data_tbtfac loop_ _audit_conform.dict_name _audit_conform.dict_version _audit_conform.dict_location cif_core.dic . ftp://ftp.iucr.org/pub/cif_core.dic cif_pd.dic . ftp://ftp.iucr.org/pub/cif_pd.dic # 5. CHEMICAL DATA _chemical_name_systematic ; theobromine trifluoroacetic acid ; _chemical_name_common 'theobromine trifluoroacetic acid' _chemical_formula_moiety 'C7 H8 N4 O2, C2 H F3 O2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C9 H9 F3 N4 O4' _chemical_formula_weight 294.20 _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source 'C' 'C' 'International Tables Vol C Table 6.1.1.4' 'H' 'H' 'International Tables Vol C Table 6.1.1.4' 'O' 'O' 'International Tables Vol C Table 6.1.1.4' 'Cl' 'Cl' 'International Tables Vol C Table 6.1.1.4' 'N' 'N' 'International Tables Vol C Table 6.1.1.4' #============================================================================== # 6. POWDER SPECIMEN AND CRYSTAL DATA _space_group_crystal_system triclinic _space_group_name_H-M_alt 'P-1' _space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz '-x, -y, -z' 'x, y, z' _cell_length_a 5.09253(14) _cell_length_b 8.33537(37) _cell_length_c 14.89683(42) _cell_angle_alpha 90.1645(18) _cell_angle_beta 95.5873(17) _cell_angle_gamma 99.7283(22) _cell_volume 620.168(37) _cell_formula_units_Z 2 _cell_measurement_temperature 298 _exptl_crystal_density_diffrn 1.576 _cell_special_details ; The pattern was indexed with Dicvol91 (Boultif \& Lou\"er, 1991). ; # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting # This field should be # used to give details of the # container. ; ? ; _pd_spec_mount_mode ? # options are 'reflection' # or 'transmission' _pd_spec_shape ? # options are 'cylinder' # 'flat_sheet' or 'irregular' _pd_char_particle_morphology ? _pd_char_colour ? # use ICDD colour descriptions # The following three fields describe the preparation of the specimen. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure 100 _pd_prep_temperature 298 # The next four fields are normally only needed for transmission experiments. _exptl_absorpt_coefficient_mu 1.360 _exptl_absorpt_correction_type none # include if applicable _exptl_absorpt_process_details ? # include if applicable _exptl_absorpt_correction_T_min ? # include if applicable _exptl_absorpt_correction_T_max ? # include if applicable #============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; # The following item is used to identify the equipment used to record # the powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; ? ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; ? ; _diffrn_ambient_temperature 298 _diffrn_source 'sealed X-ray tube' # or rotating anode _diffrn_source_target 'Cu' _diffrn_source_type ? # make or model of source _diffrn_radiation_type 'Cu K\a~1~' _diffrn_measurement_device_type ? _diffrn_detector ? # e.g. image plate, scintillation counter _diffrn_detector_type ? # make or model of detector _pd_meas_scan_method ? # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following six items are used for angular dispersive measurements only. _diffrn_radiation_wavelength 1.54056 _diffrn_radiation_monochromator ? # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 13135 _pd_meas_2theta_range_min 5.0021 _pd_meas_2theta_range_max 59.9881 _pd_meas_2theta_range_inc 0.004187 # The following three items are used for time-of-flight measurements only. _pd_instr_dist_src/spec ? _pd_instr_dist_spec/detc ? _pd_meas_2theta_fixed ? #============================================================================== # 8. REFINEMENT DATA # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; ? ; # The next three items are given as text. _pd_proc_ls_profile_function 'double-Voigt (Balzar, 1999)' _pd_proc_ls_background_function 'Chebyshev polynomial, 15 terms' _pd_proc_ls_pref_orient_corr ; March (1932), along the -114 axis, ratio = 0.9062(11) ; _pd_proc_ls_prof_R_factor 0.04426 _pd_proc_ls_prof_wR_factor 0.05726 _pd_proc_ls_prof_wR_expected 0.02279 _refine_ls_R_I_factor 0.03122 _refine_ls_R_Fsqd_factor ? _refine_ls_R_factor_all ? _refine_special_details ; Bond lengths and angles (including those with H atoms) were restrained to values taken from the CSD entries MANJAN and SEDNAQ. All atoms were constrained to have the same isotropic displacement parameter. ; _refine_ls_matrix_type sparse _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_parameters 118 _refine_ls_number_restraints 78 _refine_ls_number_constraints 1 # The following item is the same as CHI, the square root of 'CHI squared' _refine_ls_goodness_of_fit_all 1.585 _refine_ls_restrained_S_all ? _refine_ls_shift/su_max ? _refine_ls_shift/su_mean ? # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 5.0021 _pd_proc_2theta_range_max 59.9881 _pd_proc_2theta_range_inc 0.004187 _pd_proc_wavelength 1.54056 # Each refinement must be accompanied by a listing of the powder data # in CIF format. Each listing should be sent as a separate file consisting # of one data block containing a single powder profile. The value of # _pd_block_diffractogram_id is used to associate each refinement with # its corresponding powder profile, since it must match the value # of _pd_block_id in the file containing the powder data. A template # for supplying powder data in CIF format is available by ftp at # ftp://ftp.iucr.org/pub/rietdataform.cif and an example is given # at ftp://ftp.iucr.org/pub/rietdataxmpl.cif. _pd_block_diffractogram_id tbtfac # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions 'none' _pd_proc_info_data_reduction 'none' # The following items are used to identify the programs used. _computing_data_collection ? _computing_cell_refinement 'Topas V3 (Bruker AXS, 2005)' _computing_data_reduction ? _computing_structure_solution 'DASH 3.0 (David et al., 2004)' _computing_structure_refinement 'Topas V3 (Bruker AXS, 2005)' _computing_molecular_graphics ? _computing_publication_material ? #============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_symmetry_multiplicity _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_B_iso_or_equiv C1 C 0 0.10156(50) 0.65142(27) 0.62790(14) 1 9.57(11) C2 C 0 0.22772(45) 0.55171(44) 0.69525(14) 1 9.57(11) C3 C 0 -0.14233(70) 0.60153(48) 0.56866(23) 1 9.57(11) N4 N 0 0.26974(76) 0.79283(46) 0.63731(25) 1 9.57(11) N5 N 0 0.12844(73) 0.39259(45) 0.71202(23) 1 9.57(11) N6 N 0 0.45119(83) 0.62341(55) 0.74114(28) 1 9.57(11) N7 N 0 -0.22333(79) 0.43939(46) 0.59037(24) 1 9.57(11) O8 O 0 -0.26930(92) 0.67380(61) 0.51163(31) 1 9.57(11) C9 C 0 0.47753(80) 0.77256(48) 0.70363(29) 1 9.57(11) C10 C 0 0.20622(76) 0.92827(45) 0.58371(23) 1 9.57(11) C11 C 0 -0.11363(81) 0.33430(47) 0.65501(29) 1 9.57(11) C12 C 0 0.26011(70) 0.30334(41) 0.77921(22) 1 9.57(11) H13 H 0 -0.3681(26) 0.3990(14) 0.55790(83) 1 9.57(11) H14 H 0 0.6450(24) 0.8647(14) 0.72686(80) 1 9.57(11) H15 H 0 0.1571(23) 0.8902(14) 0.51851(90) 1 9.57(11) H16 H 0 0.0563(27) 0.9468(16) 0.60148(72) 1 9.57(11) H17 H 0 0.3454(24) 1.0385(18) 0.59519(74) 1 9.57(11) O18 O 0 -0.2175(10) 0.20210(60) 0.66467(33) 1 9.57(11) H19 H 0 0.1445(26) 0.2385(15) 0.81623(83) 1 9.57(11) H20 H 0 0.3675(28) 0.3863(15) 0.82062(84) 1 9.57(11) H21 H 0 0.3590(27) 0.2477(16) 0.75458(77) 1 9.57(11) C22 C 0 0.76193(43) 0.23796(37) 0.03757(15) 1 9.57(11) F23 F 0 0.67714(94) 0.38255(53) 0.02652(34) 1 9.57(11) F24 F 0 0.54644(98) 0.14693(55) 0.05252(33) 1 9.57(11) F25 F 0 0.89181(99) 0.20907(61) -0.03294(31) 1 9.57(11) C26 C 0 0.93675(36) 0.22123(25) 0.11663(13) 1 9.57(11) O27 O 0 1.10146(34) 0.37343(29) 0.13403(15) 1 9.57(11) O28 O 0 0.99695(38) 0.11918(42) 0.17642(15) 1 9.57(11) H29 H 0 1.2095(26) 0.3597(15) 0.18405(96) 1 9.57(11) #============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ? 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 1.473(4) . n C1 C3 1.451(4) . n C1 N4 1.333(4) . n C2 N5 1.370(5) . n C2 N6 1.318(5) . n C3 N7 1.393(5) . n C3 O8 1.237(6) . n N4 C9 1.408(6) . n N4 C10 1.447(5) . n N5 C11 1.438(5) . n N5 C12 1.431(5) . n N6 C9 1.356(6) . n N7 C11 1.439(6) . n N7 H13 0.858(12) . n C9 H14 1.075(12) . n C10 H15 1.015(13) . n C10 H16 0.869(15) . n C10 H17 1.064(14) . n C11 O18 1.155(6) . n C12 H19 0.949(13) . n C12 H20 0.981(13) . n C12 H21 0.847(15) . n C22 F23 1.353(6) . n C22 F24 1.264(5) . n C22 F25 1.337(6) . n C22 C26 1.428(3) . n C26 O27 1.406(3) . n C26 O28 1.285(4) . n O27 H29 0.902(14) . n 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 C2 C1 C3 127.2(2) . . n C2 C1 N4 101.5(2) . . n C3 C1 N4 131.3(3) . . n C1 C2 N5 124.4(2) . . n C1 C2 N6 116.3(3) . . n N5 C2 N6 119.3(3) . . n C1 C3 N7 103.6(3) . . n C1 C3 O8 133.1(4) . . n N7 C3 O8 123.3(4) . . n C1 N4 C9 107.3(3) . . n C1 N4 C10 118.3(3) . . n C9 N4 C10 134.3(3) . . n C2 N5 C11 111.5(3) . . n C2 N5 C12 121.4(3) . . n C11 N5 C12 127.1(3) . . n C2 N6 C9 100.1(4) . . n C3 N7 C11 132.6(3) . . n C3 N7 H13 110.2(9) . . n C11 N7 H13 117.2(9) . . n N4 C9 N6 114.7(3) . . n N4 C9 H14 125.6(7) . . n N6 C9 H14 119.6(7) . . n N4 C10 H15 109.1(8) . . n N4 C10 H16 104.4(9) . . n N4 C10 H17 114.9(7) . . n H15 C10 H16 104.1(10) . . n H15 C10 H17 116.6(9) . . n H16 C10 H17 106.4(11) . . n N5 C11 N7 120.7(3) . . n N5 C11 O18 117.4(4) . . n N7 C11 O18 121.9(4) . . n N5 C12 H19 114.9(9) . . n N5 C12 H20 105.1(8) . . n N5 C12 H21 109.6(9) . . n H19 C12 H20 104.4(11) . . n H19 C12 H21 111.6(13) . . n H20 C12 H21 111.0(12) . . n F23 C22 F24 100.7(3) . . n F23 C22 F25 108.9(4) . . n F23 C22 C26 117.1(3) . . n F24 C22 F25 120.8(4) . . n F24 C22 C26 103.2(3) . . n F25 C22 C26 106.7(3) . . n C22 C26 O27 106.8(2) . . n C22 C26 O28 143.1(2) . . n O27 C26 O28 110.06(19) . . n C26 O27 H29 105.1(8) . . n #============================================================================== # Additional structures (sections 5-10 and associated data_? identifiers) # may be added at this point. #============================================================================== # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ data_tbmalon loop_ _audit_conform.dict_name _audit_conform.dict_version _audit_conform.dict_location cif_core.dic . ftp://ftp.iucr.org/pub/cif_core.dic cif_pd.dic . ftp://ftp.iucr.org/pub/cif_pd.dic # 5. CHEMICAL DATA _chemical_name_systematic ; theobromine malonic acid ; _chemical_name_common 'theobromine malonic acid' _chemical_formula_moiety 'C7 H8 N4 O2, C3 H4 O4' _chemical_formula_sum 'C10 H12 N4 O6' _chemical_formula_weight 284.24 _chemical_melting_point ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_compound_source ? # for minerals and # natural products loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source 'C' 'C' 'International Tables Vol C Table 6.1.1.4' 'H' 'H' 'International Tables Vol C Table 6.1.1.4' 'O' 'O' 'International Tables Vol C Table 6.1.1.4' 'Cl' 'Cl' 'International Tables Vol C Table 6.1.1.4' 'N' 'N' 'International Tables Vol C Table 6.1.1.4' #============================================================================== # 6. POWDER SPECIMEN AND CRYSTAL DATA _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P21/c' _space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x,1/2+y,1/2-z' 'x,1/2-y,1/2+z' _cell_length_a 12.44248(60) _cell_length_b 12.90355(55) _cell_length_c 7.67255(26) _cell_angle_alpha 90 _cell_angle_beta 91.2464(23) _cell_angle_gamma 90 _cell_volume 1231.553(90) _cell_formula_units_Z 4 _cell_measurement_temperature 298 _cell_special_details ; The pattern was indexed with Dicvol91 (Boultif \& Lou\"er, 1991). ; # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting # This field should be # used to give details of the # container. ; ? ; _pd_spec_mount_mode ? # options are 'reflection' # or 'transmission' _pd_spec_shape ? # options are 'cylinder' # 'flat_sheet' or 'irregular' _pd_char_particle_morphology ? _pd_char_colour ? # use ICDD colour descriptions # The following three fields describe the preparation of the specimen. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure 100 _pd_prep_temperature 298 # The next four fields are normally only needed for transmission experiments. _exptl_absorpt_coefficient_mu 1.112 _exptl_absorpt_correction_type none # include if applicable _exptl_absorpt_process_details ? # include if applicable _exptl_absorpt_correction_T_min ? # include if applicable _exptl_absorpt_correction_T_max ? # include if applicable #============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; # The following item is used to identify the equipment used to record # the powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; ? ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; ? ; _diffrn_ambient_temperature 298 _diffrn_source 'sealed X-ray tube' # or rotating anode _diffrn_source_target 'Cu' _diffrn_source_type ? # make or model of source _diffrn_radiation_type 'Cu K\a~1~' _diffrn_measurement_device_type ? _diffrn_detector ? # e.g. image plate, scintillation counter _diffrn_detector_type ? # make or model of detector _pd_meas_scan_method ? # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following six items are used for angular dispersive measurements only. _diffrn_radiation_wavelength 1.54056 _diffrn_radiation_monochromator ? # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 6569 _pd_meas_2theta_range_min 5.0042 _pd_meas_2theta_range_max 59.8896 _pd_meas_2theta_range_inc 0.008373 # The following three items are used for time-of-flight measurements only. _pd_instr_dist_src/spec ? _pd_instr_dist_spec/detc ? _pd_meas_2theta_fixed ? #============================================================================== # 8. REFINEMENT DATA # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; ? ; # The next three items are given as text. _pd_proc_ls_profile_function 'double-Voigt (Balzar, 1999)' _pd_proc_ls_background_function 'Chebyshev polynomial, 15 terms' _pd_proc_ls_pref_orient_corr ; March (1932), along the 100 axis, ratio = 0.951(2) ; _pd_proc_ls_prof_R_factor 0.05166 _pd_proc_ls_prof_wR_factor 0.07485 _pd_proc_ls_prof_wR_expected 0.03035 _refine_ls_R_I_factor 0.02868 _refine_ls_R_Fsqd_factor ? _refine_ls_R_factor_all ? _refine_special_details ; Bond lengths and angles (including those with H atoms) were restrained to values taken from the CSD entries MALNAC02 and SEDNAQ. All atoms were constrained to have the same isotropic displacement parameter. ; _refine_ls_matrix_type sparse _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_parameters 119 _refine_ls_number_restraints 86 _refine_ls_number_constraints 1 # The following item is the same as CHI, the square root of 'CHI squared' _refine_ls_goodness_of_fit_all 1.570 _refine_ls_restrained_S_all ? _refine_ls_shift/su_max ? _refine_ls_shift/su_mean ? # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 5.0042 _pd_proc_2theta_range_max 59.8896 _pd_proc_2theta_range_inc 0.008373 _pd_proc_wavelength 1.54056 # Each refinement must be accompanied by a listing of the powder data # in CIF format. Each listing should be sent as a separate file consisting # of one data block containing a single powder profile. The value of # _pd_block_diffractogram_id is used to associate each refinement with # its corresponding powder profile, since it must match the value # of _pd_block_id in the file containing the powder data. A template # for supplying powder data in CIF format is available by ftp at # ftp://ftp.iucr.org/pub/rietdataform.cif and an example is given # at ftp://ftp.iucr.org/pub/rietdataxmpl.cif. _pd_block_diffractogram_id tbmalon # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions 'none' _pd_proc_info_data_reduction 'none' # The following items are used to identify the programs used. _computing_data_collection ? _computing_cell_refinement 'Topas V3 (Bruker AXS, 2005)' _computing_data_reduction ? _computing_structure_solution 'DASH 3.0 (David et al., 2004)' _computing_structure_refinement 'Topas V3 (Bruker AXS, 2005)' _computing_molecular_graphics ? _computing_publication_material ? #============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_symmetry_multiplicity _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_B_iso_or_equiv C1 C 0 0.62846(28) 0.85808(34) 0.89842(41) 1 4.351(99) C2 C 0 0.66675(21) 0.96441(43) 0.94210(41) 1 4.351(99) C3 C 0 0.71123(42) 0.78216(29) 0.93074(41) 1 4.351(99) H4 H 0 0.5682(11) 0.8456(17) 0.9709(26) 1 4.351(99) H5 H 0 0.6091(12) 0.8569(17) 0.7896(26) 1 4.351(99) O6 O 0 0.72889(26) 0.99689(57) 1.02714(39) 1 4.351(99) O7 O 0 0.58711(27) 1.00615(43) 0.82412(39) 1 4.351(99) O8 O 0 0.80663(46) 0.78850(41) 0.92050(30) 1 4.351(99) O9 O 0 0.66606(42) 0.69012(33) 0.98152(28) 1 4.351(99) H10 H 0 0.5711(13) 1.0811(15) 0.7930(31) 1 4.351(99) H11 H 0 0.7187(12) 0.6405(15) 1.0023(25) 1 4.351(99) C12 C 0 0.87113(22) 0.36154(43) 0.13762(49) 1 4.351(99) C13 C 0 0.78773(39) 0.42286(41) 0.04906(45) 1 4.351(99) C14 C 0 0.86692(42) 0.24524(43) 0.13262(69) 1 4.351(99) N15 N 0 0.94239(45) 0.43349(41) 0.21256(69) 1 4.351(99) N16 N 0 0.70025(39) 0.37486(43) -0.04160(62) 1 4.351(99) N17 N 0 0.80612(48) 0.52477(48) 0.06673(80) 1 4.351(99) N18 N 0 0.77717(41) 0.20605(41) 0.04287(69) 1 4.351(99) O19 O 0 0.92803(47) 0.18402(54) 0.19354(77) 1 4.351(99) C20 C 0 0.89962(45) 0.52735(43) 0.16520(77) 1 4.351(99) C21 C 0 1.04328(42) 0.40840(41) 0.31797(63) 1 4.351(99) C22 C 0 0.69401(46) 0.26313(44) -0.04600(79) 1 4.351(99) C23 C 0 0.61270(43) 0.43566(39) -0.12629(63) 1 4.351(99) H24 H 0 0.7741(13) 0.1421(14) 0.0383(26) 1 4.351(99) H25 H 0 0.9371(13) 0.5931(15) 0.2028(24) 1 4.351(99) H26 H 0 1.1021(12) 0.3752(16) 0.2459(26) 1 4.351(99) H27 H 0 1.0302(13) 0.3641(15) 0.4055(29) 1 4.351(99) H28 H 0 1.0694(12) 0.4790(14) 0.3679(25) 1 4.351(99) O29 O 0 0.61807(54) 0.21315(51) -0.12689(85) 1 4.351(99) H30 H 0 0.5424(13) 0.4086(16) -0.0999(23) 1 4.351(99) H31 H 0 0.6124(12) 0.5119(13) -0.0743(29) 1 4.351(99) H32 H 0 0.6198(12) 0.4369(14) -0.2425(27) 1 4.351(99) #============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ? 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 1.488(7) . n C1 C3 1.439(6) . n C1 H4 0.957(17) . n C1 H5 0.864(19) . n C2 O6 1.085(5) . n C2 O7 1.433(5) . n C3 O8 1.194(8) . n C3 O9 1.374(6) . n O7 H10 1.01(2) . n O9 H11 0.927(18) . n C12 C13 1.461(6) . n C12 C14 1.502(8) . n C12 N15 1.399(7) . n C13 N16 1.421(7) . n C13 N17 1.341(8) . n C14 N18 1.394(7) . n C14 O19 1.185(8) . n N15 C20 1.369(8) . n N15 C21 1.513(7) . n N16 C22 1.444(8) . n N16 C23 1.481(7) . n N17 C20 1.374(8) . n N18 C22 1.431(8) . n N18 H24 0.827(19) . n C20 H25 1.01(2) . n C21 H26 1.021(18) . n C21 H27 0.90(2) . n C21 H28 1.038(19) . n C22 O29 1.292(9) . n C23 H30 0.967(18) . n C23 H31 1.062(19) . n C23 H32 0.90(2) . n 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 C2 C1 C3 111.4(3) . . n C2 C1 H4 106.0(13) . . n C2 C1 H5 108.4(15) . . n C3 C1 H4 110.6(13) . . n C3 C1 H5 109.7(13) . . n H4 C1 H5 110.7(15) . . n C1 C2 O6 135.4(5) . . n C1 C2 O7 89.5(3) . . n O6 C2 O7 135.1(6) . . n C1 C3 O8 130.6(4) . . n C1 C3 O9 110.0(4) . . n O8 C3 O9 119.4(5) . . n C2 O7 H10 129.5(12) . . n C3 O9 H11 110.7(12) . . n C13 C12 C14 120.3(4) . . n C13 C12 N15 105.6(5) . . n C14 C12 N15 134.0(4) . . n C12 C13 N16 121.4(5) . . n C12 C13 N17 111.5(4) . . n N16 C13 N17 127.2(5) . . n C12 C14 N18 113.7(4) . . n C12 C14 O19 129.3(5) . . n N18 C14 O19 116.9(6) . . n C12 N15 C20 103.8(5) . . n C12 N15 C21 126.1(5) . . n C20 N15 C21 130.1(5) . . n C13 N16 C22 119.1(5) . . n C13 N16 C23 122.1(5) . . n C22 N16 C23 118.7(5) . . n C13 N17 C20 102.7(5) . . n C14 N18 C22 127.7(5) . . n C14 N18 H24 114.8(13) . . n C22 N18 H24 117.4(13) . . n N15 C20 N17 116.4(5) . . n N15 C20 H25 119.6(11) . . n N17 C20 H25 124.0(11) . . n N15 C21 H26 113.3(11) . . n N15 C21 H27 112.0(11) . . n N15 C21 H28 105.0(10) . . n H26 C21 H27 106.3(18) . . n H26 C21 H28 110.3(15) . . n H27 C21 H28 110.1(17) . . n N16 C22 N18 117.7(5) . . n N16 C22 O29 123.2(6) . . n N18 C22 O29 119.1(5) . . n N16 C23 H30 112.1(12) . . n N16 C23 H31 109.5(10) . . n N16 C23 H32 110.9(11) . . n H30 C23 H31 104.2(15) . . n H30 C23 H32 108.9(15) . . n H31 C23 H32 111.0(17) . . n #============================================================================== # Additional structures (sections 5-10 and associated data_? identifiers) # may be added at this point. #============================================================================== # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./