# Electronic Supplementary Material (ESI) for Physical Chemistry Chemical Physics # This journal is © The Owner Societies 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_240K-Pbcn #============================================================================== _audit_creation_date 2013-09-19 _audit_creation_method CRYSTALS_ver_14.52 _oxford_structure_analysis_title 002ja13-100K _chemical_name_systematic 'hexahydroxytriphenylene tetrahydrate' _chemical_melting_point 'not measured' _cell_length_a 14.2568(2) _cell_length_b 16.7791(2) _cell_length_c 7.2308(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1729.73(4) _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c n ' _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,z x+1/2,-y+1/2,-z x,-y,z+1/2 -x,y,-z+1/2 -x+1/2,-y+1/2,z+1/2 x+1/2,y+1/2,-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 0.0181 0.0091 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' O 0.0492 0.0322 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 = C72 H80 O40 # Dc = 1.52 Fooo = 832.00 Mu = 10.80 M = 198.18 # Found Formula = C72 H80 O40 # Dc = 1.52 FOOO = 832.00 Mu = 10.80 M = 198.18 _chemical_formula_sum 'C18 H20 O10' _chemical_formula_moiety 'C18 H12 O6, 4(H2 O)' _chemical_compound_source . _chemical_formula_weight 396.35 _cell_measurement_reflns_used 15238 _cell_measurement_theta_min 4.0480 _cell_measurement_theta_max 76.8220 _cell_measurement_temperature 240 _exptl_crystal_description plate _exptl_crystal_colour clear_pale_orange _exptl_crystal_size_min 0.03 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_max 0.19 _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 1.080 # Sheldrick geometric approximatio 0.90 0.97 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlis, (Oxford Diffraction, 2002)' _exptl_absorpt_correction_T_min 0.87879 _exptl_absorpt_correction_T_max 1.00000 _diffrn_measurement_device_type 'Oxford Diffraction SuperNova' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54178 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SuperNova, (Oxford Diffraction, 2010)' _computing_cell_refinement 'CrysAlis, (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis, (Oxford Diffraction, 2002)' _computing_structure_solution 'Structure refined from (modified) coordinates determined 100 K' _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 240 _diffrn_reflns_number 34892 _reflns_number_total 1816 _diffrn_reflns_av_R_equivalents 0.027 # Number of reflections with Friedels Law is 1816 # Theoretical number of reflections is about 3652 _diffrn_reflns_theta_min 4.069 _diffrn_reflns_theta_max 76.870 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 76.870 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _reflns_limit_h_min 0 _reflns_limit_h_max 17 _reflns_limit_k_min -21 _reflns_limit_k_max 0 _reflns_limit_l_min 0 _reflns_limit_l_max 9 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.53 _refine_diff_density_max 0.31 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 1806 _refine_ls_number_restraints 0 _refine_ls_number_parameters 125 _oxford_refine_ls_R_factor_ref 0.0527 _refine_ls_wR_factor_ref 0.1351 _refine_ls_goodness_of_fit_ref 0.9963 _refine_ls_shift/su_max 0.0004005 _refine_ls_shift/su_mean 0.0000474 # The values computed with all filters except I/sigma _oxford_reflns_number_all 1806 _refine_ls_R_factor_all 0.0527 _refine_ls_wR_factor_all 0.1351 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 1609 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_gt 0.1304 # 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 . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr #undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.07P)^2^ + 1.38P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached 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 0.45531(11) 0.26762(9) 0.7101(2) 0.0287 1.0000 Uani . . . . . . C2 C 0.41209(11) 0.33865(9) 0.6705(2) 0.0267 1.0000 Uani . . . . . . C3 C 0.45487(10) 0.41240(8) 0.7092(2) 0.0226 1.0000 Uani . . . . . . C4 C 0.40783(10) 0.48771(9) 0.66921(19) 0.0225 1.0000 Uani . . . . . . C5 C 0.31771(10) 0.49067(9) 0.5894(2) 0.0257 1.0000 Uani . . . . . . C6 C 0.27303(11) 0.56190(9) 0.5557(2) 0.0275 1.0000 Uani . . . . . . C7 C 0.31717(11) 0.63343(9) 0.6044(2) 0.0283 1.0000 Uani . . . . . . C8 C 0.40490(11) 0.63196(9) 0.6803(2) 0.0278 1.0000 Uani . . . . . . C9 C 0.45277(10) 0.56006(9) 0.7117(2) 0.0235 1.0000 Uani . . . . . . O1 O 0.41629(9) 0.19451(7) 0.6751(2) 0.0437 1.0000 Uani . . . . . . O6 O 0.18630(9) 0.56766(7) 0.4754(2) 0.0384 1.0000 Uani . . . . . . O7 O 0.26947(8) 0.70354(7) 0.5698(2) 0.0384 1.0000 Uani . . . . . . O100 O -0.0671(3) 0.5590(3) 0.5476(6) 0.0558(12) 0.5000 Uiso . . . . 1 . O200 O -0.1287(3) 0.6728(2) 1.3105(5) 0.0534(10) 0.5000 Uiso . . . . 1 . O300 O -0.0997(3) 0.6703(2) 1.2830(5) 0.0458(8) 0.5000 Uiso . . . . 2 . O400 O -0.0838(3) 0.5616(2) 0.5923(6) 0.0466(10) 0.5000 Uiso . . . . 2 . H21 H 0.3534 0.3384 0.6154 0.0287 1.0000 Uiso R . . . . . H51 H 0.2892 0.4447 0.5538 0.0288 1.0000 Uiso R . . . . . H81 H 0.4330 0.6795 0.7127 0.0312 1.0000 Uiso R . . . . . H11 H 0.3654 0.1974 0.6341 0.0633 1.0000 Uiso R . . . . . H61 H 0.1668 0.5263 0.4328 0.0532 1.0000 Uiso R . . . . . H71 H 0.2989 0.7372 0.6232 0.0564 1.0000 Uiso R . . . . . H1001 H -0.0642 0.5858 0.6435 0.0763 0.5000 Uiso R . . . 1 . H1002 H -0.0162 0.5381 0.5158 0.0758 0.5000 Uiso R . . . 1 . H2001 H -0.1489 0.6481 1.2185 0.0721 0.5000 Uiso R . . . 1 . H2002 H -0.0994 0.6467 1.3865 0.0713 0.5000 Uiso R . . . 1 . H3001 H -0.1446 0.6692 1.2044 0.0649 0.5000 Uiso R . . . 2 . H3002 H -0.0478 0.6651 1.2312 0.0651 0.5000 Uiso R . . . 2 . H4001 H -0.1234 0.5859 0.6559 0.0644 0.5000 Uiso R . . . 2 . H4002 H -0.0709 0.5844 0.4924 0.0638 0.5000 Uiso R . . . 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 C1 0.0271(8) 0.0195(7) 0.0395(9) -0.0012(6) -0.0027(7) -0.0029(6) C2 0.0226(7) 0.0237(8) 0.0339(8) -0.0008(6) -0.0030(6) 0.0001(5) C3 0.0235(7) 0.0204(7) 0.0238(7) -0.0004(5) 0.0021(6) 0.0007(5) C4 0.0238(7) 0.0212(7) 0.0226(7) 0.0000(5) 0.0031(5) 0.0015(5) C5 0.0258(7) 0.0213(7) 0.0299(7) -0.0020(6) 0.0002(6) 0.0008(6) C6 0.0232(7) 0.0275(8) 0.0317(8) -0.0006(6) 0.0008(6) 0.0036(6) C7 0.0269(8) 0.0216(7) 0.0365(8) 0.0014(6) 0.0059(6) 0.0057(6) C8 0.0271(7) 0.0200(7) 0.0364(8) -0.0007(6) 0.0037(6) -0.0004(6) C9 0.0242(7) 0.0216(7) 0.0248(7) 0.0001(5) 0.0042(6) 0.0008(6) O1 0.0332(7) 0.0202(6) 0.0776(10) -0.0031(6) -0.0158(6) -0.0026(5) O6 0.0300(6) 0.0279(6) 0.0574(8) -0.0029(5) -0.0120(6) 0.0055(5) O7 0.0288(6) 0.0218(6) 0.0647(9) 0.0012(5) -0.0009(5) 0.0065(4) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.548(2) 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 . C1 6_656 1.399(3) yes C1 . C2 . 1.372(2) yes C1 . O1 . 1.3704(18) yes C2 . C3 . 1.408(2) yes C2 . H21 . 0.927 no C3 . C3 6_656 1.415(3) yes C3 . C4 . 1.4596(19) yes C4 . C5 . 1.409(2) yes C4 . C9 . 1.407(2) yes C5 . C6 . 1.376(2) yes C5 . H51 . 0.909 no C6 . C7 . 1.400(2) yes C6 . O6 . 1.3696(19) yes C7 . C8 . 1.366(2) yes C7 . O7 . 1.3818(18) yes C8 . C9 . 1.405(2) yes C8 . H81 . 0.923 no C9 . C9 6_656 1.456(3) yes O1 . H11 . 0.785 no O6 . H61 . 0.808 no O7 . H71 . 0.803 no O100 . H1001 . 0.828 no O100 . H1002 . 0.837 no O200 . H2001 . 0.834 no O200 . H2002 . 0.817 no O300 . H3001 . 0.856 no O300 . H3002 . 0.833 no O400 . H4001 . 0.836 no O400 . H4002 . 0.838 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 C1 6_656 C1 . C2 . 119.68(9) yes C1 6_656 C1 . O1 . 116.48(8) yes C2 . C1 . O1 . 123.84(15) yes C1 . C2 . C3 . 121.85(15) yes C1 . C2 . H21 . 119.4 no C3 . C2 . H21 . 118.7 no C3 6_656 C3 . C2 . 118.47(9) yes C3 6_656 C3 . C4 . 120.02(8) yes C2 . C3 . C4 . 121.50(14) yes C3 . C4 . C5 . 122.04(13) yes C3 . C4 . C9 . 119.63(13) yes C5 . C4 . C9 . 118.32(13) yes C4 . C5 . C6 . 121.67(14) yes C4 . C5 . H51 . 119.6 no C6 . C5 . H51 . 118.6 no C5 . C6 . C7 . 119.47(14) yes C5 . C6 . O6 . 123.67(14) yes C7 . C6 . O6 . 116.86(13) yes C6 . C7 . C8 . 119.80(14) yes C6 . C7 . O7 . 117.58(14) yes C8 . C7 . O7 . 122.61(15) yes C7 . C8 . C9 . 121.69(14) yes C7 . C8 . H81 . 118.9 no C9 . C8 . H81 . 119.4 no C9 6_656 C9 . C4 . 120.29(8) yes C9 6_656 C9 . C8 . 120.73(9) yes C4 . C9 . C8 . 118.98(14) yes C1 . O1 . H11 . 112.9 no C6 . O6 . H61 . 114.3 no C7 . O7 . H71 . 104.8 no H1001 . O100 . H1002 . 114.5 no H2001 . O200 . H2002 . 116.6 no H3001 . O300 . H3002 . 111.3 no H4001 . O400 . H4002 . 113.6 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C8 . H81 . O300 4_567 140.79 0.923 2.562 3.329(2) yes O1 . H11 . O7 3_545 171.38 0.785 1.981 2.760(2) yes O6 . H61 . O100 2_566 145.32 0.808 2.023 2.727(2) yes O6 . H61 . O400 2_566 156.46 0.808 1.900 2.661(2) yes O7 . H71 . O200 4_567 165.72 0.803 1.891 2.677(2) yes O7 . H71 . O300 4_567 167.48 0.803 2.227 3.016(2) yes O100 . H1001 . O1 8_456 156.60 0.828 2.263 3.041(2) yes O100 . H1002 . O100 2_566 152.6 0.837 2.068 2.837(2) yes O400 . H1002 . O100 2_566 146.8 1.178 2.068 3.121(2) yes O100 . H1002 . O400 2_566 157.06 0.837 2.333 3.121(2) yes O400 . H1002 . O400 2_566 153.6 1.178 2.333 3.429(2) yes O200 . H2001 . O6 6_556 167.50 0.834 2.018 2.839(2) yes O300 . H2001 . O6 6_556 145.4 0.921 2.018 2.825(2) yes O200 . H2002 . O100 1_556 159.26 0.817 1.932 2.712(2) yes O300 . H2002 . O100 1_556 152.8 0.848 1.932 2.714(2) yes O200 . H2002 . O400 1_556 154.99 0.817 2.074 2.836(2) yes O300 . H2002 . O400 1_556 163.0 0.848 2.074 2.895(2) yes O200 . H3001 . O6 6_556 133.7 0.803 2.224 2.839(2) yes O300 . H3001 . O6 6_556 127.12 0.856 2.224 2.825(2) yes O300 . H3002 . O200 6_557 158.08 0.833 2.538 3.326(2) yes O300 . H3002 . O300 6_557 154.52 0.833 2.107 2.882(2) yes O400 . H4001 . O1 8_456 121.35 0.836 2.266 2.794(2) yes O400 . H4002 . O200 1_554 139.43 0.838 2.146 2.836(2) yes O400 . H4002 . O300 1_554 151.61 0.838 2.131 2.895(2) yes _iucr_refine_instructions_details_constraints ; # # Punched on 19/09/13 at 19:29:26 # #LIST 12 BLOCK SCALE C(1,X'S,U'S) UNTIL O(7) CONT O(100,X'S,U[ISO]) UNTIL O(400) RIDE C ( 2,X'S) H ( 21,X'S) RIDE C ( 5,X'S) H ( 51,X'S) RIDE C ( 8,X'S) H ( 81,X'S) RIDE O ( 1,X'S) H ( 11,X'S) RIDE O ( 6,X'S) H ( 61,X'S) RIDE O ( 7,X'S) H ( 71,X'S) RIDE O ( 100,X'S) H (1001,X'S) H (1002,X'S) RIDE O ( 200,X'S) H (2001,X'S) H (2002,X'S) RIDE O ( 300,X'S) H (3001,X'S) H (3002,X'S) RIDE O ( 400,X'S) H (4001,X'S) H (4002,X'S) END ; _iucr_refine_instructions_details_restraints ; # # Punched on 19/09/13 at 19:29:26 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; # Manually omitted reflections loop_ _oxford_refln_omitted_index_h _oxford_refln_omitted_index_k _oxford_refln_omitted_index_l _oxford_refln_omitted_flag _oxford_refln_omitted_details 2 0 2 x . 1 0 2 x . _database_code_depnum_ccdc_archive 'CCDC 962532' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_100K #============================================================================== _audit_creation_date 2013-09-19 _audit_creation_method CRYSTALS_ver_14.52 _oxford_structure_analysis_title 002ja13-100K _chemical_name_systematic 'hexahydroxytriphenylene tetrahydrate' _chemical_melting_point 'not measured' _cell_length_a 14.20002(19) _cell_length_b 16.7353(2) _cell_length_c 7.17809(9) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1705.82(4) _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M_alt 'P 21 c n ' _symmetry_space_group_name_Hall 'P -2n 2ab' loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,y+1/2,-z+1/2 x,-y,z+1/2 x+1/2,-y+1/2,-z 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 0.0181 0.0091 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' O 0.0492 0.0322 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 = C13.50 H15 O7.50 # Dc = 1.16 Fooo = 832.00 Mu = 8.22 M = 297.26 # Found Formula = C18 H20 O10 # Dc = 1.54 FOOO = 832.00 Mu = 10.95 M = 396.35 _chemical_formula_sum 'C18 H20 O10' _chemical_formula_moiety 'C18 H12 O6, 4(H2 O)' _chemical_compound_source . _chemical_formula_weight 396.35 _cell_measurement_reflns_used 19631 _cell_measurement_theta_min 4.0650 _cell_measurement_theta_max 76.7530 _cell_measurement_temperature 100 _exptl_crystal_description plate _exptl_crystal_colour clear_pale_orange _exptl_crystal_size_min 0.02 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_max 0.19 _exptl_crystal_density_diffrn 1.543 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 1.095 # Sheldrick geometric approximatio 0.90 0.90 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlis, (Oxford Diffraction, 2002)' _exptl_absorpt_correction_T_min 0.85253 _exptl_absorpt_correction_T_max 1.00000 _diffrn_measurement_device_type 'Oxford Diffraction SuperNova' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SuperNova, (Oxford Diffraction, 2010)' _computing_cell_refinement 'CrysAlis, (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis, (Oxford Diffraction, 2002)' _computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)' _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 100 _diffrn_reflns_number 35079 _reflns_number_total 3567 _diffrn_reflns_av_R_equivalents 0.024 # Number of reflections without Friedels Law is 3567 # Number of reflections with Friedels Law is 1861 # Theoretical number of reflections is about 1799 _diffrn_reflns_theta_min 4.083 _diffrn_reflns_theta_max 76.821 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 76.821 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _reflns_limit_h_min -17 _reflns_limit_h_max 17 _reflns_limit_k_min -21 _reflns_limit_k_max 0 _reflns_limit_l_min 0 _reflns_limit_l_max 9 _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 difmap _refine_diff_density_min -0.20 _refine_diff_density_max 0.27 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 3551 _refine_ls_number_restraints 1 _refine_ls_number_parameters 253 _oxford_refine_ls_R_factor_ref 0.0314 _refine_ls_wR_factor_ref 0.0924 _refine_ls_goodness_of_fit_ref 1.0051 _refine_ls_shift/su_max 0.0007376 _refine_ls_shift/su_mean 0.0001114 # The values computed with all filters except I/sigma _oxford_reflns_number_all 3552 _refine_ls_R_factor_all 0.0314 _refine_ls_wR_factor_all 0.0927 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3455 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_gt 0.0918 # 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 constr #undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 0.42P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached 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 0.45532(13) 0.26668(9) 0.7171(2) 0.0156 1.0000 Uani . . . . . . C2 C 0.41227(14) 0.33799(9) 0.67410(18) 0.0152 1.0000 Uani . . . . . . C3 C 0.45536(13) 0.41202(8) 0.7117(2) 0.0127 1.0000 Uani . . . . . . C4 C 0.40722(13) 0.48741(9) 0.66958(18) 0.0137 1.0000 Uani . . . . . . C5 C 0.31699(12) 0.48968(9) 0.58813(19) 0.0136 1.0000 Uani . . . . . . C6 C 0.27207(12) 0.56128(11) 0.5536(2) 0.0157 1.0000 Uani . . . . . . C7 C 0.31614(12) 0.63329(9) 0.6011(2) 0.0150 1.0000 Uani . . . . . . C8 C 0.40401(13) 0.63238(10) 0.68049(19) 0.0157 1.0000 Uani . . . . . . C9 C 0.45232(12) 0.55999(9) 0.7129(2) 0.0130 1.0000 Uani . . . . . . C10 C 0.54698(12) 0.56069(9) 0.7904(2) 0.0140 1.0000 Uani . . . . . . C11 C 0.59399(14) 0.63291(9) 0.82159(19) 0.0152 1.0000 Uani . . . . . . C12 C 0.68197(13) 0.63534(9) 0.8980(2) 0.0155 1.0000 Uani . . . . . . C13 C 0.72726(12) 0.56368(10) 0.9493(2) 0.0146 1.0000 Uani . . . . . . C14 C 0.68288(13) 0.49212(9) 0.9154(2) 0.0148 1.0000 Uani . . . . . . C15 C 0.59224(14) 0.48820(8) 0.83422(19) 0.0126 1.0000 Uani . . . . . . C16 C 0.54572(13) 0.41266(9) 0.7943(2) 0.0133 1.0000 Uani . . . . . . C17 C 0.58911(14) 0.33872(8) 0.83568(19) 0.0145 1.0000 Uani . . . . . . C18 C 0.54533(13) 0.26732(9) 0.7981(2) 0.0155 1.0000 Uani . . . . . . O1 O 0.41568(10) 0.19318(7) 0.68496(18) 0.0229 1.0000 Uani . . . . . . O6 O 0.18498(10) 0.56655(6) 0.47125(17) 0.0192 1.0000 Uani . . . . . . O7 O 0.26846(10) 0.70355(7) 0.56481(17) 0.0199 1.0000 Uani . . . . . . O12 O 0.72914(10) 0.70638(7) 0.93153(17) 0.0195 1.0000 Uani . . . . . . O13 O 0.81367(10) 0.57082(6) 1.03129(17) 0.0200 1.0000 Uani . . . . . . O18 O 0.58427(11) 0.19421(6) 0.83644(16) 0.0209 1.0000 Uani . . . . . . O100 O -0.07227(11) 0.55742(9) 0.5735(2) 0.0304 1.0000 Uani . . . . . . O200 O -0.11545(12) 0.67420(8) 1.30833(18) 0.0319 1.0000 Uani . . . . . . O300 O 0.10297(12) 0.66840(8) 1.21325(17) 0.0306 1.0000 Uani . . . . . . O400 O 0.08209(12) 0.56316(8) 0.9234(2) 0.0311 1.0000 Uani . . . . . . H11 H 0.3602 0.1971 0.6563 0.0352 1.0000 Uiso R . . . . . H21 H 0.3526 0.3370 0.6185 0.0177 1.0000 Uiso R . . . . . H51 H 0.2863 0.4426 0.5547 0.0156 1.0000 Uiso R . . . . . H61 H 0.1600 0.5234 0.4498 0.0311 1.0000 Uiso R . . . . . H71 H 0.3052 0.7414 0.5855 0.0314 1.0000 Uiso R . . . . . H81 H 0.4311 0.6819 0.7111 0.0182 1.0000 Uiso R . . . . . H111 H 0.5658 0.6826 0.7869 0.0171 1.0000 Uiso R . . . . . H121 H 0.7011 0.7425 0.8696 0.0303 1.0000 Uiso R . . . . . H131 H 0.8359 0.5278 1.0619 0.0306 1.0000 Uiso R . . . . . H141 H 0.7134 0.4444 0.9501 0.0178 1.0000 Uiso R . . . . . H171 H 0.6509 0.3383 0.8921 0.0170 1.0000 Uiso R . . . . . H181 H 0.6372 0.1984 0.8850 0.0325 1.0000 Uiso R . . . . . H1001 H -0.0523 0.5894 0.6524 0.0484 1.0000 Uiso R . . . . . H1002 H -0.0205 0.5357 0.5320 0.0472 1.0000 Uiso R . . . . . H2001 H -0.1494 0.6542 1.2217 0.0504 1.0000 Uiso R . . . . . H2002 H -0.1002 0.6417 1.3946 0.0502 1.0000 Uiso R . . . . . H3001 H 0.1314 0.6452 1.3042 0.0464 1.0000 Uiso R . . . . . H3002 H 0.0475 0.6725 1.2555 0.0471 1.0000 Uiso R . . . . . H4001 H 0.0922 0.5916 0.8282 0.0480 1.0000 Uiso R . . . . . H4002 H 0.0803 0.5887 1.0241 0.0479 1.0000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0163(7) 0.0102(7) 0.0203(7) -0.0003(5) -0.0001(6) -0.0010(6) C2 0.0140(7) 0.0146(8) 0.0169(7) -0.0001(5) -0.0014(6) -0.0002(6) C3 0.0139(7) 0.0113(7) 0.0129(6) 0.0006(5) 0.0017(6) 0.0028(6) C4 0.0158(8) 0.0129(8) 0.0123(6) 0.0004(5) 0.0023(6) 0.0008(6) C5 0.0136(7) 0.0117(7) 0.0157(7) -0.0007(5) 0.0011(6) 0.0005(6) C6 0.0140(7) 0.0168(8) 0.0165(7) -0.0004(6) -0.0001(6) 0.0010(7) C7 0.0131(7) 0.0125(7) 0.0193(7) 0.0012(6) 0.0040(6) 0.0034(6) C8 0.0160(8) 0.0121(7) 0.0188(7) -0.0001(5) 0.0031(7) -0.0019(6) C9 0.0142(7) 0.0127(7) 0.0123(6) 0.0006(5) 0.0027(6) 0.0010(6) C10 0.0147(7) 0.0131(7) 0.0142(6) 0.0003(5) 0.0027(6) -0.0004(7) C11 0.0161(7) 0.0120(6) 0.0176(7) 0.0008(5) 0.0026(7) -0.0005(6) C12 0.0182(7) 0.0107(7) 0.0177(7) -0.0006(6) 0.0022(6) -0.0033(6) C13 0.0123(7) 0.0154(8) 0.0161(7) 0.0004(6) 0.0012(6) -0.0019(6) C14 0.0172(8) 0.0112(7) 0.0160(7) 0.0019(5) 0.0009(6) 0.0005(6) C15 0.0129(7) 0.0122(7) 0.0127(6) 0.0006(5) 0.0027(6) -0.0011(7) C16 0.0159(7) 0.0118(8) 0.0124(6) 0.0004(5) 0.0016(6) 0.0013(6) C17 0.0122(7) 0.0136(7) 0.0176(6) 0.0014(5) -0.0008(6) 0.0005(6) C18 0.0158(7) 0.0125(7) 0.0182(7) 0.0014(5) 0.0002(6) 0.0027(6) O1 0.0170(6) 0.0114(5) 0.0404(7) -0.0009(4) -0.0073(5) -0.0023(5) O6 0.0165(6) 0.0137(5) 0.0275(6) -0.0016(4) -0.0054(5) 0.0019(4) O7 0.0163(5) 0.0105(5) 0.0328(6) 0.0011(4) -0.0005(5) 0.0029(4) O12 0.0155(5) 0.0115(5) 0.0315(6) 0.0004(4) -0.0009(5) -0.0029(4) O13 0.0161(6) 0.0148(5) 0.0290(6) 0.0014(4) -0.0065(5) -0.0014(5) O18 0.0175(6) 0.0111(5) 0.0342(6) 0.0020(4) -0.0053(5) 0.0011(5) O100 0.0266(7) 0.0241(6) 0.0403(7) -0.0006(5) -0.0098(6) -0.0051(5) O200 0.0460(8) 0.0173(6) 0.0324(6) -0.0008(4) -0.0111(5) 0.0002(6) O300 0.0395(7) 0.0205(6) 0.0316(6) 0.0026(5) -0.0036(6) 0.0063(5) O400 0.0330(8) 0.0219(6) 0.0384(7) -0.0013(5) -0.0097(6) 0.0048(5) _refine_ls_extinction_method None _oxford_refine_ls_scale 4.79(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 . 1.376(2) yes C1 . C18 . 1.4040(16) yes C1 . O1 . 1.3722(19) yes C2 . C3 . 1.408(2) yes C2 . H21 . 0.937 no C3 . C4 . 1.466(2) yes C3 . C16 . 1.4134(15) yes C4 . C5 . 1.409(2) yes C4 . C9 . 1.408(2) yes C5 . C6 . 1.380(2) yes C5 . H51 . 0.932 no C6 . C7 . 1.400(2) yes C6 . O6 . 1.374(2) yes C7 . C8 . 1.372(2) yes C7 . O7 . 1.3815(19) yes C8 . C9 . 1.412(2) yes C8 . H81 . 0.939 no C9 . C10 . 1.4548(14) yes C10 . C11 . 1.399(2) yes C10 . C15 . 1.408(2) yes C11 . C12 . 1.365(2) yes C11 . H111 . 0.957 no C12 . C13 . 1.410(2) yes C12 . O12 . 1.3856(19) yes C13 . C14 . 1.375(2) yes C13 . O13 . 1.366(2) yes C14 . C15 . 1.414(2) yes C14 . H141 . 0.942 no C15 . C16 . 1.455(2) yes C16 . C17 . 1.414(2) yes C17 . C18 . 1.374(2) yes C17 . H171 . 0.967 no C18 . O18 . 1.3706(19) yes O1 . H11 . 0.816 no O6 . H61 . 0.820 no O7 . H71 . 0.834 no O12 . H121 . 0.850 no O13 . H131 . 0.816 no O18 . H181 . 0.832 no O100 . H1001 . 0.830 no O100 . H1002 . 0.872 no O200 . H2001 . 0.855 no O200 . H2002 . 0.853 no O300 . H3001 . 0.860 no O300 . H3002 . 0.847 no O400 . H4001 . 0.845 no O400 . H4002 . 0.840 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 . C18 . 119.39(16) yes C2 . C1 . O1 . 123.87(16) yes C18 . C1 . O1 . 116.74(16) yes C1 . C2 . C3 . 121.81(16) yes C1 . C2 . H21 . 118.8 no C3 . C2 . H21 . 119.3 no C2 . C3 . C4 . 120.99(16) yes C2 . C3 . C16 . 118.79(16) yes C4 . C3 . C16 . 120.21(15) yes C3 . C4 . C5 . 122.19(14) yes C3 . C4 . C9 . 118.98(15) yes C5 . C4 . C9 . 118.83(14) yes C4 . C5 . C6 . 121.21(15) yes C4 . C5 . H51 . 120.6 no C6 . C5 . H51 . 118.2 no C5 . C6 . C7 . 119.82(15) yes C5 . C6 . O6 . 123.30(15) yes C7 . C6 . O6 . 116.87(15) yes C6 . C7 . C8 . 119.87(15) yes C6 . C7 . O7 . 117.88(14) yes C8 . C7 . O7 . 122.25(15) yes C7 . C8 . C9 . 121.34(15) yes C7 . C8 . H81 . 117.3 no C9 . C8 . H81 . 121.3 no C8 . C9 . C4 . 118.87(15) yes C8 . C9 . C10 . 120.35(16) yes C4 . C9 . C10 . 120.78(16) yes C9 . C10 . C11 . 120.59(16) yes C9 . C10 . C15 . 120.01(17) yes C11 . C10 . C15 . 119.40(15) yes C10 . C11 . C12 . 121.78(15) yes C10 . C11 . H111 . 120.7 no C12 . C11 . H111 . 117.5 no C11 . C12 . C13 . 119.82(15) yes C11 . C12 . O12 . 122.53(14) yes C13 . C12 . O12 . 117.65(15) yes C12 . C13 . C14 . 119.04(15) yes C12 . C13 . O13 . 116.60(14) yes C14 . C13 . O13 . 124.35(15) yes C13 . C14 . C15 . 122.04(14) yes C13 . C14 . H141 . 118.7 no C15 . C14 . H141 . 119.2 no C14 . C15 . C10 . 117.86(14) yes C14 . C15 . C16 . 122.31(14) yes C10 . C15 . C16 . 119.82(15) yes C15 . C16 . C3 . 120.09(16) yes C15 . C16 . C17 . 121.42(16) yes C3 . C16 . C17 . 118.49(16) yes C16 . C17 . C18 . 121.52(16) yes C16 . C17 . H171 . 119.4 no C18 . C17 . H171 . 119.1 no C1 . C18 . C17 . 119.99(16) yes C1 . C18 . O18 . 116.33(16) yes C17 . C18 . O18 . 123.68(15) yes C1 . O1 . H11 . 111.5 no C6 . O6 . H61 . 114.5 no C7 . O7 . H71 . 107.8 no C12 . O12 . H121 . 107.1 no C13 . O13 . H131 . 112.7 no C18 . O18 . H181 . 112.0 no H1001 . O100 . H1002 . 102.3 no H2001 . O200 . H2002 . 115.0 no H3001 . O300 . H3002 . 101.6 no H4001 . O400 . H4002 . 114.5 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag O1 . H11 . O12 2_446 175.96 0.816 1.971 2.786(2) yes O6 . H61 . O400 3_564 167.91 0.820 1.832 2.639(2) yes O7 . H71 . O200 4_567 167.38 0.834 1.961 2.781(2) yes C8 . H81 . O200 4_567 136.75 0.939 2.501 3.250(2) yes C11 . H111 . O300 4_567 139.84 0.957 2.548 3.337(2) yes O12 . H121 . O300 4_567 162.37 0.850 2.125 2.946(2) yes O13 . H131 . O100 3_665 157.37 0.816 1.935 2.706(2) yes O18 . H181 . O7 2_546 165.94 0.832 1.900 2.714(2) yes O100 . H1001 . O1 2_456 145.41 0.830 2.141 2.863(2) yes O100 . H1002 . O400 3_564 158.98 0.872 2.338 3.168(2) yes O200 . H2001 . O13 1_455 155.15 0.855 2.023 2.822(2) yes O200 . H2002 . O100 1_556 173.13 0.853 1.948 2.796(2) yes O300 . H3001 . O6 1_556 164.02 0.860 1.937 2.773(2) yes O300 . H3002 . O200 . 167.64 0.847 2.344 3.177(2) yes O400 . H4001 . O18 2_456 155.76 0.845 2.088 2.879(2) yes O400 . H4002 . O300 . 162.12 0.840 1.931 2.742(2) yes _iucr_refine_instructions_details_constraints ; # # Punched on 19/09/13 at 12:48:39 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 2,X'S) H ( 21,X'S) RIDE C ( 5,X'S) H ( 51,X'S) RIDE C ( 8,X'S) H ( 81,X'S) RIDE C ( 11,X'S) H ( 111,X'S) RIDE C ( 14,X'S) H ( 141,X'S) RIDE C ( 17,X'S) H ( 171,X'S) RIDE O ( 1,X'S) H ( 11,X'S) RIDE O ( 6,X'S) H ( 61,X'S) RIDE O ( 7,X'S) H ( 71,X'S) RIDE O ( 12,X'S) H ( 121,X'S) RIDE O ( 13,X'S) H ( 131,X'S) RIDE O ( 18,X'S) H ( 181,X'S) RIDE O ( 100,X'S) H (1001,X'S) H (1002,X'S) RIDE O ( 200,X'S) H (2001,X'S) H (2002,X'S) RIDE O ( 300,X'S) H (3001,X'S) H (3002,X'S) RIDE O ( 400,X'S) H (4001,X'S) H (4002,X'S) END ; _iucr_refine_instructions_details_restraints ; # # Punched on 19/09/13 at 12:48:39 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; #============================================================================== # start Validation Reply Form #============================================================================== _vrf_SYMM003_100K ; PROBLEM: _symmetry_space_group_name_H-M is missing RESPONSE: This structure is in a non-standard setting of Pna2(1) for better comparison with the high-temperature phase (Pbcn). This very unusual setting is not compatible with PLATON/checkCIF which misinterprets the space group as P2mm and applies this symmetry to the structure coordinates leading to short contacts, voids, double occupancies and other issues. Ton Spek is aware of the issue. ; _vrf_PLAT075_100K ; PROBLEM: Occupancy 2. greater than 1.0 for ...... C14 RESPONSE: This structure is in a non-standard setting of Pna2(1) for better comparison with the high-temperature phase (Pbcn). This very unusual setting is not compatible with PLATON/checkCIF which misinterprets the space group as P2mm and applies this symmetry to the structure coordinates leading to short contacts, voids, double occupancies and other issues. Ton Spek is aware of the issue. ; _vrf_PLAT303_100K ; PROBLEM: Full Occupancy H-Atom H21 with # Connections 4.00 RESPONSE: This structure is in a non-standard setting of Pna2(1) for better comparison with the high-temperature phase (Pbcn). This very unusual setting is not compatible with PLATON/checkCIF which misinterprets the space group as P2mm and applies this symmetry to the structure coordinates leading to short contacts, voids, double occupancies and other issues. Ton Spek is aware of the issue. ; _vrf_PLAT310_100K ; PROBLEM: H51 Deleted (Close to C6 ) Dist ..... 0.212 Ang. RESPONSE: This structure is in a non-standard setting of Pna2(1) for better comparison with the high-temperature phase (Pbcn). This very unusual setting is not compatible with PLATON/checkCIF which misinterprets the space group as P2mm and applies this symmetry to the structure coordinates leading to short contacts, voids, double occupancies and other issues. Ton Spek is aware of the issue. ; _vrf_PLAT350_100K ; PROBLEM: Short C-H (X0.96,N1.08A) C2 - H81_c ... 0.50 Ang. RESPONSE: This structure is in a non-standard setting of Pna2(1) for better comparison with the high-temperature phase (Pbcn). This very unusual setting is not compatible with PLATON/checkCIF which misinterprets the space group as P2mm and applies this symmetry to the structure coordinates leading to short contacts, voids, double occupancies and other issues. Ton Spek is aware of the issue. ; _vrf_PLAT366_100K ; PROBLEM: Short? C(sp?)-C(sp?) Bond C2 - C8_c ... 0.51 Ang. RESPONSE: This structure is in a non-standard setting of Pna2(1) for better comparison with the high-temperature phase (Pbcn). This very unusual setting is not compatible with PLATON/checkCIF which misinterprets the space group as P2mm and applies this symmetry to the structure coordinates leading to short contacts, voids, double occupancies and other issues. Ton Spek is aware of the issue. ; _vrf_PLAT410_100K ; PROBLEM: Short Intra H...H Contact H21 .. H81 .. 1.34 Ang. RESPONSE: This structure is in a non-standard setting of Pna2(1) for better comparison with the high-temperature phase (Pbcn). This very unusual setting is not compatible with PLATON/checkCIF which misinterprets the space group as P2mm and applies this symmetry to the structure coordinates leading to short contacts, voids, double occupancies and other issues. Ton Spek is aware of the issue. ; _vrf_PLAT414_100K ; PROBLEM: Short Intra D-H..H-X H21 .. H71 .. 1.49 Ang. RESPONSE: This structure is in a non-standard setting of Pna2(1) for better comparison with the high-temperature phase (Pbcn). This very unusual setting is not compatible with PLATON/checkCIF which misinterprets the space group as P2mm and applies this symmetry to the structure coordinates leading to short contacts, voids, double occupancies and other issues. Ton Spek is aware of the issue. ; _vrf_PLAT417_100K ; PROBLEM: Short Inter D-H..H-D H1001 .. H2002 .. 1.16 Ang. RESPONSE: This structure is in a non-standard setting of Pna2(1) for better comparison with the high-temperature phase (Pbcn). This very unusual setting is not compatible with PLATON/checkCIF which misinterprets the space group as P2mm and applies this symmetry to the structure coordinates leading to short contacts, voids, double occupancies and other issues. Ton Spek is aware of the issue. ; _vrf_PLAT602_100K ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! Info RESPONSE: This structure is in a non-standard setting of Pna2(1) for better comparison with the high-temperature phase (Pbcn). This very unusual setting is not compatible with PLATON/checkCIF which misinterprets the space group as P2mm and applies this symmetry to the structure coordinates leading to short contacts, voids, double occupancies and other issues. Ton Spek is aware of the issue. ; #============================================================================== # end Validation Reply Form #============================================================================== _database_code_depnum_ccdc_archive 'CCDC 962533'