 
data_s92
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C24 H28 F6 N5 Ni2 O3 P S2'
_chemical_formula_weight          761.02
 
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'
 'Ni'  'Ni'   0.3393   1.1124
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            Triclinic
_symmetry_space_group_name_H-M    P-1
_symmetry_spacE_group_name_hall   '-P 1'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    8.2994(2)
_cell_length_b                    11.9644(3)
_cell_length_c                    15.7923(3)
_cell_angle_alpha                 103.6270(10)
_cell_angle_beta                  99.058(2)
_cell_angle_gamma                 105.0280(10)
_cell_volume                      1431.42(6)
_cell_formula_units_Z             2
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     6402
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Slab
_exptl_crystal_colour             Red
_exptl_crystal_size_max           0.32
_exptl_crystal_size_mid           0.18
_exptl_crystal_size_min           0.08
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.766
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              776
_exptl_absorpt_coefficient_mu     1.594
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.6294
_exptl_absorpt_correction_T_max   0.8830
_exptl_absorpt_process_details    'SORTAV Blessing (1997)'

_exptl_special_details
;
 PLEASE NOTE cell_measurement_ fields are not relevant to area detector data,
 the entire data set is used to refine the cell, which is indexed from all
 observed reflections in a 10 degree phi range.
;
_diffrn_ambient_temperature       120(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Nonius KappaCCD Area Detector'
_diffrn_measurement_method        'φ and ω scans to fill Ewald Sphere'
_diffrn_detector_area_resol_mean  9.091
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             32596
_diffrn_reflns_av_R_equivalents   0.0718
_diffrn_reflns_av_sigmaI/netI     0.0465
_diffrn_reflns_limit_h_min        -10
_diffrn_reflns_limit_h_max        10
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_k_max        15
_diffrn_reflns_limit_l_min        -20
_diffrn_reflns_limit_l_max        20
_diffrn_reflns_theta_min          2.98
_diffrn_reflns_theta_max          27.48
_reflns_number_total              6544
_reflns_number_gt                 5354
_reflns_threshold_expression      >2σ(I)
 
_computing_data_collection
' DENZO (Otwinowski and Minor, 1997)'
_computing_cell_refinement        
' DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)'
_computing_data_reduction         
' DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997a)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997b)' 
_computing_molecular_graphics     'PLATON (Spek, 1990)'
_computing_publication_material   ? 
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0219P)²+4.8507P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.0044(5)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          6544
_refine_ls_number_parameters      397
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0606
_refine_ls_R_factor_gt            0.0457
_refine_ls_wR_factor_ref          0.1073
_refine_ls_wR_factor_gt           0.1014
_refine_ls_goodness_of_fit_ref    1.100
_refine_ls_restrained_S_all       1.100
_refine_ls_shift/su_max           0.004
_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
C1 C 0.7407(4) 0.2511(3) 0.6139(2) 0.0185(7) Uani 1 1 d . . .
H1 H 0.7192 0.2629 0.6722 0.022 Uiso 1 1 calc R . .
C2 C 0.7415(4) 0.1311(3) 0.5683(2) 0.0168(7) Uani 1 1 d . . .
C3 C 0.8126(4) 0.1043(3) 0.4941(2) 0.0158(7) Uani 1 1 d . . .
C4 C 0.7949(4) -0.0165(3) 0.4510(2) 0.0165(7) Uani 1 1 d . . .
C5 C 0.7188(4) -0.1073(3) 0.4876(2) 0.0183(7) Uani 1 1 d . . .
H5 H 0.7074 -0.1891 0.4586 0.022 Uiso 1 1 calc R . .
C6 C 0.6600(4) -0.0805(3) 0.5650(2) 0.0188(7) Uani 1 1 d . . .
C7 C 0.6674(4) 0.0372(3) 0.6026(2) 0.0179(7) Uani 1 1 d . . .
H7 H 0.6207 0.0555 0.6534 0.021 Uiso 1 1 calc R . .
C8 C 0.8575(4) -0.0555(3) 0.3712(2) 0.0189(7) Uani 1 1 d . . .
H8 H 0.8691 -0.1343 0.3585 0.023 Uiso 1 1 calc R . .
C9 C 0.5913(5) -0.1778(3) 0.6074(3) 0.0237(8) Uani 1 1 d . . .
H9A H 0.6410 -0.1487 0.6721 0.036 Uiso 1 1 calc R . .
H9B H 0.6220 -0.2500 0.5813 0.036 Uiso 1 1 calc R . .
H9C H 0.4661 -0.1980 0.5964 0.036 Uiso 1 1 calc R . .
C10 C 0.9712(5) -0.0559(3) 0.2456(2) 0.0215(7) Uani 1 1 d . . .
H10A H 0.9643 -0.1382 0.2498 0.026 Uiso 1 1 calc R . .
H10B H 1.0938 -0.0101 0.2559 0.026 Uiso 1 1 calc R . .
C11 C 0.8795(5) -0.0651(4) 0.1527(2) 0.0244(8) Uani 1 1 d . . .
H11A H 0.9224 -0.1159 0.1081 0.029 Uiso 1 1 calc R . .
H11B H 0.7554 -0.1055 0.1440 0.029 Uiso 1 1 calc R . .
C12 C 0.9047(5) 0.0566(4) 0.1363(3) 0.0278(9) Uani 1 1 d . . .
H12A H 1.0290 0.1001 0.1498 0.033 Uiso 1 1 calc R . .
H12B H 0.8564 0.0452 0.0723 0.033 Uiso 1 1 calc R . .
C13 C 0.7099(5) 0.1672(3) 0.1500(2) 0.0235(8) Uani 1 1 d . . .
H13 H 0.6844 0.1385 0.0864 0.028 Uiso 1 1 calc R . .
C14 C 0.6183(5) 0.2480(3) 0.1880(2) 0.0211(7) Uani 1 1 d . . .
C15 C 0.6751(4) 0.3287(3) 0.2742(2) 0.0170(7) Uani 1 1 d . . .
C16 C 0.5805(4) 0.4051(3) 0.3041(2) 0.0177(7) Uani 1 1 d . . .
C17 C 0.4331(5) 0.4013(3) 0.2458(2) 0.0218(7) Uani 1 1 d . . .
H17 H 0.3705 0.4545 0.2656 0.026 Uiso 1 1 calc R . .
C18 C 0.3746(5) 0.3222(4) 0.1594(2) 0.0248(8) Uani 1 1 d . . .
C19 C 0.4693(5) 0.2464(3) 0.1317(2) 0.0244(8) Uani 1 1 d . . .
H19 H 0.4319 0.1919 0.0729 0.029 Uiso 1 1 calc R . .
C20 C 0.6265(4) 0.4907(3) 0.3933(2) 0.0184(7) Uani 1 1 d . . .
H20 H 0.5895 0.5605 0.4000 0.022 Uiso 1 1 calc R . .
C21 C 0.2164(6) 0.3220(4) 0.0985(3) 0.0343(10) Uani 1 1 d . . .
H21A H 0.2394 0.3971 0.0814 0.051 Uiso 1 1 calc R . .
H21B H 0.1227 0.3158 0.1297 0.051 Uiso 1 1 calc R . .
H21C H 0.1836 0.2528 0.0447 0.051 Uiso 1 1 calc R . .
N1 N 0.7662(4) 0.3434(3) 0.58324(19) 0.0174(6) Uani 1 1 d . . .
N2 N 0.8984(4) 0.0044(3) 0.31682(19) 0.0171(6) Uani 1 1 d . . .
N3 N 0.8209(4) 0.1305(3) 0.1922(2) 0.0219(6) Uani 1 1 d . . .
N4 N 0.7129(4) 0.4786(3) 0.46317(19) 0.0184(6) Uani 1 1 d . . .
O1 O 0.7587(3) 0.4453(2) 0.64091(16) 0.0233(6) Uani 1 1 d . . .
O2 O 0.7394(3) 0.5681(2) 0.54069(16) 0.0206(5) Uani 1 1 d . . .
S1 S 0.94795(10) 0.22122(7) 0.46462(5) 0.01534(18) Uani 1 1 d . . .
S2 S 0.87642(11) 0.34654(8) 0.34171(6) 0.01749(18) Uani 1 1 d . . .
Ni1 Ni 0.81836(6) 0.35616(4) 0.47175(3) 0.01556(12) Uani 1 1 d . . .
Ni2 Ni 0.88500(6) 0.16292(4) 0.32000(3) 0.01641(12) Uani 1 1 d . . .
H1O H 0.755(8) 0.519(6) 0.590(4) 0.08(2) Uiso 1 1 d . . .
F1 F 0.3646(5) 0.7162(4) 0.0887(2) 0.0821(12) Uani 1 1 d . . .
F2 F 0.4829(4) 0.8778(4) 0.20796(18) 0.0745(12) Uani 1 1 d . . .
F3 F 0.1987(3) 0.7834(3) 0.17654(17) 0.0429(6) Uani 1 1 d . . .
F4 F 0.2948(4) 0.9652(3) 0.1570(2) 0.0621(9) Uani 1 1 d . . .
F5 F 0.1746(3) 0.8008(3) 0.03682(18) 0.0508(8) Uani 1 1 d . . .
F6 F 0.4585(3) 0.9007(3) 0.06871(18) 0.0609(9) Uani 1 1 d . . .
P1 P 0.32891(14) 0.84049(12) 0.12248(7) 0.0348(3) Uani 1 1 d . . .
C31 C 0.8785(6) 0.6051(4) 0.2526(3) 0.0375(10) Uani 1 1 d . . .
H31 H 0.9754 0.5803 0.2699 0.045 Uiso 1 1 calc R . .
C32 C 0.6591(7) 0.6049(5) 0.1320(4) 0.0571(15) Uani 1 1 d . . .
H32A H 0.6107 0.6365 0.1818 0.086 Uiso 1 1 calc R . .
H32B H 0.5717 0.5346 0.0884 0.086 Uiso 1 1 calc R . .
H32C H 0.6963 0.6678 0.1028 0.086 Uiso 1 1 calc R . .
C33 C 0.8756(10) 0.5033(6) 0.1021(4) 0.0722(19) Uani 1 1 d . . .
H33A H 0.9281 0.5551 0.0678 0.108 Uiso 1 1 calc R . .
H33B H 0.7851 0.4324 0.0612 0.108 Uiso 1 1 calc R . .
H33C H 0.9632 0.4770 0.1341 0.108 Uiso 1 1 calc R . .
N31 N 0.8031(5) 0.5697(3) 0.1654(2) 0.0343(8) Uani 1 1 d . . .
O31 O 0.8330(5) 0.6666(3) 0.3117(2) 0.0422(8) Uani 1 1 d . . .
 
 
_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 N1 1.289(4) . ?
C1 C2 1.449(5) . ?
C1 H1 0.9500 . ?
C2 C3 1.401(5) . ?
C2 C7 1.402(5) . ?
C3 C4 1.403(5) . ?
C3 S1 1.758(3) . ?
C4 C5 1.402(5) . ?
C4 C8 1.460(5) . ?
C5 C6 1.386(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.374(5) . ?
C6 C9 1.507(5) . ?
C7 H7 0.9500 . ?
C8 N2 1.274(5) . ?
C8 H8 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 N2 1.486(4) . ?
C10 C11 1.508(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.506(6) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 N3 1.480(5) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 N3 1.282(5) . ?
C13 C14 1.457(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.397(5) . ?
C14 C19 1.398(5) . ?
C15 C16 1.400(5) . ?
C15 S2 1.766(3) . ?
C16 C17 1.394(5) . ?
C16 C20 1.459(5) . ?
C17 C18 1.392(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.386(5) . ?
C18 C21 1.499(5) . ?
C19 H19 0.9500 . ?
C20 N4 1.278(5) . ?
C20 H20 0.9500 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
N1 O1 1.362(4) . ?
N1 Ni1 1.909(3) . ?
N2 Ni2 1.917(3) . ?
N3 Ni2 1.921(3) . ?
N4 O2 1.368(4) . ?
N4 Ni1 1.911(3) . ?
O1 H1O 1.33(7) . ?
O2 H1O 1.09(7) . ?
S1 Ni1 2.1515(9) . ?
S1 Ni2 2.1588(9) . ?
S2 Ni2 2.1640(9) . ?
S2 Ni1 2.1660(9) . ?
F1 P1 1.577(4) . ?
F2 P1 1.591(3) . ?
F3 P1 1.596(3) . ?
F4 P1 1.578(3) . ?
F5 P1 1.591(3) . ?
F6 P1 1.604(3) . ?
C31 O31 1.220(6) . ?
C31 N31 1.335(6) . ?
C31 H31 0.9500 . ?
C32 N31 1.432(6) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 N31 1.434(7) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 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
N1 C1 C2 126.4(3) . . ?
N1 C1 H1 116.8 . . ?
C2 C1 H1 116.8 . . ?
C3 C2 C7 118.9(3) . . ?
C3 C2 C1 124.4(3) . . ?
C7 C2 C1 116.7(3) . . ?
C2 C3 C4 119.5(3) . . ?
C2 C3 S1 120.2(3) . . ?
C4 C3 S1 119.7(3) . . ?
C5 C4 C3 119.2(3) . . ?
C5 C4 C8 116.4(3) . . ?
C3 C4 C8 124.3(3) . . ?
C6 C5 C4 121.6(3) . . ?
C6 C5 H5 119.2 . . ?
C4 C5 H5 119.2 . . ?
C7 C6 C5 118.3(3) . . ?
C7 C6 C9 120.9(3) . . ?
C5 C6 C9 120.8(3) . . ?
C6 C7 C2 122.2(3) . . ?
C6 C7 H7 118.9 . . ?
C2 C7 H7 118.9 . . ?
N2 C8 C4 127.2(3) . . ?
N2 C8 H8 116.4 . . ?
C4 C8 H8 116.4 . . ?
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 . . ?
N2 C10 C11 112.9(3) . . ?
N2 C10 H10A 109.0 . . ?
C11 C10 H10A 109.0 . . ?
N2 C10 H10B 109.0 . . ?
C11 C10 H10B 109.0 . . ?
H10A C10 H10B 107.8 . . ?
C12 C11 C10 112.5(3) . . ?
C12 C11 H11A 109.1 . . ?
C10 C11 H11A 109.1 . . ?
C12 C11 H11B 109.1 . . ?
C10 C11 H11B 109.1 . . ?
H11A C11 H11B 107.8 . . ?
N3 C12 C11 111.6(3) . . ?
N3 C12 H12A 109.3 . . ?
C11 C12 H12A 109.3 . . ?
N3 C12 H12B 109.3 . . ?
C11 C12 H12B 109.3 . . ?
H12A C12 H12B 108.0 . . ?
N3 C13 C14 127.6(3) . . ?
N3 C13 H13 116.2 . . ?
C14 C13 H13 116.2 . . ?
C15 C14 C19 119.5(3) . . ?
C15 C14 C13 123.9(3) . . ?
C19 C14 C13 116.5(3) . . ?
C14 C15 C16 119.8(3) . . ?
C14 C15 S2 120.5(3) . . ?
C16 C15 S2 119.3(3) . . ?
C17 C16 C15 119.0(3) . . ?
C17 C16 C20 116.8(3) . . ?
C15 C16 C20 124.2(3) . . ?
C18 C17 C16 122.2(3) . . ?
C18 C17 H17 118.9 . . ?
C16 C17 H17 118.9 . . ?
C19 C18 C17 117.7(3) . . ?
C19 C18 C21 121.8(3) . . ?
C17 C18 C21 120.5(3) . . ?
C18 C19 C14 121.8(3) . . ?
C18 C19 H19 119.1 . . ?
C14 C19 H19 119.1 . . ?
N4 C20 C16 124.6(3) . . ?
N4 C20 H20 117.7 . . ?
C16 C20 H20 117.7 . . ?
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 . . ?
C1 N1 O1 113.8(3) . . ?
C1 N1 Ni1 129.0(2) . . ?
O1 N1 Ni1 117.1(2) . . ?
C8 N2 C10 114.6(3) . . ?
C8 N2 Ni2 127.6(2) . . ?
C10 N2 Ni2 117.7(2) . . ?
C13 N3 C12 116.0(3) . . ?
C13 N3 Ni2 125.6(3) . . ?
C12 N3 Ni2 118.4(2) . . ?
C20 N4 O2 115.3(3) . . ?
C20 N4 Ni1 128.3(2) . . ?
O2 N4 Ni1 116.2(2) . . ?
N1 O1 H1O 103(3) . . ?
N4 O2 H1O 101(3) . . ?
C3 S1 Ni1 104.69(11) . . ?
C3 S1 Ni2 104.25(12) . . ?
Ni1 S1 Ni2 93.55(4) . . ?
C15 S2 Ni2 103.30(12) . . ?
C15 S2 Ni1 101.99(12) . . ?
Ni2 S2 Ni1 92.99(4) . . ?
N1 Ni1 N4 95.24(12) . . ?
N1 Ni1 S1 92.72(9) . . ?
N4 Ni1 S1 172.02(9) . . ?
N1 Ni1 S2 172.64(9) . . ?
N4 Ni1 S2 91.23(9) . . ?
S1 Ni1 S2 80.85(3) . . ?
N2 Ni2 N3 95.41(13) . . ?
N2 Ni2 S1 92.07(9) . . ?
N3 Ni2 S1 172.36(10) . . ?
N2 Ni2 S2 172.79(9) . . ?
N3 Ni2 S2 91.78(10) . . ?
S1 Ni2 S2 80.73(3) . . ?
F1 P1 F4 179.5(2) . . ?
F1 P1 F2 89.4(2) . . ?
F4 P1 F2 90.1(2) . . ?
F1 P1 F5 89.7(2) . . ?
F4 P1 F5 90.83(19) . . ?
F2 P1 F5 179.0(2) . . ?
F1 P1 F3 91.0(2) . . ?
F4 P1 F3 89.10(16) . . ?
F2 P1 F3 89.94(17) . . ?
F5 P1 F3 89.69(15) . . ?
F1 P1 F6 90.4(2) . . ?
F4 P1 F6 89.54(19) . . ?
F2 P1 F6 90.25(17) . . ?
F5 P1 F6 90.15(15) . . ?
F3 P1 F6 178.63(19) . . ?
O31 C31 N31 125.3(4) . . ?
O31 C31 H31 117.4 . . ?
N31 C31 H31 117.4 . . ?
N31 C32 H32A 109.5 . . ?
N31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N31 C33 H33A 109.5 . . ?
N31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 N31 C32 121.8(4) . . ?
C31 N31 C33 119.6(5) . . ?
C32 N31 C33 118.4(5) . . ?
 
loop_
 _geom_hbond_atom_site_label_D
 _geom_hbond_atom_site_label_H
 _geom_hbond_atom_site_label_A
 _geom_hbond_distance_DH
 _geom_hbond_distance_HA
 _geom_hbond_distance_DA
 _geom_hbond_angle_DHA
 _geom_hbond_site_symmetry_A
O2 H1O O1  1.09(7) 1.33(7) 2.414(4) 172(6) .
 
_diffrn_measured_fraction_theta_max    0.997
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.997
_refine_diff_density_max    0.746
_refine_diff_density_min   -0.520
_refine_diff_density_rms    0.103
