data_05src0098
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 Dr. S. Lancaster
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          
 'C25 H27 CL3 N2 O2 Ti, C4 H8 O'
_chemical_formula_sum
 'C29 H35 Cl3 N2 O3 Ti'
_chemical_formula_weight          613.84
 
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'
 'Cl'  'Cl'   0.1484   0.1585
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Ti'  'Ti'   0.2776   0.4457
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            monoclinic
_symmetry_space_group_name_H-M    P2(1)/n
_symmetry_space_group_name_hall   '-P 2yn'
 
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                    7.6644(6)
_cell_length_b                    28.644(4)
_cell_length_c                    13.768(2)
_cell_angle_alpha                 90.00
_cell_angle_beta                  104.291(9)
_cell_angle_gamma                 90.00
_cell_volume                      2929.1(7)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     6243
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Shard
_exptl_crystal_colour             Red
_exptl_crystal_size_max           0.19
_exptl_crystal_size_mid           0.13
_exptl_crystal_size_min           0.04
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.392
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1280
_exptl_absorpt_coefficient_mu     0.599
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.8947
_exptl_absorpt_correction_T_max   0.9764
_exptl_absorpt_process_details       'SADABS V2.10 (Sheldrick, G.M., 2003)'

_diffrn_ambient_temperature           120(2)
_diffrn_radiation_wavelength           0.71073
_diffrn_radiation_type                      MoK\a
_diffrn_radiation_source                  'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator    '10cm confocal mirrors'
_diffrn_measurement_device_type  'Bruker-Nonius 95mm CCD camera on κ-goniostat'
_diffrn_measurement_method          'φ & ω scans'
_diffrn_detector_area_resol_mean   9.091
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             30451
_diffrn_reflns_av_R_equivalents   0.0520
_diffrn_reflns_av_sigmaI/netI     0.0509
_diffrn_reflns_limit_h_min        -9
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        -37
_diffrn_reflns_limit_k_max        37
_diffrn_reflns_limit_l_min        -17
_diffrn_reflns_limit_l_max        17
_diffrn_reflns_theta_min          3.05
_diffrn_reflns_theta_max          27.48
_reflns_number_total              6636
_reflns_number_gt                 5018
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997a)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997b)' 
_computing_molecular_graphics     'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0333P)²+2.5843P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          6636
_refine_ls_number_parameters      347
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0681
_refine_ls_R_factor_gt            0.0443
_refine_ls_wR_factor_ref          0.1011
_refine_ls_wR_factor_gt           0.0920
_refine_ls_goodness_of_fit_ref    1.030
_refine_ls_restrained_S_all       1.030
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
C1 C 0.4350(3) 0.16863(8) 0.22376(17) 0.0214(5) Uani 1 1 d . . .
C2 C 0.3701(3) 0.18488(8) 0.12483(16) 0.0219(5) Uani 1 1 d . . .
C3 C 0.4818(3) 0.21609(8) 0.09101(18) 0.0257(5) Uani 1 1 d . . .
H3 H 0.4424 0.2281 0.0249 0.031 Uiso 1 1 calc R . .
C4 C 0.6473(3) 0.23035(9) 0.14922(18) 0.0280(6) Uani 1 1 d . . .
H4 H 0.7172 0.2524 0.1236 0.034 Uiso 1 1 calc R . .
C5 C 0.7105(3) 0.21252(8) 0.24443(18) 0.0264(5) Uani 1 1 d . . .
H5 H 0.8260 0.2213 0.2836 0.032 Uiso 1 1 calc R . .
C6 C 0.6043(3) 0.18161(8) 0.28294(17) 0.0216(5) Uani 1 1 d . . .
C7 C 0.6776(3) 0.16364(8) 0.38295(17) 0.0219(5) Uani 1 1 d . . .
H7 H 0.7997 0.1714 0.4127 0.026 Uiso 1 1 calc R . .
C8 C 0.7062(3) 0.12848(8) 0.53614(16) 0.0209(5) Uani 1 1 d . . .
C9 C 0.7152(3) 0.08398(8) 0.57564(17) 0.0233(5) Uani 1 1 d . . .
H9 H 0.6484 0.0593 0.5376 0.028 Uiso 1 1 calc R . .
C10 C 0.8220(3) 0.07539(9) 0.67097(18) 0.0270(5) Uani 1 1 d . . .
H10 H 0.8285 0.0447 0.6979 0.032 Uiso 1 1 calc R . .
C11 C 0.9190(3) 0.11093(9) 0.72702(18) 0.0289(6) Uani 1 1 d . . .
H11 H 0.9921 0.1047 0.7922 0.035 Uiso 1 1 calc R . .
C12 C 0.9095(3) 0.15556(9) 0.68812(18) 0.0294(6) Uani 1 1 d . . .
H12 H 0.9765 0.1801 0.7265 0.035 Uiso 1 1 calc R . .
C13 C 0.8027(3) 0.16454(8) 0.59349(17) 0.0255(5) Uani 1 1 d . . .
H13 H 0.7949 0.1954 0.5673 0.031 Uiso 1 1 calc R . .
C14 C 0.1865(3) 0.16996(8) 0.05964(17) 0.0246(5) Uani 1 1 d . . .
C15 C 0.0377(3) 0.18652(9) 0.10815(18) 0.0303(6) Uani 1 1 d . . .
H15A H 0.0575 0.1731 0.1755 0.045 Uiso 1 1 calc R . .
H15B H -0.0796 0.1764 0.0672 0.045 Uiso 1 1 calc R . .
H15C H 0.0401 0.2207 0.1128 0.045 Uiso 1 1 calc R . .
C16 C 0.1787(4) 0.11680(9) 0.04641(19) 0.0325(6) Uani 1 1 d . . .
H16A H 0.2740 0.1067 0.0150 0.049 Uiso 1 1 calc R . .
H16B H 0.0612 0.1079 0.0037 0.049 Uiso 1 1 calc R . .
H16C H 0.1958 0.1018 0.1121 0.049 Uiso 1 1 calc R . .
C17 C 0.1484(4) 0.19179(10) -0.04572(18) 0.0326(6) Uani 1 1 d . . .
H17A H 0.1449 0.2259 -0.0402 0.049 Uiso 1 1 calc R . .
H17B H 0.0322 0.1805 -0.0860 0.049 Uiso 1 1 calc R . .
H17C H 0.2439 0.1829 -0.0781 0.049 Uiso 1 1 calc R . .
C21 C 0.1655(3) 0.03522(8) 0.55124(19) 0.0286(6) Uani 1 1 d . . .
H21A H 0.0502 0.0453 0.5079 0.043 Uiso 1 1 calc R . .
H21B H 0.1438 0.0175 0.6080 0.043 Uiso 1 1 calc R . .
H21C H 0.2286 0.0154 0.5129 0.043 Uiso 1 1 calc R . .
C22 C 0.2772(3) 0.07673(8) 0.58896(17) 0.0216(5) Uani 1 1 d . . .
C23 C 0.4274(3) 0.11904(8) 0.74461(17) 0.0214(5) Uani 1 1 d . . .
C24 C 0.5038(4) 0.10888(9) 0.84469(18) 0.0301(6) Uani 1 1 d . . .
H24 H 0.4879 0.0789 0.8706 0.036 Uiso 1 1 calc R . .
C25 C 0.6030(4) 0.14254(9) 0.90659(19) 0.0328(6) Uani 1 1 d . . .
H25 H 0.6552 0.1356 0.9751 0.039 Uiso 1 1 calc R . .
C26 C 0.6263(3) 0.18603(8) 0.86958(18) 0.0274(5) Uani 1 1 d . . .
H26 H 0.6948 0.2091 0.9120 0.033 Uiso 1 1 calc R . .
C27 C 0.5494(3) 0.19584(8) 0.77029(18) 0.0266(5) Uani 1 1 d . . .
H27 H 0.5658 0.2259 0.7448 0.032 Uiso 1 1 calc R . .
C28 C 0.4489(3) 0.16295(8) 0.70690(17) 0.0247(5) Uani 1 1 d . . .
H28 H 0.3956 0.1703 0.6388 0.030 Uiso 1 1 calc R . .
N1 N 0.5981(2) 0.13844(6) 0.43683(14) 0.0192(4) Uani 1 1 d . . .
N21 N 0.3250(3) 0.08275(7) 0.68739(14) 0.0238(4) Uani 1 1 d . . .
H21 H 0.2875 0.0610 0.7225 0.029 Uiso 1 1 calc R . .
O1 O 0.3368(2) 0.13920(5) 0.26487(11) 0.0219(3) Uani 1 1 d . . .
O21 O 0.3244(2) 0.10512(5) 0.53028(11) 0.0200(3) Uani 1 1 d . . .
Cl1 Cl 0.00885(8) 0.10097(2) 0.33208(5) 0.03064(15) Uani 1 1 d . . .
Cl2 Cl 0.39710(8) 0.04303(2) 0.36347(4) 0.02752(14) Uani 1 1 d . . .
Cl3 Cl 0.25276(9) 0.19563(2) 0.42934(5) 0.03029(15) Uani 1 1 d . . .
Ti1 Ti 0.30770(5) 0.119234(14) 0.38442(3) 0.01914(11) Uani 1 1 d . . .
C31 C 0.3504(4) -0.02725(11) 0.8112(2) 0.0442(7) Uani 1 1 d . . .
H31A H 0.4759 -0.0158 0.8242 0.053 Uiso 1 1 calc R . .
H31B H 0.3222 -0.0448 0.7472 0.053 Uiso 1 1 calc R . .
C32 C 0.3271(4) -0.05810(11) 0.8959(2) 0.0477(8) Uani 1 1 d . . .
H32A H 0.4452 -0.0673 0.9395 0.057 Uiso 1 1 calc R . .
H32B H 0.2581 -0.0866 0.8701 0.057 Uiso 1 1 calc R . .
C33 C 0.2231(5) -0.02734(12) 0.9524(2) 0.0544(9) Uani 1 1 d . . .
H33A H 0.1466 -0.0461 0.9859 0.065 Uiso 1 1 calc R . .
H33B H 0.3048 -0.0075 1.0026 0.065 Uiso 1 1 calc R . .
C34 C 0.1124(4) 0.00104(10) 0.8686(2) 0.0417(7) Uani 1 1 d . . .
H34A H 0.0060 -0.0168 0.8317 0.050 Uiso 1 1 calc R . .
H34B H 0.0708 0.0302 0.8944 0.050 Uiso 1 1 calc R . .
O31 O 0.2281(3) 0.01105(7) 0.80614(15) 0.0472(5) Uani 1 1 d . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
C1 O1 1.344(3) . ?
C1 C6 1.401(3) . ?
C1 C2 1.409(3) . ?
C2 C3 1.395(3) . ?
C2 C14 1.532(3) . ?
C3 C4 1.385(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.378(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.393(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.447(3) . ?
C7 N1 1.291(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.381(3) . ?
C8 C13 1.396(3) . ?
C8 N1 1.442(3) . ?
C9 C10 1.387(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.379(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.381(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.381(3) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.532(3) . ?
C14 C16 1.533(3) . ?
C14 C17 1.540(3) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C21 C22 1.482(3) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 O21 1.261(3) . ?
C22 N21 1.325(3) . ?
C23 C28 1.386(3) . ?
C23 C24 1.388(3) . ?
C23 N21 1.419(3) . ?
C24 C25 1.383(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.374(3) . ?
C25 H25 0.9500 . ?
C26 C27 1.377(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.382(3) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
N1 Ti1 2.2323(19) . ?
N21 H21 0.8800 . ?
O1 Ti1 1.8077(16) . ?
O21 Ti1 2.0213(16) . ?
Cl1 Ti1 2.2857(7) . ?
Cl2 Ti1 2.3271(8) . ?
Cl3 Ti1 2.3404(8) . ?
C31 O31 1.434(4) . ?
C31 C32 1.509(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.524(5) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.492(4) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 O31 1.409(3) . ?
C34 H34A 0.9900 . ?
C34 H34B 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
O1 C1 C6 117.1(2) . . ?
O1 C1 C2 120.9(2) . . ?
C6 C1 C2 122.0(2) . . ?
C3 C2 C1 115.8(2) . . ?
C3 C2 C14 122.3(2) . . ?
C1 C2 C14 121.9(2) . . ?
C4 C3 C2 123.1(2) . . ?
C4 C3 H3 118.4 . . ?
C2 C3 H3 118.4 . . ?
C5 C4 C3 119.8(2) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 119.8(2) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C5 C6 C1 119.4(2) . . ?
C5 C6 C7 117.5(2) . . ?
C1 C6 C7 123.0(2) . . ?
N1 C7 C6 128.2(2) . . ?
N1 C7 H7 115.9 . . ?
C6 C7 H7 115.9 . . ?
C9 C8 C13 119.5(2) . . ?
C9 C8 N1 121.2(2) . . ?
C13 C8 N1 119.4(2) . . ?
C8 C9 C10 119.8(2) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
C11 C10 C9 120.6(2) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C10 C11 C12 119.8(2) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C13 C12 C11 120.0(2) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C12 C13 C8 120.2(2) . . ?
C12 C13 H13 119.9 . . ?
C8 C13 H13 119.9 . . ?
C2 C14 C15 109.46(19) . . ?
C2 C14 C16 110.49(19) . . ?
C15 C14 C16 110.4(2) . . ?
C2 C14 C17 111.8(2) . . ?
C15 C14 C17 107.3(2) . . ?
C16 C14 C17 107.4(2) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
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 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O21 C22 N21 121.4(2) . . ?
O21 C22 C21 121.7(2) . . ?
N21 C22 C21 116.9(2) . . ?
C28 C23 C24 120.1(2) . . ?
C28 C23 N21 123.9(2) . . ?
C24 C23 N21 115.9(2) . . ?
C25 C24 C23 119.9(2) . . ?
C25 C24 H24 120.1 . . ?
C23 C24 H24 120.1 . . ?
C26 C25 C24 120.4(2) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C25 C26 C27 119.3(2) . . ?
C25 C26 H26 120.3 . . ?
C27 C26 H26 120.3 . . ?
C26 C27 C28 121.5(2) . . ?
C26 C27 H27 119.2 . . ?
C28 C27 H27 119.2 . . ?
C27 C28 C23 118.8(2) . . ?
C27 C28 H28 120.6 . . ?
C23 C28 H28 120.6 . . ?
C7 N1 C8 114.40(19) . . ?
C7 N1 Ti1 121.78(15) . . ?
C8 N1 Ti1 123.48(14) . . ?
C22 N21 C23 129.7(2) . . ?
C22 N21 H21 115.2 . . ?
C23 N21 H21 115.2 . . ?
C1 O1 Ti1 142.14(14) . . ?
C22 O21 Ti1 143.90(15) . . ?
O1 Ti1 O21 167.47(7) . . ?
O1 Ti1 N1 83.05(7) . . ?
O21 Ti1 N1 85.10(7) . . ?
O1 Ti1 Cl1 97.17(5) . . ?
O21 Ti1 Cl1 94.60(5) . . ?
N1 Ti1 Cl1 178.83(5) . . ?
O1 Ti1 Cl2 94.45(5) . . ?
O21 Ti1 Cl2 89.27(5) . . ?
N1 Ti1 Cl2 88.32(5) . . ?
Cl1 Ti1 Cl2 92.81(3) . . ?
O1 Ti1 Cl3 90.89(5) . . ?
O21 Ti1 Cl3 84.02(5) . . ?
N1 Ti1 Cl3 85.08(5) . . ?
Cl1 Ti1 Cl3 93.76(3) . . ?
Cl2 Ti1 Cl3 170.96(3) . . ?
O31 C31 C32 106.6(2) . . ?
O31 C31 H31A 110.4 . . ?
C32 C31 H31A 110.4 . . ?
O31 C31 H31B 110.4 . . ?
C32 C31 H31B 110.4 . . ?
H31A C31 H31B 108.6 . . ?
C31 C32 C33 103.4(2) . . ?
C31 C32 H32A 111.1 . . ?
C33 C32 H32A 111.1 . . ?
C31 C32 H32B 111.1 . . ?
C33 C32 H32B 111.1 . . ?
H32A C32 H32B 109.0 . . ?
C34 C33 C32 101.0(2) . . ?
C34 C33 H33A 111.6 . . ?
C32 C33 H33A 111.6 . . ?
C34 C33 H33B 111.6 . . ?
C32 C33 H33B 111.6 . . ?
H33A C33 H33B 109.4 . . ?
O31 C34 C33 105.0(2) . . ?
O31 C34 H34A 110.7 . . ?
C33 C34 H34A 110.7 . . ?
O31 C34 H34B 110.7 . . ?
C33 C34 H34B 110.7 . . ?
H34A C34 H34B 108.8 . . ?
C34 O31 C31 108.5(2) . . ?
 
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
N21 H21 O31  0.88 1.96 2.836(3) 174.6 .
 
_diffrn_measured_fraction_theta_max    0.989
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.989
_refine_diff_density_max    0.621
_refine_diff_density_min   -0.369
_refine_diff_density_rms    0.066
