Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2003

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

loop_
_publ_author_name
'Dante Neculai'
'Ana Mirela Neculai'
'Herbert W. Roesky'
'Regine Herbst-Irmer'

_publ_contact_author_name        'Prof Herbert W Roesky'
_publ_contact_author_address     
;
Institut fuer Anorganische Chemie
Georg August Universitaet
Tammannstr. 4
Goettingen
D- 37077
GERMANY
;

_publ_contact_author_email       HROESKY@GWDG.DE

_publ_section_title              
;
Vanadium complexes incorporating the b-diketiminato
ligand L. Syntheses and structures of LV(OSO2CF3)2 and LVPPh2
;

data_2
_database_code_CSD               206412

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H51 F6 N4 O6 S2 V'
_chemical_formula_weight         828.84

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   15.329(2)
_cell_length_b                   13.388(2)
_cell_length_c                   19.652(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.774(3)
_cell_angle_gamma                90.00
_cell_volume                     3995.8(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9666
_cell_measurement_theta_min      2.16
_cell_measurement_theta_max      28.17

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1736
_exptl_absorpt_coefficient_mu    0.426
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8480
_exptl_absorpt_correction_T_max  0.9586
_exptl_absorpt_process_details   sadabs2

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            30036
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.34
_diffrn_reflns_theta_max         28.22
_reflns_number_total             9058
_reflns_number_gt                6850
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART-NT V5.6'
_computing_cell_refinement       'SAINT-NT V5/6.0'
_computing_data_reduction        'SAINT-NT V5/6.0'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP in SHELXTL-97'
_computing_publication_material  'XP in SHELXTL-97'

_refine_special_details          
;
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^ > 2sigma(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^)+(0.0740P)^2^+1.6935P] 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_number_reflns         9058
_refine_ls_number_parameters     477
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0514
_refine_ls_wR_factor_ref         0.1392
_refine_ls_wR_factor_gt          0.1273
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.17187(2) 0.93504(3) 0.327204(19) 0.02805(11) Uani 1 1 d . . .
C1 C 0.0058(2) 1.1565(2) 0.41511(16) 0.0570(7) Uani 1 1 d . . .
H1A H 0.0544 1.1901 0.4438 0.085 Uiso 1 1 calc R . .
H1B H -0.0422 1.1440 0.4423 0.085 Uiso 1 1 calc R . .
H1C H -0.0156 1.1991 0.3758 0.085 Uiso 1 1 calc R . .
C2 C 0.03785(16) 1.05840(18) 0.38965(12) 0.0391(5) Uani 1 1 d . . .
C3 C -0.01186(16) 0.9734(2) 0.40034(13) 0.0447(6) Uani 1 1 d . . .
H3 H -0.0631 0.9840 0.4218 0.054 Uiso 1 1 calc R . .
C4 C 0.00553(15) 0.87408(19) 0.38290(12) 0.0391(5) Uani 1 1 d . . .
C5 C -0.06295(18) 0.7970(2) 0.39490(16) 0.0573(7) Uani 1 1 d . . .
H5A H -0.0836 0.7628 0.3516 0.086 Uiso 1 1 calc R . .
H5B H -0.1127 0.8302 0.4120 0.086 Uiso 1 1 calc R . .
H5C H -0.0369 0.7482 0.4289 0.086 Uiso 1 1 calc R . .
N1 N 0.10877(13) 1.05506(13) 0.35779(10) 0.0351(4) Uani 1 1 d . . .
C6 C 0.14885(18) 1.15185(18) 0.34342(16) 0.0507(7) Uani 1 1 d . . .
H6A H 0.1883 1.1746 0.3846 0.061 Uiso 1 1 calc R . .
H6B H 0.1021 1.2026 0.3324 0.061 Uiso 1 1 calc R . .
C7 C 0.20074(17) 1.14117(18) 0.28376(14) 0.0452(6) Uani 1 1 d . . .
H7A H 0.1601 1.1273 0.2413 0.054 Uiso 1 1 calc R . .
H7B H 0.2319 1.2045 0.2772 0.054 Uiso 1 1 calc R . .
N2 N 0.26594(12) 1.05822(13) 0.29667(10) 0.0334(4) Uani 1 1 d . . .
C8 C 0.33673(17) 1.09072(19) 0.35211(13) 0.0433(6) Uani 1 1 d . . .
H8A H 0.3118 1.0929 0.3960 0.052 Uiso 1 1 calc R . .
H8B H 0.3547 1.1595 0.3418 0.052 Uiso 1 1 calc R . .
C9 C 0.41794(17) 1.0254(2) 0.36171(16) 0.0568(7) Uani 1 1 d . . .
H9A H 0.4007 0.9559 0.3679 0.085 Uiso 1 1 calc R . .
H9B H 0.4573 1.0475 0.4024 0.085 Uiso 1 1 calc R . .
H9C H 0.4484 1.0305 0.3211 0.085 Uiso 1 1 calc R . .
C10 C 0.30383(19) 1.0402(2) 0.23085(13) 0.0473(6) Uani 1 1 d . . .
H10A H 0.2550 1.0221 0.1947 0.057 Uiso 1 1 calc R . .
H10B H 0.3438 0.9819 0.2377 0.057 Uiso 1 1 calc R . .
C11 C 0.3542(2) 1.1267(2) 0.20474(16) 0.0662(9) Uani 1 1 d . . .
H11A H 0.3147 1.1841 0.1952 0.099 Uiso 1 1 calc R . .
H11B H 0.3769 1.1068 0.1625 0.099 Uiso 1 1 calc R . .
H11C H 0.4034 1.1452 0.2397 0.099 Uiso 1 1 calc R . .
N3 N 0.07820(12) 0.84744(14) 0.35780(10) 0.0341(4) Uani 1 1 d . . .
C12 C 0.09128(17) 0.73961(18) 0.34644(15) 0.0473(6) Uani 1 1 d . . .
H12A H 0.0589 0.7197 0.3014 0.057 Uiso 1 1 calc R . .
H12B H 0.0676 0.7006 0.3826 0.057 Uiso 1 1 calc R . .
C13 C 0.18764(17) 0.71752(17) 0.34794(14) 0.0440(6) Uani 1 1 d . . .
H13A H 0.2184 0.7293 0.3949 0.053 Uiso 1 1 calc R . .
H13B H 0.1952 0.6462 0.3366 0.053 Uiso 1 1 calc R . .
N4 N 0.22859(12) 0.78102(13) 0.29823(10) 0.0351(4) Uani 1 1 d . . .
C14 C 0.19767(17) 0.74205(18) 0.22734(13) 0.0439(6) Uani 1 1 d . . .
H14A H 0.1335 0.7538 0.2170 0.053 Uiso 1 1 calc R . .
H14B H 0.2072 0.6689 0.2273 0.053 Uiso 1 1 calc R . .
C15 C 0.24186(19) 0.7875(2) 0.17046(14) 0.0517(7) Uani 1 1 d . . .
H15A H 0.2349 0.8602 0.1709 0.078 Uiso 1 1 calc R . .
H15B H 0.2147 0.7610 0.1261 0.078 Uiso 1 1 calc R . .
H15C H 0.3046 0.7706 0.1775 0.078 Uiso 1 1 calc R . .
C16 C 0.32653(15) 0.77397(18) 0.31418(13) 0.0413(6) Uani 1 1 d . . .
H16A H 0.3438 0.7976 0.3618 0.050 Uiso 1 1 calc R . .
H16B H 0.3527 0.8205 0.2834 0.050 Uiso 1 1 calc R . .
C17 C 0.36726(19) 0.6707(2) 0.30742(17) 0.0579(8) Uani 1 1 d . . .
H17A H 0.3447 0.6243 0.3395 0.087 Uiso 1 1 calc R . .
H17B H 0.4315 0.6753 0.3181 0.087 Uiso 1 1 calc R . .
H17C H 0.3517 0.6462 0.2603 0.087 Uiso 1 1 calc R . .
O1 O 0.25431(10) 0.91996(11) 0.41855(8) 0.0329(3) Uani 1 1 d . . .
S1 S 0.23847(4) 0.92063(5) 0.49084(3) 0.03996(16) Uani 1 1 d . . .
O2 O 0.18897(14) 0.83755(19) 0.50903(10) 0.0732(7) Uani 1 1 d . . .
O3 O 0.21591(17) 1.01556(18) 0.51499(11) 0.0765(7) Uani 1 1 d . . .
C18 C 0.34913(18) 0.8959(3) 0.53247(14) 0.0560(7) Uani 1 1 d . . .
F1 F 0.35275(12) 0.89213(15) 0.60020(8) 0.0702(5) Uani 1 1 d . . .
F2 F 0.40186(14) 0.9700(2) 0.51905(11) 0.1152(10) Uani 1 1 d . . .
F3 F 0.37983(17) 0.8135(2) 0.51231(12) 0.1205(11) Uani 1 1 d . . .
O4 O 0.11319(10) 0.94475(11) 0.22653(8) 0.0348(4) Uani 1 1 d . . .
S2 S 0.01903(4) 0.94875(4) 0.19766(3) 0.03652(15) Uani 1 1 d . . .
O5 O -0.02466(11) 0.85464(13) 0.19993(10) 0.0486(4) Uani 1 1 d . . .
O6 O -0.02572(12) 1.03572(13) 0.21693(10) 0.0508(5) Uani 1 1 d . . .
C19 C 0.0284(2) 0.9677(2) 0.10673(14) 0.0520(7) Uani 1 1 d . . .
F4 F 0.07552(15) 1.04816(13) 0.09767(9) 0.0744(6) Uani 1 1 d . . .
F5 F 0.06607(13) 0.89057(13) 0.08023(8) 0.0659(5) Uani 1 1 d . . .
F6 F -0.05110(14) 0.98050(19) 0.07159(10) 0.0898(7) Uani 1 1 d . . .
C20 C 0.4916(2) 0.3539(3) 0.3215(2) 0.0894(12) Uani 1 1 d . . .
H20A H 0.5275 0.4145 0.3290 0.134 Uiso 1 1 calc R . .
H20B H 0.5158 0.3109 0.2883 0.134 Uiso 1 1 calc R . .
H20C H 0.4922 0.3182 0.3650 0.134 Uiso 1 1 calc R . .
C21 C 0.39843(19) 0.3820(2) 0.29388(16) 0.0535(7) Uani 1 1 d . . .
C22 C 0.33499(19) 0.3903(2) 0.33716(15) 0.0506(6) Uani 1 1 d . . .
H22 H 0.3507 0.3784 0.3849 0.061 Uiso 1 1 calc R . .
C23 C 0.24892(19) 0.4155(2) 0.31242(17) 0.0544(7) Uani 1 1 d . . .
H23 H 0.2065 0.4213 0.3433 0.065 Uiso 1 1 calc R . .
C24 C 0.2247(2) 0.4323(2) 0.24399(18) 0.0627(8) Uani 1 1 d . . .
H24 H 0.1655 0.4490 0.2272 0.075 Uiso 1 1 calc R . .
C25 C 0.2854(3) 0.4249(2) 0.19978(17) 0.0685(9) Uani 1 1 d . . .
H25 H 0.2684 0.4369 0.1522 0.082 Uiso 1 1 calc R . .
C26 C 0.3725(2) 0.3998(3) 0.22396(17) 0.0676(9) Uani 1 1 d . . .
H26 H 0.4144 0.3948 0.1927 0.081 Uiso 1 1 calc R . .
C27 C 0.2749(4) -0.0419(4) 0.0107(3) 0.127(2) Uani 1 1 d . . .
H27A H 0.2204 -0.0423 0.0317 0.190 Uiso 1 1 calc R . .
H27B H 0.3159 -0.0914 0.0337 0.190 Uiso 1 1 calc R . .
H27C H 0.2616 -0.0585 -0.0381 0.190 Uiso 1 1 calc R . .
C28 C 0.3148(3) 0.0568(3) 0.01812(17) 0.0777(11) Uani 1 1 d . . .
C29 C 0.2608(3) 0.1424(3) 0.01397(17) 0.0751(10) Uani 1 1 d . . .
H29 H 0.1986 0.1352 0.0068 0.090 Uiso 1 1 calc R . .
C30 C 0.2964(3) 0.2335(3) 0.02000(18) 0.0860(12) Uani 1 1 d . . .
H30 H 0.2590 0.2903 0.0172 0.103 Uiso 1 1 calc R . .
C31 C 0.3886(4) 0.2473(4) 0.0305(2) 0.1035(15) Uani 1 1 d . . .
H31 H 0.4136 0.3123 0.0350 0.124 Uiso 1 1 calc R . .
C32 C 0.4394(3) 0.1661(5) 0.0338(2) 0.1042(16) Uani 1 1 d . . .
H32 H 0.5016 0.1739 0.0399 0.125 Uiso 1 1 calc R . .
C33 C 0.4050(3) 0.0727(3) 0.02868(17) 0.0749(10) Uani 1 1 d . . .
H33 H 0.4435 0.0169 0.0324 0.090 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
V1 0.0311(2) 0.02477(18) 0.0275(2) -0.00125(14) 0.00111(14) -0.00039(14)
C1 0.0652(18) 0.0509(16) 0.0583(18) -0.0004(13) 0.0213(15) 0.0197(14)
C2 0.0426(13) 0.0434(13) 0.0308(12) 0.0004(10) 0.0026(10) 0.0125(10)
C3 0.0396(13) 0.0539(15) 0.0435(15) 0.0046(12) 0.0160(11) 0.0064(11)
C4 0.0364(12) 0.0470(14) 0.0336(12) 0.0043(10) 0.0041(10) -0.0049(10)
C5 0.0482(15) 0.0635(18) 0.0630(19) 0.0017(15) 0.0171(14) -0.0149(13)
N1 0.0364(10) 0.0310(9) 0.0369(11) -0.0019(8) 0.0015(8) 0.0044(8)
C6 0.0510(15) 0.0293(12) 0.073(2) -0.0067(12) 0.0113(14) 0.0043(11)
C7 0.0525(15) 0.0288(11) 0.0521(16) 0.0043(11) -0.0007(12) -0.0039(10)
N2 0.0347(10) 0.0321(9) 0.0329(10) -0.0006(8) 0.0020(8) -0.0042(8)
C8 0.0470(14) 0.0449(13) 0.0368(13) -0.0024(11) 0.0019(11) -0.0127(11)
C9 0.0389(14) 0.075(2) 0.0548(17) 0.0000(15) -0.0006(12) -0.0075(13)
C10 0.0591(16) 0.0480(14) 0.0366(14) -0.0064(11) 0.0127(12) -0.0112(12)
C11 0.090(2) 0.068(2) 0.0444(17) -0.0011(15) 0.0232(16) -0.0258(17)
N3 0.0376(10) 0.0308(9) 0.0335(10) 0.0004(8) 0.0033(8) -0.0059(8)
C12 0.0536(15) 0.0304(12) 0.0593(17) -0.0005(11) 0.0128(13) -0.0102(11)
C13 0.0560(15) 0.0251(11) 0.0503(15) 0.0019(10) 0.0051(12) 0.0004(10)
N4 0.0385(10) 0.0294(9) 0.0363(11) -0.0038(8) 0.0015(8) 0.0016(8)
C14 0.0503(14) 0.0318(12) 0.0467(15) -0.0131(11) -0.0041(11) 0.0032(10)
C15 0.0609(17) 0.0533(16) 0.0403(15) -0.0159(12) 0.0049(12) 0.0053(13)
C16 0.0398(13) 0.0376(13) 0.0451(14) -0.0064(11) 0.0007(11) 0.0060(10)
C17 0.0521(16) 0.0476(16) 0.071(2) -0.0091(14) -0.0020(14) 0.0153(13)
O1 0.0346(8) 0.0345(8) 0.0293(8) 0.0009(6) 0.0026(6) -0.0004(6)
S1 0.0419(3) 0.0488(4) 0.0288(3) 0.0027(2) 0.0034(2) 0.0027(3)
O2 0.0646(13) 0.1094(19) 0.0436(12) 0.0252(12) 0.0005(10) -0.0338(13)
O3 0.1076(19) 0.0768(15) 0.0429(12) -0.0115(11) 0.0025(11) 0.0357(14)
C18 0.0465(15) 0.083(2) 0.0357(15) 0.0115(14) -0.0052(12) -0.0025(15)
F1 0.0761(12) 0.0939(14) 0.0352(9) 0.0158(9) -0.0123(8) -0.0113(10)
F2 0.0671(13) 0.192(3) 0.0761(14) 0.0580(16) -0.0278(11) -0.0626(15)
F3 0.1165(19) 0.158(2) 0.0764(15) -0.0146(15) -0.0253(13) 0.0960(18)
O4 0.0378(8) 0.0329(8) 0.0319(8) -0.0003(6) -0.0012(7) -0.0029(6)
S2 0.0379(3) 0.0331(3) 0.0359(3) 0.0002(2) -0.0045(2) -0.0003(2)
O5 0.0442(10) 0.0433(10) 0.0562(12) -0.0031(8) -0.0013(8) -0.0092(8)
O6 0.0537(11) 0.0437(10) 0.0519(11) 0.0011(8) -0.0038(9) 0.0137(8)
C19 0.0618(17) 0.0539(16) 0.0365(14) 0.0015(12) -0.0074(13) -0.0017(13)
F4 0.1172(16) 0.0561(11) 0.0493(10) 0.0143(8) 0.0096(10) -0.0184(10)
F5 0.0930(13) 0.0624(11) 0.0428(9) -0.0091(8) 0.0109(9) -0.0038(9)
F6 0.0804(13) 0.1289(19) 0.0501(11) 0.0081(12) -0.0271(10) 0.0113(13)
C20 0.053(2) 0.112(3) 0.104(3) -0.015(3) 0.0139(19) -0.003(2)
C21 0.0555(16) 0.0473(15) 0.0592(18) -0.0082(13) 0.0132(14) -0.0088(12)
C22 0.0589(17) 0.0475(15) 0.0464(16) -0.0032(12) 0.0104(13) -0.0071(13)
C23 0.0554(17) 0.0461(15) 0.064(2) -0.0082(13) 0.0164(14) -0.0055(13)
C24 0.0645(19) 0.0490(17) 0.072(2) 0.0038(15) 0.0007(17) -0.0034(14)
C25 0.093(3) 0.063(2) 0.0470(18) 0.0070(15) 0.0018(17) -0.0178(18)
C26 0.082(2) 0.068(2) 0.059(2) -0.0108(16) 0.0305(18) -0.0213(18)
C27 0.193(6) 0.112(4) 0.082(3) -0.007(3) 0.042(4) -0.035(4)
C28 0.112(3) 0.085(3) 0.0397(18) -0.0042(16) 0.0236(19) -0.011(2)
C29 0.079(2) 0.098(3) 0.0504(19) 0.0043(19) 0.0160(17) 0.023(2)
C30 0.115(3) 0.092(3) 0.054(2) 0.009(2) 0.022(2) 0.035(3)
C31 0.145(5) 0.110(4) 0.059(3) 0.005(2) 0.027(3) 0.002(3)
C32 0.087(3) 0.167(5) 0.059(2) 0.007(3) 0.012(2) -0.023(3)
C33 0.071(2) 0.109(3) 0.0485(19) 0.0114(19) 0.0200(17) 0.025(2)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 N3 2.0080(18) . ?
V1 N1 2.0090(18) . ?
V1 O1 2.0606(16) . ?
V1 O4 2.0637(16) . ?
V1 N2 2.3223(18) . ?
V1 N4 2.3379(19) . ?
C1 C2 1.512(3) . ?
C2 N1 1.327(3) . ?
C2 C3 1.401(4) . ?
C3 C4 1.408(4) . ?
C4 N3 1.327(3) . ?
C4 C5 1.513(3) . ?
N1 C6 1.478(3) . ?
C6 C7 1.510(4) . ?
C7 N2 1.493(3) . ?
N2 C8 1.495(3) . ?
N2 C10 1.507(3) . ?
C8 C9 1.512(4) . ?
C10 C11 1.520(4) . ?
N3 C12 1.479(3) . ?
C12 C13 1.503(4) . ?
C13 N4 1.496(3) . ?
N4 C16 1.495(3) . ?
N4 C14 1.503(3) . ?
C14 C15 1.511(4) . ?
C16 C17 1.531(3) . ?
O1 S1 1.4733(16) . ?
S1 O3 1.416(2) . ?
S1 O2 1.419(2) . ?
S1 C18 1.811(3) . ?
C18 F3 1.283(4) . ?
C18 F1 1.326(3) . ?
C18 F2 1.328(4) . ?
O4 S2 1.4788(16) . ?
S2 O6 1.4283(18) . ?
S2 O5 1.4304(18) . ?
S2 C19 1.830(3) . ?
C19 F4 1.322(3) . ?
C19 F5 1.323(3) . ?
C19 F6 1.328(3) . ?
C20 C21 1.505(5) . ?
C21 C22 1.380(4) . ?
C21 C26 1.398(5) . ?
C22 C23 1.385(4) . ?
C23 C24 1.364(4) . ?
C24 C25 1.359(5) . ?
C25 C26 1.396(5) . ?
C27 C28 1.455(6) . ?
C28 C33 1.386(5) . ?
C28 C29 1.410(5) . ?
C29 C30 1.335(6) . ?
C30 C31 1.412(6) . ?
C31 C32 1.333(7) . ?
C32 C33 1.355(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 V1 N1 89.13(8) . . ?
N3 V1 O1 93.50(7) . . ?
N1 V1 O1 94.65(7) . . ?
N3 V1 O4 95.01(7) . . ?
N1 V1 O4 94.10(7) . . ?
O1 V1 O4 167.89(6) . . ?
N3 V1 N2 170.49(7) . . ?
N1 V1 N2 81.39(7) . . ?
O1 V1 N2 88.03(6) . . ?
O4 V1 N2 85.00(6) . . ?
N3 V1 N4 82.09(7) . . ?
N1 V1 N4 171.20(7) . . ?
O1 V1 N4 85.49(6) . . ?
O4 V1 N4 87.15(6) . . ?
N2 V1 N4 107.40(7) . . ?
N1 C2 C3 122.7(2) . . ?
N1 C2 C1 120.6(2) . . ?
C3 C2 C1 116.7(2) . . ?
C2 C3 C4 127.3(2) . . ?
N3 C4 C3 122.7(2) . . ?
N3 C4 C5 120.7(2) . . ?
C3 C4 C5 116.6(2) . . ?
C2 N1 C6 116.69(19) . . ?
C2 N1 V1 128.80(16) . . ?
C6 N1 V1 114.50(15) . . ?
N1 C6 C7 110.0(2) . . ?
N2 C7 C6 110.4(2) . . ?
C7 N2 C8 108.10(18) . . ?
C7 N2 C10 107.5(2) . . ?
C8 N2 C10 110.25(19) . . ?
C7 N2 V1 98.48(13) . . ?
C8 N2 V1 115.67(14) . . ?
C10 N2 V1 115.64(14) . . ?
N2 C8 C9 115.3(2) . . ?
N2 C10 C11 116.1(2) . . ?
C4 N3 C12 117.16(19) . . ?
C4 N3 V1 128.66(16) . . ?
C12 N3 V1 114.07(15) . . ?
N3 C12 C13 110.01(19) . . ?
N4 C13 C12 111.9(2) . . ?
C16 N4 C13 109.00(19) . . ?
C16 N4 C14 110.76(18) . . ?
C13 N4 C14 107.49(19) . . ?
C16 N4 V1 113.62(13) . . ?
C13 N4 V1 98.02(13) . . ?
C14 N4 V1 116.80(14) . . ?
N4 C14 C15 115.4(2) . . ?
N4 C16 C17 116.7(2) . . ?
S1 O1 V1 132.67(10) . . ?
O3 S1 O2 117.12(16) . . ?
O3 S1 O1 114.10(12) . . ?
O2 S1 O1 113.68(11) . . ?
O3 S1 C18 105.58(16) . . ?
O2 S1 C18 104.08(14) . . ?
O1 S1 C18 99.68(11) . . ?
F3 C18 F1 108.0(3) . . ?
F3 C18 F2 108.8(3) . . ?
F1 C18 F2 106.5(3) . . ?
F3 C18 S1 112.2(2) . . ?
F1 C18 S1 111.7(2) . . ?
F2 C18 S1 109.4(2) . . ?
S2 O4 V1 130.27(10) . . ?
O6 S2 O5 117.79(12) . . ?
O6 S2 O4 113.99(10) . . ?
O5 S2 O4 113.14(10) . . ?
O6 S2 C19 104.49(13) . . ?
O5 S2 C19 104.57(12) . . ?
O4 S2 C19 100.26(12) . . ?
F4 C19 F5 107.9(3) . . ?
F4 C19 F6 107.7(2) . . ?
F5 C19 F6 108.3(2) . . ?
F4 C19 S2 111.16(19) . . ?
F5 C19 S2 111.87(19) . . ?
F6 C19 S2 109.7(2) . . ?
C22 C21 C26 117.5(3) . . ?
C22 C21 C20 120.8(3) . . ?
C26 C21 C20 121.8(3) . . ?
C21 C22 C23 121.3(3) . . ?
C24 C23 C22 120.3(3) . . ?
C25 C24 C23 120.0(3) . . ?
C24 C25 C26 120.3(3) . . ?
C25 C26 C21 120.5(3) . . ?
C33 C28 C29 116.7(4) . . ?
C33 C28 C27 123.5(5) . . ?
C29 C28 C27 119.8(5) . . ?
C30 C29 C28 120.5(4) . . ?
C29 C30 C31 121.5(4) . . ?
C32 C31 C30 117.8(5) . . ?
C31 C32 C33 122.0(5) . . ?
C32 C33 C28 121.6(4) . . ?

_diffrn_measured_fraction_theta_max 0.918
_diffrn_reflns_theta_full        28.22
_diffrn_measured_fraction_theta_full 0.918
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.073

data_3
_database_code_CSD               206413

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H45 N4 P V'
_chemical_formula_weight         531.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21

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

_cell_length_a                   12.740(3)
_cell_length_b                   14.466(3)
_cell_length_c                   15.247(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.55(3)
_cell_angle_gamma                90.00
_cell_volume                     2804.6(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9999
_cell_measurement_theta_min      3.5
_cell_measurement_theta_max      59.5

_exptl_crystal_description       blocks
_exptl_crystal_colour            'dark brown'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1140
_exptl_absorpt_coefficient_mu    3.667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5275
_exptl_absorpt_correction_T_max  0.7106
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  'mirror system'
_diffrn_measurement_device_type  'Bruker three circle diffractometer'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_detector_area_resol_mean '5.602 pixels/mm'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            17902
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_av_sigmaI/netI    0.0214
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.48
_diffrn_reflns_theta_max         59.67
_reflns_number_total             7400
_reflns_number_gt                7386
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Proteum (Version 1.35)'
_computing_cell_refinement       'Bruker AXS SAINT (V. 6.31a, Bruker 2002)'
_computing_data_reduction        'Bruker AXS SAINT (V. 6.31a, Bruker 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker AXS SHELXTL (V. 5.10)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
;
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^ > 2sigma(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^)+(0.0419P)^2^+0.3970P] 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     SHELXL
_refine_ls_extinction_coef       0.0121(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.503(3)
_refine_ls_number_reflns         7400
_refine_ls_number_parameters     645
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0264
_refine_ls_wR_factor_ref         0.0648
_refine_ls_wR_factor_gt          0.0647
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_restrained_S_all      1.153
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.08348(2) 0.24856(2) 0.61523(2) 0.01623(10) Uani 1 1 d . . .
P1 P -0.06521(4) 0.19988(3) 0.50257(3) 0.01889(12) Uani 1 1 d . . .
N1 N 0.17246(13) 0.34056(12) 0.55014(11) 0.0205(4) Uani 1 1 d . . .
C1 C 0.32235(19) 0.40210(17) 0.47266(17) 0.0388(6) Uani 1 1 d . . .
H1A H 0.2824 0.4218 0.4189 0.058 Uiso 1 1 calc R . .
H1B H 0.3920 0.3804 0.4580 0.058 Uiso 1 1 calc R . .
H1C H 0.3302 0.4543 0.5135 0.058 Uiso 1 1 calc R . .
V2 V 0.44122(2) 0.49001(2) 0.89559(2) 0.01652(10) Uani 1 1 d . . .
P2 P 0.58642(4) 0.54257(3) 1.00818(3) 0.01945(12) Uani 1 1 d . . .
N2 N 0.02058(12) 0.38982(12) 0.66241(11) 0.0187(4) Uani 1 1 d . . .
C2 C 0.26442(16) 0.32447(15) 0.51522(13) 0.0233(5) Uani 1 1 d . . .
N3 N 0.18621(12) 0.14504(12) 0.58752(11) 0.0194(4) Uani 1 1 d . . .
C3 C 0.31125(15) 0.23712(16) 0.51388(13) 0.0234(4) Uani 1 1 d . . .
H3 H 0.3766 0.2343 0.4872 0.028 Uiso 1 1 calc R . .
C4 C 0.27506(15) 0.15331(14) 0.54652(13) 0.0207(5) Uani 1 1 d . . .
N4 N 0.04459(12) 0.13741(12) 0.71683(11) 0.0201(4) Uani 1 1 d . . .
N5 N 0.35169(13) 0.40369(12) 0.96582(11) 0.0199(4) Uani 1 1 d . . .
C5 C 0.34315(17) 0.06945(16) 0.53440(15) 0.0298(5) Uani 1 1 d . . .
H5A H 0.3648 0.0433 0.5920 0.045 Uiso 1 1 calc R . .
H5B H 0.4056 0.0875 0.5041 0.045 Uiso 1 1 calc R . .
H5C H 0.3032 0.0232 0.4993 0.045 Uiso 1 1 calc R . .
N6 N 0.33321(12) 0.59336(12) 0.90920(11) 0.0190(4) Uani 1 1 d . . .
C6 C 0.12901(16) 0.43371(15) 0.53980(14) 0.0246(5) Uani 1 1 d . . .
H6A H 0.1241 0.4509 0.4768 0.029 Uiso 1 1 calc R . .
H6B H 0.1761 0.4785 0.5717 0.029 Uiso 1 1 calc R . .
N7 N 0.50037(12) 0.34880(12) 0.85240(10) 0.0196(4) Uani 1 1 d . . .
C7 C 0.02035(15) 0.43738(15) 0.57585(13) 0.0221(4) Uani 1 1 d . . .
H7A H -0.0011 0.5026 0.5826 0.027 Uiso 1 1 calc R . .
H7B H -0.0313 0.4072 0.5339 0.027 Uiso 1 1 calc R . .
N8 N 0.48349(13) 0.58672(12) 0.78525(11) 0.0200(4) Uani 1 1 d . . .
C8 C -0.08798(15) 0.38438(15) 0.69311(14) 0.0236(5) Uani 1 1 d . . .
H8A H -0.0824 0.3618 0.7545 0.028 Uiso 1 1 calc R . .
H8B H -0.1264 0.3365 0.6575 0.028 Uiso 1 1 calc R . .
C9 C -0.15582(16) 0.47084(16) 0.69071(16) 0.0301(5) Uani 1 1 d . . .
H9A H -0.1239 0.5171 0.7310 0.045 Uiso 1 1 calc R . .
H9B H -0.2262 0.4553 0.7087 0.045 Uiso 1 1 calc R . .
H9C H -0.1611 0.4959 0.6309 0.045 Uiso 1 1 calc R . .
C10 C 0.09681(16) 0.43262(16) 0.72836(14) 0.0231(4) Uani 1 1 d . . .
H10A H 0.1684 0.4143 0.7133 0.028 Uiso 1 1 calc R . .
H10B H 0.0848 0.4049 0.7863 0.028 Uiso 1 1 calc R . .
C11 C 0.09605(17) 0.53789(16) 0.73923(15) 0.0285(5) Uani 1 1 d . . .
H11A H 0.1068 0.5673 0.6826 0.043 Uiso 1 1 calc R . .
H11B H 0.1526 0.5563 0.7821 0.043 Uiso 1 1 calc R . .
H11C H 0.0282 0.5574 0.7599 0.043 Uiso 1 1 calc R . .
C12 C 0.15794(16) 0.05217(15) 0.61734(14) 0.0244(4) Uani 1 1 d . . .
H12A H 0.2134 0.0289 0.6601 0.029 Uiso 1 1 calc R . .
H12B H 0.1529 0.0093 0.5666 0.029 Uiso 1 1 calc R . .
C13 C 0.05301(16) 0.05484(14) 0.66020(13) 0.0215(4) Uani 1 1 d . . .
H13A H -0.0050 0.0554 0.6139 0.026 Uiso 1 1 calc R . .
H13B H 0.0457 -0.0016 0.6960 0.026 Uiso 1 1 calc R . .
C14 C 0.12231(17) 0.12730(17) 0.79381(14) 0.0289(5) Uani 1 1 d . . .
H14A H 0.1924 0.1148 0.7717 0.035 Uiso 1 1 calc R . .
H14B H 0.1025 0.0729 0.8285 0.035 Uiso 1 1 calc R . .
C15 C 0.1310(2) 0.20994(18) 0.85393(16) 0.0430(6) Uani 1 1 d . . .
H15A H 0.1481 0.2649 0.8200 0.064 Uiso 1 1 calc R . .
H15B H 0.1867 0.1991 0.9001 0.064 Uiso 1 1 calc R . .
H15C H 0.0640 0.2195 0.8808 0.064 Uiso 1 1 calc R . .
C16 C -0.06464(16) 0.14638(15) 0.74559(14) 0.0248(5) Uani 1 1 d . . .
H16A H -0.1114 0.1631 0.6937 0.030 Uiso 1 1 calc R . .
H16B H -0.0661 0.1984 0.7877 0.030 Uiso 1 1 calc R . .
C17 C -0.11041(19) 0.06125(19) 0.78849(17) 0.0405(6) Uani 1 1 d . . .
H17A H -0.1160 0.0105 0.7458 0.061 Uiso 1 1 calc R . .
H17B H -0.1804 0.0759 0.8079 0.061 Uiso 1 1 calc R . .
H17C H -0.0643 0.0426 0.8392 0.061 Uiso 1 1 calc R . .
C18 C -0.04821(14) 0.25389(15) 0.39608(12) 0.0190(4) Uani 1 1 d . . .
C19 C -0.13054(15) 0.28043(14) 0.33582(13) 0.0205(4) Uani 1 1 d . . .
H19 H -0.2010 0.2771 0.3525 0.025 Uiso 1 1 calc R . .
C20 C -0.11085(16) 0.31132(15) 0.25250(13) 0.0225(4) Uani 1 1 d . . .
H20 H -0.1681 0.3295 0.2133 0.027 Uiso 1 1 calc R . .
C21 C -0.00974(17) 0.31626(16) 0.22522(13) 0.0252(5) Uani 1 1 d . . .
H21 H 0.0030 0.3371 0.1678 0.030 Uiso 1 1 calc R . .
C22 C 0.07262(16) 0.29019(17) 0.28326(14) 0.0286(5) Uani 1 1 d . . .
H22 H 0.1427 0.2934 0.2655 0.034 Uiso 1 1 calc R . .
C23 C 0.05421(16) 0.25945(16) 0.36710(14) 0.0262(5) Uani 1 1 d . . .
H23 H 0.1121 0.2418 0.4058 0.031 Uiso 1 1 calc R . .
C24 C -0.20149(15) 0.22498(14) 0.52746(12) 0.0200(4) Uani 1 1 d . . .
C25 C -0.25529(15) 0.30855(15) 0.51215(13) 0.0223(5) Uani 1 1 d . . .
H25 H -0.2211 0.3577 0.4840 0.027 Uiso 1 1 calc R . .
C26 C -0.35748(16) 0.32117(16) 0.53714(14) 0.0273(5) Uani 1 1 d . . .
H26 H -0.3931 0.3777 0.5242 0.033 Uiso 1 1 calc R . .
C27 C -0.40755(15) 0.25140(17) 0.58086(13) 0.0273(5) Uani 1 1 d . . .
H27 H -0.4766 0.2605 0.5994 0.033 Uiso 1 1 calc R . .
C28 C -0.35624(17) 0.16866(16) 0.59719(14) 0.0279(5) Uani 1 1 d . . .
H28 H -0.3902 0.1206 0.6270 0.033 Uiso 1 1 calc R . .
C29 C -0.25557(16) 0.15526(15) 0.57034(13) 0.0225(4) Uani 1 1 d . . .
H29 H -0.2221 0.0973 0.5812 0.027 Uiso 1 1 calc R . .
C30 C 0.21104(18) 0.35293(16) 1.05917(15) 0.0297(5) Uani 1 1 d . . .
H30A H 0.2596 0.3348 1.1085 0.045 Uiso 1 1 calc R . .
H30B H 0.1923 0.2985 1.0233 0.045 Uiso 1 1 calc R . .
H30C H 0.1473 0.3795 1.0817 0.045 Uiso 1 1 calc R . .
C31 C 0.26297(15) 0.42349(15) 1.00390(13) 0.0217(4) Uani 1 1 d . . .
C32 C 0.21481(16) 0.51056(15) 0.99745(13) 0.0214(5) Uani 1 1 d . . .
H32 H 0.1526 0.5170 1.0282 0.026 Uiso 1 1 calc R . .
C33 C 0.24512(15) 0.58917(14) 0.95238(13) 0.0195(4) Uani 1 1 d . . .
C34 C 0.17187(16) 0.67146(16) 0.95364(14) 0.0255(5) Uani 1 1 d . . .
H34A H 0.2099 0.7247 0.9796 0.038 Uiso 1 1 calc R . .
H34B H 0.1122 0.6565 0.9887 0.038 Uiso 1 1 calc R . .
H34C H 0.1461 0.6865 0.8934 0.038 Uiso 1 1 calc R . .
C35 C 0.35440(16) 0.67960(15) 0.86268(14) 0.0228(4) Uani 1 1 d . . .
H35A H 0.3490 0.7327 0.9031 0.027 Uiso 1 1 calc R . .
H35B H 0.3016 0.6879 0.8129 0.027 Uiso 1 1 calc R . .
C36 C 0.46365(16) 0.67635(15) 0.82881(14) 0.0221(4) Uani 1 1 d . . .
H36A H 0.4715 0.7273 0.7864 0.027 Uiso 1 1 calc R . .
H36B H 0.5165 0.6855 0.8784 0.027 Uiso 1 1 calc R . .
C37 C 0.39321(16) 0.30996(15) 0.97777(14) 0.0239(5) Uani 1 1 d . . .
H37A H 0.3433 0.2652 0.9491 0.029 Uiso 1 1 calc R . .
H37B H 0.4006 0.2952 1.0413 0.029 Uiso 1 1 calc R . .
C38 C 0.49893(16) 0.30082(14) 0.93875(13) 0.0218(4) Uani 1 1 d . . .
H38A H 0.5540 0.3275 0.9799 0.026 Uiso 1 1 calc R . .
H38B H 0.5152 0.2345 0.9309 0.026 Uiso 1 1 calc R . .
C39 C 0.60841(15) 0.34880(15) 0.81984(14) 0.0239(5) Uani 1 1 d . . .
H39A H 0.6501 0.3962 0.8533 0.029 Uiso 1 1 calc R . .
H39B H 0.6028 0.3690 0.7577 0.029 Uiso 1 1 calc R . .
C40 C 0.67109(16) 0.25854(16) 0.82471(15) 0.0286(5) Uani 1 1 d . . .
H40A H 0.6822 0.2393 0.8862 0.043 Uiso 1 1 calc R . .
H40B H 0.7393 0.2681 0.7997 0.043 Uiso 1 1 calc R . .
H40C H 0.6319 0.2104 0.7914 0.043 Uiso 1 1 calc R . .
C41 C 0.41936(16) 0.31251(15) 0.78636(14) 0.0223(5) Uani 1 1 d . . .
H41A H 0.4306 0.3431 0.7296 0.027 Uiso 1 1 calc R . .
H41B H 0.3497 0.3328 0.8045 0.027 Uiso 1 1 calc R . .
C42 C 0.41308(17) 0.20899(15) 0.76943(15) 0.0259(5) Uani 1 1 d . . .
H42A H 0.4795 0.1875 0.7474 0.039 Uiso 1 1 calc R . .
H42B H 0.3554 0.1960 0.7257 0.039 Uiso 1 1 calc R . .
H42C H 0.4004 0.1768 0.8243 0.039 Uiso 1 1 calc R . .
C43 C 0.59535(16) 0.58073(15) 0.76052(14) 0.0240(5) Uani 1 1 d . . .
H43A H 0.5993 0.5319 0.7153 0.029 Uiso 1 1 calc R . .
H43B H 0.6387 0.5599 0.8129 0.029 Uiso 1 1 calc R . .
C44 C 0.64597(18) 0.66781(17) 0.72569(17) 0.0364(6) Uani 1 1 d . . .
H44A H 0.6016 0.6926 0.6764 0.055 Uiso 1 1 calc R . .
H44B H 0.7156 0.6526 0.7057 0.055 Uiso 1 1 calc R . .
H44C H 0.6533 0.7141 0.7726 0.055 Uiso 1 1 calc R . .
C45 C 0.40784(16) 0.56807(16) 0.70993(13) 0.0276(5) Uani 1 1 d . . .
H45A H 0.3372 0.5619 0.7329 0.033 Uiso 1 1 calc R . .
H45B H 0.4259 0.5074 0.6848 0.033 Uiso 1 1 calc R . .
C46 C 0.40011(19) 0.63725(18) 0.63600(15) 0.0370(6) Uani 1 1 d . . .
H46A H 0.3914 0.6994 0.6600 0.056 Uiso 1 1 calc R . .
H46B H 0.3395 0.6223 0.5958 0.056 Uiso 1 1 calc R . .
H46C H 0.4645 0.6351 0.6040 0.056 Uiso 1 1 calc R . .
C47 C 0.56362(15) 0.48870(16) 1.11359(12) 0.0191(4) Uani 1 1 d . . .
C48 C 0.45934(15) 0.49266(16) 1.14051(13) 0.0246(5) Uani 1 1 d . . .
H48 H 0.4056 0.5190 1.1024 0.030 Uiso 1 1 calc R . .
C49 C 0.43443(17) 0.45869(17) 1.22174(14) 0.0295(5) Uani 1 1 d . . .
H49 H 0.3639 0.4622 1.2384 0.035 Uiso 1 1 calc R . .
C50 C 0.51094(17) 0.41964(16) 1.27916(14) 0.0288(5) Uani 1 1 d . . .
H50 H 0.4931 0.3947 1.3339 0.035 Uiso 1 1 calc R . .
C51 C 0.61332(17) 0.41791(15) 1.25472(14) 0.0248(5) Uani 1 1 d . . .
H51 H 0.6669 0.3928 1.2938 0.030 Uiso 1 1 calc R . .
C52 C 0.63942(15) 0.45227(14) 1.17380(13) 0.0215(4) Uani 1 1 d . . .
H52 H 0.7108 0.4509 1.1591 0.026 Uiso 1 1 calc R . .
C53 C 0.72328(15) 0.51476(14) 0.98706(13) 0.0196(4) Uani 1 1 d . . .
C54 C 0.77960(16) 0.58385(15) 0.94604(14) 0.0259(5) Uani 1 1 d . . .
H54 H 0.7471 0.6421 0.9347 0.031 Uiso 1 1 calc R . .
C55 C 0.88175(17) 0.56978(17) 0.92143(14) 0.0306(5) Uani 1 1 d . . .
H55 H 0.9172 0.6174 0.8922 0.037 Uiso 1 1 calc R . .
C56 C 0.93144(16) 0.48660(18) 0.93962(14) 0.0321(5) Uani 1 1 d . . .
H56 H 1.0017 0.4770 0.9240 0.039 Uiso 1 1 calc R . .
C57 C 0.87827(16) 0.41736(17) 0.98068(14) 0.0282(5) Uani 1 1 d . . .
H57 H 0.9122 0.3600 0.9935 0.034 Uiso 1 1 calc R . .
C58 C 0.77506(16) 0.43100(16) 1.00347(14) 0.0247(5) Uani 1 1 d . . .
H58 H 0.7393 0.3822 1.0307 0.030 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
V1 0.01461(16) 0.01630(18) 0.01809(18) 0.00090(13) 0.00363(13) 0.00066(14)
P1 0.0182(3) 0.0177(3) 0.0208(3) -0.00009(19) 0.0016(2) 0.00059(19)
N1 0.0212(9) 0.0194(9) 0.0213(9) 0.0010(7) 0.0043(7) 0.0002(7)
C1 0.0358(13) 0.0316(13) 0.0517(15) 0.0042(11) 0.0241(12) -0.0014(11)
V2 0.01588(17) 0.01606(18) 0.01795(19) 0.00065(13) 0.00363(13) 0.00064(14)
P2 0.0186(2) 0.0180(3) 0.0217(3) 0.0003(2) 0.0012(2) 0.0015(2)
N2 0.0153(8) 0.0183(9) 0.0228(9) -0.0003(7) 0.0050(7) 0.0002(7)
C2 0.0235(11) 0.0257(11) 0.0212(11) 0.0007(9) 0.0060(9) -0.0029(9)
N3 0.0186(8) 0.0196(9) 0.0200(9) -0.0006(7) 0.0011(7) 0.0022(7)
C3 0.0185(9) 0.0303(12) 0.0222(10) -0.0013(9) 0.0084(8) -0.0005(9)
C4 0.0183(10) 0.0269(12) 0.0170(11) -0.0028(8) 0.0005(8) 0.0035(9)
N4 0.0180(8) 0.0223(9) 0.0202(9) 0.0037(7) 0.0028(7) -0.0011(7)
N5 0.0217(8) 0.0198(9) 0.0187(9) 0.0001(7) 0.0040(7) 0.0015(7)
C5 0.0248(11) 0.0294(12) 0.0361(13) 0.0027(10) 0.0091(9) 0.0079(10)
N6 0.0194(8) 0.0194(9) 0.0184(9) 0.0016(7) 0.0017(7) 0.0005(7)
C6 0.0284(11) 0.0186(11) 0.0275(11) 0.0035(9) 0.0085(9) 0.0006(9)
N7 0.0184(8) 0.0204(9) 0.0204(9) 0.0010(7) 0.0032(7) 0.0009(7)
C7 0.0251(10) 0.0169(10) 0.0242(11) -0.0001(9) 0.0010(9) 0.0027(9)
N8 0.0199(8) 0.0195(9) 0.0207(9) -0.0019(7) 0.0035(7) 0.0005(7)
C8 0.0188(10) 0.0220(11) 0.0306(12) -0.0034(9) 0.0065(9) 0.0002(8)
C9 0.0201(10) 0.0312(13) 0.0391(12) -0.0087(10) 0.0024(9) 0.0022(9)
C10 0.0209(10) 0.0238(11) 0.0246(11) -0.0050(9) 0.0011(9) -0.0008(9)
C11 0.0262(11) 0.0256(12) 0.0333(13) -0.0077(10) 0.0002(9) -0.0015(9)
C12 0.0248(10) 0.0191(11) 0.0297(11) 0.0037(9) 0.0051(9) 0.0034(9)
C13 0.0241(10) 0.0152(10) 0.0255(11) 0.0030(8) 0.0035(9) 0.0005(8)
C14 0.0267(11) 0.0332(12) 0.0263(12) 0.0071(9) -0.0027(9) -0.0001(9)
C15 0.0513(15) 0.0438(15) 0.0322(13) -0.0017(11) -0.0104(12) 0.0021(12)
C16 0.0225(11) 0.0256(11) 0.0268(12) 0.0038(9) 0.0067(9) 0.0018(9)
C17 0.0326(12) 0.0422(15) 0.0490(15) 0.0171(12) 0.0207(11) 0.0029(11)
C18 0.0204(9) 0.0160(11) 0.0208(11) -0.0036(8) 0.0020(8) -0.0007(9)
C19 0.0169(9) 0.0195(11) 0.0255(11) -0.0010(8) 0.0030(8) -0.0016(8)
C20 0.0222(10) 0.0218(11) 0.0229(11) -0.0003(9) -0.0028(9) 0.0019(8)
C21 0.0298(11) 0.0280(12) 0.0183(11) -0.0007(9) 0.0045(9) -0.0039(9)
C22 0.0192(10) 0.0420(14) 0.0254(12) -0.0050(10) 0.0080(9) -0.0006(9)
C23 0.0204(10) 0.0334(13) 0.0245(11) -0.0050(10) 0.0007(9) 0.0047(9)
C24 0.0186(9) 0.0225(11) 0.0186(10) -0.0020(8) -0.0009(8) -0.0036(8)
C25 0.0192(10) 0.0223(11) 0.0255(11) -0.0006(9) 0.0032(9) -0.0050(9)
C26 0.0230(11) 0.0294(12) 0.0295(12) -0.0020(10) -0.0001(9) 0.0017(9)
C27 0.0194(9) 0.0386(13) 0.0245(11) -0.0047(10) 0.0052(8) -0.0051(10)
C28 0.0263(11) 0.0332(13) 0.0245(11) 0.0010(9) 0.0047(9) -0.0089(10)
C29 0.0243(10) 0.0235(11) 0.0196(11) -0.0013(8) 0.0010(9) -0.0034(9)
C30 0.0328(12) 0.0255(11) 0.0322(12) 0.0012(9) 0.0140(10) -0.0039(10)
C31 0.0219(10) 0.0248(11) 0.0186(11) -0.0016(8) 0.0037(8) -0.0044(9)
C32 0.0183(10) 0.0275(12) 0.0189(11) -0.0031(8) 0.0048(8) 0.0019(8)
C33 0.0173(10) 0.0239(11) 0.0171(10) -0.0037(8) -0.0005(8) 0.0024(8)
C34 0.0208(10) 0.0277(11) 0.0283(12) -0.0017(9) 0.0040(9) 0.0041(9)
C35 0.0231(10) 0.0209(11) 0.0244(11) 0.0025(8) 0.0021(9) 0.0027(8)
C36 0.0228(10) 0.0208(11) 0.0232(11) 0.0034(8) 0.0050(9) -0.0009(8)
C37 0.0295(11) 0.0189(11) 0.0240(11) 0.0036(9) 0.0065(9) 0.0022(9)
C38 0.0248(10) 0.0200(11) 0.0207(11) 0.0028(9) 0.0023(8) 0.0015(9)
C39 0.0199(10) 0.0254(11) 0.0272(12) -0.0023(9) 0.0064(8) -0.0009(8)
C40 0.0242(10) 0.0293(12) 0.0323(12) -0.0057(10) 0.0022(9) 0.0065(10)
C41 0.0221(10) 0.0219(11) 0.0228(11) 0.0020(9) 0.0007(9) -0.0013(8)
C42 0.0272(11) 0.0252(12) 0.0254(11) -0.0014(9) 0.0026(9) -0.0017(9)
C43 0.0200(10) 0.0280(11) 0.0247(11) 0.0027(9) 0.0061(9) 0.0010(9)
C44 0.0308(12) 0.0358(14) 0.0442(14) 0.0089(11) 0.0163(11) -0.0014(10)
C45 0.0238(11) 0.0372(13) 0.0218(11) -0.0027(9) 0.0025(9) 0.0016(9)
C46 0.0392(13) 0.0429(14) 0.0286(13) 0.0032(10) -0.0014(11) 0.0074(11)
C47 0.0210(10) 0.0163(10) 0.0202(11) -0.0057(8) 0.0028(8) -0.0005(8)
C48 0.0194(10) 0.0302(11) 0.0244(11) -0.0094(10) 0.0020(9) 0.0005(9)
C49 0.0218(10) 0.0414(14) 0.0262(12) -0.0119(10) 0.0081(9) -0.0051(9)
C50 0.0349(12) 0.0312(13) 0.0212(12) -0.0040(9) 0.0084(10) -0.0071(10)
C51 0.0298(11) 0.0216(11) 0.0228(12) -0.0014(9) -0.0008(9) -0.0031(9)
C52 0.0194(10) 0.0192(11) 0.0262(11) -0.0041(8) 0.0036(8) -0.0016(8)
C53 0.0189(10) 0.0235(11) 0.0162(10) -0.0029(8) 0.0003(8) -0.0030(8)
C54 0.0288(11) 0.0230(11) 0.0256(12) -0.0010(9) -0.0009(9) -0.0038(9)
C55 0.0281(12) 0.0361(14) 0.0284(12) -0.0031(10) 0.0078(9) -0.0110(10)
C56 0.0184(10) 0.0481(15) 0.0304(11) -0.0085(11) 0.0049(9) -0.0038(11)
C57 0.0212(10) 0.0331(13) 0.0304(12) -0.0026(9) 0.0021(9) 0.0033(9)
C58 0.0215(10) 0.0259(12) 0.0269(12) -0.0019(9) 0.0035(9) -0.0003(9)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 N1 2.0446(17) . ?
V1 N3 2.0499(17) . ?
V1 N4 2.3078(17) . ?
V1 N2 2.3253(18) . ?
V1 P1 2.5752(9) . ?
P1 C18 1.827(2) . ?
P1 C24 1.836(2) . ?
N1 C2 1.337(3) . ?
N1 C6 1.462(3) . ?
C1 C2 1.512(3) . ?
V2 N5 2.0392(17) . ?
V2 N6 2.0511(17) . ?
V2 N8 2.2781(18) . ?
V2 N7 2.2882(18) . ?
V2 P2 2.5600(9) . ?
P2 C47 1.825(2) . ?
P2 C53 1.837(2) . ?
N2 C7 1.488(3) . ?
N2 C10 1.489(3) . ?
N2 C8 1.489(2) . ?
C2 C3 1.398(3) . ?
N3 C4 1.332(3) . ?
N3 C12 1.470(3) . ?
C3 C4 1.399(3) . ?
C4 C5 1.509(3) . ?
N4 C13 1.482(3) . ?
N4 C16 1.490(2) . ?
N4 C14 1.495(3) . ?
N5 C31 1.333(3) . ?
N5 C37 1.463(3) . ?
N6 C33 1.337(3) . ?
N6 C35 1.468(3) . ?
C6 C7 1.522(3) . ?
N7 C38 1.489(2) . ?
N7 C39 1.492(2) . ?
N7 C41 1.492(3) . ?
N8 C45 1.478(3) . ?
N8 C36 1.486(3) . ?
N8 C43 1.499(3) . ?
C8 C9 1.519(3) . ?
C10 C11 1.532(3) . ?
C12 C13 1.524(3) . ?
C14 C15 1.506(3) . ?
C16 C17 1.527(3) . ?
C18 C19 1.404(3) . ?
C18 C23 1.406(3) . ?
C19 C20 1.384(3) . ?
C20 C21 1.380(3) . ?
C21 C22 1.383(3) . ?
C22 C23 1.387(3) . ?
C24 C25 1.402(3) . ?
C24 C29 1.405(3) . ?
C25 C26 1.391(3) . ?
C26 C27 1.387(3) . ?
C27 C28 1.379(3) . ?
C28 C29 1.384(3) . ?
C30 C31 1.503(3) . ?
C31 C32 1.402(3) . ?
C32 C33 1.395(3) . ?
C33 C34 1.514(3) . ?
C35 C36 1.515(3) . ?
C37 C38 1.512(3) . ?
C39 C40 1.530(3) . ?
C41 C42 1.521(3) . ?
C43 C44 1.526(3) . ?
C45 C46 1.506(3) . ?
C47 C52 1.394(3) . ?
C47 C48 1.416(3) . ?
C48 C49 1.387(3) . ?
C49 C50 1.389(3) . ?
C50 C51 1.379(3) . ?
C51 C52 1.389(3) . ?
C53 C58 1.395(3) . ?
C53 C54 1.400(3) . ?
C54 C55 1.391(3) . ?
C55 C56 1.380(4) . ?
C56 C57 1.381(3) . ?
C57 C58 1.395(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 V1 N3 89.73(7) . . ?
N1 V1 N4 158.11(7) . . ?
N3 V1 N4 78.21(7) . . ?
N1 V1 N2 77.89(6) . . ?
N3 V1 N2 160.46(6) . . ?
N4 V1 N2 108.19(6) . . ?
N1 V1 P1 105.15(5) . . ?
N3 V1 P1 96.63(5) . . ?
N4 V1 P1 94.45(5) . . ?
N2 V1 P1 101.15(4) . . ?
C18 P1 C24 105.35(9) . . ?
C18 P1 V1 110.67(7) . . ?
C24 P1 V1 118.29(7) . . ?
C2 N1 C6 116.93(17) . . ?
C2 N1 V1 127.29(14) . . ?
C6 N1 V1 115.77(12) . . ?
N5 V2 N6 89.58(7) . . ?
N5 V2 N8 158.33(6) . . ?
N6 V2 N8 79.50(6) . . ?
N5 V2 N7 79.01(6) . . ?
N6 V2 N7 156.17(6) . . ?
N8 V2 N7 103.80(6) . . ?
N5 V2 P2 103.55(5) . . ?
N6 V2 P2 100.20(5) . . ?
N8 V2 P2 96.82(5) . . ?
N7 V2 P2 102.77(4) . . ?
C47 P2 C53 105.39(9) . . ?
C47 P2 V2 108.41(7) . . ?
C53 P2 V2 118.14(7) . . ?
C7 N2 C10 111.84(16) . . ?
C7 N2 C8 110.63(15) . . ?
C10 N2 C8 112.91(15) . . ?
C7 N2 V1 96.53(11) . . ?
C10 N2 V1 110.58(12) . . ?
C8 N2 V1 113.29(12) . . ?
N1 C2 C3 123.26(19) . . ?
N1 C2 C1 120.31(19) . . ?
C3 C2 C1 116.42(18) . . ?
C4 N3 C12 117.31(16) . . ?
C4 N3 V1 127.09(14) . . ?
C12 N3 V1 115.60(12) . . ?
C2 C3 C4 128.87(17) . . ?
N3 C4 C3 123.57(18) . . ?
N3 C4 C5 119.79(18) . . ?
C3 C4 C5 116.64(17) . . ?
C13 N4 C16 110.14(15) . . ?
C13 N4 C14 108.08(16) . . ?
C16 N4 C14 111.26(16) . . ?
C13 N4 V1 98.29(11) . . ?
C16 N4 V1 112.33(12) . . ?
C14 N4 V1 115.84(12) . . ?
C31 N5 C37 117.04(16) . . ?
C31 N5 V2 127.88(14) . . ?
C37 N5 V2 115.04(12) . . ?
C33 N6 C35 117.47(16) . . ?
C33 N6 V2 127.27(14) . . ?
C35 N6 V2 115.21(12) . . ?
N1 C6 C7 109.89(16) . . ?
C38 N7 C39 110.88(15) . . ?
C38 N7 C41 112.75(16) . . ?
C39 N7 C41 112.91(15) . . ?
C38 N7 V2 98.01(11) . . ?
C39 N7 V2 115.01(12) . . ?
C41 N7 V2 106.38(12) . . ?
N2 C7 C6 110.63(16) . . ?
C45 N8 C36 112.71(16) . . ?
C45 N8 C43 112.24(15) . . ?
C36 N8 C43 110.70(16) . . ?
C45 N8 V2 106.81(12) . . ?
C36 N8 V2 98.70(11) . . ?
C43 N8 V2 114.97(12) . . ?
N2 C8 C9 119.13(17) . . ?
N2 C10 C11 118.57(19) . . ?
N3 C12 C13 110.33(16) . . ?
N4 C13 C12 111.55(16) . . ?
N4 C14 C15 114.86(19) . . ?
N4 C16 C17 116.36(18) . . ?
C19 C18 C23 116.67(17) . . ?
C19 C18 P1 125.00(14) . . ?
C23 C18 P1 117.86(15) . . ?
C20 C19 C18 121.22(18) . . ?
C21 C20 C19 121.27(19) . . ?
C20 C21 C22 118.59(19) . . ?
C21 C22 C23 120.83(19) . . ?
C22 C23 C18 121.42(19) . . ?
C25 C24 C29 116.59(17) . . ?
C25 C24 P1 126.49(15) . . ?
C29 C24 P1 116.83(15) . . ?
C26 C25 C24 121.58(19) . . ?
C27 C26 C25 120.2(2) . . ?
C28 C27 C26 119.43(19) . . ?
C27 C28 C29 120.4(2) . . ?
C28 C29 C24 121.8(2) . . ?
N5 C31 C32 122.79(18) . . ?
N5 C31 C30 120.85(19) . . ?
C32 C31 C30 116.33(18) . . ?
C33 C32 C31 129.30(18) . . ?
N6 C33 C32 123.07(18) . . ?
N6 C33 C34 120.50(18) . . ?
C32 C33 C34 116.42(17) . . ?
N6 C35 C36 109.79(16) . . ?
N8 C36 C35 111.39(17) . . ?
N5 C37 C38 110.87(16) . . ?
N7 C38 C37 111.55(16) . . ?
N7 C39 C40 118.25(17) . . ?
N7 C41 C42 119.20(18) . . ?
N8 C43 C44 117.96(18) . . ?
N8 C45 C46 118.01(19) . . ?
C52 C47 C48 116.65(18) . . ?
C52 C47 P2 126.85(15) . . ?
C48 C47 P2 116.19(16) . . ?
C49 C48 C47 121.0(2) . . ?
C48 C49 C50 121.08(19) . . ?
C51 C50 C49 118.4(2) . . ?
C50 C51 C52 121.1(2) . . ?
C51 C52 C47 121.73(18) . . ?
C58 C53 C54 116.77(18) . . ?
C58 C53 P2 127.03(15) . . ?
C54 C53 P2 116.12(16) . . ?
C55 C54 C53 122.0(2) . . ?
C56 C55 C54 119.9(2) . . ?
C55 C56 C57 119.47(19) . . ?
C56 C57 C58 120.5(2) . . ?
C57 C58 C53 121.4(2) . . ?

_diffrn_measured_fraction_theta_max 0.950
_diffrn_reflns_theta_full        59.67
_diffrn_measured_fraction_theta_full 0.950
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.088