# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1197 # Allan, Clark, Ibberson, Parsons, Pulham & Sawyer: # The influence of Pressure and Temperature on the Crystal # Structure of acetone. # These cifs are in the following order: # 1. High pressure structure (Cmcm). Room temperature. # 2. Metastable Cmcm low-temperature phase. 160K. # 3. Stable Pbca low-temperature phase. 150K # 4. Pbca phase at 5K (neutron powder data). # 5. Pbca phase at 110K (X-ray single crystal). data_HPCMCM #Data for the crystal structure of acetone at rt/15 kBar. _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Me2CO _chemical_formula_sum 'C3 H6 O' _chemical_formula_weight 58.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Cmcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z-1/2' 'x+1/2, -y+1/2, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 6.1219(11) _cell_length_b 5.2029(10) _cell_length_c 10.244(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 326.29(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5.12 _cell_measurement_theta_max 16.35 _exptl_crystal_description sphere _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.182 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 128 _exptl_absorpt_coefficient_mu 0.087 _exptl_absorpt_correction_type ; Analytical correction for the sample, gasket occlusion and cell. ; _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Note that the high pressure cell limits the volume of reciprocal space that may be sampled during data collection. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CAD-4 _diffrn_measurement_method Omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 158 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1067 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_theta_min 5.14 _diffrn_reflns_theta_max 39.14 _reflns_number_total 158 _reflns_number_gt 63 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0255P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens 'difference map' _refine_ls_hydrogen_treatment 'Rotating rigid group' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.008(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 158 _refine_ls_number_parameters 17 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1670 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.0982 _refine_ls_wR_factor_gt 0.0805 _refine_ls_goodness_of_fit_ref 0.907 _refine_ls_restrained_S_all 0.907 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.0000 0.3546(7) 0.2500 0.054(4) Uani 1 4 d S . . O1 O 1.0000 0.5861(5) 0.2500 0.061(5) Uani 1 4 d S . . C2 C 1.0000 0.2091(6) 0.1279(7) 0.055(3) Uani 1 2 d S . . H2A H 0.9146 0.2988 0.0638 0.083 Uiso 0.50 1 calc PR A -1 H2B H 0.9381 0.0421 0.1427 0.083 Uiso 0.50 1 calc PR A -1 H2C H 1.1472 0.1909 0.0970 0.083 Uiso 0.50 1 calc PR A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.033(3) 0.039(2) 0.091(14) 0.000 0.000 0.000 O1 0.091(3) 0.0513(18) 0.042(15) 0.000 0.000 0.000 C2 0.062(2) 0.0588(16) 0.044(11) 0.003(3) 0.000 0.000 _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 O1 1.205(5) . ? C1 C2 1.462(6) 10_556 ? C1 C2 1.462(6) . ? 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 O1 C1 C2 121.2(2) . 10_556 ? O1 C1 C2 121.2(2) . . ? C2 C1 C2 117.6(4) 10_556 . ? _diffrn_measured_fraction_theta_max 0.296 _diffrn_reflns_theta_full 39.14 _diffrn_measured_fraction_theta_full 0.296 _refine_diff_density_max 0.137 _refine_diff_density_min -0.137 _refine_diff_density_rms 0.039 #=END data_LTCMCM # Data for the metastable low-temperature Cmcm phase. _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Me2CO _chemical_formula_sum 'C3 H6 O' _chemical_formula_weight 58.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Cmcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z-1/2' 'x+1/2, -y+1/2, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 6.514(4) _cell_length_b 5.4159(18) _cell_length_c 10.756(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 379.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 53 _cell_measurement_theta_min 12 _cell_measurement_theta_max 16 _exptl_crystal_description cylinder _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.017 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 128 _exptl_absorpt_coefficient_mu 0.075 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% ? _diffrn_reflns_number 194 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0188 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 3.79 _diffrn_reflns_theta_max 24.96 _reflns_number_total 194 _reflns_number_gt 139 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution 'SIR92 in C2/c' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1098P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.09(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 194 _refine_ls_number_parameters 23 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0755 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1667 _refine_ls_wR_factor_gt 0.1469 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.111 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.001 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0000 0.3438(7) 0.2500 0.0491(13) Uani 1 4 d S . . O1 O 0.0000 0.5664(5) 0.2500 0.0890(18) Uani 1 4 d S . . C2 C 0.0000 0.2021(7) 0.1327(3) 0.0643(14) Uani 1 2 d S . . H2A H 0.0000 0.290(8) 0.071(4) 0.107(15) Uiso 1 2 d S . . H2B H 0.127(5) 0.136(8) 0.124(4) 0.133(13) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.040(2) 0.041(2) 0.067(3) 0.000 0.000 0.000 O1 0.113(3) 0.034(2) 0.120(3) 0.000 0.000 0.000 C2 0.080(3) 0.059(2) 0.054(2) 0.0057(14) 0.000 0.000 _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 O1 1.206(5) . ? C1 C2 1.477(4) . ? C1 C2 1.477(4) 10_556 ? 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 O1 C1 C2 121.32(18) . . ? O1 C1 C2 121.32(18) . 10_556 ? C2 C1 C2 117.4(4) . 10_556 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.96 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.279 _refine_diff_density_min -0.129 _refine_diff_density_rms 0.043 #=END data_150KPBCA # Data for the stable orthorhombic P low-temperature phase of acetone. _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H6 O' _chemical_formula_weight 58.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 8.873(3) _cell_length_b 8.000(4) _cell_length_c 22.027(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1563.5(10) _cell_formula_units_Z 16 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 64 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 16 _exptl_crystal_description cylinder _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.987 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 512 _exptl_absorpt_coefficient_mu 0.072 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2620 _diffrn_reflns_av_R_equivalents 0.1031 _diffrn_reflns_av_sigmaI/netI 0.0934 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 25.09 _reflns_number_total 1390 _reflns_number_gt 629 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0449P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment ; Positional parameters were refined subject to restraints the all CH and HH distances were similar. H(U[iso]) was constrained to be 1.5C(U[eq]). This procedure was adopted in order to obtain esd's on distances involving H. ; _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0035(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1390 _refine_ls_number_parameters 110 _refine_ls_number_restraints 132 _refine_ls_R_factor_all 0.1396 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_ref 0.1351 _refine_ls_wR_factor_gt 0.1039 _refine_ls_goodness_of_fit_ref 0.928 _refine_ls_restrained_S_all 0.890 _refine_ls_shift/su_max 0.044 _refine_ls_shift/su_mean 0.006 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1A O 0.0274(2) 0.0932(3) 0.76666(11) 0.0881(8) Uani 1 1 d . . . C1A C 0.1216(3) -0.0130(3) 0.75760(12) 0.0493(7) Uani 1 1 d . . . C2A C 0.1918(3) -0.1040(4) 0.80872(13) 0.0589(8) Uani 1 1 d D . . H2A1 H 0.169(2) -0.057(3) 0.8463(7) 0.088 Uiso 1 1 d D . . H2A2 H 0.2948(13) -0.100(3) 0.8021(10) 0.088 Uiso 1 1 d D . . H2A3 H 0.159(2) -0.2142(16) 0.8078(10) 0.088 Uiso 1 1 d D . . C3A C 0.1717(4) -0.0591(4) 0.69550(14) 0.0727(9) Uani 1 1 d D . . H3A1 H 0.116(2) 0.003(2) 0.6679(11) 0.109 Uiso 1 1 d D . . H3A2 H 0.161(3) -0.1717(13) 0.6874(12) 0.109 Uiso 1 1 d D . . H3A3 H 0.2726(13) -0.028(3) 0.6928(13) 0.109 Uiso 1 1 d D . . O1B O 0.19480(19) 0.0511(2) 0.98462(9) 0.0721(7) Uani 1 1 d . . . C1B C 0.1132(3) 0.1707(3) 0.99153(10) 0.0432(6) Uani 1 1 d . . . C2B C 0.0425(3) 0.2565(4) 0.93896(11) 0.0565(8) Uani 1 1 d D . . H2B1 H 0.059(2) 0.204(2) 0.9016(7) 0.085 Uiso 1 1 d D . . H2B2 H 0.082(2) 0.3642(16) 0.9373(9) 0.085 Uiso 1 1 d D . . H2B3 H -0.0611(12) 0.263(3) 0.9455(9) 0.085 Uiso 1 1 d D . . C3B C 0.0809(3) 0.2428(4) 1.05233(12) 0.0587(8) Uani 1 1 d D . . H3B1 H 0.1253(19) 0.173(2) 1.0809(9) 0.088 Uiso 1 1 d D . . H3B2 H -0.0223(11) 0.247(2) 1.0584(10) 0.088 Uiso 1 1 d D . . H3B3 H 0.121(2) 0.3503(15) 1.0561(11) 0.088 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1A 0.0705(14) 0.0679(14) 0.126(2) -0.0131(13) -0.0238(13) 0.0239(14) C1A 0.0423(15) 0.0375(14) 0.068(2) -0.0054(14) -0.0060(15) -0.0072(15) C2A 0.0608(18) 0.0622(17) 0.0538(17) -0.0006(15) 0.0055(16) 0.0057(18) C3A 0.090(2) 0.077(2) 0.0509(18) 0.0011(17) -0.0056(18) -0.021(2) O1B 0.0551(13) 0.0564(13) 0.1047(15) -0.0052(11) -0.0016(11) 0.0168(11) C1B 0.0318(13) 0.0414(14) 0.0563(17) 0.0010(13) 0.0016(13) -0.0062(14) C2B 0.0563(17) 0.0616(19) 0.0515(16) 0.0057(14) 0.0019(15) -0.0007(17) C3B 0.0562(17) 0.0662(19) 0.0538(17) 0.0014(15) -0.0018(15) -0.0034(16) _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 O1A C1A 1.208(3) . ? O1A H3A3 2.618(13) 6_557 ? O1A H3A2 2.71(2) 3_556 ? O1A C1A 3.458(3) 3_556 ? C1A C2A 1.478(4) . ? C1A C3A 1.485(4) . ? O1B C1B 1.210(3) . ? O1B C1B 3.300(3) 5_557 ? O1B C1B 3.491(3) 8_655 ? C1B C2B 1.485(3) . ? C1B C3B 1.486(3) . ? 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 C1A O1A H3A3 113.1(5) . 6_557 ? C1A O1A H3A2 167.3(5) . 3_556 ? H3A3 O1A H3A2 66.3(8) 6_557 3_556 ? C1A O1A C1A 151.59(17) . 3_556 ? H3A3 O1A C1A 93.5(5) 6_557 3_556 ? H3A2 O1A C1A 35.9(5) 3_556 3_556 ? O1A C1A C2A 120.8(3) . . ? O1A C1A C3A 122.2(3) . . ? C2A C1A C3A 117.0(2) . . ? C1B O1B C1B 84.82(15) . 5_557 ? C1B O1B C1B 167.51(18) . 8_655 ? C1B O1B C1B 85.90(6) 5_557 8_655 ? O1B C1B C2B 121.4(2) . . ? O1B C1B C3B 122.4(2) . . ? C2B C1B C3B 116.2(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.120 _refine_diff_density_min -0.129 _refine_diff_density_rms 0.030 #=END data_5KPBCA # CIF-file generated for Acetone-d6 5 K (unconstrained) # NEUTRON POWDER DATA _chemical_name_systematic ; Acetone-d6 ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum ' C3 D6 O' _chemical_formula_weight ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0000 0.0000 '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' C C 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,z x,1/2-y,1/2+z 1/2-x,-y,1/2+z -x,-y,-z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z 1/2+x,y,1/2-z _cell_length_a 9.1669(1) _cell_length_b 7.5323(1) _cell_length_c 21.2486(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1467.17(3) _cell_formula_units_Z 16 _cell_measurement_temperature 5 _cell_special_details ; Cell parameters included in refinement ; _exptl_crystal_density_diffrn 1.052 _diffrn_ambient_temperature 5 _diffrn_radiation_wavelength ; Time of flight ; _diffrn_radiation_type Neutron _diffrn_radiation_source ? _diffrn_radiation_monochromator ? _diffrn_measurement_device 'HRPD, ISIS' _diffrn_measurement_method ? _refine_special_details ; Anisotropic refinement of the D-atoms was found to be crucial for fitting. Two atoms (H2A2 and H3A3) adopt unreasonable adp's; the standard uncertainties in these parameters are rather high and the behaviour is not statistically significant. This feature might be owed to unmodelled hkl-dependent line-broadening. ; loop_ _atom_site_label _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv O1A Uiso 0.4993(4) -0.0669(4) 0.28376(14) 1.000 0.0040(9) C1A Uiso 0.3981(3) 0.0236(3) 0.26574(14) 1.000 0.0034(7) C2A Uiso 0.3028(3) 0.1280(4) 0.31064(16) 1.000 0.0106(8) C3A Uiso 0.3547(3) 0.0331(4) 0.19796(16) 1.000 0.0133(8) O1B Uiso 0.6890(4) 0.4607(4) 0.02165(15) 1.000 0.0076(8) C1B Uiso 0.6127(3) 0.3355(4) 0.00945(13) 1.000 0.0094(8) C2B Uiso 0.5305(3) 0.2398(5) 0.06158(15) 1.000 0.0085(8) C3B Uiso 0.5960(3) 0.2651(4) -0.05583(15) 1.000 0.0077(8) H2A1 Uani 0.3172(4) 0.0817(4) 0.35888(19) 1.000 0.03(2) H2A2 Uani 0.1903(4) 0.1212(5) 0.29879(17) 1.000 0.04(2) H2A3 Uani 0.3370(4) 0.2669(5) 0.30645(17) 1.000 0.03(2) H3A1 Uani 0.4328(4) -0.0433(4) 0.16929(16) 1.000 0.03(2) H3A2 Uani 0.3586(4) 0.1701(5) 0.18216(17) 1.000 0.03(2) H3A3 Uani 0.2447(5) -0.0226(5) 0.19109(16) 1.000 0.03(2) H2B1 Uani 0.5423(4) 0.3087(4) 0.10694(15) 1.000 0.03(2) H2B2 Uani 0.5844(5) 0.1086(5) 0.06632(17) 1.000 0.04(3) H2B3 Uani 0.4182(4) 0.2199(4) 0.04823(16) 1.000 0.03(2) H3B1 Uani 0.6390(4) 0.3592(5) -0.09029(18) 1.000 0.03(2) H3B2 Uani 0.4824(4) 0.2451(6) -0.06688(17) 1.000 0.04(2) H3B3 Uani 0.6559(4) 0.1364(5) -0.05946(17) 1.000 0.03(2) loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 H2A1 0.029(13) 0.020(9) 0.04(7) -0.007(16) 0.01(3) 0.011(7) H2A2 0.016(13) 0.040(9) 0.05(7) 0.02(2) -0.01(3) 0.017(7) H2A3 0.028(13) 0.019(9) 0.05(7) 0.003(16) -0.01(2) -0.002(7) H3A1 0.013(13) 0.045(11) 0.02(7) 0.006(16) -0.01(2) -0.008(7) H3A2 0.047(13) 0.020(6) 0.03(7) -0.004(16) 0.01(2) 0.006(7) H3A3 0.012(9) 0.047(9) 0.04(7) 0.00(2) -0.03(2) -0.009(10) H2B1 0.033(13) 0.027(9) 0.03(7) -0.011(16) 0.00(2) -0.017(7) H2B2 0.034(13) 0.026(9) 0.05(9) -0.021(16) 0.01(3) -0.009(10) H2B3 0.015(13) 0.041(9) 0.04(7) -0.01(2) -0.01(2) -0.001(7) H3B1 0.037(13) 0.036(9) 0.02(7) 0.001(16) -0.01(2) 0.004(7) H3B2 0.019(13) 0.061(11) 0.04(7) 0.00(2) 0.01(2) 0.002(7) H3B3 0.039(13) 0.016(9) 0.03(7) 0.006(16) 0.02(2) 0.015(7) # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All esds are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1A C1A 1.213(4) . . yes C1A C2A 1.514(4) . . no C1A C3A 1.496(4) . . no C2A H2A1 1.091(5) . . no C2A H2A2 1.063(5) . . no C2A H2A3 1.096(5) . . no C3A H3A1 1.102(5) . . no C3A H3A2 1.086(5) . . no C3A H3A3 1.102(5) . . no O1B C1B 1.202(4) . . yes C1B C2B 1.521(4) . . no C1B C3B 1.493(4) . . no C2B H2B1 1.100(5) . . no C2B H2B2 1.109(5) . . no C2B H2B3 1.078(5) . . no C3B H3B1 1.093(5) . . no C3B H3B2 1.078(5) . . no C3B H3B3 1.117(5) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1A C1A C2A 122.3(3) . . . yes O1A C1A C3A 122.3(3) . . . yes C2A C1A C3A 115.4(2) . . . no C1A C2A H2A1 110.9(3) . . . no C1A C2A H2A2 112.7(3) . . . no C1A C2A H2A3 106.2(3) . . . no H2A1 C2A H2A2 108.9(4) . . . no H2A1 C2A H2A3 110.3(4) . . . no H2A2 C2A H2A3 107.7(4) . . . no C1A C3A H3A1 109.5(3) . . . no C1A C3A H3A2 109.5(3) . . . no C1A C3A H3A3 110.7(3) . . . no H3A1 C3A H3A2 107.7(4) . . . no H3A1 C3A H3A3 108.8(4) . . . no H3A2 C3A H3A3 110.6(4) . . . no O1B C1B C2B 120.2(3) . . . yes O1B C1B C3B 122.6(3) . . . yes C2B C1B C3B 117.2(3) . . . no C1B C2B H2B1 111.5(3) . . . no C1B C2B H2B2 105.5(3) . . . no C1B C2B H2B3 110.3(3) . . . no H2B1 C2B H2B2 107.3(4) . . . no H2B1 C2B H2B3 113.0(4) . . . no H2B2 C2B H2B3 109.0(4) . . . no C1B C3B H3B1 110.8(3) . . . no C1B C3B H3B2 110.6(3) . . . no C1B C3B H3B3 108.8(3) . . . no H3B1 C3B H3B2 107.0(4) . . . no H3B1 C3B H3B3 109.8(4) . . . no H3B2 C3B H3B3 109.8(4) . . . no #=END data_110KPBCA # Pbca phase at 110K _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Me2CO _chemical_formula_sum 'C3 H6 O' _chemical_formula_weight 58.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 9.172(8) _cell_length_b 7.761(8) _cell_length_c 21.66(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1542(3) _cell_formula_units_Z 16 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 5 _cell_measurement_theta_max 10 _exptl_crystal_description cylinder _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.001 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 512 _exptl_absorpt_coefficient_mu 0.073 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method Omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% ? _diffrn_reflns_number 1693 _diffrn_reflns_av_R_equivalents 0.0557 _diffrn_reflns_av_sigmaI/netI 0.0983 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 1 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1349 _reflns_number_gt 690 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution 'From 150K structure' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'From 150K structure' _refine_ls_hydrogen_treatment 'As 150K structure' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0045(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1349 _refine_ls_number_parameters 110 _refine_ls_number_restraints 132 _refine_ls_R_factor_all 0.1416 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.1274 _refine_ls_wR_factor_gt 0.1012 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.923 _refine_ls_shift/su_max 0.023 _refine_ls_shift/su_mean 0.004 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1A O 0.0063(2) 0.0721(3) 0.77960(9) 0.0493(7) Uani 1 1 d . . . C1A C 0.1075(3) -0.0197(3) 0.76344(12) 0.0290(7) Uani 1 1 d . . . C2A C 0.1937(3) -0.1195(4) 0.80970(13) 0.0341(7) Uani 1 1 d D . . H2A1 H 0.179(2) -0.083(3) 0.8515(6) 0.051 Uiso 1 1 d D . . H2A2 H 0.2944(14) -0.107(3) 0.7985(10) 0.051 Uiso 1 1 d D . . H2A3 H 0.165(2) -0.2376(17) 0.8053(9) 0.051 Uiso 1 1 d D . . C3A C 0.1488(3) -0.0381(4) 0.69714(13) 0.0447(9) Uani 1 1 d D . . H3A1 H 0.086(2) 0.026(2) 0.6701(10) 0.067 Uiso 1 1 d D . . H3A2 H 0.144(2) -0.1585(14) 0.6871(12) 0.067 Uiso 1 1 d D . . H3A3 H 0.2475(13) 0.001(3) 0.6925(11) 0.067 Uiso 1 1 d D . . O1B O 0.19317(19) 0.0433(2) 0.98059(9) 0.0448(6) Uani 1 1 d . . . C1B C 0.1149(3) 0.1670(3) 0.99050(12) 0.0267(7) Uani 1 1 d . . . C2B C 0.0379(3) 0.2580(4) 0.93912(13) 0.0356(8) Uani 1 1 d D . . H2B1 H 0.049(2) 0.202(2) 0.8999(7) 0.053 Uiso 1 1 d D . . H2B2 H 0.079(2) 0.3718(18) 0.9370(9) 0.053 Uiso 1 1 d D . . H2B3 H -0.0645(13) 0.266(3) 0.9490(10) 0.053 Uiso 1 1 d D . . C3B C 0.0924(3) 0.2355(4) 1.05429(12) 0.0367(8) Uani 1 1 d D . . H3B1 H 0.131(2) 0.159(2) 1.0852(9) 0.055 Uiso 1 1 d D . . H3B2 H -0.0105(11) 0.250(3) 1.0613(10) 0.055 Uiso 1 1 d D . . H3B3 H 0.140(2) 0.3453(17) 1.0574(10) 0.055 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1A 0.0360(11) 0.0504(14) 0.0614(15) -0.0110(12) -0.0110(11) 0.0155(11) C1A 0.0245(14) 0.0273(15) 0.0353(17) -0.0040(13) -0.0048(13) -0.0074(14) C2A 0.0318(15) 0.0356(17) 0.0350(17) 0.0009(15) 0.0023(14) 0.0032(15) C3A 0.0438(18) 0.053(2) 0.0372(18) 0.0043(17) -0.0024(15) -0.0149(17) O1B 0.0417(12) 0.0369(12) 0.0557(14) -0.0051(11) -0.0043(10) 0.0172(11) C1B 0.0188(13) 0.0270(15) 0.0344(17) -0.0022(14) 0.0027(13) -0.0044(14) C2B 0.0333(16) 0.0404(19) 0.0332(17) 0.0001(15) -0.0017(14) 0.0030(15) C3B 0.0420(17) 0.0367(18) 0.0314(16) 0.0038(15) -0.0016(15) -0.0037(17) _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 O1A C1A 1.221(3) . ? O1A H3A3 2.511(12) 6_557 ? O1A H3A2 2.604(18) 3_556 ? O1A C1A 3.463(4) 3_556 ? C1A C2A 1.493(4) . ? C1A C3A 1.492(4) . ? O1B C1B 1.218(3) . ? O1B C1B 3.323(4) 5_557 ? O1B C1B 3.417(4) 8_655 ? C1B C2B 1.496(4) . ? C1B C3B 1.494(4) . ? 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 C1A O1A H3A3 131.3(5) . 6_557 ? C1A O1A H3A2 161.6(5) . 3_556 ? H3A3 O1A H3A2 67.0(8) 6_557 3_556 ? C1A O1A C1A 133.29(17) . 3_556 ? H3A3 O1A C1A 88.8(5) 6_557 3_556 ? H3A2 O1A C1A 35.0(5) 3_556 3_556 ? O1A C1A C2A 120.9(2) . . ? O1A C1A C3A 121.6(3) . . ? C2A C1A C3A 117.5(3) . . ? C1B O1B C1B 81.52(17) . 5_557 ? C1B O1B C1B 165.1(2) . 8_655 ? C1B O1B C1B 90.37(9) 5_557 8_655 ? O1B C1B C2B 121.3(2) . . ? O1B C1B C3B 121.6(2) . . ? C2B C1B C3B 117.0(2) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.170 _refine_diff_density_min -0.152 _refine_diff_density_rms 0.045 # End of Crystallographic Information File