# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name 'Foxman, Bruce' _publ_contact_author_name 'Foxman, Bruce' _publ_contact_author_email foxman1@brandeis.edu _publ_section_title ; Stereospecific Solid-State Cyclodimerization of Bis(trans-2-butenoato)calcium and Triaquabis(trans-2-butenoato)magnesium+ ; # Attachment 'compound_4.cif' data_compound_4 _database_code_depnum_ccdc_archive 'CCDC 793570' #TrackingRef 'compound_4.cif' _audit_creation_date 10-06-11 _audit_creation_method CRYSTALS_ver_14.01 _oxford_structure_analysis_title CACROPYR _chemical_name_systematic ? _chemical_melting_point ? # start Validation Reply Form: One Alert B issue _vrf_PLAT220_compound_4 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.11 Ratio RESPONSE: The 4.11 ratio is between a methyl C atom (C4) that is part of the major component (ca. 95%) of a disordered crotonate and a vinyl C atom (C21) that is part of the minor component (ca. 5%). The ratio may vary widely in cases of this type. ; # end Validation Reply Form _cell_length_a 14.536(3) _cell_length_b 5.2295(5) _cell_length_c 6.4483(8) _cell_angle_alpha 90 _cell_angle_beta 100.415(13) _cell_angle_gamma 90 _cell_volume 482.11(13) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 2/c 1 ' _symmetry_space_group_name_Hall '-P 2yc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y,-z+1/2 x,-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 Ca 0.2262 0.3064 8.6266 10.4421 7.3873 0.6599 1.5899 85.7484 1.0211 178.4370 1.3751 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 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' C 0.0033 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' _cell_formula_units_Z 4 # Given Formula = C4 H5 Ca0.50 O2 # Dc = 1.45 Fooo = 220.00 Mu = 6.30 M = 105.12 # Found Formula = C4 H5.00 Ca0.50 O2 # Dc = 1.45 FOOO = 220.00 Mu = 6.30 M = 105.12 _chemical_formula_sum 'C4 H5.00 Ca0.50 O2' _chemical_formula_moiety 'C4 H5.00 Ca0.50 O2' _chemical_compound_source ? _chemical_formula_weight 105.12 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 21 _cell_measurement_theta_max 28 _cell_measurement_temperature 294 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_min 0.072 _exptl_crystal_size_mid 0.592 _exptl_crystal_size_max 0.684 _exptl_crystal_density_diffrn 1.448 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 220 _exptl_absorpt_coefficient_mu 0.630 # Sheldrick geometric approximatio 0.69 0.96 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North et al., 1968)' _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_T_max 0.96 _diffrn_measurement_device-type 'Enraf-Nonius CAD4' _diffrn_measurement_device Serial _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'CAD4 EXPRESS, (Straver, 1992)' _computing_cell_refinement 'CAD4 EXPRESS, (Straver, 1992)' _computing_data_reduction 'RC93 (Watkin et al., 1994)' _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 7200 _diffrn_standards_interval_count . _diffrn_standards_number 3 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 294 _diffrn_reflns_number 1587 _reflns_number_total 1462 _diffrn_reflns_av_R_equivalents 0.021 # Number of reflections without Friedels Law is 1462 # Number of reflections with Friedels Law is 0 # Theoretical number of reflections is about 1463 _diffrn_reflns_theta_min 3.896 _diffrn_reflns_theta_max 30.443 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 29.834 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _reflns_limit_h_min 0 _reflns_limit_h_max 20 _reflns_limit_k_min 0 _reflns_limit_k_max 7 _reflns_limit_l_min -9 _reflns_limit_l_max 8 _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 -0.32 _refine_diff_density_max 0.36 # 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>2.0\s(I) _refine_ls_number_reflns 1246 _refine_ls_number_restraints 4 _refine_ls_number_parameters 74 _oxford_refine_ls_R_factor_ref 0.0333 _refine_ls_wR_factor_ref 0.0420 _refine_ls_goodness_of_fit_ref 1.0087 _refine_ls_shift/su_max 0.0008145 _refine_ls_shift/su_mean 0.0005897 # The values computed from all data _oxford_reflns_number_all 1462 _refine_ls_R_factor_all 0.0455 _refine_ls_wR_factor_all 0.0594 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 1246 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_gt 0.0420 # 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 F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 2.22 0.977 1.71 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., 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. North, A.C.T., Phillips, D.C. & Mathews, F.S., (1968). Acta Cryst, A24, 351-359. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Straver, L. H. (1992). CAD4-EXPRESS, Nonius, Delft, The Netherlands. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. Watkin, D.J., Prout, C.K. & Lilley, P.M.deQ. (1994). RC93, 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 _oxford_atom_site_special_shape _atom_site_attached_hydrogens Ca1 Ca 1.0000 0.30799(6) 0.2500 0.0266 1.0000 Uani S T . . . . . O1 O 1.12084(8) -0.0348(2) 0.71649(19) 0.0416 1.0000 Uani . . . . . . . O2 O 1.07671(7) 0.3551(2) 0.60365(15) 0.0356 1.0000 Uani . . . . . . . C1 C 1.13582(8) 0.1957(2) 0.69858(18) 0.0279 1.0000 Uani . . . . . . . C2 C 1.22851(11) 0.3078(4) 0.7910(3) 0.0407 0.952(5) Uani . . P 1 1 . . C3 C 1.29883(13) 0.1702(4) 0.8857(3) 0.0513 0.952(5) Uani . . P 1 1 . . C4 C 1.39291(17) 0.2749(8) 0.9807(5) 0.0825 0.952(5) Uani . . P 1 1 . . C21 C 1.2304(14) 0.188(5) 0.816(3) 0.020(5) 0.048(5) Uiso D . P 1 2 . . C31 C 1.2844(19) 0.392(5) 0.819(5) 0.042(7) 0.048(5) Uiso D U P 1 2 . . C41 C 1.382(2) 0.412(8) 0.948(6) 0.048(8) 0.048(5) Uiso D U P 1 2 . . H21 H 1.2369 0.4854 0.7831 0.0503 0.952(5) Uiso . . P 1 1 . . H31 H 1.2884 -0.0089 0.8932 0.0615 0.952(5) Uiso . . P 1 1 . . H41 H 1.3918 0.4591 0.9707 0.1229 0.952(5) Uiso . . P 1 1 . . H42 H 1.4395 0.2077 0.9047 0.1228 0.952(5) Uiso . . P 1 1 . . H43 H 1.4082 0.2230 1.1249 0.1228 0.952(5) Uiso . . P 1 1 . . H211 H 1.2517 0.0418 0.8900 0.0271 0.048(5) Uiso . . P 1 2 . . H311 H 1.2643 0.5241 0.7300 0.0590 0.048(5) Uiso . . P 1 2 . . H411 H 1.3998 0.2414 1.0102 0.0870 0.048(5) Uiso . . P 1 2 . . H412 H 1.4241 0.4719 0.8744 0.0870 0.048(5) Uiso . . P 1 2 . . H413 H 1.3771 0.5217 1.0713 0.0870 0.048(5) Uiso . . P 1 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 Ca1 0.03326(19) 0.02277(17) 0.02331(17) 0.0000 0.00414(11) 0.0000 O1 0.0485(6) 0.0297(5) 0.0481(6) 0.0034(4) 0.0129(5) -0.0054(4) O2 0.0425(5) 0.0348(5) 0.0274(4) -0.0017(3) 0.0005(4) 0.0109(4) C1 0.0301(5) 0.0291(5) 0.0247(5) 0.0004(4) 0.0054(4) 0.0007(4) C2 0.0375(8) 0.0367(9) 0.0455(8) 0.0014(7) 0.0007(6) -0.0059(6) C3 0.0384(8) 0.0577(11) 0.0545(10) 0.0047(8) -0.0001(7) 0.0001(7) C4 0.0415(11) 0.108(3) 0.088(2) 0.0064(17) -0.0138(11) -0.0071(12) _refine_ls_extinction_coef 32(11) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 2.224(7) 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 Ca1 . O2 4_564 2.3705(10) yes Ca1 . O2 2_766 2.3705(10) yes Ca1 . O2 3_755 2.3632(10) yes Ca1 . O1 2_756 2.3044(11) yes Ca1 . O1 4_554 2.3044(11) yes Ca1 . O2 . 2.3632(10) yes O1 . C1 . 1.2343(16) yes O2 . C1 . 1.2717(15) yes C1 . C2 . 1.491(2) yes C1 . C21 . 1.45(2) yes C2 . C3 . 1.308(3) yes C2 . H21 . 0.939 no C3 . C4 . 1.497(3) yes C3 . H31 . 0.951 no C4 . H41 . 0.965 no C4 . H42 . 0.971 no C4 . H43 . 0.956 no C21 . C31 . 1.32(2) yes C21 . H211 . 0.924 no C31 . C41 . 1.51(3) yes C31 . H311 . 0.912 no C41 . H411 . 0.996 no C41 . H412 . 0.895 no C41 . H413 . 0.994 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 O2 4_564 Ca1 . O2 2_766 83.97(6) yes O2 4_564 Ca1 . O2 3_755 73.28(4) yes O2 2_766 Ca1 . O2 3_755 97.64(4) yes O2 4_564 Ca1 . O1 2_756 156.86(4) yes O2 2_766 Ca1 . O1 2_756 90.11(4) yes O2 3_755 Ca1 . O1 2_756 85.43(4) yes O2 4_564 Ca1 . O1 4_554 90.11(4) yes O2 2_766 Ca1 . O1 4_554 156.86(4) yes O2 3_755 Ca1 . O1 4_554 102.05(4) yes O1 2_756 Ca1 . O1 4_554 103.39(6) yes O2 4_564 Ca1 . O2 . 97.64(4) yes O2 2_766 Ca1 . O2 . 73.28(4) yes O2 3_755 Ca1 . O2 . 168.04(5) yes O1 2_756 Ca1 . O2 . 102.05(4) yes O1 4_554 Ca1 . O2 . 85.43(4) yes Ca1 2_756 O1 . C1 . 139.87(10) yes Ca1 2_766 O2 . Ca1 . 106.72(4) yes Ca1 2_766 O2 . C1 . 128.38(8) yes Ca1 . O2 . C1 . 123.79(8) yes O2 . C1 . O1 . 124.74(13) yes O2 . C1 . C2 . 114.69(13) yes O1 . C1 . C2 . 120.56(13) yes O2 . C1 . O1 . 124.74(13) yes O2 . C1 . C21 . 140.0(11) yes O1 . C1 . C21 . 95.2(11) yes C1 . C2 . C3 . 122.94(18) yes C1 . C2 . H21 . 118.9 no C3 . C2 . H21 . 118.1 no C2 . C3 . C4 . 124.7(2) yes C2 . C3 . H31 . 116.6 no C4 . C3 . H31 . 118.7 no C3 . C4 . H41 . 109.6 no C3 . C4 . H42 . 109.3 no H41 . C4 . H42 . 109.4 no C3 . C4 . H43 . 109.2 no H41 . C4 . H43 . 110.2 no H42 . C4 . H43 . 109.1 no C1 . C21 . C31 . 119(2) yes C1 . C21 . H211 . 119.4 no C31 . C21 . H211 . 121.2 no C21 . C31 . C41 . 124.0(5) yes C21 . C31 . H311 . 118.9 no C41 . C31 . H311 . 116.9 no C31 . C41 . H411 . 108.0 no C31 . C41 . H412 . 113.4 no H411 . C41 . H412 . 111.8 no C31 . C41 . H413 . 106.8 no H411 . C41 . H413 . 104.1 no H412 . C41 . H413 . 112.2 no # Attachment 'compound_11.cif' data_compound_11 _database_code_depnum_ccdc_archive 'CCDC 793571' #TrackingRef 'compound_11.cif' _audit_creation_date 10-06-11 _audit_creation_method CRYSTALS_ver_14.01 _oxford_structure_analysis_title MGCROTON _chemical_name_systematic ? _chemical_melting_point ? # start Validation Reply Form: One Alert B issues _vrf_REFNR01_compound_11 ; PROBLEM: Ratio of reflections to parameters is < 8 for a centrosymmetric structure RESPONSE: Only very thin, weakly-diffracting crystals could be obtained. Nonetheless, a satisfactory structure analysis could be easily realized, as the material was well-ordered. ; _vrf_PLAT088_compound_11 ; PROBLEM: Poor Data / Parameter Ratio .................... 7.96 RESPONSE: Only very thin, weakly-diffracting crystals could be obtained. Nonetheless, a satisfactory structure analysis could be easily realized, as the material was well-ordered. ; _cell_length_a 17.0609(10) _cell_length_b 8.1048(10) _cell_length_c 9.1311(10) _cell_angle_alpha 90 _cell_angle_beta 101.230(10) _cell_angle_gamma 90 _cell_volume 1238.4(2) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-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 0.0033 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' O 0.0106 0.0060 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' Mg 0.0486 0.0363 5.4204 2.8275 2.1735 79.2611 1.2269 0.3808 2.3073 7.1937 0.8584 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C8 H16 Mg1 O7 # Dc = 1.33 Fooo = 528.00 Mu = 1.60 M = 248.52 # Found Formula = C8 H16 Mg1 O7 # Dc = 1.33 FOOO = 528.00 Mu = 1.60 M = 248.52 _chemical_formula_sum 'C8 H16 Mg1 O7' _chemical_formula_moiety 'C8 H16 Mg1 O7' _chemical_compound_source ? _chemical_formula_weight 248.52 _cell_measurement_reflns_used 15 _cell_measurement_theta_min 21 _cell_measurement_theta_max 43 _cell_measurement_temperature 294 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_min 0.040 _exptl_crystal_size_mid 0.380 _exptl_crystal_size_max 0.420 _exptl_crystal_density_diffrn 1.333 # Non-dispersive F(000): _exptl_crystal_F_000 528 _exptl_absorpt_coefficient_mu 0.160 # Sheldrick geometric approximatio 0.94 0.99 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9411 _exptl_absorpt_correction_T_max 0.9936 _diffrn_measurement_device-type 'Enraf-Nonius CAD4' _diffrn_measurement_device Serial _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'CAD4 EXPRESS, (Straver, 1992)' _computing_cell_refinement 'CAD4 EXPRESS, (Straver, 1992)' _computing_data_reduction 'RC93 (Watkin et al., 1994)' _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 7200 _diffrn_standards_interval_count . _diffrn_standards_number 3 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 294 _diffrn_reflns_number 2843 _reflns_number_total 2490 _diffrn_reflns_av_R_equivalents 0.028 # Number of reflections without Friedels Law is 2490 # Number of reflections with Friedels Law is 0 # Theoretical number of reflections is about 2495 _diffrn_reflns_theta_min 3.653 _diffrn_reflns_theta_max 26.241 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.241 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 0 _reflns_limit_h_min 0 _reflns_limit_h_max 21 _reflns_limit_k_min 0 _reflns_limit_k_max 10 _reflns_limit_l_min -11 _reflns_limit_l_max 11 _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 -0.35 _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>2.0\s(I) _refine_ls_number_reflns 1154 _refine_ls_number_restraints 0 _refine_ls_number_parameters 145 _oxford_refine_ls_R_factor_ref 0.0478 _refine_ls_wR_factor_ref 0.0351 _refine_ls_goodness_of_fit_ref 1.1799 _refine_ls_shift/su_max 0.0000915 _refine_ls_shift/su_mean 0.1375915 # The values computed from all data _oxford_reflns_number_all 2490 _refine_ls_R_factor_all 0.1648 _refine_ls_wR_factor_all 0.0855 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 1154 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_gt 0.0351 # 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 F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.23 -0.793 0.910 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., 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. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Straver, L. H. (1992). CAD4-EXPRESS, Nonius, Delft, The Netherlands. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. Watkin, D.J., Prout, C.K. & Lilley, P.M.deQ. (1994). RC93, 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 _oxford_atom_site_special_shape _atom_site_attached_hydrogens Mg1 Mg 0.36331(6) -0.15217(13) -0.00903(12) 0.0240 1.0000 Uani . . . . . . . O1 O 0.38563(14) -0.3936(3) 0.0702(2) 0.0377 1.0000 Uani . . . . . . . O2 O 0.43726(12) -0.0662(2) 0.1916(2) 0.0258 1.0000 Uani . . . . . . . O3 O 0.47334(12) -0.1900(3) -0.0852(2) 0.0286 1.0000 Uani . . . . . . . O4 O 0.36062(15) 0.0820(3) -0.0785(3) 0.0448 1.0000 Uani . . . . . . . O5 O 0.40127(14) 0.3323(3) -0.1151(2) 0.0357 1.0000 Uani . . . . . . . O6 O 0.26107(13) -0.3612(3) -0.4234(2) 0.0311 1.0000 Uani . . . . . . . O7 O 0.30714(13) -0.2301(3) -0.2124(3) 0.0362 1.0000 Uani . . . . . . . C1 C 0.3521(2) 0.2152(4) -0.1477(4) 0.0293 1.0000 Uani . . . . . . . C2 C 0.2838(2) 0.2382(4) -0.2740(4) 0.0395 1.0000 Uani . . . . . . . C3 C 0.2226(2) 0.1415(5) -0.3020(5) 0.0501 1.0000 Uani . . . . . . . C4 C 0.1531(3) 0.1605(7) -0.4283(6) 0.0861 1.0000 Uani . . . . . . . C5 C 0.25264(19) -0.3062(4) -0.2989(3) 0.0261 1.0000 Uani . . . . . . . C6 C 0.1753(2) -0.3234(5) -0.2515(4) 0.0400 1.0000 Uani . . . . . . . C7 C 0.1117(2) -0.3858(5) -0.3346(5) 0.0554 1.0000 Uani . . . . . . . C8 C 0.0327(3) -0.4047(7) -0.2903(6) 0.0897 1.0000 Uani . . . . . . . H11 H 0.3640 -0.4077 0.1402 0.0556 1.0000 Uiso R . . . . . . H12 H 0.3831 -0.4791 0.0222 0.0561 1.0000 Uiso R . . . . . . H21 H 0.4542 -0.1416 0.2528 0.0390 1.0000 Uiso R . . . . . . H22 H 0.4213 0.0027 0.2444 0.0392 1.0000 Uiso R . . . . . . H31 H 0.4924 -0.1104 -0.1198 0.0436 1.0000 Uiso R . . . . . . H32 H 0.5083 -0.2261 -0.0180 0.0434 1.0000 Uiso R . . . . . . H23 H 0.2860 0.3275 -0.3379 0.0474 1.0000 Uiso R . . . . . . H33 H 0.2218 0.0530 -0.2373 0.0595 1.0000 Uiso R . . . . . . H41 H 0.1629 0.2503 -0.4899 0.1291 1.0000 Uiso R . . . . . . H42 H 0.1460 0.0609 -0.4837 0.1295 1.0000 Uiso R . . . . . . H43 H 0.1065 0.1831 -0.3860 0.1287 1.0000 Uiso R . . . . . . H61 H 0.1724 -0.2884 -0.1559 0.0484 1.0000 Uiso R . . . . . . H71 H 0.1164 -0.4205 -0.4299 0.0669 1.0000 Uiso R . . . . . . H81 H 0.0350 -0.3641 -0.1898 0.1347 1.0000 Uiso R . . . . . . H82 H 0.0181 -0.5193 -0.2948 0.1347 1.0000 Uiso R . . . . . . H83 H -0.0069 -0.3451 -0.3566 0.1350 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 Mg1 0.0315(6) 0.0208(6) 0.0196(5) -0.0007(5) 0.0046(4) -0.0035(5) O1 0.0611(17) 0.0236(14) 0.0331(13) -0.0005(10) 0.0212(11) -0.0002(11) O2 0.0370(13) 0.0223(12) 0.0181(11) 0.0015(10) 0.0054(10) 0.0019(10) O3 0.0313(12) 0.0291(13) 0.0252(12) 0.0021(11) 0.0055(10) -0.0062(11) O4 0.0534(17) 0.0284(14) 0.0489(15) 0.0184(13) 0.0004(13) -0.0065(13) O5 0.0489(15) 0.0222(13) 0.0355(13) 0.0013(11) 0.0069(11) -0.0090(13) O6 0.0350(13) 0.0360(14) 0.0226(12) -0.0014(11) 0.0064(10) -0.0028(11) O7 0.0338(14) 0.0508(16) 0.0247(12) -0.0115(12) 0.0073(10) -0.0104(12) C1 0.035(2) 0.0232(18) 0.0292(19) 0.0032(15) 0.0064(15) 0.0009(16) C2 0.050(2) 0.032(2) 0.035(2) 0.0042(17) 0.0067(17) -0.0011(18) C3 0.043(2) 0.039(2) 0.065(3) 0.001(2) 0.002(2) 0.002(2) C4 0.059(3) 0.095(4) 0.092(4) 0.000(3) -0.015(3) 0.004(3) C5 0.0307(18) 0.0244(18) 0.0225(18) 0.0023(15) 0.0032(14) -0.0026(15) C6 0.036(2) 0.046(2) 0.042(2) -0.004(2) 0.0166(16) -0.0075(19) C7 0.038(2) 0.067(3) 0.061(3) -0.003(2) 0.0081(19) -0.011(2) C8 0.041(3) 0.108(5) 0.123(5) -0.011(4) 0.024(3) -0.018(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.5074(11) 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 Mg1 . O6 4_545 2.049(2) yes Mg1 . O1 . 2.095(2) yes Mg1 . O2 . 2.129(2) yes Mg1 . O3 . 2.147(2) yes Mg1 . O4 . 1.999(3) yes Mg1 . O7 . 2.018(3) yes O1 . H11 . 0.806 no O1 . H12 . 0.817 no O2 . H21 . 0.840 no O2 . H22 . 0.818 no O3 . H31 . 0.813 no O3 . H32 . 0.821 no O4 . C1 . 1.245(4) yes O5 . C1 . 1.263(4) yes O6 . C5 . 1.254(3) yes O7 . C5 . 1.258(3) yes C1 . C2 . 1.483(5) yes C2 . C3 . 1.290(5) yes C2 . H23 . 0.935 no C3 . C4 . 1.492(5) yes C3 . H33 . 0.930 no C4 . H41 . 0.955 no C4 . H42 . 0.948 no C4 . H43 . 0.966 no C5 . C6 . 1.474(4) yes C6 . C7 . 1.299(5) yes C6 . H61 . 0.928 no C7 . C8 . 1.489(6) yes C7 . H71 . 0.932 no C8 . H81 . 0.968 no C8 . H82 . 0.960 no C8 . H83 . 0.947 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 O6 4_545 Mg1 . O1 . 91.63(10) yes O6 4_545 Mg1 . O2 . 93.44(9) yes O1 . Mg1 . O2 . 88.35(9) yes O6 4_545 Mg1 . O3 . 173.87(11) yes O1 . Mg1 . O3 . 82.36(9) yes O2 . Mg1 . O3 . 85.22(9) yes O6 4_545 Mg1 . O4 . 95.89(11) yes O1 . Mg1 . O4 . 171.02(12) yes O2 . Mg1 . O4 . 86.31(10) yes O3 . Mg1 . O4 . 90.00(11) yes O6 4_545 Mg1 . O7 . 94.63(10) yes O1 . Mg1 . O7 . 92.70(10) yes O2 . Mg1 . O7 . 171.83(10) yes O3 . Mg1 . O7 . 86.89(9) yes O4 . Mg1 . O7 . 91.58(11) yes Mg1 . O1 . H11 . 109.0 no Mg1 . O1 . H12 . 128.3 no H11 . O1 . H12 . 108.8 no Mg1 . O2 . H21 . 113.8 no Mg1 . O2 . H22 . 121.4 no H21 . O2 . H22 . 102.5 no Mg1 . O3 . H31 . 117.0 no Mg1 . O3 . H32 . 111.2 no H31 . O3 . H32 . 106.6 no Mg1 . O4 . C1 . 167.9(2) yes Mg1 4_544 O6 . C5 . 125.7(2) yes Mg1 . O7 . C5 . 153.1(2) yes O5 . C1 . O4 . 121.7(3) yes O5 . C1 . C2 . 118.3(3) yes O4 . C1 . C2 . 120.0(3) yes C1 . C2 . C3 . 124.1(4) yes C1 . C2 . H23 . 117.5 no C3 . C2 . H23 . 118.4 no C2 . C3 . C4 . 125.5(4) yes C2 . C3 . H33 . 117.0 no C4 . C3 . H33 . 117.5 no C3 . C4 . H41 . 109.3 no C3 . C4 . H42 . 108.9 no H41 . C4 . H42 . 110.7 no C3 . C4 . H43 . 107.6 no H41 . C4 . H43 . 110.1 no H42 . C4 . H43 . 110.3 no O7 . C5 . O6 . 122.8(3) yes O7 . C5 . C6 . 117.2(3) yes O6 . C5 . C6 . 120.0(3) yes C5 . C6 . C7 . 124.0(3) yes C5 . C6 . H61 . 117.5 no C7 . C6 . H61 . 118.5 no C6 . C7 . C8 . 125.3(4) yes C6 . C7 . H71 . 116.7 no C8 . C7 . H71 . 118.0 no C7 . C8 . H81 . 110.6 no C7 . C8 . H82 . 109.1 no H81 . C8 . H82 . 109.3 no C7 . C8 . H83 . 110.1 no H81 . C8 . H83 . 108.9 no H82 . C8 . H83 . 108.7 no