = 1.2 times U~eq~(C)
(methylene groups, aryl CH, methine groups). Torsion angles of all methyl
groups were allowed to refine.
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0414P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 2669
_refine_ls_number_parameters 163
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1345
_refine_ls_R_factor_gt 0.0557
_refine_ls_wR_factor_ref 0.1231
_refine_ls_wR_factor_gt 0.0978
_refine_ls_goodness_of_fit_ref 1.002
_refine_ls_restrained_S_all 1.002
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
#==============================================================================
# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_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 0.59976(6) 0.50961(10) 0.22792(7) 0.0229(3) Uani 1 1 d . . .
P2 P 0.44466(6) 0.50726(11) 0.12210(7) 0.0236(3) Uani 1 1 d . . .
N1 N 0.53405(18) 0.4375(3) 0.14259(19) 0.0191(8) Uani 1 1 d . . .
N2 N 0.39863(18) 0.4283(3) 0.18180(19) 0.0216(9) Uani 1 1 d . . .
C1 C 0.6894(2) 0.4508(4) 0.2143(3) 0.0284(11) Uani 1 1 d . . .
H1A H 0.7105 0.5224 0.1898 0.034 Uiso 1 1 calc R . .
H1B H 0.7262 0.4346 0.2718 0.034 Uiso 1 1 calc R . .
C2 C 0.6892(3) 0.3328(4) 0.1616(3) 0.0266(11) Uani 1 1 d . . .
C3 C 0.6251(3) 0.2732(4) 0.1157(3) 0.0273(11) Uani 1 1 d . . .
C4 C 0.5452(2) 0.3105(4) 0.1087(3) 0.0276(11) Uani 1 1 d . . .
H4A H 0.5135 0.3077 0.0479 0.033 Uiso 1 1 calc R . .
H4B H 0.5249 0.2442 0.1383 0.033 Uiso 1 1 calc R . .
C5 C 0.7684(2) 0.2923(4) 0.1650(3) 0.0413(13) Uani 1 1 d . . .
H5A H 0.7960 0.2567 0.2212 0.062 Uiso 1 1 calc R . .
H5B H 0.7963 0.3671 0.1544 0.062 Uiso 1 1 calc R . .
H5C H 0.7645 0.2268 0.1215 0.062 Uiso 1 1 calc R . .
C6 C 0.6255(3) 0.1554(4) 0.0613(3) 0.0431(14) Uani 1 1 d . . .
H6A H 0.6232 0.1831 0.0043 0.065 Uiso 1 1 calc R . .
H6B H 0.5810 0.1013 0.0572 0.065 Uiso 1 1 calc R . .
H6C H 0.6726 0.1061 0.0874 0.065 Uiso 1 1 calc R . .
C7 C 0.3904(2) 0.4376(4) 0.0193(2) 0.0251(11) Uani 1 1 d . . .
H7A H 0.3445 0.4918 -0.0061 0.030 Uiso 1 1 calc R . .
H7B H 0.4223 0.4446 -0.0180 0.030 Uiso 1 1 calc R . .
C8 C 0.3638(2) 0.2991(4) 0.0163(3) 0.0230(10) Uani 1 1 d . . .
C9 C 0.3612(2) 0.2351(4) 0.0839(3) 0.0211(10) Uani 1 1 d . . .
C10 C 0.3834(2) 0.2887(4) 0.1726(2) 0.0251(11) Uani 1 1 d . . .
H10A H 0.3418 0.2688 0.1959 0.030 Uiso 1 1 calc R . .
H10B H 0.4299 0.2430 0.2082 0.030 Uiso 1 1 calc R . .
C11 C 0.3427(3) 0.2382(4) -0.0710(2) 0.0346(12) Uani 1 1 d . . .
H11A H 0.3273 0.1486 -0.0679 0.052 Uiso 1 1 calc R . .
H11B H 0.3871 0.2407 -0.0907 0.052 Uiso 1 1 calc R . .
H11C H 0.3002 0.2859 -0.1108 0.052 Uiso 1 1 calc R . .
C12 C 0.3376(3) 0.0956(4) 0.0820(3) 0.0316(12) Uani 1 1 d . . .
H12A H 0.2883 0.0829 0.0370 0.047 Uiso 1 1 calc R . .
H12B H 0.3326 0.0722 0.1369 0.047 Uiso 1 1 calc R . .
H12C H 0.3766 0.0411 0.0710 0.047 Uiso 1 1 calc R . .
Cl1 Cl 0.96313(9) 0.43471(13) 0.31417(9) 0.0607(5) Uani 1 1 d . . .
C13 C 1.0000 0.3389(6) 0.2500 0.051(2) Uani 1 2 d S . .
H13A H 0.9589 0.2830 0.2136 0.061 Uiso 0.50 1 calc PR . .
H13B H 1.0411 0.2830 0.2864 0.061 Uiso 0.50 1 calc PR . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.0230(7) 0.0222(7) 0.0240(7) 0.0008(6) 0.0086(5) -0.0019(6)
P2 0.0232(6) 0.0232(7) 0.0238(7) 0.0033(6) 0.0069(5) -0.0001(6)
N1 0.020(2) 0.019(2) 0.020(2) -0.0002(16) 0.0097(16) 0.0014(16)
N2 0.025(2) 0.023(2) 0.017(2) -0.0001(16) 0.0066(16) -0.0027(16)
C1 0.025(3) 0.036(3) 0.025(3) 0.006(2) 0.008(2) -0.004(2)
C2 0.030(3) 0.029(3) 0.024(3) 0.010(2) 0.013(2) 0.009(2)
C3 0.037(3) 0.024(3) 0.026(3) 0.004(2) 0.017(2) 0.003(2)
C4 0.029(3) 0.029(3) 0.027(3) -0.003(2) 0.012(2) -0.002(2)
C5 0.031(3) 0.039(3) 0.055(3) 0.003(3) 0.016(3) 0.002(2)
C6 0.042(3) 0.038(3) 0.052(3) -0.007(3) 0.019(3) 0.003(2)
C7 0.021(3) 0.034(3) 0.019(3) 0.004(2) 0.006(2) -0.001(2)
C8 0.022(3) 0.023(3) 0.022(3) -0.002(2) 0.004(2) -0.001(2)
C9 0.017(2) 0.019(3) 0.027(3) -0.005(2) 0.006(2) 0.0001(19)
C10 0.030(3) 0.023(3) 0.023(3) -0.001(2) 0.009(2) -0.001(2)
C11 0.041(3) 0.038(3) 0.025(3) -0.001(2) 0.011(2) 0.000(2)
C12 0.036(3) 0.029(3) 0.028(3) -0.004(2) 0.009(2) 0.002(2)
Cl1 0.0643(11) 0.0659(10) 0.0631(10) -0.0157(8) 0.0361(8) -0.0126(8)
C13 0.056(5) 0.041(5) 0.070(5) 0.000 0.040(4) 0.000
#==============================================================================
# MOLECULAR GEOMETRY
_geom_special_details
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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 1.709(3) . ?
P1 N2 1.719(3) 2_655 ?
P1 C1 1.848(4) . ?
P2 N2 1.717(3) . ?
P2 N1 1.732(3) . ?
P2 C7 1.827(4) . ?
N1 C4 1.477(5) . ?
N2 C10 1.476(5) . ?
N2 P1 1.719(3) 2_655 ?
C1 C2 1.508(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.332(6) . ?
C2 C5 1.507(6) . ?
C3 C4 1.494(6) . ?
C3 C6 1.526(5) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.517(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.323(5) . ?
C8 C11 1.516(5) . ?
C9 C10 1.506(5) . ?
C9 C12 1.512(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
Cl1 C13 1.756(4) . ?
C13 Cl1 1.756(4) 2_755 ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
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 108.40(16) . 2_655 ?
N1 P1 C1 99.89(17) . . ?
N2 P1 C1 100.81(17) 2_655 . ?
N2 P2 N1 107.94(16) . . ?
N2 P2 C7 97.54(17) . . ?
N1 P2 C7 102.21(18) . . ?
C4 N1 P1 124.1(3) . . ?
C4 N1 P2 122.9(3) . . ?
P1 N1 P2 110.48(17) . . ?
C10 N2 P2 121.6(3) . . ?
C10 N2 P1 121.5(2) . 2_655 ?
P2 N2 P1 113.81(18) . 2_655 ?
C2 C1 P1 120.7(3) . . ?
C2 C1 H1A 107.1 . . ?
P1 C1 H1A 107.1 . . ?
C2 C1 H1B 107.1 . . ?
P1 C1 H1B 107.1 . . ?
H1A C1 H1B 106.8 . . ?
C3 C2 C5 124.1(4) . . ?
C3 C2 C1 122.9(4) . . ?
C5 C2 C1 113.0(4) . . ?
C2 C3 C4 126.4(4) . . ?
C2 C3 C6 122.5(4) . . ?
C4 C3 C6 111.1(4) . . ?
N1 C4 C3 117.4(3) . . ?
N1 C4 H4A 107.9 . . ?
C3 C4 H4A 107.9 . . ?
N1 C4 H4B 107.9 . . ?
C3 C4 H4B 107.9 . . ?
H4A C4 H4B 107.2 . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 P2 118.6(3) . . ?
C8 C7 H7A 107.7 . . ?
P2 C7 H7A 107.7 . . ?
C8 C7 H7B 107.7 . . ?
P2 C7 H7B 107.7 . . ?
H7A C7 H7B 107.1 . . ?
C9 C8 C11 122.6(4) . . ?
C9 C8 C7 123.5(4) . . ?
C11 C8 C7 113.9(3) . . ?
C8 C9 C10 125.2(4) . . ?
C8 C9 C12 123.8(4) . . ?
C10 C9 C12 111.0(3) . . ?
N2 C10 C9 116.5(3) . . ?
N2 C10 H10A 108.2 . . ?
C9 C10 H10A 108.2 . . ?
N2 C10 H10B 108.2 . . ?
C9 C10 H10B 108.2 . . ?
H10A C10 H10B 107.3 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Cl1 C13 Cl1 110.9(4) . 2_755 ?
Cl1 C13 H13A 109.5 . . ?
Cl1 C13 H13A 109.5 2_755 . ?
Cl1 C13 H13B 109.5 . . ?
Cl1 C13 H13B 109.5 2_755 . ?
H13A C13 H13B 108.1 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 P1 N1 C4 -71.7(3) 2_655 . . . ?
C1 P1 N1 C4 33.3(3) . . . . ?
N2 P1 N1 P2 90.5(2) 2_655 . . . ?
C1 P1 N1 P2 -164.49(18) . . . . ?
N2 P2 N1 C4 74.4(3) . . . . ?
C7 P2 N1 C4 -27.8(3) . . . . ?
N2 P2 N1 P1 -88.1(2) . . . . ?
C7 P2 N1 P1 169.66(18) . . . . ?
N1 P2 N2 C10 -59.1(3) . . . . ?
C7 P2 N2 C10 46.4(3) . . . . ?
N1 P2 N2 P1 101.2(2) . . . 2_655 ?
C7 P2 N2 P1 -153.3(2) . . . 2_655 ?
N1 P1 C1 C2 -20.3(3) . . . . ?
N2 P1 C1 C2 90.7(3) 2_655 . . . ?
P1 C1 C2 C3 7.0(6) . . . . ?
P1 C1 C2 C5 -174.3(3) . . . . ?
C5 C2 C3 C4 -178.8(4) . . . . ?
C1 C2 C3 C4 -0.2(7) . . . . ?
C5 C2 C3 C6 0.3(7) . . . . ?
C1 C2 C3 C6 178.8(4) . . . . ?
P1 N1 C4 C3 -32.2(5) . . . . ?
P2 N1 C4 C3 167.7(3) . . . . ?
C2 C3 C4 N1 11.9(6) . . . . ?
C6 C3 C4 N1 -167.3(3) . . . . ?
N2 P2 C7 C8 -34.7(3) . . . . ?
N1 P2 C7 C8 75.5(3) . . . . ?
P2 C7 C8 C9 16.7(6) . . . . ?
P2 C7 C8 C11 -161.4(3) . . . . ?
C11 C8 C9 C10 178.2(4) . . . . ?
C7 C8 C9 C10 0.3(6) . . . . ?
C11 C8 C9 C12 0.3(6) . . . . ?
C7 C8 C9 C12 -177.6(4) . . . . ?
P2 N2 C10 C9 -38.0(5) . . . . ?
P1 N2 C10 C9 163.1(3) 2_655 . . . ?
C8 C9 C10 N2 9.0(6) . . . . ?
C12 C9 C10 N2 -172.9(3) . . . . ?
_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full 25.09
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max 0.335
_refine_diff_density_min -0.306
_refine_diff_density_rms 0.077
_database_code_depnum_ccdc_archive 'CCDC 956157'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_av_ch49_(Me3SiNPdmap)2_2GaCl4
_audit_creation_method SHELXL-97
#==============================================================================
# CHEMICAL DATA
_chemical_name_systematic
;
1,3-bis[4-(N,N-dimethylamino)piridyl]-2,4-bis(trimethylsilyl)-cyclo-1,3-
diphospha-2,4-diazenium bis-tetrachlorogallate
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C20 H38 N6 P2 Si2 2+, 2(Cl4 Ga -), C H2 Cl2'
_chemical_formula_sum 'C21 H40 Cl10 Ga2 N6 P2 Si2'
_chemical_formula_weight 988.65
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'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
#==============================================================================
# CRYSTAL DATA
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/c'
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_Int_Tables_number 14
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 18.2251(7)
_cell_length_b 16.1902(6)
_cell_length_c 16.0587(7)
_cell_angle_alpha 90.00
_cell_angle_beta 115.528(2)
_cell_angle_gamma 90.00
_cell_volume 4275.8(3)
_cell_formula_units_Z 4
_cell_measurement_temperature 173(2)
_cell_measurement_reflns_used 9988
_cell_measurement_theta_min 5.135
_cell_measurement_theta_max 49.269
_exptl_crystal_description block
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.35
_exptl_crystal_size_mid 0.29
_exptl_crystal_size_min 0.25
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.536
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1992
_exptl_absorpt_coefficient_mu 2.040
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.5354
_exptl_absorpt_correction_T_max 0.6296
_exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)'
#==============================================================================
# EXPERIMENTAL DATA
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 173(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker Apex Kappa II-CCD-diffractometer'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 40482
_diffrn_reflns_av_R_equivalents 0.0318
_diffrn_reflns_av_sigmaI/netI 0.0260
_diffrn_reflns_limit_h_min -21
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_theta_min 1.24
_diffrn_reflns_theta_max 24.50
_reflns_number_total 7115
_reflns_number_gt 5688
_reflns_threshold_expression >2\s(I)
_computing_data_collection 'Bruker Apex V7.51A'
_computing_cell_refinement 'Bruker Apex V7.51A'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material SHELXL-97
#==============================================================================
# REFINEMENT DATA
_refine_special_details
;
All H atoms were positioned geometrically and refined using a riding model,
with C---H = 0.98 (methyl groups), 0.99\%A (methylene groups),
1.00\%A (methine groups) or 0.95 \%A (aryl CH) and with U~iso~(H) =
1.5 times U~eq~(C) (methyl groups) or with U~iso~(H) = 1.2 times
U~eq~(C) (methylene groups, aryl CH, methine groups). Torsion angles
of all methyl groups were allowed to refine.
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0468P)^2^+3.3440P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 7115
_refine_ls_number_parameters 426
_refine_ls_number_restraints 6
_refine_ls_R_factor_all 0.0510
_refine_ls_R_factor_gt 0.0350
_refine_ls_wR_factor_ref 0.0934
_refine_ls_wR_factor_gt 0.0875
_refine_ls_goodness_of_fit_ref 1.060
_refine_ls_restrained_S_all 1.065
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
#==============================================================================
# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_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 0.33832(5) 0.94997(5) 0.30016(6) 0.02845(19) Uani 1 1 d . . .
P2 P 0.19173(5) 0.96578(5) 0.27515(6) 0.02833(19) Uani 1 1 d . . .
N1 N 0.28642(15) 0.97039(15) 0.36479(17) 0.0291(6) Uani 1 1 d . . .
N2 N 0.24380(15) 0.94749(15) 0.21069(18) 0.0304(6) Uani 1 1 d . . .
N3 N 0.36032(14) 0.84158(15) 0.32016(18) 0.0283(6) Uani 1 1 d . . .
N4 N 0.41843(18) 0.59364(17) 0.3488(2) 0.0442(7) Uani 1 1 d . . .
N5 N 0.16493(14) 1.07320(15) 0.25021(17) 0.0277(6) Uani 1 1 d . . .
N6 N 0.08207(18) 1.30762(18) 0.1543(2) 0.0461(8) Uani 1 1 d . . .
Si1 Si 0.31635(5) 0.98229(6) 0.48475(6) 0.0335(2) Uani 1 1 d . . .
Si2 Si 0.21262(5) 0.93332(6) 0.09115(6) 0.0316(2) Uani 1 1 d . . .
C1 C 0.3258(3) 0.8791(3) 0.5381(3) 0.0584(11) Uani 1 1 d . . .
H1A H 0.2739 0.8497 0.5082 0.088 Uiso 1 1 calc R . .
H1B H 0.3404 0.8854 0.6040 0.088 Uiso 1 1 calc R . .
H1C H 0.3683 0.8475 0.5302 0.088 Uiso 1 1 calc R . .
C2 C 0.4149(3) 1.0358(3) 0.5345(3) 0.0654(12) Uani 1 1 d . . .
H2A H 0.4558 1.0016 0.5266 0.098 Uiso 1 1 calc R . .
H2B H 0.4315 1.0454 0.6004 0.098 Uiso 1 1 calc R . .
H2C H 0.4100 1.0888 0.5031 0.098 Uiso 1 1 calc R . .
C3 C 0.2349(2) 1.0434(3) 0.4929(3) 0.0549(11) Uani 1 1 d . . .
H3A H 0.2311 1.0971 0.4632 0.082 Uiso 1 1 calc R . .
H3B H 0.2470 1.0517 0.5580 0.082 Uiso 1 1 calc R . .
H3C H 0.1831 1.0140 0.4619 0.082 Uiso 1 1 calc R . .
C4 C 0.2786(2) 1.0005(2) 0.0609(3) 0.0469(9) Uani 1 1 d . . .
H4A H 0.2746 1.0574 0.0794 0.070 Uiso 1 1 calc R . .
H4B H 0.2615 0.9985 -0.0059 0.070 Uiso 1 1 calc R . .
H4C H 0.3350 0.9816 0.0931 0.070 Uiso 1 1 calc R . .
C5 C 0.1044(2) 0.9624(3) 0.0377(3) 0.0520(10) Uani 1 1 d . . .
H5A H 0.0753 0.9305 0.0659 0.078 Uiso 1 1 calc R . .
H5B H 0.0811 0.9507 -0.0286 0.078 Uiso 1 1 calc R . .
H5C H 0.0992 1.0215 0.0472 0.078 Uiso 1 1 calc R . .
C6 C 0.2275(2) 0.8238(2) 0.0697(3) 0.0479(9) Uani 1 1 d . . .
H6A H 0.2848 0.8090 0.1047 0.072 Uiso 1 1 calc R . .
H6B H 0.2116 0.8156 0.0037 0.072 Uiso 1 1 calc R . .
H6C H 0.1939 0.7888 0.0892 0.072 Uiso 1 1 calc R . .
C7 C 0.3099(2) 0.78475(19) 0.3294(2) 0.0351(8) Uani 1 1 d . . .
H7 H 0.2601 0.8031 0.3286 0.042 Uiso 1 1 calc R . .
C8 C 0.3269(2) 0.7037(2) 0.3398(3) 0.0389(8) Uani 1 1 d . . .
H8 H 0.2899 0.6664 0.3471 0.047 Uiso 1 1 calc R . .
C9 C 0.4001(2) 0.6735(2) 0.3397(2) 0.0342(8) Uani 1 1 d . . .
C10 C 0.4509(2) 0.7338(2) 0.3284(2) 0.0381(8) Uani 1 1 d . . .
H10 H 0.5003 0.7173 0.3269 0.046 Uiso 1 1 calc R . .
C11 C 0.43034(18) 0.8143(2) 0.3198(2) 0.0329(7) Uani 1 1 d . . .
H11 H 0.4664 0.8534 0.3133 0.040 Uiso 1 1 calc R . .
C12 C 0.3666(3) 0.5329(2) 0.3640(3) 0.0635(12) Uani 1 1 d . . .
H12A H 0.3592 0.5480 0.4190 0.095 Uiso 1 1 calc R . .
H12B H 0.3921 0.4783 0.3731 0.095 Uiso 1 1 calc R . .
H12C H 0.3136 0.5314 0.3103 0.095 Uiso 1 1 calc R . .
C13 C 0.4948(3) 0.5642(2) 0.3501(4) 0.0661(13) Uani 1 1 d . . .
H13A H 0.4979 0.5810 0.2931 0.099 Uiso 1 1 calc R . .
H13B H 0.4971 0.5038 0.3550 0.099 Uiso 1 1 calc R . .
H13C H 0.5406 0.5881 0.4032 0.099 Uiso 1 1 calc R . .
C14 C 0.2168(2) 1.1343(2) 0.2545(3) 0.0428(9) Uani 1 1 d . . .
H14 H 0.2732 1.1220 0.2788 0.051 Uiso 1 1 calc R . .
C15 C 0.1924(2) 1.2121(2) 0.2257(3) 0.0463(10) Uani 1 1 d . . .
H15 H 0.2315 1.2531 0.2313 0.056 Uiso 1 1 calc R . .
C16 C 0.1088(2) 1.2331(2) 0.1873(2) 0.0365(8) Uani 1 1 d . . .
C17 C 0.05562(19) 1.1692(2) 0.1863(2) 0.0336(8) Uani 1 1 d . . .
H17 H -0.0010 1.1800 0.1636 0.040 Uiso 1 1 calc R . .
C18 C 0.08485(18) 1.09242(19) 0.2176(2) 0.0295(7) Uani 1 1 d . . .
H18 H 0.0478 1.0507 0.2166 0.035 Uiso 1 1 calc R . .
C19 C 0.1380(3) 1.3748(2) 0.1577(3) 0.0624(12) Uani 1 1 d . . .
H19A H 0.1709 1.3908 0.2221 0.094 Uiso 1 1 calc R . .
H19B H 0.1064 1.4225 0.1231 0.094 Uiso 1 1 calc R . .
H19C H 0.1737 1.3558 0.1303 0.094 Uiso 1 1 calc R . .
C20 C -0.0044(2) 1.3277(2) 0.1150(3) 0.0566(11) Uani 1 1 d . . .
H20A H -0.0348 1.2884 0.0657 0.085 Uiso 1 1 calc R . .
H20B H -0.0130 1.3838 0.0898 0.085 Uiso 1 1 calc R . .
H20C H -0.0236 1.3242 0.1633 0.085 Uiso 1 1 calc R . .
Ga1 Ga 0.09535(2) 0.63117(2) 0.18414(3) 0.03672(11) Uani 1 1 d . . .
Cl1 Cl 0.08618(8) 0.76350(6) 0.19288(10) 0.0756(4) Uani 1 1 d . . .
Cl2 Cl 0.13679(6) 0.58162(9) 0.32220(7) 0.0688(3) Uani 1 1 d . . .
Cl3 Cl 0.18101(7) 0.59952(7) 0.13056(8) 0.0593(3) Uani 1 1 d . . .
Cl4 Cl -0.02157(6) 0.57901(7) 0.09898(7) 0.0593(3) Uani 1 1 d . . .
Ga2 Ga 0.43448(2) 1.28486(2) 0.35034(3) 0.03988(12) Uani 1 1 d . . .
Cl5 Cl 0.55490(6) 1.33672(6) 0.41766(8) 0.0622(3) Uani 1 1 d . . .
Cl6 Cl 0.36736(8) 1.30698(8) 0.43072(9) 0.0713(3) Uani 1 1 d . . .
Cl7 Cl 0.37288(6) 1.34283(8) 0.21691(7) 0.0656(3) Uani 1 1 d . . .
Cl8 Cl 0.43973(7) 1.15341(6) 0.32950(10) 0.0683(3) Uani 1 1 d . . .
C21A C 0.1464(9) 1.2215(5) -0.0871(6) 0.087(4) Uani 0.629(13) 1 d PD A 1
H21A H 0.1869 1.2452 -0.1060 0.104 Uiso 0.629(13) 1 calc PR A 1
H21B H 0.0978 1.2575 -0.1116 0.104 Uiso 0.629(13) 1 calc PR A 1
Cl10 Cl 0.1202(5) 1.1257(4) -0.1327(4) 0.0905(15) Uani 0.629(13) 1 d PD A 1
Cl9A Cl 0.1855(8) 1.2195(3) 0.0288(3) 0.177(4) Uani 0.629(13) 1 d PD A 1
C21B C 0.1082(8) 1.2012(13) -0.0599(18) 0.117(9) Uani 0.371(13) 1 d PD A 2
H21C H 0.0770 1.2479 -0.0990 0.141 Uiso 0.371(13) 1 calc PR A 2
H21D H 0.0864 1.1906 -0.0141 0.141 Uiso 0.371(13) 1 calc PR A 2
Cl9B Cl 0.2106(4) 1.2323(3) 0.0001(8) 0.098(4) Uani 0.371(13) 1 d PD A 2
Cl1B Cl 0.0898(9) 1.1117(8) -0.1316(9) 0.117(4) Uani 0.371(13) 1 d PD A 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.0269(4) 0.0213(4) 0.0354(5) -0.0013(3) 0.0118(4) 0.0014(3)
P2 0.0266(4) 0.0223(4) 0.0346(5) 0.0001(3) 0.0118(4) 0.0022(3)
N1 0.0276(14) 0.0253(14) 0.0324(15) -0.0009(11) 0.0111(12) 0.0056(11)
N2 0.0277(14) 0.0284(14) 0.0334(15) -0.0009(11) 0.0115(12) 0.0042(12)
N3 0.0226(13) 0.0228(13) 0.0371(15) -0.0014(11) 0.0106(12) 0.0030(11)
N4 0.0488(18) 0.0246(15) 0.060(2) 0.0035(14) 0.0241(16) 0.0086(14)
N5 0.0245(13) 0.0215(13) 0.0367(15) 0.0011(11) 0.0129(12) 0.0018(11)
N6 0.0448(18) 0.0281(16) 0.068(2) 0.0080(14) 0.0268(17) 0.0032(14)
Si1 0.0296(5) 0.0355(5) 0.0338(5) -0.0025(4) 0.0121(4) 0.0052(4)
Si2 0.0289(5) 0.0325(5) 0.0328(5) -0.0011(4) 0.0128(4) 0.0038(4)
C1 0.069(3) 0.059(3) 0.053(3) 0.015(2) 0.032(2) 0.023(2)
C2 0.053(3) 0.087(3) 0.054(3) -0.023(2) 0.021(2) -0.020(2)
C3 0.056(2) 0.064(3) 0.049(2) 0.002(2) 0.027(2) 0.024(2)
C4 0.051(2) 0.044(2) 0.048(2) 0.0056(17) 0.0228(19) -0.0004(18)
C5 0.0310(19) 0.082(3) 0.036(2) -0.005(2) 0.0079(16) 0.012(2)
C6 0.062(2) 0.037(2) 0.049(2) -0.0105(17) 0.028(2) -0.0062(19)
C7 0.0284(17) 0.0259(18) 0.051(2) -0.0010(15) 0.0167(16) 0.0020(14)
C8 0.0354(19) 0.0269(18) 0.057(2) 0.0001(16) 0.0227(17) -0.0035(15)
C9 0.0373(19) 0.0249(17) 0.0364(19) -0.0004(14) 0.0121(15) 0.0049(15)
C10 0.0347(18) 0.0305(19) 0.053(2) 0.0019(16) 0.0220(17) 0.0083(15)
C11 0.0233(16) 0.0286(18) 0.045(2) -0.0009(15) 0.0124(15) -0.0028(14)
C12 0.072(3) 0.026(2) 0.098(4) 0.007(2) 0.041(3) 0.003(2)
C13 0.066(3) 0.034(2) 0.105(4) 0.005(2) 0.043(3) 0.020(2)
C14 0.0249(17) 0.034(2) 0.065(3) 0.0039(17) 0.0151(17) 0.0002(16)
C15 0.035(2) 0.0262(19) 0.076(3) 0.0061(18) 0.0229(19) -0.0054(16)
C16 0.0392(19) 0.0252(18) 0.048(2) 0.0025(15) 0.0212(17) 0.0047(15)
C17 0.0278(17) 0.0327(19) 0.041(2) 0.0023(15) 0.0152(15) 0.0028(15)
C18 0.0263(16) 0.0264(17) 0.0370(18) -0.0006(14) 0.0146(14) -0.0012(14)
C19 0.066(3) 0.030(2) 0.098(4) 0.014(2) 0.042(3) 0.002(2)
C20 0.051(2) 0.043(2) 0.077(3) 0.024(2) 0.029(2) 0.017(2)
Ga1 0.0403(2) 0.0334(2) 0.0427(2) -0.00397(17) 0.02374(19) -0.00446(17)
Cl1 0.0776(8) 0.0348(5) 0.1322(11) -0.0121(6) 0.0619(8) -0.0064(5)
Cl2 0.0527(6) 0.1086(9) 0.0478(6) 0.0199(6) 0.0243(5) 0.0095(6)
Cl3 0.0695(7) 0.0561(6) 0.0775(7) -0.0097(5) 0.0556(6) -0.0049(5)
Cl4 0.0468(6) 0.0639(7) 0.0611(7) -0.0132(5) 0.0175(5) -0.0136(5)
Ga2 0.0381(2) 0.0295(2) 0.0480(3) 0.00367(17) 0.01467(19) -0.00254(17)
Cl5 0.0435(5) 0.0459(6) 0.0762(8) 0.0036(5) 0.0059(5) -0.0114(5)
Cl6 0.0827(8) 0.0751(8) 0.0712(8) -0.0075(6) 0.0474(7) -0.0048(6)
Cl7 0.0535(6) 0.0806(8) 0.0533(6) 0.0231(6) 0.0140(5) 0.0023(6)
Cl8 0.0577(6) 0.0320(5) 0.1220(10) -0.0068(6) 0.0451(7) -0.0069(5)
C21A 0.121(11) 0.056(5) 0.070(7) 0.025(4) 0.028(7) 0.022(6)
Cl10 0.123(4) 0.069(2) 0.0623(18) 0.0067(14) 0.024(2) 0.019(2)
Cl9A 0.374(11) 0.079(3) 0.066(2) 0.0156(17) 0.084(4) 0.077(5)
C21B 0.088(14) 0.096(16) 0.14(2) -0.035(14) 0.018(13) 0.044(11)
Cl9B 0.095(5) 0.057(2) 0.155(9) 0.025(4) 0.067(5) 0.018(2)
Cl1B 0.128(8) 0.072(4) 0.126(5) 0.027(3) 0.030(5) 0.025(5)
#==============================================================================
# MOLECULAR GEOMETRY
_geom_special_details
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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 N2 1.703(3) . ?
P1 N1 1.711(3) . ?
P1 N3 1.798(3) . ?
P1 P2 2.5377(11) . ?
P2 N2 1.705(3) . ?
P2 N1 1.707(3) . ?
P2 N5 1.804(2) . ?
N1 Si1 1.772(3) . ?
N2 Si2 1.767(3) . ?
N3 C11 1.353(4) . ?
N3 C7 1.353(4) . ?
N4 C9 1.328(4) . ?
N4 C12 1.456(5) . ?
N4 C13 1.463(5) . ?
N5 C14 1.350(4) . ?
N5 C18 1.357(4) . ?
N6 C16 1.324(4) . ?
N6 C20 1.460(5) . ?
N6 C19 1.475(5) . ?
Si1 C3 1.835(4) . ?
Si1 C2 1.838(4) . ?
Si1 C1 1.852(4) . ?
Si2 C4 1.836(4) . ?
Si2 C5 1.841(3) . ?
Si2 C6 1.849(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.342(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.420(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.409(5) . ?
C10 C11 1.347(5) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.348(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.416(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.412(5) . ?
C17 C18 1.361(4) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
Ga1 Cl3 2.1441(10) . ?
Ga1 Cl4 2.1477(10) . ?
Ga1 Cl1 2.1581(11) . ?
Ga1 Cl2 2.1648(11) . ?
Ga2 Cl5 2.1553(10) . ?
Ga2 Cl6 2.1567(12) . ?
Ga2 Cl7 2.1585(11) . ?
Ga2 Cl8 2.1629(11) . ?
C21A Cl9A 1.682(8) . ?
C21A Cl10 1.693(9) . ?
C21A H21A 0.9900 . ?
C21A H21B 0.9900 . ?
C21B Cl9B 1.765(12) . ?
C21B Cl1B 1.791(12) . ?
C21B H21C 0.9900 . ?
C21B H21D 0.9900 . ?
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 P1 N1 83.89(12) . . ?
N2 P1 N3 101.21(12) . . ?
N1 P1 N3 102.66(12) . . ?
N2 P1 P2 41.90(9) . . ?
N1 P1 P2 42.01(9) . . ?
N3 P1 P2 105.38(9) . . ?
N2 P2 N1 83.95(12) . . ?
N2 P2 N5 101.59(12) . . ?
N1 P2 N5 102.93(12) . . ?
N2 P2 P1 41.84(9) . . ?
N1 P2 P1 42.12(9) . . ?
N5 P2 P1 107.35(9) . . ?
P2 N1 P1 95.87(13) . . ?
P2 N1 Si1 130.33(15) . . ?
P1 N1 Si1 133.54(15) . . ?
P1 N2 P2 96.26(14) . . ?
P1 N2 Si2 130.88(15) . . ?
P2 N2 Si2 132.83(15) . . ?
C11 N3 C7 117.7(3) . . ?
C11 N3 P1 117.1(2) . . ?
C7 N3 P1 125.0(2) . . ?
C9 N4 C12 121.7(3) . . ?
C9 N4 C13 120.8(3) . . ?
C12 N4 C13 117.4(3) . . ?
C14 N5 C18 117.7(3) . . ?
C14 N5 P2 125.3(2) . . ?
C18 N5 P2 116.7(2) . . ?
C16 N6 C20 121.2(3) . . ?
C16 N6 C19 121.9(3) . . ?
C20 N6 C19 116.9(3) . . ?
N1 Si1 C3 104.87(15) . . ?
N1 Si1 C2 108.03(17) . . ?
C3 Si1 C2 112.6(2) . . ?
N1 Si1 C1 109.16(16) . . ?
C3 Si1 C1 111.76(19) . . ?
C2 Si1 C1 110.2(2) . . ?
N2 Si2 C4 105.66(15) . . ?
N2 Si2 C5 104.60(15) . . ?
C4 Si2 C5 114.67(19) . . ?
N2 Si2 C6 108.85(15) . . ?
C4 Si2 C6 110.72(18) . . ?
C5 Si2 C6 111.82(19) . . ?
Si1 C1 H1A 109.5 . . ?
Si1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Si1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si1 C3 H3A 109.5 . . ?
Si1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Si1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si2 C4 H4A 109.5 . . ?
Si2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Si2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si2 C5 H5A 109.5 . . ?
Si2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si2 C6 H6A 109.5 . . ?
Si2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 N3 123.2(3) . . ?
C8 C7 H7 118.4 . . ?
N3 C7 H7 118.4 . . ?
C7 C8 C9 120.2(3) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 H8 119.9 . . ?
N4 C9 C10 122.6(3) . . ?
N4 C9 C8 121.8(3) . . ?
C10 C9 C8 115.5(3) . . ?
C11 C10 C9 120.9(3) . . ?
C11 C10 H10 119.5 . . ?
C9 C10 H10 119.5 . . ?
C10 C11 N3 122.4(3) . . ?
C10 C11 H11 118.8 . . ?
N3 C11 H11 118.8 . . ?
N4 C12 H12A 109.5 . . ?
N4 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N4 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N4 C13 H13A 109.5 . . ?
N4 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N4 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 N5 123.0(3) . . ?
C15 C14 H14 118.5 . . ?
N5 C14 H14 118.5 . . ?
C14 C15 C16 120.5(3) . . ?
C14 C15 H15 119.7 . . ?
C16 C15 H15 119.7 . . ?
N6 C16 C17 122.0(3) . . ?
N6 C16 C15 122.3(3) . . ?
C17 C16 C15 115.7(3) . . ?
C18 C17 C16 120.5(3) . . ?
C18 C17 H17 119.8 . . ?
C16 C17 H17 119.8 . . ?
N5 C18 C17 122.5(3) . . ?
N5 C18 H18 118.8 . . ?
C17 C18 H18 118.8 . . ?
N6 C19 H19A 109.5 . . ?
N6 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N6 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N6 C20 H20A 109.5 . . ?
N6 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N6 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Cl3 Ga1 Cl4 110.16(4) . . ?
Cl3 Ga1 Cl1 110.70(4) . . ?
Cl4 Ga1 Cl1 110.39(5) . . ?
Cl3 Ga1 Cl2 109.24(5) . . ?
Cl4 Ga1 Cl2 108.60(5) . . ?
Cl1 Ga1 Cl2 107.69(6) . . ?
Cl5 Ga2 Cl6 110.65(5) . . ?
Cl5 Ga2 Cl7 108.07(5) . . ?
Cl6 Ga2 Cl7 109.60(5) . . ?
Cl5 Ga2 Cl8 110.94(4) . . ?
Cl6 Ga2 Cl8 109.29(5) . . ?
Cl7 Ga2 Cl8 108.24(5) . . ?
Cl9A C21A Cl10 111.6(6) . . ?
Cl9A C21A H21A 109.3 . . ?
Cl10 C21A H21A 109.3 . . ?
Cl9A C21A H21B 109.3 . . ?
Cl10 C21A H21B 109.3 . . ?
H21A C21A H21B 108.0 . . ?
Cl9B C21B Cl1B 116.3(10) . . ?
Cl9B C21B H21C 108.2 . . ?
Cl1B C21B H21C 108.2 . . ?
Cl9B C21B H21D 108.2 . . ?
Cl1B C21B H21D 108.2 . . ?
H21C C21B H21D 107.4 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 P1 P2 N2 178.31(19) . . . . ?
N3 P1 P2 N2 -89.73(16) . . . . ?
N2 P1 P2 N1 -178.31(19) . . . . ?
N3 P1 P2 N1 91.96(16) . . . . ?
N2 P1 P2 N5 -88.09(16) . . . . ?
N1 P1 P2 N5 90.22(16) . . . . ?
N3 P1 P2 N5 -177.81(13) . . . . ?
N2 P2 N1 P1 -1.13(12) . . . . ?
N5 P2 N1 P1 -101.68(13) . . . . ?
N2 P2 N1 Si1 -175.7(2) . . . . ?
N5 P2 N1 Si1 83.7(2) . . . . ?
P1 P2 N1 Si1 -174.6(3) . . . . ?
N2 P1 N1 P2 1.14(12) . . . . ?
N3 P1 N1 P2 -99.02(13) . . . . ?
N2 P1 N1 Si1 175.4(2) . . . . ?
N3 P1 N1 Si1 75.3(2) . . . . ?
P2 P1 N1 Si1 174.3(3) . . . . ?
N1 P1 N2 P2 -1.14(13) . . . . ?
N3 P1 N2 P2 100.60(13) . . . . ?
N1 P1 N2 Si2 177.4(2) . . . . ?
N3 P1 N2 Si2 -80.9(2) . . . . ?
P2 P1 N2 Si2 178.5(3) . . . . ?
N1 P2 N2 P1 1.14(13) . . . . ?
N5 P2 N2 P1 103.14(13) . . . . ?
N1 P2 N2 Si2 -177.3(2) . . . . ?
N5 P2 N2 Si2 -75.3(2) . . . . ?
P1 P2 N2 Si2 -178.4(3) . . . . ?
N2 P1 N3 C11 126.0(2) . . . . ?
N1 P1 N3 C11 -147.8(2) . . . . ?
P2 P1 N3 C11 168.9(2) . . . . ?
N2 P1 N3 C7 -49.4(3) . . . . ?
N1 P1 N3 C7 36.8(3) . . . . ?
P2 P1 N3 C7 -6.5(3) . . . . ?
N2 P2 N5 C14 -49.5(3) . . . . ?
N1 P2 N5 C14 36.9(3) . . . . ?
P1 P2 N5 C14 -6.6(3) . . . . ?
N2 P2 N5 C18 125.1(2) . . . . ?
N1 P2 N5 C18 -148.6(2) . . . . ?
P1 P2 N5 C18 168.0(2) . . . . ?
P2 N1 Si1 C3 -30.1(3) . . . . ?
P1 N1 Si1 C3 157.3(2) . . . . ?
P2 N1 Si1 C2 -150.4(2) . . . . ?
P1 N1 Si1 C2 37.0(3) . . . . ?
P2 N1 Si1 C1 89.8(2) . . . . ?
P1 N1 Si1 C1 -82.8(3) . . . . ?
P1 N2 Si2 C4 -45.8(2) . . . . ?
P2 N2 Si2 C4 132.1(2) . . . . ?
P1 N2 Si2 C5 -167.2(2) . . . . ?
P2 N2 Si2 C5 10.7(3) . . . . ?
P1 N2 Si2 C6 73.1(2) . . . . ?
P2 N2 Si2 C6 -108.9(2) . . . . ?
C11 N3 C7 C8 1.2(5) . . . . ?
P1 N3 C7 C8 176.6(3) . . . . ?
N3 C7 C8 C9 -1.1(6) . . . . ?
C12 N4 C9 C10 177.5(4) . . . . ?
C13 N4 C9 C10 1.8(5) . . . . ?
C12 N4 C9 C8 -3.2(5) . . . . ?
C13 N4 C9 C8 -178.9(4) . . . . ?
C7 C8 C9 N4 -179.3(3) . . . . ?
C7 C8 C9 C10 0.0(5) . . . . ?
N4 C9 C10 C11 -179.7(3) . . . . ?
C8 C9 C10 C11 1.0(5) . . . . ?
C9 C10 C11 N3 -1.0(5) . . . . ?
C7 N3 C11 C10 -0.1(5) . . . . ?
P1 N3 C11 C10 -175.9(3) . . . . ?
C18 N5 C14 C15 -1.8(5) . . . . ?
P2 N5 C14 C15 172.7(3) . . . . ?
N5 C14 C15 C16 -1.2(6) . . . . ?
C20 N6 C16 C17 0.2(6) . . . . ?
C19 N6 C16 C17 178.3(4) . . . . ?
C20 N6 C16 C15 -180.0(4) . . . . ?
C19 N6 C16 C15 -1.9(6) . . . . ?
C14 C15 C16 N6 -176.6(4) . . . . ?
C14 C15 C16 C17 3.2(6) . . . . ?
N6 C16 C17 C18 177.4(3) . . . . ?
C15 C16 C17 C18 -2.4(5) . . . . ?
C14 N5 C18 C17 2.6(5) . . . . ?
P2 N5 C18 C17 -172.3(3) . . . . ?
C16 C17 C18 N5 -0.5(5) . . . . ?
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full 24.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max 0.875
_refine_diff_density_min -0.554
_refine_diff_density_rms 0.069
_database_code_depnum_ccdc_archive 'CCDC 956158'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_ch116_[Me3SiNP(C6H10)2][OTf]
_audit_creation_method SHELXL-97
#==============================================================================
# CHEMICAL DATA
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C15 H29 N P Si +, C F3 O3 S -'
_chemical_formula_sum 'C16 H29 F3 N O3 P S Si'
_chemical_formula_weight 431.52
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
#==============================================================================
# CRYSTAL DATA
_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M 'P -1'
_symmetry_space_group_name_Hall '-P 1'
_symmetry_Int_Tables_number 2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 11.1833(3)
_cell_length_b 16.4208(4)
_cell_length_c 19.4337(5)
_cell_angle_alpha 67.2760(10)
_cell_angle_beta 82.1900(10)
_cell_angle_gamma 83.2230(10)
_cell_volume 3252.83(14)
_cell_formula_units_Z 6
_cell_measurement_temperature 173(2)
_cell_measurement_reflns_used 6996
_cell_measurement_theta_min 5.264
_cell_measurement_theta_max 48.572
_exptl_crystal_description block
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.21
_exptl_crystal_size_mid 0.13
_exptl_crystal_size_min 0.09
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.322
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1368
_exptl_absorpt_coefficient_mu 0.318
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.9362
_exptl_absorpt_correction_T_max 0.9719
_exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)'
#==============================================================================
# EXPERIMENTAL DATA
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 173(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker Apex Kappa II-CCD-diffractometer'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 54016
_diffrn_reflns_av_R_equivalents 0.0613
_diffrn_reflns_av_sigmaI/netI 0.0939
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -20
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_theta_min 1.14
_diffrn_reflns_theta_max 28.00
_reflns_number_total 15669
_reflns_number_gt 8972
_reflns_threshold_expression >2\s(I)
_computing_data_collection 'Bruker Apex V7.51A'
_computing_cell_refinement 'Bruker Apex V7.51A'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material SHELXL-97
#==============================================================================
# REFINEMENT DATA
_refine_special_details
;
All H atoms
were positioned geometrically and refined using a riding model, with C---H =
0.98 (methyl groups), 0.99\%A (methylene groups), 1.00\%A (methine groups) or
0.95 \%A (aryl CH) and with U~iso~(H) = 1.5 times U~eq~(C)
(methyl groups) or with U~iso~(H) = 1.2 times U~eq~(C)
(methylene groups, aryl CH, methine groups). Torsion angles of all methyl
groups were allowed to refine.
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 15669
_refine_ls_number_parameters 724
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1145
_refine_ls_R_factor_gt 0.0522
_refine_ls_wR_factor_ref 0.1225
_refine_ls_wR_factor_gt 0.1001
_refine_ls_goodness_of_fit_ref 1.014
_refine_ls_restrained_S_all 1.014
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
#==============================================================================
# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_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
C1 C 0.1229(2) 0.60576(17) 0.48608(14) 0.0323(6) Uani 1 1 d . . .
H1A H 0.0336 0.6156 0.4910 0.039 Uiso 1 1 calc R . .
H1B H 0.1451 0.5436 0.5178 0.039 Uiso 1 1 calc R . .
C2 C 0.1791(2) 0.66816(17) 0.51120(14) 0.0294(6) Uani 1 1 d . . .
C3 C 0.2986(2) 0.67227(18) 0.49812(14) 0.0313(6) Uani 1 1 d . . .
C4 C 0.3706(2) 0.61509(19) 0.46002(15) 0.0351(7) Uani 1 1 d . . .
H4A H 0.4555 0.6314 0.4488 0.042 Uiso 1 1 calc R . .
H4B H 0.3703 0.5525 0.4952 0.042 Uiso 1 1 calc R . .
C5 C 0.0928(2) 0.71933(19) 0.54768(16) 0.0404(7) Uani 1 1 d . . .
H5A H 0.1372 0.7591 0.5601 0.061 Uiso 1 1 calc R . .
H5B H 0.0516 0.6783 0.5937 0.061 Uiso 1 1 calc R . .
H5C H 0.0328 0.7542 0.5133 0.061 Uiso 1 1 calc R . .
C6 C 0.3700(3) 0.7288(2) 0.51973(17) 0.0468(8) Uani 1 1 d . . .
H6A H 0.3146 0.7692 0.5372 0.070 Uiso 1 1 calc R . .
H6B H 0.4231 0.7631 0.4762 0.070 Uiso 1 1 calc R . .
H6C H 0.4192 0.6910 0.5600 0.070 Uiso 1 1 calc R . .
C7 C 0.1154(2) 0.55305(17) 0.35813(15) 0.0330(6) Uani 1 1 d . . .
H7A H 0.1794 0.5275 0.3303 0.040 Uiso 1 1 calc R . .
H7B H 0.0768 0.5043 0.4004 0.040 Uiso 1 1 calc R . .
C8 C 0.0237(3) 0.61100(19) 0.30756(16) 0.0375(7) Uani 1 1 d . . .
C9 C 0.0188(3) 0.69675(19) 0.29337(15) 0.0382(7) Uani 1 1 d . . .
C10 C 0.1050(2) 0.72733(17) 0.33031(15) 0.0343(7) Uani 1 1 d . . .
H10A H 0.0607 0.7615 0.3593 0.041 Uiso 1 1 calc R . .
H10B H 0.1651 0.7645 0.2926 0.041 Uiso 1 1 calc R . .
C14 C 0.4835(3) 0.75439(19) 0.28070(17) 0.0501(8) Uani 1 1 d . . .
H14A H 0.4141 0.7981 0.2695 0.075 Uiso 1 1 calc R . .
H14B H 0.5414 0.7665 0.2359 0.075 Uiso 1 1 calc R . .
H14C H 0.5228 0.7580 0.3215 0.075 Uiso 1 1 calc R . .
C15 C 0.5605(3) 0.5589(2) 0.33733(18) 0.0509(8) Uani 1 1 d . . .
H15A H 0.6028 0.5699 0.3735 0.076 Uiso 1 1 calc R . .
H15B H 0.6165 0.5626 0.2930 0.076 Uiso 1 1 calc R . .
H15C H 0.5300 0.4998 0.3603 0.076 Uiso 1 1 calc R . .
C16 C 0.3367(3) 0.9805(2) 0.08584(17) 0.0411(7) Uani 1 1 d . . .
C17 C 0.9062(2) 0.09493(17) 0.16904(14) 0.0307(6) Uani 1 1 d . . .
H17A H 0.8671 0.1551 0.1453 0.037 Uiso 1 1 calc R . .
H17B H 0.9944 0.0974 0.1547 0.037 Uiso 1 1 calc R . .
C18 C 0.8566(2) 0.03088(16) 0.14241(14) 0.0271(6) Uani 1 1 d . . .
C19 C 0.7435(2) 0.00953(17) 0.16701(14) 0.0283(6) Uani 1 1 d . . .
C20 C 0.6708(2) 0.05090(18) 0.21795(14) 0.0302(6) Uani 1 1 d . . .
H20A H 0.6552 0.1150 0.1893 0.036 Uiso 1 1 calc R . .
H20B H 0.5916 0.0246 0.2348 0.036 Uiso 1 1 calc R . .
C21 C 0.9422(3) -0.00163(19) 0.09121(15) 0.0393(7) Uani 1 1 d . . .
H21A H 0.9048 -0.0462 0.0809 0.059 Uiso 1 1 calc R . .
H21B H 1.0167 -0.0281 0.1150 0.059 Uiso 1 1 calc R . .
H21C H 0.9614 0.0480 0.0441 0.059 Uiso 1 1 calc R . .
C22 C 0.6794(3) -0.0535(2) 0.14839(16) 0.0430(8) Uani 1 1 d . . .
H22A H 0.6075 -0.0225 0.1233 0.064 Uiso 1 1 calc R . .
H22B H 0.6549 -0.1028 0.1946 0.064 Uiso 1 1 calc R . .
H22C H 0.7339 -0.0765 0.1150 0.064 Uiso 1 1 calc R . .
C23 C 0.9275(2) 0.13523(17) 0.30105(15) 0.0306(6) Uani 1 1 d . . .
H23A H 0.9474 0.1909 0.2587 0.037 Uiso 1 1 calc R . .
H23B H 0.8653 0.1491 0.3371 0.037 Uiso 1 1 calc R . .
C24 C 1.0390(2) 0.08739(18) 0.33850(14) 0.0315(6) Uani 1 1 d . . .
C25 C 1.0629(2) 0.00281(18) 0.34666(15) 0.0322(6) Uani 1 1 d . . .
C26 C 0.9775(2) -0.03514(17) 0.31471(15) 0.0317(6) Uani 1 1 d . . .
H26A H 0.9329 -0.0824 0.3551 0.038 Uiso 1 1 calc R . .
H26B H 1.0222 -0.0598 0.2787 0.038 Uiso 1 1 calc R . .
C28 C 1.1671(3) -0.05794(19) 0.38358(17) 0.0475(8) Uani 1 1 d . . .
H28A H 1.2141 -0.0267 0.4034 0.071 Uiso 1 1 calc R . .
H28B H 1.2191 -0.0766 0.3467 0.071 Uiso 1 1 calc R . .
H28C H 1.1359 -0.1101 0.4247 0.071 Uiso 1 1 calc R . .
C30 C 0.7387(3) -0.0153(2) 0.44800(15) 0.0494(8) Uani 1 1 d . . .
H30A H 0.7809 -0.0730 0.4536 0.074 Uiso 1 1 calc R . .
H30B H 0.6893 -0.0198 0.4948 0.074 Uiso 1 1 calc R . .
H30C H 0.7983 0.0286 0.4364 0.074 Uiso 1 1 calc R . .
C31 C 0.5422(3) -0.07018(19) 0.38617(17) 0.0476(8) Uani 1 1 d . . .
H31A H 0.4872 -0.0508 0.3467 0.071 Uiso 1 1 calc R . .
H31B H 0.4950 -0.0846 0.4352 0.071 Uiso 1 1 calc R . .
H31C H 0.5925 -0.1227 0.3848 0.071 Uiso 1 1 calc R . .
C32 C 0.2829(3) 0.31583(19) 0.44451(17) 0.0386(7) Uani 1 1 d . . .
C33 C 0.4125(2) 0.25440(17) 0.16006(14) 0.0308(6) Uani 1 1 d . . .
H33A H 0.3903 0.1925 0.1865 0.037 Uiso 1 1 calc R . .
H33B H 0.4958 0.2578 0.1702 0.037 Uiso 1 1 calc R . .
C34 C 0.3255(2) 0.31540(17) 0.18787(14) 0.0291(6) Uani 1 1 d . . .
C35 C 0.2128(2) 0.32874(17) 0.16905(14) 0.0290(6) Uani 1 1 d . . .
C36 C 0.1774(2) 0.28162(18) 0.12214(14) 0.0321(6) Uani 1 1 d . . .
H36A H 0.1763 0.2175 0.1529 0.038 Uiso 1 1 calc R . .
H36B H 0.0944 0.3037 0.1081 0.038 Uiso 1 1 calc R . .
C37 C 0.3774(3) 0.35666(19) 0.23321(16) 0.0388(7) Uani 1 1 d . . .
H37A H 0.3137 0.3935 0.2496 0.058 Uiso 1 1 calc R . .
H37B H 0.4426 0.3934 0.2024 0.058 Uiso 1 1 calc R . .
H37C H 0.4096 0.3100 0.2772 0.058 Uiso 1 1 calc R . .
C38 C 0.1140(2) 0.38662(19) 0.19127(17) 0.0414(7) Uani 1 1 d . . .
H38A H 0.0438 0.3522 0.2161 0.062 Uiso 1 1 calc R . .
H38B H 0.0908 0.4367 0.1465 0.062 Uiso 1 1 calc R . .
H38C H 0.1430 0.4087 0.2257 0.062 Uiso 1 1 calc R . .
C39 C 0.4827(2) 0.38599(16) 0.01111(14) 0.0277(6) Uani 1 1 d . . .
H39A H 0.4366 0.4271 -0.0303 0.033 Uiso 1 1 calc R . .
H39B H 0.4941 0.4164 0.0446 0.033 Uiso 1 1 calc R . .
C40 C 0.6029(2) 0.35432(17) -0.01897(14) 0.0284(6) Uani 1 1 d . . .
C41 C 0.6170(2) 0.26914(18) -0.00928(15) 0.0309(6) Uani 1 1 d . . .
C42 C 0.5086(2) 0.21485(17) 0.02752(15) 0.0310(6) Uani 1 1 d . . .
H42A H 0.5317 0.1595 0.0691 0.037 Uiso 1 1 calc R . .
H42B H 0.4720 0.1998 -0.0093 0.037 Uiso 1 1 calc R . .
C43 C 0.6951(3) 0.42135(18) -0.05720(16) 0.0410(7) Uani 1 1 d . . .
H43A H 0.7682 0.3929 -0.0747 0.062 Uiso 1 1 calc R . .
H43B H 0.7154 0.4456 -0.0217 0.062 Uiso 1 1 calc R . .
H43C H 0.6619 0.4693 -0.1001 0.062 Uiso 1 1 calc R . .
C45 C 0.3125(3) 0.3371(2) -0.11060(16) 0.0542(9) Uani 1 1 d . . .
H45A H 0.3631 0.3829 -0.1125 0.081 Uiso 1 1 calc R . .
H45B H 0.2750 0.3563 -0.1576 0.081 Uiso 1 1 calc R . .
H45C H 0.3627 0.2819 -0.1037 0.081 Uiso 1 1 calc R . .
C47 C 0.0883(3) 0.4185(2) -0.04633(17) 0.0536(9) Uani 1 1 d . . .
H47A H 0.0243 0.4067 -0.0046 0.080 Uiso 1 1 calc R . .
H47B H 0.0521 0.4342 -0.0934 0.080 Uiso 1 1 calc R . .
H47C H 0.1331 0.4676 -0.0490 0.080 Uiso 1 1 calc R . .
C48 C 0.7473(3) 0.37985(19) 0.24148(16) 0.0347(7) Uani 1 1 d . . .
F1 F 0.24594(16) 0.97050(11) 0.05296(10) 0.0563(5) Uani 1 1 d . . .
F2 F 0.3947(2) 1.04793(14) 0.03655(11) 0.0867(7) Uani 1 1 d . . .
F3 F 0.41277(15) 0.90880(12) 0.09782(11) 0.0606(5) Uani 1 1 d . . .
F4 F 0.19090(15) 0.32873(12) 0.40355(9) 0.0545(5) Uani 1 1 d . . .
F5 F 0.35386(15) 0.38220(12) 0.40752(10) 0.0566(5) Uani 1 1 d . . .
F6 F 0.34598(16) 0.24197(11) 0.44467(10) 0.0579(5) Uani 1 1 d . . .
F7 F 0.81717(17) 0.32385(11) 0.29185(10) 0.0590(5) Uani 1 1 d . . .
F8 F 0.63851(16) 0.38489(13) 0.27696(10) 0.0608(5) Uani 1 1 d . . .
F9 F 0.79066(17) 0.45853(11) 0.21969(10) 0.0592(5) Uani 1 1 d . . .
N1 N 0.32412(18) 0.62269(14) 0.38854(11) 0.0305(5) Uani 1 1 d . . .
N2 N 0.73301(17) 0.03839(13) 0.28570(11) 0.0259(5) Uani 1 1 d . . .
N3 N 0.26212(18) 0.29457(14) 0.05154(12) 0.0292(5) Uani 1 1 d . . .
O1 O 0.2005(2) 1.07378(13) 0.14762(13) 0.0595(6) Uani 1 1 d . . .
O2 O 0.2278(2) 0.91824(14) 0.21573(12) 0.0624(6) Uani 1 1 d . . .
O3 O 0.39067(18) 1.01214(16) 0.19667(13) 0.0646(7) Uani 1 1 d . . .
O4 O 0.16696(18) 0.39506(12) 0.52543(12) 0.0493(6) Uani 1 1 d . . .
O5 O 0.15685(18) 0.23716(13) 0.56785(11) 0.0487(5) Uani 1 1 d . . .
O6 O 0.34190(17) 0.29756(14) 0.57287(12) 0.0513(6) Uani 1 1 d . . .
O7 O 0.66264(17) 0.41534(12) 0.11750(11) 0.0447(5) Uani 1 1 d . . .
O8 O 0.69239(17) 0.26103(12) 0.19867(11) 0.0443(5) Uani 1 1 d . . .
O9 O 0.86538(16) 0.34388(13) 0.13259(11) 0.0448(5) Uani 1 1 d . . .
P1 P 0.17696(6) 0.62626(4) 0.39120(4) 0.02758(17) Uani 1 1 d . . .
P2 P 0.87589(6) 0.05764(4) 0.26838(4) 0.02573(16) Uani 1 1 d . . .
P3 P 0.40594(6) 0.28714(4) 0.06186(4) 0.02648(16) Uani 1 1 d . . .
S1 S 0.28401(6) 0.99838(5) 0.17154(4) 0.03439(18) Uani 1 1 d . . .
S2 S 0.23187(6) 0.31053(5) 0.53888(4) 0.03482(18) Uani 1 1 d . . .
S3 S 0.74174(6) 0.34644(5) 0.16307(4) 0.03054(17) Uani 1 1 d . . .
Si1 Si 0.43177(7) 0.64311(5) 0.30920(4) 0.0348(2) Uani 1 1 d . . .
Si2 Si 0.64006(7) 0.01930(5) 0.37082(4) 0.03137(19) Uani 1 1 d . . .
Si3 Si 0.19284(7) 0.31842(5) -0.03114(4) 0.03219(19) Uani 1 1 d . . .
C11 C -0.0559(3) 0.5648(2) 0.2799(2) 0.0668(11) Uani 1 1 d . . .
H11A H -0.1146 0.6083 0.2494 0.100 Uiso 1 1 calc R . .
H11B H -0.0990 0.5206 0.3228 0.100 Uiso 1 1 calc R . .
H11C H -0.0060 0.5355 0.2494 0.100 Uiso 1 1 calc R . .
C12 C -0.0672(3) 0.7674(2) 0.2460(2) 0.0695(12) Uani 1 1 d . . .
H12A H -0.0211 0.8114 0.2047 0.104 Uiso 1 1 calc R . .
H12B H -0.1166 0.7964 0.2769 0.104 Uiso 1 1 calc R . .
H12C H -0.1200 0.7404 0.2257 0.104 Uiso 1 1 calc R . .
C13 C 0.3598(3) 0.6321(3) 0.23308(17) 0.0642(10) Uani 1 1 d . . .
H13A H 0.3453 0.5699 0.2463 0.096 Uiso 1 1 calc R . .
H13B H 0.4134 0.6525 0.1864 0.096 Uiso 1 1 calc R . .
H13C H 0.2827 0.6680 0.2263 0.096 Uiso 1 1 calc R . .
C27 C 1.1140(3) 0.1399(2) 0.36364(18) 0.0495(8) Uani 1 1 d . . .
H27A H 1.1898 0.1053 0.3799 0.074 Uiso 1 1 calc R . .
H27B H 1.0686 0.1529 0.4055 0.074 Uiso 1 1 calc R . .
H27C H 1.1322 0.1955 0.3219 0.074 Uiso 1 1 calc R . .
C29 C 0.5464(3) 0.12257(19) 0.36341(18) 0.0563(9) Uani 1 1 d . . .
H29A H 0.5990 0.1714 0.3493 0.084 Uiso 1 1 calc R . .
H29B H 0.5003 0.1149 0.4118 0.084 Uiso 1 1 calc R . .
H29C H 0.4905 0.1361 0.3251 0.084 Uiso 1 1 calc R . .
C44 C 0.7291(3) 0.22155(19) -0.03091(18) 0.0488(8) Uani 1 1 d . . .
H44A H 0.7156 0.2057 -0.0728 0.073 Uiso 1 1 calc R . .
H44B H 0.7489 0.1677 0.0120 0.073 Uiso 1 1 calc R . .
H44C H 0.7964 0.2601 -0.0460 0.073 Uiso 1 1 calc R . .
C46 C 0.1065(3) 0.2235(2) -0.01919(18) 0.0596(10) Uani 1 1 d . . .
H46A H 0.1601 0.1692 -0.0052 0.089 Uiso 1 1 calc R . .
H46B H 0.0739 0.2336 -0.0664 0.089 Uiso 1 1 calc R . .
H46C H 0.0397 0.2176 0.0203 0.089 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0263(14) 0.0376(16) 0.0317(16) -0.0109(14) -0.0035(12) -0.0042(12)
C2 0.0290(15) 0.0374(16) 0.0197(14) -0.0070(13) -0.0048(11) -0.0047(12)
C3 0.0261(15) 0.0450(17) 0.0232(14) -0.0115(14) -0.0055(12) -0.0052(13)
C4 0.0262(15) 0.0488(18) 0.0301(16) -0.0138(14) -0.0078(12) 0.0006(13)
C5 0.0342(16) 0.057(2) 0.0357(17) -0.0242(16) -0.0035(13) -0.0014(14)
C6 0.0366(17) 0.070(2) 0.0465(19) -0.0337(18) -0.0034(15) -0.0141(16)
C7 0.0357(16) 0.0288(15) 0.0348(16) -0.0101(14) -0.0072(13) -0.0058(13)
C8 0.0400(17) 0.0424(18) 0.0381(17) -0.0214(15) -0.0154(14) 0.0013(14)
C9 0.0370(17) 0.0476(19) 0.0319(16) -0.0166(15) -0.0149(13) 0.0084(14)
C10 0.0365(16) 0.0305(16) 0.0328(16) -0.0067(13) -0.0085(13) -0.0028(13)
C14 0.051(2) 0.048(2) 0.0451(19) -0.0080(17) -0.0059(16) -0.0088(16)
C15 0.0443(19) 0.049(2) 0.053(2) -0.0192(17) 0.0093(16) 0.0033(15)
C16 0.0389(18) 0.0417(19) 0.048(2) -0.0193(17) -0.0033(15) -0.0145(15)
C17 0.0273(14) 0.0354(16) 0.0297(15) -0.0128(13) 0.0007(12) -0.0051(12)
C18 0.0300(15) 0.0301(15) 0.0209(13) -0.0089(12) -0.0042(11) -0.0020(12)
C19 0.0294(15) 0.0327(16) 0.0246(14) -0.0117(13) -0.0065(12) -0.0016(12)
C20 0.0222(14) 0.0413(17) 0.0321(15) -0.0181(14) -0.0065(12) -0.0012(12)
C21 0.0399(17) 0.0488(18) 0.0338(16) -0.0223(15) 0.0047(13) -0.0069(14)
C22 0.0352(17) 0.059(2) 0.0466(19) -0.0311(17) -0.0034(14) -0.0119(15)
C23 0.0301(15) 0.0303(15) 0.0328(16) -0.0132(13) -0.0046(12) -0.0009(12)
C24 0.0325(15) 0.0369(17) 0.0265(15) -0.0116(13) -0.0070(12) -0.0047(13)
C25 0.0289(15) 0.0390(17) 0.0282(15) -0.0108(14) -0.0087(12) -0.0007(13)
C26 0.0268(14) 0.0331(16) 0.0375(16) -0.0154(14) -0.0055(12) -0.0006(12)
C28 0.0471(19) 0.050(2) 0.0463(19) -0.0171(17) -0.0227(16) 0.0098(16)
C30 0.053(2) 0.065(2) 0.0302(17) -0.0155(17) -0.0047(15) -0.0100(17)
C31 0.0414(18) 0.052(2) 0.0437(19) -0.0101(17) 0.0037(15) -0.0163(15)
C32 0.0278(16) 0.0403(18) 0.0462(19) -0.0138(16) -0.0063(14) -0.0024(14)
C33 0.0285(14) 0.0344(16) 0.0294(15) -0.0103(13) -0.0085(12) -0.0017(12)
C34 0.0328(15) 0.0292(15) 0.0240(14) -0.0073(13) -0.0059(12) -0.0025(12)
C35 0.0271(15) 0.0316(16) 0.0268(15) -0.0088(13) -0.0024(12) -0.0052(12)
C36 0.0263(14) 0.0402(17) 0.0291(15) -0.0114(14) -0.0004(12) -0.0083(12)
C37 0.0353(16) 0.0476(18) 0.0389(17) -0.0203(15) -0.0100(14) -0.0018(14)
C38 0.0278(15) 0.0520(19) 0.0494(19) -0.0250(17) -0.0049(14) 0.0001(14)
C39 0.0270(14) 0.0260(14) 0.0325(15) -0.0129(13) -0.0048(12) -0.0025(11)
C40 0.0253(14) 0.0341(16) 0.0276(15) -0.0119(13) -0.0054(12) -0.0051(12)
C41 0.0247(14) 0.0378(17) 0.0315(15) -0.0150(14) -0.0031(12) 0.0000(12)
C42 0.0352(16) 0.0282(15) 0.0311(15) -0.0116(13) -0.0084(13) 0.0001(12)
C43 0.0384(17) 0.0407(18) 0.0421(18) -0.0139(15) 0.0043(14) -0.0105(14)
C45 0.0425(18) 0.081(2) 0.0341(18) -0.0166(18) -0.0072(15) 0.0018(17)
C47 0.051(2) 0.051(2) 0.044(2) -0.0046(17) -0.0060(16) 0.0082(16)
C48 0.0360(17) 0.0336(17) 0.0356(17) -0.0120(14) -0.0126(14) 0.0010(14)
F1 0.0522(11) 0.0677(13) 0.0623(12) -0.0351(11) -0.0201(10) -0.0012(10)
F2 0.1196(19) 0.0898(16) 0.0552(13) -0.0296(13) 0.0343(13) -0.0661(15)
F3 0.0394(10) 0.0800(14) 0.0813(14) -0.0547(12) -0.0076(10) 0.0110(10)
F4 0.0415(10) 0.0775(13) 0.0465(11) -0.0208(10) -0.0136(9) -0.0101(9)
F5 0.0462(11) 0.0621(12) 0.0540(12) -0.0124(10) 0.0049(9) -0.0202(10)
F6 0.0575(11) 0.0575(12) 0.0602(12) -0.0290(10) -0.0018(10) 0.0095(9)
F7 0.0761(13) 0.0590(12) 0.0452(11) -0.0203(10) -0.0357(10) 0.0189(10)
F8 0.0453(11) 0.0929(14) 0.0630(12) -0.0522(12) 0.0021(9) -0.0055(10)
F9 0.0857(14) 0.0429(11) 0.0607(12) -0.0248(10) -0.0177(11) -0.0193(10)
N1 0.0250(12) 0.0404(14) 0.0278(12) -0.0138(11) -0.0038(10) -0.0045(10)
N2 0.0212(11) 0.0348(13) 0.0222(11) -0.0100(10) -0.0057(9) -0.0017(9)
N3 0.0241(12) 0.0357(13) 0.0281(12) -0.0098(11) -0.0053(10) -0.0079(10)
O1 0.0592(14) 0.0500(14) 0.0786(17) -0.0355(13) -0.0265(13) 0.0229(11)
O2 0.0747(16) 0.0484(14) 0.0523(14) -0.0095(12) 0.0176(12) -0.0200(12)
O3 0.0308(12) 0.112(2) 0.0801(17) -0.0667(16) -0.0107(12) -0.0033(12)
O4 0.0483(13) 0.0396(12) 0.0580(14) -0.0193(11) -0.0072(11) 0.0096(10)
O5 0.0477(13) 0.0456(13) 0.0482(13) -0.0111(11) 0.0025(11) -0.0169(11)
O6 0.0307(11) 0.0719(15) 0.0579(14) -0.0292(13) -0.0193(10) 0.0042(11)
O7 0.0483(12) 0.0479(13) 0.0398(12) -0.0148(11) -0.0234(10) 0.0054(10)
O8 0.0465(12) 0.0375(12) 0.0540(13) -0.0200(11) -0.0046(11) -0.0128(10)
O9 0.0299(11) 0.0588(14) 0.0514(13) -0.0268(12) 0.0001(10) -0.0087(10)
P1 0.0260(4) 0.0288(4) 0.0283(4) -0.0096(3) -0.0057(3) -0.0036(3)
P2 0.0229(4) 0.0279(4) 0.0279(4) -0.0120(3) -0.0036(3) -0.0012(3)
P3 0.0250(4) 0.0265(4) 0.0288(4) -0.0104(3) -0.0059(3) -0.0014(3)
S1 0.0263(4) 0.0367(4) 0.0402(4) -0.0153(4) -0.0030(3) 0.0002(3)
S2 0.0262(4) 0.0373(4) 0.0407(4) -0.0140(4) -0.0075(3) 0.0012(3)
S3 0.0278(4) 0.0343(4) 0.0334(4) -0.0151(3) -0.0081(3) -0.0026(3)
Si1 0.0310(4) 0.0432(5) 0.0309(4) -0.0147(4) 0.0002(3) -0.0060(4)
Si2 0.0312(4) 0.0342(4) 0.0264(4) -0.0104(4) 0.0015(3) -0.0016(3)
Si3 0.0286(4) 0.0364(5) 0.0297(4) -0.0082(4) -0.0079(3) -0.0043(3)
C11 0.074(3) 0.066(2) 0.079(3) -0.038(2) -0.045(2) 0.001(2)
C12 0.093(3) 0.056(2) 0.068(3) -0.027(2) -0.055(2) 0.027(2)
C13 0.054(2) 0.113(3) 0.0372(19) -0.038(2) 0.0033(16) -0.024(2)
C27 0.050(2) 0.052(2) 0.059(2) -0.0290(18) -0.0229(17) -0.0019(16)
C29 0.064(2) 0.047(2) 0.047(2) -0.0165(17) 0.0165(17) 0.0069(17)
C44 0.0398(18) 0.0466(19) 0.060(2) -0.0253(18) 0.0019(16) 0.0063(15)
C46 0.075(3) 0.059(2) 0.047(2) -0.0095(18) -0.0300(19) -0.0228(19)
#==============================================================================
# MOLECULAR GEOMETRY
_geom_special_details
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.518(3) . ?
C1 P1 1.773(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.331(3) . ?
C2 C5 1.492(3) . ?
C3 C6 1.497(4) . ?
C3 C4 1.508(3) . ?
C4 N1 1.504(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.498(4) . ?
C7 P1 1.801(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.322(4) . ?
C8 C11 1.504(4) . ?
C9 C12 1.507(4) . ?
C9 C10 1.509(4) . ?
C10 P1 1.797(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C14 Si1 1.833(3) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 Si1 1.855(3) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 F2 1.321(3) . ?
C16 F1 1.328(3) . ?
C16 F3 1.330(3) . ?
C16 S1 1.811(3) . ?
C17 C18 1.522(3) . ?
C17 P2 1.782(3) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.328(3) . ?
C18 C21 1.491(3) . ?
C19 C22 1.501(3) . ?
C19 C20 1.508(3) . ?
C20 N2 1.505(3) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.509(3) . ?
C23 P2 1.805(2) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.334(3) . ?
C24 C27 1.514(4) . ?
C25 C28 1.505(4) . ?
C25 C26 1.512(3) . ?
C26 P2 1.798(3) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C30 Si2 1.853(3) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 Si2 1.843(3) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 F6 1.328(3) . ?
C32 F5 1.333(3) . ?
C32 F4 1.334(3) . ?
C32 S2 1.817(3) . ?
C33 C34 1.512(3) . ?
C33 P3 1.781(3) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.330(3) . ?
C34 C37 1.505(3) . ?
C35 C38 1.500(3) . ?
C35 C36 1.517(3) . ?
C36 N3 1.515(3) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C40 1.509(3) . ?
C39 P3 1.790(3) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 C41 1.330(3) . ?
C40 C43 1.502(3) . ?
C41 C44 1.496(3) . ?
C41 C42 1.517(4) . ?
C42 P3 1.804(2) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C45 Si3 1.854(3) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C47 Si3 1.849(3) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 F9 1.324(3) . ?
C48 F8 1.325(3) . ?
C48 F7 1.325(3) . ?
C48 S3 1.818(3) . ?
N1 P1 1.634(2) . ?
N1 Si1 1.769(2) . ?
N2 P2 1.630(2) . ?
N2 Si2 1.767(2) . ?
N3 P3 1.632(2) . ?
N3 Si3 1.765(2) . ?
O1 S1 1.422(2) . ?
O2 S1 1.428(2) . ?
O3 S1 1.421(2) . ?
O4 S2 1.4337(19) . ?
O5 S2 1.435(2) . ?
O6 S2 1.4304(19) . ?
O7 S3 1.4316(19) . ?
O8 S3 1.4420(19) . ?
O9 S3 1.4309(19) . ?
Si1 C13 1.853(3) . ?
Si2 C29 1.851(3) . ?
Si3 C46 1.852(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 P1 108.65(18) . . ?
C2 C1 H1A 110.0 . . ?
P1 C1 H1A 110.0 . . ?
C2 C1 H1B 110.0 . . ?
P1 C1 H1B 110.0 . . ?
H1A C1 H1B 108.3 . . ?
C3 C2 C5 126.9(2) . . ?
C3 C2 C1 117.4(2) . . ?
C5 C2 C1 115.7(2) . . ?
C2 C3 C6 125.1(3) . . ?
C2 C3 C4 118.9(2) . . ?
C6 C3 C4 116.1(2) . . ?
N1 C4 C3 114.2(2) . . ?
N1 C4 H4A 108.7 . . ?
C3 C4 H4A 108.7 . . ?
N1 C4 H4B 108.7 . . ?
C3 C4 H4B 108.7 . . ?
H4A C4 H4B 107.6 . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 P1 104.23(18) . . ?
C8 C7 H7A 110.9 . . ?
P1 C7 H7A 110.9 . . ?
C8 C7 H7B 110.9 . . ?
P1 C7 H7B 110.9 . . ?
H7A C7 H7B 108.9 . . ?
C9 C8 C7 117.0(2) . . ?
C9 C8 C11 126.7(3) . . ?
C7 C8 C11 116.3(2) . . ?
C8 C9 C12 126.7(3) . . ?
C8 C9 C10 117.1(2) . . ?
C12 C9 C10 116.1(2) . . ?
C9 C10 P1 103.94(18) . . ?
C9 C10 H10A 111.0 . . ?
P1 C10 H10A 111.0 . . ?
C9 C10 H10B 111.0 . . ?
P1 C10 H10B 111.0 . . ?
H10A C10 H10B 109.0 . . ?
Si1 C14 H14A 109.5 . . ?
Si1 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
Si1 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si1 C15 H15A 109.5 . . ?
Si1 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
Si1 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
F2 C16 F1 106.9(3) . . ?
F2 C16 F3 106.9(3) . . ?
F1 C16 F3 107.3(2) . . ?
F2 C16 S1 111.58(19) . . ?
F1 C16 S1 111.8(2) . . ?
F3 C16 S1 112.1(2) . . ?
C18 C17 P2 108.69(18) . . ?
C18 C17 H17A 110.0 . . ?
P2 C17 H17A 110.0 . . ?
C18 C17 H17B 110.0 . . ?
P2 C17 H17B 110.0 . . ?
H17A C17 H17B 108.3 . . ?
C19 C18 C21 127.0(2) . . ?
C19 C18 C17 117.4(2) . . ?
C21 C18 C17 115.6(2) . . ?
C18 C19 C22 125.4(2) . . ?
C18 C19 C20 118.8(2) . . ?
C22 C19 C20 115.8(2) . . ?
N2 C20 C19 113.06(19) . . ?
N2 C20 H20A 109.0 . . ?
C19 C20 H20A 109.0 . . ?
N2 C20 H20B 109.0 . . ?
C19 C20 H20B 109.0 . . ?
H20A C20 H20B 107.8 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 P2 103.70(17) . . ?
C24 C23 H23A 111.0 . . ?
P2 C23 H23A 111.0 . . ?
C24 C23 H23B 111.0 . . ?
P2 C23 H23B 111.0 . . ?
H23A C23 H23B 109.0 . . ?
C25 C24 C23 117.4(2) . . ?
C25 C24 C27 125.7(2) . . ?
C23 C24 C27 116.9(2) . . ?
C24 C25 C28 126.5(2) . . ?
C24 C25 C26 116.5(2) . . ?
C28 C25 C26 117.0(2) . . ?
C25 C26 P2 104.29(17) . . ?
C25 C26 H26A 110.9 . . ?
P2 C26 H26A 110.9 . . ?
C25 C26 H26B 110.9 . . ?
P2 C26 H26B 110.9 . . ?
H26A C26 H26B 108.9 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Si2 C30 H30A 109.5 . . ?
Si2 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
Si2 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
Si2 C31 H31A 109.5 . . ?
Si2 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
Si2 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
F6 C32 F5 107.0(2) . . ?
F6 C32 F4 107.2(2) . . ?
F5 C32 F4 106.5(2) . . ?
F6 C32 S2 111.9(2) . . ?
F5 C32 S2 111.8(2) . . ?
F4 C32 S2 112.12(19) . . ?
C34 C33 P3 108.87(17) . . ?
C34 C33 H33A 109.9 . . ?
P3 C33 H33A 109.9 . . ?
C34 C33 H33B 109.9 . . ?
P3 C33 H33B 109.9 . . ?
H33A C33 H33B 108.3 . . ?
C35 C34 C37 126.5(2) . . ?
C35 C34 C33 117.7(2) . . ?
C37 C34 C33 115.8(2) . . ?
C34 C35 C38 125.4(2) . . ?
C34 C35 C36 118.9(2) . . ?
C38 C35 C36 115.7(2) . . ?
N3 C36 C35 113.2(2) . . ?
N3 C36 H36A 108.9 . . ?
C35 C36 H36A 108.9 . . ?
N3 C36 H36B 108.9 . . ?
C35 C36 H36B 108.9 . . ?
H36A C36 H36B 107.7 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C35 C38 H38A 109.5 . . ?
C35 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C35 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C40 C39 P3 104.45(17) . . ?
C40 C39 H39A 110.9 . . ?
P3 C39 H39A 110.9 . . ?
C40 C39 H39B 110.9 . . ?
P3 C39 H39B 110.9 . . ?
H39A C39 H39B 108.9 . . ?
C41 C40 C43 126.0(2) . . ?
C41 C40 C39 116.6(2) . . ?
C43 C40 C39 117.4(2) . . ?
C40 C41 C44 126.5(3) . . ?
C40 C41 C42 116.7(2) . . ?
C44 C41 C42 116.8(2) . . ?
C41 C42 P3 103.48(17) . . ?
C41 C42 H42A 111.1 . . ?
P3 C42 H42A 111.1 . . ?
C41 C42 H42B 111.1 . . ?
P3 C42 H42B 111.1 . . ?
H42A C42 H42B 109.0 . . ?
C40 C43 H43A 109.5 . . ?
C40 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C40 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
Si3 C45 H45A 109.5 . . ?
Si3 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
Si3 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
Si3 C47 H47A 109.5 . . ?
Si3 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
Si3 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
F9 C48 F8 106.9(2) . . ?
F9 C48 F7 106.5(2) . . ?
F8 C48 F7 107.0(2) . . ?
F9 C48 S3 112.0(2) . . ?
F8 C48 S3 111.70(19) . . ?
F7 C48 S3 112.34(18) . . ?
C4 N1 P1 115.06(17) . . ?
C4 N1 Si1 116.38(16) . . ?
P1 N1 Si1 127.82(13) . . ?
C20 N2 P2 114.88(16) . . ?
C20 N2 Si2 116.77(15) . . ?
P2 N2 Si2 127.79(12) . . ?
C36 N3 P3 115.31(16) . . ?
C36 N3 Si3 116.10(16) . . ?
P3 N3 Si3 128.57(13) . . ?
N1 P1 C1 104.99(11) . . ?
N1 P1 C10 116.24(12) . . ?
C1 P1 C10 110.37(13) . . ?
N1 P1 C7 117.46(12) . . ?
C1 P1 C7 110.98(13) . . ?
C10 P1 C7 96.80(12) . . ?
N2 P2 C17 105.22(11) . . ?
N2 P2 C26 114.99(12) . . ?
C17 P2 C26 111.47(12) . . ?
N2 P2 C23 118.33(11) . . ?
C17 P2 C23 109.62(12) . . ?
C26 P2 C23 97.22(11) . . ?
N3 P3 C33 104.97(12) . . ?
N3 P3 C39 115.54(11) . . ?
C33 P3 C39 110.51(12) . . ?
N3 P3 C42 119.30(11) . . ?
C33 P3 C42 109.63(12) . . ?
C39 P3 C42 96.79(12) . . ?
O3 S1 O1 115.08(14) . . ?
O3 S1 O2 116.49(15) . . ?
O1 S1 O2 113.53(14) . . ?
O3 S1 C16 104.25(13) . . ?
O1 S1 C16 103.27(14) . . ?
O2 S1 C16 101.69(13) . . ?
O6 S2 O4 115.25(12) . . ?
O6 S2 O5 115.78(13) . . ?
O4 S2 O5 114.32(12) . . ?
O6 S2 C32 103.60(13) . . ?
O4 S2 C32 102.41(13) . . ?
O5 S2 C32 102.88(13) . . ?
O9 S3 O7 115.96(13) . . ?
O9 S3 O8 114.51(12) . . ?
O7 S3 O8 115.02(12) . . ?
O9 S3 C48 103.76(12) . . ?
O7 S3 C48 102.10(12) . . ?
O8 S3 C48 102.85(12) . . ?
N1 Si1 C14 109.34(13) . . ?
N1 Si1 C13 108.43(13) . . ?
C14 Si1 C13 111.13(15) . . ?
N1 Si1 C15 107.16(12) . . ?
C14 Si1 C15 110.00(14) . . ?
C13 Si1 C15 110.66(16) . . ?
N2 Si2 C31 108.78(12) . . ?
N2 Si2 C29 108.44(12) . . ?
C31 Si2 C29 110.07(15) . . ?
N2 Si2 C30 108.37(12) . . ?
C31 Si2 C30 109.46(14) . . ?
C29 Si2 C30 111.65(15) . . ?
N3 Si3 C47 108.59(13) . . ?
N3 Si3 C46 108.76(12) . . ?
C47 Si3 C46 109.53(16) . . ?
N3 Si3 C45 108.62(12) . . ?
C47 Si3 C45 110.70(15) . . ?
C46 Si3 C45 110.58(16) . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si1 C13 H13A 109.5 . . ?
Si1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
Si1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
Si2 C29 H29A 109.5 . . ?
Si2 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
Si2 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
Si3 C46 H46A 109.5 . . ?
Si3 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
Si3 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 C1 C2 C3 -50.3(3) . . . . ?
P1 C1 C2 C5 129.2(2) . . . . ?
C5 C2 C3 C6 1.5(5) . . . . ?
C1 C2 C3 C6 -179.1(2) . . . . ?
C5 C2 C3 C4 -179.7(2) . . . . ?
C1 C2 C3 C4 -0.4(4) . . . . ?
C2 C3 C4 N1 51.4(3) . . . . ?
C6 C3 C4 N1 -129.7(3) . . . . ?
P1 C7 C8 C9 6.8(3) . . . . ?
P1 C7 C8 C11 -171.6(2) . . . . ?
C7 C8 C9 C12 -178.4(3) . . . . ?
C11 C8 C9 C12 -0.3(5) . . . . ?
C7 C8 C9 C10 -0.7(4) . . . . ?
C11 C8 C9 C10 177.4(3) . . . . ?
C8 C9 C10 P1 -5.7(3) . . . . ?
C12 C9 C10 P1 172.2(2) . . . . ?
P2 C17 C18 C19 49.5(3) . . . . ?
P2 C17 C18 C21 -130.2(2) . . . . ?
C21 C18 C19 C22 0.8(4) . . . . ?
C17 C18 C19 C22 -178.8(2) . . . . ?
C21 C18 C19 C20 -179.1(2) . . . . ?
C17 C18 C19 C20 1.2(4) . . . . ?
C18 C19 C20 N2 -53.8(3) . . . . ?
C22 C19 C20 N2 126.2(2) . . . . ?
P2 C23 C24 C25 -7.7(3) . . . . ?
P2 C23 C24 C27 172.4(2) . . . . ?
C23 C24 C25 C28 -178.6(3) . . . . ?
C27 C24 C25 C28 1.3(5) . . . . ?
C23 C24 C25 C26 2.2(4) . . . . ?
C27 C24 C25 C26 -177.9(3) . . . . ?
C24 C25 C26 P2 4.6(3) . . . . ?
C28 C25 C26 P2 -174.7(2) . . . . ?
P3 C33 C34 C35 50.0(3) . . . . ?
P3 C33 C34 C37 -128.7(2) . . . . ?
C37 C34 C35 C38 -1.5(5) . . . . ?
C33 C34 C35 C38 179.9(2) . . . . ?
C37 C34 C35 C36 179.4(2) . . . . ?
C33 C34 C35 C36 0.8(4) . . . . ?
C34 C35 C36 N3 -52.1(3) . . . . ?
C38 C35 C36 N3 128.7(2) . . . . ?
P3 C39 C40 C41 7.2(3) . . . . ?
P3 C39 C40 C43 -173.06(19) . . . . ?
C43 C40 C41 C44 3.2(4) . . . . ?
C39 C40 C41 C44 -177.0(3) . . . . ?
C43 C40 C41 C42 -176.9(2) . . . . ?
C39 C40 C41 C42 2.8(3) . . . . ?
C40 C41 C42 P3 -11.2(3) . . . . ?
C44 C41 C42 P3 168.7(2) . . . . ?
C3 C4 N1 P1 -41.6(3) . . . . ?
C3 C4 N1 Si1 129.3(2) . . . . ?
C19 C20 N2 P2 45.4(3) . . . . ?
C19 C20 N2 Si2 -142.56(18) . . . . ?
C35 C36 N3 P3 42.8(3) . . . . ?
C35 C36 N3 Si3 -135.68(19) . . . . ?
C4 N1 P1 C1 -7.0(2) . . . . ?
Si1 N1 P1 C1 -176.67(15) . . . . ?
C4 N1 P1 C10 115.27(19) . . . . ?
Si1 N1 P1 C10 -54.4(2) . . . . ?
C4 N1 P1 C7 -130.84(19) . . . . ?
Si1 N1 P1 C7 59.5(2) . . . . ?
C2 C1 P1 N1 51.2(2) . . . . ?
C2 C1 P1 C10 -74.8(2) . . . . ?
C2 C1 P1 C7 179.10(17) . . . . ?
C9 C10 P1 N1 133.38(18) . . . . ?
C9 C10 P1 C1 -107.23(19) . . . . ?
C9 C10 P1 C7 8.2(2) . . . . ?
C8 C7 P1 N1 -132.87(18) . . . . ?
C8 C7 P1 C1 106.4(2) . . . . ?
C8 C7 P1 C10 -8.6(2) . . . . ?
C20 N2 P2 C17 3.5(2) . . . . ?
Si2 N2 P2 C17 -167.49(15) . . . . ?
C20 N2 P2 C26 -119.54(18) . . . . ?
Si2 N2 P2 C26 69.46(18) . . . . ?
C20 N2 P2 C23 126.32(18) . . . . ?
Si2 N2 P2 C23 -44.7(2) . . . . ?
C18 C17 P2 N2 -49.1(2) . . . . ?
C18 C17 P2 C26 76.1(2) . . . . ?
C18 C17 P2 C23 -177.37(17) . . . . ?
C25 C26 P2 N2 -133.71(17) . . . . ?
C25 C26 P2 C17 106.65(18) . . . . ?
C25 C26 P2 C23 -7.8(2) . . . . ?
C24 C23 P2 N2 132.22(17) . . . . ?
C24 C23 P2 C17 -107.19(19) . . . . ?
C24 C23 P2 C26 8.7(2) . . . . ?
C36 N3 P3 C33 5.5(2) . . . . ?
Si3 N3 P3 C33 -176.28(15) . . . . ?
C36 N3 P3 C39 -116.47(18) . . . . ?
Si3 N3 P3 C39 61.72(19) . . . . ?
C36 N3 P3 C42 128.80(18) . . . . ?
Si3 N3 P3 C42 -53.0(2) . . . . ?
C34 C33 P3 N3 -50.4(2) . . . . ?
C34 C33 P3 C39 74.8(2) . . . . ?
C34 C33 P3 C42 -179.73(17) . . . . ?
C40 C39 P3 N3 -138.92(16) . . . . ?
C40 C39 P3 C33 102.11(18) . . . . ?
C40 C39 P3 C42 -11.83(18) . . . . ?
C41 C42 P3 N3 137.40(17) . . . . ?
C41 C42 P3 C33 -101.63(19) . . . . ?
C41 C42 P3 C39 13.02(19) . . . . ?
F2 C16 S1 O3 -57.4(3) . . . . ?
F1 C16 S1 O3 -177.1(2) . . . . ?
F3 C16 S1 O3 62.4(2) . . . . ?
F2 C16 S1 O1 63.2(3) . . . . ?
F1 C16 S1 O1 -56.5(2) . . . . ?
F3 C16 S1 O1 -177.0(2) . . . . ?
F2 C16 S1 O2 -178.9(2) . . . . ?
F1 C16 S1 O2 61.4(2) . . . . ?
F3 C16 S1 O2 -59.1(2) . . . . ?
F6 C32 S2 O6 60.1(2) . . . . ?
F5 C32 S2 O6 -59.9(2) . . . . ?
F4 C32 S2 O6 -179.4(2) . . . . ?
F6 C32 S2 O4 -179.77(19) . . . . ?
F5 C32 S2 O4 60.2(2) . . . . ?
F4 C32 S2 O4 -59.3(2) . . . . ?
F6 C32 S2 O5 -60.9(2) . . . . ?
F5 C32 S2 O5 179.10(19) . . . . ?
F4 C32 S2 O5 59.6(2) . . . . ?
F9 C48 S3 O9 60.6(2) . . . . ?
F8 C48 S3 O9 -179.50(19) . . . . ?
F7 C48 S3 O9 -59.2(2) . . . . ?
F9 C48 S3 O7 -60.3(2) . . . . ?
F8 C48 S3 O7 59.6(2) . . . . ?
F7 C48 S3 O7 179.9(2) . . . . ?
F9 C48 S3 O8 -179.77(19) . . . . ?
F8 C48 S3 O8 -59.9(2) . . . . ?
F7 C48 S3 O8 60.4(2) . . . . ?
C4 N1 Si1 C14 -67.6(2) . . . . ?
P1 N1 Si1 C14 102.01(18) . . . . ?
C4 N1 Si1 C13 171.1(2) . . . . ?
P1 N1 Si1 C13 -19.3(2) . . . . ?
C4 N1 Si1 C15 51.6(2) . . . . ?
P1 N1 Si1 C15 -138.79(17) . . . . ?
C20 N2 Si2 C31 50.2(2) . . . . ?
P2 N2 Si2 C31 -138.97(16) . . . . ?
C20 N2 Si2 C29 -69.5(2) . . . . ?
P2 N2 Si2 C29 101.33(19) . . . . ?
C20 N2 Si2 C30 169.11(18) . . . . ?
P2 N2 Si2 C30 -20.0(2) . . . . ?
C36 N3 Si3 C47 56.7(2) . . . . ?
P3 N3 Si3 C47 -121.44(18) . . . . ?
C36 N3 Si3 C46 -62.4(2) . . . . ?
P3 N3 Si3 C46 119.43(19) . . . . ?
C36 N3 Si3 C45 177.20(19) . . . . ?
P3 N3 Si3 C45 -1.0(2) . . . . ?
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full 28.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max 0.335
_refine_diff_density_min -0.326
_refine_diff_density_rms 0.066
_database_code_depnum_ccdc_archive 'CCDC 956159'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_is_ch139_[Me3SiNP(C6H8)2][OTf]
_audit_creation_method SHELXL-97
#==============================================================================
# CHEMICAL DATA
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C15 H25 N P Si +, C F3 O3 S -'
_chemical_formula_sum 'C16 H25 F3 N O3 P S Si'
_chemical_formula_weight 427.49
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
#==============================================================================
# CRYSTAL DATA
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/n'
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_Int_Tables_number 14
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 8.7479(3)
_cell_length_b 10.5358(4)
_cell_length_c 42.6705(14)
_cell_angle_alpha 90.00
_cell_angle_beta 93.724(2)
_cell_angle_gamma 90.00
_cell_volume 3924.5(2)
_cell_formula_units_Z 8
_cell_measurement_temperature 173(2)
_cell_measurement_reflns_used 4475
_cell_measurement_theta_min 5.317
_cell_measurement_theta_max 44.016
_exptl_crystal_description plate
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.17
_exptl_crystal_size_min 0.02
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.447
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1792
_exptl_absorpt_coefficient_mu 0.351
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.9331
_exptl_absorpt_correction_T_max 0.9930
_exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)'
#==============================================================================
# EXPERIMENTAL DATA
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 173(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker Apex Kappa II-CCD-diffractometer'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 48811
_diffrn_reflns_av_R_equivalents 0.0887
_diffrn_reflns_av_sigmaI/netI 0.0818
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -55
_diffrn_reflns_limit_l_max 55
_diffrn_reflns_theta_min 1.99
_diffrn_reflns_theta_max 27.50
_reflns_number_total 9008
_reflns_number_gt 5097
_reflns_threshold_expression >2\s(I)
_computing_data_collection 'Bruker Apex V7.51A'
_computing_cell_refinement 'Bruker Apex V7.51A'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material SHELXL-97
#==============================================================================
# REFINEMENT DATA
_refine_special_details
;
All H atoms were positioned geometrically and refined using a
riding model, with C---H = 0.98 (methyl groups), 0.99\%A (methylene groups),
1.00\%A (methine groups) or 0.95 \%A (aryl CH) and with U~iso~(H) =
1.5 times U~eq~(C) (methyl groups) or with U~iso~(H) = 1.2 times
U~eq~(C) (methylene groups, aryl CH, methine groups). Torsion angles
of all methyl groups were allowed to refine.
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0589P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 9008
_refine_ls_number_parameters 561
_refine_ls_number_restraints 19
_refine_ls_R_factor_all 0.1195
_refine_ls_R_factor_gt 0.0550
_refine_ls_wR_factor_ref 0.1360
_refine_ls_wR_factor_gt 0.1172
_refine_ls_goodness_of_fit_ref 1.016
_refine_ls_restrained_S_all 1.016
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
#==============================================================================
# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_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 0.69838(9) 0.22844(7) 0.184168(17) 0.03226(19) Uani 1 1 d . . .
N1 N 0.6967(3) 0.3813(2) 0.17910(6) 0.0377(6) Uani 1 1 d . A .
Si1 Si 0.56228(11) 0.50808(8) 0.17864(2) 0.0459(3) Uani 1 1 d . . .
C1 C 0.5749(5) 0.5710(5) 0.21922(9) 0.0980(17) Uani 1 1 d . A .
H1A H 0.5387 0.5065 0.2335 0.147 Uiso 1 1 calc R . .
H1B H 0.5111 0.6472 0.2202 0.147 Uiso 1 1 calc R . .
H1C H 0.6816 0.5926 0.2254 0.147 Uiso 1 1 calc R . .
C2 C 0.6247(4) 0.6298(3) 0.15076(10) 0.0735(12) Uani 1 1 d . A .
H2A H 0.7280 0.6591 0.1575 0.110 Uiso 1 1 calc R . .
H2B H 0.5536 0.7018 0.1504 0.110 Uiso 1 1 calc R . .
H2C H 0.6255 0.5928 0.1297 0.110 Uiso 1 1 calc R . .
C3 C 0.3647(4) 0.4673(3) 0.16454(8) 0.0544(9) Uani 1 1 d . A .
H3A H 0.3659 0.4234 0.1443 0.082 Uiso 1 1 calc R . .
H3B H 0.3037 0.5451 0.1620 0.082 Uiso 1 1 calc R . .
H3C H 0.3193 0.4118 0.1799 0.082 Uiso 1 1 calc R . .
C4A C 0.9001(10) 0.1964(8) 0.18183(12) 0.0417(17) Uani 0.796(5) 1 d P A 1
H4A H 0.9221 0.1033 0.1829 0.050 Uiso 0.796(5) 1 calc PR A 1
C5A C 0.9815(6) 0.2663(5) 0.20863(14) 0.0434(14) Uani 0.796(5) 1 d P A 1
H5A H 1.0439 0.2241 0.2244 0.052 Uiso 0.796(5) 1 calc PR A 1
C6A C 0.9606(5) 0.3893(5) 0.20874(12) 0.0406(12) Uani 0.796(5) 1 d P A 1
H6A H 1.0036 0.4426 0.2250 0.049 Uiso 0.796(5) 1 calc PR A 1
C7A C 0.8645(5) 0.4394(4) 0.18149(11) 0.0348(10) Uani 0.796(5) 1 d P A 1
H7A H 0.8591 0.5340 0.1826 0.042 Uiso 0.796(5) 1 calc PR A 1
C8A C 0.9354(5) 0.3992(4) 0.15124(10) 0.0476(13) Uani 0.796(5) 1 d P A 1
H8A H 0.8694 0.4279 0.1329 0.057 Uiso 0.796(5) 1 calc PR A 1
H8B H 1.0372 0.4394 0.1502 0.057 Uiso 0.796(5) 1 calc PR A 1
C9A C 0.9519(6) 0.2565(5) 0.15037(12) 0.0515(14) Uani 0.796(5) 1 d P A 1
H9A H 1.0601 0.2339 0.1476 0.062 Uiso 0.796(5) 1 calc PR A 1
H9B H 0.8883 0.2219 0.1323 0.062 Uiso 0.796(5) 1 calc PR A 1
C4B C 0.901(5) 0.191(4) 0.1931(7) 0.0417(17) Uani 0.204(5) 1 d P A 2
H4B H 0.9220 0.1068 0.2032 0.050 Uiso 0.204(5) 1 calc PR A 2
C5B C 0.947(3) 0.2032(19) 0.1614(6) 0.0406(12) Uani 0.204(5) 1 d P A 2
H5B H 1.0064 0.1371 0.1532 0.049 Uiso 0.204(5) 1 calc PR A 2
C6B C 0.911(2) 0.302(2) 0.1434(5) 0.0434(14) Uani 0.204(5) 1 d P A 2
H6B H 0.9222 0.3077 0.1214 0.052 Uiso 0.204(5) 1 calc PR A 2
C7B C 0.845(2) 0.4085(15) 0.1651(4) 0.0348(10) Uani 0.204(5) 1 d P A 2
H7B H 0.8401 0.4917 0.1538 0.042 Uiso 0.204(5) 1 calc PR A 2
C8B C 0.936(3) 0.422(2) 0.1959(5) 0.0515(14) Uani 0.204(5) 1 d P A 2
H8C H 1.0387 0.4550 0.1920 0.062 Uiso 0.204(5) 1 calc PR A 2
H8D H 0.8847 0.4843 0.2089 0.062 Uiso 0.204(5) 1 calc PR A 2
C9B C 0.953(3) 0.305(3) 0.2129(7) 0.0476(13) Uani 0.204(5) 1 d P A 2
H9C H 0.8923 0.3097 0.2316 0.057 Uiso 0.204(5) 1 calc PR A 2
H9D H 1.0619 0.2944 0.2202 0.057 Uiso 0.204(5) 1 calc PR A 2
C10 C 0.6026(4) 0.1537(3) 0.21625(7) 0.0468(8) Uani 1 1 d . A .
H10 H 0.6362 0.1818 0.2380 0.056 Uiso 1 1 calc R . .
C11 C 0.6451(4) 0.0204(3) 0.20740(11) 0.0653(11) Uani 1 1 d . . .
H11 H 0.6774 -0.0437 0.2220 0.078 Uiso 1 1 calc R A .
C12 C 0.6314(4) 0.0044(3) 0.17621(11) 0.0630(11) Uani 1 1 d . A .
H12 H 0.6535 -0.0727 0.1659 0.076 Uiso 1 1 calc R . .
C13 C 0.5778(3) 0.1207(3) 0.15994(7) 0.0449(8) Uani 1 1 d . A .
H13 H 0.5905 0.1238 0.1368 0.054 Uiso 1 1 calc R . .
C14 C 0.4157(3) 0.1472(3) 0.17029(7) 0.0413(8) Uani 1 1 d . . .
H14A H 0.3485 0.0728 0.1659 0.050 Uiso 1 1 calc R A .
H14B H 0.3705 0.2214 0.1589 0.050 Uiso 1 1 calc R . .
C15 C 0.4328(4) 0.1740(3) 0.20593(7) 0.0483(8) Uani 1 1 d . A .
H15A H 0.4017 0.2622 0.2103 0.058 Uiso 1 1 calc R . .
H15B H 0.3677 0.1153 0.2173 0.058 Uiso 1 1 calc R . .
S1 S 0.03272(10) 0.80128(7) 0.184683(19) 0.0436(2) Uani 1 1 d . . .
O1 O 0.0584(3) 0.6999(2) 0.16340(5) 0.0630(7) Uani 1 1 d . . .
O2 O 0.0407(3) 0.9252(2) 0.17112(6) 0.0820(9) Uani 1 1 d . . .
O3 O -0.0878(3) 0.7802(2) 0.20548(6) 0.0684(7) Uani 1 1 d . . .
C16 C 0.2018(4) 0.7997(4) 0.21097(8) 0.0571(10) Uani 1 1 d . . .
F1 F 0.2001(3) 0.8852(3) 0.23310(5) 0.1079(9) Uani 1 1 d . . .
F2 F 0.2159(3) 0.6866(2) 0.22575(5) 0.0880(8) Uani 1 1 d . . .
F3 F 0.3282(2) 0.8164(2) 0.19545(5) 0.0821(7) Uani 1 1 d . . .
P2 P 0.12146(9) 0.75012(7) 0.066877(17) 0.03040(19) Uani 1 1 d . . .
N2 N 0.0990(2) 0.90253(19) 0.05990(5) 0.0253(5) Uani 1 1 d . . .
Si2 Si -0.06888(9) 0.99889(7) 0.061475(18) 0.0311(2) Uani 1 1 d . . .
C17 C -0.1701(4) 0.9622(3) 0.09728(7) 0.0482(8) Uani 1 1 d . . .
H17A H -0.2133 0.8764 0.0956 0.072 Uiso 1 1 calc R . .
H17B H -0.2528 1.0237 0.0994 0.072 Uiso 1 1 calc R . .
H17C H -0.0977 0.9670 0.1158 0.072 Uiso 1 1 calc R . .
C18 C -0.0077(4) 1.1674(3) 0.06247(8) 0.0521(9) Uani 1 1 d . . .
H18A H 0.0693 1.1803 0.0799 0.078 Uiso 1 1 calc R . .
H18B H -0.0965 1.2219 0.0654 0.078 Uiso 1 1 calc R . .
H18C H 0.0364 1.1892 0.0426 0.078 Uiso 1 1 calc R . .
C19 C -0.1955(3) 0.9777(3) 0.02544(7) 0.0445(8) Uani 1 1 d . . .
H19A H -0.1364 0.9905 0.0070 0.067 Uiso 1 1 calc R . .
H19B H -0.2791 1.0397 0.0252 0.067 Uiso 1 1 calc R . .
H19C H -0.2382 0.8917 0.0250 0.067 Uiso 1 1 calc R . .
C20 C 0.2544(3) 0.9712(2) 0.06330(6) 0.0309(6) Uani 1 1 d . . .
H20 H 0.2438 1.0587 0.0543 0.037 Uiso 1 1 calc R . .
C21 C 0.3753(3) 0.8998(3) 0.04728(7) 0.0401(7) Uani 1 1 d . . .
H21 H 0.4244 0.9337 0.0299 0.048 Uiso 1 1 calc R . .
C22 C 0.4090(4) 0.7858(3) 0.05906(8) 0.0518(9) Uani 1 1 d . . .
H22 H 0.4873 0.7340 0.0514 0.062 Uiso 1 1 calc R . .
C23 C 0.3139(3) 0.7450(3) 0.08528(8) 0.0469(8) Uani 1 1 d . . .
H23 H 0.3426 0.6587 0.0935 0.056 Uiso 1 1 calc R . .
C24 C 0.3234(4) 0.8477(3) 0.11126(7) 0.0562(9) Uani 1 1 d . . .
H24A H 0.2432 0.8314 0.1261 0.067 Uiso 1 1 calc R . .
H24B H 0.4243 0.8421 0.1231 0.067 Uiso 1 1 calc R . .
C25 C 0.3029(4) 0.9788(3) 0.09798(7) 0.0466(8) Uani 1 1 d . . .
H25A H 0.4003 1.0264 0.1010 0.056 Uiso 1 1 calc R . .
H25B H 0.2240 1.0246 0.1092 0.056 Uiso 1 1 calc R . .
C26 C -0.0251(4) 0.6569(3) 0.08488(8) 0.0485(8) Uani 1 1 d . . .
H26 H -0.0506 0.6813 0.1066 0.058 Uiso 1 1 calc R . .
C27 C 0.0615(4) 0.5312(3) 0.08125(10) 0.0623(11) Uani 1 1 d . . .
H27 H 0.0713 0.4682 0.0972 0.075 Uiso 1 1 calc R . .
C28 C 0.1197(4) 0.5201(3) 0.05417(10) 0.0609(10) Uani 1 1 d . . .
H28 H 0.1734 0.4474 0.0476 0.073 Uiso 1 1 calc R . .
C29 C 0.0919(3) 0.6352(3) 0.03482(8) 0.0435(8) Uani 1 1 d . . .
H29 H 0.1576 0.6459 0.0167 0.052 Uiso 1 1 calc R . .
C30 C -0.0827(4) 0.6458(3) 0.02737(8) 0.0484(8) Uani 1 1 d . . .
H30A H -0.1215 0.5697 0.0158 0.058 Uiso 1 1 calc R . .
H30B H -0.1069 0.7217 0.0143 0.058 Uiso 1 1 calc R . .
C31 C -0.1576(4) 0.6566(3) 0.05923(8) 0.0481(8) Uani 1 1 d . . .
H31A H -0.2177 0.7359 0.0601 0.058 Uiso 1 1 calc R . .
H31B H -0.2267 0.5837 0.0621 0.058 Uiso 1 1 calc R . .
S2A S 0.5132(5) 0.3377(6) 0.07674(11) 0.0382(8) Uani 0.645(15) 1 d PD B 1
O4A O 0.6385(9) 0.2693(12) 0.08957(14) 0.102(4) Uani 0.645(15) 1 d PD B 1
O5A O 0.3659(11) 0.2897(15) 0.0825(3) 0.067(4) Uani 0.645(15) 1 d PD B 1
O6A O 0.5208(8) 0.4726(4) 0.07898(18) 0.073(2) Uani 0.645(15) 1 d PD B 1
C32A C 0.5183(17) 0.3112(11) 0.03510(17) 0.046(2) Uani 0.645(15) 1 d PD B 1
F4A F 0.4987(9) 0.1926(6) 0.0279(2) 0.110(3) Uani 0.645(15) 1 d PD B 1
F5A F 0.6523(10) 0.3496(13) 0.0249(3) 0.090(5) Uani 0.645(15) 1 d PD B 1
F6A F 0.4117(7) 0.3758(11) 0.01869(13) 0.098(3) Uani 0.645(15) 1 d PD B 1
S2B S 0.5162(16) 0.3106(15) 0.0778(3) 0.073(4) Uani 0.355(15) 1 d PD B 2
O4B O 0.3614(18) 0.308(3) 0.0860(5) 0.051(5) Uani 0.355(15) 1 d PD B 2
O5B O 0.609(3) 0.409(3) 0.0900(3) 0.162(12) Uani 0.355(15) 1 d PD B 2
O6B O 0.5864(19) 0.1881(16) 0.0783(6) 0.132(8) Uani 0.355(15) 1 d PD B 2
C32B C 0.514(3) 0.348(2) 0.0368(3) 0.046(2) Uani 0.355(15) 1 d PD B 2
F4B F 0.459(2) 0.4577(18) 0.0304(5) 0.155(9) Uani 0.355(15) 1 d PD B 2
F5B F 0.422(3) 0.264(3) 0.0216(3) 0.164(11) Uani 0.355(15) 1 d PD B 2
F6B F 0.6492(17) 0.343(2) 0.0249(4) 0.065(7) Uani 0.355(15) 1 d PD B 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.0283(4) 0.0341(4) 0.0336(4) -0.0072(3) -0.0041(3) 0.0041(3)
N1 0.0273(14) 0.0408(14) 0.0452(15) 0.0078(11) 0.0022(12) 0.0078(11)
Si1 0.0406(5) 0.0464(5) 0.0483(5) -0.0151(4) -0.0142(4) 0.0177(4)
C1 0.076(3) 0.142(4) 0.072(3) -0.054(3) -0.021(2) 0.057(3)
C2 0.060(3) 0.0339(18) 0.121(3) 0.007(2) -0.035(2) 0.0068(17)
C3 0.041(2) 0.052(2) 0.068(2) -0.0082(17) -0.0050(18) 0.0140(17)
C4A 0.0299(19) 0.033(2) 0.061(5) -0.004(4) -0.004(4) 0.0099(15)
C5A 0.023(3) 0.058(4) 0.048(3) 0.014(3) -0.011(2) 0.004(2)
C6A 0.029(2) 0.052(3) 0.040(3) -0.002(2) -0.010(2) -0.005(2)
C7A 0.037(2) 0.028(2) 0.038(3) -0.0002(18) -0.006(2) -0.0019(17)
C8A 0.035(3) 0.067(3) 0.042(2) 0.006(2) 0.003(2) -0.005(2)
C9A 0.036(3) 0.078(5) 0.041(3) -0.013(3) 0.005(2) 0.006(3)
C4B 0.0299(19) 0.033(2) 0.061(5) -0.004(4) -0.004(4) 0.0099(15)
C5B 0.029(2) 0.052(3) 0.040(3) -0.002(2) -0.010(2) -0.005(2)
C6B 0.023(3) 0.058(4) 0.048(3) 0.014(3) -0.011(2) 0.004(2)
C7B 0.037(2) 0.028(2) 0.038(3) -0.0002(18) -0.006(2) -0.0019(17)
C8B 0.036(3) 0.078(5) 0.041(3) -0.013(3) 0.005(2) 0.006(3)
C9B 0.035(3) 0.067(3) 0.042(2) 0.006(2) 0.003(2) -0.005(2)
C10 0.059(2) 0.0499(19) 0.0306(16) 0.0026(14) -0.0078(16) -0.0133(17)
C11 0.048(2) 0.038(2) 0.107(3) 0.024(2) -0.022(2) -0.0093(16)
C12 0.038(2) 0.044(2) 0.107(3) -0.032(2) 0.001(2) -0.0097(16)
C13 0.0364(19) 0.055(2) 0.0444(19) -0.0210(16) 0.0075(16) -0.0054(16)
C14 0.0285(17) 0.0534(19) 0.0415(18) -0.0086(14) -0.0024(15) -0.0049(15)
C15 0.051(2) 0.056(2) 0.0395(18) -0.0067(15) 0.0150(17) 0.0000(17)
S1 0.0433(5) 0.0426(5) 0.0440(5) -0.0011(4) -0.0039(4) 0.0097(4)
O1 0.0767(19) 0.0532(14) 0.0590(15) -0.0223(12) 0.0039(14) -0.0083(13)
O2 0.114(2) 0.0519(15) 0.0807(19) 0.0267(13) 0.0121(17) 0.0388(15)
O3 0.0387(14) 0.0920(19) 0.0760(18) -0.0009(14) 0.0155(14) 0.0060(13)
C16 0.049(2) 0.074(3) 0.048(2) 0.0040(19) 0.0088(19) -0.010(2)
F1 0.115(2) 0.144(2) 0.0643(15) -0.0449(16) 0.0021(15) -0.0474(18)
F2 0.0683(16) 0.124(2) 0.0714(15) 0.0545(14) 0.0021(13) 0.0178(14)
F3 0.0450(13) 0.122(2) 0.0801(16) 0.0192(14) 0.0083(12) -0.0203(12)
P2 0.0258(4) 0.0295(4) 0.0356(4) 0.0035(3) -0.0008(3) 0.0018(3)
N2 0.0218(12) 0.0299(12) 0.0240(11) -0.0003(9) 0.0003(10) 0.0023(10)
Si2 0.0283(4) 0.0312(4) 0.0335(4) -0.0034(3) -0.0006(4) 0.0058(3)
C17 0.049(2) 0.0490(19) 0.0481(19) -0.0130(15) 0.0142(17) 0.0086(16)
C18 0.051(2) 0.0355(17) 0.069(2) -0.0059(16) -0.0017(19) 0.0109(16)
C19 0.0344(18) 0.0523(19) 0.0457(18) 0.0025(15) -0.0066(15) 0.0110(15)
C20 0.0255(16) 0.0297(15) 0.0366(16) 0.0006(12) -0.0049(13) -0.0038(12)
C21 0.0234(16) 0.0516(19) 0.0454(18) 0.0009(15) 0.0022(14) -0.0043(14)
C22 0.0211(17) 0.060(2) 0.074(2) -0.0133(19) -0.0002(17) 0.0020(15)
C23 0.0301(18) 0.0425(18) 0.066(2) 0.0154(16) -0.0143(17) 0.0038(15)
C24 0.050(2) 0.078(2) 0.0370(18) 0.0113(17) -0.0213(17) -0.0085(19)
C25 0.0389(19) 0.055(2) 0.0438(18) -0.0119(15) -0.0134(16) -0.0050(16)
C26 0.047(2) 0.0466(19) 0.053(2) 0.0063(15) 0.0131(18) -0.0071(16)
C27 0.068(3) 0.0320(18) 0.086(3) 0.0270(18) -0.006(2) -0.0073(17)
C28 0.050(2) 0.038(2) 0.095(3) -0.0036(19) 0.009(2) -0.0001(16)
C29 0.0358(19) 0.0336(16) 0.062(2) -0.0131(15) 0.0114(17) -0.0006(14)
C30 0.039(2) 0.0434(18) 0.062(2) -0.0223(16) -0.0021(17) -0.0021(15)
C31 0.0311(18) 0.0414(18) 0.072(2) -0.0080(16) 0.0089(18) -0.0065(15)
S2A 0.0284(16) 0.0514(17) 0.0346(14) 0.0024(10) 0.0009(11) 0.0050(12)
O4A 0.062(5) 0.189(10) 0.054(3) 0.037(5) -0.010(3) 0.069(6)
O5A 0.052(6) 0.054(4) 0.101(8) 0.004(4) 0.039(4) -0.011(4)
O6A 0.075(4) 0.048(3) 0.098(5) -0.040(3) 0.025(3) -0.025(2)
C32A 0.036(2) 0.054(7) 0.047(2) -0.006(3) 0.006(2) 0.014(5)
F4A 0.126(6) 0.083(4) 0.127(6) -0.070(4) 0.052(5) -0.026(3)
F5A 0.063(8) 0.134(10) 0.080(8) 0.008(6) 0.055(5) 0.006(6)
F6A 0.064(4) 0.174(9) 0.055(3) 0.032(5) -0.007(3) 0.033(5)
S2B 0.084(6) 0.084(8) 0.052(3) 0.015(3) 0.014(4) -0.019(4)
O4B 0.054(10) 0.065(10) 0.037(6) 0.015(6) 0.024(6) 0.028(7)
O5B 0.132(18) 0.28(3) 0.074(9) -0.050(14) 0.001(10) -0.14(2)
O6B 0.094(11) 0.113(11) 0.199(19) 0.114(11) 0.072(11) 0.059(8)
C32B 0.036(2) 0.054(7) 0.047(2) -0.006(3) 0.006(2) 0.014(5)
F4B 0.154(13) 0.136(12) 0.183(17) 0.134(11) 0.083(12) 0.085(10)
F5B 0.176(19) 0.26(3) 0.051(6) -0.028(12) -0.036(9) -0.111(19)
F6B 0.072(15) 0.077(11) 0.044(10) 0.005(8) -0.003(8) -0.001(10)
#==============================================================================
# MOLECULAR GEOMETRY
_geom_special_details
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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 1.625(2) . ?
P1 C4A 1.806(9) . ?
P1 C13 1.825(3) . ?
P1 C10 1.829(3) . ?
P1 C4B 1.83(4) . ?
N1 C7B 1.49(2) . ?
N1 C7A 1.588(5) . ?
N1 Si1 1.779(2) . ?
Si1 C3 1.844(3) . ?
Si1 C1 1.851(4) . ?
Si1 C2 1.855(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4A C5A 1.500(9) . ?
C4A C9A 1.577(8) . ?
C4A H4A 1.0000 . ?
C5A C6A 1.309(7) . ?
C5A H5A 0.9500 . ?
C6A C7A 1.487(6) . ?
C6A H6A 0.9500 . ?
C7A C8A 1.528(6) . ?
C7A H7A 1.0000 . ?
C8A C9A 1.511(7) . ?
C8A H8A 0.9900 . ?
C8A H8B 0.9900 . ?
C9A H9A 0.9900 . ?
C9A H9B 0.9900 . ?
C4B C5B 1.44(3) . ?
C4B C9B 1.52(5) . ?
C4B H4B 1.0000 . ?
C5B C6B 1.32(3) . ?
C5B H5B 0.9500 . ?
C6B C7B 1.59(3) . ?
C6B H6B 0.9500 . ?
C7B C8B 1.50(3) . ?
C7B H7B 1.0000 . ?
C8B C9B 1.43(3) . ?
C8B H8C 0.9900 . ?
C8B H8D 0.9900 . ?
C9B H9C 0.9900 . ?
C9B H9D 0.9900 . ?
C10 C11 1.507(5) . ?
C10 C15 1.537(5) . ?
C10 H10 1.0000 . ?
C11 C12 1.339(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.470(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.538(4) . ?
C13 H13 1.0000 . ?
C14 C15 1.544(4) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
S1 O1 1.429(2) . ?
S1 O2 1.431(2) . ?
S1 O3 1.439(3) . ?
S1 C16 1.797(4) . ?
C16 F1 1.306(4) . ?
C16 F3 1.337(4) . ?
C16 F2 1.350(4) . ?
P2 N2 1.643(2) . ?
P2 C23 1.812(3) . ?
P2 C26 1.824(3) . ?
P2 C29 1.833(3) . ?
N2 C20 1.539(3) . ?
N2 Si2 1.790(2) . ?
Si2 C19 1.850(3) . ?
Si2 C18 1.854(3) . ?
Si2 C17 1.856(3) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.499(4) . ?
C20 C25 1.515(4) . ?
C20 H20 1.0000 . ?
C21 C22 1.328(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.500(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.548(4) . ?
C23 H23 1.0000 . ?
C24 C25 1.499(4) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.538(5) . ?
C26 C31 1.542(4) . ?
C26 H26 1.0000 . ?
C27 C28 1.298(5) . ?
C27 H27 0.9500 . ?
C28 C29 1.478(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.544(4) . ?
C29 H29 1.0000 . ?
C30 C31 1.551(4) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
S2A O4A 1.394(8) . ?
S2A O5A 1.420(9) . ?
S2A O6A 1.426(8) . ?
S2A C32A 1.802(7) . ?
C32A F4A 1.295(12) . ?
C32A F6A 1.318(13) . ?
C32A F5A 1.338(15) . ?
S2B O5B 1.395(15) . ?
S2B O4B 1.420(16) . ?
S2B O6B 1.429(15) . ?
S2B C32B 1.793(12) . ?
C32B F4B 1.272(19) . ?
C32B F6B 1.32(2) . ?
C32B F5B 1.34(2) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 P1 C4A 100.3(3) . . ?
N1 P1 C13 122.78(14) . . ?
C4A P1 C13 112.5(3) . . ?
N1 P1 C10 121.72(14) . . ?
C4A P1 C10 117.2(2) . . ?
C13 P1 C10 83.11(14) . . ?
N1 P1 C4B 103.9(13) . . ?
C4A P1 C4B 15.3(10) . . ?
C13 P1 C4B 120.1(12) . . ?
C10 P1 C4B 103.7(11) . . ?
C7B N1 C7A 29.2(6) . . ?
C7B N1 P1 104.1(6) . . ?
C7A N1 P1 111.91(19) . . ?
C7B N1 Si1 116.3(6) . . ?
C7A N1 Si1 108.60(19) . . ?
P1 N1 Si1 138.26(16) . . ?
N1 Si1 C3 115.69(13) . . ?
N1 Si1 C1 105.04(16) . . ?
C3 Si1 C1 112.74(19) . . ?
N1 Si1 C2 107.72(15) . . ?
C3 Si1 C2 105.11(16) . . ?
C1 Si1 C2 110.5(2) . . ?
Si1 C1 H1A 109.5 . . ?
Si1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Si1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si1 C3 H3A 109.5 . . ?
Si1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Si1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C5A C4A C9A 107.6(6) . . ?
C5A C4A P1 106.5(4) . . ?
C9A C4A P1 107.9(4) . . ?
C5A C4A H4A 111.5 . . ?
C9A C4A H4A 111.5 . . ?
P1 C4A H4A 111.5 . . ?
C6A C5A C4A 115.4(5) . . ?
C6A C5A H5A 122.3 . . ?
C4A C5A H5A 122.3 . . ?
C5A C6A C7A 114.8(4) . . ?
C5A C6A H6A 122.6 . . ?
C7A C6A H6A 122.6 . . ?
C6A C7A C8A 108.8(3) . . ?
C6A C7A N1 112.8(3) . . ?
C8A C7A N1 105.3(3) . . ?
C6A C7A H7A 110.0 . . ?
C8A C7A H7A 110.0 . . ?
N1 C7A H7A 110.0 . . ?
C9A C8A C7A 110.0(3) . . ?
C9A C8A H8A 109.7 . . ?
C7A C8A H8A 109.7 . . ?
C9A C8A H8B 109.7 . . ?
C7A C8A H8B 109.7 . . ?
H8A C8A H8B 108.2 . . ?
C8A C9A C4A 110.2(5) . . ?
C8A C9A H9A 109.6 . . ?
C4A C9A H9A 109.6 . . ?
C8A C9A H9B 109.6 . . ?
C4A C9A H9B 109.6 . . ?
H9A C9A H9B 108.1 . . ?
C5B C4B C9B 111(3) . . ?
C5B C4B P1 96(2) . . ?
C9B C4B P1 101(2) . . ?
C5B C4B H4B 115.2 . . ?
C9B C4B H4B 115.2 . . ?
P1 C4B H4B 115.2 . . ?
C6B C5B C4B 123(3) . . ?
C6B C5B H5B 118.5 . . ?
C4B C5B H5B 118.5 . . ?
C5B C6B C7B 107(2) . . ?
C5B C6B H6B 126.3 . . ?
C7B C6B H6B 126.3 . . ?
N1 C7B C8B 95.2(15) . . ?
N1 C7B C6B 117.1(13) . . ?
C8B C7B C6B 112.7(15) . . ?
N1 C7B H7B 110.3 . . ?
C8B C7B H7B 110.3 . . ?
C6B C7B H7B 110.3 . . ?
C9B C8B C7B 114(2) . . ?
C9B C8B H8C 108.8 . . ?
C7B C8B H8C 108.8 . . ?
C9B C8B H8D 108.8 . . ?
C7B C8B H8D 108.8 . . ?
H8C C8B H8D 107.7 . . ?
C8B C9B C4B 112(2) . . ?
C8B C9B H9C 109.2 . . ?
C4B C9B H9C 109.2 . . ?
C8B C9B H9D 109.2 . . ?
C4B C9B H9D 109.2 . . ?
H9C C9B H9D 107.9 . . ?
C11 C10 C15 107.9(3) . . ?
C11 C10 P1 94.7(2) . . ?
C15 C10 P1 101.9(2) . . ?
C11 C10 H10 116.5 . . ?
C15 C10 H10 116.5 . . ?
P1 C10 H10 116.5 . . ?
C12 C11 C10 111.0(3) . . ?
C12 C11 H11 124.5 . . ?
C10 C11 H11 124.5 . . ?
C11 C12 C13 111.7(3) . . ?
C11 C12 H12 124.2 . . ?
C13 C12 H12 124.2 . . ?
C12 C13 C14 106.7(3) . . ?
C12 C13 P1 95.5(2) . . ?
C14 C13 P1 103.53(19) . . ?
C12 C13 H13 116.2 . . ?
C14 C13 H13 116.2 . . ?
P1 C13 H13 116.2 . . ?
C13 C14 C15 106.5(2) . . ?
C13 C14 H14A 110.4 . . ?
C15 C14 H14A 110.4 . . ?
C13 C14 H14B 110.4 . . ?
C15 C14 H14B 110.4 . . ?
H14A C14 H14B 108.6 . . ?
C10 C15 C14 106.7(2) . . ?
C10 C15 H15A 110.4 . . ?
C14 C15 H15A 110.4 . . ?
C10 C15 H15B 110.4 . . ?
C14 C15 H15B 110.4 . . ?
H15A C15 H15B 108.6 . . ?
O1 S1 O2 114.25(16) . . ?
O1 S1 O3 115.38(15) . . ?
O2 S1 O3 116.52(15) . . ?
O1 S1 C16 103.45(17) . . ?
O2 S1 C16 101.62(18) . . ?
O3 S1 C16 102.71(16) . . ?
F1 C16 F3 108.4(3) . . ?
F1 C16 F2 106.0(3) . . ?
F3 C16 F2 107.1(3) . . ?
F1 C16 S1 113.4(3) . . ?
F3 C16 S1 111.3(2) . . ?
F2 C16 S1 110.3(3) . . ?
N2 P2 C23 101.82(13) . . ?
N2 P2 C26 121.58(13) . . ?
C23 P2 C26 117.39(15) . . ?
N2 P2 C29 120.08(13) . . ?
C23 P2 C29 112.69(15) . . ?
C26 P2 C29 83.65(15) . . ?
C20 N2 P2 110.36(16) . . ?
C20 N2 Si2 116.85(16) . . ?
P2 N2 Si2 129.53(13) . . ?
N2 Si2 C19 110.41(12) . . ?
N2 Si2 C18 107.92(13) . . ?
C19 Si2 C18 106.93(15) . . ?
N2 Si2 C17 110.44(12) . . ?
C19 Si2 C17 111.55(15) . . ?
C18 Si2 C17 109.46(14) . . ?
Si2 C17 H17A 109.5 . . ?
Si2 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Si2 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si2 C18 H18A 109.5 . . ?
Si2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
Si2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si2 C19 H19A 109.5 . . ?
Si2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
Si2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 C25 108.1(2) . . ?
C21 C20 N2 111.5(2) . . ?
C25 C20 N2 107.9(2) . . ?
C21 C20 H20 109.8 . . ?
C25 C20 H20 109.8 . . ?
N2 C20 H20 109.8 . . ?
C22 C21 C20 115.3(3) . . ?
C22 C21 H21 122.4 . . ?
C20 C21 H21 122.4 . . ?
C21 C22 C23 115.0(3) . . ?
C21 C22 H22 122.5 . . ?
C23 C22 H22 122.5 . . ?
C22 C23 C24 109.1(3) . . ?
C22 C23 P2 102.3(2) . . ?
C24 C23 P2 107.1(2) . . ?
C22 C23 H23 112.6 . . ?
C24 C23 H23 112.6 . . ?
P2 C23 H23 112.6 . . ?
C25 C24 C23 111.9(3) . . ?
C25 C24 H24A 109.2 . . ?
C23 C24 H24A 109.2 . . ?
C25 C24 H24B 109.2 . . ?
C23 C24 H24B 109.2 . . ?
H24A C24 H24B 107.9 . . ?
C24 C25 C20 109.9(2) . . ?
C24 C25 H25A 109.7 . . ?
C20 C25 H25A 109.7 . . ?
C24 C25 H25B 109.7 . . ?
C20 C25 H25B 109.7 . . ?
H25A C25 H25B 108.2 . . ?
C27 C26 C31 106.2(3) . . ?
C27 C26 P2 93.3(2) . . ?
C31 C26 P2 102.6(2) . . ?
C27 C26 H26 117.1 . . ?
C31 C26 H26 117.1 . . ?
P2 C26 H26 117.1 . . ?
C28 C27 C26 113.0(3) . . ?
C28 C27 H27 123.5 . . ?
C26 C27 H27 123.5 . . ?
C27 C28 C29 111.3(3) . . ?
C27 C28 H28 124.3 . . ?
C29 C28 H28 124.3 . . ?
C28 C29 C30 107.4(3) . . ?
C28 C29 P2 96.6(2) . . ?
C30 C29 P2 101.29(19) . . ?
C28 C29 H29 116.3 . . ?
C30 C29 H29 116.3 . . ?
P2 C29 H29 116.3 . . ?
C29 C30 C31 107.1(3) . . ?
C29 C30 H30A 110.3 . . ?
C31 C30 H30A 110.3 . . ?
C29 C30 H30B 110.3 . . ?
C31 C30 H30B 110.3 . . ?
H30A C30 H30B 108.6 . . ?
C26 C31 C30 106.4(3) . . ?
C26 C31 H31A 110.5 . . ?
C30 C31 H31A 110.5 . . ?
C26 C31 H31B 110.5 . . ?
C30 C31 H31B 110.5 . . ?
H31A C31 H31B 108.6 . . ?
O4A S2A O5A 116.6(8) . . ?
O4A S2A O6A 117.2(5) . . ?
O5A S2A O6A 112.5(7) . . ?
O4A S2A C32A 103.8(6) . . ?
O5A S2A C32A 101.3(8) . . ?
O6A S2A C32A 102.5(5) . . ?
F4A C32A F6A 107.2(10) . . ?
F4A C32A F5A 108.7(9) . . ?
F6A C32A F5A 106.0(9) . . ?
F4A C32A S2A 111.7(6) . . ?
F6A C32A S2A 112.5(7) . . ?
F5A C32A S2A 110.5(9) . . ?
O5B S2B O4B 117.9(16) . . ?
O5B S2B O6B 115.0(14) . . ?
O4B S2B O6B 113.1(15) . . ?
O5B S2B C32B 99.8(12) . . ?
O4B S2B C32B 107.1(13) . . ?
O6B S2B C32B 101.0(11) . . ?
F4B C32B F6B 106.9(19) . . ?
F4B C32B F5B 107.1(19) . . ?
F6B C32B F5B 108.2(17) . . ?
F4B C32B S2B 112.9(12) . . ?
F6B C32B S2B 114.3(16) . . ?
F5B C32B S2B 107.0(15) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4A P1 N1 C7B 17.9(8) . . . . ?
C13 P1 N1 C7B -107.6(7) . . . . ?
C10 P1 N1 C7B 149.1(7) . . . . ?
C4B P1 N1 C7B 33.0(12) . . . . ?
C4A P1 N1 C7A -11.7(3) . . . . ?
C13 P1 N1 C7A -137.2(2) . . . . ?
C10 P1 N1 C7A 119.5(2) . . . . ?
C4B P1 N1 C7A 3.4(10) . . . . ?
C4A P1 N1 Si1 -177.0(3) . . . . ?
C13 P1 N1 Si1 57.6(3) . . . . ?
C10 P1 N1 Si1 -45.7(3) . . . . ?
C4B P1 N1 Si1 -161.8(10) . . . . ?
C7B N1 Si1 C3 132.3(8) . . . . ?
C7A N1 Si1 C3 162.8(2) . . . . ?
P1 N1 Si1 C3 -31.7(3) . . . . ?
C7B N1 Si1 C1 -102.7(8) . . . . ?
C7A N1 Si1 C1 -72.2(3) . . . . ?
P1 N1 Si1 C1 93.3(3) . . . . ?
C7B N1 Si1 C2 15.1(8) . . . . ?
C7A N1 Si1 C2 45.6(3) . . . . ?
P1 N1 Si1 C2 -148.9(2) . . . . ?
N1 P1 C4A C5A 62.5(5) . . . . ?
C13 P1 C4A C5A -165.4(4) . . . . ?
C10 P1 C4A C5A -71.5(5) . . . . ?
C4B P1 C4A C5A -43(6) . . . . ?
N1 P1 C4A C9A -52.8(5) . . . . ?
C13 P1 C4A C9A 79.3(5) . . . . ?
C10 P1 C4A C9A 173.2(4) . . . . ?
C4B P1 C4A C9A -158(6) . . . . ?
C9A C4A C5A C6A 56.4(7) . . . . ?
P1 C4A C5A C6A -59.2(6) . . . . ?
C4A C5A C6A C7A -2.3(7) . . . . ?
C5A C6A C7A C8A -56.3(6) . . . . ?
C5A C6A C7A N1 60.2(5) . . . . ?
C7B N1 C7A C6A -124.9(14) . . . . ?
P1 N1 C7A C6A -45.5(4) . . . . ?
Si1 N1 C7A C6A 124.2(3) . . . . ?
C7B N1 C7A C8A -6.4(13) . . . . ?
P1 N1 C7A C8A 73.1(3) . . . . ?
Si1 N1 C7A C8A -117.3(3) . . . . ?
C6A C7A C8A C9A 56.3(5) . . . . ?
N1 C7A C8A C9A -64.9(4) . . . . ?
C7A C8A C9A C4A -3.4(6) . . . . ?
C5A C4A C9A C8A -50.4(7) . . . . ?
P1 C4A C9A C8A 64.1(6) . . . . ?
N1 P1 C4B C5B -76(2) . . . . ?
C4A P1 C4B C5B 2(4) . . . . ?
C13 P1 C4B C5B 66(3) . . . . ?
C10 P1 C4B C5B 156.1(19) . . . . ?
N1 P1 C4B C9B 37(2) . . . . ?
C4A P1 C4B C9B 115(7) . . . . ?
C13 P1 C4B C9B 179.3(15) . . . . ?
C10 P1 C4B C9B -91(2) . . . . ?
C9B C4B C5B C6B -56(4) . . . . ?
P1 C4B C5B C6B 49(3) . . . . ?
C4B C5B C6B C7B 12(3) . . . . ?
C7A N1 C7B C8B 22.7(13) . . . . ?
P1 N1 C7B C8B -87.2(13) . . . . ?
Si1 N1 C7B C8B 103.8(12) . . . . ?
C7A N1 C7B C6B 142(2) . . . . ?
P1 N1 C7B C6B 31.6(14) . . . . ?
Si1 N1 C7B C6B -137.4(11) . . . . ?
C5B C6B C7B N1 -66(2) . . . . ?
C5B C6B C7B C8B 42(2) . . . . ?
N1 C7B C8B C9B 68(2) . . . . ?
C6B C7B C8B C9B -54(3) . . . . ?
C7B C8B C9B C4B 11(3) . . . . ?
C5B C4B C9B C8B 40(4) . . . . ?
P1 C4B C9B C8B -62(3) . . . . ?
N1 P1 C10 C11 179.40(19) . . . . ?
C4A P1 C10 C11 -56.9(4) . . . . ?
C13 P1 C10 C11 54.9(2) . . . . ?
C4B P1 C10 C11 -64.5(13) . . . . ?
N1 P1 C10 C15 70.0(2) . . . . ?
C4A P1 C10 C15 -166.4(3) . . . . ?
C13 P1 C10 C15 -54.5(2) . . . . ?
C4B P1 C10 C15 -173.9(13) . . . . ?
C15 C10 C11 C12 63.2(4) . . . . ?
P1 C10 C11 C12 -40.9(3) . . . . ?
C10 C11 C12 C13 -0.5(4) . . . . ?
C11 C12 C13 C14 -64.0(4) . . . . ?
C11 C12 C13 P1 41.9(3) . . . . ?
N1 P1 C13 C12 -179.4(2) . . . . ?
C4A P1 C13 C12 60.7(3) . . . . ?
C10 P1 C13 C12 -55.9(2) . . . . ?
C4B P1 C13 C12 45.9(13) . . . . ?
N1 P1 C13 C14 -70.8(2) . . . . ?
C4A P1 C13 C14 169.4(3) . . . . ?
C10 P1 C13 C14 52.7(2) . . . . ?
C4B P1 C13 C14 154.6(13) . . . . ?
C12 C13 C14 C15 64.1(3) . . . . ?
P1 C13 C14 C15 -36.0(3) . . . . ?
C11 C10 C15 C14 -57.1(3) . . . . ?
P1 C10 C15 C14 41.9(3) . . . . ?
C13 C14 C15 C10 -3.8(3) . . . . ?
O1 S1 C16 F1 -178.7(3) . . . . ?
O2 S1 C16 F1 62.6(3) . . . . ?
O3 S1 C16 F1 -58.3(3) . . . . ?
O1 S1 C16 F3 58.7(3) . . . . ?
O2 S1 C16 F3 -60.0(3) . . . . ?
O3 S1 C16 F3 179.1(3) . . . . ?
O1 S1 C16 F2 -60.0(3) . . . . ?
O2 S1 C16 F2 -178.7(2) . . . . ?
O3 S1 C16 F2 60.4(3) . . . . ?
C23 P2 N2 C20 14.4(2) . . . . ?
C26 P2 N2 C20 147.32(18) . . . . ?
C29 P2 N2 C20 -110.78(19) . . . . ?
C23 P2 N2 Si2 -144.14(18) . . . . ?
C26 P2 N2 Si2 -11.3(2) . . . . ?
C29 P2 N2 Si2 90.64(19) . . . . ?
C20 N2 Si2 C19 123.01(19) . . . . ?
P2 N2 Si2 C19 -79.55(19) . . . . ?
C20 N2 Si2 C18 6.5(2) . . . . ?
P2 N2 Si2 C18 163.90(17) . . . . ?
C20 N2 Si2 C17 -113.15(19) . . . . ?
P2 N2 Si2 C17 44.3(2) . . . . ?
P2 N2 C20 C21 45.1(3) . . . . ?
Si2 N2 C20 C21 -153.26(19) . . . . ?
P2 N2 C20 C25 -73.4(2) . . . . ?
Si2 N2 C20 C25 88.2(2) . . . . ?
C25 C20 C21 C22 54.8(3) . . . . ?
N2 C20 C21 C22 -63.6(3) . . . . ?
C20 C21 C22 C23 3.2(4) . . . . ?
C21 C22 C23 C24 -54.4(4) . . . . ?
C21 C22 C23 P2 58.9(3) . . . . ?
N2 P2 C23 C22 -65.7(2) . . . . ?
C26 P2 C23 C22 159.0(2) . . . . ?
C29 P2 C23 C22 64.3(2) . . . . ?
N2 P2 C23 C24 49.0(2) . . . . ?
C26 P2 C23 C24 -86.3(2) . . . . ?
C29 P2 C23 C24 179.0(2) . . . . ?
C22 C23 C24 C25 45.9(4) . . . . ?
P2 C23 C24 C25 -64.1(3) . . . . ?
C23 C24 C25 C20 8.7(4) . . . . ?
C21 C20 C25 C24 -58.6(3) . . . . ?
N2 C20 C25 C24 62.1(3) . . . . ?
N2 P2 C26 C27 175.01(19) . . . . ?
C23 P2 C26 C27 -58.9(3) . . . . ?
C29 P2 C26 C27 53.4(2) . . . . ?
N2 P2 C26 C31 67.6(2) . . . . ?
C23 P2 C26 C31 -166.3(2) . . . . ?
C29 P2 C26 C31 -54.0(2) . . . . ?
C31 C26 C27 C28 61.5(4) . . . . ?
P2 C26 C27 C28 -42.6(3) . . . . ?
C26 C27 C28 C29 2.6(5) . . . . ?
C27 C28 C29 C30 -65.2(4) . . . . ?
C27 C28 C29 P2 38.8(3) . . . . ?
N2 P2 C29 C28 -177.77(19) . . . . ?
C23 P2 C29 C28 62.3(2) . . . . ?
C26 P2 C29 C28 -54.8(2) . . . . ?
N2 P2 C29 C30 -68.5(2) . . . . ?
C23 P2 C29 C30 171.6(2) . . . . ?
C26 P2 C29 C30 54.5(2) . . . . ?
C28 C29 C30 C31 60.2(3) . . . . ?
P2 C29 C30 C31 -40.5(3) . . . . ?
C27 C26 C31 C30 -59.4(3) . . . . ?
P2 C26 C31 C30 37.8(3) . . . . ?
C29 C30 C31 C26 1.9(3) . . . . ?
O4A S2A C32A F4A 63.3(11) . . . . ?
O5A S2A C32A F4A -58.0(12) . . . . ?
O6A S2A C32A F4A -174.3(8) . . . . ?
O4A S2A C32A F6A -176.2(9) . . . . ?
O5A S2A C32A F6A 62.6(11) . . . . ?
O6A S2A C32A F6A -53.7(10) . . . . ?
O4A S2A C32A F5A -57.9(10) . . . . ?
O5A S2A C32A F5A -179.2(10) . . . . ?
O6A S2A C32A F5A 64.5(9) . . . . ?
O5B S2B C32B F4B -60(2) . . . . ?
O4B S2B C32B F4B 63(2) . . . . ?
O6B S2B C32B F4B -178(2) . . . . ?
O5B S2B C32B F6B 63(2) . . . . ?
O4B S2B C32B F6B -174(2) . . . . ?
O6B S2B C32B F6B -55(2) . . . . ?
O5B S2B C32B F5B -177.5(17) . . . . ?
O4B S2B C32B F5B -54(2) . . . . ?
O6B S2B C32B F5B 64.4(19) . . . . ?
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full 27.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max 0.510
_refine_diff_density_min -0.448
_refine_diff_density_rms 0.069
_database_code_depnum_ccdc_archive 'CCDC 956160'
#######################################################################
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# CCDC
#
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# as required by the journal to which it was submitted.
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# to carry out CIF format checking respectively.
#
data_ch115_2_[P(O)H(C6H10)2NH2]
_audit_creation_method SHELXL-97
#==============================================================================
# CHEMICAL DATA
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety
;
C12 H23 N O P +, C F3 O3 S -, C H2 Cl2
;
_chemical_formula_sum 'C14 H25 Cl2 F3 N O4 P S'
_chemical_formula_weight 462.28
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
#==============================================================================
# CRYSTAL DATA
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_H-M 'P n a 21'
_symmetry_space_group_name_Hall 'P 2c -2n'
_symmetry_Int_Tables_number 33
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'
_cell_length_a 17.3330(14)
_cell_length_b 8.3372(6)
_cell_length_c 14.4037(10)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 2081.5(3)
_cell_formula_units_Z 4
_cell_measurement_temperature 173(2)
_cell_measurement_reflns_used 1974
_cell_measurement_theta_min 4.700
_cell_measurement_theta_max 41.585
_exptl_crystal_description needle
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.36
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.06
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.475
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 960
_exptl_absorpt_coefficient_mu 0.534
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.8310
_exptl_absorpt_correction_T_max 0.9687
_exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)'
#==============================================================================
# EXPERIMENTAL DATA
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 173(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker Apex Kappa II-CCD-diffractometer'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 14093
_diffrn_reflns_av_R_equivalents 0.0621
_diffrn_reflns_av_sigmaI/netI 0.0794
_diffrn_reflns_limit_h_min -23
_diffrn_reflns_limit_h_max 23
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_theta_min 2.35
_diffrn_reflns_theta_max 29.00
_reflns_number_total 4994
_reflns_number_gt 3252
_reflns_threshold_expression >2\s(I)
_computing_data_collection 'Bruker Apex V7.51A'
_computing_cell_refinement 'Bruker Apex V7.51A'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material SHELXL-97
#==============================================================================
# REFINEMENT DATA
_refine_special_details
;
All H atoms
were positioned geometrically and refined using a riding model, with C---H =
0.98 (methyl groups), 0.99\%A (methylene groups), 1.00\%A (methine groups) or
0.95 \%A (aryl CH) and with U~iso~(H) = 1.5 times U~eq~(C)
(methyl groups) or with U~iso~(H) = 1.2 times U~eq~(C)
(methylene groups, aryl CH, methine groups). Torsion angles of all methyl
groups were allowed to refine. All N-H (and both P-H) distances were
restrained to be equal to each other. The geometry of both disordred molecule
parts was restrained to be similar within an esd of 0.01.
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0597P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment 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 0.29(9)
_refine_ls_number_reflns 4994
_refine_ls_number_parameters 299
_refine_ls_number_restraints 38
_refine_ls_R_factor_all 0.0945
_refine_ls_R_factor_gt 0.0530
_refine_ls_wR_factor_ref 0.1300
_refine_ls_wR_factor_gt 0.1155
_refine_ls_goodness_of_fit_ref 0.970
_refine_ls_restrained_S_all 0.967
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
#==============================================================================
# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_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
P1A P 0.96050(8) 1.19922(17) 0.47196(9) 0.0307(3) Uani 0.896(3) 1 d PD A 1
O1A O 0.92549(19) 1.1993(4) 0.37676(18) 0.0360(7) Uani 0.896(3) 1 d PD A 1
N1A N 1.0220(3) 0.7775(6) 0.6976(3) 0.0324(11) Uani 0.896(3) 1 d PD A 1
C1A C 1.0472(3) 1.0819(5) 0.4778(3) 0.0334(10) Uani 0.896(3) 1 d PD A 1
H1A H 1.0330 0.9674 0.4713 0.040 Uiso 0.896(3) 1 calc PR A 1
H1B H 1.0800 1.1103 0.4240 0.040 Uiso 0.896(3) 1 calc PR A 1
C2A C 1.0949(3) 1.1005(6) 0.5653(3) 0.0348(10) Uani 0.896(3) 1 d PD A 1
C3A C 1.1069(3) 0.9840(6) 0.6271(3) 0.0347(10) Uani 0.896(3) 1 d PD A 1
C4A C 1.0757(3) 0.8189(5) 0.6188(3) 0.0319(9) Uani 0.896(3) 1 d PD A 1
H4A H 1.1190 0.7414 0.6178 0.038 Uiso 0.896(3) 1 calc PR A 1
H4B H 1.0475 0.8089 0.5592 0.038 Uiso 0.896(3) 1 calc PR A 1
C5A C 1.1295(3) 1.2679(6) 0.5760(4) 0.0470(12) Uani 0.896(3) 1 d PD A 1
H5A H 1.1827 1.2589 0.5984 0.070 Uiso 0.896(3) 1 calc PR A 1
H5B H 1.0989 1.3296 0.6207 0.070 Uiso 0.896(3) 1 calc PR A 1
H5C H 1.1291 1.3227 0.5158 0.070 Uiso 0.896(3) 1 calc PR A 1
C6A C 1.1576(3) 1.0129(7) 0.7115(3) 0.0467(12) Uani 0.896(3) 1 d PD A 1
H6A H 1.1375 1.1043 0.7468 0.070 Uiso 0.896(3) 1 calc PR A 1
H6B H 1.2104 1.0360 0.6913 0.070 Uiso 0.896(3) 1 calc PR A 1
H6C H 1.1575 0.9171 0.7509 0.070 Uiso 0.896(3) 1 calc PR A 1
C7A C 0.8989(3) 1.1270(5) 0.5631(3) 0.0304(9) Uani 0.896(3) 1 d PD A 1
H7A H 0.9255 1.1422 0.6233 0.037 Uiso 0.896(3) 1 calc PR A 1
H7B H 0.8514 1.1927 0.5641 0.037 Uiso 0.896(3) 1 calc PR A 1
C8A C 0.8766(2) 0.9521(5) 0.5535(3) 0.0280(9) Uani 0.896(3) 1 d PD A 1
C9A C 0.9004(3) 0.8369(5) 0.6102(3) 0.0295(10) Uani 0.896(3) 1 d PD A 1
C10A C 0.9471(3) 0.8669(5) 0.6963(3) 0.0282(10) Uani 0.896(3) 1 d PD A 1
H10A H 0.9578 0.9832 0.7013 0.034 Uiso 0.896(3) 1 calc PR A 1
H10B H 0.9163 0.8352 0.7512 0.034 Uiso 0.896(3) 1 calc PR A 1
C11A C 0.8238(3) 0.9179(6) 0.4728(4) 0.0472(11) Uani 0.896(3) 1 d PD A 1
H11A H 0.7825 0.8456 0.4929 0.071 Uiso 0.896(3) 1 calc PR A 1
H11B H 0.8533 0.8673 0.4227 0.071 Uiso 0.896(3) 1 calc PR A 1
H11C H 0.8013 1.0186 0.4505 0.071 Uiso 0.896(3) 1 calc PR A 1
C12A C 0.8770(3) 0.6633(5) 0.5983(3) 0.0440(12) Uani 0.896(3) 1 d PD A 1
H12A H 0.9110 0.6119 0.5527 0.066 Uiso 0.896(3) 1 calc PR A 1
H12B H 0.8235 0.6580 0.5764 0.066 Uiso 0.896(3) 1 calc PR A 1
H12C H 0.8814 0.6075 0.6579 0.066 Uiso 0.896(3) 1 calc PR A 1
P1B P 1.0423(8) 0.7932(17) 0.6742(9) 0.0307(3) Uani 0.104(3) 1 d PD A 2
H1J H 1.0291(10) 0.644(6) 0.6537(12) 0.064(16) Uiso 0.104(3) 1 calc PRD A 2
O1B O 1.0743(14) 0.799(3) 0.7719(11) 0.0360(7) Uani 0.104(3) 1 d PD A 2
N1B N 0.9744(15) 1.216(5) 0.451(3) 0.0324(11) Uani 0.104(3) 1 d PD A 2
H1G H 0.9502 1.1914 0.3958 0.039 Uiso 0.104(3) 1 calc PR A 2
H1H H 0.9839 1.3242 0.4514 0.039 Uiso 0.104(3) 1 calc PR A 2
C1B C 0.9524(12) 0.899(4) 0.6677(15) 0.0334(10) Uani 0.104(3) 1 d PD A 2
H1C H 0.9189 0.8595 0.7185 0.040 Uiso 0.104(3) 1 calc PR A 2
H1D H 0.9628 1.0137 0.6799 0.040 Uiso 0.104(3) 1 calc PR A 2
C2B C 0.9074(17) 0.887(3) 0.578(2) 0.0348(10) Uani 0.104(3) 1 d PD A 2
C3B C 0.890(2) 1.010(3) 0.5222(19) 0.0347(10) Uani 0.104(3) 1 d PD A 2
C4B C 0.9210(18) 1.175(3) 0.530(2) 0.0319(9) Uani 0.104(3) 1 d PD A 2
H4C H 0.9491 1.1866 0.5895 0.038 Uiso 0.104(3) 1 calc PR A 2
H4D H 0.8775 1.2524 0.5306 0.038 Uiso 0.104(3) 1 calc PR A 2
C5B C 0.870(3) 0.722(4) 0.566(3) 0.0470(12) Uani 0.104(3) 1 d PD A 2
H5D H 0.8918 0.6468 0.6106 0.070 Uiso 0.104(3) 1 calc PR A 2
H5E H 0.8791 0.6832 0.5026 0.070 Uiso 0.104(3) 1 calc PR A 2
H5F H 0.8140 0.7314 0.5762 0.070 Uiso 0.104(3) 1 calc PR A 2
C6B C 0.843(3) 0.981(5) 0.434(2) 0.0467(12) Uani 0.104(3) 1 d PD A 2
H6D H 0.8332 1.0834 0.4035 0.070 Uiso 0.104(3) 1 calc PR A 2
H6E H 0.7939 0.9303 0.4510 0.070 Uiso 0.104(3) 1 calc PR A 2
H6F H 0.8718 0.9101 0.3925 0.070 Uiso 0.104(3) 1 calc PR A 2
C7B C 1.1047(14) 0.873(2) 0.5870(14) 0.0304(9) Uani 0.104(3) 1 d PD A 2
H7C H 1.1541 0.8139 0.5884 0.037 Uiso 0.104(3) 1 calc PR A 2
H7D H 1.0809 0.8557 0.5254 0.037 Uiso 0.104(3) 1 calc PR A 2
C8B C 1.1210(17) 1.050(3) 0.5988(18) 0.0280(9) Uani 0.104(3) 1 d PD A 2
C9B C 1.093(2) 1.163(2) 0.543(2) 0.0295(10) Uani 0.104(3) 1 d PD A 2
C10B C 1.0498(17) 1.128(4) 0.4549(18) 0.0282(10) Uani 0.104(3) 1 d PD A 2
H10C H 1.0818 1.1594 0.4010 0.034 Uiso 0.104(3) 1 calc PR A 2
H10D H 1.0400 1.0111 0.4506 0.034 Uiso 0.104(3) 1 calc PR A 2
C11B C 1.177(2) 1.089(4) 0.676(3) 0.0472(11) Uani 0.104(3) 1 d PD A 2
H11D H 1.1908 0.9909 0.7088 0.071 Uiso 0.104(3) 1 calc PR A 2
H11E H 1.1530 1.1652 0.7189 0.071 Uiso 0.104(3) 1 calc PR A 2
H11F H 1.2236 1.1377 0.6491 0.071 Uiso 0.104(3) 1 calc PR A 2
C12B C 1.117(3) 1.337(3) 0.550(3) 0.0440(12) Uani 0.104(3) 1 d PD A 2
H12D H 1.0908 1.3994 0.5019 0.066 Uiso 0.104(3) 1 calc PR A 2
H12E H 1.1730 1.3458 0.5419 0.066 Uiso 0.104(3) 1 calc PR A 2
H12F H 1.1028 1.3790 0.6115 0.066 Uiso 0.104(3) 1 calc PR A 2
H1E H 1.046(3) 0.797(6) 0.753(3) 0.033(14) Uiso 0.896(3) 1 d PD A 1
H1F H 1.014(3) 0.671(4) 0.707(4) 0.071(18) Uiso 0.896(3) 1 d PD A 1
H1I H 0.982(3) 1.337(6) 0.505(3) 0.064(16) Uiso 0.896(3) 1 d PD A 1
S1 S 0.98209(5) 0.35321(9) 0.82038(8) 0.0324(2) Uani 1 1 d . . .
O2 O 1.0130(3) 0.4100(6) 0.9037(3) 0.0901(14) Uani 1 1 d . . .
O3 O 1.0006(2) 0.4436(4) 0.7394(3) 0.0717(11) Uani 1 1 d . . .
O4 O 0.9893(2) 0.1856(3) 0.8055(3) 0.0688(11) Uani 1 1 d . . .
F1 F 0.8407(2) 0.3280(5) 0.7632(3) 0.1059(13) Uani 1 1 d . . .
F2 F 0.8551(2) 0.3066(5) 0.9096(3) 0.1080(15) Uani 1 1 d . . .
F3 F 0.8626(2) 0.5348(4) 0.8431(3) 0.1020(12) Uani 1 1 d . . .
C13 C 0.8799(3) 0.3793(5) 0.8351(4) 0.0546(11) Uani 1 1 d . . .
Cl1 Cl 0.75766(9) 1.44511(17) 0.22799(10) 0.0646(4) Uani 1 1 d . . .
Cl2 Cl 0.75183(9) 1.43912(19) 0.42867(11) 0.0721(4) Uani 1 1 d . . .
C14 C 0.8061(2) 1.4917(5) 0.3307(4) 0.0503(10) Uani 1 1 d . . .
H14A H 0.8170 1.6082 0.3323 0.060 Uiso 1 1 calc R . .
H14B H 0.8560 1.4340 0.3322 0.060 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1A 0.0416(7) 0.0278(5) 0.0227(7) 0.0025(5) 0.0010(6) -0.0010(5)
O1A 0.0451(19) 0.0385(15) 0.0244(15) 0.0051(12) -0.0022(14) 0.0035(13)
N1A 0.034(3) 0.034(2) 0.029(3) 0.0007(19) -0.004(2) 0.0029(19)
C1A 0.034(2) 0.037(2) 0.029(2) 0.007(2) 0.008(2) -0.0057(18)
C2A 0.032(3) 0.047(3) 0.025(2) -0.003(2) 0.007(2) -0.010(2)
C3A 0.028(2) 0.050(3) 0.027(2) -0.0022(19) 0.0019(19) -0.0068(19)
C4A 0.032(2) 0.039(2) 0.025(2) -0.0027(17) 0.0004(19) 0.0041(18)
C5A 0.041(3) 0.058(3) 0.043(3) 0.003(2) -0.001(2) -0.016(2)
C6A 0.037(3) 0.071(3) 0.032(3) 0.000(2) -0.012(2) -0.016(2)
C7A 0.032(2) 0.034(2) 0.025(2) 0.0058(18) 0.0031(19) 0.0084(18)
C8A 0.024(2) 0.037(2) 0.023(2) 0.0005(17) 0.0001(18) -0.0035(18)
C9A 0.029(2) 0.039(2) 0.021(2) 0.0036(17) 0.0040(18) -0.0096(18)
C10A 0.033(2) 0.036(2) 0.0162(19) -0.0007(16) 0.0020(18) -0.0058(18)
C11A 0.038(3) 0.063(3) 0.041(3) 0.009(2) -0.009(3) -0.010(2)
C12A 0.053(3) 0.040(2) 0.040(3) 0.006(2) -0.017(2) -0.017(2)
P1B 0.0416(7) 0.0278(5) 0.0227(7) 0.0025(5) 0.0010(6) -0.0010(5)
O1B 0.0451(19) 0.0385(15) 0.0244(15) 0.0051(12) -0.0022(14) 0.0035(13)
N1B 0.034(3) 0.034(2) 0.029(3) 0.0007(19) -0.004(2) 0.0029(19)
C1B 0.034(2) 0.037(2) 0.029(2) 0.007(2) 0.008(2) -0.0057(18)
C2B 0.032(3) 0.047(3) 0.025(2) -0.003(2) 0.007(2) -0.010(2)
C3B 0.028(2) 0.050(3) 0.027(2) -0.0022(19) 0.0019(19) -0.0068(19)
C4B 0.032(2) 0.039(2) 0.025(2) -0.0027(17) 0.0004(19) 0.0041(18)
C5B 0.041(3) 0.058(3) 0.043(3) 0.003(2) -0.001(2) -0.016(2)
C6B 0.037(3) 0.071(3) 0.032(3) 0.000(2) -0.012(2) -0.016(2)
C7B 0.032(2) 0.034(2) 0.025(2) 0.0058(18) 0.0031(19) 0.0084(18)
C8B 0.024(2) 0.037(2) 0.023(2) 0.0005(17) 0.0001(18) -0.0035(18)
C9B 0.029(2) 0.039(2) 0.021(2) 0.0036(17) 0.0040(18) -0.0096(18)
C10B 0.033(2) 0.036(2) 0.0162(19) -0.0007(16) 0.0020(18) -0.0058(18)
C11B 0.038(3) 0.063(3) 0.041(3) 0.009(2) -0.009(3) -0.010(2)
C12B 0.053(3) 0.040(2) 0.040(3) 0.006(2) -0.017(2) -0.017(2)
S1 0.0334(5) 0.0269(4) 0.0369(5) 0.0001(4) -0.0016(5) -0.0043(3)
O2 0.081(3) 0.117(3) 0.072(3) -0.036(2) -0.033(2) -0.005(3)
O3 0.065(2) 0.069(2) 0.081(3) 0.036(2) 0.024(2) 0.0070(18)
O4 0.074(2) 0.0310(13) 0.101(3) -0.0068(18) 0.008(2) 0.0066(13)
F1 0.049(2) 0.140(3) 0.129(3) -0.010(2) -0.041(2) -0.008(2)
F2 0.066(3) 0.139(3) 0.119(3) 0.068(2) 0.047(2) 0.015(2)
F3 0.099(3) 0.087(2) 0.120(3) 0.004(2) 0.028(3) 0.0566(19)
C13 0.048(3) 0.063(3) 0.053(3) 0.005(3) 0.008(3) 0.007(2)
Cl1 0.0667(10) 0.0727(8) 0.0545(8) -0.0017(6) -0.0064(7) -0.0023(7)
Cl2 0.0540(9) 0.1035(12) 0.0590(8) 0.0054(8) 0.0029(7) -0.0109(8)
C14 0.036(2) 0.049(2) 0.066(3) -0.004(3) -0.003(3) -0.0046(17)
#==============================================================================
# MOLECULAR GEOMETRY
_geom_special_details
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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
P1A O1A 1.500(3) . ?
P1A C1A 1.795(5) . ?
P1A C7A 1.795(4) . ?
P1A H1I 1.30(5) . ?
N1A C10A 1.497(6) . ?
N1A C4A 1.509(6) . ?
N1A H1E 0.92(3) . ?
N1A H1F 0.91(4) . ?
C1A C2A 1.514(6) . ?
C1A H1A 0.9900 . ?
C1A H1B 0.9900 . ?
C2A C3A 1.334(6) . ?
C2A C5A 1.528(6) . ?
C3A C4A 1.485(6) . ?
C3A C6A 1.518(6) . ?
C4A H4A 0.9900 . ?
C4A H4B 0.9900 . ?
C5A H5A 0.9800 . ?
C5A H5B 0.9800 . ?
C5A H5C 0.9800 . ?
C6A H6A 0.9800 . ?
C6A H6B 0.9800 . ?
C6A H6C 0.9800 . ?
C7A C8A 1.515(5) . ?
C7A H7A 0.9900 . ?
C7A H7B 0.9900 . ?
C8A C9A 1.327(6) . ?
C8A C11A 1.506(6) . ?
C9A C10A 1.501(6) . ?
C9A C12A 1.513(5) . ?
C10A H10A 0.9900 . ?
C10A H10B 0.9900 . ?
C11A H11A 0.9800 . ?
C11A H11B 0.9800 . ?
C11A H11C 0.9800 . ?
C12A H12A 0.9800 . ?
C12A H12B 0.9800 . ?
C12A H12C 0.9800 . ?
P1B O1B 1.513(10) . ?
P1B C7B 1.787(10) . ?
P1B C1B 1.793(11) . ?
P1B H1J 1.2971 . ?
P1B H1E 1.14(4) . ?
P1B H1F 1.22(4) . ?
O1B H1E 0.56(5) . ?
N1B C10B 1.499(12) . ?
N1B C4B 1.506(11) . ?
N1B H1G 0.9200 . ?
N1B H1H 0.9200 . ?
N1B H1I 1.28(6) . ?
C1B C2B 1.512(11) . ?
C1B H1C 0.9900 . ?
C1B H1D 0.9900 . ?
C2B C3B 1.333(10) . ?
C2B C5B 1.533(11) . ?
C3B C4B 1.486(11) . ?
C3B C6B 1.524(11) . ?
C4B H4C 0.9900 . ?
C4B H4D 0.9900 . ?
C5B H5D 0.9800 . ?
C5B H5E 0.9800 . ?
C5B H5F 0.9800 . ?
C6B H6D 0.9800 . ?
C6B H6E 0.9800 . ?
C6B H6F 0.9800 . ?
C7B C8B 1.513(11) . ?
C7B H7C 0.9900 . ?
C7B H7D 0.9900 . ?
C8B C9B 1.326(10) . ?
C8B C11B 1.508(11) . ?
C9B C10B 1.506(11) . ?
C9B C12B 1.513(11) . ?
C10B H10C 0.9900 . ?
C10B H10D 0.9900 . ?
C11B H11D 0.9800 . ?
C11B H11E 0.9800 . ?
C11B H11F 0.9800 . ?
C12B H12D 0.9800 . ?
C12B H12E 0.9800 . ?
C12B H12F 0.9800 . ?
S1 O2 1.397(4) . ?
S1 O4 1.420(3) . ?
S1 O3 1.425(3) . ?
S1 C13 1.798(5) . ?
F1 C13 1.310(6) . ?
F2 C13 1.305(6) . ?
F3 C13 1.335(5) . ?
Cl1 C14 1.745(6) . ?
Cl2 C14 1.751(6) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
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
O1A P1A C1A 112.5(2) . . ?
O1A P1A C7A 115.3(2) . . ?
C1A P1A C7A 106.3(2) . . ?
O1A P1A H1I 117(2) . . ?
C1A P1A H1I 103(2) . . ?
C7A P1A H1I 102(2) . . ?
C10A N1A C4A 114.3(4) . . ?
C10A N1A H1E 108(3) . . ?
C4A N1A H1E 110(3) . . ?
C10A N1A H1F 111(3) . . ?
C4A N1A H1F 115(4) . . ?
H1E N1A H1F 96(5) . . ?
C2A C1A P1A 116.1(3) . . ?
C2A C1A H1A 108.3 . . ?
P1A C1A H1A 108.3 . . ?
C2A C1A H1B 108.3 . . ?
P1A C1A H1B 108.3 . . ?
H1A C1A H1B 107.4 . . ?
C3A C2A C1A 124.5(4) . . ?
C3A C2A C5A 122.4(4) . . ?
C1A C2A C5A 113.1(4) . . ?
C2A C3A C4A 124.3(4) . . ?
C2A C3A C6A 120.6(4) . . ?
C4A C3A C6A 115.1(4) . . ?
C3A C4A N1A 112.1(4) . . ?
C3A C4A H4A 109.2 . . ?
N1A C4A H4A 109.2 . . ?
C3A C4A H4B 109.2 . . ?
N1A C4A H4B 109.2 . . ?
H4A C4A H4B 107.9 . . ?
C8A C7A P1A 114.0(3) . . ?
C8A C7A H7A 108.7 . . ?
P1A C7A H7A 108.7 . . ?
C8A C7A H7B 108.7 . . ?
P1A C7A H7B 108.7 . . ?
H7A C7A H7B 107.6 . . ?
C9A C8A C11A 121.8(4) . . ?
C9A C8A C7A 124.2(4) . . ?
C11A C8A C7A 114.1(4) . . ?
C8A C9A C10A 123.7(4) . . ?
C8A C9A C12A 122.6(4) . . ?
C10A C9A C12A 113.4(3) . . ?
N1A C10A C9A 113.3(4) . . ?
N1A C10A H10A 108.9 . . ?
C9A C10A H10A 108.9 . . ?
N1A C10A H10B 108.9 . . ?
C9A C10A H10B 108.9 . . ?
H10A C10A H10B 107.7 . . ?
O1B P1B C7B 114.8(11) . . ?
O1B P1B C1B 110.6(11) . . ?
C7B P1B C1B 107.8(10) . . ?
O1B P1B H1J 107.8 . . ?
C7B P1B H1J 107.8 . . ?
C1B P1B H1J 107.8 . . ?
O1B P1B H1E 18(3) . . ?
C7B P1B H1E 131(3) . . ?
C1B P1B H1E 95(3) . . ?
H1J P1B H1E 105.2 . . ?
O1B P1B H1F 79(3) . . ?
C7B P1B H1F 145(3) . . ?
C1B P1B H1F 95(3) . . ?
H1J P1B H1F 38.8 . . ?
H1E P1B H1F 70(4) . . ?
P1B O1B H1E 40(5) . . ?
C10B N1B C4B 113.5(14) . . ?
C10B N1B H1G 108.9 . . ?
C4B N1B H1G 108.9 . . ?
C10B N1B H1H 108.9 . . ?
C4B N1B H1H 108.9 . . ?
H1G N1B H1H 107.7 . . ?
C10B N1B H1I 106(3) . . ?
C4B N1B H1I 78(3) . . ?
H1G N1B H1I 137.9 . . ?
H1H N1B H1I 36.7 . . ?
C2B C1B P1B 117.5(14) . . ?
C2B C1B H1C 107.9 . . ?
P1B C1B H1C 107.9 . . ?
C2B C1B H1D 107.9 . . ?
P1B C1B H1D 107.9 . . ?
H1C C1B H1D 107.2 . . ?
C3B C2B C1B 125.6(13) . . ?
C3B C2B C5B 121.5(13) . . ?
C1B C2B C5B 112.1(13) . . ?
C2B C3B C4B 125.9(14) . . ?
C2B C3B C6B 119.9(14) . . ?
C4B C3B C6B 113.8(12) . . ?
C3B C4B N1B 111.7(14) . . ?
C3B C4B H4C 109.3 . . ?
N1B C4B H4C 109.3 . . ?
C3B C4B H4D 109.3 . . ?
N1B C4B H4D 109.3 . . ?
H4C C4B H4D 107.9 . . ?
C2B C5B H5D 109.5 . . ?
C2B C5B H5E 109.5 . . ?
H5D C5B H5E 109.5 . . ?
C2B C5B H5F 109.5 . . ?
H5D C5B H5F 109.5 . . ?
H5E C5B H5F 109.5 . . ?
C3B C6B H6D 109.5 . . ?
C3B C6B H6E 109.5 . . ?
H6D C6B H6E 109.5 . . ?
C3B C6B H6F 109.5 . . ?
H6D C6B H6F 109.5 . . ?
H6E C6B H6F 109.5 . . ?
C8B C7B P1B 113.5(13) . . ?
C8B C7B H7C 108.9 . . ?
P1B C7B H7C 108.9 . . ?
C8B C7B H7D 108.9 . . ?
P1B C7B H7D 108.9 . . ?
H7C C7B H7D 107.7 . . ?
C9B C8B C11B 121.6(13) . . ?
C9B C8B C7B 123.8(13) . . ?
C11B C8B C7B 114.5(13) . . ?
C8B C9B C10B 123.6(14) . . ?
C8B C9B C12B 122.7(14) . . ?
C10B C9B C12B 112.4(13) . . ?
N1B C10B C9B 111.9(14) . . ?
N1B C10B H10C 109.2 . . ?
C9B C10B H10C 109.2 . . ?
N1B C10B H10D 109.2 . . ?
C9B C10B H10D 109.2 . . ?
H10C C10B H10D 107.9 . . ?
C8B C11B H11D 109.5 . . ?
C8B C11B H11E 109.5 . . ?
H11D C11B H11E 109.5 . . ?
C8B C11B H11F 109.5 . . ?
H11D C11B H11F 109.5 . . ?
H11E C11B H11F 109.5 . . ?
C9B C12B H12D 109.5 . . ?
C9B C12B H12E 109.5 . . ?
H12D C12B H12E 109.5 . . ?
C9B C12B H12F 109.5 . . ?
H12D C12B H12F 109.5 . . ?
H12E C12B H12F 109.5 . . ?
O2 S1 O4 115.4(3) . . ?
O2 S1 O3 115.9(2) . . ?
O4 S1 O3 112.2(2) . . ?
O2 S1 C13 103.6(3) . . ?
O4 S1 C13 103.0(2) . . ?
O3 S1 C13 104.7(2) . . ?
F2 C13 F1 109.2(4) . . ?
F2 C13 F3 107.9(4) . . ?
F1 C13 F3 105.6(4) . . ?
F2 C13 S1 111.4(4) . . ?
F1 C13 S1 112.2(3) . . ?
F3 C13 S1 110.4(3) . . ?
Cl1 C14 Cl2 111.7(2) . . ?
Cl1 C14 H14A 109.3 . . ?
Cl2 C14 H14A 109.3 . . ?
Cl1 C14 H14B 109.3 . . ?
Cl2 C14 H14B 109.3 . . ?
H14A C14 H14B 107.9 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1A P1A C1A C2A 168.5(3) . . . . ?
C7A P1A C1A C2A -64.4(4) . . . . ?
P1A C1A C2A C3A 114.8(5) . . . . ?
P1A C1A C2A C5A -65.9(5) . . . . ?
C1A C2A C3A C4A 0.4(8) . . . . ?
C5A C2A C3A C4A -178.9(5) . . . . ?
C1A C2A C3A C6A 178.3(5) . . . . ?
C5A C2A C3A C6A -1.0(8) . . . . ?
C2A C3A C4A N1A -118.1(5) . . . . ?
C6A C3A C4A N1A 63.9(5) . . . . ?
C10A N1A C4A C3A 69.3(5) . . . . ?
O1A P1A C7A C8A 64.1(4) . . . . ?
C1A P1A C7A C8A -61.3(4) . . . . ?
P1A C7A C8A C9A 111.7(4) . . . . ?
P1A C7A C8A C11A -68.6(5) . . . . ?
C11A C8A C9A C10A -174.3(4) . . . . ?
C7A C8A C9A C10A 5.4(7) . . . . ?
C11A C8A C9A C12A 0.4(7) . . . . ?
C7A C8A C9A C12A -179.9(4) . . . . ?
C4A N1A C10A C9A 60.4(5) . . . . ?
C8A C9A C10A N1A -123.2(5) . . . . ?
C12A C9A C10A N1A 61.7(5) . . . . ?
O1B P1B C1B C2B -172(2) . . . . ?
C7B P1B C1B C2B 61(2) . . . . ?
P1B C1B C2B C3B -118(3) . . . . ?
P1B C1B C2B C5B 73(4) . . . . ?
C1B C2B C3B C4B 9(6) . . . . ?
C5B C2B C3B C4B 177(4) . . . . ?
C1B C2B C3B C6B -179(3) . . . . ?
C5B C2B C3B C6B -11(6) . . . . ?
C2B C3B C4B N1B 111(4) . . . . ?
C6B C3B C4B N1B -61(4) . . . . ?
C10B N1B C4B C3B -70(4) . . . . ?
O1B P1B C7B C8B -64(2) . . . . ?
C1B P1B C7B C8B 60(2) . . . . ?
P1B C7B C8B C9B -109(3) . . . . ?
P1B C7B C8B C11B 75(3) . . . . ?
C11B C8B C9B C10B 168(4) . . . . ?
C7B C8B C9B C10B -8(6) . . . . ?
C11B C8B C9B C12B 2(6) . . . . ?
C7B C8B C9B C12B -173(3) . . . . ?
C4B N1B C10B C9B -59(4) . . . . ?
C8B C9B C10B N1B 128(3) . . . . ?
C12B C9B C10B N1B -65(4) . . . . ?
O2 S1 C13 F2 -55.8(4) . . . . ?
O4 S1 C13 F2 64.8(4) . . . . ?
O3 S1 C13 F2 -177.7(4) . . . . ?
O2 S1 C13 F1 -178.5(4) . . . . ?
O4 S1 C13 F1 -57.9(4) . . . . ?
O3 S1 C13 F1 59.6(4) . . . . ?
O2 S1 C13 F3 64.0(4) . . . . ?
O4 S1 C13 F3 -175.3(4) . . . . ?
O3 S1 C13 F3 -57.9(4) . . . . ?
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full 29.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max 0.485
_refine_diff_density_min -0.284
_refine_diff_density_rms 0.064
_database_code_depnum_ccdc_archive 'CCDC 956161'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_ch163_[PN(C6H10)]4Mo(CO)3
_audit_creation_method SHELXL-97
#==============================================================================
# CHEMICAL DATA
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C27 H40 Mo N4 O3 P4, 1.4(C7 H8)'
_chemical_formula_sum 'C36.81 H51.21 Mo N4 O3 P4'
_chemical_formula_weight 817.50
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
#==============================================================================
# CRYSTAL DATA
_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M 'P -1'
_symmetry_space_group_name_Hall '-P 1'
_symmetry_Int_Tables_number 2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 9.1199(3)
_cell_length_b 13.8435(5)
_cell_length_c 17.1181(7)
_cell_angle_alpha 70.892(2)
_cell_angle_beta 88.485(2)
_cell_angle_gamma 89.599(2)
_cell_volume 2041.39(13)
_cell_formula_units_Z 2
_cell_measurement_temperature 173(2)
_cell_measurement_reflns_used 9953
_cell_measurement_theta_min 4.468
_cell_measurement_theta_max 59.448
_exptl_crystal_description block
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.18
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.06
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.330
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 852
_exptl_absorpt_coefficient_mu 0.516
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.9128
_exptl_absorpt_correction_T_max 0.9697
_exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)'
#==============================================================================
# EXPERIMENTAL DATA
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 173(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker Apex Kappa II-CCD-diffractometer'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 60358
_diffrn_reflns_av_R_equivalents 0.0564
_diffrn_reflns_av_sigmaI/netI 0.0591
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -20
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_theta_min 1.56
_diffrn_reflns_theta_max 31.00
_reflns_number_total 12924
_reflns_number_gt 9108
_reflns_threshold_expression >2\s(I)
_computing_data_collection 'Bruker Apex V7.51A'
_computing_cell_refinement 'Bruker Apex V7.51A'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material SHELXL-97
#==============================================================================
# REFINEMENT DATA
_refine_special_details
;
All H atoms
were positioned geometrically and refined using a riding model, with C---H =
0.98 (methyl groups), 0.99\%A (methylene groups), 1.00\%A (methine groups) or
0.95 \%A (aryl CH) and with U~iso~(H) = 1.5 times U~eq~(C)
(methyl groups) or with U~iso~(H) = 1.2 times U~eq~(C)
(methylene groups, aryl CH, methine groups). Torsion angles of all methyl
groups (except at C35a/b/c) were allowed to refine.
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0659P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 12924
_refine_ls_number_parameters 425
_refine_ls_number_restraints 8
_refine_ls_R_factor_all 0.0807
_refine_ls_R_factor_gt 0.0463
_refine_ls_wR_factor_ref 0.1217
_refine_ls_wR_factor_gt 0.1118
_refine_ls_goodness_of_fit_ref 1.034
_refine_ls_restrained_S_all 1.035
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
#==============================================================================
# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_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
Mo1 Mo -0.143887(19) 0.091545(15) 1.212564(12) 0.02531(7) Uani 1 1 d . . .
P1 P 0.08826(6) 0.16252(4) 1.13053(4) 0.02430(12) Uani 1 1 d . . .
P2 P 0.02124(6) -0.03460(4) 1.18122(4) 0.02533(12) Uani 1 1 d . . .
P3 P 0.02554(6) 0.00184(5) 1.32569(4) 0.02617(13) Uani 1 1 d . . .
P4 P 0.16634(7) 0.19445(5) 1.28221(4) 0.02980(14) Uani 1 1 d . . .
N1 N 0.12868(19) 0.05300(14) 1.10986(12) 0.0264(4) Uani 1 1 d . . .
N2 N 0.0987(2) -0.07650(14) 1.27497(12) 0.0270(4) Uani 1 1 d . . .
N3 N 0.1596(2) 0.06891(15) 1.34976(12) 0.0285(4) Uani 1 1 d . . .
N4 N 0.22186(19) 0.18664(14) 1.18779(12) 0.0275(4) Uani 1 1 d . . .
O1 O -0.3341(2) 0.15851(18) 1.05448(13) 0.0532(5) Uani 1 1 d . . .
O2 O -0.2451(2) 0.27756(15) 1.26726(13) 0.0459(5) Uani 1 1 d . . .
O3 O -0.4060(2) -0.04421(18) 1.30845(15) 0.0621(6) Uani 1 1 d . . .
C1 C -0.2096(2) 0.2086(2) 1.24733(15) 0.0326(5) Uani 1 1 d . . .
C2 C -0.2629(2) 0.13600(19) 1.11254(16) 0.0336(5) Uani 1 1 d . . .
C3 C -0.3090(3) 0.0060(2) 1.27387(17) 0.0369(6) Uani 1 1 d . . .
C4 C 0.1191(3) 0.25335(18) 1.02750(15) 0.0317(5) Uani 1 1 d . . .
H4A H 0.0235 0.2669 0.9998 0.038 Uiso 1 1 calc R . .
H4B H 0.1525 0.3184 1.0334 0.038 Uiso 1 1 calc R . .
C5 C 0.2279(3) 0.22427(19) 0.97044(15) 0.0323(5) Uani 1 1 d . . .
C6 C 0.2854(3) 0.13104(18) 0.98430(15) 0.0311(5) Uani 1 1 d . . .
C7 C 0.2556(3) 0.04080(18) 1.06014(15) 0.0334(5) Uani 1 1 d . . .
H7A H 0.2400 -0.0201 1.0432 0.040 Uiso 1 1 calc R . .
H7B H 0.3433 0.0280 1.0949 0.040 Uiso 1 1 calc R . .
C8 C 0.2666(3) 0.3137(2) 0.89474(18) 0.0457(7) Uani 1 1 d . . .
H8A H 0.3398 0.3565 0.9087 0.069 Uiso 1 1 calc R . .
H8B H 0.1783 0.3542 0.8750 0.069 Uiso 1 1 calc R . .
H8C H 0.3067 0.2886 0.8513 0.069 Uiso 1 1 calc R . .
C9 C 0.3929(3) 0.1078(2) 0.92430(16) 0.0401(6) Uani 1 1 d . . .
H9A H 0.3575 0.1376 0.8679 0.060 Uiso 1 1 calc R . .
H9B H 0.4023 0.0336 0.9379 0.060 Uiso 1 1 calc R . .
H9C H 0.4888 0.1372 0.9282 0.060 Uiso 1 1 calc R . .
C10 C 0.0355(3) -0.14869(18) 1.15243(16) 0.0338(5) Uani 1 1 d . . .
H10A H -0.0526 -0.1914 1.1744 0.041 Uiso 1 1 calc R . .
H10B H 0.0346 -0.1285 1.0914 0.041 Uiso 1 1 calc R . .
C11 C 0.1713(3) -0.21385(18) 1.18251(15) 0.0314(5) Uani 1 1 d . . .
C12 C 0.2550(3) -0.20867(18) 1.24292(15) 0.0318(5) Uani 1 1 d . . .
C13 C 0.2322(3) -0.1382(2) 1.29258(18) 0.0396(6) Uani 1 1 d . . .
H13A H 0.2300 -0.1796 1.3520 0.048 Uiso 1 1 calc R . .
H13B H 0.3176 -0.0916 1.2826 0.048 Uiso 1 1 calc R . .
C14 C 0.1969(4) -0.2916(2) 1.13806(19) 0.0495(7) Uani 1 1 d . . .
H14A H 0.2310 -0.2563 1.0811 0.074 Uiso 1 1 calc R . .
H14B H 0.1050 -0.3276 1.1375 0.074 Uiso 1 1 calc R . .
H14C H 0.2713 -0.3409 1.1669 0.074 Uiso 1 1 calc R . .
C15 C 0.3886(3) -0.2744(2) 1.27141(18) 0.0475(7) Uani 1 1 d . . .
H15A H 0.3676 -0.3252 1.3257 0.071 Uiso 1 1 calc R . .
H15B H 0.4710 -0.2313 1.2754 0.071 Uiso 1 1 calc R . .
H15C H 0.4142 -0.3094 1.2316 0.071 Uiso 1 1 calc R . .
C16 C -0.0229(3) -0.0842(2) 1.42710(16) 0.0358(6) Uani 1 1 d . . .
H16A H -0.0850 -0.0470 1.4560 0.043 Uiso 1 1 calc R . .
H16B H -0.0827 -0.1406 1.4209 0.043 Uiso 1 1 calc R . .
C17 C 0.1063(3) -0.1300(2) 1.48076(15) 0.0336(5) Uani 1 1 d . . .
C18 C 0.2350(3) -0.0828(2) 1.47243(15) 0.0338(5) Uani 1 1 d . . .
C19 C 0.2726(2) 0.01970(19) 1.40976(15) 0.0320(5) Uani 1 1 d . . .
H19A H 0.2976 0.0669 1.4401 0.038 Uiso 1 1 calc R . .
H19B H 0.3619 0.0113 1.3785 0.038 Uiso 1 1 calc R . .
C20 C 0.0730(3) -0.2334(2) 1.54344(18) 0.0504(7) Uani 1 1 d . . .
H20A H 0.1582 -0.2574 1.5782 0.076 Uiso 1 1 calc R . .
H20B H 0.0510 -0.2820 1.5147 0.076 Uiso 1 1 calc R . .
H20C H -0.0118 -0.2279 1.5781 0.076 Uiso 1 1 calc R . .
C21 C 0.3648(3) -0.1250(2) 1.52557(19) 0.0518(8) Uani 1 1 d . . .
H21A H 0.3432 -0.1950 1.5614 0.078 Uiso 1 1 calc R . .
H21B H 0.3848 -0.0822 1.5597 0.078 Uiso 1 1 calc R . .
H21C H 0.4509 -0.1254 1.4902 0.078 Uiso 1 1 calc R . .
C22 C 0.3457(3) 0.2372(2) 1.30783(18) 0.0401(6) Uani 1 1 d . . .
H22A H 0.3340 0.2581 1.3577 0.048 Uiso 1 1 calc R . .
H22B H 0.4165 0.1800 1.3201 0.048 Uiso 1 1 calc R . .
C23 C 0.4042(3) 0.3263(2) 1.2362(2) 0.0437(7) Uani 1 1 d . . .
C24 C 0.4239(2) 0.31058(19) 1.16394(19) 0.0401(6) Uani 1 1 d . . .
C25 C 0.3766(2) 0.20910(18) 1.15752(16) 0.0329(5) Uani 1 1 d . . .
H25A H 0.3855 0.2112 1.0992 0.039 Uiso 1 1 calc R . .
H25B H 0.4414 0.1542 1.1909 0.039 Uiso 1 1 calc R . .
C26 C 0.4386(4) 0.4223(2) 1.2544(3) 0.0641(10) Uani 1 1 d . . .
H26A H 0.4796 0.4732 1.2044 0.096 Uiso 1 1 calc R . .
H26B H 0.5102 0.4073 1.2985 0.096 Uiso 1 1 calc R . .
H26C H 0.3486 0.4491 1.2721 0.096 Uiso 1 1 calc R . .
C27 C 0.4898(3) 0.3850(2) 1.0864(2) 0.0589(9) Uani 1 1 d . . .
H27A H 0.5246 0.4455 1.0980 0.088 Uiso 1 1 calc R . .
H27B H 0.4155 0.4052 1.0437 0.088 Uiso 1 1 calc R . .
H27C H 0.5724 0.3526 1.0668 0.088 Uiso 1 1 calc R . .
C28 C 0.0393(9) 0.4538(6) 1.1634(5) 0.0681(19) Uiso 0.50 1 d P . .
H28A H -0.0183 0.5002 1.1847 0.102 Uiso 0.50 1 calc PR . .
H28B H 0.1433 0.4597 1.1741 0.102 Uiso 0.50 1 calc PR . .
H28C H 0.0063 0.3834 1.1910 0.102 Uiso 0.50 1 calc PR . .
C29 C 0.0181(4) 0.4825(3) 1.06922(16) 0.0417(12) Uiso 0.50 1 d PG . .
C30 C 0.1240(4) 0.5364(3) 1.0119(2) 0.0310(10) Uiso 0.50 1 d PG . .
H30 H 0.2127 0.5565 1.0302 0.037 Uiso 0.50 1 calc PR . .
C31 C 0.1002(5) 0.5610(3) 0.92777(19) 0.0501(15) Uiso 0.50 1 d PG . .
H31 H 0.1726 0.5978 0.8886 0.060 Uiso 0.50 1 calc PR . .
C32 C -0.0295(5) 0.5317(4) 0.90094(16) 0.0545(16) Uiso 0.50 1 d PG . .
H32 H -0.0458 0.5485 0.8434 0.065 Uiso 0.50 1 calc PR . .
C33 C -0.1354(4) 0.4778(4) 0.9583(2) 0.0551(17) Uiso 0.50 1 d PG . .
H33 H -0.2240 0.4578 0.9399 0.066 Uiso 0.50 1 calc PR . .
C34 C -0.1116(4) 0.4532(3) 1.0424(2) 0.0419(13) Uiso 0.50 1 d PG . .
H34 H -0.1839 0.4164 1.0816 0.050 Uiso 0.50 1 calc PR . .
C35A C -0.462(2) -0.4124(14) 1.5056(12) 0.154(8) Uiso 0.328(7) 1 d PD A 1
H35A H -0.5084 -0.4801 1.5220 0.231 Uiso 0.328(7) 1 calc PR A 1
H35B H -0.5362 -0.3599 1.4817 0.231 Uiso 0.328(7) 1 calc PR A 1
H35C H -0.4211 -0.4011 1.5542 0.231 Uiso 0.328(7) 1 calc PR A 1
C36A C -0.3428(11) -0.4063(9) 1.4427(7) 0.159(9) Uiso 0.328(7) 1 d PG A 1
C37A C -0.2601(14) -0.3174(8) 1.4115(7) 0.086(3) Uiso 0.328(7) 1 d PGD A 1
H37A H -0.2810 -0.2604 1.4293 0.103 Uiso 0.328(7) 1 calc PR A 1
C38A C -0.1468(12) -0.3117(7) 1.3542(7) 0.131(8) Uiso 0.328(7) 1 d PG A 1
H38A H -0.0903 -0.2509 1.3329 0.157 Uiso 0.328(7) 1 calc PR A 1
C39A C -0.1162(10) -0.3950(9) 1.3282(6) 0.077(3) Uiso 0.328(7) 1 d PG A 1
H39A H -0.0387 -0.3912 1.2891 0.092 Uiso 0.328(7) 1 calc PR A 1
C40A C -0.1989(12) -0.4840(7) 1.3594(7) 0.133(7) Uiso 0.328(7) 1 d PG A 1
H40A H -0.1780 -0.5409 1.3417 0.160 Uiso 0.328(7) 1 calc PR A 1
C41A C -0.3122(12) -0.4896(7) 1.4167(7) 0.106(5) Uiso 0.328(7) 1 d PGD A 1
H41A H -0.3687 -0.5504 1.4380 0.127 Uiso 0.328(7) 1 calc PR A 1
C35B C 0.048(3) -0.4752(19) 1.3787(17) 0.181(7) Uiso 0.340(7) 1 d P B 2
H35D H 0.0811 -0.4395 1.3217 0.271 Uiso 0.340(7) 1 calc PR B 2
H35E H 0.0194 -0.5454 1.3841 0.271 Uiso 0.340(7) 1 calc PR B 2
H35F H 0.1270 -0.4767 1.4165 0.271 Uiso 0.340(7) 1 calc PR B 2
C36B C -0.1060(13) -0.4102(10) 1.4037(8) 0.157(8) Uiso 0.340(7) 1 d PG B 2
C37B C -0.1260(14) -0.4690(8) 1.4863(8) 0.110(6) Uiso 0.340(7) 1 d PG B 2
H37B H -0.0649 -0.5265 1.5100 0.133 Uiso 0.340(7) 1 calc PR B 2
C38B C -0.2352(16) -0.4435(10) 1.5343(6) 0.151(8) Uiso 0.340(7) 1 d PG B 2
H38B H -0.2488 -0.4837 1.5908 0.181 Uiso 0.340(7) 1 calc PR B 2
C39B C -0.3245(14) -0.3594(10) 1.4996(8) 0.197(11) Uiso 0.340(7) 1 d PG B 2
H39B H -0.3991 -0.3420 1.5324 0.236 Uiso 0.340(7) 1 calc PR B 2
C40B C -0.3046(13) -0.3007(8) 1.4170(8) 0.086(3) Uiso 0.340(7) 1 d PG B 2
H40B H -0.3656 -0.2432 1.3932 0.103 Uiso 0.340(7) 1 calc PR B 2
C41B C -0.1953(15) -0.3261(9) 1.3690(6) 0.090(5) Uiso 0.340(7) 1 d PG B 2
H41B H -0.1817 -0.2860 1.3125 0.108 Uiso 0.340(7) 1 calc PR B 2
C35C C -0.2281(18) -0.2770(12) 1.3575(10) 0.074(5) Uiso 0.233(5) 1 d PD C 3
H35G H -0.3263 -0.2820 1.3373 0.111 Uiso 0.233(5) 1 calc PR C 3
H35H H -0.1833 -0.2117 1.3247 0.111 Uiso 0.233(5) 1 calc PR C 3
H35I H -0.2354 -0.2810 1.4157 0.111 Uiso 0.233(5) 1 calc PR C 3
C36C C -0.1370(15) -0.3614(8) 1.3498(7) 0.077(3) Uiso 0.233(5) 1 d PGD C 3
C37C C 0.0065(16) -0.3804(12) 1.3760(11) 0.112(8) Uiso 0.233(5) 1 d PGD C 3
H37C H 0.0527 -0.3371 1.4010 0.134 Uiso 0.233(5) 1 calc PR C 3
C38C C 0.0825(15) -0.4629(14) 1.3655(13) 0.181(7) Uiso 0.233(5) 1 d PGD C 3
H38C H 0.1806 -0.4759 1.3834 0.217 Uiso 0.233(5) 1 calc PR C 3
C39C C 0.0150(19) -0.5264(10) 1.3289(10) 0.105(7) Uiso 0.233(5) 1 d PGD C 3
H39C H 0.0669 -0.5828 1.3218 0.126 Uiso 0.233(5) 1 calc PR C 3
C40C C -0.1285(19) -0.5074(11) 1.3028(10) 0.110(8) Uiso 0.233(5) 1 d PGD C 3
H40C H -0.1747 -0.5507 1.2778 0.132 Uiso 0.233(5) 1 calc PR C 3
C41C C -0.2045(14) -0.4249(12) 1.3132(10) 0.23(2) Uiso 0.233(5) 1 d PGD C 3
H41C H -0.3026 -0.4119 1.2953 0.273 Uiso 0.233(5) 1 calc PR C 3
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.01345(9) 0.02848(11) 0.03447(12) -0.01093(8) -0.00106(7) 0.00165(7)
P1 0.0159(2) 0.0233(3) 0.0340(3) -0.0098(2) -0.0011(2) 0.0034(2)
P2 0.0203(3) 0.0246(3) 0.0316(3) -0.0096(2) -0.0039(2) 0.0008(2)
P3 0.0177(2) 0.0293(3) 0.0330(3) -0.0121(2) -0.0009(2) -0.0005(2)
P4 0.0254(3) 0.0272(3) 0.0399(4) -0.0150(3) -0.0033(2) 0.0004(2)
N1 0.0214(8) 0.0248(9) 0.0338(10) -0.0111(8) 0.0015(7) 0.0043(7)
N2 0.0214(8) 0.0265(10) 0.0344(10) -0.0115(8) -0.0055(7) 0.0025(7)
N3 0.0213(9) 0.0301(10) 0.0350(11) -0.0118(8) -0.0031(8) 0.0004(7)
N4 0.0160(8) 0.0274(10) 0.0378(11) -0.0089(8) -0.0007(7) -0.0008(7)
O1 0.0425(11) 0.0730(15) 0.0414(11) -0.0145(10) -0.0116(9) 0.0121(10)
O2 0.0414(11) 0.0482(11) 0.0563(12) -0.0283(10) -0.0064(9) 0.0158(9)
O3 0.0320(10) 0.0637(14) 0.0815(17) -0.0125(12) 0.0173(10) -0.0144(10)
C1 0.0217(10) 0.0404(14) 0.0357(13) -0.0125(11) -0.0017(9) 0.0024(9)
C2 0.0223(11) 0.0404(14) 0.0391(14) -0.0147(11) 0.0013(10) 0.0054(10)
C3 0.0214(11) 0.0413(14) 0.0464(15) -0.0122(12) 0.0007(10) 0.0012(10)
C4 0.0289(11) 0.0277(12) 0.0369(13) -0.0086(10) -0.0013(10) 0.0081(9)
C5 0.0271(11) 0.0340(13) 0.0330(13) -0.0071(10) -0.0017(9) 0.0030(9)
C6 0.0267(11) 0.0331(13) 0.0331(13) -0.0104(10) 0.0002(9) 0.0050(9)
C7 0.0301(12) 0.0305(12) 0.0376(14) -0.0091(10) 0.0054(10) 0.0093(10)
C8 0.0474(16) 0.0374(15) 0.0430(16) -0.0011(12) 0.0063(13) 0.0047(12)
C9 0.0375(14) 0.0418(15) 0.0385(15) -0.0105(12) 0.0071(11) 0.0092(11)
C10 0.0402(13) 0.0268(12) 0.0368(14) -0.0130(10) -0.0097(11) 0.0009(10)
C11 0.0379(13) 0.0240(11) 0.0317(12) -0.0084(10) -0.0004(10) 0.0016(9)
C12 0.0333(12) 0.0273(12) 0.0338(13) -0.0086(10) -0.0009(10) 0.0052(9)
C13 0.0336(13) 0.0447(15) 0.0488(16) -0.0259(13) -0.0151(11) 0.0162(11)
C14 0.067(2) 0.0436(16) 0.0450(16) -0.0239(13) -0.0081(14) 0.0133(14)
C15 0.0485(16) 0.0507(17) 0.0457(16) -0.0189(14) -0.0067(13) 0.0230(13)
C16 0.0270(11) 0.0426(14) 0.0385(14) -0.0145(11) 0.0050(10) -0.0059(10)
C17 0.0366(13) 0.0402(14) 0.0256(12) -0.0133(10) 0.0025(10) -0.0026(11)
C18 0.0330(12) 0.0412(14) 0.0277(12) -0.0116(11) -0.0025(10) 0.0005(10)
C19 0.0241(11) 0.0385(13) 0.0324(13) -0.0099(10) -0.0027(9) -0.0020(9)
C20 0.0554(18) 0.0508(18) 0.0386(15) -0.0055(13) -0.0037(13) -0.0128(14)
C21 0.0470(17) 0.0561(18) 0.0442(17) -0.0043(14) -0.0156(13) -0.0021(14)
C22 0.0374(13) 0.0367(14) 0.0487(16) -0.0167(12) -0.0090(12) -0.0082(11)
C23 0.0275(12) 0.0313(13) 0.069(2) -0.0115(13) -0.0132(12) -0.0054(10)
C24 0.0186(10) 0.0290(13) 0.0629(19) -0.0011(12) -0.0050(11) -0.0030(9)
C25 0.0158(9) 0.0351(13) 0.0415(14) -0.0040(11) 0.0004(9) -0.0003(9)
C26 0.0524(19) 0.0423(17) 0.099(3) -0.0245(18) -0.0109(18) -0.0124(14)
C27 0.0381(15) 0.0476(18) 0.073(2) 0.0054(16) -0.0009(15) -0.0117(13)
#==============================================================================
# MOLECULAR GEOMETRY
_geom_special_details
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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
Mo1 C2 1.972(3) . ?
Mo1 C3 1.975(3) . ?
Mo1 C1 1.985(3) . ?
Mo1 P2 2.4778(6) . ?
Mo1 P3 2.4973(6) . ?
Mo1 P1 2.5275(6) . ?
P1 N4 1.685(2) . ?
P1 N1 1.7019(19) . ?
P1 C4 1.816(2) . ?
P1 P2 2.6493(8) . ?
P2 N2 1.690(2) . ?
P2 N1 1.705(2) . ?
P2 C10 1.805(2) . ?
P2 P3 2.6823(9) . ?
P3 N3 1.679(2) . ?
P3 N2 1.718(2) . ?
P3 C16 1.800(3) . ?
P4 N4 1.718(2) . ?
P4 N3 1.744(2) . ?
P4 C22 1.855(3) . ?
N1 C7 1.460(3) . ?
N2 C13 1.463(3) . ?
N3 C19 1.473(3) . ?
N4 C25 1.490(3) . ?
O1 C2 1.155(3) . ?
O2 C1 1.155(3) . ?
O3 C3 1.152(3) . ?
C4 C5 1.517(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.339(3) . ?
C5 C8 1.506(4) . ?
C6 C7 1.498(3) . ?
C6 C9 1.509(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.525(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.323(3) . ?
C11 C14 1.522(4) . ?
C12 C13 1.500(3) . ?
C12 C15 1.509(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.517(4) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.328(3) . ?
C17 C20 1.509(4) . ?
C18 C21 1.507(4) . ?
C18 C19 1.507(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.514(4) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.332(4) . ?
C23 C26 1.497(4) . ?
C24 C27 1.502(4) . ?
C24 C25 1.511(4) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.546(8) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.3900 . ?
C29 C34 1.3900 . ?
C29 C34 1.995(6) 2_567 ?
C29 C30 2.004(6) 2_567 ?
C30 C31 1.3900 . ?
C30 C29 2.004(6) 2_567 ?
C30 H30 0.9500 . ?
C31 C32 1.3900 . ?
C31 H31 0.9500 . ?
C32 C33 1.3900 . ?
C32 H32 0.9500 . ?
C33 C34 1.3900 . ?
C33 H33 0.9500 . ?
C34 C29 1.995(6) 2_567 ?
C34 H34 0.9500 . ?
C35A C36A 1.495(13) . ?
C35A H35A 0.9800 . ?
C35A H35B 0.9800 . ?
C35A H35C 0.9800 . ?
C36A C37A 1.3900 . ?
C36A C41A 1.3900 . ?
C37A C38A 1.3900 . ?
C37A H37A 0.9500 . ?
C38A C39A 1.3900 . ?
C38A H38A 0.9500 . ?
C39A C40A 1.3900 . ?
C39A H39A 0.9500 . ?
C40A C41A 1.3900 . ?
C40A H40A 0.9500 . ?
C41A H41A 0.9500 . ?
C35B C36B 1.78(2) . ?
C35B H35D 0.9800 . ?
C35B H35E 0.9800 . ?
C35B H35F 0.9800 . ?
C36B C37B 1.3900 . ?
C36B C41B 1.3900 . ?
C37B C38B 1.3900 . ?
C37B H37B 0.9500 . ?
C38B C39B 1.3900 . ?
C38B H38B 0.9500 . ?
C39B C40B 1.3900 . ?
C39B H39B 0.9500 . ?
C40B C41B 1.3900 . ?
C40B H40B 0.9500 . ?
C41B H41B 0.9500 . ?
C35C C36C 1.468(13) . ?
C35C H35G 0.9800 . ?
C35C H35H 0.9800 . ?
C35C H35I 0.9800 . ?
C36C C37C 1.3900 . ?
C36C C41C 1.3900 . ?
C37C C38C 1.3900 . ?
C37C H37C 0.9500 . ?
C38C C39C 1.3900 . ?
C38C H38C 0.9500 . ?
C39C C40C 1.3900 . ?
C39C H39C 0.9500 . ?
C40C C41C 1.3900 . ?
C40C H40C 0.9500 . ?
C41C H41C 0.9500 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Mo1 C3 89.63(11) . . ?
C2 Mo1 C1 92.40(10) . . ?
C3 Mo1 C1 91.74(10) . . ?
C2 Mo1 P2 101.25(7) . . ?
C3 Mo1 P2 102.82(8) . . ?
C1 Mo1 P2 159.98(7) . . ?
C2 Mo1 P3 166.13(7) . . ?
C3 Mo1 P3 90.41(8) . . ?
C1 Mo1 P3 101.46(7) . . ?
P2 Mo1 P3 65.25(2) . . ?
C2 Mo1 P1 92.04(7) . . ?
C3 Mo1 P1 166.69(8) . . ?
C1 Mo1 P1 101.38(7) . . ?
P2 Mo1 P1 63.906(19) . . ?
P3 Mo1 P1 84.83(2) . . ?
N4 P1 N1 109.19(9) . . ?
N4 P1 C4 105.03(11) . . ?
N1 P1 C4 98.72(10) . . ?
N4 P1 Mo1 113.75(7) . . ?
N1 P1 Mo1 94.23(7) . . ?
C4 P1 Mo1 132.05(8) . . ?
N4 P1 P2 110.98(7) . . ?
N1 P1 P2 38.99(7) . . ?
C4 P1 P2 131.33(9) . . ?
Mo1 P1 P2 57.135(18) . . ?
N2 P2 N1 112.06(10) . . ?
N2 P2 C10 100.04(10) . . ?
N1 P2 C10 104.63(11) . . ?
N2 P2 Mo1 96.01(7) . . ?
N1 P2 Mo1 95.93(6) . . ?
C10 P2 Mo1 146.70(9) . . ?
N2 P2 P1 101.92(7) . . ?
N1 P2 P1 38.91(6) . . ?
C10 P2 P1 142.82(9) . . ?
Mo1 P2 P1 58.959(18) . . ?
N2 P2 P3 38.45(7) . . ?
N1 P2 P3 109.47(7) . . ?
C10 P2 P3 133.99(9) . . ?
Mo1 P2 P3 57.727(18) . . ?
P1 P2 P3 78.94(2) . . ?
N3 P3 N2 109.96(10) . . ?
N3 P3 C16 100.03(11) . . ?
N2 P3 C16 104.03(11) . . ?
N3 P3 Mo1 119.02(7) . . ?
N2 P3 Mo1 94.58(7) . . ?
C16 P3 Mo1 127.49(8) . . ?
N3 P3 P2 122.80(7) . . ?
N2 P3 P2 37.71(7) . . ?
C16 P3 P2 127.93(9) . . ?
Mo1 P3 P2 57.024(18) . . ?
N4 P4 N3 105.91(10) . . ?
N4 P4 C22 96.07(11) . . ?
N3 P4 C22 101.02(11) . . ?
C7 N1 P1 124.12(16) . . ?
C7 N1 P2 131.45(15) . . ?
P1 N1 P2 102.09(10) . . ?
C13 N2 P2 123.98(17) . . ?
C13 N2 P3 128.87(17) . . ?
P2 N2 P3 103.84(10) . . ?
C19 N3 P3 122.16(16) . . ?
C19 N3 P4 125.28(15) . . ?
P3 N3 P4 111.50(11) . . ?
C25 N4 P1 123.47(17) . . ?
C25 N4 P4 120.67(16) . . ?
P1 N4 P4 115.66(10) . . ?
O2 C1 Mo1 178.7(2) . . ?
O1 C2 Mo1 177.6(2) . . ?
O3 C3 Mo1 178.9(3) . . ?
C5 C4 P1 117.70(16) . . ?
C5 C4 H4A 107.9 . . ?
P1 C4 H4A 107.9 . . ?
C5 C4 H4B 107.9 . . ?
P1 C4 H4B 107.9 . . ?
H4A C4 H4B 107.2 . . ?
C6 C5 C8 122.7(2) . . ?
C6 C5 C4 125.2(2) . . ?
C8 C5 C4 112.0(2) . . ?
C5 C6 C7 124.9(2) . . ?
C5 C6 C9 122.2(2) . . ?
C7 C6 C9 113.0(2) . . ?
N1 C7 C6 114.18(18) . . ?
N1 C7 H7A 108.7 . . ?
C6 C7 H7A 108.7 . . ?
N1 C7 H7B 108.7 . . ?
C6 C7 H7B 108.7 . . ?
H7A C7 H7B 107.6 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 P2 115.43(17) . . ?
C11 C10 H10A 108.4 . . ?
P2 C10 H10A 108.4 . . ?
C11 C10 H10B 108.4 . . ?
P2 C10 H10B 108.4 . . ?
H10A C10 H10B 107.5 . . ?
C12 C11 C14 122.5(2) . . ?
C12 C11 C10 125.1(2) . . ?
C14 C11 C10 112.3(2) . . ?
C11 C12 C13 125.7(2) . . ?
C11 C12 C15 123.9(2) . . ?
C13 C12 C15 110.4(2) . . ?
N2 C13 C12 115.3(2) . . ?
N2 C13 H13A 108.5 . . ?
C12 C13 H13A 108.5 . . ?
N2 C13 H13B 108.5 . . ?
C12 C13 H13B 108.5 . . ?
H13A C13 H13B 107.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 P3 114.81(17) . . ?
C17 C16 H16A 108.6 . . ?
P3 C16 H16A 108.6 . . ?
C17 C16 H16B 108.6 . . ?
P3 C16 H16B 108.6 . . ?
H16A C16 H16B 107.5 . . ?
C18 C17 C20 124.2(2) . . ?
C18 C17 C16 122.7(2) . . ?
C20 C17 C16 113.1(2) . . ?
C17 C18 C21 124.1(2) . . ?
C17 C18 C19 125.6(2) . . ?
C21 C18 C19 110.2(2) . . ?
N3 C19 C18 117.05(19) . . ?
N3 C19 H19A 108.0 . . ?
C18 C19 H19A 108.0 . . ?
N3 C19 H19B 108.0 . . ?
C18 C19 H19B 108.0 . . ?
H19A C19 H19B 107.3 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 P4 110.27(18) . . ?
C23 C22 H22A 109.6 . . ?
P4 C22 H22A 109.6 . . ?
C23 C22 H22B 109.6 . . ?
P4 C22 H22B 109.6 . . ?
H22A C22 H22B 108.1 . . ?
C24 C23 C26 126.5(3) . . ?
C24 C23 C22 116.8(2) . . ?
C26 C23 C22 116.7(3) . . ?
C23 C24 C27 126.1(3) . . ?
C23 C24 C25 118.3(2) . . ?
C27 C24 C25 115.6(3) . . ?
N4 C25 C24 110.1(2) . . ?
N4 C25 H25A 109.6 . . ?
C24 C25 H25A 109.6 . . ?
N4 C25 H25B 109.6 . . ?
C24 C25 H25B 109.6 . . ?
H25A C25 H25B 108.2 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C28 H28A 109.5 . . ?
C29 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C29 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 C34 120.0 . . ?
C30 C29 C28 121.9(4) . . ?
C34 C29 C28 118.1(4) . . ?
C30 C29 C34 23.2(2) . 2_567 ?
C34 C29 C34 96.9(2) . 2_567 ?
C28 C29 C34 145.0(4) . 2_567 ?
C30 C29 C30 97.2(2) . 2_567 ?
C34 C29 C30 22.9(2) . 2_567 ?
C28 C29 C30 140.8(4) . 2_567 ?
C34 C29 C30 74.03(17) 2_567 2_567 ?
C29 C30 C31 120.0 . . ?
C29 C30 C29 82.78(18) . 2_567 ?
C31 C30 C29 37.29(18) . 2_567 ?
C29 C30 H30 120.0 . . ?
C31 C30 H30 120.0 . . ?
C29 C30 H30 157.1 2_567 . ?
C32 C31 C30 120.0 . . ?
C32 C31 H31 120.0 . . ?
C30 C31 H31 120.0 . . ?
C33 C32 C31 120.0 . . ?
C33 C32 H32 120.0 . . ?
C31 C32 H32 120.0 . . ?
C32 C33 C34 120.0 . . ?
C32 C33 H33 120.0 . . ?
C34 C33 H33 120.0 . . ?
C33 C34 C29 120.0 . . ?
C33 C34 C29 36.93(18) . 2_567 ?
C29 C34 C29 83.14(18) . 2_567 ?
C33 C34 H34 120.0 . . ?
C29 C34 H34 120.0 . . ?
C29 C34 H34 156.8 2_567 . ?
C36A C35A H35A 109.5 . . ?
C36A C35A H35B 109.5 . . ?
H35A C35A H35B 109.5 . . ?
C36A C35A H35C 109.5 . . ?
H35A C35A H35C 109.5 . . ?
H35B C35A H35C 109.5 . . ?
C37A C36A C41A 120.0 . . ?
C37A C36A C35A 119.6(8) . . ?
C41A C36A C35A 120.4(8) . . ?
C36A C37A C38A 120.0 . . ?
C36A C37A H37A 120.0 . . ?
C38A C37A H37A 120.0 . . ?
C39A C38A C37A 120.0 . . ?
C39A C38A H38A 120.0 . . ?
C37A C38A H38A 120.0 . . ?
C40A C39A C38A 120.0 . . ?
C40A C39A H39A 120.0 . . ?
C38A C39A H39A 120.0 . . ?
C39A C40A C41A 120.0 . . ?
C39A C40A H40A 120.0 . . ?
C41A C40A H40A 120.0 . . ?
C40A C41A C36A 120.0 . . ?
C40A C41A H41A 120.0 . . ?
C36A C41A H41A 120.0 . . ?
C36B C35B H35D 109.5 . . ?
C36B C35B H35E 109.5 . . ?
H35D C35B H35E 109.5 . . ?
C36B C35B H35F 109.5 . . ?
H35D C35B H35F 109.5 . . ?
H35E C35B H35F 109.5 . . ?
C37B C36B C41B 120.0 . . ?
C37B C36B C35B 98.9(12) . . ?
C41B C36B C35B 141.0(12) . . ?
C36B C37B C38B 120.0 . . ?
C36B C37B H37B 120.0 . . ?
C38B C37B H37B 120.0 . . ?
C39B C38B C37B 120.0 . . ?
C39B C38B H38B 120.0 . . ?
C37B C38B H38B 120.0 . . ?
C38B C39B C40B 120.0 . . ?
C38B C39B H39B 120.0 . . ?
C40B C39B H39B 120.0 . . ?
C41B C40B C39B 120.0 . . ?
C41B C40B H40B 120.0 . . ?
C39B C40B H40B 120.0 . . ?
C40B C41B C36B 120.0 . . ?
C40B C41B H41B 120.0 . . ?
C36B C41B H41B 120.0 . . ?
C36C C35C H35G 109.5 . . ?
C36C C35C H35H 109.5 . . ?
H35G C35C H35H 109.5 . . ?
C36C C35C H35I 109.5 . . ?
H35G C35C H35I 109.5 . . ?
H35H C35C H35I 109.5 . . ?
C37C C36C C41C 120.0 . . ?
C37C C36C C35C 125.0(9) . . ?
C41C C36C C35C 115.0(9) . . ?
C38C C37C C36C 120.0 . . ?
C38C C37C H37C 120.0 . . ?
C36C C37C H37C 120.0 . . ?
C37C C38C C39C 120.0 . . ?
C37C C38C H38C 120.0 . . ?
C39C C38C H38C 120.0 . . ?
C40C C39C C38C 120.0 . . ?
C40C C39C H39C 120.0 . . ?
C38C C39C H39C 120.0 . . ?
C41C C40C C39C 120.0 . . ?
C41C C40C H40C 120.0 . . ?
C39C C40C H40C 120.0 . . ?
C40C C41C C36C 120.0 . . ?
C40C C41C H41C 120.0 . . ?
C36C C41C H41C 120.0 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 Mo1 P1 N4 158.01(11) . . . . ?
C3 Mo1 P1 N4 -105.0(4) . . . . ?
C1 Mo1 P1 N4 65.15(10) . . . . ?
P2 Mo1 P1 N4 -100.45(8) . . . . ?
P3 Mo1 P1 N4 -35.53(8) . . . . ?
C2 Mo1 P1 N1 -88.87(10) . . . . ?
C3 Mo1 P1 N1 8.1(4) . . . . ?
C1 Mo1 P1 N1 178.27(10) . . . . ?
P2 Mo1 P1 N1 12.67(7) . . . . ?
P3 Mo1 P1 N1 77.60(7) . . . . ?
C2 Mo1 P1 C4 16.89(13) . . . . ?
C3 Mo1 P1 C4 113.9(4) . . . . ?
C1 Mo1 P1 C4 -75.97(13) . . . . ?
P2 Mo1 P1 C4 118.42(11) . . . . ?
P3 Mo1 P1 C4 -176.65(11) . . . . ?
C2 Mo1 P1 P2 -101.54(8) . . . . ?
C3 Mo1 P1 P2 -4.5(3) . . . . ?
C1 Mo1 P1 P2 165.60(7) . . . . ?
P3 Mo1 P1 P2 64.93(2) . . . . ?
C2 Mo1 P2 N2 -172.97(10) . . . . ?
C3 Mo1 P2 N2 -80.76(11) . . . . ?
C1 Mo1 P2 N2 54.9(2) . . . . ?
P3 Mo1 P2 N2 3.68(7) . . . . ?
P1 Mo1 P2 N2 100.31(7) . . . . ?
C2 Mo1 P2 N1 74.04(10) . . . . ?
C3 Mo1 P2 N1 166.25(11) . . . . ?
C1 Mo1 P2 N1 -58.1(2) . . . . ?
P3 Mo1 P2 N1 -109.31(7) . . . . ?
P1 Mo1 P2 N1 -12.68(7) . . . . ?
C2 Mo1 P2 C10 -54.31(18) . . . . ?
C3 Mo1 P2 C10 37.89(18) . . . . ?
C1 Mo1 P2 C10 173.6(3) . . . . ?
P3 Mo1 P2 C10 122.33(16) . . . . ?
P1 Mo1 P2 C10 -141.04(16) . . . . ?
C2 Mo1 P2 P1 86.73(8) . . . . ?
C3 Mo1 P2 P1 178.93(8) . . . . ?
C1 Mo1 P2 P1 -45.4(2) . . . . ?
P3 Mo1 P2 P1 -96.62(2) . . . . ?
C2 Mo1 P2 P3 -176.65(8) . . . . ?
C3 Mo1 P2 P3 -84.44(8) . . . . ?
C1 Mo1 P2 P3 51.2(2) . . . . ?
P1 Mo1 P2 P3 96.62(2) . . . . ?
N4 P1 P2 N2 15.54(10) . . . . ?
N1 P1 P2 N2 110.46(13) . . . . ?
C4 P1 P2 N2 150.54(12) . . . . ?
Mo1 P1 P2 N2 -89.88(7) . . . . ?
N4 P1 P2 N1 -94.93(13) . . . . ?
C4 P1 P2 N1 40.07(14) . . . . ?
Mo1 P1 P2 N1 159.65(11) . . . . ?
N4 P1 P2 C10 -109.42(15) . . . . ?
N1 P1 P2 C10 -14.50(17) . . . . ?
C4 P1 P2 C10 25.57(17) . . . . ?
Mo1 P1 P2 C10 145.16(14) . . . . ?
N4 P1 P2 Mo1 105.42(8) . . . . ?
N1 P1 P2 Mo1 -159.65(11) . . . . ?
C4 P1 P2 Mo1 -119.58(10) . . . . ?
N4 P1 P2 P3 46.58(8) . . . . ?
N1 P1 P2 P3 141.50(10) . . . . ?
C4 P1 P2 P3 -178.42(10) . . . . ?
Mo1 P1 P2 P3 -58.842(18) . . . . ?
C2 Mo1 P3 N3 126.1(3) . . . . ?
C3 Mo1 P3 N3 -143.82(11) . . . . ?
C1 Mo1 P3 N3 -51.96(11) . . . . ?
P2 Mo1 P3 N3 112.24(8) . . . . ?
P1 Mo1 P3 N3 48.64(8) . . . . ?
C2 Mo1 P3 N2 10.2(3) . . . . ?
C3 Mo1 P3 N2 100.33(10) . . . . ?
C1 Mo1 P3 N2 -167.81(10) . . . . ?
P2 Mo1 P3 N2 -3.61(7) . . . . ?
P1 Mo1 P3 N2 -67.21(7) . . . . ?
C2 Mo1 P3 C16 -101.4(3) . . . . ?
C3 Mo1 P3 C16 -11.26(14) . . . . ?
C1 Mo1 P3 C16 80.60(13) . . . . ?
P2 Mo1 P3 C16 -115.20(12) . . . . ?
P1 Mo1 P3 C16 -178.80(12) . . . . ?
C2 Mo1 P3 P2 13.8(3) . . . . ?
C3 Mo1 P3 P2 103.95(8) . . . . ?
C1 Mo1 P3 P2 -164.20(7) . . . . ?
P1 Mo1 P3 P2 -63.60(2) . . . . ?
N2 P2 P3 N3 80.25(13) . . . . ?
N1 P2 P3 N3 -21.02(11) . . . . ?
C10 P2 P3 N3 114.51(15) . . . . ?
Mo1 P2 P3 N3 -105.65(8) . . . . ?
P1 P2 P3 N3 -45.52(8) . . . . ?
N1 P2 P3 N2 -101.26(13) . . . . ?
C10 P2 P3 N2 34.26(16) . . . . ?
Mo1 P2 P3 N2 174.10(11) . . . . ?
P1 P2 P3 N2 -125.76(11) . . . . ?
N2 P2 P3 C16 -59.64(15) . . . . ?
N1 P2 P3 C16 -160.90(12) . . . . ?
C10 P2 P3 C16 -25.38(16) . . . . ?
Mo1 P2 P3 C16 114.47(11) . . . . ?
P1 P2 P3 C16 174.60(10) . . . . ?
N2 P2 P3 Mo1 -174.10(11) . . . . ?
N1 P2 P3 Mo1 84.63(7) . . . . ?
C10 P2 P3 Mo1 -139.84(12) . . . . ?
P1 P2 P3 Mo1 60.132(17) . . . . ?
N4 P1 N1 C7 -64.4(2) . . . . ?
C4 P1 N1 C7 44.9(2) . . . . ?
Mo1 P1 N1 C7 178.60(18) . . . . ?
P2 P1 N1 C7 -164.4(2) . . . . ?
N4 P1 N1 P2 99.94(11) . . . . ?
C4 P1 N1 P2 -150.72(11) . . . . ?
Mo1 P1 N1 P2 -17.03(9) . . . . ?
N2 P2 N1 C7 81.2(2) . . . . ?
C10 P2 N1 C7 -26.3(2) . . . . ?
Mo1 P2 N1 C7 -179.9(2) . . . . ?
P1 P2 N1 C7 162.7(3) . . . . ?
P3 P2 N1 C7 122.3(2) . . . . ?
N2 P2 N1 P1 -81.53(11) . . . . ?
C10 P2 N1 P1 171.01(10) . . . . ?
Mo1 P2 N1 P1 17.43(9) . . . . ?
P3 P2 N1 P1 -40.39(10) . . . . ?
N1 P2 N2 C13 -67.1(2) . . . . ?
C10 P2 N2 C13 43.3(2) . . . . ?
Mo1 P2 N2 C13 -165.98(19) . . . . ?
P1 P2 N2 C13 -106.5(2) . . . . ?
P3 P2 N2 C13 -161.0(3) . . . . ?
N1 P2 N2 P3 93.90(11) . . . . ?
C10 P2 N2 P3 -155.71(11) . . . . ?
Mo1 P2 N2 P3 -5.01(9) . . . . ?
P1 P2 N2 P3 54.48(9) . . . . ?
N3 P3 N2 C13 41.5(3) . . . . ?
C16 P3 N2 C13 -64.9(2) . . . . ?
Mo1 P3 N2 C13 164.6(2) . . . . ?
P2 P3 N2 C13 159.7(3) . . . . ?
N3 P3 N2 P2 -118.19(11) . . . . ?
C16 P3 N2 P2 135.45(11) . . . . ?
Mo1 P3 N2 P2 4.96(9) . . . . ?
N2 P3 N3 C19 -66.4(2) . . . . ?
C16 P3 N3 C19 42.6(2) . . . . ?
Mo1 P3 N3 C19 -173.76(15) . . . . ?
P2 P3 N3 C19 -106.28(18) . . . . ?
N2 P3 N3 P4 102.40(12) . . . . ?
C16 P3 N3 P4 -148.57(12) . . . . ?
Mo1 P3 N3 P4 -4.98(14) . . . . ?
P2 P3 N3 P4 62.50(13) . . . . ?
N4 P4 N3 C19 100.8(2) . . . . ?
C22 P4 N3 C19 1.2(2) . . . . ?
N4 P4 N3 P3 -67.52(13) . . . . ?
C22 P4 N3 P3 -167.16(13) . . . . ?
N1 P1 N4 C25 63.8(2) . . . . ?
C4 P1 N4 C25 -41.2(2) . . . . ?
Mo1 P1 N4 C25 167.64(15) . . . . ?
P2 P1 N4 C25 105.43(17) . . . . ?
N1 P1 N4 P4 -121.35(12) . . . . ?
C4 P1 N4 P4 133.59(12) . . . . ?
Mo1 P1 N4 P4 -17.55(13) . . . . ?
P2 P1 N4 P4 -79.76(11) . . . . ?
N3 P4 N4 C25 -101.36(18) . . . . ?
C22 P4 N4 C25 1.95(19) . . . . ?
N3 P4 N4 P1 83.68(13) . . . . ?
C22 P4 N4 P1 -173.02(13) . . . . ?
C2 Mo1 C1 O2 -112(9) . . . . ?
C3 Mo1 C1 O2 158(9) . . . . ?
P2 Mo1 C1 O2 21(9) . . . . ?
P3 Mo1 C1 O2 67(9) . . . . ?
P1 Mo1 C1 O2 -19(9) . . . . ?
C3 Mo1 C2 O1 -46(5) . . . . ?
C1 Mo1 C2 O1 -138(5) . . . . ?
P2 Mo1 C2 O1 57(5) . . . . ?
P3 Mo1 C2 O1 44(5) . . . . ?
P1 Mo1 C2 O1 121(5) . . . . ?
C2 Mo1 C3 O3 32(12) . . . . ?
C1 Mo1 C3 O3 125(12) . . . . ?
P2 Mo1 C3 O3 -69(12) . . . . ?
P3 Mo1 C3 O3 -134(12) . . . . ?
P1 Mo1 C3 O3 -65(12) . . . . ?
N4 P1 C4 C5 85.2(2) . . . . ?
N1 P1 C4 C5 -27.5(2) . . . . ?
Mo1 P1 C4 C5 -131.27(16) . . . . ?
P2 P1 C4 C5 -51.6(2) . . . . ?
P1 C4 C5 C6 11.5(4) . . . . ?
P1 C4 C5 C8 -168.0(2) . . . . ?
C8 C5 C6 C7 177.2(3) . . . . ?
C4 C5 C6 C7 -2.3(4) . . . . ?
C8 C5 C6 C9 -0.7(4) . . . . ?
C4 C5 C6 C9 179.8(2) . . . . ?
P1 N1 C7 C6 -41.8(3) . . . . ?
P2 N1 C7 C6 158.78(18) . . . . ?
C5 C6 C7 N1 15.4(4) . . . . ?
C9 C6 C7 N1 -166.5(2) . . . . ?
N2 P2 C10 C11 -34.1(2) . . . . ?
N1 P2 C10 C11 82.0(2) . . . . ?
Mo1 P2 C10 C11 -151.69(13) . . . . ?
P1 P2 C10 C11 91.4(2) . . . . ?
P3 P2 C10 C11 -54.9(2) . . . . ?
P2 C10 C11 C12 18.3(3) . . . . ?
P2 C10 C11 C14 -164.9(2) . . . . ?
C14 C11 C12 C13 -176.6(3) . . . . ?
C10 C11 C12 C13 -0.1(4) . . . . ?
C14 C11 C12 C15 3.4(4) . . . . ?
C10 C11 C12 C15 179.9(3) . . . . ?
P2 N2 C13 C12 -31.5(3) . . . . ?
P3 N2 C13 C12 172.49(17) . . . . ?
C11 C12 C13 N2 4.7(4) . . . . ?
C15 C12 C13 N2 -175.2(2) . . . . ?
N3 P3 C16 C17 -43.3(2) . . . . ?
N2 P3 C16 C17 70.3(2) . . . . ?
Mo1 P3 C16 C17 177.52(14) . . . . ?
P2 P3 C16 C17 103.30(18) . . . . ?
P3 C16 C17 C18 27.8(3) . . . . ?
P3 C16 C17 C20 -152.1(2) . . . . ?
C20 C17 C18 C21 -1.2(4) . . . . ?
C16 C17 C18 C21 178.9(3) . . . . ?
C20 C17 C18 C19 179.1(3) . . . . ?
C16 C17 C18 C19 -0.8(4) . . . . ?
P3 N3 C19 C18 -23.0(3) . . . . ?
P4 N3 C19 C18 169.78(18) . . . . ?
C17 C18 C19 N3 -3.6(4) . . . . ?
C21 C18 C19 N3 176.7(2) . . . . ?
N4 P4 C22 C23 49.7(2) . . . . ?
N3 P4 C22 C23 157.3(2) . . . . ?
P4 C22 C23 C24 -58.3(3) . . . . ?
P4 C22 C23 C26 123.6(2) . . . . ?
C26 C23 C24 C27 2.3(4) . . . . ?
C22 C23 C24 C27 -175.6(2) . . . . ?
C26 C23 C24 C25 -177.8(3) . . . . ?
C22 C23 C24 C25 4.4(3) . . . . ?
P1 N4 C25 C24 123.8(2) . . . . ?
P4 N4 C25 C24 -50.8(2) . . . . ?
C23 C24 C25 N4 52.0(3) . . . . ?
C27 C24 C25 N4 -128.1(2) . . . . ?
C34 C29 C30 C31 0.0 . . . . ?
C28 C29 C30 C31 -179.7(5) . . . . ?
C34 C29 C30 C31 5.8(6) 2_567 . . . ?
C30 C29 C30 C31 2.3(3) 2_567 . . . ?
C34 C29 C30 C29 -2.31(19) . . . 2_567 ?
C28 C29 C30 C29 178.0(5) . . . 2_567 ?
C34 C29 C30 C29 3.5(4) 2_567 . . 2_567 ?
C30 C29 C30 C29 0.00(13) 2_567 . . 2_567 ?
C29 C30 C31 C32 0.0 . . . . ?
C29 C30 C31 C32 3.8(3) 2_567 . . . ?
C30 C31 C32 C33 0.0 . . . . ?
C31 C32 C33 C34 0.0 . . . . ?
C32 C33 C34 C29 0.0 . . . . ?
C32 C33 C34 C29 -3.8(3) . . . 2_567 ?
C30 C29 C34 C33 0.0 . . . . ?
C28 C29 C34 C33 179.7(4) . . . . ?
C34 C29 C34 C33 -2.3(2) 2_567 . . . ?
C30 C29 C34 C33 -5.9(6) 2_567 . . . ?
C30 C29 C34 C29 2.3(2) . . . 2_567 ?
C28 C29 C34 C29 -177.9(5) . . . 2_567 ?
C34 C29 C34 C29 0.00(13) 2_567 . . 2_567 ?
C30 C29 C34 C29 -3.6(5) 2_567 . . 2_567 ?
C41A C36A C37A C38A 0.0 . . . . ?
C35A C36A C37A C38A 178.7(14) . . . . ?
C36A C37A C38A C39A 0.0 . . . . ?
C37A C38A C39A C40A 0.0 . . . . ?
C38A C39A C40A C41A 0.0 . . . . ?
C39A C40A C41A C36A 0.0 . . . . ?
C37A C36A C41A C40A 0.0 . . . . ?
C35A C36A C41A C40A -178.7(14) . . . . ?
C41B C36B C37B C38B 0.0 . . . . ?
C35B C36B C37B C38B 177.7(12) . . . . ?
C36B C37B C38B C39B 0.0 . . . . ?
C37B C38B C39B C40B 0.0 . . . . ?
C38B C39B C40B C41B 0.0 . . . . ?
C39B C40B C41B C36B 0.0 . . . . ?
C37B C36B C41B C40B 0.0 . . . . ?
C35B C36B C41B C40B -176.3(18) . . . . ?
C41C C36C C37C C38C 0.0 . . . . ?
C35C C36C C37C C38C 179.95(9) . . . . ?
C36C C37C C38C C39C 0.0 . . . . ?
C37C C38C C39C C40C 0.0 . . . . ?
C38C C39C C40C C41C 0.0 . . . . ?
C39C C40C C41C C36C 0.0 . . . . ?
C37C C36C C41C C40C 0.0 . . . . ?
C35C C36C C41C C40C -179.96(8) . . . . ?
_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full 31.00
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max 0.907
_refine_diff_density_min -0.499
_refine_diff_density_rms 0.089
_database_code_depnum_ccdc_archive 'CCDC 956162'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_is_ch268_[PN(C6H10)]4Mo(CO)3
_audit_creation_method SHELXL-97
#==============================================================================
# CHEMICAL DATA
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C27 H40 Mo N4 O3 P4'
_chemical_formula_sum 'C27 H40 Mo N4 O3 P4'
_chemical_formula_weight 688.45
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
#==============================================================================
# CRYSTAL DATA
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/c'
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_Int_Tables_number 14
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 9.0715(4)
_cell_length_b 18.1902(6)
_cell_length_c 18.4948(7)
_cell_angle_alpha 90.00
_cell_angle_beta 94.483(2)
_cell_angle_gamma 90.00
_cell_volume 3042.5(2)
_cell_formula_units_Z 4
_cell_measurement_temperature 173(2)
_cell_measurement_reflns_used 3043
_cell_measurement_theta_min 4.504
_cell_measurement_theta_max 47.106
_exptl_crystal_description block
_exptl_crystal_colour yellow
_exptl_crystal_size_max 0.12
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.08
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.503
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1424
_exptl_absorpt_coefficient_mu 0.677
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.9231
_exptl_absorpt_correction_T_max 0.9478
_exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)'
#==============================================================================
# EXPERIMENTAL DATA
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 173(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker Apex Kappa II-CCD-diffractometer'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 39864
_diffrn_reflns_av_R_equivalents 0.1066
_diffrn_reflns_av_sigmaI/netI 0.1163
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_k_max 24
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_theta_min 1.57
_diffrn_reflns_theta_max 28.00
_reflns_number_total 7327
_reflns_number_gt 4492
_reflns_threshold_expression >2\s(I)
_computing_data_collection 'Bruker Apex V7.51A'
_computing_cell_refinement 'Bruker Apex V7.51A'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material SHELXL-97
#==============================================================================
# REFINEMENT DATA
_refine_special_details
;
All H atoms were positioned geometrically and refined using a riding model,
with C---H = 0.98 (methyl groups), 0.99\%A (methylene groups),
1.00\%A (methine groups) or 0.95 \%A (aryl CH) and with U~iso~(H) =
1.5 times U~eq~(C) (methyl groups) or with U~iso~(H) = 1.2 times
U~eq~(C) (methylene groups, aryl CH, methine groups). Torsion angles
of all methyl groups were allowed to refine.
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0326P)^2^+3.2702P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 7327
_refine_ls_number_parameters 360
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1145
_refine_ls_R_factor_gt 0.0522
_refine_ls_wR_factor_ref 0.1104
_refine_ls_wR_factor_gt 0.0897
_refine_ls_goodness_of_fit_ref 1.013
_refine_ls_restrained_S_all 1.013
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
#==============================================================================
# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_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
Mo1 Mo 0.34802(4) 0.273530(19) 0.862409(19) 0.01522(10) Uani 1 1 d . . .
P1 P 0.51923(12) 0.37874(6) 0.87926(6) 0.0216(3) Uani 1 1 d . . .
P2 P 0.49517(13) 0.29758(6) 0.75900(6) 0.0223(3) Uani 1 1 d . . .
P3 P 0.57677(12) 0.19788(6) 0.85775(6) 0.0214(3) Uani 1 1 d . . .
P4 P 0.68104(13) 0.28585(6) 0.98113(6) 0.0228(3) Uani 1 1 d . . .
N1 N 0.6637(4) 0.37281(18) 0.94107(18) 0.0236(8) Uani 1 1 d . . .
N2 N 0.5787(4) 0.37376(18) 0.79341(18) 0.0231(8) Uani 1 1 d . . .
N3 N 0.6075(4) 0.22249(18) 0.77138(18) 0.0226(8) Uani 1 1 d . . .
N4 N 0.7216(4) 0.22536(19) 0.91349(18) 0.0227(8) Uani 1 1 d . . .
O1 O 0.2752(4) 0.2468(2) 1.02268(19) 0.0448(9) Uani 1 1 d . . .
O2 O 0.0810(4) 0.3803(2) 0.8345(2) 0.0593(11) Uani 1 1 d . . .
O3 O 0.1487(4) 0.1488(2) 0.7936(2) 0.0612(12) Uani 1 1 d . . .
C1 C 0.4664(5) 0.4741(2) 0.8896(2) 0.0279(11) Uani 1 1 d . . .
H1A H 0.4064 0.4894 0.8452 0.034 Uiso 1 1 calc R . .
H1B H 0.4024 0.4774 0.9305 0.034 Uiso 1 1 calc R . .
C2 C 0.5921(5) 0.5278(2) 0.9031(2) 0.0257(10) Uani 1 1 d . . .
C3 C 0.7278(5) 0.5085(2) 0.9291(2) 0.0247(10) Uani 1 1 d . . .
C4 C 0.7776(5) 0.4310(2) 0.9476(2) 0.0273(11) Uani 1 1 d . . .
H4A H 0.8564 0.4178 0.9158 0.033 Uiso 1 1 calc R . .
H4B H 0.8226 0.4309 0.9982 0.033 Uiso 1 1 calc R . .
C5 C 0.5486(5) 0.6061(2) 0.8863(3) 0.0382(13) Uani 1 1 d . . .
H5A H 0.6312 0.6387 0.9015 0.057 Uiso 1 1 calc R . .
H5B H 0.4625 0.6191 0.9125 0.057 Uiso 1 1 calc R . .
H5C H 0.5239 0.6114 0.8341 0.057 Uiso 1 1 calc R . .
C6 C 0.8514(5) 0.5618(3) 0.9444(3) 0.0387(13) Uani 1 1 d . . .
H6A H 0.8335 0.6057 0.9143 0.058 Uiso 1 1 calc R . .
H6B H 0.9448 0.5390 0.9332 0.058 Uiso 1 1 calc R . .
H6C H 0.8572 0.5758 0.9957 0.058 Uiso 1 1 calc R . .
C7 C 0.4843(5) 0.3190(2) 0.6629(2) 0.0275(11) Uani 1 1 d . . .
H7A H 0.5050 0.2733 0.6365 0.033 Uiso 1 1 calc R . .
H7B H 0.3809 0.3331 0.6481 0.033 Uiso 1 1 calc R . .
C8 C 0.5832(5) 0.3781(2) 0.6372(2) 0.0284(11) Uani 1 1 d . . .
C9 C 0.6806(5) 0.4165(2) 0.6798(3) 0.0309(11) Uani 1 1 d . . .
C10 C 0.6997(5) 0.4122(3) 0.7618(2) 0.0315(11) Uani 1 1 d . . .
H10A H 0.7938 0.3867 0.7763 0.038 Uiso 1 1 calc R . .
H10B H 0.7069 0.4627 0.7818 0.038 Uiso 1 1 calc R . .
C11 C 0.5570(6) 0.3925(3) 0.5567(2) 0.0455(14) Uani 1 1 d . . .
H11A H 0.6155 0.4351 0.5436 0.068 Uiso 1 1 calc R . .
H11B H 0.4518 0.4024 0.5445 0.068 Uiso 1 1 calc R . .
H11C H 0.5869 0.3493 0.5297 0.068 Uiso 1 1 calc R . .
C12 C 0.7843(6) 0.4720(3) 0.6501(3) 0.0464(14) Uani 1 1 d . . .
H12A H 0.7999 0.4597 0.5997 0.070 Uiso 1 1 calc R . .
H12B H 0.8792 0.4711 0.6792 0.070 Uiso 1 1 calc R . .
H12C H 0.7409 0.5213 0.6521 0.070 Uiso 1 1 calc R . .
C13 C 0.6003(5) 0.0990(2) 0.8488(2) 0.0269(11) Uani 1 1 d . . .
H13A H 0.6341 0.0792 0.8972 0.032 Uiso 1 1 calc R . .
H13B H 0.5021 0.0773 0.8350 0.032 Uiso 1 1 calc R . .
C14 C 0.7068(5) 0.0724(2) 0.7949(2) 0.0258(10) Uani 1 1 d . . .
C15 C 0.7645(5) 0.1139(2) 0.7448(2) 0.0242(10) Uani 1 1 d . . .
C16 C 0.7322(5) 0.1954(2) 0.7336(2) 0.0271(11) Uani 1 1 d . . .
H16A H 0.8216 0.2237 0.7503 0.033 Uiso 1 1 calc R . .
H16B H 0.7119 0.2047 0.6810 0.033 Uiso 1 1 calc R . .
C17 C 0.7401(5) -0.0081(2) 0.8054(2) 0.0334(12) Uani 1 1 d . . .
H17A H 0.8028 -0.0249 0.7678 0.050 Uiso 1 1 calc R . .
H17B H 0.6474 -0.0361 0.8018 0.050 Uiso 1 1 calc R . .
H17C H 0.7917 -0.0159 0.8533 0.050 Uiso 1 1 calc R . .
C18 C 0.8717(5) 0.0857(2) 0.6934(2) 0.0318(11) Uani 1 1 d . . .
H18A H 0.9187 0.0408 0.7132 0.048 Uiso 1 1 calc R . .
H18B H 0.9476 0.1231 0.6872 0.048 Uiso 1 1 calc R . .
H18C H 0.8188 0.0750 0.6464 0.048 Uiso 1 1 calc R . .
C19 C 0.8719(5) 0.2913(2) 1.0241(2) 0.0268(11) Uani 1 1 d . . .
H19A H 0.9342 0.3193 0.9921 0.032 Uiso 1 1 calc R . .
H19B H 0.8711 0.3182 1.0706 0.032 Uiso 1 1 calc R . .
C20 C 0.9383(5) 0.2157(2) 1.0380(2) 0.0254(10) Uani 1 1 d . . .
C21 C 0.9448(5) 0.1719(2) 0.9808(2) 0.0261(10) Uani 1 1 d . . .
C22 C 0.8764(5) 0.1997(2) 0.9086(2) 0.0269(10) Uani 1 1 d . . .
H22A H 0.9368 0.2407 0.8919 0.032 Uiso 1 1 calc R . .
H22B H 0.8773 0.1597 0.8723 0.032 Uiso 1 1 calc R . .
C23 C 1.0005(5) 0.1992(3) 1.1143(2) 0.0341(12) Uani 1 1 d . . .
H23A H 0.9197 0.1971 1.1464 0.051 Uiso 1 1 calc R . .
H23B H 1.0702 0.2380 1.1308 0.051 Uiso 1 1 calc R . .
H23C H 1.0519 0.1518 1.1151 0.051 Uiso 1 1 calc R . .
C24 C 1.0200(6) 0.0985(3) 0.9795(3) 0.0422(13) Uani 1 1 d . . .
H24A H 1.0624 0.0863 1.0284 0.063 Uiso 1 1 calc R . .
H24B H 1.0990 0.1005 0.9463 0.063 Uiso 1 1 calc R . .
H24C H 0.9478 0.0608 0.9630 0.063 Uiso 1 1 calc R . .
C25 C 0.3012(5) 0.2565(2) 0.9627(3) 0.0289(11) Uani 1 1 d . . .
C26 C 0.1823(6) 0.3405(3) 0.8448(3) 0.0365(12) Uani 1 1 d . . .
C27 C 0.2251(5) 0.1942(3) 0.8203(3) 0.0346(12) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.01251(18) 0.01449(19) 0.01855(18) 0.00016(16) 0.00055(13) -0.00175(16)
P1 0.0199(6) 0.0222(6) 0.0227(6) -0.0003(5) 0.0011(5) 0.0002(5)
P2 0.0234(6) 0.0203(6) 0.0231(6) -0.0001(5) 0.0008(5) -0.0016(5)
P3 0.0222(6) 0.0192(6) 0.0229(6) -0.0002(5) 0.0030(5) -0.0028(5)
P4 0.0241(6) 0.0213(7) 0.0230(6) -0.0002(5) 0.0020(5) 0.0009(5)
N1 0.023(2) 0.019(2) 0.028(2) -0.0010(16) -0.0015(16) -0.0048(16)
N2 0.023(2) 0.020(2) 0.026(2) -0.0018(16) 0.0024(16) -0.0059(16)
N3 0.0236(19) 0.020(2) 0.0252(19) 0.0018(16) 0.0051(15) 0.0020(16)
N4 0.0171(18) 0.026(2) 0.0253(19) -0.0044(17) 0.0018(15) 0.0011(16)
O1 0.040(2) 0.061(3) 0.034(2) 0.0026(18) 0.0060(17) -0.0082(18)
O2 0.035(2) 0.059(3) 0.085(3) 0.021(2) 0.009(2) 0.016(2)
O3 0.055(3) 0.052(3) 0.073(3) -0.014(2) -0.013(2) -0.013(2)
C1 0.028(3) 0.025(3) 0.031(3) -0.002(2) 0.000(2) 0.003(2)
C2 0.037(3) 0.016(2) 0.025(2) -0.0017(19) 0.001(2) 0.001(2)
C3 0.030(3) 0.021(3) 0.024(2) 0.0034(19) 0.002(2) -0.004(2)
C4 0.020(2) 0.028(3) 0.034(3) -0.002(2) -0.002(2) 0.000(2)
C5 0.039(3) 0.023(3) 0.051(3) -0.004(2) -0.009(3) 0.005(2)
C6 0.037(3) 0.026(3) 0.052(3) 0.007(2) -0.007(3) -0.003(2)
C7 0.031(3) 0.022(3) 0.029(3) -0.003(2) -0.001(2) 0.001(2)
C8 0.040(3) 0.022(3) 0.024(2) 0.000(2) 0.009(2) 0.004(2)
C9 0.038(3) 0.021(3) 0.035(3) -0.002(2) 0.015(2) -0.003(2)
C10 0.032(3) 0.032(3) 0.031(3) -0.002(2) 0.009(2) -0.010(2)
C11 0.070(4) 0.041(3) 0.026(3) 0.000(2) 0.009(3) -0.002(3)
C12 0.056(4) 0.040(3) 0.046(3) 0.000(3) 0.024(3) -0.015(3)
C13 0.034(3) 0.021(3) 0.027(2) 0.001(2) 0.008(2) -0.006(2)
C14 0.025(3) 0.025(3) 0.028(2) -0.003(2) 0.001(2) 0.000(2)
C15 0.026(3) 0.023(3) 0.023(2) -0.002(2) -0.001(2) -0.002(2)
C16 0.025(3) 0.030(3) 0.027(2) 0.002(2) 0.006(2) -0.001(2)
C17 0.043(3) 0.022(3) 0.035(3) -0.003(2) 0.003(2) -0.004(2)
C18 0.035(3) 0.029(3) 0.031(3) -0.003(2) 0.004(2) 0.000(2)
C19 0.035(3) 0.018(3) 0.027(2) -0.0035(19) -0.002(2) 0.003(2)
C20 0.022(2) 0.025(3) 0.028(2) 0.000(2) -0.0025(19) -0.0021(19)
C21 0.022(2) 0.025(3) 0.031(3) 0.004(2) 0.001(2) 0.002(2)
C22 0.018(2) 0.031(3) 0.032(3) -0.004(2) 0.003(2) 0.001(2)
C23 0.037(3) 0.032(3) 0.034(3) 0.004(2) 0.006(2) 0.007(2)
C24 0.047(3) 0.035(3) 0.043(3) -0.003(2) -0.003(3) 0.015(3)
C25 0.019(2) 0.026(3) 0.041(3) -0.003(2) -0.005(2) -0.0053(19)
C26 0.031(3) 0.036(3) 0.043(3) 0.002(2) 0.003(2) -0.009(2)
C27 0.035(3) 0.030(3) 0.037(3) 0.000(2) -0.002(2) 0.002(2)
#==============================================================================
# MOLECULAR GEOMETRY
_geom_special_details
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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
Mo1 C26 1.942(5) . ?
Mo1 C27 1.949(5) . ?
Mo1 C25 1.960(5) . ?
Mo1 P2 2.4557(12) . ?
Mo1 P1 2.4690(12) . ?
Mo1 P3 2.4970(12) . ?
P1 N1 1.674(3) . ?
P1 N2 1.719(4) . ?
P1 C1 1.814(4) . ?
P1 P2 2.6644(16) . ?
P2 N2 1.681(3) . ?
P2 N3 1.709(3) . ?
P2 C7 1.814(4) . ?
P2 P3 2.6385(16) . ?
P3 N4 1.681(3) . ?
P3 N3 1.703(3) . ?
P3 C13 1.820(4) . ?
P4 N4 1.727(3) . ?
P4 N1 1.749(4) . ?
P4 C19 1.850(4) . ?
N1 C4 1.477(5) . ?
N2 C10 1.462(5) . ?
N3 C16 1.462(5) . ?
N4 C22 1.490(5) . ?
O1 C25 1.165(5) . ?
O2 C26 1.174(6) . ?
O3 C27 1.163(5) . ?
C1 C2 1.507(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.333(6) . ?
C2 C5 1.504(6) . ?
C3 C6 1.492(6) . ?
C3 C4 1.512(6) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.502(6) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.334(6) . ?
C8 C11 1.512(6) . ?
C9 C12 1.513(6) . ?
C9 C10 1.515(6) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.520(6) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.334(6) . ?
C14 C17 1.506(6) . ?
C15 C18 1.502(6) . ?
C15 C16 1.521(6) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.516(6) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.329(6) . ?
C20 C23 1.507(6) . ?
C21 C24 1.500(6) . ?
C21 C22 1.515(6) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
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
C26 Mo1 C27 89.2(2) . . ?
C26 Mo1 C25 92.0(2) . . ?
C27 Mo1 C25 95.81(19) . . ?
C26 Mo1 P2 102.62(15) . . ?
C27 Mo1 P2 98.61(15) . . ?
C25 Mo1 P2 159.49(13) . . ?
C26 Mo1 P1 90.34(14) . . ?
C27 Mo1 P1 163.59(15) . . ?
C25 Mo1 P1 100.59(13) . . ?
P2 Mo1 P1 65.51(4) . . ?
C26 Mo1 P3 166.95(15) . . ?
C27 Mo1 P3 91.67(14) . . ?
C25 Mo1 P3 100.81(13) . . ?
P2 Mo1 P3 64.37(4) . . ?
P1 Mo1 P3 85.14(4) . . ?
N1 P1 N2 109.98(18) . . ?
N1 P1 C1 100.88(19) . . ?
N2 P1 C1 104.64(19) . . ?
N1 P1 Mo1 119.18(13) . . ?
N2 P1 Mo1 94.73(12) . . ?
C1 P1 Mo1 125.85(15) . . ?
N1 P1 P2 122.89(13) . . ?
N2 P1 P2 37.89(11) . . ?
C1 P1 P2 127.81(15) . . ?
Mo1 P1 P2 57.01(4) . . ?
N2 P2 N3 111.21(17) . . ?
N2 P2 C7 100.49(19) . . ?
N3 P2 C7 106.82(19) . . ?
N2 P2 Mo1 96.22(13) . . ?
N3 P2 Mo1 96.20(12) . . ?
C7 P2 Mo1 144.07(15) . . ?
N2 P2 P3 102.16(13) . . ?
N3 P2 P3 39.26(12) . . ?
C7 P2 P3 144.75(15) . . ?
Mo1 P2 P3 58.57(4) . . ?
N2 P2 P1 38.91(12) . . ?
N3 P2 P1 108.78(13) . . ?
C7 P2 P1 133.88(15) . . ?
Mo1 P2 P1 57.49(4) . . ?
P3 P2 P1 78.62(5) . . ?
N4 P3 N3 108.64(18) . . ?
N4 P3 C13 104.93(19) . . ?
N3 P3 C13 98.37(19) . . ?
N4 P3 Mo1 115.26(13) . . ?
N3 P3 Mo1 94.87(12) . . ?
C13 P3 Mo1 130.66(15) . . ?
N4 P3 P2 112.55(13) . . ?
N3 P3 P2 39.42(12) . . ?
C13 P3 P2 130.16(15) . . ?
Mo1 P3 P2 57.05(4) . . ?
N4 P4 N1 106.66(17) . . ?
N4 P4 C19 95.75(18) . . ?
N1 P4 C19 100.55(18) . . ?
C4 N1 P1 121.0(3) . . ?
C4 N1 P4 125.1(3) . . ?
P1 N1 P4 112.77(19) . . ?
C10 N2 P2 125.0(3) . . ?
C10 N2 P1 130.1(3) . . ?
P2 N2 P1 103.20(19) . . ?
C16 N3 P3 123.3(3) . . ?
C16 N3 P2 133.0(3) . . ?
P3 N3 P2 101.32(18) . . ?
C22 N4 P3 124.4(3) . . ?
C22 N4 P4 119.9(3) . . ?
P3 N4 P4 115.65(19) . . ?
C2 C1 P1 115.7(3) . . ?
C2 C1 H1A 108.4 . . ?
P1 C1 H1A 108.4 . . ?
C2 C1 H1B 108.3 . . ?
P1 C1 H1B 108.4 . . ?
H1A C1 H1B 107.4 . . ?
C3 C2 C5 122.9(4) . . ?
C3 C2 C1 123.7(4) . . ?
C5 C2 C1 113.4(4) . . ?
C2 C3 C6 123.8(4) . . ?
C2 C3 C4 125.3(4) . . ?
C6 C3 C4 110.9(4) . . ?
N1 C4 C3 117.1(4) . . ?
N1 C4 H4A 108.0 . . ?
C3 C4 H4A 108.0 . . ?
N1 C4 H4B 108.0 . . ?
C3 C4 H4B 108.0 . . ?
H4A C4 H4B 107.3 . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 P2 118.4(3) . . ?
C8 C7 H7A 107.7 . . ?
P2 C7 H7A 107.7 . . ?
C8 C7 H7B 107.7 . . ?
P2 C7 H7B 107.7 . . ?
H7A C7 H7B 107.1 . . ?
C9 C8 C7 124.8(4) . . ?
C9 C8 C11 122.5(4) . . ?
C7 C8 C11 112.6(4) . . ?
C8 C9 C12 122.4(4) . . ?
C8 C9 C10 125.8(4) . . ?
C12 C9 C10 111.8(4) . . ?
N2 C10 C9 113.2(4) . . ?
N2 C10 H10A 108.9 . . ?
C9 C10 H10A 108.9 . . ?
N2 C10 H10B 108.9 . . ?
C9 C10 H10B 108.9 . . ?
H10A C10 H10B 107.8 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 P3 117.3(3) . . ?
C14 C13 H13A 108.0 . . ?
P3 C13 H13A 108.0 . . ?
C14 C13 H13B 108.0 . . ?
P3 C13 H13B 108.0 . . ?
H13A C13 H13B 107.2 . . ?
C15 C14 C17 123.6(4) . . ?
C15 C14 C13 125.4(4) . . ?
C17 C14 C13 110.9(4) . . ?
C14 C15 C18 123.7(4) . . ?
C14 C15 C16 124.3(4) . . ?
C18 C15 C16 111.9(4) . . ?
N3 C16 C15 114.3(3) . . ?
N3 C16 H16A 108.7 . . ?
C15 C16 H16A 108.7 . . ?
N3 C16 H16B 108.7 . . ?
C15 C16 H16B 108.7 . . ?
H16A C16 H16B 107.6 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 P4 111.7(3) . . ?
C20 C19 H19A 109.3 . . ?
P4 C19 H19A 109.3 . . ?
C20 C19 H19B 109.3 . . ?
P4 C19 H19B 109.3 . . ?
H19A C19 H19B 107.9 . . ?
C21 C20 C23 126.0(4) . . ?
C21 C20 C19 116.8(4) . . ?
C23 C20 C19 117.0(4) . . ?
C20 C21 C24 126.5(4) . . ?
C20 C21 C22 117.4(4) . . ?
C24 C21 C22 116.0(4) . . ?
N4 C22 C21 112.0(4) . . ?
N4 C22 H22A 109.2 . . ?
C21 C22 H22A 109.2 . . ?
N4 C22 H22B 109.2 . . ?
C21 C22 H22B 109.2 . . ?
H22A C22 H22B 107.9 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O1 C25 Mo1 179.1(4) . . ?
O2 C26 Mo1 179.2(5) . . ?
O3 C27 Mo1 177.4(4) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C26 Mo1 P1 N1 144.0(2) . . . . ?
C27 Mo1 P1 N1 -127.6(5) . . . . ?
C25 Mo1 P1 N1 51.8(2) . . . . ?
P2 Mo1 P1 N1 -112.27(16) . . . . ?
P3 Mo1 P1 N1 -48.26(15) . . . . ?
C26 Mo1 P1 N2 -99.97(19) . . . . ?
C27 Mo1 P1 N2 -11.5(5) . . . . ?
C25 Mo1 P1 N2 167.88(18) . . . . ?
P2 Mo1 P1 N2 3.76(12) . . . . ?
P3 Mo1 P1 N2 67.77(12) . . . . ?
C26 Mo1 P1 C1 11.9(2) . . . . ?
C27 Mo1 P1 C1 100.3(5) . . . . ?
C25 Mo1 P1 C1 -80.2(2) . . . . ?
P2 Mo1 P1 C1 115.63(19) . . . . ?
P3 Mo1 P1 C1 179.64(19) . . . . ?
C26 Mo1 P1 P2 -103.73(15) . . . . ?
C27 Mo1 P1 P2 -15.3(5) . . . . ?
C25 Mo1 P1 P2 164.12(14) . . . . ?
P3 Mo1 P1 P2 64.01(4) . . . . ?
C26 Mo1 P2 N2 80.68(19) . . . . ?
C27 Mo1 P2 N2 171.82(19) . . . . ?
C25 Mo1 P2 N2 -54.0(4) . . . . ?
P1 Mo1 P2 N2 -3.85(12) . . . . ?
P3 Mo1 P2 N2 -100.47(13) . . . . ?
C26 Mo1 P2 N3 -167.12(19) . . . . ?
C27 Mo1 P2 N3 -75.97(19) . . . . ?
C25 Mo1 P2 N3 58.2(4) . . . . ?
P1 Mo1 P2 N3 108.35(13) . . . . ?
P3 Mo1 P2 N3 11.73(12) . . . . ?
C26 Mo1 P2 C7 -36.9(3) . . . . ?
C27 Mo1 P2 C7 54.3(3) . . . . ?
C25 Mo1 P2 C7 -171.5(4) . . . . ?
P1 Mo1 P2 C7 -121.4(3) . . . . ?
P3 Mo1 P2 C7 142.0(3) . . . . ?
C26 Mo1 P2 P3 -178.85(15) . . . . ?
C27 Mo1 P2 P3 -87.71(14) . . . . ?
C25 Mo1 P2 P3 46.5(4) . . . . ?
P1 Mo1 P2 P3 96.62(4) . . . . ?
C26 Mo1 P2 P1 84.53(15) . . . . ?
C27 Mo1 P2 P1 175.68(14) . . . . ?
C25 Mo1 P2 P1 -50.1(4) . . . . ?
P3 Mo1 P2 P1 -96.62(4) . . . . ?
N1 P1 P2 N2 -80.3(2) . . . . ?
C1 P1 P2 N2 61.6(3) . . . . ?
Mo1 P1 P2 N2 173.9(2) . . . . ?
N1 P1 P2 N3 20.5(2) . . . . ?
N2 P1 P2 N3 100.8(2) . . . . ?
C1 P1 P2 N3 162.3(2) . . . . ?
Mo1 P1 P2 N3 -85.32(13) . . . . ?
N1 P1 P2 C7 -118.2(3) . . . . ?
N2 P1 P2 C7 -37.9(3) . . . . ?
C1 P1 P2 C7 23.7(3) . . . . ?
Mo1 P1 P2 C7 136.0(2) . . . . ?
N1 P1 P2 Mo1 105.81(16) . . . . ?
N2 P1 P2 Mo1 -173.9(2) . . . . ?
C1 P1 P2 Mo1 -112.3(2) . . . . ?
N1 P1 P2 P3 45.97(16) . . . . ?
N2 P1 P2 P3 126.3(2) . . . . ?
C1 P1 P2 P3 -172.2(2) . . . . ?
Mo1 P1 P2 P3 -59.84(4) . . . . ?
C26 Mo1 P3 N4 106.5(6) . . . . ?
C27 Mo1 P3 N4 -159.7(2) . . . . ?
C25 Mo1 P3 N4 -63.49(19) . . . . ?
P2 Mo1 P3 N4 101.52(14) . . . . ?
P1 Mo1 P3 N4 36.39(14) . . . . ?
C26 Mo1 P3 N3 -6.8(6) . . . . ?
C27 Mo1 P3 N3 87.01(19) . . . . ?
C25 Mo1 P3 N3 -176.75(17) . . . . ?
P2 Mo1 P3 N3 -11.75(12) . . . . ?
P1 Mo1 P3 N3 -76.87(12) . . . . ?
C26 Mo1 P3 C13 -112.2(7) . . . . ?
C27 Mo1 P3 C13 -18.4(2) . . . . ?
C25 Mo1 P3 C13 77.8(2) . . . . ?
P2 Mo1 P3 C13 -117.2(2) . . . . ?
P1 Mo1 P3 C13 177.72(19) . . . . ?
C26 Mo1 P3 P2 5.0(6) . . . . ?
C27 Mo1 P3 P2 98.75(15) . . . . ?
C25 Mo1 P3 P2 -165.00(13) . . . . ?
P1 Mo1 P3 P2 -65.12(4) . . . . ?
N2 P2 P3 N4 -16.44(19) . . . . ?
N3 P2 P3 N4 92.3(2) . . . . ?
C7 P2 P3 N4 112.4(3) . . . . ?
Mo1 P2 P3 N4 -106.34(14) . . . . ?
P1 P2 P3 N4 -47.64(14) . . . . ?
N2 P2 P3 N3 -108.7(2) . . . . ?
C7 P2 P3 N3 20.2(3) . . . . ?
Mo1 P2 P3 N3 161.37(19) . . . . ?
P1 P2 P3 N3 -139.93(19) . . . . ?
N2 P2 P3 C13 -152.1(2) . . . . ?
N3 P2 P3 C13 -43.4(3) . . . . ?
C7 P2 P3 C13 -23.3(3) . . . . ?
Mo1 P2 P3 C13 118.0(2) . . . . ?
P1 P2 P3 C13 176.7(2) . . . . ?
N2 P2 P3 Mo1 89.90(13) . . . . ?
N3 P2 P3 Mo1 -161.37(19) . . . . ?
C7 P2 P3 Mo1 -141.2(3) . . . . ?
P1 P2 P3 Mo1 58.70(3) . . . . ?
N2 P1 N1 C4 65.8(4) . . . . ?
C1 P1 N1 C4 -44.3(4) . . . . ?
Mo1 P1 N1 C4 173.4(3) . . . . ?
P2 P1 N1 C4 105.9(3) . . . . ?
N2 P1 N1 P4 -102.5(2) . . . . ?
C1 P1 N1 P4 147.4(2) . . . . ?
Mo1 P1 N1 P4 5.2(3) . . . . ?
P2 P1 N1 P4 -62.4(2) . . . . ?
N4 P4 N1 C4 -102.1(4) . . . . ?
C19 P4 N1 C4 -2.7(4) . . . . ?
N4 P4 N1 P1 65.6(2) . . . . ?
C19 P4 N1 P1 164.9(2) . . . . ?
N3 P2 N2 C10 72.5(4) . . . . ?
C7 P2 N2 C10 -40.3(4) . . . . ?
Mo1 P2 N2 C10 171.6(3) . . . . ?
P3 P2 N2 C10 112.5(3) . . . . ?
P1 P2 N2 C10 166.4(5) . . . . ?
N3 P2 N2 P1 -94.0(2) . . . . ?
C7 P2 N2 P1 153.2(2) . . . . ?
Mo1 P2 N2 P1 5.18(17) . . . . ?
P3 P2 N2 P1 -53.96(17) . . . . ?
N1 P1 N2 C10 -47.2(4) . . . . ?
C1 P1 N2 C10 60.4(4) . . . . ?
Mo1 P1 N2 C10 -170.6(4) . . . . ?
P2 P1 N2 C10 -165.5(5) . . . . ?
N1 P1 N2 P2 118.28(19) . . . . ?
C1 P1 N2 P2 -134.1(2) . . . . ?
Mo1 P1 N2 P2 -5.14(16) . . . . ?
N4 P3 N3 C16 61.4(4) . . . . ?
C13 P3 N3 C16 -47.6(4) . . . . ?
Mo1 P3 N3 C16 -179.9(3) . . . . ?
P2 P3 N3 C16 164.5(4) . . . . ?
N4 P3 N3 P2 -103.12(19) . . . . ?
C13 P3 N3 P2 147.9(2) . . . . ?
Mo1 P3 N3 P2 15.61(16) . . . . ?
N2 P2 N3 C16 -79.0(4) . . . . ?
C7 P2 N3 C16 29.7(4) . . . . ?
Mo1 P2 N3 C16 -178.2(4) . . . . ?
P3 P2 N3 C16 -162.2(5) . . . . ?
P1 P2 N3 C16 -120.4(4) . . . . ?
N2 P2 N3 P3 83.2(2) . . . . ?
C7 P2 N3 P3 -168.01(18) . . . . ?
Mo1 P2 N3 P3 -15.91(16) . . . . ?
P1 P2 N3 P3 41.80(18) . . . . ?
N3 P3 N4 C22 -61.0(4) . . . . ?
C13 P3 N4 C22 43.4(4) . . . . ?
Mo1 P3 N4 C22 -166.0(3) . . . . ?
P2 P3 N4 C22 -103.0(3) . . . . ?
N3 P3 N4 P4 120.5(2) . . . . ?
C13 P3 N4 P4 -135.1(2) . . . . ?
Mo1 P3 N4 P4 15.5(2) . . . . ?
P2 P3 N4 P4 78.4(2) . . . . ?
N1 P4 N4 C22 101.7(3) . . . . ?
C19 P4 N4 C22 -1.1(3) . . . . ?
N1 P4 N4 P3 -79.7(2) . . . . ?
C19 P4 N4 P3 177.5(2) . . . . ?
N1 P1 C1 C2 38.2(4) . . . . ?
N2 P1 C1 C2 -76.0(3) . . . . ?
Mo1 P1 C1 C2 176.9(2) . . . . ?
P2 P1 C1 C2 -109.9(3) . . . . ?
P1 C1 C2 C3 -21.3(6) . . . . ?
P1 C1 C2 C5 160.4(3) . . . . ?
C5 C2 C3 C6 -0.1(7) . . . . ?
C1 C2 C3 C6 -178.3(4) . . . . ?
C5 C2 C3 C4 179.4(4) . . . . ?
C1 C2 C3 C4 1.2(7) . . . . ?
P1 N1 C4 C3 31.2(5) . . . . ?
P4 N1 C4 C3 -162.1(3) . . . . ?
C2 C3 C4 N1 -4.5(6) . . . . ?
C6 C3 C4 N1 175.1(4) . . . . ?
N2 P2 C7 C8 18.5(4) . . . . ?
N3 P2 C7 C8 -97.7(4) . . . . ?
Mo1 P2 C7 C8 134.8(3) . . . . ?
P3 P2 C7 C8 -110.8(3) . . . . ?
P1 P2 C7 C8 41.6(4) . . . . ?
P2 C7 C8 C9 0.4(6) . . . . ?
P2 C7 C8 C11 -177.3(3) . . . . ?
C7 C8 C9 C12 176.0(4) . . . . ?
C11 C8 C9 C12 -6.6(7) . . . . ?
C7 C8 C9 C10 -5.6(8) . . . . ?
C11 C8 C9 C10 171.8(5) . . . . ?
P2 N2 C10 C9 40.1(5) . . . . ?
P1 N2 C10 C9 -157.3(3) . . . . ?
C8 C9 C10 N2 -13.0(7) . . . . ?
C12 C9 C10 N2 165.6(4) . . . . ?
N4 P3 C13 C14 -81.4(4) . . . . ?
N3 P3 C13 C14 30.5(4) . . . . ?
Mo1 P3 C13 C14 134.4(3) . . . . ?
P2 P3 C13 C14 56.7(4) . . . . ?
P3 C13 C14 C15 -12.5(6) . . . . ?
P3 C13 C14 C17 167.5(3) . . . . ?
C17 C14 C15 C18 -1.1(7) . . . . ?
C13 C14 C15 C18 178.8(4) . . . . ?
C17 C14 C15 C16 -180.0(4) . . . . ?
C13 C14 C15 C16 0.0(7) . . . . ?
P3 N3 C16 C15 42.0(5) . . . . ?
P2 N3 C16 C15 -159.0(3) . . . . ?
C14 C15 C16 N3 -12.7(6) . . . . ?
C18 C15 C16 N3 168.3(4) . . . . ?
N4 P4 C19 C20 -49.8(3) . . . . ?
N1 P4 C19 C20 -158.0(3) . . . . ?
P4 C19 C20 C21 57.7(5) . . . . ?
P4 C19 C20 C23 -126.5(4) . . . . ?
C23 C20 C21 C24 -2.6(8) . . . . ?
C19 C20 C21 C24 172.8(4) . . . . ?
C23 C20 C21 C22 -179.3(4) . . . . ?
C19 C20 C21 C22 -3.9(6) . . . . ?
P3 N4 C22 C21 -128.5(3) . . . . ?
P4 N4 C22 C21 49.9(5) . . . . ?
C20 C21 C22 N4 -51.8(5) . . . . ?
C24 C21 C22 N4 131.1(4) . . . . ?
C26 Mo1 C25 O1 -114(28) . . . . ?
C27 Mo1 C25 O1 156(28) . . . . ?
P2 Mo1 C25 O1 22(29) . . . . ?
P1 Mo1 C25 O1 -24(28) . . . . ?
P3 Mo1 C25 O1 63(28) . . . . ?
C27 Mo1 C26 O2 45(35) . . . . ?
C25 Mo1 C26 O2 -51(35) . . . . ?
P2 Mo1 C26 O2 144(35) . . . . ?
P1 Mo1 C26 O2 -151(35) . . . . ?
P3 Mo1 C26 O2 139(35) . . . . ?
C26 Mo1 C27 O3 28(10) . . . . ?
C25 Mo1 C27 O3 120(10) . . . . ?
P2 Mo1 C27 O3 -75(10) . . . . ?
P1 Mo1 C27 O3 -61(10) . . . . ?
P3 Mo1 C27 O3 -139(10) . . . . ?
_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full 28.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max 0.783
_refine_diff_density_min -1.001
_refine_diff_density_rms 0.138
_database_code_depnum_ccdc_archive 'CCDC 956163'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_is_ch169_[PN(C6H10)]4W2(CO)7
_audit_creation_method SHELXL-97
#==============================================================================
# CHEMICAL DATA
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C31 H40 N4 O7 P4 W2'
_chemical_formula_sum 'C31 H40 N4 O7 P4 W2'
_chemical_formula_weight 1072.25
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
#==============================================================================
# CRYSTAL DATA
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/c'
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_Int_Tables_number 14
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 20.4707(8)
_cell_length_b 20.2868(7)
_cell_length_c 18.9919(6)
_cell_angle_alpha 90.00
_cell_angle_beta 110.519(2)
_cell_angle_gamma 90.00
_cell_volume 7386.7(5)
_cell_formula_units_Z 8
_cell_measurement_temperature 173(2)
_cell_measurement_reflns_used 9920
_cell_measurement_theta_min 4.529
_cell_measurement_theta_max 56.933
_exptl_crystal_description block
_exptl_crystal_colour yellow
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.06
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.928
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 4144
_exptl_absorpt_coefficient_mu 6.447
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.4447
_exptl_absorpt_correction_T_max 0.6983
_exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)'
#==============================================================================
# EXPERIMENTAL DATA
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 173(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker Apex Kappa II-CCD-diffractometer'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 132908
_diffrn_reflns_av_R_equivalents 0.0954
_diffrn_reflns_av_sigmaI/netI 0.1022
_diffrn_reflns_limit_h_min -30
_diffrn_reflns_limit_h_max 30
_diffrn_reflns_limit_k_min -29
_diffrn_reflns_limit_k_max 30
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_theta_min 1.06
_diffrn_reflns_theta_max 32.50
_reflns_number_total 26725
_reflns_number_gt 15113
_reflns_threshold_expression >2\s(I)
_computing_data_collection 'Bruker Apex V7.51A'
_computing_cell_refinement 'Bruker Apex V7.51A'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material SHELXL-97
#==============================================================================
# REFINEMENT DATA
_refine_special_details
;
All H atoms
were positioned geometrically and refined using a riding model, with C---H =
0.98 (methyl groups), 0.99\%A (methylene groups), 1.00\%A (methine groups) or
0.95 \%A (aryl CH) and with U~iso~(H) = 1.5 times U~eq~(C)
(methyl groups) or with U~iso~(H) = 1.2 times U~eq~(C)
(methylene groups, aryl CH, methine groups). Torsion angles of all methyl
groups were allowed to refine.
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0264P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 26725
_refine_ls_number_parameters 881
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1160
_refine_ls_R_factor_gt 0.0475
_refine_ls_wR_factor_ref 0.1003
_refine_ls_wR_factor_gt 0.0798
_refine_ls_goodness_of_fit_ref 1.013
_refine_ls_restrained_S_all 1.013
_refine_ls_shift/su_max 0.024
_refine_ls_shift/su_mean 0.000
#==============================================================================
# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_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
W1 W 0.545712(12) 0.915388(11) 0.256814(11) 0.02370(6) Uani 1 1 d . . .
W2 W 0.445059(11) 0.796186(10) 0.227686(11) 0.02080(5) Uani 1 1 d . . .
P1 P 0.42312(8) 0.71024(7) 0.30589(7) 0.0238(3) Uani 1 1 d . . .
P2 P 0.41899(7) 0.83493(7) 0.33896(7) 0.0213(3) Uani 1 1 d . . .
P3 P 0.56318(7) 0.86806(7) 0.38118(7) 0.0209(3) Uani 1 1 d . . .
P4 P 0.55100(8) 0.73999(7) 0.32027(7) 0.0228(3) Uani 1 1 d . . .
N1 N 0.3970(2) 0.7593(2) 0.3618(2) 0.0225(10) Uani 1 1 d . . .
N2 N 0.4896(2) 0.8673(2) 0.4058(2) 0.0204(9) Uani 1 1 d . . .
N3 N 0.5957(2) 0.7900(2) 0.3925(2) 0.0230(10) Uani 1 1 d . . .
N4 N 0.5047(2) 0.6839(2) 0.3495(2) 0.0242(10) Uani 1 1 d . . .
O1 O 0.6658(2) 0.8249(2) 0.2423(2) 0.0463(12) Uani 1 1 d . . .
O2 O 0.6680(2) 1.01356(19) 0.3263(2) 0.0403(11) Uani 1 1 d . . .
O3 O 0.5161(2) 0.9551(3) 0.0877(2) 0.0598(14) Uani 1 1 d . . .
O4 O 0.4483(3) 1.0264(2) 0.2850(3) 0.0577(14) Uani 1 1 d . . .
O5 O 0.5113(2) 0.7539(2) 0.1084(2) 0.0529(13) Uani 1 1 d . . .
O6 O 0.3013(3) 0.7455(3) 0.1190(3) 0.0709(17) Uani 1 1 d . . .
O7 O 0.3679(2) 0.9261(2) 0.1527(2) 0.0462(12) Uani 1 1 d . . .
C1 C 0.3664(3) 0.6406(3) 0.2930(3) 0.0377(16) Uani 1 1 d . . .
H1A H 0.3223 0.6501 0.2513 0.045 Uiso 1 1 calc R . .
H1B H 0.3884 0.6022 0.2780 0.045 Uiso 1 1 calc R . .
C2 C 0.3498(3) 0.6226(3) 0.3621(3) 0.0286(13) Uani 1 1 d . . .
C3 C 0.3558(3) 0.6639(3) 0.4185(3) 0.0302(13) Uani 1 1 d . . .
C4 C 0.3762(3) 0.7350(3) 0.4241(3) 0.0340(14) Uani 1 1 d . . .
H4A H 0.3364 0.7618 0.4260 0.041 Uiso 1 1 calc R . .
H4B H 0.4155 0.7420 0.4719 0.041 Uiso 1 1 calc R . .
C5 C 0.3260(3) 0.5523(3) 0.3594(3) 0.0416(16) Uani 1 1 d . . .
H5A H 0.3650 0.5227 0.3638 0.062 Uiso 1 1 calc R . .
H5B H 0.2881 0.5442 0.3116 0.062 Uiso 1 1 calc R . .
H5C H 0.3093 0.5442 0.4011 0.062 Uiso 1 1 calc R . .
C6 C 0.3403(4) 0.6436(3) 0.4880(3) 0.0464(18) Uani 1 1 d . . .
H6A H 0.3116 0.6036 0.4771 0.070 Uiso 1 1 calc R . .
H6B H 0.3151 0.6791 0.5024 0.070 Uiso 1 1 calc R . .
H6C H 0.3842 0.6349 0.5294 0.070 Uiso 1 1 calc R . .
C7 C 0.3533(3) 0.8891(3) 0.3496(3) 0.0306(13) Uani 1 1 d . . .
H7A H 0.3571 0.9327 0.3278 0.037 Uiso 1 1 calc R . .
H7B H 0.3066 0.8709 0.3210 0.037 Uiso 1 1 calc R . .
C8 C 0.3595(3) 0.8983(3) 0.4311(3) 0.0332(14) Uani 1 1 d . . .
C9 C 0.4193(3) 0.8932(3) 0.4879(3) 0.0295(13) Uani 1 1 d . . .
C10 C 0.4891(3) 0.8801(3) 0.4816(3) 0.0304(13) Uani 1 1 d . . .
H10A H 0.5196 0.9185 0.5024 0.036 Uiso 1 1 calc R . .
H10B H 0.5102 0.8416 0.5136 0.036 Uiso 1 1 calc R . .
C11 C 0.2918(4) 0.9110(4) 0.4417(4) 0.056(2) Uani 1 1 d . . .
H11A H 0.2664 0.8694 0.4375 0.084 Uiso 1 1 calc R . .
H11B H 0.2639 0.9417 0.4030 0.084 Uiso 1 1 calc R . .
H11C H 0.3006 0.9302 0.4916 0.084 Uiso 1 1 calc R . .
C12 C 0.4244(3) 0.8992(3) 0.5690(3) 0.0436(17) Uani 1 1 d . . .
H12A H 0.4009 0.9396 0.5755 0.065 Uiso 1 1 calc R . .
H12B H 0.4736 0.9009 0.6015 0.065 Uiso 1 1 calc R . .
H12C H 0.4021 0.8610 0.5826 0.065 Uiso 1 1 calc R . .
C13 C 0.6292(3) 0.9048(2) 0.4634(3) 0.0242(12) Uani 1 1 d . . .
H13A H 0.6713 0.9136 0.4507 0.029 Uiso 1 1 calc R . .
H13B H 0.6114 0.9479 0.4733 0.029 Uiso 1 1 calc R . .
C14 C 0.6509(3) 0.8651(3) 0.5353(3) 0.0272(13) Uani 1 1 d . . .
C15 C 0.6612(3) 0.8009(3) 0.5323(3) 0.0306(13) Uani 1 1 d . . .
C16 C 0.6542(4) 0.7675(3) 0.4589(3) 0.0472(18) Uani 1 1 d . . .
H16A H 0.6981 0.7743 0.4490 0.057 Uiso 1 1 calc R . .
H16B H 0.6491 0.7195 0.4649 0.057 Uiso 1 1 calc R . .
C17 C 0.6622(4) 0.9027(3) 0.6071(3) 0.0485(19) Uani 1 1 d . . .
H17A H 0.6221 0.9316 0.6007 0.073 Uiso 1 1 calc R . .
H17B H 0.7046 0.9294 0.6192 0.073 Uiso 1 1 calc R . .
H17C H 0.6672 0.8716 0.6482 0.073 Uiso 1 1 calc R . .
C18 C 0.6845(4) 0.7557(3) 0.5990(3) 0.056(2) Uani 1 1 d . . .
H18A H 0.7273 0.7330 0.6008 0.084 Uiso 1 1 calc R . .
H18B H 0.6479 0.7231 0.5946 0.084 Uiso 1 1 calc R . .
H18C H 0.6934 0.7814 0.6451 0.084 Uiso 1 1 calc R . .
C19 C 0.6134(3) 0.6840(3) 0.3044(3) 0.0318(13) Uani 1 1 d . . .
H19A H 0.5930 0.6661 0.2528 0.038 Uiso 1 1 calc R . .
H19B H 0.6556 0.7093 0.3074 0.038 Uiso 1 1 calc R . .
C20 C 0.6351(3) 0.6269(3) 0.3587(3) 0.0319(14) Uani 1 1 d . . .
C21 C 0.6027(3) 0.6060(3) 0.4043(3) 0.0358(14) Uani 1 1 d . . .
C22 C 0.5348(3) 0.6335(3) 0.4064(3) 0.0411(16) Uani 1 1 d . . .
H22A H 0.5010 0.5970 0.3989 0.049 Uiso 1 1 calc R . .
H22B H 0.5430 0.6527 0.4567 0.049 Uiso 1 1 calc R . .
C23 C 0.6987(3) 0.5920(3) 0.3537(4) 0.0458(17) Uani 1 1 d . . .
H23A H 0.7243 0.5711 0.4020 0.069 Uiso 1 1 calc R . .
H23B H 0.7290 0.6241 0.3416 0.069 Uiso 1 1 calc R . .
H23C H 0.6840 0.5584 0.3143 0.069 Uiso 1 1 calc R . .
C24 C 0.6303(4) 0.5519(3) 0.4611(3) 0.0480(18) Uani 1 1 d . . .
H24A H 0.6368 0.5118 0.4355 0.072 Uiso 1 1 calc R . .
H24B H 0.5969 0.5432 0.4865 0.072 Uiso 1 1 calc R . .
H24C H 0.6751 0.5654 0.4982 0.072 Uiso 1 1 calc R . .
C25 C 0.6199(3) 0.8545(3) 0.2464(3) 0.0307(14) Uani 1 1 d . . .
C26 C 0.6219(3) 0.9768(3) 0.2994(3) 0.0267(12) Uani 1 1 d . . .
C27 C 0.5270(3) 0.9423(3) 0.1506(3) 0.0396(16) Uani 1 1 d . . .
C28 C 0.4826(3) 0.9853(3) 0.2741(3) 0.0330(14) Uani 1 1 d . . .
C29 C 0.4858(3) 0.7691(3) 0.1517(3) 0.0346(14) Uani 1 1 d . . .
C30 C 0.3554(3) 0.7663(3) 0.1588(3) 0.0434(17) Uani 1 1 d . . .
C31 C 0.4062(3) 0.8829(3) 0.1821(3) 0.0353(15) Uani 1 1 d . . .
W3 W -0.054489(12) 0.596840(11) 0.252474(11) 0.02474(6) Uani 1 1 d . . .
W4 W 0.052669(12) 0.709007(10) 0.277091(11) 0.02170(5) Uani 1 1 d . . .
P5 P 0.06853(7) 0.66712(7) 0.15885(7) 0.0222(3) Uani 1 1 d . . .
P6 P 0.07826(8) 0.79103(7) 0.19802(8) 0.0264(3) Uani 1 1 d . . .
P7 P -0.04915(8) 0.77253(7) 0.19261(8) 0.0254(3) Uani 1 1 d . . .
P8 P -0.07419(7) 0.64420(7) 0.12777(7) 0.0215(3) Uani 1 1 d . . .
N5 N -0.0051(2) 0.6363(2) 0.0965(2) 0.0228(10) Uani 1 1 d . . .
N6 N 0.0909(2) 0.7420(2) 0.1334(2) 0.0251(10) Uani 1 1 d . . .
N7 N -0.0003(2) 0.8272(2) 0.1655(3) 0.0297(11) Uani 1 1 d . . .
N8 N -0.0972(2) 0.7256(2) 0.1180(2) 0.0238(10) Uani 1 1 d . . .
O8 O 0.0606(3) 0.5025(2) 0.2325(3) 0.0588(14) Uani 1 1 d . . .
O9 O -0.1570(3) 0.4836(2) 0.1758(3) 0.0663(16) Uani 1 1 d . . .
O10 O -0.0343(3) 0.5495(2) 0.4168(2) 0.0601(14) Uani 1 1 d . . .
O11 O -0.1879(2) 0.6749(2) 0.2528(2) 0.0493(12) Uani 1 1 d . . .
O12 O -0.0235(2) 0.7103(3) 0.3946(2) 0.0579(14) Uani 1 1 d . . .
O13 O 0.1754(3) 0.6091(3) 0.3502(3) 0.0665(16) Uani 1 1 d . . .
O14 O 0.1412(3) 0.8033(3) 0.4052(3) 0.087(2) Uani 1 1 d . . .
C32 C -0.0102(3) 0.6172(3) 0.0202(3) 0.0376(15) Uani 1 1 d . . .
H32A H -0.0292 0.6550 -0.0137 0.045 Uiso 1 1 calc R . .
H32B H -0.0442 0.5807 0.0034 0.045 Uiso 1 1 calc R . .
C33 C 0.0568(3) 0.5958(3) 0.0106(3) 0.0308(14) Uani 1 1 d . . .
C34 C 0.1197(3) 0.5958(3) 0.0639(3) 0.0312(14) Uani 1 1 d . . .
C35 C 0.1325(3) 0.6126(3) 0.1452(3) 0.0313(13) Uani 1 1 d . . .
H35A H 0.1791 0.6332 0.1671 0.038 Uiso 1 1 calc R . .
H35B H 0.1333 0.5711 0.1731 0.038 Uiso 1 1 calc R . .
C36 C 0.0421(3) 0.5778(3) -0.0709(3) 0.0496(19) Uani 1 1 d . . .
H36A H 0.0858 0.5652 -0.0777 0.074 Uiso 1 1 calc R . .
H36B H 0.0217 0.6158 -0.1029 0.074 Uiso 1 1 calc R . .
H36C H 0.0094 0.5407 -0.0849 0.074 Uiso 1 1 calc R . .
C37 C 0.1857(3) 0.5799(3) 0.0507(4) 0.0442(17) Uani 1 1 d . . .
H37A H 0.1747 0.5585 0.0017 0.066 Uiso 1 1 calc R . .
H37B H 0.2141 0.5502 0.0903 0.066 Uiso 1 1 calc R . .
H37C H 0.2118 0.6206 0.0516 0.066 Uiso 1 1 calc R . .
C38 C 0.1112(3) 0.7643(3) 0.0704(3) 0.0312(14) Uani 1 1 d . . .
H38A H 0.0696 0.7626 0.0238 0.037 Uiso 1 1 calc R . .
H38B H 0.1460 0.7331 0.0643 0.037 Uiso 1 1 calc R . .
C39 C 0.1411(3) 0.8325(3) 0.0789(3) 0.0283(13) Uani 1 1 d . . .
C40 C 0.1548(3) 0.8722(3) 0.1385(3) 0.0299(13) Uani 1 1 d . . .
C41 C 0.1432(3) 0.8533(3) 0.2105(3) 0.0391(16) Uani 1 1 d . . .
H41A H 0.1293 0.8931 0.2319 0.047 Uiso 1 1 calc R . .
H41B H 0.1878 0.8374 0.2473 0.047 Uiso 1 1 calc R . .
C42 C 0.1563(4) 0.8519(3) 0.0095(3) 0.0457(17) Uani 1 1 d . . .
H42A H 0.1126 0.8634 -0.0308 0.069 Uiso 1 1 calc R . .
H42B H 0.1784 0.8149 -0.0066 0.069 Uiso 1 1 calc R . .
H42C H 0.1878 0.8900 0.0209 0.069 Uiso 1 1 calc R . .
C43 C 0.1875(3) 0.9400(3) 0.1430(3) 0.0417(16) Uani 1 1 d . . .
H43A H 0.2065 0.9447 0.1026 0.063 Uiso 1 1 calc R . .
H43B H 0.2251 0.9451 0.1917 0.063 Uiso 1 1 calc R . .
H43C H 0.1519 0.9739 0.1376 0.063 Uiso 1 1 calc R . .
C44 C -0.0260(3) 0.8857(3) 0.1179(4) 0.0416(16) Uani 1 1 d . . .
H44A H -0.0283 0.8753 0.0662 0.050 Uiso 1 1 calc R . .
H44B H 0.0081 0.9219 0.1369 0.050 Uiso 1 1 calc R . .
C45 C -0.0966(4) 0.9097(3) 0.1148(4) 0.0416(16) Uani 1 1 d . . .
C46 C -0.1327(3) 0.8854(3) 0.1559(3) 0.0381(15) Uani 1 1 d . . .
C47 C -0.1092(3) 0.8284(3) 0.2115(3) 0.0353(14) Uani 1 1 d . . .
H47A H -0.1508 0.8033 0.2109 0.042 Uiso 1 1 calc R . .
H47B H -0.0869 0.8467 0.2627 0.042 Uiso 1 1 calc R . .
C48 C -0.1221(4) 0.9652(3) 0.0603(4) 0.059(2) Uani 1 1 d . . .
H48A H -0.1696 0.9558 0.0263 0.088 Uiso 1 1 calc R . .
H48B H -0.0913 0.9702 0.0311 0.088 Uiso 1 1 calc R . .
H48C H -0.1220 1.0061 0.0878 0.088 Uiso 1 1 calc R . .
C49 C -0.1997(3) 0.9162(3) 0.1545(4) 0.0540(19) Uani 1 1 d . . .
H49A H -0.1922 0.9388 0.2023 0.081 Uiso 1 1 calc R . .
H49B H -0.2352 0.8819 0.1471 0.081 Uiso 1 1 calc R . .
H49C H -0.2156 0.9481 0.1132 0.081 Uiso 1 1 calc R . .
C50 C -0.1478(3) 0.6117(3) 0.0498(3) 0.0272(12) Uani 1 1 d . . .
H50A H -0.1371 0.5656 0.0406 0.033 Uiso 1 1 calc R . .
H50B H -0.1891 0.6106 0.0655 0.033 Uiso 1 1 calc R . .
C51 C -0.1670(3) 0.6491(3) -0.0234(3) 0.0277(13) Uani 1 1 d . . .
C52 C -0.1609(3) 0.7136(3) -0.0238(3) 0.0334(14) Uani 1 1 d . . .
C53 C -0.1345(4) 0.7564(3) 0.0450(3) 0.055(2) Uani 1 1 d . . .
H53A H -0.1031 0.7898 0.0359 0.066 Uiso 1 1 calc R . .
H53B H -0.1749 0.7803 0.0495 0.066 Uiso 1 1 calc R . .
C54 C -0.1929(4) 0.6079(3) -0.0930(3) 0.0502(19) Uani 1 1 d . . .
H54A H -0.2146 0.6363 -0.1367 0.075 Uiso 1 1 calc R . .
H54B H -0.2273 0.5761 -0.0885 0.075 Uiso 1 1 calc R . .
H54C H -0.1537 0.5841 -0.0995 0.075 Uiso 1 1 calc R . .
C55 C -0.1807(3) 0.7547(3) -0.0948(3) 0.0481(18) Uani 1 1 d . . .
H55A H -0.1405 0.7809 -0.0946 0.072 Uiso 1 1 calc R . .
H55B H -0.2193 0.7841 -0.0970 0.072 Uiso 1 1 calc R . .
H55C H -0.1951 0.7255 -0.1387 0.072 Uiso 1 1 calc R . .
C56 C 0.0202(4) 0.5377(3) 0.2412(3) 0.0392(16) Uani 1 1 d . . .
C57 C -0.1183(3) 0.5264(3) 0.2062(3) 0.0377(15) Uani 1 1 d . . .
C58 C -0.0403(3) 0.5653(3) 0.3570(3) 0.0395(16) Uani 1 1 d . . .
C59 C -0.1372(3) 0.6490(3) 0.2544(3) 0.0333(14) Uani 1 1 d . . .
C60 C -0.0001(3) 0.6993(3) 0.3480(3) 0.0426(17) Uani 1 1 d . . .
C61 C 0.1304(4) 0.6463(3) 0.3246(3) 0.0448(18) Uani 1 1 d . . .
C62 C 0.1066(4) 0.7673(3) 0.3569(4) 0.060(2) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
W1 0.02516(14) 0.02347(11) 0.02043(10) 0.00459(8) 0.00542(9) -0.00516(10)
W2 0.02186(13) 0.02219(11) 0.01711(10) -0.00072(8) 0.00528(9) -0.00401(9)
P1 0.0273(9) 0.0228(7) 0.0218(7) -0.0040(5) 0.0093(6) -0.0079(6)
P2 0.0215(8) 0.0227(7) 0.0180(6) 0.0003(5) 0.0047(6) -0.0015(6)
P3 0.0207(8) 0.0201(7) 0.0197(6) 0.0012(5) 0.0044(6) -0.0038(6)
P4 0.0249(8) 0.0208(7) 0.0233(7) 0.0019(5) 0.0094(6) -0.0003(6)
N1 0.020(3) 0.027(2) 0.021(2) -0.0036(18) 0.0095(19) -0.007(2)
N2 0.019(3) 0.021(2) 0.021(2) -0.0019(17) 0.0074(18) -0.0028(18)
N3 0.021(3) 0.021(2) 0.025(2) 0.0006(18) 0.0062(19) -0.0027(19)
N4 0.031(3) 0.014(2) 0.032(2) 0.0011(18) 0.017(2) -0.001(2)
O1 0.049(3) 0.044(3) 0.051(3) -0.008(2) 0.024(2) 0.001(2)
O2 0.038(3) 0.030(2) 0.043(2) 0.0025(19) 0.001(2) -0.013(2)
O3 0.054(3) 0.091(4) 0.029(2) 0.024(2) 0.009(2) -0.006(3)
O4 0.061(4) 0.048(3) 0.052(3) -0.005(2) 0.004(3) 0.016(3)
O5 0.057(3) 0.072(4) 0.036(2) -0.014(2) 0.025(2) 0.002(3)
O6 0.052(4) 0.086(4) 0.052(3) 0.014(3) -0.010(3) -0.032(3)
O7 0.051(3) 0.043(3) 0.035(2) 0.006(2) 0.003(2) 0.012(2)
C1 0.052(4) 0.032(3) 0.032(3) -0.011(3) 0.018(3) -0.023(3)
C2 0.021(3) 0.032(3) 0.033(3) 0.004(2) 0.010(3) -0.007(3)
C3 0.029(3) 0.036(3) 0.029(3) 0.005(2) 0.013(3) -0.005(3)
C4 0.041(4) 0.040(4) 0.025(3) -0.006(2) 0.017(3) -0.012(3)
C5 0.054(5) 0.028(3) 0.052(4) 0.006(3) 0.030(4) -0.002(3)
C6 0.065(5) 0.044(4) 0.038(3) 0.005(3) 0.028(3) -0.010(4)
C7 0.019(3) 0.035(3) 0.032(3) -0.002(3) 0.002(2) -0.002(3)
C8 0.029(4) 0.034(3) 0.038(3) -0.004(3) 0.014(3) 0.007(3)
C9 0.031(4) 0.029(3) 0.029(3) -0.006(2) 0.012(3) 0.003(3)
C10 0.026(3) 0.041(4) 0.022(3) -0.004(2) 0.006(2) -0.002(3)
C11 0.041(5) 0.079(6) 0.056(4) 0.000(4) 0.027(4) 0.017(4)
C12 0.046(4) 0.051(4) 0.037(3) -0.008(3) 0.019(3) 0.010(3)
C13 0.021(3) 0.025(3) 0.022(2) -0.004(2) 0.002(2) -0.007(2)
C14 0.014(3) 0.042(4) 0.020(2) -0.005(2) -0.002(2) -0.004(2)
C15 0.030(4) 0.034(3) 0.023(3) 0.007(2) 0.003(2) 0.003(3)
C16 0.058(5) 0.041(4) 0.031(3) -0.003(3) 0.001(3) 0.014(3)
C17 0.058(5) 0.044(4) 0.030(3) -0.007(3) -0.001(3) 0.004(3)
C18 0.066(6) 0.056(5) 0.036(4) 0.016(3) 0.006(4) 0.012(4)
C19 0.032(4) 0.035(3) 0.031(3) 0.000(3) 0.014(3) 0.006(3)
C20 0.034(4) 0.020(3) 0.037(3) -0.003(2) 0.006(3) 0.004(3)
C21 0.042(4) 0.022(3) 0.041(3) 0.002(3) 0.013(3) 0.005(3)
C22 0.054(5) 0.025(3) 0.048(4) 0.012(3) 0.022(3) 0.002(3)
C23 0.034(4) 0.029(4) 0.072(5) -0.005(3) 0.016(4) -0.002(3)
C24 0.060(5) 0.027(4) 0.051(4) 0.012(3) 0.012(4) 0.004(3)
C25 0.039(4) 0.027(3) 0.029(3) -0.003(2) 0.015(3) -0.011(3)
C26 0.026(3) 0.025(3) 0.028(3) 0.003(2) 0.008(2) 0.003(3)
C27 0.032(4) 0.049(4) 0.033(3) 0.006(3) 0.005(3) -0.008(3)
C28 0.032(4) 0.031(3) 0.030(3) 0.000(3) 0.003(3) 0.001(3)
C29 0.040(4) 0.036(4) 0.024(3) -0.005(3) 0.007(3) 0.000(3)
C30 0.029(4) 0.058(4) 0.031(3) 0.010(3) -0.004(3) -0.015(3)
C31 0.044(4) 0.037(4) 0.020(3) 0.000(2) 0.007(3) -0.001(3)
W3 0.02671(14) 0.02368(12) 0.02178(11) 0.00343(8) 0.00592(10) -0.00404(10)
W4 0.02063(13) 0.02345(11) 0.02068(10) -0.00281(8) 0.00682(9) -0.00273(9)
P5 0.0213(8) 0.0247(7) 0.0199(6) -0.0011(5) 0.0064(6) 0.0005(6)
P6 0.0298(9) 0.0249(8) 0.0265(7) -0.0052(6) 0.0123(6) -0.0092(6)
P7 0.0268(9) 0.0214(7) 0.0313(8) 0.0023(6) 0.0143(7) 0.0030(6)
P8 0.0199(8) 0.0208(7) 0.0219(6) 0.0023(5) 0.0048(6) -0.0016(6)
N5 0.019(3) 0.025(2) 0.022(2) -0.0057(18) 0.0052(19) -0.0031(19)
N6 0.027(3) 0.026(2) 0.024(2) -0.0006(18) 0.010(2) -0.004(2)
N7 0.031(3) 0.018(2) 0.044(3) 0.003(2) 0.019(2) -0.003(2)
N8 0.025(3) 0.017(2) 0.029(2) 0.0026(18) 0.009(2) -0.0011(19)
O8 0.072(4) 0.053(3) 0.056(3) 0.009(2) 0.028(3) 0.028(3)
O9 0.080(4) 0.045(3) 0.057(3) 0.006(2) 0.002(3) -0.035(3)
O10 0.071(4) 0.078(4) 0.033(2) 0.020(2) 0.021(2) 0.004(3)
O11 0.036(3) 0.068(3) 0.041(3) -0.010(2) 0.010(2) 0.008(3)
O12 0.035(3) 0.105(4) 0.039(3) -0.017(3) 0.020(2) -0.004(3)
O13 0.066(4) 0.079(4) 0.048(3) 0.002(3) 0.012(3) 0.034(3)
O14 0.119(6) 0.074(4) 0.056(3) -0.017(3) 0.013(3) -0.046(4)
C32 0.037(4) 0.050(4) 0.024(3) -0.011(3) 0.009(3) 0.005(3)
C33 0.032(4) 0.029(3) 0.034(3) -0.003(2) 0.015(3) 0.004(3)
C34 0.038(4) 0.022(3) 0.038(3) 0.000(2) 0.019(3) 0.002(3)
C35 0.022(3) 0.039(3) 0.032(3) 0.003(3) 0.007(3) 0.008(3)
C36 0.050(5) 0.071(5) 0.033(3) -0.008(3) 0.021(3) 0.016(4)
C37 0.035(4) 0.047(4) 0.055(4) -0.006(3) 0.022(3) 0.011(3)
C38 0.035(4) 0.037(3) 0.025(3) 0.000(2) 0.015(3) -0.007(3)
C39 0.024(3) 0.037(3) 0.026(3) 0.006(2) 0.010(2) 0.000(3)
C40 0.020(3) 0.034(3) 0.034(3) 0.002(3) 0.006(3) -0.005(3)
C41 0.046(4) 0.039(4) 0.037(3) -0.007(3) 0.019(3) -0.024(3)
C42 0.063(5) 0.038(4) 0.042(4) 0.008(3) 0.026(4) -0.003(3)
C43 0.044(4) 0.035(4) 0.049(4) -0.002(3) 0.021(3) -0.008(3)
C44 0.052(5) 0.024(3) 0.053(4) 0.012(3) 0.025(3) 0.004(3)
C45 0.049(5) 0.019(3) 0.051(4) -0.003(3) 0.011(3) 0.003(3)
C46 0.035(4) 0.024(3) 0.048(4) -0.009(3) 0.006(3) 0.003(3)
C47 0.039(4) 0.025(3) 0.046(4) -0.002(3) 0.020(3) 0.006(3)
C48 0.062(6) 0.036(4) 0.070(5) 0.014(4) 0.014(4) 0.005(4)
C49 0.040(5) 0.039(4) 0.077(5) -0.001(4) 0.014(4) 0.004(3)
C50 0.022(3) 0.032(3) 0.026(3) 0.001(2) 0.006(2) -0.004(2)
C51 0.019(3) 0.034(3) 0.026(3) 0.005(2) 0.002(2) 0.000(2)
C52 0.021(3) 0.047(4) 0.032(3) 0.007(3) 0.010(3) 0.003(3)
C53 0.077(6) 0.034(4) 0.034(4) 0.001(3) -0.006(3) 0.011(4)
C54 0.061(5) 0.041(4) 0.037(3) 0.001(3) 0.002(3) -0.006(4)
C55 0.044(5) 0.056(5) 0.036(3) 0.020(3) 0.002(3) 0.002(3)
C56 0.050(5) 0.041(4) 0.028(3) 0.009(3) 0.015(3) 0.004(3)
C57 0.046(4) 0.033(4) 0.027(3) 0.005(3) 0.004(3) -0.009(3)
C58 0.039(4) 0.049(4) 0.029(3) 0.002(3) 0.009(3) 0.000(3)
C59 0.037(4) 0.039(4) 0.021(3) 0.000(2) 0.008(3) -0.003(3)
C60 0.034(4) 0.064(5) 0.029(3) -0.003(3) 0.011(3) 0.004(3)
C61 0.052(5) 0.058(5) 0.022(3) 0.001(3) 0.009(3) 0.018(4)
C62 0.091(7) 0.045(4) 0.032(4) 0.000(3) 0.004(4) -0.024(4)
#==============================================================================
# MOLECULAR GEOMETRY
_geom_special_details
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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
W1 C26 1.939(6) . ?
W1 C27 1.994(6) . ?
W1 C25 2.021(6) . ?
W1 C28 2.021(6) . ?
W1 P3 2.4568(13) . ?
W1 W2 3.0984(3) . ?
W2 C30 1.940(6) . ?
W2 C29 1.981(6) . ?
W2 C31 1.999(6) . ?
W2 P1 2.4322(13) . ?
W2 P2 2.4818(13) . ?
W2 P4 2.5340(14) . ?
P1 N4 1.671(5) . ?
P1 N1 1.674(4) . ?
P1 C1 1.789(5) . ?
P1 P4 2.606(2) . ?
P1 P2 2.6149(19) . ?
P2 N2 1.687(4) . ?
P2 N1 1.698(4) . ?
P2 C7 1.803(6) . ?
P3 N3 1.703(4) . ?
P3 N2 1.727(4) . ?
P3 C13 1.828(5) . ?
P4 N3 1.693(4) . ?
P4 N4 1.694(4) . ?
P4 C19 1.812(5) . ?
N1 C4 1.474(6) . ?
N2 C10 1.465(6) . ?
N3 C16 1.475(7) . ?
N4 C22 1.458(7) . ?
O1 C25 1.141(7) . ?
O2 C26 1.169(6) . ?
O3 C27 1.164(6) . ?
O4 C28 1.155(7) . ?
O5 C29 1.159(6) . ?
O6 C30 1.178(7) . ?
O7 C31 1.178(7) . ?
C1 C2 1.511(7) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.332(7) . ?
C2 C5 1.502(8) . ?
C3 C4 1.495(8) . ?
C3 C6 1.519(7) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.520(7) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.322(8) . ?
C8 C11 1.491(8) . ?
C9 C10 1.499(8) . ?
C9 C12 1.511(7) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.512(7) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.323(7) . ?
C14 C17 1.508(7) . ?
C15 C18 1.499(7) . ?
C15 C16 1.512(8) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.510(7) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.330(8) . ?
C20 C23 1.513(8) . ?
C21 C24 1.502(8) . ?
C21 C22 1.511(8) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
W3 C57 1.929(6) . ?
W3 C58 2.007(6) . ?
W3 C59 2.008(7) . ?
W3 C56 2.013(7) . ?
W3 P8 2.4548(13) . ?
W3 W4 3.0805(3) . ?
W4 C62 1.934(7) . ?
W4 C61 1.990(7) . ?
W4 C60 2.010(6) . ?
W4 P6 2.4187(14) . ?
W4 P7 2.4969(15) . ?
W4 P5 2.5261(13) . ?
P5 N5 1.678(4) . ?
P5 N6 1.704(4) . ?
P5 C35 1.801(5) . ?
P5 P6 2.6093(19) . ?
P6 N6 1.670(4) . ?
P6 N7 1.676(5) . ?
P6 C41 1.789(5) . ?
P6 P7 2.601(2) . ?
P7 N7 1.691(4) . ?
P7 N8 1.704(4) . ?
P7 C47 1.798(5) . ?
P8 N8 1.710(4) . ?
P8 N5 1.721(4) . ?
P8 C50 1.826(5) . ?
N5 C32 1.470(6) . ?
N6 C38 1.469(6) . ?
N7 C44 1.473(7) . ?
N8 C53 1.466(7) . ?
O8 C56 1.148(7) . ?
O9 C57 1.180(7) . ?
O10 C58 1.146(6) . ?
O11 C59 1.154(7) . ?
O12 C60 1.167(7) . ?
O13 C61 1.158(7) . ?
O14 C62 1.192(7) . ?
C32 C33 1.508(8) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.330(8) . ?
C33 C36 1.514(7) . ?
C34 C37 1.494(8) . ?
C34 C35 1.512(7) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C39 1.500(8) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.336(7) . ?
C39 C42 1.507(7) . ?
C40 C41 1.516(7) . ?
C40 C43 1.519(8) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 C45 1.506(9) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 C46 1.341(9) . ?
C45 C48 1.495(8) . ?
C46 C49 1.500(8) . ?
C46 C47 1.526(8) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 C51 1.511(7) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 C52 1.316(8) . ?
C51 C54 1.496(7) . ?
C52 C53 1.502(8) . ?
C52 C55 1.514(7) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
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
C26 W1 C27 95.0(2) . . ?
C26 W1 C25 84.9(2) . . ?
C27 W1 C25 87.3(2) . . ?
C26 W1 C28 87.0(2) . . ?
C27 W1 C28 93.7(2) . . ?
C25 W1 C28 171.9(2) . . ?
C26 W1 P3 91.45(15) . . ?
C27 W1 P3 172.61(18) . . ?
C25 W1 P3 89.67(15) . . ?
C28 W1 P3 90.25(16) . . ?
C26 W1 W2 164.57(15) . . ?
C27 W1 W2 98.84(18) . . ?
C25 W1 W2 88.93(16) . . ?
C28 W1 W2 98.84(17) . . ?
P3 W1 W2 74.35(3) . . ?
C30 W2 C29 87.8(3) . . ?
C30 W2 C31 81.0(3) . . ?
C29 W2 C31 97.7(2) . . ?
C30 W2 P1 81.62(18) . . ?
C29 W2 P1 117.43(17) . . ?
C31 W2 P1 139.92(18) . . ?
C30 W2 P2 103.8(2) . . ?
C29 W2 P2 168.35(18) . . ?
C31 W2 P2 85.34(16) . . ?
P1 W2 P2 64.29(4) . . ?
C30 W2 P4 134.8(2) . . ?
C29 W2 P4 84.51(17) . . ?
C31 W2 P4 144.14(18) . . ?
P1 W2 P4 63.26(5) . . ?
P2 W2 P4 86.49(4) . . ?
C30 W2 W1 140.98(18) . . ?
C29 W2 W1 85.62(17) . . ?
C31 W2 W1 61.90(18) . . ?
P1 W2 W1 134.76(3) . . ?
P2 W2 W1 85.92(3) . . ?
P4 W2 W1 82.73(3) . . ?
N4 P1 N1 111.2(2) . . ?
N4 P1 C1 107.6(3) . . ?
N1 P1 C1 102.7(2) . . ?
N4 P1 W2 99.52(15) . . ?
N1 P1 W2 97.48(15) . . ?
C1 P1 W2 137.04(19) . . ?
N4 P1 P4 39.57(14) . . ?
N1 P1 P4 109.16(16) . . ?
C1 P1 P4 140.9(2) . . ?
W2 P1 P4 60.28(4) . . ?
N4 P1 P2 107.53(16) . . ?
N1 P1 P2 39.50(14) . . ?
C1 P1 P2 136.3(2) . . ?
W2 P1 P2 58.78(4) . . ?
P4 P1 P2 82.33(6) . . ?
N2 P2 N1 113.1(2) . . ?
N2 P2 C7 98.9(2) . . ?
N1 P2 C7 104.3(2) . . ?
N2 P2 W2 112.39(15) . . ?
N1 P2 W2 94.98(14) . . ?
C7 P2 W2 132.87(18) . . ?
N2 P2 P1 117.75(16) . . ?
N1 P2 P1 38.81(14) . . ?
C7 P2 P1 134.8(2) . . ?
W2 P2 P1 56.93(4) . . ?
N3 P3 N2 107.3(2) . . ?
N3 P3 C13 97.6(2) . . ?
N2 P3 C13 103.0(2) . . ?
N3 P3 W1 113.79(15) . . ?
N2 P3 W1 114.68(15) . . ?
C13 P3 W1 118.48(17) . . ?
N3 P4 N4 110.0(2) . . ?
N3 P4 C19 107.3(3) . . ?
N4 P4 C19 98.1(2) . . ?
N3 P4 W2 112.38(16) . . ?
N4 P4 W2 95.10(16) . . ?
C19 P4 W2 130.44(18) . . ?
N3 P4 P1 117.49(16) . . ?
N4 P4 P1 38.93(16) . . ?
C19 P4 P1 125.3(2) . . ?
W2 P4 P1 56.46(4) . . ?
C4 N1 P1 123.9(4) . . ?
C4 N1 P2 133.1(4) . . ?
P1 N1 P2 101.7(2) . . ?
C10 N2 P2 120.6(3) . . ?
C10 N2 P3 124.8(4) . . ?
P2 N2 P3 113.5(2) . . ?
C16 N3 P4 123.7(4) . . ?
C16 N3 P3 124.0(4) . . ?
P4 N3 P3 112.3(2) . . ?
C22 N4 P1 133.0(4) . . ?
C22 N4 P4 125.0(4) . . ?
P1 N4 P4 101.5(2) . . ?
C2 C1 P1 113.8(4) . . ?
C2 C1 H1A 108.8 . . ?
P1 C1 H1A 108.8 . . ?
C2 C1 H1B 108.8 . . ?
P1 C1 H1B 108.8 . . ?
H1A C1 H1B 107.7 . . ?
C3 C2 C5 124.2(5) . . ?
C3 C2 C1 124.1(5) . . ?
C5 C2 C1 111.7(5) . . ?
C2 C3 C4 127.5(5) . . ?
C2 C3 C6 122.7(5) . . ?
C4 C3 C6 109.8(5) . . ?
N1 C4 C3 114.7(4) . . ?
N1 C4 H4A 108.6 . . ?
C3 C4 H4A 108.6 . . ?
N1 C4 H4B 108.6 . . ?
C3 C4 H4B 108.6 . . ?
H4A C4 H4B 107.6 . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 P2 112.9(4) . . ?
C8 C7 H7A 109.0 . . ?
P2 C7 H7A 109.0 . . ?
C8 C7 H7B 109.0 . . ?
P2 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
C9 C8 C11 122.9(6) . . ?
C9 C8 C7 123.0(5) . . ?
C11 C8 C7 114.1(5) . . ?
C8 C9 C10 125.8(5) . . ?
C8 C9 C12 122.6(6) . . ?
C10 C9 C12 111.6(5) . . ?
N2 C10 C9 116.4(4) . . ?
N2 C10 H10A 108.2 . . ?
C9 C10 H10A 108.2 . . ?
N2 C10 H10B 108.2 . . ?
C9 C10 H10B 108.2 . . ?
H10A C10 H10B 107.3 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 P3 116.7(4) . . ?
C14 C13 H13A 108.1 . . ?
P3 C13 H13A 108.1 . . ?
C14 C13 H13B 108.1 . . ?
P3 C13 H13B 108.1 . . ?
H13A C13 H13B 107.3 . . ?
C15 C14 C17 124.1(5) . . ?
C15 C14 C13 119.1(5) . . ?
C17 C14 C13 116.8(5) . . ?
C14 C15 C18 125.0(5) . . ?
C14 C15 C16 121.0(5) . . ?
C18 C15 C16 113.8(5) . . ?
N3 C16 C15 115.9(5) . . ?
N3 C16 H16A 108.3 . . ?
C15 C16 H16A 108.3 . . ?
N3 C16 H16B 108.3 . . ?
C15 C16 H16B 108.3 . . ?
H16A C16 H16B 107.4 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 P4 115.1(4) . . ?
C20 C19 H19A 108.5 . . ?
P4 C19 H19A 108.5 . . ?
C20 C19 H19B 108.5 . . ?
P4 C19 H19B 108.5 . . ?
H19A C19 H19B 107.5 . . ?
C21 C20 C19 126.5(5) . . ?
C21 C20 C23 121.8(5) . . ?
C19 C20 C23 111.7(5) . . ?
C20 C21 C24 123.5(6) . . ?
C20 C21 C22 124.8(5) . . ?
C24 C21 C22 111.6(5) . . ?
N4 C22 C21 113.2(5) . . ?
N4 C22 H22A 108.9 . . ?
C21 C22 H22A 108.9 . . ?
N4 C22 H22B 108.9 . . ?
C21 C22 H22B 108.9 . . ?
H22A C22 H22B 107.8 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O1 C25 W1 173.9(5) . . ?
O2 C26 W1 178.9(5) . . ?
O3 C27 W1 176.9(6) . . ?
O4 C28 W1 177.9(6) . . ?
O5 C29 W2 178.2(6) . . ?
O6 C30 W2 176.8(6) . . ?
O7 C31 W2 163.3(6) . . ?
C57 W3 C58 93.2(2) . . ?
C57 W3 C59 87.6(3) . . ?
C58 W3 C59 88.9(2) . . ?
C57 W3 C56 85.9(3) . . ?
C58 W3 C56 93.6(2) . . ?
C59 W3 C56 173.1(2) . . ?
C57 W3 P8 89.67(16) . . ?
C58 W3 P8 175.35(19) . . ?
C59 W3 P8 87.51(15) . . ?
C56 W3 P8 90.28(16) . . ?
C57 W3 W4 161.70(17) . . ?
C58 W3 W4 103.69(18) . . ?
C59 W3 W4 99.65(17) . . ?
C56 W3 W4 85.97(19) . . ?
P8 W3 W4 74.02(3) . . ?
C62 W4 C61 83.7(3) . . ?
C62 W4 C60 80.1(3) . . ?
C61 W4 C60 99.5(3) . . ?
C62 W4 P6 83.0(2) . . ?
C61 W4 P6 114.1(2) . . ?
C60 W4 P6 140.17(19) . . ?
C62 W4 P7 107.9(2) . . ?
C61 W4 P7 167.48(17) . . ?
C60 W4 P7 87.58(18) . . ?
P6 W4 P7 63.88(5) . . ?
C62 W4 P5 133.3(2) . . ?
C61 W4 P5 81.76(16) . . ?
C60 W4 P5 146.03(19) . . ?
P6 W4 P5 63.65(4) . . ?
P7 W4 P5 86.61(4) . . ?
C62 W4 W3 138.7(2) . . ?
C61 W4 W3 90.6(2) . . ?
C60 W4 W3 60.50(19) . . ?
P6 W4 W3 135.37(4) . . ?
P7 W4 W3 83.92(3) . . ?
P5 W4 W3 85.59(3) . . ?
N5 P5 N6 113.4(2) . . ?
N5 P5 C35 100.9(2) . . ?
N6 P5 C35 103.0(2) . . ?
N5 P5 W4 112.87(15) . . ?
N6 P5 W4 94.80(15) . . ?
C35 P5 W4 131.36(18) . . ?
N5 P5 P6 121.34(16) . . ?
N6 P5 P6 38.86(14) . . ?
C35 P5 P6 130.3(2) . . ?
W4 P5 P6 56.17(4) . . ?
N6 P6 N7 111.5(2) . . ?
N6 P6 C41 102.6(3) . . ?
N7 P6 C41 108.2(3) . . ?
N6 P6 W4 99.76(16) . . ?
N7 P6 W4 98.13(16) . . ?
C41 P6 W4 135.8(2) . . ?
N6 P6 P7 107.27(17) . . ?
N7 P6 P7 39.61(15) . . ?
C41 P6 P7 142.7(2) . . ?
W4 P6 P7 59.52(4) . . ?
N6 P6 P5 39.83(15) . . ?
N7 P6 P5 110.45(17) . . ?
C41 P6 P5 134.2(2) . . ?
W4 P6 P5 60.18(4) . . ?
P7 P6 P5 82.78(6) . . ?
N7 P7 N8 110.1(2) . . ?
N7 P7 C47 99.5(3) . . ?
N8 P7 C47 106.4(3) . . ?
N7 P7 W4 94.85(17) . . ?
N8 P7 W4 110.77(16) . . ?
C47 P7 W4 132.2(2) . . ?
N7 P7 P6 39.20(16) . . ?
N8 P7 P6 113.04(16) . . ?
C47 P7 P6 130.3(2) . . ?
W4 P7 P6 56.60(5) . . ?
N8 P8 N5 106.3(2) . . ?
N8 P8 C50 98.3(2) . . ?
N5 P8 C50 103.4(2) . . ?
N8 P8 W3 115.42(15) . . ?
N5 P8 W3 114.77(15) . . ?
C50 P8 W3 116.77(17) . . ?
C32 N5 P5 121.9(4) . . ?
C32 N5 P8 125.7(4) . . ?
P5 N5 P8 111.4(2) . . ?
C38 N6 P6 125.2(4) . . ?
C38 N6 P5 133.4(4) . . ?
P6 N6 P5 101.3(2) . . ?
C44 N7 P6 132.0(4) . . ?
C44 N7 P7 126.4(4) . . ?
P6 N7 P7 101.2(2) . . ?
C53 N8 P7 120.4(4) . . ?
C53 N8 P8 123.1(4) . . ?
P7 N8 P8 113.1(2) . . ?
N5 C32 C33 116.3(5) . . ?
N5 C32 H32A 108.2 . . ?
C33 C32 H32A 108.2 . . ?
N5 C32 H32B 108.2 . . ?
C33 C32 H32B 108.2 . . ?
H32A C32 H32B 107.4 . . ?
C34 C33 C32 125.9(5) . . ?
C34 C33 C36 124.8(5) . . ?
C32 C33 C36 109.3(5) . . ?
C33 C34 C37 124.3(5) . . ?
C33 C34 C35 123.6(5) . . ?
C37 C34 C35 112.1(5) . . ?
C34 C35 P5 114.2(4) . . ?
C34 C35 H35A 108.7 . . ?
P5 C35 H35A 108.7 . . ?
C34 C35 H35B 108.7 . . ?
P5 C35 H35B 108.7 . . ?
H35A C35 H35B 107.6 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N6 C38 C39 114.7(4) . . ?
N6 C38 H38A 108.6 . . ?
C39 C38 H38A 108.6 . . ?
N6 C38 H38B 108.6 . . ?
C39 C38 H38B 108.6 . . ?
H38A C38 H38B 107.6 . . ?
C40 C39 C38 127.1(5) . . ?
C40 C39 C42 122.5(5) . . ?
C38 C39 C42 110.4(5) . . ?
C39 C40 C41 124.1(5) . . ?
C39 C40 C43 123.3(5) . . ?
C41 C40 C43 112.5(5) . . ?
C40 C41 P6 113.7(4) . . ?
C40 C41 H41A 108.8 . . ?
P6 C41 H41A 108.8 . . ?
C40 C41 H41B 108.8 . . ?
P6 C41 H41B 108.8 . . ?
H41A C41 H41B 107.7 . . ?
C39 C42 H42A 109.5 . . ?
C39 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C39 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C40 C43 H43A 109.5 . . ?
C40 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C40 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
N7 C44 C45 114.6(5) . . ?
N7 C44 H44A 108.6 . . ?
C45 C44 H44A 108.6 . . ?
N7 C44 H44B 108.6 . . ?
C45 C44 H44B 108.6 . . ?
H44A C44 H44B 107.6 . . ?
C46 C45 C48 123.4(6) . . ?
C46 C45 C44 125.1(6) . . ?
C48 C45 C44 111.5(6) . . ?
C45 C46 C49 121.6(6) . . ?
C45 C46 C47 125.2(6) . . ?
C49 C46 C47 113.1(6) . . ?
C46 C47 P7 114.3(4) . . ?
C46 C47 H47A 108.7 . . ?
P7 C47 H47A 108.7 . . ?
C46 C47 H47B 108.7 . . ?
P7 C47 H47B 108.7 . . ?
H47A C47 H47B 107.6 . . ?
C45 C48 H48A 109.5 . . ?
C45 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C45 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C46 C49 H49A 109.5 . . ?
C46 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C46 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C51 C50 P8 116.0(4) . . ?
C51 C50 H50A 108.3 . . ?
P8 C50 H50A 108.3 . . ?
C51 C50 H50B 108.3 . . ?
P8 C50 H50B 108.3 . . ?
H50A C50 H50B 107.4 . . ?
C52 C51 C54 123.8(5) . . ?
C52 C51 C50 120.7(5) . . ?
C54 C51 C50 115.5(5) . . ?
C51 C52 C53 125.1(5) . . ?
C51 C52 C55 123.8(6) . . ?
C53 C52 C55 111.1(5) . . ?
N8 C53 C52 119.1(5) . . ?
N8 C53 H53A 107.5 . . ?
C52 C53 H53A 107.5 . . ?
N8 C53 H53B 107.5 . . ?
C52 C53 H53B 107.5 . . ?
H53A C53 H53B 107.0 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C52 C55 H55A 109.5 . . ?
C52 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C52 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
O8 C56 W3 177.1(6) . . ?
O9 C57 W3 178.0(5) . . ?
O10 C58 W3 176.9(6) . . ?
O11 C59 W3 174.7(5) . . ?
O12 C60 W4 161.8(6) . . ?
O13 C61 W4 178.0(5) . . ?
O14 C62 W4 178.2(7) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C26 W1 W2 C30 172.7(7) . . . . ?
C27 W1 W2 C30 -33.8(4) . . . . ?
C25 W1 W2 C30 -120.9(4) . . . . ?
C28 W1 W2 C30 61.3(4) . . . . ?
P3 W1 W2 C30 149.1(3) . . . . ?
C26 W1 W2 C29 -106.2(6) . . . . ?
C27 W1 W2 C29 47.2(3) . . . . ?
C25 W1 W2 C29 -39.8(2) . . . . ?
C28 W1 W2 C29 142.4(2) . . . . ?
P3 W1 W2 C29 -129.81(17) . . . . ?
C26 W1 W2 C31 152.7(6) . . . . ?
C27 W1 W2 C31 -53.9(3) . . . . ?
C25 W1 W2 C31 -141.0(2) . . . . ?
C28 W1 W2 C31 41.3(2) . . . . ?
P3 W1 W2 C31 129.06(18) . . . . ?
C26 W1 W2 P1 18.9(6) . . . . ?
C27 W1 W2 P1 172.3(2) . . . . ?
C25 W1 W2 P1 85.23(16) . . . . ?
C28 W1 W2 P1 -92.49(16) . . . . ?
P3 W1 W2 P1 -4.73(6) . . . . ?
C26 W1 W2 P2 65.8(6) . . . . ?
C27 W1 W2 P2 -140.77(19) . . . . ?
C25 W1 W2 P2 132.13(15) . . . . ?
C28 W1 W2 P2 -45.59(16) . . . . ?
P3 W1 W2 P2 42.18(5) . . . . ?
C26 W1 W2 P4 -21.2(6) . . . . ?
C27 W1 W2 P4 132.26(19) . . . . ?
C25 W1 W2 P4 45.16(15) . . . . ?
C28 W1 W2 P4 -132.56(16) . . . . ?
P3 W1 W2 P4 -44.80(5) . . . . ?
C30 W2 P1 N4 145.4(3) . . . . ?
C29 W2 P1 N4 62.3(2) . . . . ?
C31 W2 P1 N4 -149.4(3) . . . . ?
P2 W2 P1 N4 -104.80(15) . . . . ?
P4 W2 P1 N4 -5.22(15) . . . . ?
W1 W2 P1 N4 -50.86(16) . . . . ?
C30 W2 P1 N1 -101.5(3) . . . . ?
C29 W2 P1 N1 175.4(2) . . . . ?
C31 W2 P1 N1 -36.3(3) . . . . ?
P2 W2 P1 N1 8.25(15) . . . . ?
P4 W2 P1 N1 107.83(16) . . . . ?
W1 W2 P1 N1 62.19(17) . . . . ?
C30 W2 P1 C1 16.3(4) . . . . ?
C29 W2 P1 C1 -66.8(4) . . . . ?
C31 W2 P1 C1 81.5(4) . . . . ?
P2 W2 P1 C1 126.1(3) . . . . ?
P4 W2 P1 C1 -134.4(3) . . . . ?
W1 W2 P1 C1 180.0(3) . . . . ?
C30 W2 P1 P4 150.7(2) . . . . ?
C29 W2 P1 P4 67.5(2) . . . . ?
C31 W2 P1 P4 -144.2(3) . . . . ?
P2 W2 P1 P4 -99.58(6) . . . . ?
W1 W2 P1 P4 -45.64(6) . . . . ?
C30 W2 P1 P2 -109.8(2) . . . . ?
C29 W2 P1 P2 167.1(2) . . . . ?
C31 W2 P1 P2 -44.6(3) . . . . ?
P4 W2 P1 P2 99.58(6) . . . . ?
W1 W2 P1 P2 53.94(6) . . . . ?
C30 W2 P2 N2 -177.1(3) . . . . ?
C29 W2 P2 N2 8.1(9) . . . . ?
C31 W2 P2 N2 -97.5(2) . . . . ?
P1 W2 P2 N2 109.44(17) . . . . ?
P4 W2 P2 N2 47.52(16) . . . . ?
W1 W2 P2 N2 -35.43(16) . . . . ?
C30 W2 P2 N1 65.4(2) . . . . ?
C29 W2 P2 N1 -109.4(9) . . . . ?
C31 W2 P2 N1 144.9(2) . . . . ?
P1 W2 P2 N1 -8.09(15) . . . . ?
P4 W2 P2 N1 -70.01(16) . . . . ?
W1 W2 P2 N1 -152.96(15) . . . . ?
C30 W2 P2 C7 -49.5(3) . . . . ?
C29 W2 P2 C7 135.7(9) . . . . ?
C31 W2 P2 C7 30.1(3) . . . . ?
P1 W2 P2 C7 -122.9(3) . . . . ?
P4 W2 P2 C7 175.2(3) . . . . ?
W1 W2 P2 C7 92.2(3) . . . . ?
C30 W2 P2 P1 73.5(2) . . . . ?
C29 W2 P2 P1 -101.3(9) . . . . ?
C31 W2 P2 P1 153.03(19) . . . . ?
P4 W2 P2 P1 -61.92(5) . . . . ?
W1 W2 P2 P1 -144.87(4) . . . . ?
N4 P1 P2 N2 -9.2(2) . . . . ?
N1 P1 P2 N2 93.1(3) . . . . ?
C1 P1 P2 N2 133.0(3) . . . . ?
W2 P1 P2 N2 -99.85(17) . . . . ?
P4 P1 P2 N2 -40.07(17) . . . . ?
N4 P1 P2 N1 -102.3(3) . . . . ?
C1 P1 P2 N1 39.9(4) . . . . ?
W2 P1 P2 N1 167.1(2) . . . . ?
P4 P1 P2 N1 -133.2(2) . . . . ?
N4 P1 P2 C7 -149.5(3) . . . . ?
N1 P1 P2 C7 -47.2(3) . . . . ?
C1 P1 P2 C7 -7.3(4) . . . . ?
W2 P1 P2 C7 119.8(3) . . . . ?
P4 P1 P2 C7 179.6(2) . . . . ?
N4 P1 P2 W2 90.66(16) . . . . ?
N1 P1 P2 W2 -167.1(2) . . . . ?
C1 P1 P2 W2 -127.2(3) . . . . ?
P4 P1 P2 W2 59.77(4) . . . . ?
C26 W1 P3 N3 -110.1(2) . . . . ?
C27 W1 P3 N3 40.6(15) . . . . ?
C25 W1 P3 N3 -25.2(2) . . . . ?
C28 W1 P3 N3 162.9(2) . . . . ?
W2 W1 P3 N3 63.81(17) . . . . ?
C26 W1 P3 N2 125.9(2) . . . . ?
C27 W1 P3 N2 -83.5(15) . . . . ?
C25 W1 P3 N2 -149.2(2) . . . . ?
C28 W1 P3 N2 38.9(2) . . . . ?
W2 W1 P3 N2 -60.20(16) . . . . ?
C26 W1 P3 C13 3.8(3) . . . . ?
C27 W1 P3 C13 154.4(15) . . . . ?
C25 W1 P3 C13 88.7(3) . . . . ?
C28 W1 P3 C13 -83.2(3) . . . . ?
W2 W1 P3 C13 177.7(2) . . . . ?
C30 W2 P4 N3 -152.1(3) . . . . ?
C29 W2 P4 N3 126.5(2) . . . . ?
C31 W2 P4 N3 30.9(3) . . . . ?
P1 W2 P4 N3 -109.03(17) . . . . ?
P2 W2 P4 N3 -46.14(17) . . . . ?
W1 W2 P4 N3 40.18(16) . . . . ?
C30 W2 P4 N4 -38.0(3) . . . . ?
C29 W2 P4 N4 -119.4(2) . . . . ?
C31 W2 P4 N4 145.0(3) . . . . ?
P1 W2 P4 N4 5.10(14) . . . . ?
P2 W2 P4 N4 67.99(15) . . . . ?
W1 W2 P4 N4 154.31(15) . . . . ?
C30 W2 P4 C19 67.2(4) . . . . ?
C29 W2 P4 C19 -14.3(3) . . . . ?
C31 W2 P4 C19 -109.8(4) . . . . ?
P1 W2 P4 C19 110.3(3) . . . . ?
P2 W2 P4 C19 173.1(3) . . . . ?
W1 W2 P4 C19 -100.5(3) . . . . ?
C30 W2 P4 P1 -43.1(3) . . . . ?
C29 W2 P4 P1 -124.52(18) . . . . ?
C31 W2 P4 P1 139.9(3) . . . . ?
P2 W2 P4 P1 62.89(5) . . . . ?
W1 W2 P4 P1 149.21(4) . . . . ?
N4 P1 P4 N3 -88.3(3) . . . . ?
N1 P1 P4 N3 12.1(2) . . . . ?
C1 P1 P4 N3 -130.9(3) . . . . ?
W2 P1 P4 N3 99.78(17) . . . . ?
P2 P1 P4 N3 41.48(18) . . . . ?
N1 P1 P4 N4 100.4(3) . . . . ?
C1 P1 P4 N4 -42.6(4) . . . . ?
W2 P1 P4 N4 -171.9(2) . . . . ?
P2 P1 P4 N4 129.8(2) . . . . ?
N4 P1 P4 C19 52.9(3) . . . . ?
N1 P1 P4 C19 153.3(3) . . . . ?
C1 P1 P4 C19 10.4(4) . . . . ?
W2 P1 P4 C19 -119.0(2) . . . . ?
P2 P1 P4 C19 -177.3(2) . . . . ?
N4 P1 P4 W2 171.9(2) . . . . ?
N1 P1 P4 W2 -87.72(17) . . . . ?
C1 P1 P4 W2 129.3(3) . . . . ?
P2 P1 P4 W2 -58.30(4) . . . . ?
N4 P1 N1 C4 -76.1(5) . . . . ?
C1 P1 N1 C4 38.8(5) . . . . ?
W2 P1 N1 C4 -179.4(4) . . . . ?
P4 P1 N1 C4 -118.3(4) . . . . ?
P2 P1 N1 C4 -168.3(6) . . . . ?
N4 P1 N1 P2 92.2(2) . . . . ?
C1 P1 N1 P2 -153.0(3) . . . . ?
W2 P1 N1 P2 -11.1(2) . . . . ?
P4 P1 N1 P2 49.9(2) . . . . ?
N2 P2 N1 C4 60.6(6) . . . . ?
C7 P2 N1 C4 -45.9(6) . . . . ?
W2 P2 N1 C4 177.5(5) . . . . ?
P1 P2 N1 C4 166.6(6) . . . . ?
N2 P2 N1 P1 -106.1(2) . . . . ?
C7 P2 N1 P1 147.5(2) . . . . ?
W2 P2 N1 P1 10.9(2) . . . . ?
N1 P2 N2 C10 -61.0(4) . . . . ?
C7 P2 N2 C10 48.9(4) . . . . ?
W2 P2 N2 C10 -167.1(3) . . . . ?
P1 P2 N2 C10 -103.8(4) . . . . ?
N1 P2 N2 P3 107.6(3) . . . . ?
C7 P2 N2 P3 -142.5(3) . . . . ?
W2 P2 N2 P3 1.5(3) . . . . ?
P1 P2 N2 P3 64.8(3) . . . . ?
N3 P3 N2 C10 90.6(4) . . . . ?
C13 P3 N2 C10 -11.8(5) . . . . ?
W1 P3 N2 C10 -141.9(4) . . . . ?
N3 P3 N2 P2 -77.4(3) . . . . ?
C13 P3 N2 P2 -179.8(2) . . . . ?
W1 P3 N2 P2 50.0(3) . . . . ?
N4 P4 N3 C16 67.6(5) . . . . ?
C19 P4 N3 C16 -38.1(5) . . . . ?
W2 P4 N3 C16 172.2(4) . . . . ?
P1 P4 N3 C16 109.6(4) . . . . ?
N4 P4 N3 P3 -110.0(3) . . . . ?
C19 P4 N3 P3 144.3(3) . . . . ?
W2 P4 N3 P3 -5.4(3) . . . . ?
P1 P4 N3 P3 -68.1(3) . . . . ?
N2 P3 N3 C16 -98.9(5) . . . . ?
C13 P3 N3 C16 7.3(5) . . . . ?
W1 P3 N3 C16 133.1(4) . . . . ?
N2 P3 N3 P4 78.7(3) . . . . ?
C13 P3 N3 P4 -175.1(3) . . . . ?
W1 P3 N3 P4 -49.3(3) . . . . ?
N1 P1 N4 C22 77.0(5) . . . . ?
C1 P1 N4 C22 -34.8(6) . . . . ?
W2 P1 N4 C22 178.9(5) . . . . ?
P4 P1 N4 C22 171.8(6) . . . . ?
P2 P1 N4 C22 118.8(5) . . . . ?
N1 P1 N4 P4 -94.8(2) . . . . ?
C1 P1 N4 P4 153.4(2) . . . . ?
W2 P1 N4 P4 7.1(2) . . . . ?
P2 P1 N4 P4 -53.0(2) . . . . ?
N3 P4 N4 C22 -63.3(5) . . . . ?
C19 P4 N4 C22 48.5(5) . . . . ?
W2 P4 N4 C22 -179.4(4) . . . . ?
P1 P4 N4 C22 -172.6(6) . . . . ?
N3 P4 N4 P1 109.3(2) . . . . ?
C19 P4 N4 P1 -138.9(2) . . . . ?
W2 P4 N4 P1 -6.77(19) . . . . ?
N4 P1 C1 C2 80.7(5) . . . . ?
N1 P1 C1 C2 -36.7(5) . . . . ?
W2 P1 C1 C2 -152.7(3) . . . . ?
P4 P1 C1 C2 107.6(4) . . . . ?
P2 P1 C1 C2 -61.4(6) . . . . ?
P1 C1 C2 C3 21.1(8) . . . . ?
P1 C1 C2 C5 -158.7(4) . . . . ?
C5 C2 C3 C4 -177.3(6) . . . . ?
C1 C2 C3 C4 2.9(10) . . . . ?
C5 C2 C3 C6 1.3(10) . . . . ?
C1 C2 C3 C6 -178.5(6) . . . . ?
P1 N1 C4 C3 -20.5(7) . . . . ?
P2 N1 C4 C3 175.3(4) . . . . ?
C2 C3 C4 N1 -5.1(9) . . . . ?
C6 C3 C4 N1 176.1(5) . . . . ?
N2 P2 C7 C8 -47.1(4) . . . . ?
N1 P2 C7 C8 69.6(4) . . . . ?
W2 P2 C7 C8 -179.3(3) . . . . ?
P1 P2 C7 C8 98.0(4) . . . . ?
P2 C7 C8 C9 27.8(8) . . . . ?
P2 C7 C8 C11 -149.8(5) . . . . ?
C11 C8 C9 C10 179.6(6) . . . . ?
C7 C8 C9 C10 2.2(10) . . . . ?
C11 C8 C9 C12 0.4(10) . . . . ?
C7 C8 C9 C12 -177.0(5) . . . . ?
P2 N2 C10 C9 -27.0(6) . . . . ?
P3 N2 C10 C9 165.7(4) . . . . ?
C8 C9 C10 N2 -4.7(9) . . . . ?
C12 C9 C10 N2 174.6(5) . . . . ?
N3 P3 C13 C14 -43.0(4) . . . . ?
N2 P3 C13 C14 66.8(4) . . . . ?
W1 P3 C13 C14 -165.4(3) . . . . ?
P3 C13 C14 C15 42.5(7) . . . . ?
P3 C13 C14 C17 -139.9(5) . . . . ?
C17 C14 C15 C18 0.9(10) . . . . ?
C13 C14 C15 C18 178.4(6) . . . . ?
C17 C14 C15 C16 -175.1(6) . . . . ?
C13 C14 C15 C16 2.4(9) . . . . ?
P4 N3 C16 C15 -146.3(4) . . . . ?
P3 N3 C16 C15 31.1(8) . . . . ?
C14 C15 C16 N3 -40.6(9) . . . . ?
C18 C15 C16 N3 143.0(6) . . . . ?
N3 P4 C19 C20 78.9(5) . . . . ?
N4 P4 C19 C20 -35.1(5) . . . . ?
W2 P4 C19 C20 -138.9(3) . . . . ?
P1 P4 C19 C20 -65.5(5) . . . . ?
P4 C19 C20 C21 16.0(8) . . . . ?
P4 C19 C20 C23 -166.6(4) . . . . ?
C19 C20 C21 C24 -175.3(6) . . . . ?
C23 C20 C21 C24 7.6(9) . . . . ?
C19 C20 C21 C22 4.0(10) . . . . ?
C23 C20 C21 C22 -173.1(6) . . . . ?
P1 N4 C22 C21 154.2(4) . . . . ?
P4 N4 C22 C21 -35.7(7) . . . . ?
C20 C21 C22 N4 3.5(9) . . . . ?
C24 C21 C22 N4 -177.1(5) . . . . ?
C26 W1 C25 O1 -9(5) . . . . ?
C27 W1 C25 O1 86(5) . . . . ?
C28 W1 C25 O1 -11(6) . . . . ?
P3 W1 C25 O1 -101(5) . . . . ?
W2 W1 C25 O1 -175(5) . . . . ?
C27 W1 C26 O2 176(100) . . . . ?
C25 W1 C26 O2 -97(28) . . . . ?
C28 W1 C26 O2 83(28) . . . . ?
P3 W1 C26 O2 -7(28) . . . . ?
W2 W1 C26 O2 -30(28) . . . . ?
C26 W1 C27 O3 131(10) . . . . ?
C25 W1 C27 O3 47(10) . . . . ?
C28 W1 C27 O3 -141(10) . . . . ?
P3 W1 C27 O3 -19(11) . . . . ?
W2 W1 C27 O3 -42(10) . . . . ?
C26 W1 C28 O4 -4(14) . . . . ?
C27 W1 C28 O4 -99(14) . . . . ?
C25 W1 C28 O4 -2(15) . . . . ?
P3 W1 C28 O4 88(14) . . . . ?
W2 W1 C28 O4 162(14) . . . . ?
C30 W2 C29 O5 175(100) . . . . ?
C31 W2 C29 O5 95(18) . . . . ?
P1 W2 C29 O5 -105(18) . . . . ?
P2 W2 C29 O5 -10(19) . . . . ?
P4 W2 C29 O5 -49(18) . . . . ?
W1 W2 C29 O5 34(18) . . . . ?
C29 W2 C30 O6 102(12) . . . . ?
C31 W2 C30 O6 -160(12) . . . . ?
P1 W2 C30 O6 -16(12) . . . . ?
P2 W2 C30 O6 -77(12) . . . . ?
P4 W2 C30 O6 22(12) . . . . ?
W1 W2 C30 O6 -178(100) . . . . ?
C30 W2 C31 O7 26.9(16) . . . . ?
C29 W2 C31 O7 113.5(16) . . . . ?
P1 W2 C31 O7 -38.4(17) . . . . ?
P2 W2 C31 O7 -77.8(16) . . . . ?
P4 W2 C31 O7 -155.3(14) . . . . ?
W1 W2 C31 O7 -165.7(17) . . . . ?
C57 W3 W4 C62 -176.4(7) . . . . ?
C58 W3 W4 C62 -20.0(4) . . . . ?
C59 W3 W4 C62 71.3(4) . . . . ?
C56 W3 W4 C62 -112.7(4) . . . . ?
P8 W3 W4 C62 155.8(4) . . . . ?
C57 W3 W4 C61 -95.4(6) . . . . ?
C58 W3 W4 C61 61.0(2) . . . . ?
C59 W3 W4 C61 152.3(2) . . . . ?
C56 W3 W4 C61 -31.7(2) . . . . ?
P8 W3 W4 C61 -123.15(16) . . . . ?
C57 W3 W4 C60 164.0(6) . . . . ?
C58 W3 W4 C60 -39.6(3) . . . . ?
C59 W3 W4 C60 51.7(3) . . . . ?
C56 W3 W4 C60 -132.3(3) . . . . ?
P8 W3 W4 C60 136.2(2) . . . . ?
C57 W3 W4 P6 30.9(6) . . . . ?
C58 W3 W4 P6 -172.6(2) . . . . ?
C59 W3 W4 P6 -81.40(16) . . . . ?
C56 W3 W4 P6 94.61(16) . . . . ?
P8 W3 W4 P6 3.17(6) . . . . ?
C57 W3 W4 P7 73.4(6) . . . . ?
C58 W3 W4 P7 -130.22(19) . . . . ?
C59 W3 W4 P7 -38.99(15) . . . . ?
C56 W3 W4 P7 137.03(16) . . . . ?
P8 W3 W4 P7 45.59(5) . . . . ?
C57 W3 W4 P5 -13.7(6) . . . . ?
C58 W3 W4 P5 142.73(19) . . . . ?
C59 W3 W4 P5 -126.03(15) . . . . ?
C56 W3 W4 P5 49.98(16) . . . . ?
P8 W3 W4 P5 -41.46(5) . . . . ?
C62 W4 P5 N5 -162.5(3) . . . . ?
C61 W4 P5 N5 124.4(3) . . . . ?
C60 W4 P5 N5 29.6(4) . . . . ?
P6 W4 P5 N5 -113.38(18) . . . . ?
P7 W4 P5 N5 -50.96(17) . . . . ?
W3 W4 P5 N5 33.20(17) . . . . ?
C62 W4 P5 N6 -44.6(3) . . . . ?
C61 W4 P5 N6 -117.7(3) . . . . ?
C60 W4 P5 N6 147.5(4) . . . . ?
P6 W4 P5 N6 4.48(16) . . . . ?
P7 W4 P5 N6 66.91(16) . . . . ?
W3 W4 P5 N6 151.07(16) . . . . ?
C62 W4 P5 C35 67.5(4) . . . . ?
C61 W4 P5 C35 -5.7(3) . . . . ?
C60 W4 P5 C35 -100.5(4) . . . . ?
P6 W4 P5 C35 116.5(3) . . . . ?
P7 W4 P5 C35 179.0(3) . . . . ?
W3 W4 P5 C35 -96.9(3) . . . . ?
C62 W4 P5 P6 -49.1(3) . . . . ?
C61 W4 P5 P6 -122.2(2) . . . . ?
C60 W4 P5 P6 143.0(3) . . . . ?
P7 W4 P5 P6 62.43(6) . . . . ?
W3 W4 P5 P6 146.58(5) . . . . ?
C62 W4 P6 N6 141.8(3) . . . . ?
C61 W4 P6 N6 62.0(3) . . . . ?
C60 W4 P6 N6 -153.0(3) . . . . ?
P7 W4 P6 N6 -104.38(17) . . . . ?
P5 W4 P6 N6 -4.63(16) . . . . ?
W3 W4 P6 N6 -56.04(18) . . . . ?
C62 W4 P6 N7 -104.7(3) . . . . ?
C61 W4 P6 N7 175.5(3) . . . . ?
C60 W4 P6 N7 -39.4(3) . . . . ?
P7 W4 P6 N7 9.21(16) . . . . ?
P5 W4 P6 N7 108.96(17) . . . . ?
W3 W4 P6 N7 57.55(17) . . . . ?
C62 W4 P6 C41 22.1(4) . . . . ?
C61 W4 P6 C41 -57.7(4) . . . . ?
C60 W4 P6 C41 87.4(4) . . . . ?
P7 W4 P6 C41 136.0(3) . . . . ?
P5 W4 P6 C41 -124.3(3) . . . . ?
W3 W4 P6 C41 -175.7(3) . . . . ?
C62 W4 P6 P7 -113.9(3) . . . . ?
C61 W4 P6 P7 166.3(2) . . . . ?
C60 W4 P6 P7 -48.6(3) . . . . ?
P5 W4 P6 P7 99.75(6) . . . . ?
W3 W4 P6 P7 48.34(6) . . . . ?
C62 W4 P6 P5 146.4(3) . . . . ?
C61 W4 P6 P5 66.6(2) . . . . ?
C60 W4 P6 P5 -148.3(3) . . . . ?
P7 W4 P6 P5 -99.75(6) . . . . ?
W3 W4 P6 P5 -51.41(6) . . . . ?
N5 P5 P6 N6 -89.1(3) . . . . ?
C35 P5 P6 N6 54.5(3) . . . . ?
W4 P5 P6 N6 172.9(3) . . . . ?
N5 P5 P6 N7 10.3(3) . . . . ?
N6 P5 P6 N7 99.4(3) . . . . ?
C35 P5 P6 N7 153.9(3) . . . . ?
W4 P5 P6 N7 -87.73(17) . . . . ?
N5 P5 P6 C41 -135.5(3) . . . . ?
N6 P5 P6 C41 -46.4(4) . . . . ?
C35 P5 P6 C41 8.1(4) . . . . ?
W4 P5 P6 C41 126.5(3) . . . . ?
N5 P5 P6 W4 98.03(18) . . . . ?
N6 P5 P6 W4 -172.9(3) . . . . ?
C35 P5 P6 W4 -118.3(2) . . . . ?
N5 P5 P6 P7 39.14(18) . . . . ?
N6 P5 P6 P7 128.2(2) . . . . ?
C35 P5 P6 P7 -177.2(2) . . . . ?
W4 P5 P6 P7 -58.89(4) . . . . ?
C62 W4 P7 N7 63.4(3) . . . . ?
C61 W4 P7 N7 -92.9(10) . . . . ?
C60 W4 P7 N7 142.2(2) . . . . ?
P6 W4 P7 N7 -9.07(16) . . . . ?
P5 W4 P7 N7 -71.29(16) . . . . ?
W3 W4 P7 N7 -157.21(16) . . . . ?
C62 W4 P7 N8 177.0(3) . . . . ?
C61 W4 P7 N8 20.7(10) . . . . ?
C60 W4 P7 N8 -104.2(2) . . . . ?
P6 W4 P7 N8 104.55(17) . . . . ?
P5 W4 P7 N8 42.33(16) . . . . ?
W3 W4 P7 N8 -43.59(16) . . . . ?
C62 W4 P7 C47 -44.2(4) . . . . ?
C61 W4 P7 C47 159.5(10) . . . . ?
C60 W4 P7 C47 34.6(3) . . . . ?
P6 W4 P7 C47 -116.6(3) . . . . ?
P5 W4 P7 C47 -178.9(3) . . . . ?
W3 W4 P7 C47 95.2(3) . . . . ?
C62 W4 P7 P6 72.5(2) . . . . ?
C61 W4 P7 P6 -83.9(10) . . . . ?
C60 W4 P7 P6 151.27(19) . . . . ?
P5 W4 P7 P6 -62.22(5) . . . . ?
W3 W4 P7 P6 -148.14(4) . . . . ?
N6 P6 P7 N7 -103.1(3) . . . . ?
C41 P6 P7 N7 38.8(4) . . . . ?
W4 P6 P7 N7 165.6(3) . . . . ?
P5 P6 P7 N7 -134.9(3) . . . . ?
N6 P6 P7 N8 -9.1(2) . . . . ?
N7 P6 P7 N8 94.0(3) . . . . ?
C41 P6 P7 N8 132.8(4) . . . . ?
W4 P6 P7 N8 -100.43(17) . . . . ?
P5 P6 P7 N8 -40.91(17) . . . . ?
N6 P6 P7 C47 -148.9(3) . . . . ?
N7 P6 P7 C47 -45.8(4) . . . . ?
C41 P6 P7 C47 -7.1(4) . . . . ?
W4 P6 P7 C47 119.8(3) . . . . ?
P5 P6 P7 C47 179.3(3) . . . . ?
N6 P6 P7 W4 91.32(17) . . . . ?
N7 P6 P7 W4 -165.6(3) . . . . ?
C41 P6 P7 W4 -126.8(3) . . . . ?
P5 P6 P7 W4 59.53(4) . . . . ?
C57 W3 P8 N8 127.7(3) . . . . ?
C58 W3 P8 N8 0(2) . . . . ?
C59 W3 P8 N8 40.1(2) . . . . ?
C56 W3 P8 N8 -146.4(3) . . . . ?
W4 W3 P8 N8 -60.70(17) . . . . ?
C57 W3 P8 N5 -108.2(3) . . . . ?
C58 W3 P8 N5 124(2) . . . . ?
C59 W3 P8 N5 164.2(2) . . . . ?
C56 W3 P8 N5 -22.3(2) . . . . ?
W4 W3 P8 N5 63.43(16) . . . . ?
C57 W3 P8 C50 13.0(3) . . . . ?
C58 W3 P8 C50 -114(2) . . . . ?
C59 W3 P8 C50 -74.6(3) . . . . ?
C56 W3 P8 C50 98.9(3) . . . . ?
W4 W3 P8 C50 -175.4(2) . . . . ?
N6 P5 N5 C32 65.6(5) . . . . ?
C35 P5 N5 C32 -43.9(5) . . . . ?
W4 P5 N5 C32 171.9(4) . . . . ?
P6 P5 N5 C32 108.7(4) . . . . ?
N6 P5 N5 P8 -103.9(3) . . . . ?
C35 P5 N5 P8 146.7(3) . . . . ?
W4 P5 N5 P8 2.5(3) . . . . ?
P6 P5 N5 P8 -60.7(3) . . . . ?
N8 P8 N5 C32 -94.6(5) . . . . ?
C50 P8 N5 C32 8.3(5) . . . . ?
W3 P8 N5 C32 136.6(4) . . . . ?
N8 P8 N5 P5 74.4(3) . . . . ?
C50 P8 N5 P5 177.2(3) . . . . ?
W3 P8 N5 P5 -54.5(3) . . . . ?
N7 P6 N6 C38 79.5(5) . . . . ?
C41 P6 N6 C38 -36.1(5) . . . . ?
W4 P6 N6 C38 -177.6(4) . . . . ?
P7 P6 N6 C38 121.4(4) . . . . ?
P5 P6 N6 C38 176.1(6) . . . . ?
N7 P6 N6 P5 -96.6(3) . . . . ?
C41 P6 N6 P5 147.9(3) . . . . ?
W4 P6 N6 P5 6.3(2) . . . . ?
P7 P6 N6 P5 -54.7(2) . . . . ?
N5 P5 N6 C38 -64.1(6) . . . . ?
C35 P5 N6 C38 44.0(6) . . . . ?
W4 P5 N6 C38 178.5(5) . . . . ?
P6 P5 N6 C38 -175.6(7) . . . . ?
N5 P5 N6 P6 111.5(2) . . . . ?
C35 P5 N6 P6 -140.4(2) . . . . ?
W4 P5 N6 P6 -5.9(2) . . . . ?
N6 P6 N7 C44 -81.5(5) . . . . ?
C41 P6 N7 C44 30.6(6) . . . . ?
W4 P6 N7 C44 174.6(5) . . . . ?
P7 P6 N7 C44 -172.9(7) . . . . ?
P5 P6 N7 C44 -124.3(5) . . . . ?
N6 P6 N7 P7 91.4(3) . . . . ?
C41 P6 N7 P7 -156.5(2) . . . . ?
W4 P6 N7 P7 -12.5(2) . . . . ?
P5 P6 N7 P7 48.6(2) . . . . ?
N8 P7 N7 C44 71.3(5) . . . . ?
C47 P7 N7 C44 -40.2(5) . . . . ?
W4 P7 N7 C44 -174.5(4) . . . . ?
P6 P7 N7 C44 173.5(6) . . . . ?
N8 P7 N7 P6 -102.2(3) . . . . ?
C47 P7 N7 P6 146.3(3) . . . . ?
W4 P7 N7 P6 12.0(2) . . . . ?
N7 P7 N8 C53 -45.0(5) . . . . ?
C47 P7 N8 C53 62.0(5) . . . . ?
W4 P7 N8 C53 -148.6(4) . . . . ?
P6 P7 N8 C53 -87.2(5) . . . . ?
N7 P7 N8 P8 114.8(3) . . . . ?
C47 P7 N8 P8 -138.2(3) . . . . ?
W4 P7 N8 P8 11.3(3) . . . . ?
P6 P7 N8 P8 72.7(3) . . . . ?
N5 P8 N8 C53 74.1(5) . . . . ?
C50 P8 N8 C53 -32.5(5) . . . . ?
W3 P8 N8 C53 -157.4(5) . . . . ?
N5 P8 N8 P7 -85.1(3) . . . . ?
C50 P8 N8 P7 168.3(3) . . . . ?
W3 P8 N8 P7 43.3(3) . . . . ?
P5 N5 C32 C33 28.0(7) . . . . ?
P8 N5 C32 C33 -164.2(4) . . . . ?
N5 C32 C33 C34 -3.5(9) . . . . ?
N5 C32 C33 C36 179.8(5) . . . . ?
C32 C33 C34 C37 -174.4(6) . . . . ?
C36 C33 C34 C37 1.8(10) . . . . ?
C32 C33 C34 C35 5.3(9) . . . . ?
C36 C33 C34 C35 -178.5(5) . . . . ?
C33 C34 C35 P5 -27.3(7) . . . . ?
C37 C34 C35 P5 152.4(4) . . . . ?
N5 P5 C35 C34 41.3(5) . . . . ?
N6 P5 C35 C34 -76.0(5) . . . . ?
W4 P5 C35 C34 175.4(3) . . . . ?
P6 P5 C35 C34 -107.6(4) . . . . ?
P6 N6 C38 C39 17.6(7) . . . . ?
P5 N6 C38 C39 -167.7(4) . . . . ?
N6 C38 C39 C40 4.4(9) . . . . ?
N6 C38 C39 C42 -176.8(5) . . . . ?
C38 C39 C40 C41 1.5(10) . . . . ?
C42 C39 C40 C41 -177.2(6) . . . . ?
C38 C39 C40 C43 177.9(6) . . . . ?
C42 C39 C40 C43 -0.7(9) . . . . ?
C39 C40 C41 P6 -25.0(8) . . . . ?
C43 C40 C41 P6 158.3(4) . . . . ?
N6 P6 C41 C40 36.9(5) . . . . ?
N7 P6 C41 C40 -81.0(5) . . . . ?
W4 P6 C41 C40 155.6(3) . . . . ?
P7 P6 C41 C40 -105.9(5) . . . . ?
P5 P6 C41 C40 65.3(6) . . . . ?
P6 N7 C44 C45 -167.9(4) . . . . ?
P7 N7 C44 C45 20.7(8) . . . . ?
N7 C44 C45 C46 5.7(9) . . . . ?
N7 C44 C45 C48 -174.9(5) . . . . ?
C48 C45 C46 C49 -5.0(10) . . . . ?
C44 C45 C46 C49 174.3(6) . . . . ?
C48 C45 C46 C47 179.3(6) . . . . ?
C44 C45 C46 C47 -1.3(10) . . . . ?
C45 C46 C47 P7 -24.9(8) . . . . ?
C49 C46 C47 P7 159.1(5) . . . . ?
N7 P7 C47 C46 38.9(5) . . . . ?
N8 P7 C47 C46 -75.5(5) . . . . ?
W4 P7 C47 C46 144.5(3) . . . . ?
P6 P7 C47 C46 66.3(5) . . . . ?
N8 P8 C50 C51 45.7(4) . . . . ?
N5 P8 C50 C51 -63.3(5) . . . . ?
W3 P8 C50 C51 169.6(3) . . . . ?
P8 C50 C51 C52 -35.1(7) . . . . ?
P8 C50 C51 C54 145.2(5) . . . . ?
C54 C51 C52 C53 -179.4(6) . . . . ?
C50 C51 C52 C53 1.0(10) . . . . ?
C54 C51 C52 C55 1.2(10) . . . . ?
C50 C51 C52 C55 -178.5(5) . . . . ?
P7 N8 C53 C52 164.7(5) . . . . ?
P8 N8 C53 C52 6.9(9) . . . . ?
C51 C52 C53 N8 15.2(10) . . . . ?
C55 C52 C53 N8 -165.3(6) . . . . ?
C57 W3 C56 O8 20(11) . . . . ?
C58 W3 C56 O8 113(11) . . . . ?
C59 W3 C56 O8 2(12) . . . . ?
P8 W3 C56 O8 -69(11) . . . . ?
W4 W3 C56 O8 -143(11) . . . . ?
C58 W3 C57 O9 -160(18) . . . . ?
C59 W3 C57 O9 111(18) . . . . ?
C56 W3 C57 O9 -67(18) . . . . ?
P8 W3 C57 O9 24(18) . . . . ?
W4 W3 C57 O9 -3(18) . . . . ?
C57 W3 C58 O10 -100(12) . . . . ?
C59 W3 C58 O10 -12(11) . . . . ?
C56 W3 C58 O10 174(11) . . . . ?
P8 W3 C58 O10 28(13) . . . . ?
W4 W3 C58 O10 88(12) . . . . ?
C57 W3 C59 O11 -1(5) . . . . ?
C58 W3 C59 O11 -94(5) . . . . ?
C56 W3 C59 O11 18(6) . . . . ?
P8 W3 C59 O11 89(5) . . . . ?
W4 W3 C59 O11 162(5) . . . . ?
C62 W4 C60 O12 26.6(17) . . . . ?
C61 W4 C60 O12 108.4(18) . . . . ?
P6 W4 C60 O12 -39.6(19) . . . . ?
P7 W4 C60 O12 -82.0(18) . . . . ?
P5 W4 C60 O12 -162.3(15) . . . . ?
W3 W4 C60 O12 -166.4(18) . . . . ?
C62 W4 C61 O13 -143(20) . . . . ?
C60 W4 C61 O13 138(20) . . . . ?
P6 W4 C61 O13 -63(20) . . . . ?
P7 W4 C61 O13 15(21) . . . . ?
P5 W4 C61 O13 -7(20) . . . . ?
W3 W4 C61 O13 78(20) . . . . ?
C61 W4 C62 O14 68(22) . . . . ?
C60 W4 C62 O14 168(22) . . . . ?
P6 W4 C62 O14 -48(22) . . . . ?
P7 W4 C62 O14 -107(22) . . . . ?
P5 W4 C62 O14 -5(22) . . . . ?
W3 W4 C62 O14 151(22) . . . . ?
_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full 32.50
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max 2.302
_refine_diff_density_min -1.953
_refine_diff_density_rms 0.229
_database_code_depnum_ccdc_archive 'CCDC 956164'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_ch157_[Mo(C2H5CN)3(CO)3]
_audit_creation_method SHELXL-97
#==============================================================================
# CHEMICAL DATA
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C12 H15 Mo N3 O3'
_chemical_formula_sum 'C12 H15 Mo N3 O3'
_chemical_formula_weight 345.21
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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
#==============================================================================
# CRYSTAL DATA
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/m'
_symmetry_space_group_name_Hall '-P 2yb'
_symmetry_Int_Tables_number 11
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
_cell_length_a 5.9362(2)
_cell_length_b 13.8472(5)
_cell_length_c 9.4000(3)
_cell_angle_alpha 90.00
_cell_angle_beta 97.888(2)
_cell_angle_gamma 90.00
_cell_volume 765.37(5)
_cell_formula_units_Z 2
_cell_measurement_temperature 173(2)
_cell_measurement_reflns_used 6097
_cell_measurement_theta_min 4.375
_cell_measurement_theta_max 66.072
_exptl_crystal_description plate
_exptl_crystal_colour yellow
_exptl_crystal_size_max 0.18
_exptl_crystal_size_mid 0.09
_exptl_crystal_size_min 0.03
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.498
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 348
_exptl_absorpt_coefficient_mu 0.863
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.8601
_exptl_absorpt_correction_T_max 0.9746
_exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)'
#==============================================================================
# EXPERIMENTAL DATA
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 173(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker Apex Kappa II-CCD-diffractometer'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 14262
_diffrn_reflns_av_R_equivalents 0.0411
_diffrn_reflns_av_sigmaI/netI 0.0344
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_k_min -20
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_theta_min 2.19
_diffrn_reflns_theta_max 32.50
_reflns_number_total 2862
_reflns_number_gt 2611
_reflns_threshold_expression >2\s(I)
_computing_data_collection 'Bruker Apex V7.51A'
_computing_cell_refinement 'Bruker Apex V7.51A'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material SHELXL-97
#==============================================================================
# REFINEMENT DATA
_refine_special_details
;
All H atoms
were positioned geometrically and refined using a riding model, with C---H =
0.98 (methyl groups), 0.99\%A (methylene groups), 1.00\%A (methine groups) or
0.95 \%A (aryl CH) and with U~iso~(H) = 1.5 times U~eq~(C)
(methyl groups) or with U~iso~(H) = 1.2 times U~eq~(C)
(methylene groups, aryl CH, methine groups). Torsion angles of all methyl
groups were allowed to refine.
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0130P)^2^+0.1749P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 2862
_refine_ls_number_parameters 102
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0276
_refine_ls_R_factor_gt 0.0231
_refine_ls_wR_factor_ref 0.0478
_refine_ls_wR_factor_gt 0.0460
_refine_ls_goodness_of_fit_ref 1.059
_refine_ls_restrained_S_all 1.059
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
#==============================================================================
# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_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
Mo1 Mo 0.86420(2) 0.2500 -0.000358(14) 0.01484(4) Uani 1 2 d S . .
N1 N 0.6637(3) 0.2500 0.18221(16) 0.0242(3) Uani 1 2 d S . .
N2 N 0.60406(19) 0.14430(8) -0.09416(11) 0.0227(2) Uani 1 1 d . . .
O1 O 1.20381(18) 0.09652(8) 0.14196(11) 0.0340(2) Uani 1 1 d . . .
O2 O 1.1191(3) 0.2500 -0.26718(15) 0.0343(3) Uani 1 2 d S . .
C1 C 1.0749(2) 0.15392(10) 0.08731(13) 0.0227(2) Uani 1 1 d . . .
C2 C 1.0231(3) 0.2500 -0.16635(18) 0.0230(3) Uani 1 2 d S . .
C3 C 0.5591(3) 0.2500 0.27520(19) 0.0261(4) Uani 1 2 d S . .
C4 C 0.4326(5) 0.2411(16) 0.3978(2) 0.031(2) Uani 0.50 1 d P . .
H4A H 0.3547 0.1778 0.3936 0.038 Uiso 0.50 1 calc PR . .
H4B H 0.3148 0.2921 0.3919 0.038 Uiso 0.50 1 calc PR . .
C5 C 0.5882(4) 0.2500 0.5407(2) 0.0430(6) Uani 1 2 d S . .
H5A H 0.7025 0.1986 0.5481 0.064 Uiso 0.50 1 calc PR . .
H5B H 0.4976 0.2442 0.6199 0.064 Uiso 0.50 1 calc PR . .
H5C H 0.6642 0.3130 0.5457 0.064 Uiso 0.50 1 calc PR . .
C6 C 0.4644(2) 0.09131(9) -0.13817(13) 0.0228(2) Uani 1 1 d . . .
C7 C 0.2864(2) 0.02265(10) -0.19318(14) 0.0290(3) Uani 1 1 d . . .
H7A H 0.1389 0.0456 -0.1681 0.035 Uiso 1 1 calc R . .
H7B H 0.3197 -0.0406 -0.1459 0.035 Uiso 1 1 calc R . .
C8 C 0.2668(4) 0.00962(14) -0.35392(18) 0.0550(5) Uani 1 1 d . . .
H8A H 0.2219 0.0709 -0.4016 0.083 Uiso 1 1 calc R . .
H8B H 0.1517 -0.0396 -0.3847 0.083 Uiso 1 1 calc R . .
H8C H 0.4139 -0.0109 -0.3797 0.083 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.01279(7) 0.01540(7) 0.01628(6) 0.000 0.00179(4) 0.000
N1 0.0235(8) 0.0246(8) 0.0237(7) 0.000 0.0008(6) 0.000
N2 0.0222(6) 0.0230(5) 0.0226(5) 0.0012(4) 0.0024(4) 0.0015(4)
O1 0.0285(6) 0.0299(6) 0.0420(6) 0.0062(4) -0.0010(4) 0.0052(4)
O2 0.0295(8) 0.0453(9) 0.0297(7) 0.000 0.0091(6) 0.000
C1 0.0209(6) 0.0230(6) 0.0242(5) -0.0012(4) 0.0037(4) -0.0043(5)
C2 0.0214(9) 0.0225(9) 0.0243(8) 0.000 0.0001(6) 0.000
C3 0.0253(10) 0.0294(10) 0.0232(8) 0.000 0.0020(6) 0.000
C4 0.0301(11) 0.042(6) 0.0241(9) 0.004(2) 0.0106(7) 0.001(2)
C5 0.0490(15) 0.0585(16) 0.0217(9) 0.000 0.0057(8) 0.000
C6 0.0246(7) 0.0223(6) 0.0212(5) 0.0019(4) 0.0020(4) 0.0007(5)
C7 0.0292(7) 0.0262(7) 0.0301(6) 0.0000(5) -0.0015(5) -0.0075(5)
C8 0.0755(15) 0.0528(12) 0.0329(8) -0.0092(7) -0.0066(8) -0.0208(10)
#==============================================================================
# MOLECULAR GEOMETRY
_geom_special_details
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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
Mo1 C2 1.9307(19) . ?
Mo1 C1 1.9315(13) 4_565 ?
Mo1 C1 1.9315(13) . ?
Mo1 N1 2.2185(16) . ?
Mo1 N2 2.2206(11) . ?
Mo1 N2 2.2205(11) 4_565 ?
N1 C3 1.140(2) . ?
N2 C6 1.1414(16) . ?
O1 C1 1.1719(16) . ?
O2 C2 1.171(2) . ?
C3 C4 1.465(4) 4_565 ?
C3 C4 1.465(4) . ?
C4 C5 1.526(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.4620(18) . ?
C7 C8 1.510(2) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Mo1 C1 89.16(5) . 4_565 ?
C2 Mo1 C1 89.16(5) . . ?
C1 Mo1 C1 87.08(7) 4_565 . ?
C2 Mo1 N1 176.84(6) . . ?
C1 Mo1 N1 93.13(5) 4_565 . ?
C1 Mo1 N1 93.13(5) . . ?
C2 Mo1 N2 93.97(5) . . ?
C1 Mo1 N2 176.18(5) 4_565 . ?
C1 Mo1 N2 95.14(5) . . ?
N1 Mo1 N2 83.66(4) . . ?
C2 Mo1 N2 93.97(5) . 4_565 ?
C1 Mo1 N2 95.14(5) 4_565 4_565 ?
C1 Mo1 N2 176.18(5) . 4_565 ?
N1 Mo1 N2 83.66(4) . 4_565 ?
N2 Mo1 N2 82.47(5) . 4_565 ?
C3 N1 Mo1 179.43(15) . . ?
C6 N2 Mo1 177.01(11) . . ?
O1 C1 Mo1 179.07(11) . . ?
O2 C2 Mo1 179.91(16) . . ?
N1 C3 C4 174.8(8) . 4_565 ?
N1 C3 C4 174.8(8) . . ?
C4 C3 C4 9.6(17) 4_565 . ?
C3 C4 C5 111.8(3) . . ?
C3 C4 H4A 109.3 . . ?
C5 C4 H4A 109.3 . . ?
C3 C4 H4B 109.3 . . ?
C5 C4 H4B 109.3 . . ?
H4A C4 H4B 107.9 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N2 C6 C7 179.32(14) . . ?
C6 C7 C8 112.61(13) . . ?
C6 C7 H7A 109.1 . . ?
C8 C7 H7A 109.1 . . ?
C6 C7 H7B 109.1 . . ?
C8 C7 H7B 109.1 . . ?
H7A C7 H7B 107.8 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 Mo1 N1 C3 0.00(2) . . . . ?
C1 Mo1 N1 C3 136.38(4) 4_565 . . . ?
C1 Mo1 N1 C3 -136.38(4) . . . . ?
N2 Mo1 N1 C3 -41.54(4) . . . . ?
N2 Mo1 N1 C3 41.55(4) 4_565 . . . ?
C2 Mo1 N2 C6 -160.3(19) . . . . ?
C1 Mo1 N2 C6 -15(2) 4_565 . . . ?
C1 Mo1 N2 C6 110.2(19) . . . . ?
N1 Mo1 N2 C6 17.6(19) . . . . ?
N2 Mo1 N2 C6 -66.8(19) 4_565 . . . ?
C2 Mo1 C1 O1 115(8) . . . . ?
C1 Mo1 C1 O1 26(8) 4_565 . . . ?
N1 Mo1 C1 O1 -67(8) . . . . ?
N2 Mo1 C1 O1 -151(8) . . . . ?
N2 Mo1 C1 O1 -99(8) 4_565 . . . ?
C1 Mo1 C2 O2 -136.5(3) 4_565 . . . ?
C1 Mo1 C2 O2 136.5(3) . . . . ?
N1 Mo1 C2 O2 0.0(3) . . . . ?
N2 Mo1 C2 O2 41.4(3) . . . . ?
N2 Mo1 C2 O2 -41.4(3) 4_565 . . . ?
Mo1 N1 C3 C4 -113(4) . . . 4_565 ?
Mo1 N1 C3 C4 113(4) . . . . ?
N1 C3 C4 C5 74(5) . . . . ?
C4 C3 C4 C5 -83.1(12) 4_565 . . . ?
Mo1 N2 C6 C7 -83(14) . . . . ?
N2 C6 C7 C8 -134(14) . . . . ?
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full 32.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max 0.407
_refine_diff_density_min -0.405
_refine_diff_density_rms 0.074
_database_code_depnum_ccdc_archive 'CCDC 956165'