| 1 |
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| 2 | data_1a
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| 3 |
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| 4 | _audit_creation_method SHELXL-97
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| 5 | _chemical_name_systematic
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| 6 | ;
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| 7 | ?
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| 8 | ;
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| 9 | _chemical_name_common S2-dipyridyl
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| 10 | _chemical_melting_point ?
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| 11 | _chemical_formula_moiety 'C10 H8 N2 S2'
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| 12 | _chemical_formula_sum 'C10 H8 N2 S2'
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| 13 | _chemical_formula_weight 220.30
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| 14 |
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| 15 | loop_
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| 16 | _atom_type_symbol
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| 17 | _atom_type_description
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| 18 | _atom_type_scat_dispersion_real
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| 19 | _atom_type_scat_dispersion_imag
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| 20 | _atom_type_scat_source
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| 21 | 'C' 'C' 0.0033 0.0016
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| 22 | 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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| 23 | 'H' 'H' 0.0000 0.0000
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| 24 | 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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| 25 | 'N' 'N' 0.0061 0.0033
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| 26 | 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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| 27 | 'S' 'S' 0.1246 0.1234
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| 28 | 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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| 29 |
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| 30 | _symmetry_cell_setting 'Monoclinic'
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| 31 | _symmetry_space_group_name_H-M 'P21/c '
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| 32 |
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| 33 | loop_
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| 34 | _symmetry_equiv_pos_as_xyz
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| 35 | 'x, y, z'
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| 36 | '-x, y+1/2, -z+1/2'
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| 37 | '-x, -y, -z'
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| 38 | 'x, -y-1/2, z-1/2'
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| 39 |
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| 40 | _cell_length_a 15.8489(14)
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| 41 | _cell_length_b 5.5008(5)
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| 42 | _cell_length_c 23.118(2)
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| 43 | _cell_angle_alpha 90.00
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| 44 | _cell_angle_beta 96.9160(10)
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| 45 | _cell_angle_gamma 90.00
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| 46 | _cell_volume 2000.8(3)
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| 47 | _cell_formula_units_Z 8
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| 48 | _cell_measurement_temperature 173(2)
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| 49 | _cell_measurement_reflns_used 2857
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| 50 | _cell_measurement_theta_min 2.59
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| 51 | _cell_measurement_theta_max 27.32
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| 52 |
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| 53 | _exptl_crystal_description block
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| 54 | _exptl_crystal_colour colorless
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| 55 | _exptl_crystal_size_max 0.45
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| 56 | _exptl_crystal_size_mid 0.21
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| 57 | _exptl_crystal_size_min 0.09
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| 58 | _exptl_crystal_density_meas ?
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| 59 | _exptl_crystal_density_diffrn 1.463
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| 60 | _exptl_crystal_density_method 'not measured'
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| 61 | _exptl_crystal_F_000 912
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| 62 | _exptl_absorpt_coefficient_mu 0.489
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| 63 | _exptl_absorpt_correction_type multi-scan
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| 64 | _exptl_absorpt_correction_T_min 0.86
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| 65 | _exptl_absorpt_correction_T_max 0.93
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| 66 | _exptl_absorpt_process_details 'SADABS (sHELDRICK, 2008)'
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| 67 |
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| 68 | _exptl_special_details
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| 69 | ;
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| 70 | ?
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| 71 | ;
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| 72 |
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| 73 | _diffrn_ambient_temperature 173(2)
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| 74 | _diffrn_radiation_wavelength 0.71073
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| 75 | _diffrn_radiation_type MoK\a
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| 76 | _diffrn_radiation_source 'sealed tube'
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| 77 | _diffrn_radiation_monochromator 'graphite'
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| 78 | _diffrn_measurement_device_type 'Bruker APEX-II CCD'
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| 79 | _diffrn_measurement_method '\f and \w scans'
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| 80 | _diffrn_detector_area_resol_mean ?
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| 81 | _diffrn_reflns_number 22851
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| 82 | _diffrn_reflns_av_R_equivalents 0.0296
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| 83 | _diffrn_reflns_av_sigmaI/netI 0.0191
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| 84 | _diffrn_reflns_limit_h_min -20
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| 85 | _diffrn_reflns_limit_h_max 20
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| 86 | _diffrn_reflns_limit_k_min 0
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| 87 | _diffrn_reflns_limit_k_max 7
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| 88 | _diffrn_reflns_limit_l_min 0
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| 89 | _diffrn_reflns_limit_l_max 29
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| 90 | _diffrn_reflns_theta_min 2.07
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| 91 | _diffrn_reflns_theta_max 27.35
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| 92 | _reflns_number_total 4508
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| 93 | _reflns_number_gt 3950
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| 94 | _reflns_threshold_expression >2sigma(I)
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| 95 |
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| 96 | _computing_data_collection 'Bruker APEX2'
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| 97 | _computing_cell_refinement 'Bruker SAINT'
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| 98 | _computing_data_reduction 'Bruker SAINT'
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| 99 | _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
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| 100 | _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
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| 101 | _computing_molecular_graphics 'Bruker SHELXTL'
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| 102 | _computing_publication_material 'Bruker SHELXTL'
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| 103 |
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| 104 | _refine_special_details
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| 105 | ;
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| 106 | Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
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| 107 | goodness of fit S are based on F^2^, conventional R-factors R are based
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| 108 | on F, with F set to zero for negative F^2^. The threshold expression of
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| 109 | F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
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| 110 | not relevant to the choice of reflections for refinement. R-factors based
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| 111 | on F^2^ are statistically about twice as large as those based on F, and R-
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| 112 | factors based on ALL data will be even larger.
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| 113 | ;
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| 114 |
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| 115 | _refine_ls_structure_factor_coef Fsqd
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| 116 | _refine_ls_matrix_type full
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| 117 | _refine_ls_weighting_scheme calc
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| 118 | _refine_ls_weighting_details
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| 119 | 'calc w=1/[\s^2^(Fo^2^)+(0.0362P)^2^+0.7686P] where P=(Fo^2^+2Fc^2^)/3'
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| 120 | _atom_sites_solution_primary direct
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| 121 | _atom_sites_solution_secondary difmap
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| 122 | _atom_sites_solution_hydrogens geom
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| 123 | _refine_ls_hydrogen_treatment mixed
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| 124 | _refine_ls_extinction_method SHELXL
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| 125 | _refine_ls_extinction_coef 0.0151(6)
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| 126 | _refine_ls_extinction_expression
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| 127 | 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
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| 128 | _refine_ls_number_reflns 4508
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| 129 | _refine_ls_number_parameters 254
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| 130 | _refine_ls_number_restraints 0
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| 131 | _refine_ls_R_factor_all 0.0339
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| 132 | _refine_ls_R_factor_gt 0.0286
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| 133 | _refine_ls_wR_factor_ref 0.0786
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| 134 | _refine_ls_wR_factor_gt 0.0745
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| 135 | _refine_ls_goodness_of_fit_ref 1.041
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| 136 | _refine_ls_restrained_S_all 1.041
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| 137 | _refine_ls_shift/su_max 0.001
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| 138 | _refine_ls_shift/su_mean 0.000
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| 139 |
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| 140 | loop_
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| 141 | _atom_site_label
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| 142 | _atom_site_type_symbol
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| 143 | _atom_site_fract_x
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| 144 | _atom_site_fract_y
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| 145 | _atom_site_fract_z
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| 146 | _atom_site_U_iso_or_equiv
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| 147 | _atom_site_adp_type
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| 148 | _atom_site_occupancy
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| 149 | _atom_site_symmetry_multiplicity
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| 150 | _atom_site_calc_flag
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| 151 | _atom_site_refinement_flags
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| 152 | _atom_site_disorder_assembly
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| 153 | _atom_site_disorder_group
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| 154 | N1A N 0.41020(8) 0.7497(2) 0.05416(5) 0.0331(3) Uani 1 1 d . . .
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| 155 | C2A C 0.40875(10) 0.7474(3) -0.00387(7) 0.0387(4) Uani 1 1 d . . .
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| 156 | H2A H 0.4357 0.8770 -0.0217 0.046 Uiso 1 1 calc R . .
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| 157 | C3A C 0.37018(10) 0.5668(3) -0.03921(7) 0.0370(3) Uani 1 1 d . . .
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| 158 | H3A H 0.3695 0.5744 -0.0803 0.044 Uiso 1 1 calc R . .
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| 159 | C4A C 0.33281(10) 0.3755(3) -0.01356(7) 0.0366(3) Uani 1 1 d . . .
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| 160 | H4A H 0.3063 0.2478 -0.0368 0.044 Uiso 1 1 calc R . .
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| 161 | C5A C 0.33420(9) 0.3710(3) 0.04661(6) 0.0317(3) Uani 1 1 d . . .
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| 162 | H5A H 0.3094 0.2408 0.0656 0.038 Uiso 1 1 calc R . .
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| 163 | C6A C 0.37306(8) 0.5635(2) 0.07779(6) 0.0251(3) Uani 1 1 d . . .
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| 164 | S1A S 0.37820(2) 0.60478(7) 0.154800(15) 0.02788(10) Uani 1 1 d . . .
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| 165 | S2A S 0.33111(2) 0.29532(7) 0.185588(15) 0.02893(10) Uani 1 1 d . . .
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| 166 | C7A C 0.21859(8) 0.3355(2) 0.17827(5) 0.0227(3) Uani 1 1 d . . .
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| 167 | C8A C 0.17589(8) 0.5331(2) 0.15206(6) 0.0251(3) Uani 1 1 d . . .
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| 168 | H8A H 0.2057 0.6646 0.1372 0.030 Uiso 1 1 calc R . .
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| 169 | C9A C 0.08821(8) 0.5324(3) 0.14827(6) 0.0294(3) Uani 1 1 d . . .
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| 170 | H9A H 0.0562 0.6631 0.1299 0.035 Uiso 1 1 calc R . .
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| 171 | C10A C 0.04751(9) 0.3396(3) 0.17142(6) 0.0313(3) Uani 1 1 d . . .
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| 172 | H10A H -0.0127 0.3355 0.1693 0.038 Uiso 1 1 calc R . .
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| 173 | C11A C 0.09619(9) 0.1532(3) 0.19771(6) 0.0304(3) Uani 1 1 d . . .
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| 174 | H11A H 0.0681 0.0227 0.2143 0.037 Uiso 1 1 calc R . .
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| 175 | N2A N 0.18131(7) 0.1469(2) 0.20095(5) 0.0268(2) Uani 1 1 d . . .
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| 176 | N1B N 0.08652(7) 0.2235(2) 0.44962(5) 0.0316(3) Uani 1 1 d . . .
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| 177 | C2B C 0.08364(10) 0.2580(3) 0.50675(6) 0.0358(3) Uani 1 1 d . . .
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| 178 | H2B H 0.0556 0.1395 0.5275 0.043 Uiso 1 1 calc R . .
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| 179 | C3B C 0.11918(10) 0.4563(3) 0.53707(6) 0.0358(3) Uani 1 1 d . . .
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| 180 | H3B H 0.1166 0.4723 0.5777 0.043 Uiso 1 1 calc R . .
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| 181 | C4B C 0.15860(10) 0.6308(3) 0.50690(7) 0.0364(3) Uani 1 1 d . . .
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| 182 | H4B H 0.1832 0.7700 0.5266 0.044 Uiso 1 1 calc R . .
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| 183 | C5B C 0.16197(9) 0.6018(3) 0.44785(6) 0.0314(3) Uani 1 1 d . . .
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| 184 | H5B H 0.1882 0.7199 0.4259 0.038 Uiso 1 1 calc R . .
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| 185 | C6B C 0.12570(8) 0.3940(2) 0.42186(6) 0.0249(3) Uani 1 1 d . . .
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| 186 | S1B S 0.12772(2) 0.31377(7) 0.347233(15) 0.02940(10) Uani 1 1 d . . .
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| 187 | S2B S 0.16689(2) 0.61660(7) 0.309160(15) 0.02815(10) Uani 1 1 d . . .
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| 188 | C7B C 0.28043(8) 0.6043(2) 0.32021(5) 0.0229(3) Uani 1 1 d . . .
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| 189 | C8B C 0.32129(9) 0.7899(3) 0.29400(6) 0.0282(3) Uani 1 1 d . . .
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| 190 | H8B H 0.2900 0.9129 0.2720 0.034 Uiso 1 1 calc R . .
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| 191 | C9B C 0.40893(9) 0.7894(3) 0.30108(6) 0.0316(3) Uani 1 1 d . . .
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| 192 | H9B H 0.4396 0.9129 0.2839 0.038 Uiso 1 1 calc R . .
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| 193 | C10B C 0.45149(9) 0.6062(3) 0.33366(7) 0.0325(3) Uani 1 1 d . . .
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| 194 | H10B H 0.5118 0.6012 0.3391 0.039 Uiso 1 1 calc R . .
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| 195 | C11B C 0.40449(9) 0.4315(3) 0.35800(6) 0.0307(3) Uani 1 1 d . . .
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| 196 | H11B H 0.4341 0.3061 0.3802 0.037 Uiso 1 1 calc R . .
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| 197 | N2B N 0.31912(7) 0.4281(2) 0.35212(5) 0.0275(2) Uani 1 1 d . . .
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| 198 |
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| 199 | loop_
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| 200 | _atom_site_aniso_label
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| 201 | _atom_site_aniso_U_11
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| 202 | _atom_site_aniso_U_22
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| 203 | _atom_site_aniso_U_33
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| 204 | _atom_site_aniso_U_23
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| 205 | _atom_site_aniso_U_13
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| 206 | _atom_site_aniso_U_12
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| 207 | N1A 0.0355(7) 0.0297(6) 0.0331(6) 0.0025(5) 0.0005(5) -0.0068(5)
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| 208 | C2A 0.0441(9) 0.0354(8) 0.0363(8) 0.0067(7) 0.0036(7) -0.0043(7)
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| 209 | C3A 0.0407(8) 0.0406(9) 0.0293(7) 0.0002(6) 0.0033(6) 0.0069(7)
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| 210 | C4A 0.0372(8) 0.0346(8) 0.0374(8) -0.0102(6) 0.0022(6) -0.0009(6)
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| 211 | C5A 0.0308(7) 0.0283(7) 0.0368(8) -0.0044(6) 0.0064(6) -0.0044(6)
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| 212 | C6A 0.0207(6) 0.0248(7) 0.0295(7) -0.0007(5) 0.0017(5) 0.0020(5)
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| 213 | S1A 0.02503(17) 0.02972(19) 0.02881(18) -0.00220(13) 0.00288(13) -0.00401(13)
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| 214 | S2A 0.02179(17) 0.0297(2) 0.03566(19) 0.00761(14) 0.00493(13) 0.00532(13)
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| 215 | C7A 0.0216(6) 0.0249(6) 0.0218(6) -0.0017(5) 0.0030(5) 0.0017(5)
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| 216 | C8A 0.0253(6) 0.0239(6) 0.0264(6) 0.0027(5) 0.0038(5) 0.0013(5)
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| 217 | C9A 0.0257(7) 0.0301(7) 0.0319(7) 0.0011(6) 0.0015(5) 0.0050(6)
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| 218 | C10A 0.0218(6) 0.0357(8) 0.0367(8) -0.0044(6) 0.0045(6) -0.0018(6)
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| 219 | C11A 0.0313(7) 0.0282(7) 0.0329(7) -0.0012(6) 0.0081(6) -0.0062(6)
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| 220 | N2A 0.0285(6) 0.0244(6) 0.0280(6) 0.0014(5) 0.0050(5) -0.0001(5)
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| 221 | N1B 0.0315(6) 0.0301(6) 0.0324(6) 0.0026(5) 0.0008(5) -0.0053(5)
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| 222 | C2B 0.0373(8) 0.0371(8) 0.0327(7) 0.0076(6) 0.0029(6) -0.0029(7)
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| 223 | C3B 0.0407(8) 0.0394(8) 0.0269(7) 0.0000(6) 0.0032(6) 0.0053(7)
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| 224 | C4B 0.0450(9) 0.0298(8) 0.0335(8) -0.0066(6) 0.0010(6) -0.0021(7)
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| 225 | C5B 0.0334(7) 0.0281(7) 0.0330(7) -0.0027(6) 0.0047(6) -0.0052(6)
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| 226 | C6B 0.0199(6) 0.0262(7) 0.0281(6) -0.0010(5) 0.0012(5) 0.0018(5)
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| 227 | S1B 0.02656(18) 0.0318(2) 0.03031(18) -0.00701(14) 0.00549(13) -0.00722(14)
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| 228 | S2B 0.02059(16) 0.0349(2) 0.02883(18) 0.00295(14) 0.00236(13) 0.00282(13)
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| 229 | C7B 0.0220(6) 0.0259(7) 0.0209(6) -0.0020(5) 0.0036(5) 0.0014(5)
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| 230 | C8B 0.0293(7) 0.0287(7) 0.0266(7) 0.0048(5) 0.0027(5) 0.0007(6)
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| 231 | C9B 0.0310(7) 0.0321(8) 0.0324(7) 0.0041(6) 0.0066(6) -0.0067(6)
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| 232 | C10B 0.0208(6) 0.0369(8) 0.0401(8) -0.0007(6) 0.0044(6) -0.0012(6)
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| 233 | C11B 0.0244(6) 0.0303(7) 0.0372(8) 0.0058(6) 0.0021(6) 0.0032(6)
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| 234 | N2B 0.0231(5) 0.0275(6) 0.0321(6) 0.0051(5) 0.0038(4) 0.0014(5)
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| 235 |
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| 236 | _geom_special_details
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| 237 | ;
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| 238 | All esds (except the esd in the dihedral angle between two l.s. planes)
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| 239 | are estimated using the full covariance matrix. The cell esds are taken
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| 240 | into account individually in the estimation of esds in distances, angles
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| 241 | and torsion angles; correlations between esds in cell parameters are only
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| 242 | used when they are defined by crystal symmetry. An approximate (isotropic)
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| 243 | treatment of cell esds is used for estimating esds involving l.s. planes.
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| 244 | ;
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| 245 |
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| 246 | loop_
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| 247 | _geom_bond_atom_site_label_1
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| 248 | _geom_bond_atom_site_label_2
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| 249 | _geom_bond_distance
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| 250 | _geom_bond_site_symmetry_2
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| 251 | _geom_bond_publ_flag
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| 252 | N1A C6A 1.3312(18) . ?
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| 253 | N1A C2A 1.3389(19) . ?
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| 254 | C2A C3A 1.381(2) . ?
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| 255 | C2A H2A 0.9500 . ?
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| 256 | C3A C4A 1.376(2) . ?
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| 257 | C3A H3A 0.9500 . ?
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| 258 | C4A C5A 1.389(2) . ?
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| 259 | C4A H4A 0.9500 . ?
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| 260 | C5A C6A 1.3829(19) . ?
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| 261 | C5A H5A 0.9500 . ?
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| 262 | C6A S1A 1.7869(14) . ?
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| 263 | S1A S2A 2.0222(5) . ?
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| 264 | S2A C7A 1.7846(13) . ?
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| 265 | C7A N2A 1.3321(17) . ?
|
|---|
| 266 | C7A C8A 1.3816(18) . ?
|
|---|
| 267 | C8A C9A 1.3818(18) . ?
|
|---|
| 268 | C8A H8A 0.9500 . ?
|
|---|
| 269 | C9A C10A 1.382(2) . ?
|
|---|
| 270 | C9A H9A 0.9500 . ?
|
|---|
| 271 | C10A C11A 1.380(2) . ?
|
|---|
| 272 | C10A H10A 0.9500 . ?
|
|---|
| 273 | C11A N2A 1.3426(18) . ?
|
|---|
| 274 | C11A H11A 0.9500 . ?
|
|---|
| 275 | N1B C6B 1.3314(18) . ?
|
|---|
| 276 | N1B C2B 1.3405(19) . ?
|
|---|
| 277 | C2B C3B 1.380(2) . ?
|
|---|
| 278 | C2B H2B 0.9500 . ?
|
|---|
| 279 | C3B C4B 1.380(2) . ?
|
|---|
| 280 | C3B H3B 0.9500 . ?
|
|---|
| 281 | C4B C5B 1.382(2) . ?
|
|---|
| 282 | C4B H4B 0.9500 . ?
|
|---|
| 283 | C5B C6B 1.3838(19) . ?
|
|---|
| 284 | C5B H5B 0.9500 . ?
|
|---|
| 285 | C6B S1B 1.7847(14) . ?
|
|---|
| 286 | S1B S2B 2.0165(5) . ?
|
|---|
| 287 | S2B C7B 1.7881(13) . ?
|
|---|
| 288 | C7B N2B 1.3233(17) . ?
|
|---|
| 289 | C7B C8B 1.3867(18) . ?
|
|---|
| 290 | C8B C9B 1.3789(19) . ?
|
|---|
| 291 | C8B H8B 0.9500 . ?
|
|---|
| 292 | C9B C10B 1.384(2) . ?
|
|---|
| 293 | C9B H9B 0.9500 . ?
|
|---|
| 294 | C10B C11B 1.377(2) . ?
|
|---|
| 295 | C10B H10B 0.9500 . ?
|
|---|
| 296 | C11B N2B 1.3437(17) . ?
|
|---|
| 297 | C11B H11B 0.9500 . ?
|
|---|
| 298 |
|
|---|
| 299 | loop_
|
|---|
| 300 | _geom_angle_atom_site_label_1
|
|---|
| 301 | _geom_angle_atom_site_label_2
|
|---|
| 302 | _geom_angle_atom_site_label_3
|
|---|
| 303 | _geom_angle
|
|---|
| 304 | _geom_angle_site_symmetry_1
|
|---|
| 305 | _geom_angle_site_symmetry_3
|
|---|
| 306 | _geom_angle_publ_flag
|
|---|
| 307 | C6A N1A C2A 116.66(13) . . ?
|
|---|
| 308 | N1A C2A C3A 123.53(14) . . ?
|
|---|
| 309 | N1A C2A H2A 118.2 . . ?
|
|---|
| 310 | C3A C2A H2A 118.2 . . ?
|
|---|
| 311 | C4A C3A C2A 118.54(14) . . ?
|
|---|
| 312 | C4A C3A H3A 120.7 . . ?
|
|---|
| 313 | C2A C3A H3A 120.7 . . ?
|
|---|
| 314 | C3A C4A C5A 119.29(14) . . ?
|
|---|
| 315 | C3A C4A H4A 120.4 . . ?
|
|---|
| 316 | C5A C4A H4A 120.4 . . ?
|
|---|
| 317 | C4A C5A C6A 117.44(14) . . ?
|
|---|
| 318 | C4A C5A H5A 121.3 . . ?
|
|---|
| 319 | C6A C5A H5A 121.3 . . ?
|
|---|
| 320 | N1A C6A C5A 124.51(13) . . ?
|
|---|
| 321 | N1A C6A S1A 109.98(10) . . ?
|
|---|
| 322 | C5A C6A S1A 125.49(11) . . ?
|
|---|
| 323 | C6A S1A S2A 105.61(5) . . ?
|
|---|
| 324 | C7A S2A S1A 105.63(5) . . ?
|
|---|
| 325 | N2A C7A C8A 124.64(12) . . ?
|
|---|
| 326 | N2A C7A S2A 110.60(9) . . ?
|
|---|
| 327 | C8A C7A S2A 124.76(10) . . ?
|
|---|
| 328 | C9A C8A C7A 117.47(12) . . ?
|
|---|
| 329 | C9A C8A H8A 121.3 . . ?
|
|---|
| 330 | C7A C8A H8A 121.3 . . ?
|
|---|
| 331 | C8A C9A C10A 119.37(13) . . ?
|
|---|
| 332 | C8A C9A H9A 120.3 . . ?
|
|---|
| 333 | C10A C9A H9A 120.3 . . ?
|
|---|
| 334 | C11A C10A C9A 118.60(13) . . ?
|
|---|
| 335 | C11A C10A H10A 120.7 . . ?
|
|---|
| 336 | C9A C10A H10A 120.7 . . ?
|
|---|
| 337 | N2A C11A C10A 123.26(13) . . ?
|
|---|
| 338 | N2A C11A H11A 118.4 . . ?
|
|---|
| 339 | C10A C11A H11A 118.4 . . ?
|
|---|
| 340 | C7A N2A C11A 116.64(12) . . ?
|
|---|
| 341 | C6B N1B C2B 116.64(13) . . ?
|
|---|
| 342 | N1B C2B C3B 123.52(14) . . ?
|
|---|
| 343 | N1B C2B H2B 118.2 . . ?
|
|---|
| 344 | C3B C2B H2B 118.2 . . ?
|
|---|
| 345 | C2B C3B C4B 118.39(13) . . ?
|
|---|
| 346 | C2B C3B H3B 120.8 . . ?
|
|---|
| 347 | C4B C3B H3B 120.8 . . ?
|
|---|
| 348 | C3B C4B C5B 119.50(14) . . ?
|
|---|
| 349 | C3B C4B H4B 120.2 . . ?
|
|---|
| 350 | C5B C4B H4B 120.2 . . ?
|
|---|
| 351 | C4B C5B C6B 117.46(14) . . ?
|
|---|
| 352 | C4B C5B H5B 121.3 . . ?
|
|---|
| 353 | C6B C5B H5B 121.3 . . ?
|
|---|
| 354 | N1B C6B C5B 124.47(13) . . ?
|
|---|
| 355 | N1B C6B S1B 110.82(10) . . ?
|
|---|
| 356 | C5B C6B S1B 124.69(11) . . ?
|
|---|
| 357 | C6B S1B S2B 105.07(5) . . ?
|
|---|
| 358 | C7B S2B S1B 105.30(5) . . ?
|
|---|
| 359 | N2B C7B C8B 125.00(12) . . ?
|
|---|
| 360 | N2B C7B S2B 119.87(10) . . ?
|
|---|
| 361 | C8B C7B S2B 115.13(10) . . ?
|
|---|
| 362 | C9B C8B C7B 117.61(13) . . ?
|
|---|
| 363 | C9B C8B H8B 121.2 . . ?
|
|---|
| 364 | C7B C8B H8B 121.2 . . ?
|
|---|
| 365 | C8B C9B C10B 118.94(13) . . ?
|
|---|
| 366 | C8B C9B H9B 120.5 . . ?
|
|---|
| 367 | C10B C9B H9B 120.5 . . ?
|
|---|
| 368 | C11B C10B C9B 118.59(13) . . ?
|
|---|
| 369 | C11B C10B H10B 120.7 . . ?
|
|---|
| 370 | C9B C10B H10B 120.7 . . ?
|
|---|
| 371 | N2B C11B C10B 123.78(13) . . ?
|
|---|
| 372 | N2B C11B H11B 118.1 . . ?
|
|---|
| 373 | C10B C11B H11B 118.1 . . ?
|
|---|
| 374 | C7B N2B C11B 116.07(12) . . ?
|
|---|
| 375 |
|
|---|
| 376 | loop_
|
|---|
| 377 | _geom_torsion_atom_site_label_1
|
|---|
| 378 | _geom_torsion_atom_site_label_2
|
|---|
| 379 | _geom_torsion_atom_site_label_3
|
|---|
| 380 | _geom_torsion_atom_site_label_4
|
|---|
| 381 | _geom_torsion
|
|---|
| 382 | _geom_torsion_site_symmetry_1
|
|---|
| 383 | _geom_torsion_site_symmetry_2
|
|---|
| 384 | _geom_torsion_site_symmetry_3
|
|---|
| 385 | _geom_torsion_site_symmetry_4
|
|---|
| 386 | _geom_torsion_publ_flag
|
|---|
| 387 | C6A N1A C2A C3A 1.0(2) . . . . ?
|
|---|
| 388 | N1A C2A C3A C4A -1.5(2) . . . . ?
|
|---|
| 389 | C2A C3A C4A C5A 0.7(2) . . . . ?
|
|---|
| 390 | C3A C4A C5A C6A 0.6(2) . . . . ?
|
|---|
| 391 | C2A N1A C6A C5A 0.3(2) . . . . ?
|
|---|
| 392 | C2A N1A C6A S1A -177.91(11) . . . . ?
|
|---|
| 393 | C4A C5A C6A N1A -1.1(2) . . . . ?
|
|---|
| 394 | C4A C5A C6A S1A 176.84(11) . . . . ?
|
|---|
| 395 | N1A C6A S1A S2A -174.22(8) . . . . ?
|
|---|
| 396 | C5A C6A S1A S2A 7.58(13) . . . . ?
|
|---|
| 397 | C6A S1A S2A C7A -85.28(6) . . . . ?
|
|---|
| 398 | S1A S2A C7A N2A -175.96(8) . . . . ?
|
|---|
| 399 | S1A S2A C7A C8A 4.80(12) . . . . ?
|
|---|
| 400 | N2A C7A C8A C9A -1.2(2) . . . . ?
|
|---|
| 401 | S2A C7A C8A C9A 177.91(10) . . . . ?
|
|---|
| 402 | C7A C8A C9A C10A 1.2(2) . . . . ?
|
|---|
| 403 | C8A C9A C10A C11A 0.0(2) . . . . ?
|
|---|
| 404 | C9A C10A C11A N2A -1.4(2) . . . . ?
|
|---|
| 405 | C8A C7A N2A C11A -0.08(19) . . . . ?
|
|---|
| 406 | S2A C7A N2A C11A -179.32(10) . . . . ?
|
|---|
| 407 | C10A C11A N2A C7A 1.4(2) . . . . ?
|
|---|
| 408 | C6B N1B C2B C3B -0.5(2) . . . . ?
|
|---|
| 409 | N1B C2B C3B C4B 1.1(2) . . . . ?
|
|---|
| 410 | C2B C3B C4B C5B -0.5(2) . . . . ?
|
|---|
| 411 | C3B C4B C5B C6B -0.7(2) . . . . ?
|
|---|
| 412 | C2B N1B C6B C5B -0.8(2) . . . . ?
|
|---|
| 413 | C2B N1B C6B S1B 177.54(10) . . . . ?
|
|---|
| 414 | C4B C5B C6B N1B 1.4(2) . . . . ?
|
|---|
| 415 | C4B C5B C6B S1B -176.73(11) . . . . ?
|
|---|
| 416 | N1B C6B S1B S2B 168.91(8) . . . . ?
|
|---|
| 417 | C5B C6B S1B S2B -12.76(13) . . . . ?
|
|---|
| 418 | C6B S1B S2B C7B 86.16(6) . . . . ?
|
|---|
| 419 | S1B S2B C7B N2B -4.70(11) . . . . ?
|
|---|
| 420 | S1B S2B C7B C8B 176.10(9) . . . . ?
|
|---|
| 421 | N2B C7B C8B C9B 0.8(2) . . . . ?
|
|---|
| 422 | S2B C7B C8B C9B -179.99(11) . . . . ?
|
|---|
| 423 | C7B C8B C9B C10B -0.1(2) . . . . ?
|
|---|
| 424 | C8B C9B C10B C11B -0.2(2) . . . . ?
|
|---|
| 425 | C9B C10B C11B N2B -0.1(2) . . . . ?
|
|---|
| 426 | C8B C7B N2B C11B -1.2(2) . . . . ?
|
|---|
| 427 | S2B C7B N2B C11B 179.68(10) . . . . ?
|
|---|
| 428 | C10B C11B N2B C7B 0.8(2) . . . . ?
|
|---|
| 429 |
|
|---|
| 430 | loop_
|
|---|
| 431 | _geom_hbond_atom_site_label_D
|
|---|
| 432 | _geom_hbond_atom_site_label_H
|
|---|
| 433 | _geom_hbond_atom_site_label_A
|
|---|
| 434 | _geom_hbond_distance_DH
|
|---|
| 435 | _geom_hbond_distance_HA
|
|---|
| 436 | _geom_hbond_distance_DA
|
|---|
| 437 | _geom_hbond_angle_DHA
|
|---|
| 438 | _geom_hbond_site_symmetry_A
|
|---|
| 439 | C11B H11B N1A 0.95 2.75 3.5089(18) 137.0 2_645
|
|---|
| 440 | C8B H8B N2A 0.95 2.58 3.5009(19) 164.4 1_565
|
|---|
| 441 | C9A H9A N1B 0.95 2.76 3.5194(18) 137.7 2
|
|---|
| 442 | C4A H4A N2B 0.95 2.77 3.5091(19) 134.8 4_565
|
|---|
| 443 |
|
|---|
| 444 | _diffrn_measured_fraction_theta_max 0.998
|
|---|
| 445 | _diffrn_reflns_theta_full 27.35
|
|---|
| 446 | _diffrn_measured_fraction_theta_full 0.998
|
|---|
| 447 | _refine_diff_density_max 0.270
|
|---|
| 448 | _refine_diff_density_min -0.220
|
|---|
| 449 | _refine_diff_density_rms 0.043
|
|---|
