# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Christian Serre' _publ_contact_author_email serre@chimie.uvsq.fr _publ_section_title ; Small chemical causes, drastic structural effects : the case of calcium glutarate ; loop_ _publ_author_name 'Stuart Miller' 'Patricia Horcajada' 'Christian Serre' # Attachment '- BioMIL-2.cif' data_XYZPROF3_publ _database_code_depnum_ccdc_archive 'CCDC 775557' #TrackingRef '- BioMIL-2.cif' # start Validation Reply Form _vrf_PLAT306_XYZPROF3_publ ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O4 RESPONSE: No Hydrogen atoms were placed in the refinement as the model was proposed from powder dirrection data. Idealised positions for hydrogen atoms are listed in the supplementary information ; # end Validation Reply Form #============================================================================= # this information describes the project, paper etc. for the CIF # # Acta Cryst. Section C papers and editorial correspondence is generated # # from the information in this section # # # # (from) CIF submission form for Rietveld refinements (Acta Cryst. C) # # Version 14 December 1998 # #============================================================================= #============================================================================= # 5. OVERALL REFINEMENT & COMPUTING DETAILS _refine_special_details ; ? ; _pd_proc_ls_special_details ; ? ; # The following items are used to identify the programs used. _computing_molecular_graphics ? _computing_publication_material ? _refine_ls_weighting_scheme ? _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_number_constraints ? _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? #============================================================================== # 6. SAMPLE PREPARATION DATA # (In the unusual case where multiple samples are used in a single # Rietveld study, this information should be moved into the phase # blocks) # The following three fields describe the preparation of the material. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? _pd_char_colour ? # use ICDD colour descriptions _refine_ls_shift/su_max 0.04 _refine_ls_shift/su_mean 0.01 _computing_structure_refinement GSAS _refine_ls_number_parameters 75 _refine_ls_goodness_of_fit_all 3.66 _refine_ls_number_restraints 10 _refine_ls_matrix_type full #============================================================================== # 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA _pd_char_particle_morphology ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? # If you change Z, be sure to change all 3 of the following _chemical_formula_sum 'C5 Ca O5' _chemical_compound_source ? # for minerals and _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_melting_point ? _exptl_crystal_colour 'white powder' _diffrn_ambient_temperature 293 # natural products _symmetry_space_group_name_Hall 'P 2ac 2ab' _exptl_crystal_F_000 ? _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _cell_measurement_temperature 293 _cell_special_details ; ? ; _geom_special_details ? # The following item identifies the program(s) used (if appropriate). _computing_structure_solution ? #============================================================================== # 8. Phase information from GSAS _pd_phase_name 'from C:/Documents and Settings/Stu/Bureau/hydrated Calcium glutara' _cell_length_a 6.78048(6) _cell_length_b 18.42351(23) _cell_length_c 5.86807(6) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_volume 733.041(16) _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_int_tables_number 19 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 +x+1/2,-y+1/2,-z 3 -x,+y+1/2,-z+1/2 4 -x+1/2,-y,+z+1/2 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity Ca CA1 -0.11707(30) 0.20243(8) 0.4140(4) 1.0 Uiso 0.0060(4) 4 O O5 -0.1182(8) 0.10773(25) 1.1273(8) 1.0 Uiso 0.0120(4) 4 O O1 -0.1536(8) 0.16482(29) 0.8015(7) 1.0 Uiso 0.0120(4) 4 C C5 -0.0940(13) 0.1098(4) 0.9170(15) 1.0 Uiso 0.0167(4) 4 O O2 0.2783(6) -0.18108(30) 0.9551(9) 1.0 Uiso 0.0120(4) 4 O O3 -0.0395(5) -0.18475(29) 0.8915(14) 1.0 Uiso 0.0120(4) 4 O O4 -0.0329(6) 0.27532(25) 0.0998(10) 1.0 Uiso 0.0120(4) 4 C C1 0.1195(14) -0.1480(4) 0.8966(17) 1.0 Uiso 0.0167(4) 4 C C2 0.1250(15) -0.0699(4) 0.7807(14) 1.0 Uiso 0.0167(4) 4 C C3 -0.0005(12) -0.0249(4) 0.9239(13) 1.0 Uiso 0.0167(4) 4 C C4 0.0042(14) 0.0443(4) 0.7932(12) 1.0 Uiso 0.0167(4) 4 _chemical_formula_weight 180.13 _cell_formula_units_Z 4 # MOLECULAR GEOMETRY 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 CA1 CA1 3.9478(17) . 2_456 N CA1 CA1 3.9478(17) . 2_556 N CA1 O5 2.424(5) . 1_554 N CA1 O1 2.390(4) . 1_555 N CA1 O2 2.528(6) . 3_556 N CA1 O2 2.343(5) . 4_554 N CA1 O3 2.598(6) . 3_556 N CA1 O3 2.355(5) . 4_454 N CA1 O4 2.351(6) . 1_555 N CA1 C1 2.972(8) . 3_556 N O5 CA1 2.424(5) . 1_556 N O5 C5 1.246(9) . 1_555 N O1 CA1 2.390(4) . 1_555 N O1 C5 1.284(8) . 1_555 N C5 O5 1.246(9) . 1_555 N C5 O1 1.284(8) . 1_555 N C5 C4 1.559(10) . 1_555 N O2 CA1 2.528(6) . 3_546 N O2 CA1 2.343(5) . 4_555 N O2 C1 1.284(8) . 1_555 N O3 CA1 2.598(6) . 3_546 N O3 CA1 2.355(5) . 4_455 N O3 C1 1.274(9) . 1_555 N O4 CA1 2.351(6) . 1_555 N C1 CA1 2.972(8) . 3_546 N C1 O2 1.284(8) . 1_555 N C1 O3 1.274(9) . 1_555 N C1 C2 1.591(9) . 1_555 N C2 C1 1.591(9) . 1_555 N C2 C3 1.456(11) . 1_555 N C3 C2 1.456(11) . 1_555 N C3 C4 1.487(9) . 1_555 N C4 C5 1.559(10) . 1_555 N C4 C3 1.487(9) . 1_555 N loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 CA1 O1 116.83(18) 1_554 . 1_555 N O5 CA1 O2 145.16(18) 1_554 . 3_556 N O5 CA1 O2 87.35(20) 1_554 . 4_554 N O5 CA1 O3 151.90(21) 1_554 . 3_556 N O5 CA1 O3 81.87(22) 1_554 . 4_454 N O5 CA1 O4 82.40(14) 1_554 . 1_555 N O1 CA1 O2 84.96(16) 1_555 . 3_556 N O1 CA1 O2 87.42(21) 1_555 . 4_554 N O1 CA1 O3 81.74(18) 1_555 . 3_556 N O1 CA1 O3 84.87(23) 1_555 . 4_454 N O1 CA1 O4 159.52(18) 1_555 . 1_555 N O2 CA1 O2 122.35(15) 3_556 . 4_554 N O2 CA1 O3 50.51(8) 3_556 . 3_556 N O2 CA1 O3 72.95(16) 3_556 . 4_454 N O2 CA1 O4 81.86(18) 3_556 . 1_555 N O2 CA1 O3 71.85(17) 4_554 . 3_556 N O2 CA1 O3 162.17(18) 4_554 . 4_454 N O2 CA1 O4 86.48(18) 4_554 . 1_555 N O3 CA1 O3 122.63(15) 3_556 . 4_454 N O3 CA1 O4 77.78(18) 3_556 . 1_555 N O3 CA1 O4 105.97(22) 4_454 . 1_555 N CA1 O5 C5 131.7(5) 1_556 . 1_555 N CA1 O1 C5 134.3(6) 1_555 . 1_555 N O5 C5 O1 120.4(8) 1_555 . 1_555 N O5 C5 C4 119.6(8) 1_555 . 1_555 N O1 C5 C4 120.0(9) 1_555 . 1_555 N CA1 O2 CA1 108.22(21) 3_546 . 4_555 N CA1 O2 C1 97.0(5) 3_546 . 1_555 N CA1 O2 C1 151.0(6) 4_555 . 1_555 N CA1 O3 CA1 105.59(24) 3_546 . 4_455 N CA1 O3 C1 94.0(5) 3_546 . 1_555 N CA1 O3 C1 155.4(5) 4_455 . 1_555 N O2 C1 O3 117.6(7) 1_555 . 1_555 N O2 C1 C2 121.6(10) 1_555 . 1_555 N O3 C1 C2 119.4(9) 1_555 . 1_555 N C1 C2 C3 104.7(8) 1_555 . 1_555 N C2 C3 C4 100.3(8) 1_555 . 1_555 N C5 C4 C3 114.5(9) 1_555 . 1_555 N # Powder diffraction data for histogram 1 #============================================================================== # 9. INSTRUMENT CHARACTERIZATION _exptl_special_details ; ? ; # if regions of the data are excluded, the reason(s) are supplied here: _pd_proc_info_excluded_regions ; ? ; # The following item is used to identify the equipment used to record # the powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; ? ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54056 _diffrn_source ? _diffrn_source_type ? _diffrn_source_target ? _diffrn_measurement_device_type 'Bruker D8' _diffrn_detector ? _diffrn_detector_type ? # make or model of detector _pd_meas_scan_method ? # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following two items identify the program(s) used (if appropriate). _computing_data_collection ? _computing_data_reduction ? # Describe any processing performed on the data, prior to refinement. # For example: a manual Lp correction or a precomputed absorption correction _pd_proc_info_data_reduction ? # The following item is used for angular dispersive measurements only. _diffrn_radiation_monochromator ? # The following items are used to define the size of the instrument. # Not all distances are appropriate for all instrument types. _pd_instr_dist_src/mono ? _pd_instr_dist_mono/spec ? _pd_instr_dist_src/spec ? _pd_instr_dist_spec/anal ? _pd_instr_dist_anal/detc ? _pd_instr_dist_spec/detc ? # 10. Specimen size and mounting information # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection _pd_spec_mounting # This field should be # used to give details of the # container. ; ? ; _pd_spec_mount_mode ? # options are 'reflection' # or 'transmission' _pd_spec_shape ? # options are 'cylinder' # 'flat_sheet' or 'irregular' loop_ _atom_type_symbol _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source Ca 4.0 0.000 0.000 8.62660 10.4421 7.38730 0.65990 1.58990 85.7484 1.02110 178.437 1.37510 International_Tables_Vol_C O 20.0 0.000 0.000 3.04850 13.2771 2.28680 5.70110 1.54630 0.32390 0.86700 32.9089 0.25080 International_Tables_Vol_C C 20.0 0.000 0.000 2.31000 20.8439 1.02000 10.2075 1.58860 0.56870 0.86500 51.6512 0.21560 International_Tables_Vol_C _diffrn_radiation_polarisn_ratio 0.55 _pd_proc_ls_prof_R_factor 0.0204 _pd_proc_ls_prof_wR_factor 0.0286 _pd_proc_ls_prof_wR_expected 0.0079 _refine_ls_R_Fsqd_factor 0.06356 _pd_proc_ls_background_function ; GSAS Background function number 7 with 36 terms. Linear interpolation 1: 11421.3 2: 10014.3 3: 9492.19 4: 9789.68 5: 10649.7 6: 13040.2 7: 15799.3 8: 19514.5 9: 23884.8 10: 26627.8 11: 26288.5 12: 23049.4 13: 19718.8 14: 18518.2 15: 17226.2 16: 16418.0 17: 15356.2 18: 13306.7 19: 11722.6 20: 10233.2 21: 9839.15 22: 9447.89 23: 9119.54 24: 9095.03 25: 8908.06 26: 8689.10 27: 8335.21 28: 8049.42 29: 8001.17 30: 7792.79 31: 7660.23 32: 7553.22 33: 7344.52 34: 7302.52 35: 7262.87 36: 7357.42 ; _exptl_absorpt_process_details ; GSAS Absorption/surface roughness correction: function number 0 No correction is applied. ; _exptl_absorpt_correction_T_min 1.00000 _exptl_absorpt_correction_T_max 1.00000 # Extinction correction _gsas_exptl_extinct_corr_T_min 1.00000 _gsas_exptl_extinct_corr_T_max 1.00000 _pd_proc_ls_profile_function ; CW Profile function number 3 with 19 terms Pseudovoigt profile coefficients as parameterized in P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994). J. Appl. Cryst.,27,892-900. #1(GU) = 114.780 #2(GV) = 40.931 #3(GW) = -7.876 #4(GP) = 2.073 #5(LX) = 3.074 #6(LY) = 0.000 #7(S/L) = 0.0256 #8(H/L) = 0.0253 #9(trns) = 1.46 #10(shft)= -4.0587 #11(stec)= 0.06 #12(ptec)= -0.18 #13(sfec)= 0.00 #14(L11) = -0.195 #15(L22) = -0.021 #16(L33) = -0.097 #17(L12) = 0.066 #18(L13) = 0.082 #19(L23) = 0.032 Peak tails are ignored where the intensity is below 0.0025 times the peak Aniso. broadening axis 0.0 0.0 1.0 ; _pd_proc_ls_peak_cutoff 0.00250 _pd_proc_info_datetime 2009-09-29T17:15:09 _pd_calc_method 'Rietveld Refinement' #---- raw/calc data loop ----- _pd_meas_2theta_range_min 6.0 _pd_meas_2theta_range_max 90.2064 _pd_meas_2theta_range_inc 0.0159 _pd_proc_2theta_range_min 5.91044 _pd_proc_2theta_range_max 90.11684 _pd_proc_2theta_range_inc 0.0159 loop_ _pd_meas_counts_total _pd_proc_ls_weight _pd_proc_intensity_bkg_calc _pd_calc_intensity_total 0.0 0.0 12014.27246 . 0.0 0.0 12004.86035 . 0.0 0.0 11995.44824 . 2.0 0.0 11986.03613 . 0.0 0.0 11976.62402 . 0.0 0.0 11967.21094 . 0.0 0.0 11957.79883 . 0.0 0.0 11948.38672 . 0.0 0.0 11938.97461 . 0.0 0.0 11929.56152 . 12125.0 0.0 11920.14941 . 12070.0 0.0 11910.73828 . 12092.0 0.0 11901.32520 . 12114.0 0.0 11891.91309 . 12003.0 0.0 11882.50098 . 11850.0 0.0 11873.08887 . 12027.0 0.0 11863.67578 . 12045.0 0.0 11854.26367 . 11877.0 0.0 11844.85156 . 12120.0 0.0 11835.43945 . 11912.0 0.0 11826.02734 . 12059.0 0.0 11816.61523 . 11862.0 0.0 11807.20313 . 11904.0 0.0 11797.79004 . 11773.0 0.0 11788.37793 . 11920.0 0.0 11778.96582 . 11863.0 0.0 11769.55371 . 11995.0 0.0 11760.14160 . 11844.0 0.0 11750.72949 . 11812.0 0.0 11741.31738 . 11953.0 0.0 11731.90430 . 11795.0 0.0 11722.49219 . 11803.0 0.0 11713.08008 . 11875.0 0.0 11703.66797 . 11508.0 0.0 11694.25488 . 11499.0 0.0 11684.84277 . 11544.0 0.0 11675.43066 . 11695.0 0.0 11666.01855 . 11669.0 0.0 11656.60645 . 11659.0 0.0 11647.19434 . 11458.0 0.0 11637.78223 . 11736.0 0.0 11628.36914 . 11596.0 0.0 11618.95703 . 11852.0 0.0 11609.54492 . 11497.0 0.0 11600.13281 . 11492.0 0.0 11590.72070 . 11677.0 0.0 11581.30859 . 11500.0 0.0 11571.89648 . 11522.0 0.0 11562.48340 . 11546.0 0.0 11553.07129 . 11333.0 0.0 11543.65918 . 11655.0 0.0 11534.24707 . 11524.0 0.0 11524.83496 . 11649.0 0.0 11515.42285 . 11493.0 0.0 11506.01074 . 11567.0 0.0 11496.59766 . 11334.0 0.0 11487.18555 . 11413.0 0.0 11477.77344 . 11521.0 0.0 11468.36133 . 11588.0 0.0 11458.94824 . 11395.0 0.0 11449.53613 . 11381.0 0.0 11440.12402 . 11467.0 0.0 11430.71191 . 11555.0 0.0000865 11421.29980 11421.29980 11378.0 0.0000879 11411.88770 11411.88770 11418.0 0.0000876 11402.47559 11402.47559 11294.0 0.0000885 11393.06250 11393.06250 11358.0 0.0000880 11383.65039 11383.65039 11274.0 0.0000887 11374.23828 11374.23828 11308.0 0.0000884 11364.82617 11364.82617 11279.0 0.0000887 11355.41406 11355.41406 11404.0 0.0000877 11346.00195 11346.00195 11265.0 0.0000888 11336.58984 11336.58984 11276.0 0.0000887 11327.17676 11327.17676 11437.0 0.0000874 11317.76465 11317.76465 11242.0 0.0000890 11308.35254 11308.35254 11269.0 0.0000887 11298.94043 11298.94043 11245.0 0.0000889 11289.52734 11289.52734 11167.0 0.0000895 11280.11523 11280.11523 11430.0 0.0000875 11270.70313 11270.70313 11197.0 0.0000893 11261.29102 11261.29102 11280.0 0.0000887 11251.87891 11251.87891 11156.0 0.0000896 11242.46680 11242.46680 11104.0 0.0000901 11233.05469 11233.05469 11192.0 0.0000893 11223.64160 11223.64160 11174.0 0.0000895 11214.22949 11214.22949 11097.0 0.0000901 11204.81738 11204.81738 11089.0 0.0000902 11195.40527 11195.40527 11204.0 0.0000893 11185.99316 11185.99316 11092.0 0.0000902 11176.58105 11176.58105 11175.0 0.0000895 11167.16895 11167.16895 11196.0 0.0000893 11157.75586 11157.75586 11163.0 0.0000896 11148.34375 11148.34375 11060.0 0.0000904 11138.93164 11138.93164 11109.0 0.0000900 11129.51953 11129.51953 10865.0 0.0000920 11120.10645 11120.10645 11039.0 0.0000906 11110.69434 11110.69434 11207.0 0.0000892 11101.28223 11101.28223 10924.0 0.0000915 11091.87012 11091.87012 10961.0 0.0000912 11082.45801 11082.45801 10931.0 0.0000915 11073.04590 11073.04590 10961.0 0.0000912 11063.63281 11063.63281 11071.0 0.0000903 11054.22070 11054.22070 10796.0 0.0000926 11044.80859 11044.80859 10893.0 0.0000918 11035.39648 11035.39648 10773.0 0.0000928 11025.98438 11025.98438 10879.0 0.0000919 11016.57227 11016.57227 11023.0 0.0000907 11007.16016 11007.16016 10929.0 0.0000915 10997.74805 10997.74805 11084.0 0.0000902 10988.33496 10988.33496 10890.0 0.0000918 10978.92285 10978.92285 11062.0 0.0000904 10969.51074 10969.51074 10888.0 0.0000918 10960.09863 10960.09863 10987.0 0.0000910 10950.68555 10950.68555 10930.0 0.0000915 10941.27344 10941.27344 10753.0 0.0000930 10931.86133 10931.86133 10782.0 0.0000927 10922.44922 10922.44922 10799.0 0.0000926 10913.03711 10913.03711 10741.0 0.0000931 10903.62500 10903.62500 10820.0 0.0000924 10894.21191 10894.21191 10879.0 0.0000919 10884.79980 10884.79980 10910.0 0.0000917 10875.38770 10875.38770 10888.0 0.0000918 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0.0001232 7276.26855 8254.34570 7812.0 0.0001280 7276.00342 8256.74219 8090.0 0.0001236 7275.73779 8259.01563 7786.0 0.0001284 7275.47266 8261.03906 8046.0 0.0001243 7275.20752 8262.86230 8032.0 0.0001245 7274.94238 8264.76270 8152.0 0.0001227 7274.67725 8267.23535 8326.0 0.0001201 7274.41211 8270.91504 7972.0 0.0001254 7274.14648 8276.37695 8212.0 0.0001218 7273.88135 8284.43164 8304.0 0.0001204 7273.61621 8295.28418 8274.0 0.0001209 7273.35107 8308.81836 7970.0 0.0001255 7273.08545 8325.45703 8178.0 0.0001223 7272.82031 8345.66504 8290.0 0.0001206 7272.55566 8368.59082 8250.0 0.0001212 7272.29004 8394.70605 8610.0 0.0001161 7272.02490 8424.39746 8350.0 0.0001198 7271.75928 8456.94727 8580.0 0.0001166 7271.49414 8491.00488 8624.0 0.0001160 7271.22900 8530.35840 8598.0 0.0001163 7270.96387 8573.09570 8624.0 0.0001160 7270.69824 8619.06152 8548.0 0.0001170 7270.43311 8667.85547 8634.0 0.0001158 7270.16797 8718.92480 8924.0 0.0001121 7269.90283 8771.38965 8726.0 0.0001146 7269.63770 8823.98535 8596.0 0.0001163 7269.37256 8874.92871 8800.0 0.0001136 7269.10693 8922.11426 8962.0 0.0001116 7268.84180 8962.74609 9160.0 0.0001092 7268.57666 8994.03809 8740.0 0.0001144 7268.31104 9013.15234 9116.0 0.0001097 7268.04639 9017.67578 8994.0 0.0001112 7267.78076 9005.69922 9018.0 0.0001109 7267.51563 8976.37988 8946.0 0.0001118 7267.25049 8929.84277 8920.0 0.0001121 7266.98486 8867.35840 8732.0 0.0001145 7266.71973 8791.03125 8776.0 0.0001139 7266.45459 8703.68945 8512.0 0.0001175 7266.18945 8608.57813 8438.0 0.0001185 7265.92432 8501.94336 8250.0 0.0001212 7265.65869 8402.06738 8058.0 0.0001241 7265.39355 8305.11523 7994.0 0.0001251 7265.12842 8213.98535 8026.0 0.0001246 7264.86328 8131.30322 7994.0 0.0001251 7264.59814 8059.26367 7928.0 0.0001261 7264.33252 8000.02832 8040.0 0.0001244 7264.06738 7954.13965 7830.0 0.0001277 7263.80225 7924.34570 8066.0 0.0001240 7263.53711 7908.87744 8068.0 0.0001239 7263.27197 7909.45654 8046.0 0.0001243 7263.00635 7926.32275 8138.0 0.0001229 7263.17725 7959.81787 8044.0 0.0001243 7263.81006 8008.33545 8136.0 0.0001229 7264.44238 8073.64941 8318.0 0.0001202 7265.07520 8152.84424 8802.0 0.0001136 7265.70752 8244.06641 8672.0 0.0001153 7266.33984 8344.86914 8600.0 0.0001163 7266.97217 8452.23340 8862.0 0.0001128 7267.60449 8562.64844 8966.0 0.0001115 7268.23730 8672.35742 9110.0 0.0001098 7268.87012 8777.34277 9226.0 0.0001084 7269.50244 8874.01953 9272.0 0.0001079 7270.13477 8959.17383 9422.0 0.0001061 7270.76758 9030.17773 9532.0 0.0001049 7271.39941 9084.95801 9754.0 0.0001025 7272.03271 9122.15723 9744.0 0.0001026 7272.66504 9140.81641 9760.0 0.0001025 7273.29736 9140.89746 9306.0 0.0001075 7273.92969 9123.14941 9356.0 0.0001069 7274.56250 9089.15137 8966.0 0.0001115 7275.19482 9041.18945 9122.0 0.0001096 7275.82764 8981.97754 9078.0 0.0001102 7276.45996 8914.55078 9012.0 0.0001110 7277.09277 8841.77930 8724.0 0.0001146 7277.72510 8766.26953 8560.0 0.0001168 7278.35742 8689.86035 8380.0 0.0001193 7278.98926 8614.77539 8570.0 0.0001167 7279.62256 8541.49316 8286.0 0.0001207 7280.25488 8471.12305 8478.0 0.0001180 7280.88770 8402.92969 8552.0 0.0001169 7281.52002 8334.07910 8302.0 0.0001205 7282.15234 8270.51563 8130.0 0.0001230 7282.78516 8209.21582 8012.0 0.0001248 7283.41699 8150.27344 8040.0 0.0001244 7284.04980 8093.96191 8028.0 0.0001246 7284.68262 8040.87158 8134.0 0.0001229 7285.31494 7991.70801 7834.0 0.0001276 7285.94727 7947.38672 7772.0 0.0001287 7286.58008 7908.92725 7784.0 0.0001285 7287.21191 7877.73975 7976.0 0.0001254 7287.84521 7854.13965 7680.0 0.0001302 7288.47754 7839.49756 7698.0 0.0001299 7289.10986 7834.81592 7900.0 0.0001266 7289.74219 7840.52197 8086.0 0.0001237 7290.37500 7857.49658 7900.0 0.0001266 7291.00732 7886.16357 7964.0 0.0001256 7291.64014 7927.05176 8094.0 0.0001235 7292.27246 7980.42578 8294.0 0.0001206 7292.90527 8046.50000 7934.0 0.0001260 7293.53760 8125.27588 8272.0 0.0001209 7294.16992 8216.54102 8460.0 0.0001182 7294.80176 8319.71973 8374.0 0.0001194 7295.43506 8434.24707 8302.0 0.0001205 7296.06738 8558.54395 8710.0 0.0001148 7296.70020 8691.06250 8654.0 0.0001156 7297.33252 8830.74902 8820.0 0.0001134 7297.96484 8972.68555 9230.0 0.0001083 7298.59766 9113.44336 9194.0 0.0001088 7299.22949 9252.18066 9092.0 0.0001100 7299.86279 9381.95605 9164.0 0.0001091 7300.49512 9498.54785 9298.0 0.0001076 7301.12744 9597.28223 9650.0 0.0001036 7301.75977 9673.69238 9926.0 0.0001007 7302.39258 9723.91406 9850.0 0.0001015 7303.02441 9744.90918 9778.0 0.0001023 7303.65771 9734.87109 9548.0 0.0001047 7304.29004 9692.74512 9640.0 0.0001037 7304.92285 9620.54102 9460.0 0.0001057 7305.55469 9518.15723 9034.0 0.0001107 7306.18750 9390.37012 8944.0 0.0001118 7306.81982 9242.04199 8526.0 0.0001173 7307.45264 9079.21191 8324.0 0.0001201 7308.08496 8907.34473 8248.0 0.0001212 7308.71777 8732.63867 8088.0 0.0001236 7309.35010 8560.59766 7938.0 0.0001260 7309.98242 8395.90332 7958.0 0.0001257 7310.61426 8242.39746 7792.0 0.0001283 7311.24805 8102.48389 7672.0 0.0001303 7311.87988 7978.38477 7636.0 0.0001310 7312.51270 7870.82910 7588.0 0.0001318 7313.14502 7779.96045 7608.0 0.0001314 7313.77734 7705.37744 7436.0 0.0001345 7314.41016 7646.06348 7678.0 0.0001302 7315.04248 7600.83838 7436.0 0.0001345 7315.67529 7568.27148 7600.0 0.0001316 7316.30762 7546.87500 7692.0 0.0001300 7316.93994 7535.08691 7482.0 0.0001337 7317.57227 7529.76123 7718.0 0.0001296 7318.20508 7532.70850 7488.0 0.0001335 7318.83691 7540.86816 7518.0 0.0001330 7319.47021 7552.94336 7552.0 0.0001324 7320.10254 7567.64258 7864.0 0.0001272 7320.73535 7583.78223 7854.0 0.0001273 7321.36768 7600.08594 7886.0 0.0001268 7322.00000 7615.84326 7760.0 0.0001289 7322.63232 7629.94434 7860.0 0.0001272 7323.26514 7641.56494 8088.0 0.0001236 7323.89746 7650.00684 7866.0 0.0001271 7324.53027 7655.08838 7822.0 0.0001278 7325.16260 7655.98926 7922.0 0.0001262 7325.79492 7653.02344 7626.0 0.0001311 7326.42676 7646.53076 7986.0 0.0001252 7327.06055 7637.08936 7872.0 0.0001270 7327.69287 7625.59717 7796.0 0.0001283 7328.32520 7613.09180 7628.0 0.0001311 7328.95752 7601.92480 7664.0 0.0001305 7329.58984 7591.17334 7600.0 0.0001316 7330.22266 7583.32275 7504.0 0.0001333 7330.85498 7579.48193 7698.0 0.0001299 7331.48779 7581.66455 7780.0 0.0001285 7332.12012 7590.87744 7528.0 0.0001328 7332.75293 7608.32324 7780.0 0.0001285 7333.38477 7635.00342 7720.0 0.0001295 7334.01758 7671.68018 7724.0 0.0001295 7334.64941 7718.73340 7940.0 0.0001259 7335.28271 7776.30615 7852.0 0.0001274 7335.91504 7843.76904 7946.0 0.0001258 7336.54785 7920.19873 8224.0 0.0001216 7337.18018 8004.07031 8290.0 0.0001206 7337.81250 8093.31201 8096.0 0.0001235 7338.44482 8185.37305 8354.0 0.0001197 7339.07764 8277.36426 8400.0 0.0001190 7339.70996 8365.96484 8402.0 0.0001190 7340.34277 8447.93457 8760.0 0.0001142 7340.97510 8519.03125 8956.0 0.0001117 7341.60742 8578.56641 9004.0 0.0001111 7342.23926 8623.14160 9012.0 0.0001110 7342.87305 8651.29395 8926.0 0.0001120 7343.50537 8662.26855 8826.0 0.0001133 7344.13770 8656.39648 8712.0 0.0001148 7344.77002 8634.88477 8470.0 0.0001181 7345.40234 8600.04199 8496.0 0.0001177 7346.03516 8554.11133 8340.0 0.0001199 7346.66748 8500.04199 8212.0 0.0001218 7347.30029 8441.69043 8264.0 0.0001210 7347.93262 8381.24219 8026.0 0.0001246 7348.56543 8322.02734 8134.0 0.0001229 7349.19727 8266.48730 7928.0 0.0001261 7349.83008 8216.54688 7878.0 0.0001269 7350.46191 8173.59082 8220.0 0.0001217 7351.09521 8138.31396 8110.0 0.0001233 7351.72754 8111.22705 7942.0 0.0001259 7352.36035 8091.83691 7950.0 0.0001258 7352.99268 8079.74463 8064.0 0.0001240 7353.62500 8074.22412 8022.0 0.0001247 7354.25732 8074.48096 8020.0 0.0001247 7354.89014 8079.79150 8204.0 0.0001219 7355.52246 8089.56641 7942.0 0.0001259 7356.15527 8103.39111 8164.0 0.0001225 7356.78760 8120.99707 8078.0 0.0001238 7357.41992 8142.18701 8166.0 . . . _pd_meas_number_of_points 5297 _pd_proc_number_of_points 5297 loop_ _refln_index_h _refln_index_k _refln_index_l _refln_observed_status _refln_F_squared_meas _refln_F_squared_calc _refln_phase_calc _refln_d_spacing _gsas_i100_meas 0 2 0 o 7704.931 7755.509 180.00 9.21176 100.00 1 1 0 o 313.029 338.351 -90.00 6.36321 3.87 0 1 1 o 4120.383 4206.145 -90.00 5.59131 38.99 1 2 0 o 1175.289 1214.230 90.00 5.46068 10.60 0 2 1 o 1538.219 1585.341 -180.00 4.94920 11.17 0 4 0 o 182.911 180.897 180.00 4.60588 0.54 1 3 0 o 1655.775 1648.903 90.00 4.55174 10.27 1 0 1 o 1048.648 1008.631 -90.00 4.43714 5.80 1 1 1 o 2133.618 2059.073 -3.80 4.31379 22.68 0 3 1 o 2359.639 2439.209 90.00 4.24262 12.59 1 2 1 o 3145.911 3084.864 -54.80 3.99756 28.91 1 4 0 o 65.252 43.663 -90.00 3.80999 0.36 0 4 1 o 355.787 353.175 0.00 3.62311 1.42 1 3 1 o 919.982 880.916 -52.24 3.59658 7.00 2 0 0 o 3978.815 3931.666 0.00 3.39024 6.45 2 1 0 o 13826.246 13570.735 0.00 3.33426 44.02 1 5 0 o 341.140 202.242 -90.00 3.23754 1.09 1 4 1 o 567.954 581.411 46.96 3.19552 3.42 2 2 0 o 53.095 68.502 0.00 3.18161 0.14 0 5 1 o 298.855 445.675 90.00 3.12051 0.81 0 6 0 o 2186.955 2125.052 0.00 3.07059 2.90 2 3 0 o 381.743 217.681 0.00 2.96801 0.90 2 0 1 o 28.061 32.492 90.00 2.93553 0.13 0 0 2 o 1050.900 1169.053 0.00 2.93404 1.30 2 1 1 o 730.573 738.011 39.18 2.89896 3.40 0 1 2 o 4319.117 4397.941 -90.00 2.89752 10.06 1 5 1 o 2709.940 2830.055 159.75 2.83472 12.32 1 6 0 o 77.039 69.234 -90.00 2.79713 0.17 2 2 1 o 837.407 748.635 -96.66 2.79695 3.80 0 2 2 o 2561.784 2308.325 180.00 2.79565 5.57 2 4 0 o 1227.701 1286.353 0.00 2.73034 2.50 0 6 1 o 208.113 315.926 -180.00 2.72062 0.47 1 0 2 o 118.496 161.598 -180.00 2.69275 0.28 1 1 2 o 120.277 82.748 -179.21 2.66444 0.46 2 3 1 o 104.710 99.937 -91.58 2.64850 0.41 0 3 2 o 7900.721 7638.988 90.00 2.64741 15.30 1 2 2 o 612.167 725.712 0.87 2.58458 2.34 1 6 1 o 2670.460 2688.702 -149.51 2.52495 9.34 2 5 0 o 249.031 121.602 180.00 2.49488 0.41 2 4 1 o 1363.345 1253.846 61.65 2.47550 4.55 1 3 2 o 400.354 524.295 -118.18 2.46610 1.33 0 4 2 o 271.218 251.473 0.00 2.47460 0.46 1 7 0 o 25.950 244.493 90.00 2.45357 0.09 0 7 1 o 10062.160 9376.765 -90.00 2.40145 15.55 1 4 2 o 275.092 418.927 -157.97 2.32462 0.84 2 5 1 o 62.660 61.346 157.35 2.29598 0.17 0 5 2 o 12169.954 11646.820 -90.00 2.29526 17.18 0 8 0 o 5475.605 4862.655 180.00 2.30294 3.90 2 6 0 o 289.033 251.752 -180.00 2.27587 0.39 1 7 1 o 3097.149 3005.215 -15.87 2.26366 8.48 3 1 0 o 1167.896 1103.556 -90.00 2.24334 1.56 2 0 2 o 0.740 0.524 0.00 2.21857 0.00 2 1 2 o 435.753 559.713 -71.21 2.20266 1.13 3 2 0 o 2909.258 3059.350 -90.00 2.19505 3.71 1 5 2 o 82.831 102.748 105.51 2.17408 0.19 1 8 0 o 387.976 590.055 -90.00 2.18060 0.52 2 2 2 o 969.857 1098.011 -97.07 2.15690 2.42 0 8 1 o 969.411 832.078 0.00 2.14376 1.18 2 6 1 o 309.258 288.982 60.68 2.12187 0.73 0 6 2 o 317.977 304.277 0.00 2.12131 0.37 3 3 0 o 4596.220 4426.304 90.00 2.12107 5.44 3 0 1 o 142.427 141.925 -90.00 2.10912 0.17 2 3 2 o 483.736 414.340 172.04 2.08658 1.11 2 7 0 o 41.937 24.382 -180.00 2.07898 0.05 3 1 1 o 1006.559 1045.439 69.57 2.09544 2.35 3 2 1 o 273.321 237.457 -148.89 2.05592 0.62 1 8 1 o 1054.869 994.787 31.49 2.04403 2.28 1 6 2 o 188.957 214.789 -176.85 2.02454 0.41 3 4 0 o 5628.302 5829.579 90.00 2.02903 6.00 2 4 2 o 2315.172 2354.113 86.14 1.99878 4.88 3 3 1 o 721.516 744.138 -106.22 1.99476 1.50 2 7 1 o 1287.501 1166.136 -152.51 1.95963 2.55 1 9 0 o 1195.353 1076.213 -90.00 1.95969 1.17 0 7 2 o 2194.274 1961.151 90.00 1.95919 2.20 0 1 3 o 658.331 555.957 -90.00 1.94509 0.62 3 5 0 o 1675.643 1502.135 -90.00 1.92660 1.63 0 9 1 o 2438.321 2327.434 90.00 1.93283 2.37 3 4 1 o 4120.064 4226.500 -11.97 1.91763 7.76 2 5 2 o 657.751 648.590 -73.93 1.90064 1.20 0 2 3 o 3865.379 3970.393 -180.00 1.91337 3.62 2 8 0 o 25.502 24.973 0.00 1.90499 0.02 1 7 2 o 802.432 871.365 60.07 1.88219 1.47 1 0 3 o 1515.778 1678.575 90.00 1.87939 1.40 1 1 3 o 1528.510 1611.616 127.75 1.86968 2.74 1 9 1 o 550.086 750.016 -147.64 1.85878 0.99 0 3 3 o 45.535 56.998 -90.00 1.86377 0.04 1 2 3 o 1491.055 1448.811 -109.01 1.84145 2.58 3 5 1 o 2336.908 2081.006 3.07 1.83047 3.93 3 6 0 o 1634.503 1489.304 -90.00 1.82023 1.37 0 10 0 o 3028.826 2952.401 0.00 1.84235 1.33 2 8 1 o 1145.519 965.873 -107.54 1.81191 1.91 2 6 2 o 1536.733 1641.336 -94.46 1.79829 2.58 0 8 2 o 49.744 40.448 180.00 1.81156 0.05 1 3 3 o 402.019 437.155 -45.87 1.79712 0.66 0 4 3 o 4563.040 4800.718 0.00 1.80040 3.75 3 0 2 o 860.247 918.668 -180.00 1.79051 0.72 3 1 2 o 2401.930 2577.623 -159.83 1.78211 3.83 1 10 0 o 3.641 3.074 90.00 1.77789 0.00 3 2 2 o 1284.616 1305.878 -23.73 1.75762 2.01 2 9 0 o 950.710 981.167 -180.00 1.75239 0.76 1 8 2 o 1507.305 1502.781 -51.95 1.75017 2.30 0 10 1 o 100.733 104.404 0.00 1.75775 0.07 3 6 1 o 4562.786 4370.496 -178.68 1.73851 6.82 1 4 3 o 590.341 586.866 115.28 1.74010 0.89 0 5 3 o 58.828 46.748 90.00 1.72768 0.04 3 3 2 o 2250.679 2161.286 26.10 1.71894 3.27 3 7 0 o 640.276 614.238 90.00 1.71468 0.48 2 7 2 o 356.513 383.489 117.34 1.69631 0.50 1 10 1 o 1391.014 1493.737 113.68 1.70151 1.98 2 0 3 o 180.171 190.160 90.00 1.69426 0.12 2 1 3 o 189.450 269.217 45.09 1.68714 0.27 2 9 1 o 436.308 443.844 -9.50 1.67911 0.61 4 0 0 o 2097.448 2223.350 180.00 1.69512 0.76 3 4 2 o 186.353 151.950 -162.33 1.66885 0.26 1 5 3 o 177.571 171.169 71.64 1.67419 0.24 0 9 2 o 48.295 48.419 90.00 1.67883 0.03 4 1 0 o 150.516 215.532 0.00 1.68799 0.11 2 2 3 o 35.032 30.590 -93.71 1.66631 0.05 4 2 0 o 905.739 756.274 0.00 1.66713 0.63 3 7 1 o 454.815 377.939 152.72 1.64586 0.61 0 6 3 o 2606.963 2390.228 -180.00 1.64973 1.75 2 3 3 o 1653.160 1655.102 -170.55 1.63324 2.18 1 9 2 o 988.484 986.164 -136.68 1.62962 1.29 4 3 0 o 42.897 43.441 -180.00 1.63401 0.03 1 11 0 o 90.896 95.645 -90.00 1.62599 0.06 2 10 0 o 28.846 26.309 0.00 1.61877 0.02 3 5 2 o 280.550 296.446 -92.08 1.61044 0.36 4 0 1 o 19.265 19.350 -90.00 1.62853 0.01 3 8 0 o 475.108 473.099 90.00 1.61309 0.30 4 1 1 o 422.219 446.936 81.04 1.62221 0.58 1 6 3 o 511.039 558.743 -52.65 1.60297 0.62 2 8 2 o 419.081 358.888 45.35 1.59776 0.53 0 11 1 o 603.180 639.576 -90.00 1.61055 0.40 4 2 1 o 371.205 423.212 -1.10 1.60366 0.47 2 4 3 o 304.548 303.361 -140.19 1.59009 0.36 4 4 0 o 1044.662 1085.876 0.00 1.59080 0.61 0 7 3 o 23.462 24.525 -90.00 1.56994 0.01 4 3 1 o 1172.324 1304.759 -96.98 1.57413 1.41 1 11 1 o 1648.215 1617.741 70.03 1.56695 1.92 2 10 1 o 348.950 339.858 44.03 1.56048 0.44 3 8 1 o 471.284 369.816 33.51 1.55539 0.56 0 10 2 o 1836.145 1801.172 0.00 1.56026 1.07 3 6 2 o 1594.886 1765.115 -127.84 1.54675 1.81 2 5 3 o 1680.456 1623.759 -29.81 1.53933 1.94 4 4 1 o 34.180 31.194 -9.24 1.53538 0.04 4 5 0 o 138.989 137.124 0.00 1.53997 0.08 1 7 3 o 143.404 80.623 112.39 1.52947 0.16 1 10 2 o 530.808 479.532 -161.41 1.52052 0.60 0 12 0 o 1088.811 1006.601 180.00 1.53529 0.32 3 9 0 o 381.569 276.418 -90.00 1.51725 0.21 2 9 2 o 285.317 233.750 -118.43 1.50447 0.31 2 11 0 o 1263.640 1226.594 0.00 1.50162 0.70 0 8 3 o 231.193 207.532 -180.00 1.49084 0.11 4 5 1 o 243.301 205.238 86.95 1.48954 0.25 1 12 0 o 614.407 934.341 90.00 1.49739 0.33 2 6 3 o 112.490 108.009 156.96 1.48342 0.11 3 7 2 o 1426.966 1480.480 147.48 1.48041 1.47 4 6 0 o 34.739 32.726 0.00 1.48400 0.02 3 0 3 o 1631.753 1689.925 -90.00 1.47905 0.85 3 1 3 o 2456.368 2770.562 79.59 1.47430 2.55 0 12 1 o 940.151 823.360 -180.00 1.48530 0.48 3 9 1 o 514.767 545.870 -110.53 1.46894 0.53 0 0 4 o 2723.960 2758.113 180.00 1.46702 0.69 1 8 3 o 656.366 538.525 -96.07 1.45606 0.66 3 2 3 o 503.284 441.077 134.27 1.46034 0.51 4 0 2 o 3.483 3.626 0.00 1.46777 0.00 2 11 1 o 55.978 44.756 -119.46 1.45474 0.05 4 1 2 o 346.335 357.000 -6.34 1.46313 0.34 0 1 4 o 247.003 244.465 -90.00 1.46239 0.12 1 12 1 o 490.818 419.023 -78.97 1.45089 0.49 0 11 2 o 7.669 5.799 -90.00 1.45456 0.00 4 2 2 o 43.486 40.482 -10.86 1.44948 0.05 0 2 4 o 1147.056 1119.479 0.00 1.44876 0.57 4 6 1 o 561.827 583.480 31.86 1.43871 0.55 3 3 3 o 1129.188 1132.817 -119.84 1.43793 1.09 2 7 3 o 272.347 294.891 135.84 1.42460 0.29 3 10 0 o 18.424 18.203 -90.00 1.42803 0.01 1 0 4 o 60.853 40.776 180.00 1.43384 0.03 1 1 4 o 305.752 289.135 61.77 1.42952 0.30 4 3 2 o 817.873 815.788 -95.91 1.42756 0.79 0 3 4 o 1533.768 1545.592 90.00 1.42687 0.74 1 11 2 o 228.555 270.536 30.60 1.42220 0.23 4 7 0 o 258.891 274.965 -180.00 1.42512 0.12 3 8 2 o 1634.661 1633.031 16.54 1.41354 1.53 2 10 2 o 61.929 68.972 -58.37 1.41736 0.06 1 2 4 o 13.648 16.289 -60.70 1.41678 0.02 0 9 3 o 25.941 27.170 -90.00 1.41421 0.01 3 4 3 o 6.450 3.897 157.65 1.40822 0.01 4 4 2 o 54.045 48.864 165.02 1.39847 0.05 2 12 0 o 677.531 627.798 180.00 1.39857 0.30 0 4 4 o 0.046 0.074 0.00 1.39783 0.00 1 3 4 o 264.049 291.568 -119.07 1.39629 0.25 3 10 1 o 695.527 673.781 -67.38 1.38753 0.62 4 7 1 o 103.711 105.616 47.73 1.38486 0.10 1 9 3 o 885.108 890.228 -61.47 1.38441 0.80 3 5 3 o 65.380 48.675 107.81 1.37260 0.06 1 13 0 o 744.292 757.196 90.00 1.38722 0.33 2 8 3 o 276.687 289.560 158.24 1.36472 0.23 1 4 4 o 268.281 222.655 -139.17 1.36904 0.23 4 8 0 o 83.576 90.039 0.00 1.36517 0.04 0 13 1 o 186.230 165.606 90.00 1.37759 0.09 4 5 2 o 463.575 487.693 106.89 1.36357 0.43 2 12 1 o 924.576 990.374 -115.18 1.36046 0.82 0 5 4 o 1867.451 1972.422 -90.00 1.36297 0.82 0 12 2 o 418.485 462.306 180.00 1.36031 0.18 3 9 2 o 599.517 529.037 -0.63 1.34771 0.51 1 13 1 o 276.472 188.371 -113.50 1.35001 0.23 3 11 0 o 1380.781 1489.952 -90.00 1.34566 0.57 2 0 4 o 714.959 745.681 180.00 1.34637 0.29 2 11 2 o 1281.074 1224.495 17.89 1.33672 1.05 5 1 0 o 197.739 94.275 90.00 1.35244 0.08 2 1 4 o 842.828 916.049 -172.53 1.34279 0.71 0 10 3 o 144.542 148.234 0.00 1.34113 0.06 3 6 3 o 510.921 518.909 -70.11 1.33252 0.41 1 5 4 o 59.227 56.200 113.73 1.33624 0.05 1 12 2 o 333.743 328.407 20.06 1.33374 0.28 2 2 4 o 488.184 502.774 -29.46 1.33222 0.40 4 8 1 o 806.626 833.936 -158.13 1.32966 0.66 5 2 0 o 400.220 417.918 -90.00 1.34164 0.17 4 6 2 o 77.602 74.833 -47.86 1.32425 0.06 0 6 4 o 3.721 3.530 180.00 1.32370 0.00 1 10 3 o 437.180 390.584 93.18 1.31564 0.37 3 11 1 o 1189.527 1130.804 58.44 1.31161 0.94 2 3 4 o 40.276 35.621 32.88 1.31514 0.04 5 3 0 o 732.023 703.359 -90.00 1.32419 0.30 5 0 1 o 400.514 370.971 -90.00 1.32127 0.16 2 9 3 o 207.808 315.915 -44.60 1.30520 0.17 5 1 1 o 117.953 109.841 90.63 1.31789 0.09 4 9 0 o 10.164 15.983 180.00 1.30560 0.00 0 14 0 o 172.547 154.398 180.00 1.31597 0.03 2 13 0 o 483.387 611.586 180.00 1.30755 0.20 1 6 4 o 333.971 362.920 24.07 1.29918 0.25 5 2 1 o 23.835 30.154 135.02 1.30789 0.02 3 7 3 o 786.199 703.714 78.55 1.28940 0.60 2 4 4 o 527.287 412.057 99.76 1.29229 0.42 5 4 0 o 468.425 595.295 90.00 1.30088 0.20 3 10 2 o 1036.463 1149.587 -167.83 1.28402 0.80 4 7 2 o 222.095 249.913 -61.03 1.28190 0.19 5 3 1 o 6.196 3.818 46.71 1.29171 0.01 1 14 0 o 1461.064 1165.185 -90.00 1.29186 0.56 4 9 1 o 390.028 378.891 -119.87 1.27443 0.31 0 7 4 o 638.453 713.625 90.00 1.28140 0.25 2 13 1 o 171.720 167.760 -164.50 1.27625 0.13 4 0 3 o 26.625 29.382 90.00 1.28102 0.01 4 1 3 o 21.477 21.926 -172.42 1.27793 0.02 0 14 1 o 643.313 728.615 0.00 1.28407 0.25 3 12 0 o 1243.447 1203.986 -90.00 1.27000 0.45 0 13 2 o 230.661 223.730 90.00 1.27613 0.09 0 11 3 o 8.911 8.725 -90.00 1.27221 0.00 4 2 3 o 346.377 325.199 -15.96 1.26881 0.27 2 5 4 o 65.588 56.907 -49.78 1.26460 0.05 5 4 1 o 127.584 123.513 -128.80 1.27005 0.10 5 5 0 o 638.103 622.452 90.00 1.27264 0.24 2 12 2 o 118.752 120.858 86.41 1.26248 0.08 1 7 4 o 454.489 447.056 -115.74 1.25912 0.33 1 14 1 o 487.732 531.022 37.01 1.26165 0.37 1 13 2 o 478.973 462.497 161.63 1.25411 0.35 4 3 3 o 28.101 27.225 29.71 1.25402 0.02 2 10 3 o 17.289 17.322 90.19 1.24709 0.01 1 11 3 o 530.341 477.930 109.51 1.25039 0.39 3 8 3 o 844.905 848.511 93.86 1.24449 0.60 4 10 0 o 1160.416 1153.384 180.00 1.24744 0.43 3 12 1 o 879.649 861.973 116.65 1.24126 0.62 4 8 2 o 228.802 243.148 91.52 1.23775 0.16 5 5 1 o 1272.646 1255.975 -6.88 1.24373 0.92 4 4 3 o 1762.159 1905.238 176.56 1.23417 1.26 5 6 0 o 414.457 407.449 -90.00 1.24050 0.16 0 8 4 o 2.122 2.462 180.00 1.23730 0.00 2 6 4 o 417.079 442.385 -110.98 1.23305 0.31 3 1 4 o 721.129 725.529 149.65 1.22780 0.51 3 0 4 o 1255.581 1235.409 -180.00 1.23053 0.44 3 11 2 o 779.423 572.982 -146.27 1.22315 0.53 2 14 0 o 0.335 0.320 -180.00 1.22679 0.00 4 10 1 o 175.807 177.144 -7.86 1.22017 0.12 5 0 2 o 172.732 170.926 0.00 1.23097 0.06 1 8 4 o 488.951 483.914 76.16 1.21720 0.34 5 1 2 o 489.294 500.599 174.56 1.22823 0.36 3 2 4 o 587.785 616.813 44.47 1.21970 0.41 5 2 2 o 577.722 600.269 -147.58 1.22013 0.40 5 6 1 o 205.684 168.180 -29.59 1.21368 0.14 4 5 3 o 146.711 155.876 -87.63 1.20998 0.10 3 3 4 o 171.588 193.301 -57.78 1.20655 0.12 3 9 3 o 1650.140 1655.341 -91.00 1.19886 1.11 0 12 3 o 1552.625 1816.177 -180.00 1.20770 0.53 5 3 2 o 625.977 720.602 -3.15 1.20696 0.43 5 7 0 o 213.853 225.074 -90.00 1.20549 0.08 2 7 4 o 62.842 63.469 2.72 1.19864 0.04 1 15 0 o 35.475 44.511 -90.00 1.20857 0.02 2 14 1 o 1468.035 1375.789 92.58 1.20082 0.97 3 13 0 o 2835.459 2671.162 90.00 1.20068 0.94 4 9 2 o 18.798 17.646 -172.86 1.19283 0.01 2 13 2 o 394.038 342.847 162.96 1.19432 0.26 2 11 3 o 17.370 18.811 -77.28 1.19110 0.01 0 14 2 o 4.111 3.851 180.00 1.20072 0.00 0 15 1 o 8.261 7.265 -90.00 1.20218 0.00 0 9 4 o 1017.552 993.890 -90.00 1.19243 0.33 1 12 3 o 545.832 621.652 -75.51 1.18899 0.37 3 4 4 o 30.053 34.688 -111.27 1.18883 0.02 4 11 0 o 262.573 279.851 0.00 1.19140 0.09 5 4 2 o 283.365 323.955 -9.98 1.18923 0.19 4 6 3 o 262.495 237.747 -3.85 1.18226 0.19 1 14 2 o 397.652 363.698 -118.02 1.18233 0.26 1 15 1 o 723.206 662.045 -175.03 1.18372 0.48 5 7 1 o 547.392 495.480 152.49 1.18083 0.36 3 13 1 o 931.206 861.764 -171.64 1.17631 0.60 1 9 4 o 1040.847 1052.486 162.60 1.17441 0.67 3 12 2 o 342.689 340.742 -26.04 1.16550 0.23 4 11 1 o 128.551 145.998 77.63 1.16758 0.10 3 5 4 o 417.251 459.249 172.89 1.16717 0.26 0 1 5 o 1008.642 1074.195 90.00 1.17124 0.33 5 8 0 o 1361.743 1527.589 90.00 1.16855 0.44 2 8 4 o 1017.457 892.476 76.49 1.16231 0.65 5 5 2 o 149.578 167.833 145.30 1.16754 0.10 0 2 5 o 45.172 40.623 180.00 1.16420 0.02 3 10 3 o 1013.960 902.353 -79.68 1.15336 0.64 4 7 3 o 87.402 90.806 -90.93 1.15183 0.05 1 0 5 o 1.465 0.040 90.00 1.15642 0.00 4 10 2 o 297.982 370.228 -130.97 1.14799 0.19 2 15 0 o 349.045 270.664 0.00 1.15479 0.11 1 1 5 o 24.466 20.163 -59.27 1.15415 0.02 0 3 5 o 385.496 368.050 -90.00 1.15275 0.12 5 8 1 o 114.425 142.618 120.12 1.14605 0.08 3 6 4 o 474.659 478.309 104.44 1.14222 0.29 0 10 4 o 825.095 1058.863 180.00 1.14763 0.26 1 2 5 o 426.377 550.111 -55.42 1.14741 0.27 5 6 2 o 377.316 382.027 -81.61 1.14258 0.24 0 13 3 o 143.201 183.611 -90.00 1.14763 0.04 2 12 3 o 243.114 188.020 163.30 1.13767 0.15 0 16 0 o 3.979 4.395 180.00 1.15147 0.00 4 12 0 o 408.276 306.157 0.00 1.13794 0.13 3 14 0 o 2.060 0.252 90.00 1.13724 0.00 1 3 5 o 278.107 212.320 -131.70 1.13645 0.18 0 4 5 o 483.327 361.799 0.00 1.13728 0.15 2 14 2 o 232.247 237.747 60.20 1.13183 0.15 1 13 3 o 323.369 332.370 -68.20 1.13154 0.20 1 10 4 o 531.953 545.717 -175.89 1.13154 0.33 2 15 1 o 816.139 807.442 -9.68 1.13306 0.50 5 9 0 o 191.570 196.015 90.00 1.13053 0.06 2 9 4 o 271.852 242.327 -56.83 1.12488 0.17 1 16 0 o 3.615 1.096 90.00 1.13522 0.00 0 15 2 o 371.945 373.031 -90.00 1.13297 0.12 4 8 3 o 724.028 878.853 -173.65 1.11948 0.45 4 12 1 o 49.753 52.806 167.39 1.11712 0.03 6 0 0 o -0.034 0.008 0.00 1.13008 0.00 0 16 1 o 1048.172 1063.349 -180.00 1.12992 0.32 1 4 5 o 666.781 743.799 166.50 1.12161 0.41 6 1 0 o 3155.173 2932.441 -180.00 1.12796 0.96 3 7 4 o 436.162 448.157 -129.74 1.11471 0.26 3 14 1 o 593.130 619.014 33.52 1.11647 0.36 0 5 5 o 148.499 169.469 -90.00 1.11826 0.04 5 7 2 o 423.708 436.050 -124.88 1.11504 0.26 1 15 2 o 371.799 403.506 -95.67 1.11748 0.22 3 13 2 o 301.369 262.221 85.58 1.11123 0.18 6 2 0 o 141.612 157.845 0.00 1.12167 0.04 3 11 3 o 714.520 644.332 78.09 1.10864 0.44 5 9 1 o 45.496 37.714 70.79 1.11011 0.03 1 16 1 o 769.541 794.346 -172.67 1.11455 0.47 5 0 3 o 415.014 429.878 -90.00 1.11446 0.13 5 1 3 o 147.356 138.950 -85.01 1.11242 0.09 4 11 2 o 0.444 0.451 66.00 1.10387 0.00 4 1 4 o 20.554 20.229 160.75 1.10728 0.01 2 1 5 o 2.799 2.783 134.31 1.10704 0.00 4 0 4 o 535.685 459.312 0.00 1.10928 0.16 2 0 5 o 497.231 430.546 -90.00 1.10904 0.16 5 2 3 o 466.737 472.067 32.67 1.10639 0.28 1 5 5 o 714.599 728.875 10.09 1.10336 0.43 6 3 0 o 1.328 0.288 -180.00 1.11142 0.00 0 11 4 o 96.753 97.964 -90.00 1.10355 0.03 6 0 1 o 2255.010 1867.051 -90.00 1.10969 0.67 4 2 4 o 258.435 298.086 -122.39 1.10133 0.16 2 2 5 o 751.571 885.999 74.54 1.10109 0.46 6 1 1 o 421.395 409.111 144.09 1.10768 0.25 5 3 3 o 21.854 14.869 -69.37 1.09655 0.01 0 6 5 o 1101.771 740.850 -180.00 1.09627 0.32 6 2 1 o 1458.575 1639.707 73.10 1.10172 0.87 5 10 0 o 727.340 676.892 -90.00 1.09214 0.21 4 3 4 o 145.195 140.672 -87.81 1.09162 0.09 2 3 5 o 50.986 50.587 121.32 1.09139 0.03 6 4 0 o 123.721 92.608 0.00 1.09753 0.03 1 11 4 o 498.149 544.393 33.43 1.08922 0.30 0 14 3 o 888.775 845.200 0.00 1.09186 0.27 2 16 0 o 82.043 88.703 180.00 1.09030 0.02 6 3 1 o 705.945 664.193 -32.09 1.09200 0.41 _reflns_number_total 383 _reflns_limit_h_min 0 _reflns_limit_h_max 6 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 5 _reflns_d_resolution_high 1.089 _reflns_d_resolution_low 9.212 #--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--# # Attachment '- BioMIL-2ht.cif' data_smv206 _database_code_depnum_ccdc_archive 'CCDC 775558' #TrackingRef '- BioMIL-2ht.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common BioMIL-2ht _chemical_formula_moiety 'C5 H6 Ca O4 ' _chemical_formula_sum 'C5 H6 Ca O4 ' _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour white _diffrn_ambient_temperature 293(2) _chemical_formula_weight 170.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 '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' _symmetry_cell_setting rhombohedral _symmetry_space_group_name_H-M 'R -3' _symmetry_int_tables_number 148 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 20.659(8) _cell_length_b 20.659(8) _cell_length_c 8.637(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3192.4(19) _cell_formula_units_Z 18 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2926 _cell_measurement_theta_min 29.57 _cell_measurement_theta_max 0.987 _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.593 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 0.835 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7862 _diffrn_reflns_av_R_equivalents 0.2158 _diffrn_reflns_av_sigmaI/netI 0.2756 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 29.62 _reflns_number_total 1991 _reflns_number_gt 784 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0683P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1991 _refine_ls_number_parameters 91 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2020 _refine_ls_R_factor_gt 0.0699 _refine_ls_wR_factor_ref 0.1829 _refine_ls_wR_factor_gt 0.1438 _refine_ls_goodness_of_fit_ref 0.891 _refine_ls_restrained_S_all 0.891 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ca1 Ca 0.74233(6) 0.06033(6) 0.66841(12) 0.0159(3) Uani 1 1 d . . . O1 O 0.6150(2) -0.0359(2) 0.7570(4) 0.0223(10) Uani 1 1 d . . . O2 O 0.5795(2) -0.1141(2) 0.5562(5) 0.0362(12) Uani 1 1 d . . . O3 O 0.6021(2) -0.2001(2) 1.2463(5) 0.0330(11) Uani 1 1 d . . . O4 O 0.5820(2) -0.3034(2) 1.1366(5) 0.0264(10) Uani 1 1 d . . . C1 C 0.5750(3) -0.0994(3) 0.6936(7) 0.0189(13) Uani 1 1 d . . . C2 C 0.5221(4) -0.1634(4) 0.7952(7) 0.0310(17) Uani 1 1 d . . . H2A H 0.4890 -0.2059 0.7315 0.037 Uiso 1 1 calc R . . H2B H 0.4918 -0.1488 0.8553 0.037 Uiso 1 1 calc R . . C3 C 0.5670(3) -0.1853(4) 0.9051(7) 0.0291(16) Uani 1 1 d . . . H3A H 0.5934 -0.2039 0.8435 0.035 Uiso 1 1 calc R . . H3B H 0.6042 -0.1407 0.9582 0.035 Uiso 1 1 calc R . . C4 C 0.5202(3) -0.2440(3) 1.0258(7) 0.0250(14) Uani 1 1 d . . . H4A H 0.4868 -0.2303 1.0765 0.030 Uiso 1 1 calc R . . H4B H 0.4900 -0.2920 0.9759 0.030 Uiso 1 1 calc R . . C5 C 0.5707(3) -0.2494(3) 1.1434(6) 0.0194(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ca1 0.0207(7) 0.0175(7) 0.0068(5) -0.0011(5) 0.0014(5) 0.0074(6) O1 0.028(2) 0.021(2) 0.013(2) -0.0008(18) -0.0007(18) 0.009(2) O2 0.046(3) 0.041(3) 0.007(2) -0.0049(19) 0.000(2) 0.011(2) O3 0.047(3) 0.027(3) 0.030(3) -0.018(2) -0.018(2) 0.023(2) O4 0.038(3) 0.023(2) 0.026(2) -0.0066(19) -0.012(2) 0.021(2) C1 0.011(3) 0.025(3) 0.019(3) -0.002(3) -0.001(2) 0.008(3) C2 0.028(4) 0.038(4) 0.021(4) 0.001(3) -0.003(3) 0.012(3) C3 0.029(4) 0.035(4) 0.021(4) 0.004(3) -0.002(3) 0.014(3) C4 0.025(4) 0.026(4) 0.019(3) 0.003(3) -0.001(3) 0.009(3) C5 0.023(3) 0.019(3) 0.011(3) -0.002(2) -0.003(3) 0.006(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ca1 O4 2.299(4) 16_646 ? Ca1 O2 2.302(4) 5_545 ? Ca1 O3 2.370(4) 5_544 ? Ca1 O1 2.410(4) 9_654 ? Ca1 O4 2.459(4) 11_667 ? Ca1 O1 2.495(4) . ? Ca1 O3 2.578(4) 11_667 ? Ca1 C5 2.889(6) 11_667 ? Ca1 Ca1 3.7993(15) 9_654 ? Ca1 Ca1 3.7993(15) 5_545 ? Ca1 Ca1 4.114(3) 13_656 ? O1 C1 1.273(6) . ? O1 Ca1 2.410(4) 5_545 ? O2 C1 1.240(7) . ? O2 Ca1 2.303(4) 9_654 ? O3 C5 1.260(6) . ? O3 Ca1 2.370(4) 9_655 ? O3 Ca1 2.578(4) 12_547 ? O4 C5 1.251(7) . ? O4 Ca1 2.299(4) 16_646 ? O4 Ca1 2.459(4) 12_547 ? C1 C2 1.505(8) . ? C2 C3 1.544(8) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.523(8) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.501(8) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 Ca1 2.889(6) 12_547 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Ca1 O2 90.50(15) 16_646 5_545 ? O4 Ca1 O3 82.08(15) 16_646 5_544 ? O2 Ca1 O3 92.35(16) 5_545 5_544 ? O4 Ca1 O1 74.37(14) 16_646 9_654 ? O2 Ca1 O1 161.16(16) 5_545 9_654 ? O3 Ca1 O1 96.49(15) 5_544 9_654 ? O4 Ca1 O4 158.63(16) 16_646 11_667 ? O2 Ca1 O4 80.62(15) 5_545 11_667 ? O3 Ca1 O4 117.45(14) 5_544 11_667 ? O1 Ca1 O4 109.55(14) 9_654 11_667 ? O4 Ca1 O1 89.67(14) 16_646 . ? O2 Ca1 O1 83.77(15) 5_545 . ? O3 Ca1 O1 170.86(15) 5_544 . ? O1 Ca1 O1 84.97(8) 9_654 . ? O4 Ca1 O1 70.16(13) 11_667 . ? O4 Ca1 O3 149.53(15) 16_646 11_667 ? O2 Ca1 O3 93.11(16) 5_545 11_667 ? O3 Ca1 O3 67.56(16) 5_544 11_667 ? O1 Ca1 O3 105.64(14) 9_654 11_667 ? O4 Ca1 O3 51.17(13) 11_667 11_667 ? O1 Ca1 O3 120.80(13) . 11_667 ? O4 Ca1 C5 172.45(16) 16_646 11_667 ? O2 Ca1 C5 84.67(16) 5_545 11_667 ? O3 Ca1 C5 92.30(16) 5_544 11_667 ? O1 Ca1 C5 111.46(15) 9_654 11_667 ? O4 Ca1 C5 25.45(14) 11_667 11_667 ? O1 Ca1 C5 95.56(15) . 11_667 ? O3 Ca1 C5 25.84(14) 11_667 11_667 ? O4 Ca1 Ca1 38.49(10) 16_646 9_654 ? O2 Ca1 Ca1 121.64(13) 5_545 9_654 ? O3 Ca1 Ca1 102.31(11) 5_544 9_654 ? O1 Ca1 Ca1 40.06(9) 9_654 9_654 ? O4 Ca1 Ca1 134.05(11) 11_667 9_654 ? O1 Ca1 Ca1 73.05(9) . 9_654 ? O3 Ca1 Ca1 144.73(11) 11_667 9_654 ? C5 Ca1 Ca1 148.69(12) 11_667 9_654 ? O4 Ca1 Ca1 123.05(12) 16_646 5_545 ? O2 Ca1 Ca1 67.77(11) 5_545 5_545 ? O3 Ca1 Ca1 146.37(11) 5_544 5_545 ? O1 Ca1 Ca1 110.93(11) 9_654 5_545 ? O4 Ca1 Ca1 35.58(10) 11_667 5_545 ? O1 Ca1 Ca1 38.44(9) . 5_545 ? O3 Ca1 Ca1 86.02(9) 11_667 5_545 ? C5 Ca1 Ca1 60.23(12) 11_667 5_545 ? Ca1 Ca1 Ca1 111.18(4) 9_654 5_545 ? O4 Ca1 Ca1 117.43(12) 16_646 13_656 ? O2 Ca1 Ca1 93.30(12) 5_545 13_656 ? O3 Ca1 Ca1 35.39(10) 5_544 13_656 ? O1 Ca1 Ca1 103.53(10) 9_654 13_656 ? O4 Ca1 Ca1 82.68(10) 11_667 13_656 ? O1 Ca1 Ca1 152.82(10) . 13_656 ? O3 Ca1 Ca1 32.17(9) 11_667 13_656 ? C5 Ca1 Ca1 57.26(12) 11_667 13_656 ? Ca1 Ca1 Ca1 129.37(4) 9_654 13_656 ? Ca1 Ca1 Ca1 115.86(5) 5_545 13_656 ? C1 O1 Ca1 132.6(4) . 5_545 ? C1 O1 Ca1 124.9(3) . . ? Ca1 O1 Ca1 101.50(14) 5_545 . ? C1 O2 Ca1 145.5(4) . 9_654 ? C5 O3 Ca1 150.8(4) . 9_655 ? C5 O3 Ca1 91.0(4) . 12_547 ? Ca1 O3 Ca1 112.44(16) 9_655 12_547 ? C5 O4 Ca1 151.1(4) . 16_646 ? C5 O4 Ca1 96.9(3) . 12_547 ? Ca1 O4 Ca1 105.93(16) 16_646 12_547 ? O2 C1 O1 125.0(6) . . ? O2 C1 C2 117.0(5) . . ? O1 C1 C2 117.8(5) . . ? C1 C2 C3 109.7(5) . . ? C1 C2 H2A 109.7 . . ? C3 C2 H2A 109.7 . . ? C1 C2 H2B 109.7 . . ? C3 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C4 C3 C2 114.7(5) . . ? C4 C3 H3A 108.6 . . ? C2 C3 H3A 108.6 . . ? C4 C3 H3B 108.6 . . ? C2 C3 H3B 108.6 . . ? H3A C3 H3B 107.6 . . ? C5 C4 C3 109.5(5) . . ? C5 C4 H4A 109.8 . . ? C3 C4 H4A 109.8 . . ? C5 C4 H4B 109.8 . . ? C3 C4 H4B 109.8 . . ? H4A C4 H4B 108.2 . . ? O4 C5 O3 120.3(5) . . ? O4 C5 C4 118.8(5) . . ? O3 C5 C4 120.9(6) . . ? O4 C5 Ca1 57.7(3) . 12_547 ? O3 C5 Ca1 63.1(3) . 12_547 ? C4 C5 Ca1 171.5(4) . 12_547 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.568 _refine_diff_density_min -0.561 _refine_diff_density_rms 0.136