 
data_AIN_3_52
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C18 H36 N3 O2, C24 H20 B, C3.5 H3.5'
_chemical_formula_sum
 'C45.50 H59.50 B N3 O2'
_chemical_formula_weight          691.27
 
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'
 'B'  'B'   0.0090   0.0039
 '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'
 'O'  'O'   0.0492   0.0322
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/n'
_space_group_name_Hall            '-P 2yn'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_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                    10.11500(10)
_cell_length_b                    34.9730(4)
_cell_length_c                    11.60680(10)
_cell_angle_alpha                 90
_cell_angle_beta                  102.9550(10)
_cell_angle_gamma                 90
_cell_volume                      4001.42(7)
_cell_formula_units_Z             4
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used     35095
_cell_measurement_theta_min       3.9510
_cell_measurement_theta_max       78.9280
 
_exptl_crystal_description        block
_exptl_crystal_colour             colourless
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.147
_exptl_crystal_F_000              1498
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.450
_exptl_crystal_size_mid           0.180
_exptl_crystal_size_min           0.130
_exptl_absorpt_coefficient_mu     0.530
_shelx_estimated_absorpt_T_min    0.797
_shelx_estimated_absorpt_T_max    0.934
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.94495
_exptl_absorpt_correction_T_max   1.00000
_exptl_absorpt_process_details
;
Olex2 1.2-ac3
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       100(2)
_diffrn_radiation_wavelength      1.54184
_diffrn_radiation_type            CuK\a
_diffrn_source                    'Rotating-anode X-ray tube'
_diffrn_measurement_device_type   'ROD, Synergy Custom DW system, Pilatus 200K'
_diffrn_measurement_method        'ω scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             52514
_diffrn_reflns_av_unetI/netI      0.0240
_diffrn_reflns_av_R_equivalents   0.0370
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        12
_diffrn_reflns_limit_k_min        -43
_diffrn_reflns_limit_k_max        43
_diffrn_reflns_limit_l_min        -14
_diffrn_reflns_limit_l_max        10
_diffrn_reflns_theta_min          4.108
_diffrn_reflns_theta_max          74.488
_diffrn_reflns_theta_full         74.000
_diffrn_measured_fraction_theta_max   0.998
_diffrn_measured_fraction_theta_full  0.998
_diffrn_reflns_Laue_measured_fraction_max    0.998
_diffrn_reflns_Laue_measured_fraction_full   0.998
_diffrn_reflns_point_group_measured_fraction_max   0.998
_diffrn_reflns_point_group_measured_fraction_full  0.998
_reflns_number_total              8168
_reflns_number_gt                 7753
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_cell_refinement        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction         'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_structure_solution     'ShelXT (Sheldrick, 2015)'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material   'Olex2 (Dolomanov et al., 2009)'
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0347P)²+2.4766P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      dual
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    mixed
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          8168
_refine_ls_number_parameters      480
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0512
_refine_ls_R_factor_gt            0.0492
_refine_ls_wR_factor_ref          0.1174
_refine_ls_wR_factor_gt           0.1162
_refine_ls_goodness_of_fit_ref    1.085
_refine_ls_restrained_S_all       1.085
_refine_ls_shift/su_max           0.001
_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_site_symmetry_order
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
C1 C 0.4754(2) 0.73239(5) 0.49220(16) 0.0470(5) Uani 1 1 d . . . . .
H1A H 0.4950 0.7241 0.5759 0.056 Uiso 1 1 calc R U . . .
H1B H 0.4217 0.7563 0.4851 0.056 Uiso 1 1 calc R U . . .
C2 C 0.6073(2) 0.73925(5) 0.45292(19) 0.0528(5) Uani 1 1 d . . . . .
H2A H 0.6620 0.7155 0.4642 0.063 Uiso 1 1 calc R U . . .
H2B H 0.6600 0.7594 0.5030 0.063 Uiso 1 1 calc R U . . .
C3 C 0.58163(17) 0.75143(5) 0.32316(19) 0.0443(4) Uani 1 1 d . . . . .
H3A H 0.5369 0.7771 0.3159 0.053 Uiso 1 1 calc R U . . .
C4 C 0.7126(2) 0.75506(6) 0.2796(3) 0.0699(7) Uani 1 1 d . . . . .
H4A H 0.7558 0.7299 0.2816 0.105 Uiso 1 1 calc R U . . .
H4B H 0.7742 0.7728 0.3309 0.105 Uiso 1 1 calc R U . . .
H4C H 0.6919 0.7648 0.1984 0.105 Uiso 1 1 calc R U . . .
C5 C 0.48450(17) 0.72333(5) 0.24481(16) 0.0362(4) Uani 1 1 d . . . . .
H5A H 0.4558 0.7342 0.1643 0.043 Uiso 1 1 calc R U . . .
H5B H 0.5332 0.6991 0.2388 0.043 Uiso 1 1 calc R U . . .
C6 C 0.35932(15) 0.71486(4) 0.29260(13) 0.0307(3) Uani 1 1 d . . . . .
H6A H 0.3022 0.7381 0.2867 0.037 Uiso 1 1 calc R U . . .
H6B H 0.3052 0.6945 0.2446 0.037 Uiso 1 1 calc R U . . .
C7 C 0.39969(14) 0.66673(4) 0.45594(12) 0.0258(3) Uani 1 1 d . . . . .
C8 C 0.33840(13) 0.63526(4) 0.36930(12) 0.0234(3) Uani 1 1 d . . . . .
H8A H 0.2388 0.6349 0.3609 0.028 Uiso 1 1 calc R U . . .
H8B H 0.3567 0.6410 0.2908 0.028 Uiso 1 1 calc R U . . .
C9 C 0.52196(14) 0.58733(4) 0.40099(12) 0.0262(3) Uani 1 1 d . . . . .
C10 C 0.61237(15) 0.61809(5) 0.37122(14) 0.0321(3) Uani 1 1 d . . . . .
H10A H 0.6313 0.6370 0.4352 0.048 Uiso 1 1 calc R U . . .
H10B H 0.5671 0.6307 0.2975 0.048 Uiso 1 1 calc R U . . .
H10C H 0.6978 0.6067 0.3615 0.048 Uiso 1 1 calc R U . . .
C11 C 0.30320(14) 0.56862(4) 0.43762(12) 0.0245(3) Uani 1 1 d . . . . .
H11A H 0.3513 0.5438 0.4476 0.029 Uiso 1 1 calc R U . . .
H11B H 0.2235 0.5660 0.3707 0.029 Uiso 1 1 calc R U . . .
C12 C 0.25383(14) 0.57731(4) 0.54948(12) 0.0257(3) Uani 1 1 d . . . . .
H12A H 0.1829 0.5973 0.5314 0.031 Uiso 1 1 calc R U . . .
H12B H 0.2114 0.5540 0.5735 0.031 Uiso 1 1 calc R U . . .
C13 C 0.48382(14) 0.56340(4) 0.68562(13) 0.0282(3) Uani 1 1 d . . . . .
H13 H 0.5093 0.5554 0.6108 0.034 Uiso 1 1 calc R U . . .
C14 C 0.60392(17) 0.58508(5) 0.75879(17) 0.0430(4) Uani 1 1 d . . . . .
H14A H 0.6164 0.6090 0.7188 0.065 Uiso 1 1 calc R U . . .
H14B H 0.6860 0.5694 0.7679 0.065 Uiso 1 1 calc R U . . .
H14C H 0.5869 0.5907 0.8369 0.065 Uiso 1 1 calc R U . . .
C15 C 0.45148(17) 0.52743(5) 0.74592(15) 0.0353(4) Uani 1 1 d . . . . .
H15A H 0.4341 0.5339 0.8233 0.053 Uiso 1 1 calc R U . . .
H15B H 0.5285 0.5098 0.7564 0.053 Uiso 1 1 calc R U . . .
H15C H 0.3708 0.5152 0.6972 0.053 Uiso 1 1 calc R U . . .
C16 C 0.30400(16) 0.60429(4) 0.75504(13) 0.0300(3) Uani 1 1 d . . . . .
H16 H 0.3783 0.6033 0.8281 0.036 Uiso 1 1 calc R U . . .
C17 C 0.26166(19) 0.64579(5) 0.73422(14) 0.0368(4) Uani 1 1 d . . . . .
H17A H 0.3419 0.6616 0.7351 0.055 Uiso 1 1 calc R U . . .
H17B H 0.2176 0.6544 0.7968 0.055 Uiso 1 1 calc R U . . .
H17C H 0.1981 0.6483 0.6573 0.055 Uiso 1 1 calc R U . . .
C18 C 0.18769(17) 0.57978(5) 0.77700(14) 0.0357(4) Uani 1 1 d . . . . .
H18A H 0.1076 0.5836 0.7127 0.054 Uiso 1 1 calc R U . . .
H18B H 0.1664 0.5872 0.8523 0.054 Uiso 1 1 calc R U . . .
H18C H 0.2142 0.5528 0.7801 0.054 Uiso 1 1 calc R U . . .
C19 C -0.13582(14) 0.65250(4) -0.00762(13) 0.0270(3) Uani 1 1 d . . . . .
C20 C -0.12473(17) 0.65359(5) -0.12528(14) 0.0345(4) Uani 1 1 d . . . . .
H20 H -0.0519 0.6404 -0.1470 0.041 Uiso 1 1 calc R U . . .
C21 C -0.2172(2) 0.67347(5) -0.21211(16) 0.0471(5) Uani 1 1 d . . . . .
H21 H -0.2061 0.6738 -0.2913 0.057 Uiso 1 1 calc R U . . .
C22 C -0.32511(19) 0.69272(5) -0.18299(19) 0.0514(5) Uani 1 1 d . . . . .
H22 H -0.3889 0.7059 -0.2421 0.062 Uiso 1 1 calc R U . . .
C23 C -0.33901(17) 0.69253(5) -0.06813(19) 0.0471(5) Uani 1 1 d . . . . .
H23 H -0.4122 0.7058 -0.0474 0.057 Uiso 1 1 calc R U . . .
C24 C -0.24601(15) 0.67292(4) 0.01800(16) 0.0351(4) Uani 1 1 d . . . . .
H24 H -0.2571 0.6733 0.0971 0.042 Uiso 1 1 calc R U . . .
C25 C -0.02853(13) 0.64288(4) 0.22491(12) 0.0227(3) Uani 1 1 d . . . . .
C26 C 0.00693(14) 0.68159(4) 0.24534(14) 0.0292(3) Uani 1 1 d . . . . .
H26 H 0.0185 0.6968 0.1805 0.035 Uiso 1 1 calc R U . . .
C27 C 0.02576(16) 0.69856(5) 0.35623(15) 0.0356(4) Uani 1 1 d . . . . .
H27 H 0.0516 0.7247 0.3661 0.043 Uiso 1 1 calc R U . . .
C28 C 0.00688(16) 0.67748(5) 0.45210(15) 0.0369(4) Uani 1 1 d . . . . .
H28 H 0.0169 0.6891 0.5275 0.044 Uiso 1 1 calc R U . . .
C29 C -0.02678(14) 0.63919(5) 0.43632(14) 0.0321(3) Uani 1 1 d . . . . .
H29 H -0.0398 0.6244 0.5014 0.038 Uiso 1 1 calc R U . . .
C30 C -0.04169(13) 0.62222(4) 0.32523(13) 0.0255(3) Uani 1 1 d . . . . .
H30 H -0.0615 0.5957 0.3173 0.031 Uiso 1 1 calc R U . . .
C31 C -0.12433(13) 0.58362(4) 0.07279(12) 0.0214(3) Uani 1 1 d . . . . .
C32 C -0.24043(13) 0.57770(4) 0.11799(13) 0.0242(3) Uani 1 1 d . . . . .
H32 H -0.2673 0.5972 0.1648 0.029 Uiso 1 1 calc R U . . .
C33 C -0.31762(14) 0.54449(4) 0.09715(13) 0.0273(3) Uani 1 1 d . . . . .
H33 H -0.3949 0.5416 0.1302 0.033 Uiso 1 1 calc R U . . .
C34 C -0.28234(14) 0.51551(4) 0.02830(13) 0.0279(3) Uani 1 1 d . . . . .
H34 H -0.3339 0.4926 0.0147 0.033 Uiso 1 1 calc R U . . .
C35 C -0.17040(14) 0.52063(4) -0.02018(13) 0.0276(3) Uani 1 1 d . . . . .
H35 H -0.1455 0.5012 -0.0685 0.033 Uiso 1 1 calc R U . . .
C36 C -0.09402(14) 0.55406(4) 0.00128(12) 0.0242(3) Uani 1 1 d . . . . .
H36 H -0.0184 0.5569 -0.0339 0.029 Uiso 1 1 calc R U . . .
C37 C 0.11492(13) 0.62044(4) 0.07834(12) 0.0223(3) Uani 1 1 d . . . . .
C38 C 0.19323(14) 0.58779(4) 0.11761(12) 0.0245(3) Uani 1 1 d . . . . .
H38 H 0.1513 0.5669 0.1478 0.029 Uiso 1 1 calc R U . . .
C39 C 0.32973(14) 0.58474(5) 0.11413(13) 0.0291(3) Uani 1 1 d . . . . .
H39 H 0.3782 0.5619 0.1401 0.035 Uiso 1 1 calc R U . . .
C40 C 0.39480(15) 0.61499(5) 0.07279(13) 0.0332(4) Uani 1 1 d . . . . .
H40 H 0.4877 0.6131 0.0698 0.040 Uiso 1 1 calc R U . . .
C41 C 0.32218(15) 0.64806(5) 0.03588(13) 0.0315(3) Uani 1 1 d . . . . .
H41 H 0.3660 0.6692 0.0091 0.038 Uiso 1 1 calc R U . . .
C42 C 0.18495(14) 0.65044(4) 0.03781(12) 0.0264(3) Uani 1 1 d . . . . .
H42 H 0.1370 0.6732 0.0106 0.032 Uiso 1 1 calc R U . . .
C43 C 0.8909(2) 0.52282(6) 0.4586(3) 0.0652(7) Uani 1 1 d . . . . .
H43 H 0.8144 0.5387 0.4305 0.078 Uiso 1 1 calc R U . . .
C44 C 0.9256(2) 0.51329(6) 0.5789(3) 0.0673(7) Uani 1 1 d . . . . .
C45 C 1.0366(2) 0.48999(6) 0.6187(2) 0.0650(7) Uani 1 1 d . . . . .
H45 H 1.0621 0.4830 0.6998 0.078 Uiso 1 1 calc R U . . .
C46 C 0.8524(5) 0.52720(14) 0.6494(4) 0.0611(12) Uani 0.5 1 d . . P . .
H46A H 0.8744 0.5136 0.7252 0.092 Uiso 0.5 1 calc R U P . .
H46B H 0.7559 0.5239 0.6130 0.092 Uiso 0.5 1 calc R U P . .
H46C H 0.8724 0.5545 0.6627 0.092 Uiso 0.5 1 calc R U P . .
B1 B -0.04227(15) 0.62447(4) 0.09213(14) 0.0218(3) Uani 1 1 d . . . . .
N1 N 0.39881(14) 0.70258(4) 0.41627(11) 0.0333(3) Uani 1 1 d . . . . .
N2 N 0.39360(11) 0.59771(3) 0.40814(10) 0.0223(2) Uani 1 1 d . . . . .
N3 N 0.36341(12) 0.59052(4) 0.65158(10) 0.0242(2) Uani 1 1 d . . . . .
O1 O 0.44885(11) 0.65827(3) 0.56096(9) 0.0316(2) Uani 1 1 d . . . . .
O2 O 0.56343(11) 0.55444(3) 0.42157(10) 0.0351(3) Uani 1 1 d . . . . .
H3 H 0.3971(19) 0.6126(6) 0.6226(16) 0.038(5) Uiso 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 N1 1.469(2) . ?
C1 C2 1.523(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.530(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.525(3) . ?
C3 C5 1.535(2) . ?
C3 H3A 1.0000 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.521(2) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 N1 1.4653(19) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 O1 1.2445(17) . ?
C7 N1 1.335(2) . ?
C7 C8 1.5255(19) . ?
C8 N2 1.4584(18) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 O2 1.2291(18) . ?
C9 N2 1.3685(18) . ?
C9 C10 1.502(2) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 N2 1.4590(18) . ?
C11 C12 1.5225(19) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 N3 1.5024(17) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C15 1.511(2) . ?
C13 C14 1.520(2) . ?
C13 N3 1.5244(18) . ?
C13 H13 1.0000 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.517(2) . ?
C16 C18 1.523(2) . ?
C16 N3 1.5357(19) . ?
C16 H16 1.0000 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.396(2) . ?
C19 C24 1.410(2) . ?
C19 B1 1.645(2) . ?
C20 C21 1.397(2) . ?
C20 H20 0.9500 . ?
C21 C22 1.388(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.372(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.390(2) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C30 1.402(2) . ?
C25 C26 1.407(2) . ?
C25 B1 1.647(2) . ?
C26 C27 1.391(2) . ?
C26 H26 0.9500 . ?
C27 C28 1.383(3) . ?
C27 H27 0.9500 . ?
C28 C29 1.384(2) . ?
C28 H28 0.9500 . ?
C29 C30 1.396(2) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C36 1.402(2) . ?
C31 C32 1.4049(19) . ?
C31 B1 1.642(2) . ?
C32 C33 1.390(2) . ?
C32 H32 0.9500 . ?
C33 C34 1.386(2) . ?
C33 H33 0.9500 . ?
C34 C35 1.384(2) . ?
C34 H34 0.9500 . ?
C35 C36 1.392(2) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 C42 1.405(2) . ?
C37 C38 1.406(2) . ?
C37 B1 1.639(2) . ?
C38 C39 1.3944(19) . ?
C38 H38 0.9500 . ?
C39 C40 1.387(2) . ?
C39 H39 0.9500 . ?
C40 C41 1.386(2) . ?
C40 H40 0.9500 . ?
C41 C42 1.396(2) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C43 C45 1.356(4) 3_766 ?
C43 C44 1.401(4) . ?
C43 H43 0.9500 . ?
C44 C46 1.314(5) . ?
C44 C45 1.381(3) . ?
C45 C43 1.356(4) 3_766 ?
C45 H45 0.9500 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
N3 H3 0.94(2) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
N1 C1 C2 108.17(16) . . ?
N1 C1 H1A 110.1 . . ?
C2 C1 H1A 110.1 . . ?
N1 C1 H1B 110.1 . . ?
C2 C1 H1B 110.1 . . ?
H1A C1 H1B 108.4 . . ?
C1 C2 C3 111.83(14) . . ?
C1 C2 H2A 109.2 . . ?
C3 C2 H2A 109.2 . . ?
C1 C2 H2B 109.3 . . ?
C3 C2 H2B 109.3 . . ?
H2A C2 H2B 107.9 . . ?
C4 C3 C2 112.39(17) . . ?
C4 C3 C5 110.18(18) . . ?
C2 C3 C5 110.48(14) . . ?
C4 C3 H3A 107.9 . . ?
C2 C3 H3A 107.9 . . ?
C5 C3 H3A 107.9 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 C3 112.52(15) . . ?
C6 C5 H5A 109.1 . . ?
C3 C5 H5A 109.1 . . ?
C6 C5 H5B 109.1 . . ?
C3 C5 H5B 109.1 . . ?
H5A C5 H5B 107.8 . . ?
N1 C6 C5 110.36(13) . . ?
N1 C6 H6A 109.6 . . ?
C5 C6 H6A 109.6 . . ?
N1 C6 H6B 109.6 . . ?
C5 C6 H6B 109.6 . . ?
H6A C6 H6B 108.1 . . ?
O1 C7 N1 122.10(13) . . ?
O1 C7 C8 119.22(13) . . ?
N1 C7 C8 118.68(12) . . ?
N2 C8 C7 112.02(11) . . ?
N2 C8 H8A 109.2 . . ?
C7 C8 H8A 109.2 . . ?
N2 C8 H8B 109.2 . . ?
C7 C8 H8B 109.2 . . ?
H8A C8 H8B 107.9 . . ?
O2 C9 N2 121.57(14) . . ?
O2 C9 C10 121.08(13) . . ?
N2 C9 C10 117.31(13) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C11 C12 113.79(11) . . ?
N2 C11 H11A 108.8 . . ?
C12 C11 H11A 108.8 . . ?
N2 C11 H11B 108.8 . . ?
C12 C11 H11B 108.8 . . ?
H11A C11 H11B 107.7 . . ?
N3 C12 C11 114.14(11) . . ?
N3 C12 H12A 108.7 . . ?
C11 C12 H12A 108.7 . . ?
N3 C12 H12B 108.7 . . ?
C11 C12 H12B 108.7 . . ?
H12A C12 H12B 107.6 . . ?
C15 C13 C14 112.68(13) . . ?
C15 C13 N3 113.26(12) . . ?
C14 C13 N3 109.05(12) . . ?
C15 C13 H13 107.2 . . ?
C14 C13 H13 107.2 . . ?
N3 C13 H13 107.2 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 C18 111.35(14) . . ?
C17 C16 N3 108.74(12) . . ?
C18 C16 N3 114.01(12) . . ?
C17 C16 H16 107.5 . . ?
C18 C16 H16 107.5 . . ?
N3 C16 H16 107.5 . . ?
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 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 C24 115.67(14) . . ?
C20 C19 B1 123.05(14) . . ?
C24 C19 B1 120.69(14) . . ?
C19 C20 C21 122.14(18) . . ?
C19 C20 H20 118.9 . . ?
C21 C20 H20 118.9 . . ?
C22 C21 C20 120.12(18) . . ?
C22 C21 H21 119.9 . . ?
C20 C21 H21 119.9 . . ?
C23 C22 C21 119.48(16) . . ?
C23 C22 H22 120.3 . . ?
C21 C22 H22 120.3 . . ?
C22 C23 C24 120.07(19) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C23 C24 C19 122.51(18) . . ?
C23 C24 H24 118.7 . . ?
C19 C24 H24 118.7 . . ?
C30 C25 C26 115.08(13) . . ?
C30 C25 B1 124.89(12) . . ?
C26 C25 B1 119.91(13) . . ?
C27 C26 C25 122.91(15) . . ?
C27 C26 H26 118.5 . . ?
C25 C26 H26 118.5 . . ?
C28 C27 C26 120.12(15) . . ?
C28 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
C27 C28 C29 118.92(15) . . ?
C27 C28 H28 120.5 . . ?
C29 C28 H28 120.5 . . ?
C28 C29 C30 120.39(15) . . ?
C28 C29 H29 119.8 . . ?
C30 C29 H29 119.8 . . ?
C29 C30 C25 122.50(14) . . ?
C29 C30 H30 118.7 . . ?
C25 C30 H30 118.7 . . ?
C36 C31 C32 115.12(12) . . ?
C36 C31 B1 123.47(12) . . ?
C32 C31 B1 121.09(12) . . ?
C33 C32 C31 122.83(13) . . ?
C33 C32 H32 118.6 . . ?
C31 C32 H32 118.6 . . ?
C34 C33 C32 120.26(13) . . ?
C34 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?
C35 C34 C33 118.66(13) . . ?
C35 C34 H34 120.7 . . ?
C33 C34 H34 120.7 . . ?
C34 C35 C36 120.49(14) . . ?
C34 C35 H35 119.8 . . ?
C36 C35 H35 119.8 . . ?
C35 C36 C31 122.60(13) . . ?
C35 C36 H36 118.7 . . ?
C31 C36 H36 118.7 . . ?
C42 C37 C38 115.18(13) . . ?
C42 C37 B1 122.77(13) . . ?
C38 C37 B1 121.77(12) . . ?
C39 C38 C37 122.84(14) . . ?
C39 C38 H38 118.6 . . ?
C37 C38 H38 118.6 . . ?
C40 C39 C38 120.09(15) . . ?
C40 C39 H39 120.0 . . ?
C38 C39 H39 120.0 . . ?
C41 C40 C39 118.93(13) . . ?
C41 C40 H40 120.5 . . ?
C39 C40 H40 120.5 . . ?
C40 C41 C42 120.32(15) . . ?
C40 C41 H41 119.8 . . ?
C42 C41 H41 119.8 . . ?
C41 C42 C37 122.61(14) . . ?
C41 C42 H42 118.7 . . ?
C37 C42 H42 118.7 . . ?
C45 C43 C44 122.0(2) 3_766 . ?
C45 C43 H43 119.0 3_766 . ?
C44 C43 H43 119.0 . . ?
C46 C44 C45 122.6(4) . . ?
C46 C44 C43 118.9(3) . . ?
C45 C44 C43 118.5(2) . . ?
C43 C45 C44 119.5(2) 3_766 . ?
C43 C45 H45 120.2 3_766 . ?
C44 C45 H45 120.2 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C37 B1 C31 112.53(11) . . ?
C37 B1 C19 113.58(12) . . ?
C31 B1 C19 103.23(10) . . ?
C37 B1 C25 104.17(10) . . ?
C31 B1 C25 113.70(11) . . ?
C19 B1 C25 109.89(11) . . ?
C7 N1 C6 126.32(13) . . ?
C7 N1 C1 119.85(13) . . ?
C6 N1 C1 111.79(13) . . ?
C9 N2 C8 121.53(12) . . ?
C9 N2 C11 118.83(12) . . ?
C8 N2 C11 118.94(11) . . ?
C12 N3 C13 114.73(11) . . ?
C12 N3 C16 111.37(11) . . ?
C13 N3 C16 114.98(11) . . ?
C12 N3 H3 103.5(12) . . ?
C13 N3 H3 105.8(12) . . ?
C16 N3 H3 105.1(12) . . ?
 
loop_
 _geom_torsion_atom_site_label_1
 _geom_torsion_atom_site_label_2
 _geom_torsion_atom_site_label_3
 _geom_torsion_atom_site_label_4
 _geom_torsion
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
N1 C1 C2 C3 58.61(18) . . . . ?
C1 C2 C3 C4 -175.05(15) . . . . ?
C1 C2 C3 C5 -51.5(2) . . . . ?
C4 C3 C5 C6 173.08(15) . . . . ?
C2 C3 C5 C6 48.29(19) . . . . ?
C3 C5 C6 N1 -52.78(17) . . . . ?
O1 C7 C8 N2 -23.63(18) . . . . ?
N1 C7 C8 N2 156.33(13) . . . . ?
N2 C11 C12 N3 -45.54(17) . . . . ?
C24 C19 C20 C21 -0.3(2) . . . . ?
B1 C19 C20 C21 170.91(14) . . . . ?
C19 C20 C21 C22 -0.6(2) . . . . ?
C20 C21 C22 C23 1.0(3) . . . . ?
C21 C22 C23 C24 -0.5(3) . . . . ?
C22 C23 C24 C19 -0.4(3) . . . . ?
C20 C19 C24 C23 0.8(2) . . . . ?
B1 C19 C24 C23 -170.65(14) . . . . ?
C30 C25 C26 C27 -0.9(2) . . . . ?
B1 C25 C26 C27 -177.27(13) . . . . ?
C25 C26 C27 C28 -1.4(2) . . . . ?
C26 C27 C28 C29 1.9(2) . . . . ?
C27 C28 C29 C30 -0.2(2) . . . . ?
C28 C29 C30 C25 -2.3(2) . . . . ?
C26 C25 C30 C29 2.78(19) . . . . ?
B1 C25 C30 C29 178.89(12) . . . . ?
C36 C31 C32 C33 2.1(2) . . . . ?
B1 C31 C32 C33 175.78(13) . . . . ?
C31 C32 C33 C34 -0.6(2) . . . . ?
C32 C33 C34 C35 -0.9(2) . . . . ?
C33 C34 C35 C36 0.8(2) . . . . ?
C34 C35 C36 C31 0.8(2) . . . . ?
C32 C31 C36 C35 -2.2(2) . . . . ?
B1 C31 C36 C35 -175.68(13) . . . . ?
C42 C37 C38 C39 -1.6(2) . . . . ?
B1 C37 C38 C39 -175.58(13) . . . . ?
C37 C38 C39 C40 1.3(2) . . . . ?
C38 C39 C40 C41 0.3(2) . . . . ?
C39 C40 C41 C42 -1.5(2) . . . . ?
C40 C41 C42 C37 1.2(2) . . . . ?
C38 C37 C42 C41 0.3(2) . . . . ?
B1 C37 C42 C41 174.28(13) . . . . ?
C45 C43 C44 C46 178.9(3) 3_766 . . . ?
C45 C43 C44 C45 -0.3(3) 3_766 . . . ?
C46 C44 C45 C43 -178.8(3) . . . 3_766 ?
C43 C44 C45 C43 0.3(3) . . . 3_766 ?
C42 C37 B1 C31 150.20(13) . . . . ?
C38 C37 B1 C31 -36.25(17) . . . . ?
C42 C37 B1 C19 33.36(18) . . . . ?
C38 C37 B1 C19 -153.09(13) . . . . ?
C42 C37 B1 C25 -86.19(15) . . . . ?
C38 C37 B1 C25 87.36(15) . . . . ?
C36 C31 B1 C37 -28.33(18) . . . . ?
C32 C31 B1 C37 158.53(12) . . . . ?
C36 C31 B1 C19 94.52(15) . . . . ?
C32 C31 B1 C19 -78.61(15) . . . . ?
C36 C31 B1 C25 -146.47(12) . . . . ?
C32 C31 B1 C25 40.40(17) . . . . ?
C20 C19 B1 C37 38.19(18) . . . . ?
C24 C19 B1 C37 -151.04(13) . . . . ?
C20 C19 B1 C31 -83.97(15) . . . . ?
C24 C19 B1 C31 86.81(15) . . . . ?
C20 C19 B1 C25 154.42(13) . . . . ?
C24 C19 B1 C25 -34.81(17) . . . . ?
C30 C25 B1 C37 -102.45(14) . . . . ?
C26 C25 B1 C37 73.48(15) . . . . ?
C30 C25 B1 C31 20.40(18) . . . . ?
C26 C25 B1 C31 -163.66(12) . . . . ?
C30 C25 B1 C19 135.53(13) . . . . ?
C26 C25 B1 C19 -48.53(16) . . . . ?
O1 C7 N1 C6 171.86(14) . . . . ?
C8 C7 N1 C6 -8.1(2) . . . . ?
O1 C7 N1 C1 9.5(2) . . . . ?
C8 C7 N1 C1 -170.45(15) . . . . ?
C5 C6 N1 C7 -102.30(18) . . . . ?
C5 C6 N1 C1 61.25(18) . . . . ?
C2 C1 N1 C7 101.02(17) . . . . ?
C2 C1 N1 C6 -63.73(18) . . . . ?
O2 C9 N2 C8 -172.04(13) . . . . ?
C10 C9 N2 C8 10.14(19) . . . . ?
O2 C9 N2 C11 -1.8(2) . . . . ?
C10 C9 N2 C11 -179.61(12) . . . . ?
C7 C8 N2 C9 -74.17(16) . . . . ?
C7 C8 N2 C11 115.59(13) . . . . ?
C12 C11 N2 C9 120.53(14) . . . . ?
C12 C11 N2 C8 -68.97(16) . . . . ?
C11 C12 N3 C13 -55.46(16) . . . . ?
C11 C12 N3 C16 171.74(12) . . . . ?
C15 C13 N3 C12 -72.28(16) . . . . ?
C14 C13 N3 C12 161.38(13) . . . . ?
C15 C13 N3 C16 58.80(16) . . . . ?
C14 C13 N3 C16 -67.54(16) . . . . ?
C17 C16 N3 C12 -84.77(15) . . . . ?
C18 C16 N3 C12 40.13(17) . . . . ?
C17 C16 N3 C13 142.56(13) . . . . ?
C18 C16 N3 C13 -92.55(15) . . . . ?
 
_refine_diff_density_max    0.463
_refine_diff_density_min   -0.270
_refine_diff_density_rms    0.039
 
 
 
