# Electronic Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Simon Parsons' 'Duncan J. Francis' 'Russell D L Johnstone' 'Alistair Lennie' 'William G Marshall' 'Stephen A Moggach' 'Elna Pidcock' 'John E Warren' _publ_contact_author_name 'Simon Parsons' _publ_contact_author_email S.PARSONS@ED.AC.UK _publ_section_title ; High-Pressure Polymorphism in L-Serine Monohydrate: Identification of Driving Forces in High Pressure Phase Transitions and Implications for Pressure-Induced Protein Denaturation ; # Attachment 'all_structures.cif' data_x_serhyI_10kbar _database_code_depnum_ccdc_archive 'CCDC 692787' #Serine hydrate I at 1 GPa. #Pure single crystal Xray refinement. #Edinburgh dataset code = serhy1 _oxford_structure_analysis_title 'serhy1 in P2(1)2(1)2(1)' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 9.3344(6) _cell_length_b 11.822(3) _cell_length_c 4.7387(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 522.92(14) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,-y+1/2,-z -x,y+1/2,-z+1/2 -x+1/2,-y,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0010 0.0010 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0020 0.0010 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0040 0.0030 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C3 H9 N1 O4 # Dc = 1.56 Fooo = 264.00 Mu = 1.45 M = 123.11 # Found Formula = C3 H9 N1 O4 # Dc = 1.56 FOOO = 264.00 Mu = 1.45 M = 123.11 _chemical_formula_sum 'C3 H9 N1 O4' _chemical_formula_moiety 'C3 H9 N1 O4' _chemical_compound_source ? _chemical_formula_weight 123.11 _cell_measurement_reflns_used 604 _cell_measurement_theta_min 3 _cell_measurement_theta_max 16 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 264 _exptl_absorpt_coefficient_mu 0.145 # Sheldrick geometric approximatio 0.97 0.99 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.26 _exptl_absorpt_correction_T_max 0.99 _diffrn_measurement_device_type 'Bruker SMART' _diffrn_radiation_monochromator silicon _diffrn_radiation_type ' synchrotron ' _diffrn_radiation_wavelength 0.48650 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_ambient_pressure 1000000 _diffrn_reflns_number 2795 _reflns_number_total 306 _diffrn_reflns_av_R_equivalents 0.0988 # Number of reflections with Friedels Law is 306 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 531 _diffrn_reflns_reduction_process ; Merged with SORTAV R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 ; _diffrn_reflns_theta_min 2.988 _diffrn_reflns_theta_max 17.662 _diffrn_measured_fraction_theta_max 0.473 _diffrn_reflns_theta_full 14.129 _diffrn_measured_fraction_theta_full 0.495 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 5 _reflns_limit_h_min 0 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 6 _reflns_limit_l_min 0 _reflns_limit_l_max 5 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.19 _refine_diff_density_max 0.18 _refine_ls_number_reflns 299 _refine_ls_number_restraints 85 _refine_ls_number_parameters 100 #_refine_ls_R_factor_ref 0.0531 _refine_ls_wR_factor_ref 0.0427 _refine_ls_goodness_of_fit_ref 1.0694 #_reflns_number_all 299 _refine_ls_R_factor_all 0.0531 _refine_ls_wR_factor_all 0.0427 # No actual I/u(I) cutoff was used for refinement. The # threshold below is used for "_gt" information ONLY: _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 256 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_gt 0.0411 _refine_ls_shift/su_max 0.000145 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration unk _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment refxyz # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ; Method= SQRT(W) = 1/(Data with the key SIGMA(/FO/) in list 6) ; _publ_section_exptl_refinement ; Checkcif Output: 199_ALERT_1_A Check the Reported _cell_measurement_temperature 293 K 200_ALERT_1_A Check the Reported _diffrn_ambient_temperature . 293 K Data were collected at 293K 022_ALERT_3_A Ratio Unique / Expected Reflections too Low .... 0.47 027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 14.13 Deg. 029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.50 089_ALERT_3_A Poor Data / Parameter Ratio (Zmax .LT. 18) ..... 2.99 911_ALERT_3_B # Missing FCF Refl Between THmin & STh/l= 298 910_ALERT_3_C # Missing FCF Reflections Below TH(Min) ........ 3 912_ALERT_3_C # Missing FCF Reflections Above STH/L=0.6 ...... 40 340_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 5 The high pressure cell causes shading of a significant proportion of the sphere of reflections. This means that the completeness is reduced. 042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? The one given is chemically more meaningful 250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.14 This is probably due to the lack of information in one direction which occurs as a result of the Merrill-Bassett diamond-anvil cell shading a significant region of reciprocal space. The effect of this shading is often to cause a smearing out of electron density in one particular direction. 731_ALERT_1_C Bond Calc 0.80(4), Rep 0.807(17) ...... 2.35 su-Rat O3 -H7 1.555 1.555 731_ALERT_1_C Bond Calc 0.81(5), Rep 0.815(17) ...... 2.94 su-Rat O4 -H8 1.555 1.555 731_ALERT_1_C Bond Calc 0.82(4), Rep 0.818(17) ...... 2.35 su-Rat O4 -H9 1.555 1.555 This alert is due to the fact that PLATON calculates esds using only the variances whereas CRYSTALS uses the full variance/covariance matrix. ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens C1 C 0.5373(2) 0.2325(4) 0.3042(5) 0.0264 1.0000 Uani D U . . . . C2 C 0.3998(3) 0.2490(4) 0.1372(5) 0.0303 1.0000 Uani D U . . . . C3 C 0.3438(3) 0.3677(5) 0.1700(6) 0.0381 1.0000 Uani D U . . . . N1 N 0.2920(2) 0.1642(5) 0.2190(5) 0.0333 1.0000 Uani D U . . . . O1 O 0.54452(19) 0.1526(6) 0.4736(5) 0.0456 1.0000 Uani D U . . . . O2 O 0.63545(16) 0.3031(4) 0.2597(4) 0.0310 1.0000 Uani D U . . . . O3 O 0.32879(18) 0.3961(5) 0.4599(4) 0.0400 1.0000 Uani D U . . . . O4 O 0.0795(2) -0.0044(5) 0.3484(5) 0.0385 1.0000 Uani D . . . . . H1 H 0.4192(19) 0.237(2) -0.061(3) 0.0385 1.0000 Uiso D . . . . . H2 H 0.413(2) 0.4188(19) 0.083(4) 0.0456 1.0000 Uiso D . . . . . H3 H 0.2519(18) 0.374(2) 0.071(4) 0.0456 1.0000 Uiso D . . . . . H4 H 0.266(2) 0.178(2) 0.393(4) 0.0517 1.0000 Uiso D . . . . . H5 H 0.217(2) 0.170(3) 0.093(4) 0.0517 1.0000 Uiso D . . . . . H6 H 0.335(2) 0.0967(17) 0.205(6) 0.0517 1.0000 Uiso D . . . . . H7 H 0.260(4) 0.362(5) 0.515(8) 0.0607 1.0000 Uiso D . . . . . H8 H 0.042(4) -0.039(6) 0.220(9) 0.0588 1.0000 Uiso D . . . . . H9 H 0.007(3) 0.020(6) 0.424(8) 0.0588 1.0000 Uiso 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 0.0215(11) 0.037(6) 0.0205(14) 0.000(3) 0.0049(10) -0.0022(17) C2 0.0205(11) 0.052(6) 0.0186(11) 0.000(2) 0.0022(9) -0.0011(18) C3 0.0263(13) 0.052(6) 0.0357(13) -0.006(3) -0.0015(12) 0.000(2) N1 0.0207(10) 0.051(7) 0.0280(11) -0.002(2) -0.0008(9) -0.0028(19) O1 0.0282(10) 0.058(7) 0.0511(15) 0.025(3) -0.0055(10) -0.0059(19) O2 0.0247(8) 0.041(6) 0.0275(9) 0.0009(16) 0.0024(8) -0.0066(15) O3 0.0280(10) 0.054(8) 0.0382(10) -0.009(2) 0.0078(8) -0.009(2) O4 0.0389(12) 0.033(11) 0.0433(13) -0.007(2) -0.0056(9) 0.006(2) _refine_ls_extinction_method None _oxford_refine_ls_scale 2.26(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 . C2 . 1.521(3) yes C1 . O1 . 1.242(6) yes C1 . O2 . 1.257(5) yes C2 . C3 . 1.505(7) yes C2 . N1 . 1.472(5) yes C2 . H1 . 0.968(16) no C3 . O3 . 1.422(4) yes C3 . H2 . 0.976(16) no C3 . H3 . 0.980(15) no N1 . H4 . 0.874(16) no N1 . H5 . 0.923(16) no N1 . H6 . 0.894(17) no O3 . H7 . 0.807(17) no O4 . H8 . 0.815(17) no O4 . H9 . 0.818(17) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 . C1 . O1 . 118.7(2) yes C2 . C1 . O2 . 116.3(2) yes O1 . C1 . O2 . 125.0(2) yes C1 . C2 . C3 . 111.0(3) yes C1 . C2 . N1 . 110.6(2) yes C3 . C2 . N1 . 111.7(2) yes C1 . C2 . H1 . 109.1(11) no C3 . C2 . H1 . 107.8(14) no N1 . C2 . H1 . 106.3(13) no C2 . C3 . O3 . 110.8(3) yes C2 . C3 . H2 . 107.8(13) no O3 . C3 . H2 . 109.0(13) no C2 . C3 . H3 . 109.1(15) no O3 . C3 . H3 . 110.9(11) no H2 . C3 . H3 . 109.2(14) no C2 . N1 . H4 . 108.2(15) no C2 . N1 . H5 . 107.5(14) no H4 . N1 . H5 . 112.7(14) no C2 . N1 . H6 . 106.5(13) no H4 . N1 . H6 . 111.1(15) no H5 . N1 . H6 . 110.6(15) no C3 . O3 . H7 . 106(3) no H8 . O4 . H9 . 99(4) no _chemical_name_common 'Serine Monohydrate' _exptl_crystal_recrystallization_method 'From H2O/EtOH' data_x_serhyI_26kbar.cif _database_code_depnum_ccdc_archive 'CCDC 692788' #Serine hydrate I at 2.6 GPa. #Pure single crystal Xray refinement. #Edinburgh dataset code = serhy2 _oxford_structure_analysis_title 'serhy2 in P2(1)2(1)2(1)' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 9.3563(6) _cell_length_b 11.443(2) _cell_length_c 4.6166(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 494.28(10) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,-y+1/2,-z -x,y+1/2,-z+1/2 -x+1/2,-y,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0010 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0020 0.0010 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0040 0.0030 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C3 H9 N1 O4 # Dc = 1.65 Fooo = 264.00 Mu = 1.54 M = 123.11 # Found Formula = C3 H9 N1 O4 # Dc = 1.65 FOOO = 264.00 Mu = 1.54 M = 123.11 _chemical_formula_sum 'C3 H9 N1 O4' _chemical_formula_moiety 'C3 H9 N1 O4' _chemical_compound_source ? _chemical_formula_weight 123.11 _cell_measurement_reflns_used 832 _cell_measurement_theta_min 3 _cell_measurement_theta_max 17 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.654 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 264 _exptl_absorpt_coefficient_mu 0.154 # Sheldrick geometric approximatio 0.97 0.98 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.34 _exptl_absorpt_correction_T_max 0.98 _diffrn_measurement_device_type 'Bruker SMART' _diffrn_radiation_monochromator silicon _diffrn_radiation_type ' synchrotron ' _diffrn_radiation_wavelength 0.48650 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_ambient_pressure 2600000 _diffrn_reflns_number 2930 _reflns_number_total 311 _diffrn_reflns_av_R_equivalents 0.0898 # Number of reflections with Friedels Law is 311 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 506 _diffrn_reflns_reduction_process ; Merged with SORTAV R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 ; _diffrn_reflns_theta_min 1.925 _diffrn_reflns_theta_max 17.714 _diffrn_measured_fraction_theta_max 0.498 _diffrn_reflns_theta_full 13.463 _diffrn_measured_fraction_theta_full 0.535 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 5 _reflns_limit_h_min 0 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 6 _reflns_limit_l_min 0 _reflns_limit_l_max 5 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.19 _refine_diff_density_max 0.15 _refine_ls_number_reflns 307 _refine_ls_number_restraints 85 _refine_ls_number_parameters 100 #_refine_ls_R_factor_ref 0.0517 _refine_ls_wR_factor_ref 0.0497 _refine_ls_goodness_of_fit_ref 0.9923 #_reflns_number_all 307 _refine_ls_R_factor_all 0.0517 _refine_ls_wR_factor_all 0.0497 # No actual I/u(I) cutoff was used for refinement. The # threshold below is used for "_gt" information ONLY: _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 264 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_gt 0.0478 _refine_ls_shift/su_max 0.000159 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration unk _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment refxyz # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ; Method= SQRT(W) = 1/(Data with the key SIGMA(/FO/) in list 6) ; _publ_section_exptl_refinement ; Checkcif Output: 022_ALERT_3_A Ratio Unique / Expected Reflections too Low .... 0.50 027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 13.46 Deg. 029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.54 089_ALERT_3_A Poor Data / Parameter Ratio (Zmax .LT. 18) ..... 3.07 911_ALERT_3_B # Missing FCF Refl Between THmin & STh/l= 271 912_ALERT_3_C # Missing FCF Reflections Above STH/L=0.6 ...... 43 340_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 5 The high pressure cell causes shading of a significant proportion of the sphere of reflections. This means that the completeness is reduced. 199_ALERT_1_A Check the Reported _cell_measurement_temperature 293 K 200_ALERT_1_A Check the Reported _diffrn_ambient_temperature . 293 K Data were collected at 293K 042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? The one given is chemically more meaningful 250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.36 This is probably due to the lack of information in one direction which occurs as a result of the Merrill-Bassett diamond-anvil cell shading a significant region of reciprocal space. The effect of this shading is often to cause a smearing out of electron density in one particular direction. 731_ALERT_1_C Bond Calc 0.82(5), Rep 0.825(17) ...... 2.94 su-Rat O4 -H8 1.555 1.555 731_ALERT_1_C Bond Calc 0.83(4), Rep 0.828(17) ...... 2.35 su-Rat O4 -H9 1.555 1.555 This alert is due to the fact that PLATON calculates esds using only the variances whereas CRYSTALS uses the full variance/covariance matrix. ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens C1 C 0.5405(2) 0.2349(4) 0.2945(5) 0.0269 1.0000 Uani D U . . . . C2 C 0.3989(2) 0.2494(4) 0.1331(5) 0.0254 1.0000 Uani D U . . . . C3 C 0.3404(2) 0.3697(5) 0.1741(5) 0.0289 1.0000 Uani D U . . . . N1 N 0.29608(17) 0.1593(5) 0.2293(5) 0.0269 1.0000 Uani D U . . . . O1 O 0.55313(17) 0.1505(5) 0.4624(5) 0.0456 1.0000 Uani D U . . . . O2 O 0.63350(16) 0.3105(4) 0.2482(4) 0.0354 1.0000 Uani D U . . . . O3 O 0.33047(16) 0.3969(4) 0.4730(4) 0.0318 1.0000 Uani D U . . . . O4 O 0.07893(19) -0.0039(5) 0.3349(5) 0.0434 1.0000 Uani D . . . . . H1 H 0.4171(18) 0.237(2) -0.074(3) 0.0303 1.0000 Uiso D . . . . . H2 H 0.400(2) 0.4264(19) 0.082(4) 0.0340 1.0000 Uiso D . . . . . H3 H 0.2475(17) 0.372(2) 0.086(4) 0.0340 1.0000 Uiso D . . . . . H4 H 0.269(2) 0.172(2) 0.415(4) 0.0389 1.0000 Uiso D . . . . . H5 H 0.2215(19) 0.162(2) 0.111(4) 0.0389 1.0000 Uiso D . . . . . H6 H 0.337(2) 0.0899(17) 0.212(5) 0.0389 1.0000 Uiso D . . . . . H7 H 0.247(2) 0.384(6) 0.516(6) 0.0444 1.0000 Uiso D . . . . . H8 H 0.042(4) -0.040(7) 0.200(9) 0.0710 1.0000 Uiso D . . . . . H9 H 0.009(3) 0.029(5) 0.409(8) 0.0710 1.0000 Uiso 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 0.0175(9) 0.046(5) 0.0170(11) 0.000(2) 0.0031(8) 0.0007(14) C2 0.0177(9) 0.041(5) 0.0181(10) 0.001(2) 0.0010(8) -0.0002(16) C3 0.0214(10) 0.038(5) 0.0277(11) 0.003(2) -0.0001(9) -0.0022(19) N1 0.0169(8) 0.037(6) 0.0274(11) -0.003(2) -0.0012(7) -0.0019(14) O1 0.0255(7) 0.063(6) 0.0482(13) 0.023(2) -0.0061(8) -0.0027(17) O2 0.0214(7) 0.059(6) 0.0263(9) 0.0026(17) 0.0034(7) -0.0078(13) O3 0.0217(8) 0.040(6) 0.0339(9) -0.0059(17) 0.0072(7) -0.0027(16) O4 0.0304(9) 0.063(9) 0.0370(12) -0.004(2) -0.0031(8) 0.0024(15) _refine_ls_extinction_method None _oxford_refine_ls_scale 2.33(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 . C2 . 1.529(3) yes C1 . O1 . 1.244(5) yes C1 . O2 . 1.245(4) yes C2 . C3 . 1.493(6) yes C2 . N1 . 1.479(5) yes C2 . H1 . 0.982(15) no C3 . O3 . 1.417(3) yes C3 . H2 . 0.955(17) no C3 . H3 . 0.959(15) no N1 . H4 . 0.904(16) no N1 . H5 . 0.886(16) no N1 . H6 . 0.885(17) no O3 . H7 . 0.819(16) no O4 . H8 . 0.825(17) no O4 . H9 . 0.828(17) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 . C1 . O1 . 118.0(2) yes C2 . C1 . O2 . 116.5(2) yes O1 . C1 . O2 . 125.4(2) yes C1 . C2 . C3 . 110.9(2) yes C1 . C2 . N1 . 110.0(2) yes C3 . C2 . N1 . 111.5(2) yes C1 . C2 . H1 . 107.9(10) no C3 . C2 . H1 . 109.0(13) no N1 . C2 . H1 . 107.5(12) no C2 . C3 . O3 . 110.5(3) yes C2 . C3 . H2 . 110.8(13) no O3 . C3 . H2 . 108.9(12) no C2 . C3 . H3 . 108.0(14) no O3 . C3 . H3 . 110.2(11) no H2 . C3 . H3 . 108.5(14) no C2 . N1 . H4 . 110.6(14) no C2 . N1 . H5 . 107.7(14) no H4 . N1 . H5 . 111.2(14) no C2 . N1 . H6 . 108.4(13) no H4 . N1 . H6 . 110.5(15) no H5 . N1 . H6 . 108.3(15) no C3 . O3 . H7 . 105(2) no H8 . O4 . H9 . 102(4) no _chemical_name_common 'Serine Monohydrate' _exptl_crystal_recrystallization_method 'From H2O/EtOH' data_x_serhyI_37kbar _database_code_depnum_ccdc_archive 'CCDC 692789' #Parameters quoted are from a joint X-N refinement of phase I #Serine hydrate I at 3.7 GPa. #X-N refinement. This cif contains data used to model the Xray data set. #Edinburgh dataset code = serhy3 #Notes on this cif: #The structural data comes from a joint X-N refinement (see text in paper) #The majority of this cif was generated with CRYSTALS. #The Topas cif was processed using Platon so that x's and u's conform to the #'rule of 19'. The x's, u's and geometrical parameters were then pasted into #this cif. R-factors: _refine_ls_wR_factor_ref corresponds to the Topas Rwp. #Other R-factors were calculated by importing the final model into crystals #and doing a structure factor calculation. _oxford_structure_analysis_title 'serhy3 in P2(1)2(1)2(1)' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 9.3706(6) _cell_length_b 11.204(2) _cell_length_c 4.5341(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 476.02(10) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,-y+1/2,-z -x,y+1/2,-z+1/2 -x+1/2,-y,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0010 0.0010 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0020 0.0010 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0040 0.0030 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C3 H9 N1 O4 # Dc = 1.72 Fooo = 264.00 Mu = 1.59 M = 123.11 # Found Formula = C3 H9 N1 O4 # Dc = 1.72 FOOO = 264.00 Mu = 1.59 M = 123.11 _chemical_formula_sum 'C3 H9 N1 O4' _chemical_formula_moiety 'C3 H9 N1 O4' _chemical_compound_source ? _chemical_formula_weight 123.11 _cell_measurement_reflns_used 597 _cell_measurement_theta_min 3 _cell_measurement_theta_max 17 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.718 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 264 _exptl_absorpt_coefficient_mu 0.159 # Sheldrick geometric approximatio 0.97 0.98 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.06 _exptl_absorpt_correction_T_max 0.98 _diffrn_measurement_device_type 'Bruker SMART' _diffrn_radiation_monochromator silicon _diffrn_radiation_type ' Synchrotron ' _diffrn_radiation_wavelength 0.48650 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_structure_solution 'Frey et al' _computing_structure_refinement 'Crystals and Topas' _computing_publication_material 'Topas, Crystals and Platon' _computing_molecular_graphics Diamond _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_ambient_pressure 3700000 _diffrn_reflns_number 2574 _reflns_number_total 288 _diffrn_reflns_av_R_equivalents 0.1235 # Number of reflections with Friedels Law is 288 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 495 _diffrn_reflns_reduction_process ; Merged with SORTAV R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 ; _diffrn_reflns_theta_min 2.976 _diffrn_reflns_theta_max 17.807 _diffrn_measured_fraction_theta_max 0.470 _diffrn_reflns_theta_full 13.890 _diffrn_measured_fraction_theta_full 0.481 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 5 _reflns_limit_h_min 0 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 6 _reflns_limit_l_min 0 _reflns_limit_l_max 5 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'from Frey et al' _refine_diff_density_min -0.19 _refine_diff_density_max 0.20 _refine_ls_number_reflns 275 _refine_ls_number_restraints 2 _refine_ls_number_parameters 131 #131 parameters in joint x-n refinement _refine_ls_wR_factor_ref 0.07813 _refine_ls_goodness_of_fit_ref 1.559 #_reflns_number_all 275 _refine_ls_R_factor_all 0.0546 _refine_ls_wR_factor_all 0.0781 # No actual I/u(I) cutoff was used for refinement. The # threshold below is used for "_gt" information ONLY: _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 233 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_gt 0.0947 _refine_ls_shift/su_max 0.000 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration syn _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment refall # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _publ_section_exptl_refinement ; Checkcif output: 022_ALERT_3_A Ratio Unique / Expected Reflections too Low .... 0.47 027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 13.89 Deg. 029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.48 089_ALERT_3_A Poor Data / Parameter Ratio (Zmax .LT. 18) ..... 2.10 The high pressure cell causes shading of a significant proportion of the sphere of reflections. This means that the completeness is reduced. 340_ALERT_3_B Low Bond Precision on C-C Bonds (x 1000) Ang ... 11 The Platon su calculation does not take the variance covarience off diagonal terms into account. The C-C sus are actually much better than this: see text. 020_ALERT_3_C The value of Rint is greater than 0.10 ......... 0.12 Mostly due to weak data at high resolution. 042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? The one given is chemically more meaningful 125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? No action 245_ALERT_2_C U(iso) H1 Smaller than U(eq) C2 by ... 0.02 AngSq 245_ALERT_2_C U(iso) H2 Smaller than U(eq) C3 by ... 0.02 AngSq 245_ALERT_2_C U(iso) H3 Smaller than U(eq) C3 by ... 0.02 AngSq 245_ALERT_2_C U(iso) H4 Smaller than U(eq) N1 by ... 0.02 AngSq 245_ALERT_2_C U(iso) H5 Smaller than U(eq) N1 by ... 0.02 AngSq 245_ALERT_2_C U(iso) H6 Smaller than U(eq) N1 by ... 0.02 AngSq 245_ALERT_2_C U(iso) H7 Smaller than U(eq) O3 by ... 0.03 AngSq 245_ALERT_2_C U(iso) H8 Smaller than U(eq) O4 by ... 0.03 AngSq 245_ALERT_2_C U(iso) H9 Smaller than U(eq) O4 by ... 0.03 AngSq A common overall istropic parameter was refined for the H-atoms. B(H, overall)= 0.44564 +- 0.29752 199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K 200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K OK 791_ALERT_1_G Confirm the Absolute Configuration of C2 = . S 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 2 OK ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint loop_ _atom_site_label _atom_site_type_symbol _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 _atom_site_calc_flag _atom_site_refinement_flags O1 O Uani 0.5579(7) 0.1506(8) 0.4547(18) 1.000 0.039(4) . . O2 O Uani 0.6311(8) 0.3147(8) 0.2401(18) 1.000 0.024(3) . . O3 O Uani 0.332(2) 0.396(2) 0.482(5) 1.000 0.032(3) . . N1 N Uani 0.2990(9) 0.1544(10) 0.233(2) 1.000 0.025(4) . . C1 C Uani 0.5409(2) 0.2368(3) 0.2882(5) 1.000 0.023(4) . . C2 C Uani 0.3989(3) 0.2486(7) 0.1300(10) 1.000 0.022(4) . . C3 C Uani 0.3379(11) 0.3727(15) 0.177(3) 1.000 0.025(5) . . O4 O Uani 0.0786(2) -0.0017(6) 0.3261(6) 1.000 0.033(3) . . H1 H Uiso 0.413(2) 0.2355(16) -0.075(4) 1.000 0.006(4) . . H2 H Uiso 0.3977(19) 0.429(2) 0.083(5) 1.000 0.006(4) . . H3 H Uiso 0.245(3) 0.376(2) 0.095(5) 1.000 0.006(4) . . H4 H Uiso 0.2718(18) 0.1719(17) 0.412(4) 1.000 0.006(4) . . H5 H Uiso 0.226(2) 0.1527(17) 0.115(4) 1.000 0.006(4) . . H6 H Uiso 0.343(2) 0.0862(16) 0.231(4) 1.000 0.006(4) . . H7 H Uiso 0.245(4) 0.383(3) 0.524(7) 1.000 0.006(4) . . H8 H Uiso 0.041(2) -0.048(2) 0.197(4) 1.000 0.006(4) . . H9 H Uiso 0.008(2) 0.0374(19) 0.399(4) 1.000 0.006(4) . . 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 O1 0.0224(10) 0.041(11) 0.0525(17) 0.025(3) -0.0061(10) -0.003(2) O2 0.0223(9) 0.029(9) 0.0217(11) 0.0032(18) 0.0026(8) -0.0038(17) O3 0.0194(10) 0.048(9) 0.0299(12) -0.006(2) 0.0043(8) -0.0021(19) N1 0.0155(9) 0.034(11) 0.0242(13) -0.003(2) -0.0026(9) 0.001(2) C1 0.0142(13) 0.038(12) 0.0158(14) 0.000(3) 0.0038(11) 0.002(2) C2 0.0194(13) 0.028(13) 0.0185(14) 0.001(3) 0.0011(10) 0.000(3) C3 0.0206(14) 0.031(14) 0.0230(15) -0.001(3) -0.0003(11) 0.004(3) O4 0.0258(10) 0.042(10) 0.0314(12) -0.002(2) -0.0019(9) 0.0004(17) 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 O1 C1 1.236(9) . . yes O2 C1 1.234(9) . . yes O3 C3 1.41(3) . . yes O3 H7 0.85(4) . . no O4 H9 0.86(2) . . no O4 H8 0.86(2) . . no N1 C2 1.486(12) . . yes N1 H5 0.87(2) . . no N1 H4 0.87(2) . . no N1 H6 0.87(2) . . no C1 C2 1.517(4) . . no C2 C3 1.518(18) . . no C2 H1 0.950(19) . . no C3 H3 0.95(3) . . no C3 H2 0.95(3) . . 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 C3 O3 H7 103(3) . . . no H8 O4 H9 104.7(18) . . . no C2 N1 H5 108.6(15) . . . no C2 N1 H6 108.8(14) . . . no H4 N1 H5 110.3(19) . . . no H4 N1 H6 110(2) . . . no H5 N1 H6 110(2) . . . no C2 N1 H4 108.5(15) . . . no O1 C1 O2 124.9(5) . . . yes O2 C1 C2 117.1(5) . . . yes O1 C1 C2 118.0(5) . . . yes N1 C2 C1 110.0(5) . . . yes N1 C2 C3 111.7(6) . . . yes C1 C2 C3 110.1(6) . . . no O3 C3 C2 108.8(13) . . . yes N1 C2 H1 106.6(13) . . . no C3 C2 H1 109.3(13) . . . no C1 C2 H1 109.1(12) . . . no O3 C3 H2 110(2) . . . no O3 C3 H3 110.0(19) . . . no C2 C3 H3 109.1(19) . . . no H2 C3 H3 110(2) . . . no C2 C3 H2 108.9(16) . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 N1 5.1(8) . . . . no O1 C1 C2 C3 128.6(8) . . . . no O2 C1 C2 N1 -174.9(6) . . . . no O2 C1 C2 C3 -51.4(8) . . . . no N1 C2 C3 O3 68.6(12) . . . . no C1 C2 C3 O3 -53.9(12) . . . . no _chemical_name_common 'Serine Monohydrate' _exptl_crystal_recrystallization_method 'From H2O/EtOH' data_n_serhyI_38kbar.cif _database_code_depnum_ccdc_archive 'CCDC 692790' #X-N refinement of phase 1 at 3.8 GPa. #Serine hydrate I at 3.8 GPa. #X-N refinement. This cif contains strutural parameters used to #model the neutron powder data set. #ISIS data set code: PRL57149_54_40TNS_ASCII_TOF _chemical_name_systematic ; perdeuterated L-serine hydrate ; _chemical_name_common 'Serine hydrate' _chemical_formula_moiety 'C3 D7 N O3, D2 O1' _chemical_formula_structural ? _chemical_formula_sum 'C3 D9 N O4' _chemical_formula_weight 132.13 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 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' N N 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 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 P212121 _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 _cell_length_a 9.3701(14) _cell_length_b 11.1831(10) _cell_length_c 4.52938(59) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 474.62(10) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_measurement_temperature 298 _cell_measurement_pressure 3805000 #3.805(12) GPa _cell_measurement_reflns_used 1119 _cell_formula_units_Z 4 _cell_special_details ; Cell parameters included in refinement ; _exptl_crystal_density_diffrn 1.849 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 ? _pd_spec_mounting 'TiZr Capsule' _pd_spec_mount_mode transmission _pd_char_particle_morphology Block _pd_char_colour Colourless _chemical_absolute_configuration rm _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ; Calculated using custom ISIS software. ; _pd_instr_location 'ISIS, Rutherford Appleton Laboratory' _diffrn_ambient_temperature 298 _diffrn_source 'Pulsed neutron source' _diffrn_source_target ? _diffrn_radiation_type Neutron _diffrn_measurement_device_type 'HiPr/PEARL, ISIS' _diffrn_radiation_monochromator ? _diffrn_detector 'ZnS scintillator' _diffrn_detector_type custom _pd_meas_scan_method Time-of-flight _pd_meas_special_details ; Time of flight method using a pulsed neutron source ; _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_number 1119 # The following three items are used for time-of-flight measurements only. _pd_instr_dist_src/spec 12600 _pd_instr_dist_spec/detc 600 _pd_meas_2theta_fixed 90 _pd_proc_ls_profile_function ; Voigt function convoluted with a back-to-back double exponential. ; _pd_proc_ls_background_function 'Chebychev polynomial' _pd_proc_ls_pref_orient_corr ; Modelling of preferred orientation was found to be unnecessary. ; _pd_proc_ls_prof_R_factor 1.956 _pd_proc_ls_prof_wR_factor 1.565 _pd_proc_ls_prof_R_expected 1.395 _refine_ls_goodness_of_fit_all 1.121 _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 131 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_diff_density_max ? _refine_diff_density_min ? _refine_ls_shift/su_max <0.001 _pd_proc_info_excluded_regions ; excluded short TOF region above ; _pd_proc_info_data_reduction ; Custom ISIS software ; _refine_special_details ; Refinement was carried out against neutron and X-ray data simultaneously. The X-ray data had been collected using synchrotron radiation, and the pressure (ruby fluorescence) was 3.7 GPa. wR2 = 7.813 and S = 1.559 for pure 1/sigma^2 weights. Checkcif output: 023_ALERT_3_A Resolution (too) Low [sin(th)/Lambda < 0.6]..... 0.00 Deg. 027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 0.00 Deg. 029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.00 037_ALERT_1_A _diffrn_reflns_theta_full .......... Not Given . ? 038_ALERT_1_A _diffrn_measured_fraction_theta_max Not Given . ? 039_ALERT_1_A _diffrn_measured_fraction_theta_full Not Given . ? The resolution range was 0.64 to 4.14 Ang. 050_ALERT_1_A Absorption Coefficient mu Missing .............. ? TOF data - the absorption coefficient is variable. 095_ALERT_1_A No Residual Density Maximum Given .............. ? 096_ALERT_1_A No Residual Density Minimum Given .............. ? These data are not yet output by TOPAS. 201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 8 210_ALERT_3_B No Anisotropic ADP's Found in CIF .............. ? Powder data: see text of paper. 340_ALERT_3_B Low Bond Precision on C-C Bonds (x 1000) Ang ... 11 This is quite good for a high pressure neutron powder refinement! 040_ALERT_1_C No H-atoms in this Carbon Containing Compound .. ? 720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 9 The sample was deuterated. ; 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 0.54093(22) 0.23680(32) 0.28819(46) 1 0.802(84) C2 C 0 0.39887(35) 0.24861(65) 0.13003(98) 1 0.802(84) C3 C 0 0.3379(11) 0.3727(15) 0.1768(31) 1 0.802(84) N1 N 0 0.29903(93) 0.15440(99) 0.2333(20) 1 0.802(84) O1 O 0 0.55791(74) 0.15057(80) 0.4547(18) 1 0.802(84) O2 O 0 0.63113(75) 0.31465(80) 0.2401(18) 1 0.802(84) O3 O 0 0.3317(21) 0.3959(22) 0.4816(48) 1 0.802(84) H1 D 0 0.4140(21) 0.2341(14) -0.0963(38) 1 0.96(10) H2 D 0 0.4040(19) 0.4354(22) 0.0730(51) 1 0.96(10) H3 D 0 0.2353(24) 0.3764(20) 0.0856(48) 1 0.96(10) H4 D 0 0.2687(18) 0.1737(16) 0.4326(38) 1 0.96(10) H5 D 0 0.2174(19) 0.1523(18) 0.1014(39) 1 0.96(10) H6 D 0 0.3484(18) 0.0781(15) 0.2307(38) 1 0.96(10) H7 D 0 0.2350(39) 0.3812(33) 0.5295(78) 1 0.96(10) O4 O 0 0.07859(22) -0.00173(62) 0.32605(60) 1 0.802(84) H8 D 0 0.0367(21) -0.0534(19) 0.1818(40) 1 0.96(10) H9 D 0 0.0003(17) 0.0421(20) 0.4078(42) 1 0.96(10) data_x_serhyI_45kbar.cif _database_code_depnum_ccdc_archive 'CCDC 692791' #Serine hydrate I at 4.5 GPa. #Pure single crystal Xray refinement. #Edinburgh dataset code = serhy4 _oxford_structure_analysis_title 'serhy4 in P2(1)2(1)2(1)' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 9.3728(5) _cell_length_b 11.0359(17) _cell_length_c 4.4782(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 463.21(8) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,-y+1/2,-z -x,y+1/2,-z+1/2 -x+1/2,-y,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0010 0.0010 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0020 0.0010 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0040 0.0030 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C3 H9 N1 O4 # Dc = 1.77 Fooo = 264.00 Mu = 1.64 M = 123.11 # Found Formula = C3 H9 N1 O4 # Dc = 1.77 FOOO = 264.00 Mu = 1.64 M = 123.11 _chemical_formula_sum 'C3 H9 N1 O4' _chemical_formula_moiety 'C3 H9 N1 O4' _chemical_compound_source ? _chemical_formula_weight 123.11 _cell_measurement_reflns_used 730 _cell_measurement_theta_min 3 _cell_measurement_theta_max 18 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.765 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 264 _exptl_absorpt_coefficient_mu 0.164 # Sheldrick geometric approximatio 0.97 0.98 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.41 _exptl_absorpt_correction_T_max 0.98 _diffrn_measurement_device_type 'Bruker SMART' _diffrn_radiation_monochromator silicon _diffrn_radiation_type ' synchrotron ' _diffrn_radiation_wavelength 0.48650 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_ambient_pressure 4500000 _diffrn_reflns_number 2738 _reflns_number_total 299 _diffrn_reflns_av_R_equivalents 0.1011 # Number of reflections with Friedels Law is 299 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 524 _diffrn_reflns_reduction_process ; Merged with SORTAV R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 ; _diffrn_reflns_theta_min 2.975 _diffrn_reflns_theta_max 18.333 _diffrn_measured_fraction_theta_max 0.460 _diffrn_reflns_theta_full 13.933 _diffrn_measured_fraction_theta_full 0.467 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 5 _reflns_limit_h_min 0 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 6 _reflns_limit_l_min 0 _reflns_limit_l_max 5 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.20 _refine_diff_density_max 0.22 _refine_ls_number_reflns 298 _refine_ls_number_restraints 85 _refine_ls_number_parameters 100 #_refine_ls_R_factor_ref 0.0465 _refine_ls_wR_factor_ref 0.0436 _refine_ls_goodness_of_fit_ref 0.8385 #_reflns_number_all 298 _refine_ls_R_factor_all 0.0465 _refine_ls_wR_factor_all 0.0436 # No actual I/u(I) cutoff was used for refinement. The # threshold below is used for "_gt" information ONLY: _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 251 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_gt 0.0421 _refine_ls_shift/su_max 0.000121 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration unk _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment refxyz # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ; Method= SQRT(W) = 1/(Data with the key SIGMA(/FO/) in list 6) ; _publ_section_exptl_refinement ; checkcif Output: 022_ALERT_3_A Ratio Unique / Expected Reflections too Low .... 0.46 027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 13.93 Deg. 029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.47 089_ALERT_3_A Poor Data / Parameter Ratio (Zmax .LT. 18) ..... 2.98 910_ALERT_3_C # Missing FCF Reflections Below TH(Min) ........ 3 912_ALERT_3_C # Missing FCF Reflections Above STH/L=0.6 ...... 69 911_ALERT_3_B # Missing FCF Refl Between THmin & STh/l= 278 The high pressure cell causes shading of a significant proportion of the sphere of reflections. This means that the completeness is reduced. 199_ALERT_1_A Check the Reported _cell_measurement_temperature 293 K 200_ALERT_1_A Check the Reported _diffrn_ambient_temperature . 293 K Data were collected at 293K 042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? The one given is chemically more meaningful 250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.55 This is probably due to the lack of information in one direction which occurs as a result of the Merrill-Bassett diamond-anvil cell shading a significant region of reciprocal space. The effect of this shading is often to cause a smearing out of electron density in one particular direction. 731_ALERT_1_C Bond Calc 0.82(5), Rep 0.821(18) ...... 2.78 su-Rat O4 -H8 1.555 1.555 731_ALERT_1_C Bond Calc 0.83(4), Rep 0.826(18) ...... 2.22 su-Rat O4 -H9 1.555 1.555 This alert is due to the fact that PLATON calculates esds using only the variances whereas CRYSTALS uses the full variance/covariance matrix. ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens C1 C 0.54201(19) 0.2365(4) 0.2821(4) 0.0218 1.0000 Uani D U . . . . C2 C 0.39741(18) 0.2470(4) 0.1279(4) 0.0219 1.0000 Uani D U . . . . C3 C 0.33594(19) 0.3698(4) 0.1761(5) 0.0237 1.0000 Uani D U . . . . N1 N 0.30095(15) 0.1515(5) 0.2388(4) 0.0238 1.0000 Uani D U . . . . O1 O 0.56151(14) 0.1490(4) 0.4485(5) 0.0420 1.0000 Uani D U . . . . O2 O 0.63011(13) 0.3198(4) 0.2343(3) 0.0278 1.0000 Uani D U . . . . O3 O 0.33259(15) 0.3969(4) 0.4859(3) 0.0314 1.0000 Uani D U . . . . O4 O 0.07828(15) -0.0024(4) 0.3199(5) 0.0253 1.0000 Uani D . . . . . H1 H 0.4134(18) 0.236(2) -0.085(3) 0.0276 1.0000 Uiso D . . . . . H2 H 0.394(2) 0.430(2) 0.077(4) 0.0289 1.0000 Uiso D . . . . . H3 H 0.2403(16) 0.371(2) 0.098(4) 0.0289 1.0000 Uiso D . . . . . H4 H 0.278(2) 0.166(2) 0.430(4) 0.0362 1.0000 Uiso D . . . . . H5 H 0.2230(19) 0.150(3) 0.126(4) 0.0362 1.0000 Uiso D . . . . . H6 H 0.344(2) 0.0797(18) 0.227(6) 0.0362 1.0000 Uiso D . . . . . H7 H 0.257(3) 0.363(5) 0.529(8) 0.0460 1.0000 Uiso D . . . . . H8 H 0.037(4) -0.043(6) 0.193(9) 0.0523 1.0000 Uiso D . . . . . H9 H 0.011(3) 0.033(6) 0.401(9) 0.0523 1.0000 Uiso 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 0.0150(7) 0.038(4) 0.0123(9) 0.0026(16) 0.0025(7) 0.0001(13) C2 0.0159(8) 0.035(4) 0.0146(8) -0.0018(16) 0.0012(6) 0.0006(14) C3 0.0173(8) 0.032(4) 0.0222(9) 0.0012(17) 0.0001(6) -0.0021(16) N1 0.0163(6) 0.034(5) 0.0208(8) -0.0011(16) -0.0017(6) -0.0031(14) O1 0.0180(6) 0.055(5) 0.0527(11) 0.030(2) -0.0067(7) -0.0094(16) O2 0.0189(6) 0.043(4) 0.0214(7) 0.0039(12) 0.0018(5) -0.0055(11) O3 0.0185(6) 0.049(5) 0.0269(8) -0.0128(14) 0.0060(5) -0.0065(13) O4 0.0258(7) 0.020(6) 0.0300(8) 0.0022(14) -0.0019(6) 0.0010(12) _refine_ls_extinction_method None _oxford_refine_ls_scale 3.15(9) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 . C2 . 1.526(2) yes C1 . O1 . 1.233(5) yes C1 . O2 . 1.255(4) yes C2 . C3 . 1.488(6) yes C2 . N1 . 1.475(5) yes C2 . H1 . 0.973(15) no C3 . O3 . 1.419(3) yes C3 . H2 . 0.968(17) no C3 . H3 . 0.962(15) no N1 . H4 . 0.896(16) no N1 . H5 . 0.889(16) no N1 . H6 . 0.888(17) no O3 . H7 . 0.826(17) no O4 . H8 . 0.821(18) no O4 . H9 . 0.826(18) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 . C1 . O1 . 117.7(2) yes C2 . C1 . O2 . 116.8(2) yes O1 . C1 . O2 . 125.42(18) yes C1 . C2 . C3 . 110.4(2) yes C1 . C2 . N1 . 109.7(2) yes C3 . C2 . N1 . 111.40(18) yes C1 . C2 . H1 . 107.3(10) no C3 . C2 . H1 . 108.1(14) no N1 . C2 . H1 . 109.8(13) no C2 . C3 . O3 . 110.0(2) yes C2 . C3 . H2 . 110.2(13) no O3 . C3 . H2 . 108.4(12) no C2 . C3 . H3 . 108.7(15) no O3 . C3 . H3 . 109.4(11) no H2 . C3 . H3 . 110.1(14) no C2 . N1 . H4 . 109.5(15) no C2 . N1 . H5 . 109.1(14) no H4 . N1 . H5 . 110.8(14) no C2 . N1 . H6 . 110.0(13) no H4 . N1 . H6 . 109.1(16) no H5 . N1 . H6 . 108.4(16) no C3 . O3 . H7 . 99(3) no H8 . O4 . H9 . 102(4) no _chemical_name_common 'Serine Monohydrate' _exptl_crystal_recrystallization_method 'From H2O/EtOH' data_x_serhyII_52kbar _database_code_depnum_ccdc_archive 'CCDC 692792' #Serine hydrate phase II at 5.2 GPa. #X-N refinement. #X-N refinement. Xray data set is x_serhyII_52kbar. #Edinburgh dataset code = serhy5 #Notes on this cif: #The structural data comes from a joint X-N refinement (see text in paper) #The majority of this cif was generated with CRYSTALS. #The Topas cif was processed using Platon so that x's and u's conform to the #'rule of 19'. The x's, u's and geometrical parameters were then pasted into #this cif. R-factors: _refine_ls_wR_factor_ref corresponds to the Topas Rwp. #Other R-factors were calculated by importing the final model into crystals #and doing a structure factor calculation. _oxford_structure_analysis_title 'serhy5 in P2(1)2(1)2(1)' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 9.8778(13) _cell_length_b 10.155(4) _cell_length_c 4.4175(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 443.13(18) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,-y+1/2,-z -x,y+1/2,-z+1/2 -x+1/2,-y,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0010 0.0010 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0020 0.0010 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0040 0.0030 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C3 H9 N1 O4 # Dc = 1.85 Fooo = 264.00 Mu = 1.71 M = 123.11 # Found Formula = C3 H9 N1 O4 # Dc = 1.85 FOOO = 264.00 Mu = 1.71 M = 123.11 _chemical_formula_sum 'C3 H9 N1 O4' _chemical_formula_moiety 'C3 H9 N1 O4' _chemical_compound_source ? _chemical_formula_weight 123.11 _cell_measurement_reflns_used 542 _cell_measurement_theta_min 3 _cell_measurement_theta_max 17 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.845 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 264 _exptl_absorpt_coefficient_mu 0.171 # Sheldrick geometric approximatio 0.97 0.98 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.68 _exptl_absorpt_correction_T_max 0.98 _diffrn_measurement_device_type 'Bruker SMART' _diffrn_radiation_monochromator silicon _diffrn_radiation_type ' synchrotron ' _diffrn_radiation_wavelength 0.48650 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_ambient_pressure 5200000 _diffrn_reflns_number 2207 _reflns_number_total 276 _diffrn_reflns_av_R_equivalents 0.1768 # Number of reflections with Friedels Law is 276 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 455 _diffrn_reflns_reduction_process ; Merged with SORTAV R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 ; _diffrn_reflns_theta_min 2.823 _diffrn_reflns_theta_max 17.722 _diffrn_measured_fraction_theta_max 0.484 _diffrn_reflns_theta_full 15.063 _diffrn_measured_fraction_theta_full 0.492 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 5 _reflns_limit_h_min 0 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 6 _reflns_limit_l_min 0 _reflns_limit_l_max 5 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.36 _refine_diff_density_max 0.29 _refine_ls_number_reflns 246 _refine_ls_number_restraints 3 _refine_ls_number_parameters 109 #in full x-n refinement _refine_ls_wR_factor_ref 0.1110 _refine_ls_goodness_of_fit_ref 1.670 #_reflns_number_all 253 _refine_ls_R_factor_all 0.1128 _refine_ls_wR_factor_all 0.1110 # No actual I/u(I) cutoff was used for refinement. The # threshold below is used for "_gt" information ONLY: _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 167 _refine_ls_R_factor_gt 0.0718 _refine_ls_wR_factor_gt 0.1032 _refine_ls_shift/su_max 0.000 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration unk _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _publ_section_exptl_refinement ; Checkcif Output: 022_ALERT_3_A Ratio Unique / Expected Reflections too Low .... 0.49 027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 15.06 Deg. 029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.49 089_ALERT_3_A Poor Data / Parameter Ratio (Zmax .LT. 18) ..... 2.26 020_ALERT_3_B The value of Rint is greater than 0.10 ......... 0.18 250_ALERT_2_B Large U3/U1 Ratio for Average U(i,j) Tensor .... 6.35 213_ALERT_2_C Atom C2 has ADP max/min Ratio ............. 3.10 prola The TLS formalism was used to constarin the Uijs. The lack of data in one direction of reciprocal space (due to the pressure cell) will distirt these tensors, though the distortion is not as great as on full independent Uij refinement. 340_ALERT_3_B Low Bond Precision on C-C Bonds (x 1000) Ang ... 13 This calculation does not take the off diagonal variance-covariance terms into account. See text. 417_ALERT_2_B Short Inter D-H..H-D H6 .. H8 .. 2.06 Ang. 415_ALERT_2_C Short Inter D-H..H-X H2 .. H9 .. 2.12 Ang. This is a high-pressure crystal structure. H...H distances can fall as low as 1.7 Ang. 042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? No action. 125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? No action. 152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? Just a rounding error: Volume Reported 443.13(18) Calculated 443.1(2) 245_ALERT_2_C U(iso) H4 Smaller than U(eq) N1 by ... 0.01 AngSq 245_ALERT_2_C U(iso) H5 Smaller than U(eq) N1 by ... 0.01 AngSq 245_ALERT_2_C U(iso) H6 Smaller than U(eq) N1 by ... 0.01 AngSq 245_ALERT_2_C U(iso) H7 Smaller than U(eq) O3 by ... 0.01 AngSq No action. 199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K 200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K 791_ALERT_1_G Confirm the Absolute Configuration of C2 = . S 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 3 All OK. ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint loop_ _atom_site_label _atom_site_type_symbol _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 _atom_site_calc_flag _atom_site_refinement_flags O1 O Uani 0.6052(9) 0.1840(11) 0.489(2) 1.000 0.043(4) . . O2 O Uani 0.6580(10) 0.3339(11) 0.139(2) 1.000 0.043(4) . . O3 O Uani 0.348(3) 0.416(3) 0.487(6) 1.000 0.044(4) . . N1 N Uani 0.3572(11) 0.1445(16) 0.292(3) 1.000 0.043(3) . . C1 C Uani 0.5769(3) 0.2564(5) 0.2663(7) 1.000 0.038(3) . . C2 C Uani 0.4336(5) 0.2507(12) 0.1385(16) 1.000 0.037(3) . . C3 C Uani 0.3633(14) 0.384(2) 0.173(4) 1.000 0.040(3) . . O4 O Uani 0.0869(3) 0.0103(8) 0.3104(11) 1.000 0.024(5) . . H1 H Uiso 0.433(2) 0.228(2) -0.079(5) 1.000 0.030(9) . . H2 H Uiso 0.420(2) 0.451(3) 0.072(6) 1.000 0.030(9) . . H3 H Uiso 0.274(3) 0.377(3) 0.077(6) 1.000 0.030(9) . . H4 H Uiso 0.273(2) 0.177(3) 0.360(5) 1.000 0.030(9) . . H5 H Uiso 0.342(2) 0.075(3) 0.158(5) 1.000 0.030(9) . . H6 H Uiso 0.406(2) 0.1135(19) 0.460(4) 1.000 0.030(9) . . H7 H Uiso 0.270(4) 0.383(4) 0.538(9) 1.000 0.030(9) . . H8 H Uiso 0.108(2) 0.067(2) 0.168(5) 1.000 0.030(9) . . H9 H Uiso 0.005(2) 0.032(2) 0.366(4) 1.000 0.030(9) . . 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 O1 0.013(3) 0.099(12) 0.018(5) 0.005(5) -0.003(3) -0.005(3) O2 0.016(2) 0.086(10) 0.026(8) 0.001(6) 0.003(3) -0.005(3) O3 0.016(4) 0.096(10) 0.021(7) -0.017(5) -0.003(4) -0.005(4) N1 0.018(3) 0.087(8) 0.025(5) -0.004(5) -0.007(3) -0.010(3) C1 0.0139(18) 0.084(8) 0.015(4) -0.002(4) -0.002(2) -0.005(2) C2 0.016(2) 0.083(8) 0.012(3) -0.006(3) -0.004(2) -0.004(3) C3 0.017(2) 0.086(9) 0.017(5) -0.005(4) 0.000(3) 0.000(3) O4 0.0220(17) 0.029(16) 0.022(3) 0.005(4) 0.0032(17) 0.006(3) 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 O1 C1 1.260(10) . . yes O2 C1 1.256(11) . . yes O3 C3 1.43(3) . . yes O3 H7 0.87(5) . . no O4 H9 0.87(2) . . no O4 H8 0.88(2) . . no N1 C2 1.481(17) . . yes N1 H5 0.93(3) . . no N1 H4 0.94(2) . . no N1 H6 0.94(2) . . no C1 C2 1.525(6) . . no C2 C3 1.53(2) . . no C2 H1 0.99(2) . . no C3 H3 0.98(3) . . no C3 H2 0.99(3) . . 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 C3 O3 H7 105(4) . . . no H8 O4 H9 104.8(19) . . . no C2 N1 H5 110.0(19) . . . no C2 N1 H6 110.1(16) . . . no H4 N1 H5 109(2) . . . no H4 N1 H6 109(2) . . . no H5 N1 H6 109(3) . . . no C2 N1 H4 110(2) . . . no O1 C1 O2 125.0(7) . . . yes O2 C1 C2 116.8(6) . . . yes O1 C1 C2 118.2(6) . . . yes N1 C2 C1 109.3(7) . . . yes N1 C2 C3 111.6(9) . . . yes C1 C2 C3 110.6(9) . . . no O3 C3 C2 110.2(17) . . . yes N1 C2 H1 105.8(15) . . . no C3 C2 H1 107.5(15) . . . no C1 C2 H1 112.0(12) . . . no O3 C3 H2 110(3) . . . no O3 C3 H3 110(2) . . . no C2 C3 H3 108(2) . . . no H2 C3 H3 111(3) . . . no C2 C3 H2 107.9(19) . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 N1 -6.3(11) . . . . no O1 C1 C2 C3 116.9(10) . . . . no O2 C1 C2 N1 173.7(9) . . . . no O2 C1 C2 C3 -63.1(10) . . . . no N1 C2 C3 O3 58.3(18) . . . . no C1 C2 C3 O3 -63.6(17) . . . . no _chemical_name_common 'Serine Monohydrate' _exptl_crystal_recrystallization_method 'From H2O/EtOH' data_n_serhyII_58kbar _database_code_depnum_ccdc_archive 'CCDC 692793' #Serine hydrate phase II at 5.8 GPa. #X-N refinement. #Structural parameters here model the neutron powder data set. #ISIS data set code: PRL57157_66_60TNS_ASCII_TOF _chemical_name_systematic ; perdeuterated L-serine hydrate ; _chemical_name_common 'Serine hydrate' _chemical_formula_moiety 'C3 D7 N O3, D2 O1' _chemical_formula_structural ? _chemical_formula_sum 'C3 D9 N O4' _chemical_formula_weight 132.13 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 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' N N 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 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 P212121 _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 _cell_length_a 9.8641(14) _cell_length_b 10.09910(93) _cell_length_c 4.39860(65) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 438.18(10) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_measurement_temperature 298 _cell_measurement_pressure 5810000 #5.810(11) GPa _cell_measurement_reflns_used 1034 _cell_formula_units_Z 4 _cell_special_details ; Cell parameters included in refinement ; _exptl_crystal_density_diffrn 2.003 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 ? _pd_spec_mounting 'TiZr Capsule' _pd_spec_mount_mode transmission _pd_char_particle_morphology Block _pd_char_colour Colourless _chemical_absolute_configuration rm _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ; Calculated using custom ISIS software. ; _pd_instr_location 'ISIS, Rutherford Appleton Laboratory' _diffrn_ambient_temperature 298 _diffrn_source 'Pulsed neutron source' _diffrn_source_target ? _diffrn_radiation_type Neutron _diffrn_measurement_device_type 'HiPr/PEARL, ISIS' _diffrn_radiation_monochromator ? _diffrn_detector 'ZnS scintillator' _diffrn_detector_type custom _pd_meas_scan_method Time-of-flight _pd_meas_special_details ; Time of flight method using a pulsed neutron source ; _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_number 1034 # The following three items are used for time-of-flight measurements only. _pd_instr_dist_src/spec 12600 _pd_instr_dist_spec/detc 600 _pd_meas_2theta_fixed 90 _pd_proc_ls_profile_function ; Voigt function convoluted with a back-to-back double exponential. ; _pd_proc_ls_background_function 'Chebychev polynomial' _pd_proc_ls_pref_orient_corr ; Modelling of preferred orientation was found to be unnecessary. ; _pd_proc_ls_prof_R_factor 1.829 _pd_proc_ls_prof_wR_factor 1.484 _pd_proc_ls_prof_R_expected 1.226 _refine_ls_goodness_of_fit_all 1.211 _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 109 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_diff_density_max ? _refine_diff_density_min ? _refine_ls_shift/su_max <0.001 _pd_proc_info_excluded_regions ; excluded short TOF region above ; _pd_proc_info_data_reduction ; Custom ISIS software ; _refine_special_details ; Refinement was carried out against neutron and X-ray data simultaneously. The X-ray data had been collected using synchrotron radiation, and the pressure (ruby fluorescence) was 3.7 GPa. wR2 = 11.103 and S = 1.670 for pure 1/sigma^2 weights. Checkcif output: 023_ALERT_3_A Resolution (too) Low [sin(th)/Lambda < 0.6]..... 0.00 Deg. 027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 0.00 Deg. 029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.00 037_ALERT_1_A _diffrn_reflns_theta_full .......... Not Given . ? 038_ALERT_1_A _diffrn_measured_fraction_theta_max Not Given . ? 039_ALERT_1_A _diffrn_measured_fraction_theta_full Not Given . ? The resolution range was 0.64 to 4.14 Ang. 050_ALERT_1_A Absorption Coefficient mu Missing .............. ? TOF data - the absorption coefficient is variable. 095_ALERT_1_A No Residual Density Maximum Given .............. ? 096_ALERT_1_A No Residual Density Minimum Given .............. ? These data are not yet output by TOPAS. 201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 8 210_ALERT_3_B No Anisotropic ADP's Found in CIF .............. ? Powder data: see text of paper. 340_ALERT_3_B Low Bond Precision on C-C Bonds (x 1000) Ang ... 13 This is quite good for a high pressure neutron powder refinement! 415_ALERT_2_B Short Inter D-H..H-X H2 .. H8 .. 2.08 Ang. 415_ALERT_2_B Short Inter D-H..H-X H2 .. H9 .. 2.04 Ang. 417_ALERT_2_B Short Inter D-H..H-D H4 .. H8 .. 2.09 Ang. 417_ALERT_2_B Short Inter D-H..H-D H6 .. H8 .. 2.01 Ang. 432_ALERT_2_C Short Inter X...Y Contact O4 .. C1 .. 3.01 Ang. 432_ALERT_2_C Short Inter X...Y Contact O4 .. C2 .. 3.01 Ang. This is a high pressure structure. H...H contacts may be as short as 1.7 Ang in structures below 10 GPa. 040_ALERT_1_C No H-atoms in this Carbon Containing Compound .. ? 720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 9 The sample was deuterated. 152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? A rounding error: Volume Reported 438.18(10) Calculated 438.18(9) ; 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 0.57685(32) 0.25635(53) 0.26630(67) 1 1.254(89) C2 C 0 0.43359(49) 0.2507(12) 0.1385(16) 1 1.254(89) C3 C 0 0.3633(14) 0.3839(22) 0.1730(40) 1 1.254(89) N1 N 0 0.3572(11) 0.1445(16) 0.2922(26) 1 1.254(89) O1 O 0 0.60520(93) 0.1840(11) 0.4892(22) 1 1.254(89) O2 O 0 0.65801(97) 0.3339(11) 0.1387(23) 1 1.254(89) O3 O 0 0.3484(26) 0.4155(31) 0.4868(63) 1 1.254(89) H1 D 0 0.4329(25) 0.2255(21) -0.1003(43) 1 1.50(11) H2 D 0 0.4251(23) 0.4578(28) 0.0618(60) 1 1.50(11) H3 D 0 0.2648(27) 0.3768(30) 0.0666(59) 1 1.50(11) H4 D 0 0.2647(19) 0.1797(24) 0.3670(44) 1 1.50(11) H5 D 0 0.3403(19) 0.0668(23) 0.1443(43) 1 1.50(11) H6 D 0 0.4110(19) 0.1096(18) 0.4771(40) 1 1.50(11) H7 D 0 0.2611(44) 0.3804(43) 0.5446(93) 1 1.50(11) O4 O 0 0.08688(34) 0.01031(79) 0.3104(11) 1 1.254(89) H8 D 0 0.1104(21) 0.0727(21) 0.1525(46) 1 1.50(11) H9 D 0 -0.0037(16) 0.0347(19) 0.3725(48) 1 1.50(11)