 
data_s92
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C17 H29 Br N2 O'
_chemical_formula_weight          357.33
 
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'
 'Br'  'Br'  -0.2901   2.4595
 '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'
 
 
_symmetry_cell_setting            Monoclinic
_symmetry_space_group_name_H-M    P2(1)
_symmetry_space_group_name_hall   'P 2yb'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, y+1/2, -z'
 
_cell_length_a                    8.6737(2)
_cell_length_b                    22.2346(4)
_cell_length_c                    9.8649(2)
_cell_angle_alpha                 90.00
_cell_angle_beta                  104.9240(10)
_cell_angle_gamma                 90.00
_cell_volume                      1838.33(7)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     7747
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        rod
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.48
_exptl_crystal_size_mid           0.14
_exptl_crystal_size_min           0.12
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.291
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              752
_exptl_absorpt_coefficient_mu     2.238
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.4130
_exptl_absorpt_correction_T_max   0.7750
_exptl_absorpt_process_details    'SORTAV (Blessing, 1997)'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       120(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'Enraf Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Enraf Nonius KappaCCD area detector'
_diffrn_measurement_method        'ω and φ scans to fill Ewald sphere'
_diffrn_detector_area_resol_mean  '9.091 pixels/mm'
_diffrn_standards_number          'n/a'
_diffrn_standards_interval_count  'n/a'
_diffrn_standards_interval_time   'n/a'
_diffrn_standards_decay_%         'n/a'
_diffrn_reflns_number             14259
_diffrn_reflns_av_R_equivalents   0.0410
_diffrn_reflns_av_sigmaI/netI     0.0487
_diffrn_reflns_limit_h_min        -10
_diffrn_reflns_limit_h_max        11
_diffrn_reflns_limit_k_min        -28
_diffrn_reflns_limit_k_max        26
_diffrn_reflns_limit_l_min        -12
_diffrn_reflns_limit_l_max        12
_diffrn_reflns_theta_min          2.94
_diffrn_reflns_theta_max          27.47
_reflns_number_total              7353
_reflns_number_gt                 6655
_reflns_threshold_expression      >2σ(I)
 
_computing_data_collection        
;
'DENZO (Otwinowski and Minor, 1997) & COLLECT (Hooft, 1998) '
;
_computing_cell_refinement        'DENZO and COLLECT'
_computing_data_reduction         'DENZO and COLLECT'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_computing_molecular_graphics     ?
_computing_publication_material   SHELXL-97
 
_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)+(0.0239P)²+2.0927P] 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        0.0091(6)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_abs_structure_details
 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack    0.342(10)
_refine_ls_number_reflns          7353
_refine_ls_number_parameters      421
_refine_ls_number_restraints      2
_refine_ls_R_factor_all           0.0480
_refine_ls_R_factor_gt            0.0403
_refine_ls_wR_factor_ref          0.0895
_refine_ls_wR_factor_gt           0.0854
_refine_ls_goodness_of_fit_ref    1.037
_refine_ls_restrained_S_all       1.037
_refine_ls_shift/su_max           0.003
_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 0.995(2) 0.2792(7) 0.714(2) 0.107(6) Uani 0.649(18) 1 d P A 1
H1A H 0.8978 0.2748 0.6381 0.160 Uiso 0.649(18) 1 calc PR A 1
H1B H 0.9709 0.2702 0.8041 0.160 Uiso 0.649(18) 1 calc PR A 1
H1C H 1.0765 0.2513 0.6997 0.160 Uiso 0.649(18) 1 calc PR A 1
C2 C 1.0519(11) 0.3387(5) 0.7167(11) 0.063(3) Uani 0.649(18) 1 d PD A 1
H2A H 1.0556 0.3511 0.6212 0.075 Uiso 0.649(18) 1 calc PR A 1
H2B H 1.1609 0.3415 0.7795 0.075 Uiso 0.649(18) 1 calc PR A 1
C1' C 1.039(3) 0.3094(10) 0.630(2) 0.079(7) Uani 0.351(18) 1 d P A 2
H1'1 H 1.1383 0.3326 0.6504 0.119 Uiso 0.351(18) 1 calc PR A 2
H1'2 H 0.9617 0.3274 0.5499 0.119 Uiso 0.351(18) 1 calc PR A 2
H1'3 H 1.0608 0.2678 0.6071 0.119 Uiso 0.351(18) 1 calc PR A 2
C2' C 0.970(2) 0.3097(10) 0.760(2) 0.064(6) Uani 0.351(18) 1 d P A 2
H2'1 H 1.0484 0.2949 0.8447 0.076 Uiso 0.351(18) 1 calc PR A 2
H2'2 H 0.8713 0.2853 0.7440 0.076 Uiso 0.351(18) 1 calc PR A 2
C3 C 0.9321(10) 0.3812(3) 0.7727(7) 0.088(3) Uani 1 1 d D . .
H3A H 0.8318 0.3884 0.6995 0.105 Uiso 1 1 calc R A 1
H3B H 0.9069 0.3643 0.8573 0.105 Uiso 1 1 calc R A 1
C4 C 1.0279(7) 0.4360(4) 0.8051(5) 0.071(2) Uani 1 1 d . A .
H4A H 1.0667 0.4469 0.7224 0.085 Uiso 1 1 calc R . .
H4B H 1.1225 0.4274 0.8834 0.085 Uiso 1 1 calc R . .
C5 C 0.9428(5) 0.4880(3) 0.8438(4) 0.0439(13) Uani 1 1 d . . .
H5A H 1.0156 0.5231 0.8618 0.053 Uiso 1 1 calc R A .
H5B H 0.8514 0.4982 0.7639 0.053 Uiso 1 1 calc R . .
C6 C 0.7345(5) 0.46981(19) 0.9703(4) 0.0281(9) Uani 1 1 d . . .
H6 H 0.6463 0.4720 0.8901 0.034 Uiso 1 1 calc R A .
C7 C 0.9784(4) 0.47085(18) 1.1050(4) 0.0231(8) Uani 1 1 d . . .
C8 C 1.1418(4) 0.47629(19) 1.1599(4) 0.0285(9) Uani 1 1 d . A .
H8 H 1.2113 0.4853 1.1024 0.034 Uiso 1 1 calc R . .
C9 C 1.1977(5) 0.4679(2) 1.3024(4) 0.0311(10) Uani 1 1 d . . .
H9 H 1.3089 0.4708 1.3447 0.037 Uiso 1 1 calc R A .
C10 C 1.0932(5) 0.4551(2) 1.3866(4) 0.0331(9) Uani 1 1 d . A .
H10 H 1.1360 0.4491 1.4845 0.040 Uiso 1 1 calc R . .
C11 C 0.9314(5) 0.4511(2) 1.3316(4) 0.0307(10) Uani 1 1 d . . .
H11 H 0.8610 0.4433 1.3890 0.037 Uiso 1 1 calc R A .
C12 C 0.8756(4) 0.45905(18) 1.1875(4) 0.0236(8) Uani 1 1 d . A .
C13 C 0.5728(5) 0.4502(2) 1.1406(4) 0.0338(9) Uani 1 1 d . . .
H13A H 0.4846 0.4695 1.0701 0.041 Uiso 1 1 calc R A .
H13B H 0.5815 0.4705 1.2317 0.041 Uiso 1 1 calc R . .
C14 C 0.5320(5) 0.3851(2) 1.1540(5) 0.0404(11) Uani 1 1 d . A .
H14A H 0.4385 0.3827 1.1939 0.048 Uiso 1 1 calc R . .
H14B H 0.6228 0.3652 1.2204 0.048 Uiso 1 1 calc R . .
C15 C 0.4945(7) 0.3513(2) 1.0148(6) 0.0562(14) Uani 1 1 d . . .
H15A H 0.5947 0.3449 0.9864 0.067 Uiso 1 1 calc R A .
H15B H 0.4230 0.3763 0.9419 0.067 Uiso 1 1 calc R . .
C16 C 0.4140(8) 0.2897(3) 1.0223(7) 0.0712(17) Uani 1 1 d . A .
H16A H 0.3175 0.2959 1.0567 0.085 Uiso 1 1 calc R . .
H16B H 0.3795 0.2725 0.9267 0.085 Uiso 1 1 calc R . .
C17 C 0.5179(12) 0.2472(3) 1.1132(8) 0.100(3) Uani 1 1 d . . .
H17A H 0.5592 0.2651 1.2062 0.149 Uiso 1 1 calc R A .
H17B H 0.6070 0.2369 1.0734 0.149 Uiso 1 1 calc R . .
H17C H 0.4577 0.2106 1.1215 0.149 Uiso 1 1 calc R . .
C18 C 1.5264(9) 0.8332(3) 1.5084(7) 0.0727(19) Uani 1 1 d . . .
H18A H 1.6055 0.8143 1.5857 0.109 Uiso 1 1 calc R . .
H18B H 1.4238 0.8357 1.5324 0.109 Uiso 1 1 calc R . .
H18C H 1.5624 0.8738 1.4923 0.109 Uiso 1 1 calc R . .
C19 C 1.5073(7) 0.7962(2) 1.3773(6) 0.0561(14) Uani 1 1 d . . .
H19A H 1.4253 0.8150 1.3003 0.067 Uiso 1 1 calc R . .
H19B H 1.6093 0.7963 1.3497 0.067 Uiso 1 1 calc R . .
C20 C 1.4598(5) 0.7322(2) 1.3957(5) 0.0390(10) Uani 1 1 d . . .
H20A H 1.3629 0.7323 1.4312 0.047 Uiso 1 1 calc R . .
H20B H 1.5462 0.7125 1.4673 0.047 Uiso 1 1 calc R . .
C21 C 1.4267(5) 0.6956(2) 1.2610(4) 0.0353(10) Uani 1 1 d . . .
H21A H 1.3358 0.7140 1.1914 0.042 Uiso 1 1 calc R . .
H21B H 1.5211 0.6978 1.2223 0.042 Uiso 1 1 calc R . .
C22 C 1.3890(5) 0.6307(2) 1.2795(4) 0.0324(9) Uani 1 1 d . . .
H22A H 1.3816 0.6090 1.1904 0.039 Uiso 1 1 calc R . .
H22B H 1.4773 0.6126 1.3522 0.039 Uiso 1 1 calc R . .
C23 C 1.2271(5) 0.61348(19) 1.4498(4) 0.0286(9) Uani 1 1 d . . .
H23 H 1.3147 0.6114 1.5305 0.034 Uiso 1 1 calc R . .
C24 C 1.0875(5) 0.6238(2) 1.2308(4) 0.0258(9) Uani 1 1 d . . .
C25 C 1.0324(5) 0.6314(2) 1.0866(4) 0.0313(9) Uani 1 1 d . . .
H25 H 1.1030 0.6389 1.0291 0.038 Uiso 1 1 calc R . .
C26 C 0.8709(5) 0.6276(2) 1.0322(4) 0.0355(10) Uani 1 1 d . . .
H26 H 0.8290 0.6332 0.9342 0.043 Uiso 1 1 calc R . .
C27 C 0.7646(5) 0.6158(2) 1.1139(4) 0.0315(9) Uani 1 1 d . . .
H27 H 0.6537 0.6129 1.0703 0.038 Uiso 1 1 calc R . .
C28 C 0.8192(5) 0.6084(2) 1.2579(4) 0.0305(10) Uani 1 1 d . . .
H28 H 0.7485 0.6002 1.3149 0.037 Uiso 1 1 calc R . .
C29 C 0.9810(5) 0.61344(18) 1.3137(4) 0.0260(8) Uani 1 1 d . . .
C30 C 1.0141(6) 0.5962(2) 1.5738(4) 0.0402(11) Uani 1 1 d . . .
H30A H 1.1032 0.5841 1.6539 0.048 Uiso 1 1 calc R . .
H30B H 0.9367 0.5626 1.5531 0.048 Uiso 1 1 calc R . .
C31 C 0.9344(6) 0.6503(3) 1.6138(5) 0.0625(17) Uani 1 1 d . . .
H31A H 0.8544 0.6648 1.5294 0.075 Uiso 1 1 calc R . .
H31B H 0.8758 0.6379 1.6831 0.075 Uiso 1 1 calc R . .
C32 C 1.0402(10) 0.7013(3) 1.6736(7) 0.094(3) Uani 1 1 d . . .
H32A H 1.0959 0.7156 1.6039 0.112 Uiso 1 1 calc R . .
H32B H 1.1217 0.6875 1.7577 0.112 Uiso 1 1 calc R . .
C33 C 0.9443(18) 0.7529(5) 1.7138(12) 0.200(8) Uani 1 1 d . . .
H33A H 0.8984 0.7755 1.6262 0.240 Uiso 1 1 calc R . .
H33B H 0.8532 0.7341 1.7410 0.240 Uiso 1 1 calc R . .
C34 C 1.0005(15) 0.7918(5) 1.8066(11) 0.148(5) Uani 1 1 d . . .
H34A H 1.0687 0.8197 1.7716 0.222 Uiso 1 1 calc R . .
H34B H 1.0636 0.7717 1.8912 0.222 Uiso 1 1 calc R . .
H34C H 0.9128 0.8141 1.8291 0.222 Uiso 1 1 calc R . .
N1 N 0.8845(4) 0.47689(16) 0.9677(3) 0.0277(7) Uani 1 1 d . A .
N2 N 0.7225(4) 0.45929(15) 1.0992(3) 0.0261(7) Uani 1 1 d . A .
N3 N 1.2397(4) 0.62305(15) 1.3203(3) 0.0272(7) Uani 1 1 d . . .
N4 N 1.0759(4) 0.60728(16) 1.4510(3) 0.0280(8) Uani 1 1 d . . .
Br1 Br 0.62293(4) 0.50916(2) 0.51172(4) 0.03659(12) Uani 1 1 d . . .
O1 O 0.4023(5) 0.4543(2) 0.7146(4) 0.0521(10) Uani 1 1 d . . .
O2 O 1.5610(5) 0.6235(2) 1.7011(4) 0.0550(10) Uani 1 1 d . . .
H1O H 0.459(7) 0.470(3) 0.643(6) 0.067(17) Uiso 1 1 d . . .
H2O H 0.378(7) 0.482(3) 0.743(6) 0.050(19) Uiso 1 1 d . . .
H3O H 1.589(7) 0.593(3) 1.652(6) 0.062(18) Uiso 1 1 d . . .
H4O H 1.512(8) 0.610(3) 1.768(8) 0.09(2) Uiso 1 1 d . . .
Br2 Br 0.34041(4) 0.570763(19) 0.90578(4) 0.03547(11) 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 C2 1.410(18) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.605(11) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C1' C2' 1.55(3) . ?
C1' H1'1 0.9800 . ?
C1' H1'2 0.9800 . ?
C1' H1'3 0.9800 . ?
C2' C3 1.63(2) . ?
C2' H2'1 0.9900 . ?
C2' H2'2 0.9900 . ?
C3 C4 1.463(10) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.475(8) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N1 1.459(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 N1 1.318(5) . ?
C6 N2 1.323(5) . ?
C6 H6 0.9500 . ?
C7 C12 1.378(5) . ?
C7 C8 1.386(5) . ?
C7 N1 1.396(5) . ?
C8 C9 1.377(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.407(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.371(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.390(5) . ?
C11 H11 0.9500 . ?
C12 N2 1.387(5) . ?
C13 N2 1.472(5) . ?
C13 C14 1.503(7) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.525(7) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.548(8) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.447(10) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.506(8) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.505(7) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.521(6) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.501(6) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 N3 1.462(5) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 N4 1.322(5) . ?
C23 N3 1.327(5) . ?
C23 H23 0.9500 . ?
C24 N3 1.386(5) . ?
C24 C25 1.389(5) . ?
C24 C29 1.401(5) . ?
C25 C26 1.368(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.396(6) . ?
C26 H26 0.9500 . ?
C27 C28 1.387(5) . ?
C27 H27 0.9500 . ?
C28 C29 1.374(6) . ?
C28 H28 0.9500 . ?
C29 N4 1.399(5) . ?
C30 N4 1.467(5) . ?
C30 C31 1.491(8) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.482(10) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.529(12) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.262(13) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
O1 H1O 1.02(6) . ?
O1 H2O 0.72(5) . ?
O2 H3O 0.89(6) . ?
O2 H4O 0.92(7) . ?
 
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
C1 C2 C3 107.6(10) . . ?
C1 C2 H2A 110.2 . . ?
C3 C2 H2A 110.2 . . ?
C1 C2 H2B 110.2 . . ?
C3 C2 H2B 110.2 . . ?
H2A C2 H2B 108.5 . . ?
C2' C1' H1'1 109.5 . . ?
C2' C1' H1'2 109.5 . . ?
H1'1 C1' H1'2 109.5 . . ?
C2' C1' H1'3 109.5 . . ?
H1'1 C1' H1'3 109.5 . . ?
H1'2 C1' H1'3 109.5 . . ?
C1' C2' C3 101.3(15) . . ?
C1' C2' H2'1 111.5 . . ?
C3 C2' H2'1 111.5 . . ?
C1' C2' H2'2 111.5 . . ?
C3 C2' H2'2 111.5 . . ?
H2'1 C2' H2'2 109.3 . . ?
C4 C3 C2 100.6(7) . . ?
C4 C3 C2' 135.5(9) . . ?
C4 C3 H3A 111.6 . . ?
C2 C3 H3A 111.6 . . ?
C2' C3 H3A 104.8 . . ?
C4 C3 H3B 111.6 . . ?
C2 C3 H3B 111.6 . . ?
C2' C3 H3B 77.6 . . ?
H3A C3 H3B 109.4 . . ?
C3 C4 C5 114.6(5) . . ?
C3 C4 H4A 108.6 . . ?
C5 C4 H4A 108.6 . . ?
C3 C4 H4B 108.6 . . ?
C5 C4 H4B 108.6 . . ?
H4A C4 H4B 107.6 . . ?
N1 C5 C4 112.8(4) . . ?
N1 C5 H5A 109.0 . . ?
C4 C5 H5A 109.0 . . ?
N1 C5 H5B 109.0 . . ?
C4 C5 H5B 109.0 . . ?
H5A C5 H5B 107.8 . . ?
N1 C6 N2 111.2(3) . . ?
N1 C6 H6 124.4 . . ?
N2 C6 H6 124.4 . . ?
C12 C7 C8 122.5(4) . . ?
C12 C7 N1 106.7(3) . . ?
C8 C7 N1 130.8(4) . . ?
C9 C8 C7 116.3(4) . . ?
C9 C8 H8 121.8 . . ?
C7 C8 H8 121.8 . . ?
C8 C9 C10 121.3(4) . . ?
C8 C9 H9 119.4 . . ?
C10 C9 H9 119.4 . . ?
C11 C10 C9 121.9(4) . . ?
C11 C10 H10 119.0 . . ?
C9 C10 H10 119.0 . . ?
C10 C11 C12 116.6(4) . . ?
C10 C11 H11 121.7 . . ?
C12 C11 H11 121.7 . . ?
C7 C12 N2 106.8(3) . . ?
C7 C12 C11 121.3(4) . . ?
N2 C12 C11 131.8(3) . . ?
N2 C13 C14 113.6(3) . . ?
N2 C13 H13A 108.8 . . ?
C14 C13 H13A 108.8 . . ?
N2 C13 H13B 108.8 . . ?
C14 C13 H13B 108.8 . . ?
H13A C13 H13B 107.7 . . ?
C13 C14 C15 113.3(4) . . ?
C13 C14 H14A 108.9 . . ?
C15 C14 H14A 108.9 . . ?
C13 C14 H14B 108.9 . . ?
C15 C14 H14B 108.9 . . ?
H14A C14 H14B 107.7 . . ?
C14 C15 C16 112.8(5) . . ?
C14 C15 H15A 109.0 . . ?
C16 C15 H15A 109.0 . . ?
C14 C15 H15B 109.0 . . ?
C16 C15 H15B 109.0 . . ?
H15A C15 H15B 107.8 . . ?
C17 C16 C15 113.1(6) . . ?
C17 C16 H16A 109.0 . . ?
C15 C16 H16A 109.0 . . ?
C17 C16 H16B 109.0 . . ?
C15 C16 H16B 109.0 . . ?
H16A C16 H16B 107.8 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 H18A 109.5 . . ?
C19 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C19 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 C18 112.7(5) . . ?
C20 C19 H19A 109.1 . . ?
C18 C19 H19A 109.1 . . ?
C20 C19 H19B 109.1 . . ?
C18 C19 H19B 109.1 . . ?
H19A C19 H19B 107.8 . . ?
C19 C20 C21 113.3(4) . . ?
C19 C20 H20A 108.9 . . ?
C21 C20 H20A 108.9 . . ?
C19 C20 H20B 108.9 . . ?
C21 C20 H20B 108.9 . . ?
H20A C20 H20B 107.7 . . ?
C22 C21 C20 114.0(4) . . ?
C22 C21 H21A 108.8 . . ?
C20 C21 H21A 108.8 . . ?
C22 C21 H21B 108.8 . . ?
C20 C21 H21B 108.8 . . ?
H21A C21 H21B 107.7 . . ?
N3 C22 C21 112.5(3) . . ?
N3 C22 H22A 109.1 . . ?
C21 C22 H22A 109.1 . . ?
N3 C22 H22B 109.1 . . ?
C21 C22 H22B 109.1 . . ?
H22A C22 H22B 107.8 . . ?
N4 C23 N3 110.7(4) . . ?
N4 C23 H23 124.7 . . ?
N3 C23 H23 124.7 . . ?
N3 C24 C25 132.3(4) . . ?
N3 C24 C29 106.8(3) . . ?
C25 C24 C29 120.9(4) . . ?
C26 C25 C24 116.2(4) . . ?
C26 C25 H25 121.9 . . ?
C24 C25 H25 121.9 . . ?
C25 C26 C27 123.2(4) . . ?
C25 C26 H26 118.4 . . ?
C27 C26 H26 118.4 . . ?
C28 C27 C26 120.8(4) . . ?
C28 C27 H27 119.6 . . ?
C26 C27 H27 119.6 . . ?
C29 C28 C27 116.4(4) . . ?
C29 C28 H28 121.8 . . ?
C27 C28 H28 121.8 . . ?
C28 C29 N4 131.7(4) . . ?
C28 C29 C24 122.6(4) . . ?
N4 C29 C24 105.6(3) . . ?
N4 C30 C31 112.1(4) . . ?
N4 C30 H30A 109.2 . . ?
C31 C30 H30A 109.2 . . ?
N4 C30 H30B 109.2 . . ?
C31 C30 H30B 109.2 . . ?
H30A C30 H30B 107.9 . . ?
C32 C31 C30 116.2(5) . . ?
C32 C31 H31A 108.2 . . ?
C30 C31 H31A 108.2 . . ?
C32 C31 H31B 108.2 . . ?
C30 C31 H31B 108.2 . . ?
H31A C31 H31B 107.4 . . ?
C31 C32 C33 110.8(9) . . ?
C31 C32 H32A 109.5 . . ?
C33 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C33 C32 H32B 109.5 . . ?
H32A C32 H32B 108.1 . . ?
C34 C33 C32 124.6(11) . . ?
C34 C33 H33A 106.2 . . ?
C32 C33 H33A 106.2 . . ?
C34 C33 H33B 106.2 . . ?
C32 C33 H33B 106.2 . . ?
H33A C33 H33B 106.4 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C6 N1 C7 107.5(3) . . ?
C6 N1 C5 126.5(3) . . ?
C7 N1 C5 126.0(3) . . ?
C6 N2 C12 107.7(3) . . ?
C6 N2 C13 125.7(3) . . ?
C12 N2 C13 126.5(3) . . ?
C23 N3 C24 108.3(3) . . ?
C23 N3 C22 125.6(3) . . ?
C24 N3 C22 126.1(3) . . ?
C23 N4 C29 108.6(3) . . ?
C23 N4 C30 126.8(3) . . ?
C29 N4 C30 124.6(3) . . ?
H1O O1 H2O 104(6) . . ?
H3O O2 H4O 112(6) . . ?
 
_diffrn_measured_fraction_theta_max    0.979
_diffrn_reflns_theta_full              27.47
_diffrn_measured_fraction_theta_full   0.979
_refine_diff_density_max    0.648
_refine_diff_density_min   -0.604
_refine_diff_density_rms    0.064
