#============================================================================== data__compound3a #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C10 H21 N2 O0.50 ' _chemical_formula_moiety 'C10 H21 N2 O0.50 ' _chemical_formula_weight 177.29 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 '+X,+Y,+Z' 2 '-X,+Y,1/2-Z' 3 '-X,-Y,-Z' 4 '+X,-Y,1/2+Z' 5 '1/2+X,1/2+Y,+Z' 6 '1/2-X,1/2+Y,1/2-Z' 7 '1/2-X,1/2-Y,-Z' 8 '1/2+X,1/2-Y,1/2+Z' #------------------------------------------------------------------------------ _cell_length_a 22.675(3) _cell_length_b 6.1256(9) _cell_length_c 16.5599(18) _cell_angle_alpha 90.0000 _cell_angle_beta 113.194(3) _cell_angle_gamma 90.0000 _cell_volume 2114.3(5) _cell_formula_units_Z 8 _cell_measurement_reflns_used 7397 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 27.4 _cell_measurement_temperature 173.1 #------------------------------------------------------------------------------ _exptl_crystal_description 'needle' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.114 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792.00 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.007 _exptl_absorpt_correction_T_max 0.999 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 173.1 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 8937 _diffrn_reflns_av_R_equivalents 0.087 _diffrn_reflns_theta_max 27.45 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2388 _reflns_number_gt 1293 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.0660 _refine_ls_hydrogen_treatment refU _refine_ls_number_reflns 1311 _refine_ls_number_parameters 135 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0020Fo^2^ + 1.0000\s(Fo^2^)]' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.36 _refine_diff_density_min -0.26 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'N' 'N' 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'O' 'O' 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 O(1) O 1.0000 0.0864(4) 0.7500 0.0397(7) Uani 1.00 2 d S . . N(1) N 0.86944(9) 0.2795(3) 0.69757(12) 0.0227(5) Uani 1.00 1 d . . . N(2) N 0.87855(9) -0.1975(3) 0.75204(13) 0.0241(5) Uani 1.00 1 d . . . C(1) C 0.84548(11) 0.2726(4) 0.60070(15) 0.0267(6) Uani 1.00 1 d . . . C(2) C 0.83971(11) 0.0337(4) 0.57103(15) 0.0284(6) Uani 1.00 1 d . . . C(3) C 0.79730(11) -0.0972(4) 0.60560(15) 0.0290(6) Uani 1.00 1 d . . . C(4) C 0.81910(10) -0.0735(4) 0.70492(15) 0.0246(6) Uani 1.00 1 d . . . C(5) C 0.82516(10) 0.1704(3) 0.73013(15) 0.0239(6) Uani 1.00 1 d . . . C(6) C 0.84727(12) 0.1941(4) 0.82968(16) 0.0283(6) Uani 1.00 1 d . . . C(7) C 0.90809(11) 0.0615(4) 0.87932(15) 0.0277(6) Uani 1.00 1 d . . . C(8) C 0.90056(11) -0.1765(4) 0.84844(16) 0.0278(6) Uani 1.00 1 d . . . C(9) C 0.88950(12) 0.4031(4) 0.56958(17) 0.0350(7) Uani 1.00 1 d . . . C(10) C 0.96300(12) -0.3026(4) 0.89170(17) 0.0372(7) Uani 1.00 1 d . . . H(1) H 0.8028 0.3302 0.5725 0.025 Uiso 1.00 1 c R . . H(2) H 0.8216 0.0241 0.5084 0.021 Uiso 1.00 1 c R . . H(3) H 0.8848 -0.0295 0.5911 0.033 Uiso 1.00 1 c R . . H(4) H 0.7540 -0.0449 0.5767 0.028 Uiso 1.00 1 c R . . H(5) H 0.7956 -0.2545 0.5904 0.035 Uiso 1.00 1 c R . . H(6) H 0.7869 -0.1341 0.7220 0.029 Uiso 1.00 1 c R . . H(7) H 0.7829 0.2301 0.7014 0.018 Uiso 1.00 1 c R . . H(8) H 0.8532 0.3488 0.8445 0.029 Uiso 1.00 1 c R . . H(9) H 0.8116 0.1409 0.8465 0.038 Uiso 1.00 1 c R . . H(10) H 0.9468 0.1265 0.8726 0.027 Uiso 1.00 1 c R . . H(11) H 0.9171 0.0648 0.9414 0.021 Uiso 1.00 1 c R . . H(12) H 0.8670 -0.2415 0.8641 0.031 Uiso 1.00 1 c R . . H(13) H 0.8968 0.5530 0.5946 0.047 Uiso 1.00 1 c R . . H(14) H 0.8704 0.4118 0.5063 0.053 Uiso 1.00 1 c R . . H(15) H 0.9301 0.3348 0.5902 0.038 Uiso 1.00 1 c R . . H(16) H 0.9579 -0.4614 0.8731 0.044 Uiso 1.00 1 c R . . H(17) H 0.9791 -0.2981 0.9557 0.043 Uiso 1.00 1 c R . . H(18) H 0.9985 -0.2306 0.8778 0.045 Uiso 1.00 1 c R . . H(19) H 0.8741 0.4225 0.7134 0.044 Uiso 1.00 1 c R . . H(20) H 0.9090 -0.1472 0.7386 0.022 Uiso 1.00 1 c R . . H(21) H 1.0354 0.1720 0.7629 0.078 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O(1) 0.0279(13) 0.0329(15) 0.0610(18) 0.0000 0.0206(12) 0.0000 N(1) 0.0277(10) 0.0195(10) 0.0220(10) -0.0007(8) 0.0110(8) -0.0013(8) N(2) 0.0255(10) 0.0237(10) 0.0234(10) -0.0003(8) 0.0099(8) 0.0015(8) C(1) 0.0274(11) 0.0264(13) 0.0263(13) 0.0030(10) 0.0105(10) 0.0035(10) C(2) 0.0322(12) 0.0331(15) 0.0198(12) -0.0003(11) 0.0101(10) -0.0036(10) C(3) 0.0279(12) 0.0281(13) 0.0256(13) -0.0030(10) 0.0046(10) -0.0027(11) C(4) 0.0203(10) 0.0266(13) 0.0278(13) -0.0040(10) 0.0104(9) 0.0011(10) C(5) 0.0215(11) 0.0247(13) 0.0275(12) 0.0032(9) 0.0118(9) 0.0007(10) C(6) 0.0352(13) 0.0285(13) 0.0271(13) 0.0008(11) 0.0186(11) -0.0022(11) C(7) 0.0312(12) 0.0327(14) 0.0208(12) -0.0011(11) 0.0119(10) -0.0011(10) C(8) 0.0258(11) 0.0279(14) 0.0278(13) -0.0020(10) 0.0086(10) 0.0038(10) C(9) 0.0402(15) 0.0341(16) 0.0352(15) -0.0017(12) 0.0195(12) 0.0043(12) C(10) 0.0360(14) 0.0331(15) 0.0330(15) 0.0022(12) 0.0035(11) 0.0054(12) #============================================================================== _computing_data_collection 'PROCESS-AUTO' _computing_cell_refinement 'PROCESS-AUTO' _computing_data_reduction 'CrystalStructure' _computing_structure_solution 'SIR92' _computing_structure_refinement 'CRYSTALS' _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 N(1) C(1) 1.478(3) yes . . N(1) C(5) 1.474(3) yes . . N(2) C(4) 1.475(2) yes . . N(2) C(8) 1.479(3) yes . . C(1) C(2) 1.532(3) yes . . C(1) C(9) 1.519(4) yes . . C(2) C(3) 1.526(3) yes . . C(3) C(4) 1.526(3) yes . . C(4) C(5) 1.543(3) yes . . C(5) C(6) 1.529(3) yes . . C(6) C(7) 1.531(3) yes . . C(7) C(8) 1.532(3) yes . . C(8) C(10) 1.522(3) yes . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 C(1) N(1) C(5) 111.84(16) yes . . . C(4) N(2) C(8) 112.1(2) yes . . . N(1) C(1) C(2) 108.90(18) yes . . . N(1) C(1) C(9) 110.09(17) yes . . . C(2) C(1) C(9) 112.2(2) yes . . . C(1) C(2) C(3) 111.6(2) yes . . . C(2) C(3) C(4) 111.70(18) yes . . . N(2) C(4) C(3) 111.2(2) yes . . . N(2) C(4) C(5) 112.97(16) yes . . . C(3) C(4) C(5) 109.9(2) yes . . . N(1) C(5) C(4) 109.9(2) yes . . . N(1) C(5) C(6) 111.73(17) yes . . . C(4) C(5) C(6) 109.86(19) yes . . . C(5) C(6) C(7) 111.8(2) yes . . . C(6) C(7) C(8) 111.54(17) yes . . . N(2) C(8) C(7) 112.90(19) yes . . . N(2) C(8) C(10) 108.7(2) yes . . . C(7) C(8) C(10) 111.41(18) yes . . . #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================