Hi, Here are the results obtained with the peak fitting in DASH and DICVOL as implemented in DASH: A= 8.8752 B=16.4077 C= 7.1366 BETA= 93.838 VOLUME=1036.92 M(20)= 196.7 F(20)=1079.6(0.0006, 32) (see also original DICVOL output attached). The space-group determination in DASH returns P21/n or P2/n as possible space groups. The crystal structure easily solves with DASH in P21/n (10 out of 11 times), see cif attached. There are hydrogen bonds between Cl- and -NH2 and there are no other close contacts (except several involving hydrogens). P2/n did not give a solution (9 out of 9 times). The crystal structure is not refined, and the starting molecule is not very good, so there is room for improvement, but the fit to the powder pattern is fairly good (see .png). You can reveal my name on the sdpd mailing list. Best wishes, -- Jacco van de Streek Research Scientist Cambridge Crystallographic Data Centre Cambridge, United Kingdom INPUT DATA EXPERIMENTAL EXPERIMENTAL 2-THETA ERROR 4.887 0.020 6.139 0.020 6.663 0.020 6.988 0.020 7.404 0.020 7.460 0.020 7.851 0.020 8.530 0.020 8.922 0.020 9.062 0.020 9.250 0.020 9.386 0.020 9.782 0.020 10.136 0.020 10.300 0.020 10.468 0.020 10.633 0.020 10.783 0.020 11.449 0.020 11.537 0.020 ****************************************** ------- PARAMETER LIMITS -------- -------- VOLUME LIMITS --------- | | | | | A MAXIMUM = 30.00 A | | | | B MAXIMUM = 30.00 A | | VOLUME MINIMUM = 0.00 A**3 | | C MAXIMUM = 30.00 A | | | | BETA MINIMUM = 90.00 Deg. | | VOLUME MAXIMUM = 6000.00 A**3 | | BETA MAXIMUM = 125.00 Deg. | | | | | | | ----------------------------------- ---------------------------------- WAVELENGTH = 0.699500 LOWER FIGURE OF MERIT REQUIRED FOR PRINTED SOLUTION(S) : M( 20) = 5.0 O R T H O R H O M B I C S Y S T E M DIRECT PARAMETERS : A= 26.94014 B= 16.40428 C= 11.74874 VOLUME= 5192.16 STANDARD DEVIATIONS : 0.01696 0.00393 0.00392 H K L DOBS DCAL DOBS-DCAL 2TH.OBS 2TH.CAL DIF.2TH. 0 2 0 8.20434 8.20214 0.00221 4.887 4.888 -0.001 1 2 1 6.53120 6.52511 0.00609 6.139 6.145 -0.006 3 1 1 6.54261 -0.01141 6.129 0.011 2 2 1 6.01802 6.01707 0.00095 6.663 6.665 -0.001 1 0 2 5.73885 5.73950 -0.00065 6.988 6.987 0.001 1 1 2 5.41702 5.41748 -0.00046 7.404 7.403 0.001 3 2 1 5.37591 5.38307 -0.00716 7.460 7.451 0.010 5 0 0 5.38803 -0.01212 7.444 0.017 2 0 2 5.38460 -0.00869 7.448 0.012 2 1 2 5.10879 5.11604 -0.00725 7.851 7.840 0.011 5 1 0 5.11898 -0.01019 7.835 0.016 1 2 2 4.70285 4.70252 0.00033 8.530 8.531 -0.001 3 1 2 4.70906 -0.00621 8.519 0.011 2 2 2 4.49656 4.50129 -0.00474 8.922 8.913 0.009 5 2 0 4.50329 -0.00674 8.909 0.013 6 0 0 4.49002 0.00653 8.935 -0.013 4 0 2 4.42734 4.42703 0.00031 9.062 9.063 -0.001 3 3 1 4.33745 4.34004 -0.00259 9.250 9.245 0.006 4 1 2 4.27465 4.27412 0.00053 9.386 9.387 -0.001 0 4 0 4.10200 4.10107 0.00093 9.782 9.785 -0.002 1 3 2 3.95922 3.95900 0.00022 10.136 10.137 -0.001 5 0 2 3.97073 -0.01152 10.107 0.029 4 2 2 3.89638 3.89579 0.00060 10.300 10.301 -0.002 1 4 1 3.83386 3.83257 0.00129 10.468 10.472 -0.004 2 3 2 3.83666 -0.00280 10.461 0.008 5 3 0 3.83790 -0.00404 10.457 0.011 1 1 3 3.77479 3.77168 0.00310 10.633 10.641 -0.009 2 4 1 3.72220 3.72127 0.00093 10.783 10.786 -0.003 3 4 0 3.73046 -0.00826 10.759 0.024 6 2 1 3.73427 -0.01207 10.748 0.035 1 2 3 3.50645 3.50405 0.00240 11.449 11.457 -0.008 3 1 3 3.50675 -0.00031 11.448 0.001 6 1 2 3.47978 3.48584 -0.00606 11.537 11.517 0.020 7 2 0 3.48411 -0.00433 11.523 0.014 * NUMBER OF LINES .- INPUT DATA = 20 .- CALCULATED = 101 * MEAN ABSOLUTE DISCREPANCIES =0.4699E-04 =0.4138E-02 MAX. ERROR ACCEPTED (DEG. 2-THETA) =0.3500E-01 * FIGURES OF MERIT 1.- M( 20) = 8.7 (REF. 4) 2.- F( 20) = 47.9(0.0041, 101) (REF. 5) =====> CELL VOLUME = 5192.2 A**3 M(20)= 8.7 F(20)= 47.9(0.0041,101) SEARCH OF MONOCLINIC SOLUTION(S) WITHIN THE LIMITS ON LINEAR PARAMETERS *********************************************************************** (SLIGHT TOLERANCE ACCEPTED): A MAX= 16.976 B MAX= 16.976 C MAX= 16.976 M O N O C L I N I C S Y S T E M DIRECT PARAMETERS : A= 8.8752 B=16.4077 C= 7.1366 BETA= 93.838 VOLUME=1036.92 STANDARD DEVIATIONS : 0.0004 0.0009 0.0004 0.005 H K L DOBS DCAL DOBS-DCAL 2TH.OBS 2TH.CAL DIF.2TH. 0 2 0 8.20434 8.20387 0.00047 4.887 4.887 0.000 0 1 1 6.53120 6.53203 -0.00084 6.139 6.139 0.001 1 2 0 6.01802 6.01813 -0.00011 6.663 6.663 0.000 1 0 -1 5.73885 5.73994 -0.00109 6.988 6.987 0.001 1 1 -1 5.41702 5.41798 -0.00096 7.404 7.402 0.001 0 2 1 5.37591 5.37754 -0.00163 7.460 7.458 0.002 1 0 1 5.37615 -0.00024 7.460 0.000 1 1 1 5.10879 5.10889 -0.00011 7.851 7.851 0.000 1 2 -1 4.70285 4.70309 -0.00024 8.530 8.530 0.000 1 2 1 4.49656 4.49664 -0.00008 8.922 8.922 0.000 2 0 0 4.42734 4.42762 -0.00028 9.062 9.061 0.001 0 3 1 4.33745 4.33746 -0.00001 9.250 9.250 0.000 2 1 0 4.27465 4.27472 -0.00007 9.386 9.386 0.000 0 4 0 4.10200 4.10194 0.00007 9.782 9.782 0.000 1 3 -1 3.95922 3.95958 -0.00037 10.136 10.135 0.001 2 2 0 3.89638 3.89638 0.00000 10.300 10.300 0.000 1 3 1 3.83386 3.83400 -0.00014 10.468 10.468 0.000 2 1 -1 3.77479 3.77424 0.00055 10.633 10.634 -0.002 1 4 0 3.72220 3.72201 0.00020 10.783 10.784 -0.001 2 2 -1 3.50645 3.50620 0.00025 11.449 11.450 -0.001 0 1 2 3.47978 3.47935 0.00043 11.537 11.538 -0.001 * NUMBER OF LINES .- INPUT DATA = 20 .- CALCULATED = 32 * MEAN ABSOLUTE DISCREPANCIES =0.6559E-05 =0.5789E-03 MAX. ERROR ACCEPTED (DEG. 2-THETA) =0.3500E-01 * FIGURES OF MERIT 1.- M( 20) = 196.7 (REF. 4) 2.- F( 20) = 1079.6(0.0006, 32) (REF. 5) =====> CELL VOLUME = 1036.9 A**3 M(20)= 196.7 F(20)=1079.6(0.0006, 32) T R I C L I N I C S Y S T E M DIRECT PARAMETERS AND THEIR STANDARD DEVIATIONS : A= 8.9135 B= 8.0775 C=17.5103 ALP= 57.419 BET=106.576 GAM=112.725 VOL= 975.00 0.0176 0.0111 0.0295 0.160 0.181 0.134 H K L DOBS DCAL DOBS-DCAL 2TH.OBS 2TH.CAL DIF.2TH. 1 0 0 8.20434 8.18083 0.02351 4.887 4.901 -0.014 0 1 0 6.53120 6.51774 0.01345 6.139 6.152 -0.013 1 -1 0 6.01802 6.01111 0.00691 6.663 6.671 -0.008 1 0 -2 5.73885 5.75548 -0.01663 6.988 6.968 0.020 1 -1 -3 5.41702 5.41642 0.00061 7.404 7.405 -0.001 0 1 3 5.37591 5.35159 0.02432 7.460 7.494 -0.034 0 1 -1 5.10879 5.10945 -0.00066 7.851 7.850 0.001 1 1 1 4.70285 4.69026 0.01259 8.530 8.553 -0.023 1 1 0 4.49656 4.50430 -0.00774 8.922 8.907 0.015 1 1 2 4.42734 4.43219 -0.00485 9.062 9.052 0.010 2 -1 -2 4.33745 4.32828 0.00916 9.250 9.270 -0.020 2 -1 -1 4.34794 -0.01049 9.228 0.022 1 -1 -4 4.27465 4.27257 0.00208 9.386 9.391 -0.005 2 0 0 4.10200 4.09042 0.01159 9.782 9.810 -0.028 1 -2 -3 3.95922 3.96766 -0.00845 10.136 10.114 0.022 1 1 3 3.89638 3.90341 -0.00703 10.300 10.281 0.019 2 0 1 3.83386 3.84282 -0.00895 10.468 10.444 0.024 1 -2 -1 3.77479 3.77368 0.00111 10.633 10.636 -0.003 0 2 2 3.72220 3.72123 0.00097 10.783 10.786 -0.003 2 -2 -3 3.50645 3.49708 0.00937 11.449 11.480 -0.031 1 0 -4 3.47978 3.48053 -0.00075 11.537 11.534 0.003 2 -2 -2 3.48929 -0.00951 11.505 0.032 2 -1 -4 3.48838 -0.00860 11.508 0.029 * NUMBER OF LINES .- INPUT DATA = 20 .- CALCULATED = 50 * MEAN ABSOLUTE DISCREPANCIES =0.1635E-03 =0.1473E-01 MAX. ERROR ACCEPTED (DEG. 2-THETA) =0.3500E-01 * FIGURES OF MERIT 1.- M( 20) = 5.1 (REF. 4) 2.- F( 20) = 27.2(0.0147, 50) (REF. 5) =====> CELL VOLUME = 975.0 A**3 M(20)= 5.1 F(20)= 27.2(0.0147, 50) DICVOL : Useful References ------ 1 D. Louër & M. Louër (1972). J. Appl. Cryst. 5, 271-275. 2 A. Boultif & D. Louër (1991). J. Appl. Cryst. 24, 987-993. 3 D. Louër & R. Vargas (1982). J. Appl. Cryst. 15, 542-545. 4 P.M. de Wolff (1968). J. Appl. Cryst. 5, 108-113. 5 G.S. Smith & R.L. Snyder (1979). J. Appl. Cryst. 12, 60- 65. data_global # chi**2= 107.88 and profile chi**2= 97.10 max. moves=15000000 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '1/2-x,1/2+y,1/2-z' '1/2+x,1/2-y,1/2+z' _cell_length_a 8.8794 _cell_length_b 16.4140 _cell_length_c 7.1393 _cell_angle_alpha 90.0000 _cell_angle_beta 93.8245 _cell_angle_gamma 90.0000 _cell_volume 1038.2 _cell_formula_units_Z ? _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.69950 _refine_ls_goodness_of_fit_all 10.387 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_adp_type _atom_site_B_iso_or_equiv Cl1 0.79068 0.50535 0.26096 1.000 Biso 3.00 N1 0.83378 0.89702 0.73892 1.000 Biso 3.00 C2 0.66602 0.89495 0.69208 1.000 Biso 3.00 C3 0.88661 0.98927 0.75273 1.000 Biso 3.00 C4 0.91106 0.85598 0.57980 1.000 Biso 3.00 C5 0.87284 0.85174 0.91708 1.000 Biso 3.00 C6 0.80650 0.77167 0.93175 1.000 Biso 3.00 C7 0.81790 0.74364 1.13792 1.000 Biso 3.00 O8 0.89503 0.71200 0.83135 1.000 Biso 3.00 C9 0.83118 0.66075 0.67638 1.000 Biso 3.00 O10 0.70063 0.68230 0.62133 1.000 Biso 3.00 N11 0.94751 0.60882 0.60287 1.000 Biso 3.00 H12 1.02722 0.87009 0.55097 1.000 Biso 6.00 H13 0.85807 0.89003 0.46200 1.000 Biso 6.00 H14 0.62972 0.83228 0.66624 1.000 Biso 6.00 H15 0.61710 0.94167 0.77795 1.000 Biso 6.00 H16 0.63642 0.92851 0.56310 1.000 Biso 6.00 H17 1.00900 0.98649 0.77703 1.000 Biso 6.00 H18 0.80989 0.99830 0.86390 1.000 Biso 6.00 H19 0.85747 1.02409 0.62544 1.000 Biso 6.00 H20 0.98886 0.83323 0.95446 1.000 Biso 6.00 H21 0.87481 0.87467 1.06050 1.000 Biso 6.00 H22 0.69518 0.77144 0.85750 1.000 Biso 6.00 H23 0.77022 0.79290 1.21750 1.000 Biso 6.00 H24 0.91260 0.71370 1.21479 1.000 Biso 6.00 H25 0.74373 0.69402 1.17452 1.000 Biso 6.00 UPPW11.png