# Electronic Supplementary Material (ESI) for Chemical Science. # This journal is © The Royal Society of Chemistry 2021 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_ROY_ON_0p02GPa _database_code_depnum_ccdc_archive 'CCDC 2098636' loop_ _audit_author_name _audit_author_address 'Nicholas Funnell' ;STFC, ISIS Neutron Facility United Kingdom ; _audit_update_record ; 2021-07-22 deposited with the CCDC. 2021-08-27 downloaded from the CCDC. ; _audit_creation_date 2021-01-25 _audit_creation_method 'CRYSTALS_ver_14.61_build_7795 ' _chemical_name_systematic ; 5-methyl-2[(2-nitrophenyl)amino]-3-thiophenecarbonitrile ; # CheckCIF alerts _vrf_THETM01_ROY_ON_0p02GPa ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575 RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT027_ROY_ON_0p02GPa ; PROBLEM: _diffrn_reflns_theta_full value (too) Low ...... 17.44 Degree RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT029_ROY_ON_0p02GPa ; PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.727 Why? RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT201_ROY_ON_0p02GPa ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 17 Report RESPONSE: The model could only be refined isotropically in order to maintain a favourable data-to-parameter ratio, due to numerous unmeasured reflections. The relatively electron-rich sulfur atom has been modelled anisotropically. ; _vrf_PLAT340_ROY_ON_0p02GPa ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.01236 Ang. RESPONSE: These are poor-quality diffraction data. ; _vrf_PLAT911_ROY_ON_0p02GPa ; PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.555 473 Report RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT082_ROY_ON_0p02GPa ; PROBLEM: High R1 Value .................................. 0.15 Report RESPONSE: These are poor-quality diffraction data and the model has only been refined isotropically. ; _vrf_PLAT910_ROY_ON_0p02GPa ; PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 8 Note RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _refine_special_details ; In the absence of significant anomalous scattering, Friedel pairs were merged. Data were collected in a Merrill-Bassett diamond anvil cell, which significantly restricts the regions over which reciprocal space can be sampled. Thus, these data are poor quality/incomplete, reflected in numerous CheckCIF alerts regarding refinement statistics. At all pressures, the atomic connectivity is known. All non-sulfur atoms were refined isotropically; sulfur was refined anisotropically. Hydrogen atoms were constrained to ride on their host atoms. #=============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Total Missing #------------------------------------------------------------------------------- 20.82 0.500 0.728 1231 896 335 23.01 0.550 0.713 1632 1163 469 23.25 0.555 0.712 1672 1191 481 ------------------------------------------------------------ ACTA Min. Res. --- Note: The Reported Completeness refers to the Actual H,K,L Index Range ; #end of refcif _cell_length_a 3.920050(19) _cell_length_b 18.56291(5) _cell_length_c 16.40883(5) _cell_angle_alpha 90 _cell_angle_beta 93.655(6) _cell_angle_gamma 90 _cell_volume 1191.601(11) _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' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 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' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C12 H9 N3 O2 S1 # Dc = 1.45 Fooo = 536.00 Mu = 2.68 M = 259.29 # Found Formula = C12 H9 N3 O2 S1 # Dc = 1.45 FOOO = 536.00 Mu = 2.68 M = 259.29 _chemical_formula_sum 'C12 H9 N3 O2 S1' _chemical_formula_moiety 'C12 H9 N3 O2 S1' _chemical_compound_source 'TCI Chemicals' _chemical_formula_weight 259.29 _cell_measurement_reflns_used 1582 _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 22.15 _cell_measurement_temperature 293 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_min 0.050 _exptl_crystal_size_mid 0.072 _exptl_crystal_size_max 0.248 _exptl_crystal_density_diffrn 1.445 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 0.268 # Sheldrick geometric approximatio 0.98 0.99 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North et al., 1968)' _exptl_absorpt_correction_T_min 0.09 _exptl_absorpt_correction_T_max 0.99 _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_device 'four-circle diffractometer' _diffrn_radiation_monochromator mirror _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 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction ; CrysAlisPro (Rigaku Oxford Diffraction, 2017) ; _computing_structure_solution 'Model from previously-determined structure' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 293 _diffrn_reflns_number 3968 _diffrn_reflns_av_unetI/netI 0.065 _reflns_number_total 1201 _diffrn_reflns_av_R_equivalents 0.068 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 1201 # Theoretical number of reflections is about 3421 _diffrn_reflns_theta_min 1.658 _diffrn_reflns_theta_max 23.252 _diffrn_measured_fraction_theta_max 0.699 _diffrn_reflns_theta_full 17.439 _diffrn_measured_fraction_theta_full 0.727 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -4 _reflns_limit_h_max 4 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 16 _oxford_diffrn_Wilson_B_factor 5.12 _oxford_diffrn_Wilson_scale 5.48 _atom_sites_solution_primary geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -1.09 _refine_diff_density_max 0.99 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # Explicitly named reflections are ALWAYS excluded from R&wR # The values actually used during refinement # These are labelled "all" for compatibility with PLATON _oxford_refine_reflns_threshold_expression I>-3.0\s(I) _refine_ls_number_restraints 94 _refine_ls_number_parameters 82 _refine_ls_number_reflns 1191 _oxford_refine_ls_R_factor_ref 0.2379 _refine_ls_R_factor_all 0.2379 _refine_ls_wR_factor_ref 0.0829 _refine_ls_wR_factor_all 0.0829 _refine_ls_goodness_of_fit_ref 0.9062 _refine_ls_shift/su_max 0.0001567 _refine_ls_shift/su_mean 0.0000411 # Computed with I/sigma = -10 _oxford_reflns_number_all 1191 _oxford_refine_ls_R_factor_all 0.2379 _oxford_refine_ls_wR_factor_all 0.0829 # Computed with no filters except I/sigma = +2 a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 662 _refine_ls_R_factor_gt 0.1525 _refine_ls_wR_factor_gt 0.0718 _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed #undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ; Method= SQRT(W) = 1/(Data with the key SIGMA(/FO/) in list 6) ; # 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 S1 S 0.8453(6) 0.59696(13) 0.42922(16) 0.0694 1.0000 Uani D U . . . . O1 O 0.5061(12) 0.6178(3) 0.0298(4) 0.0788(19) 1.0000 Uiso D U . . . . O2 O 0.5900(14) 0.6889(3) 0.1346(4) 0.0792(17) 1.0000 Uiso D U . . . . C1 C 0.9395(16) 0.5807(5) 0.2234(6) 0.0690(17) 1.0000 Uiso D U . . . . C2 C 1.1230(18) 0.5224(5) 0.2624(6) 0.0681(18) 1.0000 Uiso D U . . . . C3 C 1.1652(18) 0.4616(5) 0.2176(6) 0.0678(19) 1.0000 Uiso D U . . . . C4 C 1.0334(16) 0.4544(4) 0.1379(6) 0.0684(19) 1.0000 Uiso D U . . . . C5 C 0.8590(18) 0.5096(4) 0.0997(6) 0.0702(18) 1.0000 Uiso D U . . . . C6 C 0.8146(17) 0.5722(5) 0.1450(6) 0.0715(17) 1.0000 Uiso D U . . . . C7 C 0.9687(17) 0.6549(4) 0.3547(6) 0.0648(17) 1.0000 Uiso D U . . . . C8 C 1.1236(17) 0.7138(4) 0.3860(6) 0.0660(17) 1.0000 Uiso D U . . . . C9 C 1.1448(18) 0.7136(4) 0.4744(6) 0.0656(18) 1.0000 Uiso D U . . . . C10 C 1.0077(12) 0.6557(3) 0.5057(6) 0.0665(17) 1.0000 Uiso D U . . . . C11 C 0.9802(12) 0.6358(3) 0.5929(5) 0.071(2) 1.0000 Uiso D U . . . . C12 C 1.2666(18) 0.7640(5) 0.3337(6) 0.0656(18) 1.0000 Uiso D U . . . . N1 N 0.9001(14) 0.6410(4) 0.2726(5) 0.0675(16) 1.0000 Uiso D U . . . . N2 N 1.3954(17) 0.8025(4) 0.2897(5) 0.0708(18) 1.0000 Uiso D U . . . . N3 N 0.6246(17) 0.6297(4) 0.1004(5) 0.0751(18) 1.0000 Uiso D U . . . . H1 H 0.788(6) 0.6745(17) 0.2473(19) 0.083(3) 1.0000 Uiso D . . . . . H2 H 1.2110 0.5259 0.3158 0.0979 1.0000 Uiso R . . . . . H3 H 1.2877 0.4241 0.2424 0.0949 1.0000 Uiso R . . . . . H4 H 1.0634 0.4117 0.1092 0.0979 1.0000 Uiso R . . . . . H5 H 0.7719 0.5068 0.0457 0.0939 1.0000 Uiso R . . . . . H9 H 1.2434 0.7510 0.5059 0.0970 1.0000 Uiso R . . . . . H111 H 1.1859 0.6084 0.6125 0.1829 1.0000 Uiso DR . . . . . H112 H 0.9622 0.6799 0.6258 0.1829 1.0000 Uiso DR . . . . . H113 H 0.7746 0.6058 0.5981 0.1831 1.0000 Uiso DR . . . . . 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 S1 0.0890(13) 0.0526(18) 0.065(2) 0.0051(10) -0.0110(12) -0.0016(13) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.4448(18) 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 S1 . C7 . 1.721(9) yes S1 . C10 . 1.751(8) yes O1 . N3 . 1.240(8) yes O2 . N3 . 1.245(8) yes C1 . C2 . 1.429(12) yes C1 . C6 . 1.356(11) yes C1 . N1 . 1.394(11) yes C2 . C3 . 1.362(11) yes C2 . H2 . 0.923 no C3 . C4 . 1.383(11) yes C3 . H3 . 0.925 no C4 . C5 . 1.362(10) yes C4 . H4 . 0.933 no C5 . C6 . 1.398(12) yes C5 . H5 . 0.930 no C6 . N3 . 1.470(10) yes C7 . C8 . 1.337(11) yes C7 . N1 . 1.380(10) yes C8 . C9 . 1.449(11) yes C8 . C12 . 1.407(11) yes C9 . C10 . 1.320(9) yes C9 . H9 . 0.934 no C10 . C11 . 1.488(11) yes C11 . H111 . 0.990 no C11 . H112 . 0.986 no C11 . H113 . 0.988 no C12 . N2 . 1.155(11) yes N1 . H1 . 0.85(3) 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 C7 . S1 . C10 . 90.8(5) yes C2 . C1 . C6 . 118.5(8) yes C2 . C1 . N1 . 114.9(9) yes C6 . C1 . N1 . 126.6(8) yes C1 . C2 . C3 . 117.4(9) yes C1 . C2 . H2 . 121.2 no C3 . C2 . H2 . 121.3 no C2 . C3 . C4 . 122.7(8) yes C2 . C3 . H3 . 117.5 no C4 . C3 . H3 . 119.7 no C3 . C4 . C5 . 120.6(9) yes C3 . C4 . H4 . 120.6 no C5 . C4 . H4 . 118.9 no C4 . C5 . C6 . 117.2(10) yes C4 . C5 . H5 . 122.6 no C6 . C5 . H5 . 120.2 no C5 . C6 . C1 . 123.5(8) yes C5 . C6 . N3 . 114.5(10) yes C1 . C6 . N3 . 122.0(8) yes S1 . C7 . C8 . 112.3(8) yes S1 . C7 . N1 . 122.0(6) yes C8 . C7 . N1 . 125.7(8) yes C7 . C8 . C9 . 112.3(8) yes C7 . C8 . C12 . 119.8(9) yes C9 . C8 . C12 . 127.7(8) yes C8 . C9 . C10 . 113.1(7) yes C8 . C9 . H9 . 123.1 no C10 . C9 . H9 . 123.7 no S1 . C10 . C9 . 111.5(8) yes S1 . C10 . C11 . 119.3(3) yes C9 . C10 . C11 . 129.2(6) yes C10 . C11 . H111 . 109.5 no C10 . C11 . H112 . 109.5 no H111 . C11 . H112 . 109.5 no C10 . C11 . H113 . 109.5 no H111 . C11 . H113 . 109.5 no H112 . C11 . H113 . 109.5 no C8 . C12 . N2 . 176.4(11) yes C1 . N1 . C7 . 133.8(8) yes C1 . N1 . H1 . 112(2) no C7 . N1 . H1 . 114(2) no C6 . N3 . O2 . 118.8(9) yes C6 . N3 . O1 . 119.0(8) yes O2 . N3 . O1 . 122.2(7) yes 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 N1 . H1 . O2 . 135(3) 0.85(3) 1.98(3) 2.654(11) yes _iucr_refine_instructions_details ; # # Punched on 25/01/21 at 12:17:07 # #LIST 12 BLOCK CONT SCALE CONT S ( 1 ,X'S,U'S) CONT O ( 1 ,X'S,U[ISO]) UNTIL H ( 1 ) RIDE C ( 2,X'S) H ( 2,X'S) RIDE C ( 3,X'S) H ( 3,X'S) RIDE C ( 4,X'S) H ( 4,X'S) RIDE C ( 5,X'S) H ( 5,X'S) RIDE C ( 9,X'S) H ( 9,X'S) RIDE C ( 11,X'S) H ( 111,X'S) H ( 112,X'S) H ( 113,X'S) END # # Punched on 25/01/21 at 12:17:07 # #LIST 16 NO REM REM NPF NOTE - FIRST UNTIL LAST REM REM HREST START (DO NOT REMOVE THIS LINE) REM NO H NO #H U MULT DIST REM C-H REM >4 1.5 .96 DISORDER REM 1 1 1.2 .93 C C-H (ACETYLENE) REM 1 2 1.2 .93 C-C(H)-C REM 1 3 1.2 .98 (C)3-C-H REM 2 1 1.2 .93 C=C-H(2) REM 2 2 1.2 .97 (C)2-C-(H)2 REM 3 1 1.5 .96 C-C-(H)3 REM N-H REM >4 1.5 .89 DISORDER REM 1 1 1.2 .86 N-N/H REM 1 2 1.2 .86 (C)2-N-H REM 1 3 1.2 .89 (C)3-N-H REM 2 1 1.2 .86 C-N-(H)2 REM 2 2 1.2 .89 (C)2-N-(H)2 REM 3 1 1.2 .89 C-H-(H)3 REM O-H REM 1 1 1.5 .82 O-H REM REM DIST ESD = 0.02 REM VIB ESD = 0.002 REM ANGLE ESD = 2.0 REM REM TO ACTIVATE THE VIB RESTRAINTS, REMOVE LEADING REM REM H1-N-R2 DIST 0.86, 0.02 = CONT N ( 1) TO H(1) REST 0.083, 0.002 = H(1,U[ISO]) ANGLE 0.0, 2.0 = MEAN CONT H(1) TO N ( 1) TO C(1) CONT H(1) TO N ( 1) TO C(7) REM HREST END (DO NOT REMOVE THIS LINE) REM DELU START (DO NOT REMOVE THIS LINE) VIBR .0, 0.00200 = S(1) TO C(10) VIBR .0, 0.00200 = S(1) TO C(7) VIBR .0, 0.00500 = C(7) TO C(10) VIBR .0, 0.00200 = N(2) TO C(12) VIBR .0, 0.00200 = C(10) TO C(9) VIBR .0, 0.00200 = C(10) TO C(11) VIBR .0, 0.00500 = C(9) TO S(1) VIBR .0, 0.00500 = C(11) TO S(1) VIBR .0, 0.00500 = C(11) TO C(9) VIBR .0, 0.00200 = C(12) TO C(8) VIBR .0, 0.00500 = C(8) TO N(2) VIBR .0, 0.00200 = O(1) TO N(3) VIBR .0, 0.00200 = C(2) TO C(1) VIBR .0, 0.00200 = C(2) TO C(3) VIBR .0, 0.00500 = C(3) TO C(1) VIBR .0, 0.00200 = N(1) TO C(7) VIBR .0, 0.00200 = N(1) TO C(1) VIBR .0, 0.00500 = C(1) TO C(7) VIBR .0, 0.00200 = C(7) TO C(8) VIBR .0, 0.00500 = N(1) TO S(1) VIBR .0, 0.00500 = C(8) TO S(1) VIBR .0, 0.00500 = C(8) TO N(1) VIBR .0, 0.00200 = O(2) TO N(3) VIBR .0, 0.00200 = N(3) TO C(6) VIBR .0, 0.00500 = O(1) TO O(2) VIBR .0, 0.00500 = C(6) TO O(2) VIBR .0, 0.00500 = C(6) TO O(1) VIBR .0, 0.00200 = C(5) TO C(4) VIBR .0, 0.00200 = C(5) TO C(6) VIBR .0, 0.00500 = C(6) TO C(4) VIBR .0, 0.00200 = C(4) TO C(3) VIBR .0, 0.00500 = C(3) TO C(5) VIBR .0, 0.00200 = C(1) TO C(6) VIBR .0, 0.00500 = N(1) TO C(2) VIBR .0, 0.00500 = C(6) TO C(2) VIBR .0, 0.00500 = C(6) TO N(1) VIBR .0, 0.00500 = C(5) TO N(3) VIBR .0, 0.00500 = C(1) TO N(3) VIBR .0, 0.00500 = C(1) TO C(5) VIBR .0, 0.00200 = C(9) TO C(8) VIBR .0, 0.00500 = C(8) TO C(10) VIBR .0, 0.00500 = C(2) TO C(4) VIBR .0, 0.00500 = C(12) TO C(9) VIBR .0, 0.00500 = C(7) TO C(9) VIBR .0, 0.00500 = C(7) TO C(12) REM DELU END (DO NOT REMOVE THIS LINE) ANGLE 110.000000 , 0.020000 = C(10) TO C(11) TO H(111) ANGLE 110.000000 , 0.020000 = C(10) TO C(11) TO H(112) ANGLE 110.000000 , 0.020000 = C(10) TO C(11) TO H(113) DISTANCE 1.225000 , 0.050000 = O(2) TO N(3) DISTANCE 1.225000 , 0.050000 = O(1) TO N(3) DISTANCE 1.440000 , 0.050000 = C(6) TO N(3) DISTANCE 1.390000 , 0.050000 = C(5) TO C(6) DISTANCE 1.364000 , 0.050000 = C(4) TO C(5) DISTANCE 1.222000 , 0.050000 = O(1) TO N(3) DISTANCE 1.232000 , 0.050000 = O(2) TO N(3) DISTANCE 1.440000 , 0.050000 = C(6) TO N(3) DISTANCE 1.392000 , 0.050000 = C(5) TO C(6) DISTANCE 1.364000 , 0.050000 = C(4) TO C(5) DISTANCE 1.391000 , 0.050000 = C(3) TO C(4) DISTANCE 1.371000 , 0.050000 = C(2) TO C(3) DISTANCE 1.400000 , 0.050000 = C(1) TO C(2) DISTANCE 1.408000 , 0.050000 = C(1) TO C(6) DISTANCE 1.382000 , 0.050000 = C(1) TO N(1) DISTANCE 1.387000 , 0.050000 = C(7) TO N(1) DISTANCE 1.728000 , 0.050000 = S(1) TO C(7) DISTANCE 1.724000 , 0.050000 = S(1) TO C(10) DISTANCE 1.500000 , 0.050000 = C(10) TO C(11) DISTANCE 1.349000 , 0.050000 = C(9) TO C(10) DISTANCE 1.427000 , 0.050000 = C(8) TO C(9) DISTANCE 1.372000 , 0.050000 = C(7) TO C(8) DISTANCE 1.422000 , 0.050000 = C(8) TO C(12) DISTANCE 1.141000 , 0.050000 = C(12) TO N(2) REM THERMSIM START (DO NOT REMOVE THIS LINE) U(IJ) .0, 0.04000 = S(1) TO C(7) U(IJ) .0, 0.04000 = S(1) TO C(10) U(IJ) .0, 0.08000 = O(1) TO N(3) U(IJ) .0, 0.08000 = O(2) TO N(3) U(IJ) .0, 0.04000 = C(1) TO C(2) U(IJ) .0, 0.04000 = C(1) TO C(6) U(IJ) .0, 0.04000 = C(1) TO N(1) U(IJ) .0, 0.04000 = C(2) TO C(3) U(IJ) .0, 0.04000 = C(3) TO C(4) U(IJ) .0, 0.04000 = C(4) TO C(5) U(IJ) .0, 0.04000 = C(5) TO C(6) U(IJ) .0, 0.04000 = C(6) TO N(3) U(IJ) .0, 0.04000 = C(7) TO C(8) U(IJ) .0, 0.04000 = C(7) TO N(1) U(IJ) .0, 0.04000 = C(8) TO C(9) U(IJ) .0, 0.04000 = C(8) TO C(12) U(IJ) .0, 0.04000 = C(9) TO C(10) U(IJ) .0, 0.08000 = C(10) TO C(11) U(IJ) .0, 0.08000 = C(12) TO N(2) REM THERMSIM END (DO NOT REMOVE THIS LINE) PLANAR 0.010000 C(1) C(6) N(1) H(1) PLANAR 0.010000 C(1) C(2) C(3) C(4) C(5) C(6) N(1) N(3) PLANAR 0.010000 S(1) C(7) C(8) C(9) C(10) N(1) 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 0 12 3 x . -1 6 1 x . 1 2 7 x . 0 2 5 x . # looking for ARCHIVE-HKL.CIF _iucr_refine_reflections_details ; # Data was input as F-squared # punching LIST 6 as LIST 6 with all keys set # NBGNXT= 36 #LIST 6 READ NCOEF= 8 TYPE=FIX, F'S = FSQ UNIT=DATA, CHECK=NO L30=NO ARCH=NO STORE NCOEF= 6 OUTPUT INDICES /FO/ SIGMA(/FO/) RATIO/JCODE CORRECTIONS SERIAL CONT INPUT H K L /FO/ SIGMA(/FO/) JCODE CONT CORRECTIONS SERIAL FOR (I4,I4,I4,F10.2,F8.2,F4.0,F7.4,F7.0) END 0 1 1 16.52 0.72 0. 1.0000 0. 0 -1 -2 128.75 5.22 0. 1.0000 0. 0 -1 -3 635.22 25.38 0. 1.0000 0. 0 -1 -4 180.14 8.40 0. 1.0000 0. 0 2 1 1666.05 65.50 0. 1.0000 0. 0 -2 -1 1688.27 65.46 0. 1.0000 0. 0 2 1 1670.79 65.44 0. 1.0000 0. 0 -2 -1 1713.32 65.54 0. 1.0000 0. 0 2 1 1680.52 65.41 0. 1.0000 0. 0 2 2 161.14 6.14 0. 1.0000 0. 0 -2 -2 166.57 6.24 0. 1.0000 0. 0 2 2 136.11 6.14 0. 1.0000 0. 0 -2 -2 166.42 6.11 0. 1.0000 0. 0 2 2 144.57 6.15 0. 1.0000 0. 0 -2 -2 173.89 6.15 0. 1.0000 0. 0 2 2 148.98 6.11 0. 1.0000 0. 0 2 2 145.30 6.08 0. 1.0000 0. 0 -2 -3 909.24 33.60 0. 1.0000 0. 0 -2 -3 877.26 33.47 0. 1.0000 0. 0 2 3 823.60 33.62 0. 1.0000 0. 0 2 3 784.30 33.70 0. 1.0000 0. 0 -2 -4 24.91 1.40 0. 1.0000 0. 0 -2 -4 22.00 1.40 0. 1.0000 0. 0 2 5 18.42 1.12 0. 1.0000 0. 0 -2 -5 0.11 0.71 0. 1.0000 0. 0 -2 -6 765.92 30.92 0. 1.0000 0. 0 -2 -7 0.09 1.19 0. 1.0000 0. 0 3 1 829.89 32.07 0. 1.0000 0. 0 -3 -1 837.79 31.82 0. 1.0000 0. 0 3 1 873.78 32.01 0. 1.0000 0. 0 -3 -1 766.11 31.69 0. 1.0000 0. 0 3 1 799.69 31.81 0. 1.0000 0. 0 3 2 96.74 4.08 0. 1.0000 0. 0 3 2 91.54 3.85 0. 1.0000 0. 0 -3 -2 93.25 3.86 0. 1.0000 0. 0 -3 -2 93.87 3.84 0. 1.0000 0. 0 -3 -2 105.74 4.05 0. 1.0000 0. 0 3 2 97.58 4.00 0. 1.0000 0. 0 -3 -2 94.88 3.76 0. 1.0000 0. 0 3 2 91.58 3.81 0. 1.0000 0. 0 -3 -2 99.04 4.01 0. 1.0000 0. 0 3 2 98.15 3.95 0. 1.0000 0. 0 3 2 96.43 3.90 0. 1.0000 0. 0 3 2 92.06 3.84 0. 1.0000 0. 0 3 3 4.15 0.42 0. 1.0000 0. 0 -3 -3 4.64 0.44 0. 1.0000 0. 0 -3 -3 4.85 0.44 0. 1.0000 0. 0 3 3 4.44 0.55 0. 1.0000 0. 0 3 3 4.43 0.42 0. 1.0000 0. 0 3 3 4.12 0.54 0. 1.0000 0. 0 3 3 5.09 0.36 0. 1.0000 0. 0 3 3 4.68 0.50 0. 1.0000 0. 0 3 3 4.11 0.48 0. 1.0000 0. 0 -3 -3 5.33 0.65 0. 1.0000 0. 0 3 4 57.39 3.08 0. 1.0000 0. 0 3 4 67.35 3.14 0. 1.0000 0. 0 3 4 65.55 3.01 0. 1.0000 0. 0 -3 -4 67.69 3.07 0. 1.0000 0. 0 -3 -4 72.71 2.90 0. 1.0000 0. 0 3 4 63.45 3.19 0. 1.0000 0. 0 -3 -4 78.09 2.94 0. 1.0000 0. 0 -3 -5 61.05 2.63 0. 1.0000 0. 0 -3 -5 57.26 2.30 0. 1.0000 0. 0 -3 -5 55.00 2.59 0. 1.0000 0. 0 -3 -5 53.54 2.51 0. 1.0000 0. 0 -3 -5 53.84 2.31 0. 1.0000 0. 0 -3 -6 1.48 1.22 0. 1.0000 0. 0 -3 -6 2.27 0.97 0. 1.0000 0. 0 -3 -6 1.47 0.83 0. 1.0000 0. 0 -3 -7 -0.84 1.36 0. 1.0000 0. 0 -3 -7 0.70 1.13 0. 1.0000 0. 0 -3 -7 0.68 1.29 0. 1.0000 0. 0 -3 -8 103.93 5.33 0. 1.0000 0. 0 -4 -1 0.84 0.48 0. 1.0000 0. 0 4 1 2.82 0.75 0. 1.0000 0. 0 4 1 3.44 1.05 0. 1.0000 0. 0 -4 -2 787.17 27.42 0. 1.0000 0. 0 -4 -2 684.76 27.05 0. 1.0000 0. 0 4 2 730.55 27.52 0. 1.0000 0. 0 4 2 641.05 27.14 0. 1.0000 0. 0 4 2 718.95 27.31 0. 1.0000 0. 0 4 2 681.61 27.06 0. 1.0000 0. 0 4 2 671.78 27.33 0. 1.0000 0. 0 4 3 26.36 1.45 0. 1.0000 0. 0 -4 -3 30.42 1.65 0. 1.0000 0. 0 -4 -3 33.37 1.70 0. 1.0000 0. 0 4 3 32.07 1.56 0. 1.0000 0. 0 4 3 30.72 1.50 0. 1.0000 0. 0 -4 -3 32.53 1.51 0. 1.0000 0. 0 -4 -3 35.22 1.40 0. 1.0000 0. 0 4 3 30.45 1.67 0. 1.0000 0. 0 4 3 34.82 1.83 0. 1.0000 0. 0 4 3 30.68 1.62 0. 1.0000 0. 0 -4 -3 36.03 1.53 0. 1.0000 0. 0 4 3 30.89 1.44 0. 1.0000 0. 0 4 4 1.30 0.43 0. 1.0000 0. 0 4 4 0.71 0.55 0. 1.0000 0. 0 -4 -4 2.37 0.82 0. 1.0000 0. 0 4 4 1.95 0.70 0. 1.0000 0. 0 4 4 1.41 0.51 0. 1.0000 0. 0 4 4 1.24 0.46 0. 1.0000 0. 0 -4 -4 1.97 0.52 0. 1.0000 0. 0 -4 -4 2.19 0.70 0. 1.0000 0. 0 4 4 1.58 0.63 0. 1.0000 0. 0 4 4 2.07 0.68 0. 1.0000 0. 0 -4 -4 1.96 0.47 0. 1.0000 0. 0 -4 -4 1.35 0.42 0. 1.0000 0. 0 4 4 1.77 0.34 0. 1.0000 0. 0 -4 -5 474.87 18.20 0. 1.0000 0. 0 -4 -5 485.25 18.23 0. 1.0000 0. 0 4 5 414.00 18.47 0. 1.0000 0. 0 -4 -5 481.01 18.39 0. 1.0000 0. 0 4 5 479.81 18.16 0. 1.0000 0. 0 4 5 491.63 18.36 0. 1.0000 0. 0 -4 -5 459.87 18.44 0. 1.0000 0. 0 -4 -6 251.35 9.59 0. 1.0000 0. 0 -4 -6 256.05 9.37 0. 1.0000 0. 0 -4 -6 245.43 9.69 0. 1.0000 0. 0 -4 -6 245.74 9.31 0. 1.0000 0. 0 -4 -6 248.23 9.61 0. 1.0000 0. 0 -4 -7 50.83 2.30 0. 1.0000 0. 0 -4 -7 55.58 2.38 0. 1.0000 0. 0 -4 -7 52.53 2.75 0. 1.0000 0. 0 -4 -7 63.11 2.91 0. 1.0000 0. 0 -4 -8 25.59 2.16 0. 1.0000 0. 0 -4 -8 25.42 2.27 0. 1.0000 0. 0 -4 -9 329.12 14.03 0. 1.0000 0. 0 -4 -10 -0.07 2.42 0. 1.0000 0. 0 -4 -10 -1.40 1.63 0. 1.0000 0. 0 5 1 91.61 5.18 0. 1.0000 0. 0 5 2 517.62 21.76 0. 1.0000 0. 0 -5 -2 552.75 21.85 0. 1.0000 0. 0 5 2 543.74 21.53 0. 1.0000 0. 0 5 2 591.12 22.29 0. 1.0000 0. 0 5 2 568.14 22.02 0. 1.0000 0. 0 5 2 512.28 21.89 0. 1.0000 0. 0 -5 -2 558.94 21.53 0. 1.0000 0. 0 5 3 219.26 8.99 0. 1.0000 0. 0 -5 -3 224.03 9.18 0. 1.0000 0. 0 5 3 242.48 9.23 0. 1.0000 0. 0 -5 -3 265.54 9.36 0. 1.0000 0. 0 5 3 218.39 8.97 0. 1.0000 0. 0 -5 -3 232.44 8.91 0. 1.0000 0. 0 -5 -3 214.47 8.95 0. 1.0000 0. 0 -5 -3 222.07 8.78 0. 1.0000 0. 0 5 3 212.50 8.90 0. 1.0000 0. 0 5 3 214.74 8.85 0. 1.0000 0. 0 5 4 162.08 6.71 0. 1.0000 0. 0 -5 -4 175.61 6.79 0. 1.0000 0. 0 5 4 153.26 6.65 0. 1.0000 0. 0 5 4 156.07 6.75 0. 1.0000 0. 0 -5 -4 174.83 6.76 0. 1.0000 0. 0 -5 -4 185.67 7.06 0. 1.0000 0. 0 5 4 169.64 7.02 0. 1.0000 0. 0 5 4 181.81 7.24 0. 1.0000 0. 0 -5 -5 261.47 10.67 0. 1.0000 0. 0 -5 -5 268.40 10.49 0. 1.0000 0. 0 5 5 273.04 10.80 0. 1.0000 0. 0 5 5 249.56 10.50 0. 1.0000 0. 0 5 5 258.49 10.30 0. 1.0000 0. 0 5 5 267.95 10.50 0. 1.0000 0. 0 -5 -5 256.81 10.43 0. 1.0000 0. 0 5 6 1.92 0.60 0. 1.0000 0. 0 -5 -6 2.29 0.83 0. 1.0000 0. 0 -5 -6 1.88 0.78 0. 1.0000 0. 0 -5 -6 -0.59 1.21 0. 1.0000 0. 0 -5 -6 3.37 1.33 0. 1.0000 0. 0 5 6 2.11 1.32 0. 1.0000 0. 0 5 6 2.21 0.84 0. 1.0000 0. 0 -5 -7 390.98 14.16 0. 1.0000 0. 0 -5 -7 409.19 13.70 0. 1.0000 0. 0 5 7 274.95 13.77 0. 1.0000 0. 0 -5 -7 411.72 14.07 0. 1.0000 0. 0 -5 -7 322.97 13.65 0. 1.0000 0. 0 5 7 280.80 13.55 0. 1.0000 0. 0 -5 -7 407.22 14.02 0. 1.0000 0. 0 -5 -8 -0.42 1.11 0. 1.0000 0. 0 5 8 -0.31 1.23 0. 1.0000 0. 0 -5 -8 -1.00 1.33 0. 1.0000 0. 0 -5 -9 73.02 3.58 0. 1.0000 0. 0 -5 -9 75.90 2.83 0. 1.0000 0. 0 -5 -9 69.98 3.41 0. 1.0000 0. 0 -5 -10 -1.36 2.45 0. 1.0000 0. 0 5 10 -0.06 2.20 0. 1.0000 0. 0 -5 -10 -0.73 1.64 0. 1.0000 0. 0 -5 -10 0.58 1.83 0. 1.0000 0. 0 5 11 -0.59 2.30 0. 1.0000 0. 0 -5 -11 3.03 1.80 0. 1.0000 0. 0 6 2 103.56 4.45 0. 1.0000 0. 0 6 2 110.12 5.58 0. 1.0000 0. 0 6 2 103.42 5.16 0. 1.0000 0. 0 6 3 47.73 2.46 0. 1.0000 0. 0 6 3 44.97 2.12 0. 1.0000 0. 0 6 3 46.01 2.86 0. 1.0000 0. 0 6 3 44.99 2.13 0. 1.0000 0. 0 6 3 50.03 2.69 0. 1.0000 0. 0 -6 -3 47.69 2.62 0. 1.0000 0. 0 -6 -3 47.81 2.16 0. 1.0000 0. 0 6 4 7.80 0.73 0. 1.0000 0. 0 6 4 6.32 1.04 0. 1.0000 0. 0 -6 -4 8.11 0.63 0. 1.0000 0. 0 -6 -4 8.16 0.79 0. 1.0000 0. 0 6 4 6.76 0.82 0. 1.0000 0. 0 -6 -4 7.49 0.89 0. 1.0000 0. 0 6 5 137.63 5.94 0. 1.0000 0. 0 6 5 121.22 5.45 0. 1.0000 0. 0 -6 -5 156.06 5.66 0. 1.0000 0. 0 6 5 137.20 5.60 0. 1.0000 0. 0 6 5 128.18 5.52 0. 1.0000 0. 0 6 6 14.59 1.22 0. 1.0000 0. 0 -6 -6 15.78 1.28 0. 1.0000 0. 0 -6 -6 15.53 1.63 0. 1.0000 0. 0 6 6 13.18 1.57 0. 1.0000 0. 0 6 6 14.77 1.41 0. 1.0000 0. 0 6 7 58.13 3.61 0. 1.0000 0. 0 6 7 61.94 2.82 0. 1.0000 0. 0 6 7 62.16 3.18 0. 1.0000 0. 0 -6 -7 73.12 3.48 0. 1.0000 0. 0 -6 -7 81.36 3.16 0. 1.0000 0. 0 6 7 54.76 3.56 0. 1.0000 0. 0 6 8 222.37 11.36 0. 1.0000 0. 0 6 8 226.38 11.11 0. 1.0000 0. 0 -6 -8 371.88 11.43 0. 1.0000 0. 0 -6 -8 363.51 12.03 0. 1.0000 0. 0 -6 -8 328.42 11.61 0. 1.0000 0. 0 -6 -9 41.81 2.50 0. 1.0000 0. 0 -6 -9 42.49 2.83 0. 1.0000 0. 0 6 9 12.91 1.56 0. 1.0000 0. 0 6 9 12.33 2.03 0. 1.0000 0. 0 -6 -10 63.83 2.82 0. 1.0000 0. 0 -6 -10 58.65 3.33 0. 1.0000 0. 0 -6 -10 65.73 3.60 0. 1.0000 0. 0 -6 -11 18.07 2.52 0. 1.0000 0. 0 -6 -11 18.46 2.13 0. 1.0000 0. 0 -6 -11 18.52 2.98 0. 1.0000 0. 0 6 12 -0.14 2.64 0. 1.0000 0. 0 -6 -12 3.86 2.98 0. 1.0000 0. 0 7 2 23.27 2.25 0. 1.0000 0. 0 -7 -2 26.58 1.66 0. 1.0000 0. 0 7 2 26.49 1.57 0. 1.0000 0. 0 7 2 25.91 2.87 0. 1.0000 0. 0 7 3 760.08 30.86 0. 1.0000 0. 0 7 3 807.44 31.25 0. 1.0000 0. 0 -7 -3 836.09 30.73 0. 1.0000 0. 0 -7 -3 747.15 30.06 0. 1.0000 0. 0 7 3 730.91 30.47 0. 1.0000 0. 0 7 4 267.77 11.41 0. 1.0000 0. 0 7 4 254.27 10.70 0. 1.0000 0. 0 7 4 263.78 11.10 0. 1.0000 0. 0 7 4 255.06 10.46 0. 1.0000 0. 0 7 4 249.28 10.39 0. 1.0000 0. 0 -7 -4 269.84 10.49 0. 1.0000 0. 0 -7 -4 266.23 10.31 0. 1.0000 0. 0 7 5 460.53 18.54 0. 1.0000 0. 0 7 5 475.95 19.09 0. 1.0000 0. 0 7 5 487.08 18.63 0. 1.0000 0. 0 7 5 462.18 18.73 0. 1.0000 0. 0 7 6 64.31 3.17 0. 1.0000 0. 0 -7 -6 86.10 3.87 0. 1.0000 0. 0 7 6 70.31 3.72 0. 1.0000 0. 0 7 6 69.77 3.24 0. 1.0000 0. 0 7 7 34.79 2.40 0. 1.0000 0. 0 7 7 34.72 2.52 0. 1.0000 0. 0 -7 -7 40.31 2.51 0. 1.0000 0. 0 7 7 34.95 2.10 0. 1.0000 0. 0 7 8 0.99 2.04 0. 1.0000 0. 0 7 8 2.57 1.24 0. 1.0000 0. 0 -7 -8 6.20 1.93 0. 1.0000 0. 0 -7 -8 4.63 1.71 0. 1.0000 0. 0 -7 -8 3.63 1.50 0. 1.0000 0. 0 7 8 4.50 0.85 0. 1.0000 0. 0 7 8 4.90 1.78 0. 1.0000 0. 0 -7 -9 34.39 2.01 0. 1.0000 0. 0 7 9 15.12 1.90 0. 1.0000 0. 0 7 9 16.18 1.39 0. 1.0000 0. 0 -7 -9 37.14 2.76 0. 1.0000 0. 0 7 9 13.36 2.40 0. 1.0000 0. 0 -7 -10 290.90 8.66 0. 1.0000 0. 0 -7 -10 277.73 7.73 0. 1.0000 0. 0 -7 -11 136.85 4.96 0. 1.0000 0. 0 -7 -11 136.10 4.42 0. 1.0000 0. 0 -7 -11 151.73 5.68 0. 1.0000 0. 0 -7 -12 36.54 4.05 0. 1.0000 0. 0 -7 -12 28.86 2.84 0. 1.0000 0. 0 7 13 -1.46 3.26 0. 1.0000 0. 0 -7 -13 165.09 5.88 0. 1.0000 0. 0 8 2 349.47 16.59 0. 1.0000 0. 0 8 3 705.16 26.67 0. 1.0000 0. 0 8 3 673.30 27.77 0. 1.0000 0. 0 8 3 700.83 28.36 0. 1.0000 0. 0 8 4 22.88 1.91 0. 1.0000 0. 0 -8 -4 25.73 2.12 0. 1.0000 0. 0 8 4 24.94 2.25 0. 1.0000 0. 0 -8 -4 23.90 1.30 0. 1.0000 0. 0 8 4 20.19 2.48 0. 1.0000 0. 0 8 4 23.21 1.44 0. 1.0000 0. 0 8 4 23.94 1.46 0. 1.0000 0. 0 -8 -4 27.99 2.38 0. 1.0000 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2.98 0. 1.0000 0. 3 12 6 5.65 3.06 0. 1.0000 0. -3 -12 -6 3.15 2.85 0. 1.0000 0. 3 12 7 -2.46 3.50 0. 1.0000 0. -3 13 7 0.98 4.79 0. 1.0000 0. -3 13 6 4.01 4.66 0. 1.0000 0. 3 -13 -6 4.91 3.85 0. 1.0000 0. 3 -13 -5 1.26 3.53 0. 1.0000 0. -3 -13 -2 3.45 3.40 0. 1.0000 0. -3 -13 -2 -1.21 2.95 0. 1.0000 0. 3 13 3 3.85 2.82 0. 1.0000 0. -3 -13 -3 -2.06 3.07 0. 1.0000 0. 3 13 4 5.73 3.15 0. 1.0000 0. -3 -13 -4 1.69 3.12 0. 1.0000 0. 3 13 5 11.87 3.31 0. 1.0000 0. -3 -13 -5 5.73 3.37 0. 1.0000 0. -3 -14 -2 -0.50 2.82 0. 1.0000 0. -3 -14 -2 -0.22 2.66 0. 1.0000 0. 3 14 3 3.25 2.89 0. 1.0000 0. -3 -14 -3 -1.52 3.28 0. 1.0000 0. -4 0 8 2.11 3.22 0. 1.0000 0. -4 0 7 -1.30 3.12 0. 1.0000 0. -4 0 6 3.06 2.66 0. 1.0000 0. 4 0 -5 4.24 3.45 0. 1.0000 0. -4 0 5 2.97 2.90 0. 1.0000 0. 4 0 -4 3.32 3.76 0. 1.0000 0. -4 0 4 1.45 2.51 0. 1.0000 0. 4 0 -3 4.90 4.43 0. 1.0000 0. -4 0 3 -2.42 2.74 0. 1.0000 0. 4 0 -2 1.00 4.65 0. 1.0000 0. -4 0 2 0.27 2.89 0. 1.0000 0. 4 0 -1 0.45 5.26 0. 1.0000 0. -4 0 1 -0.42 2.96 0. 1.0000 0. 4 0 0 18.92 6.26 0. 1.0000 0. -4 0 0 17.23 3.54 0. 1.0000 0. 4 0 1 -8.28 6.62 0. 1.0000 0. -4 0 -1 0.15 3.07 0. 1.0000 0. -4 0 -2 -1.27 3.35 0. 1.0000 0. 4 0 2 5.48 7.15 0. 1.0000 0. -4 0 -3 -0.89 3.10 0. 1.0000 0. 4 0 4 1.95 3.04 0. 1.0000 0. -4 0 -4 2.98 3.16 0. 1.0000 0. 4 0 5 -0.07 2.81 0. 1.0000 0. -4 0 -5 0.55 3.14 0. 1.0000 0. -4 1 8 0.57 3.33 0. 1.0000 0. -4 -1 8 -2.92 3.07 0. 1.0000 0. -4 1 7 -0.35 3.08 0. 1.0000 0. -4 -1 7 -0.17 2.93 0. 1.0000 0. 4 1 -6 5.17 2.61 0. 1.0000 0. -4 -1 6 0.47 2.73 0. 1.0000 0. -4 1 6 1.61 2.89 0. 1.0000 0. -4 -1 5 -0.95 2.72 0. 1.0000 0. 4 1 -5 -0.52 2.91 0. 1.0000 0. -4 1 5 1.13 3.00 0. 1.0000 0. 4 -1 -4 9.76 4.88 0. 1.0000 0. 4 1 -4 14.08 3.56 0. 1.0000 0. -4 1 4 0.70 2.99 0. 1.0000 0. -4 -1 4 1.90 2.54 0. 1.0000 0. 4 -1 -3 27.87 5.77 0. 1.0000 0. 4 1 -3 25.61 3.95 0. 1.0000 0. -4 1 3 8.07 3.24 0. 1.0000 0. -4 -1 3 7.98 2.78 0. 1.0000 0. 4 -1 -2 2.64 5.93 0. 1.0000 0. 4 1 -2 -2.66 3.98 0. 1.0000 0. -4 1 2 0.54 3.32 0. 1.0000 0. -4 -1 2 -1.40 2.75 0. 1.0000 0. 4 -1 -1 -1.94 6.12 0. 1.0000 0. 4 1 -1 0.38 4.67 0. 1.0000 0. -4 1 1 0.12 3.05 0. 1.0000 0. -4 -1 1 1.61 2.99 0. 1.0000 0. -4 1 0 3.44 3.00 0. 1.0000 0. 4 1 0 -0.14 5.22 0. 1.0000 0. -4 -1 0 -0.98 2.98 0. 1.0000 0. 4 -1 0 -1.39 6.32 0. 1.0000 0. 4 1 1 7.83 5.89 0. 1.0000 0. -4 1 -1 -2.43 3.03 0. 1.0000 0. 4 -1 1 -0.76 6.29 0. 1.0000 0. 4 1 2 3.16 6.46 0. 1.0000 0. 4 -1 2 3.05 3.24 0. 1.0000 0. -4 1 -2 4.25 3.04 0. 1.0000 0. -4 -1 -2 3.94 3.37 0. 1.0000 0. 4 -1 3 5.82 3.33 0. 1.0000 0. -4 1 -3 3.09 2.87 0. 1.0000 0. -4 -1 -3 5.84 3.55 0. 1.0000 0. 4 1 3 5.65 6.72 0. 1.0000 0. 4 -1 4 0.28 2.95 0. 1.0000 0. -4 1 -4 2.89 2.99 0. 1.0000 0. -4 -1 -4 2.13 3.21 0. 1.0000 0. 4 1 4 1.03 6.80 0. 1.0000 0. 4 -1 5 3.01 2.73 0. 1.0000 0. 4 1 5 -1.82 3.11 0. 1.0000 0. -4 1 -5 0.99 2.63 0. 1.0000 0. -4 -1 -5 1.38 3.34 0. 1.0000 0. -4 -1 -6 7.92 3.51 0. 1.0000 0. 4 2 -7 6.56 2.68 0. 1.0000 0. -4 -2 7 -0.96 2.91 0. 1.0000 0. -4 2 7 -0.47 3.24 0. 1.0000 0. 4 2 -6 1.57 2.70 0. 1.0000 0. -4 -2 6 -0.30 2.74 0. 1.0000 0. -4 2 6 0.62 2.95 0. 1.0000 0. 4 2 -5 11.16 2.96 0. 1.0000 0. -4 -2 5 3.02 2.71 0. 1.0000 0. -4 2 5 4.44 3.23 0. 1.0000 0. 4 -2 -4 -2.93 5.90 0. 1.0000 0. 4 2 -4 2.74 2.67 0. 1.0000 0. -4 2 4 0.57 3.18 0. 1.0000 0. -4 -2 4 0.81 2.40 0. 1.0000 0. 4 -2 -3 1.54 5.79 0. 1.0000 0. 4 2 -3 4.85 3.15 0. 1.0000 0. -4 2 3 0.73 3.25 0. 1.0000 0. -4 -2 3 3.04 2.36 0. 1.0000 0. 4 2 -2 -0.19 3.46 0. 1.0000 0. -4 2 2 0.12 3.50 0. 1.0000 0. -4 -2 2 2.47 2.57 0. 1.0000 0. 4 -2 -2 7.24 6.10 0. 1.0000 0. 4 2 -1 -2.26 4.02 0. 1.0000 0. -4 2 1 0.89 3.15 0. 1.0000 0. -4 -2 1 0.84 2.73 0. 1.0000 0. 4 -2 -1 6.66 6.69 0. 1.0000 0. 4 2 0 1.79 4.70 0. 1.0000 0. -4 -2 0 -3.18 2.95 0. 1.0000 0. -4 2 0 5.20 2.92 0. 1.0000 0. 4 2 1 5.62 5.47 0. 1.0000 0. 4 -2 1 8.06 3.46 0. 1.0000 0. -4 2 -1 5.47 3.00 0. 1.0000 0. 4 2 2 -2.35 6.05 0. 1.0000 0. -4 2 -2 0.45 1.50 0. 1.0000 0. 4 -2 2 1.24 3.13 0. 1.0000 0. -4 2 -2 1.15 2.78 0. 1.0000 0. 4 2 3 11.51 6.64 0. 1.0000 0. 4 -2 3 7.10 3.05 0. 1.0000 0. -4 2 -3 15.29 3.08 0. 1.0000 0. -4 -2 -3 12.75 3.61 0. 1.0000 0. 4 -2 4 -1.79 2.70 0. 1.0000 0. -4 2 -4 1.44 2.77 0. 1.0000 0. -4 -2 -4 1.80 3.64 0. 1.0000 0. 4 2 4 2.26 6.99 0. 1.0000 0. -4 -2 -5 7.28 3.61 0. 1.0000 0. 4 2 5 11.57 7.28 0. 1.0000 0. 4 3 -7 -0.56 2.43 0. 1.0000 0. -4 -3 7 -2.22 2.66 0. 1.0000 0. -4 3 7 -0.29 3.48 0. 1.0000 0. 4 3 -6 8.73 2.80 0. 1.0000 0. -4 -3 6 -1.01 2.57 0. 1.0000 0. -4 3 6 2.04 3.31 0. 1.0000 0. 4 3 -5 1.69 2.75 0. 1.0000 0. -4 -3 5 -2.19 2.68 0. 1.0000 0. -4 3 5 -0.41 3.53 0. 1.0000 0. -4 -3 4 -0.38 2.39 0. 1.0000 0. 4 3 -4 1.59 2.67 0. 1.0000 0. -4 3 4 0.11 3.44 0. 1.0000 0. 4 3 -3 -0.98 2.80 0. 1.0000 0. -4 3 3 3.69 3.32 0. 1.0000 0. -4 -3 3 0.06 2.21 0. 1.0000 0. 4 3 -2 0.16 2.79 0. 1.0000 0. -4 3 2 1.90 3.41 0. 1.0000 0. -4 -3 2 -0.68 2.42 0. 1.0000 0. -4 3 1 0.14 3.22 0. 1.0000 0. 4 3 -1 0.84 3.57 0. 1.0000 0. -4 -3 1 2.26 2.56 0. 1.0000 0. -4 3 1 -1.79 2.77 0. 1.0000 0. 4 3 0 0.33 4.13 0. 1.0000 0. 4 -3 0 1.48 3.31 0. 1.0000 0. -4 3 0 4.41 3.00 0. 1.0000 0. -4 3 -1 -1.95 1.65 0. 1.0000 0. 4 3 1 4.38 4.70 0. 1.0000 0. 4 -3 1 -2.09 3.55 0. 1.0000 0. -4 3 -1 -0.39 2.69 0. 1.0000 0. -4 3 -2 6.59 1.84 0. 1.0000 0. 4 3 2 12.06 5.52 0. 1.0000 0. 4 -3 2 6.10 3.13 0. 1.0000 0. -4 3 -2 7.09 2.76 0. 1.0000 0. -4 3 -3 0.19 1.65 0. 1.0000 0. 4 3 3 2.38 5.94 0. 1.0000 0. 4 -3 3 0.93 3.01 0. 1.0000 0. -4 3 -3 -0.47 2.65 0. 1.0000 0. 4 3 4 -0.37 6.58 0. 1.0000 0. -4 -3 -4 -0.45 3.74 0. 1.0000 0. -4 -3 -5 3.85 3.79 0. 1.0000 0. 4 3 5 1.17 6.94 0. 1.0000 0. -4 4 7 0.40 3.42 0. 1.0000 0. 4 4 -6 0.94 2.46 0. 1.0000 0. -4 4 6 -1.23 4.04 0. 1.0000 0. -4 -4 6 0.21 2.46 0. 1.0000 0. 4 4 -5 0.08 2.70 0. 1.0000 0. -4 -4 5 -0.64 2.41 0. 1.0000 0. -4 -4 4 0.31 2.35 0. 1.0000 0. 4 4 -4 6.87 2.84 0. 1.0000 0. -4 4 4 -1.18 3.75 0. 1.0000 0. 4 4 -3 -2.13 2.85 0. 1.0000 0. -4 4 3 1.50 3.96 0. 1.0000 0. -4 -4 3 -2.13 2.23 0. 1.0000 0. -4 4 2 -2.69 3.77 0. 1.0000 0. 4 4 -2 4.51 2.78 0. 1.0000 0. -4 -4 2 -0.88 2.22 0. 1.0000 0. -4 4 1 0.75 3.21 0. 1.0000 0. 4 4 -1 -1.02 3.05 0. 1.0000 0. 4 -4 -1 -2.78 3.76 0. 1.0000 0. -4 4 0 -0.44 1.71 0. 1.0000 0. 4 4 0 -0.78 3.61 0. 1.0000 0. 4 -4 0 -2.52 3.32 0. 1.0000 0. -4 4 0 -0.79 2.59 0. 1.0000 0. -4 4 -1 4.57 1.85 0. 1.0000 0. 4 4 1 4.17 4.05 0. 1.0000 0. 4 -4 1 4.94 3.43 0. 1.0000 0. -4 4 -1 0.31 2.66 0. 1.0000 0. -4 4 -2 2.53 1.87 0. 1.0000 0. 4 4 2 -3.17 5.20 0. 1.0000 0. 4 -4 2 2.09 3.11 0. 1.0000 0. -4 4 -2 0.70 2.57 0. 1.0000 0. 4 4 3 0.29 5.52 0. 1.0000 0. 4 4 4 9.02 6.54 0. 1.0000 0. 4 4 5 -6.36 6.87 0. 1.0000 0. -4 -4 -5 2.66 3.84 0. 1.0000 0. 4 5 -6 -1.11 2.20 0. 1.0000 0. -4 5 6 2.43 4.06 0. 1.0000 0. 4 5 -5 -0.91 2.59 0. 1.0000 0. -4 5 5 5.27 4.20 0. 1.0000 0. -4 -5 5 0.51 2.38 0. 1.0000 0. 4 5 -4 1.80 2.68 0. 1.0000 0. -4 5 4 -1.79 3.97 0. 1.0000 0. -4 -5 4 -0.06 2.34 0. 1.0000 0. -4 5 3 10.82 4.16 0. 1.0000 0. 4 5 -3 10.96 3.10 0. 1.0000 0. -4 5 2 -0.31 3.66 0. 1.0000 0. 4 5 -2 0.33 2.93 0. 1.0000 0. 4 5 -1 4.28 2.95 0. 1.0000 0. 4 -5 -1 3.77 3.82 0. 1.0000 0. -4 5 0 0.72 1.90 0. 1.0000 0. 4 5 0 3.54 3.24 0. 1.0000 0. 4 -5 0 0.91 3.47 0. 1.0000 0. -4 5 0 1.18 2.54 0. 1.0000 0. -4 5 -1 -2.45 1.96 0. 1.0000 0. 4 5 1 5.26 3.81 0. 1.0000 0. 4 -5 1 -4.03 3.17 0. 1.0000 0. -4 5 -1 -0.84 2.50 0. 1.0000 0. 4 5 3 2.86 5.53 0. 1.0000 0. 4 5 4 -1.37 5.45 0. 1.0000 0. 4 6 -5 -1.39 2.41 0. 1.0000 0. -4 6 5 3.80 4.14 0. 1.0000 0. -4 -6 5 0.06 2.04 0. 1.0000 0. 4 6 -4 -0.47 2.67 0. 1.0000 0. -4 6 4 2.86 4.08 0. 1.0000 0. -4 6 3 0.95 4.03 0. 1.0000 0. 4 6 -3 -3.85 2.98 0. 1.0000 0. -4 6 2 15.82 4.30 0. 1.0000 0. 4 6 -2 15.71 3.25 0. 1.0000 0. 4 -6 -2 17.41 4.02 0. 1.0000 0. -4 6 1 3.32 2.00 0. 1.0000 0. 4 6 -1 4.87 2.94 0. 1.0000 0. 4 -6 -1 1.18 3.75 0. 1.0000 0. 4 6 0 1.44 2.98 0. 1.0000 0. 4 6 1 1.84 3.35 0. 1.0000 0. 4 6 2 2.78 4.21 0. 1.0000 0. 4 6 3 -4.26 4.69 0. 1.0000 0. -4 7 4 16.96 4.76 0. 1.0000 0. 4 7 -4 -0.56 2.45 0. 1.0000 0. -4 7 3 2.80 4.34 0. 1.0000 0. 4 7 -3 -1.16 2.82 0. 1.0000 0. -4 7 2 0.62 2.06 0. 1.0000 0. 4 7 -2 -1.96 3.03 0. 1.0000 0. 4 -7 -2 -1.52 3.91 0. 1.0000 0. -4 7 1 15.11 2.54 0. 1.0000 0. 4 7 -1 16.43 3.45 0. 1.0000 0. -4 7 0 0.74 2.02 0. 1.0000 0. 4 7 0 1.25 3.12 0. 1.0000 0. 4 -7 0 -1.46 3.27 0. 1.0000 0. 4 7 1 8.64 3.22 0. 1.0000 0. 4 7 2 8.56 3.90 0. 1.0000 0. -4 8 2 2.01 2.32 0. 1.0000 0. 4 8 -2 1.57 3.02 0. 1.0000 0. -4 8 1 1.09 2.09 0. 1.0000 0. 4 8 -1 0.99 3.05 0. 1.0000 0. 4 -8 -1 0.37 3.39 0. 1.0000 0. 4 8 0 -0.73 3.07 0. 1.0000 0. -512 # 4050 reflections output ; # end of ARCHIVE-HKL.CIF _chemical_name_common ROY _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: acetone' ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_ROY_ON_0p62GPa _database_code_depnum_ccdc_archive 'CCDC 2098637' loop_ _audit_author_name _audit_author_address 'Nicholas Funnell' ;STFC, ISIS Neutron Facility United Kingdom ; _audit_update_record ; 2021-07-22 deposited with the CCDC. 2021-08-27 downloaded from the CCDC. ; _audit_creation_date 2021-01-25 _audit_creation_method 'CRYSTALS_ver_14.61_build_7795 ' _chemical_name_systematic ; 5-methyl-2[(2-nitrophenyl)amino]-3-thiophenecarbonitrile ; # CheckCIF alerts _vrf_THETM01_ROY_ON_0p62GPa ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575 RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT027_ROY_ON_0p62GPa ; PROBLEM: _diffrn_reflns_theta_full value (too) Low ...... 17.44 Degree RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT029_ROY_ON_0p62GPa ; PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.725 Why? RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT201_ROY_ON_0p62GPa ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 17 Report RESPONSE: The model could only be refined isotropically in order to maintain a favourable data-to-parameter ratio, due to numerous unmeasured reflections. The relatively electron-rich sulfur atom has been modelled anisotropically. ; _vrf_PLAT911_ROY_ON_0p62GPa ; PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.556 425 Report RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT082_ROY_ON_0p62GPa ; PROBLEM: High R1 Value .................................. 0.11 Report RESPONSE: These are poor-quality diffraction data and the model has only been refined isotropically. ; _vrf_PLAT340_ROY_ON_0p62GPa ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.00864 Ang. RESPONSE: These are poor-quality diffraction data. ; _vrf_PLAT910_ROY_ON_0p62GPa ; PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 8 Note RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; # end Validation Reply Form _refine_special_details ; In the absence of significant anomalous scattering, Friedel pairs were merged. Data were collected in a Merrill-Bassett diamond anvil cell, which significantly restricts the regions over which reciprocal space can be sampled. Thus, these data are poor quality/incomplete, reflected in numerous CheckCIF alerts regarding refinement statistics. At all pressures, the atomic connectivity is known. All non-sulfur atoms were refined isotropically; sulfur was refined anisotropically. Hydrogen atoms were constrained to ride on their host atoms. #=============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Total Missing #------------------------------------------------------------------------------- 20.82 0.500 0.725 1161 842 319 23.01 0.550 0.715 1486 1062 424 23.25 0.556 0.717 1528 1095 433 ------------------------------------------------------------ ACTA Min. Res. --- Note: The Reported Completeness refers to the Actual H,K,L Index Range ; #end of refcif _cell_length_a 3.767380(17) _cell_length_b 18.14088(5) _cell_length_c 16.22092(5) _cell_angle_alpha 90 _cell_angle_beta 91.918(5) _cell_angle_gamma 90 _cell_volume 1107.975(8) _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' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 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' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C12 H9 N3 O2 S1 # Dc = 1.55 Fooo = 536.00 Mu = 2.89 M = 259.29 # Found Formula = C12 H9 N3 O2 S1 # Dc = 1.55 FOOO = 536.00 Mu = 2.89 M = 259.29 _chemical_formula_sum 'C12 H9 N3 O2 S1' _chemical_formula_moiety 'C12 H9 N3 O2 S1' _chemical_compound_source 'TCI Chemicals' _chemical_formula_weight 259.29 _cell_measurement_reflns_used 1869 _cell_measurement_theta_min 1.68 _cell_measurement_theta_max 23.25 _cell_measurement_temperature 293 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_min 0.050 _exptl_crystal_size_mid 0.072 _exptl_crystal_size_max 0.248 _exptl_crystal_density_diffrn 1.554 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 0.289 # Sheldrick geometric approximatio 0.98 0.99 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North et al., 1968)' _exptl_absorpt_correction_T_min 0.19 _exptl_absorpt_correction_T_max 0.99 _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_device 'four-circle diffractometer' _diffrn_radiation_monochromator mirror _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 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction ; CrysAlisPro (Rigaku Oxford Diffraction, 2017) ; _computing_structure_solution 'Model from previously-determined structure' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 293 _diffrn_ambient_pressure 620000 _diffrn_reflns_number 3792 _diffrn_reflns_av_unetI/netI 0.056 _reflns_number_total 1103 _diffrn_reflns_av_R_equivalents 0.053 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 1103 # Theoretical number of reflections is about 3182 _diffrn_reflns_theta_min 1.685 _diffrn_reflns_theta_max 23.254 _diffrn_measured_fraction_theta_max 0.693 _diffrn_reflns_theta_full 17.441 _diffrn_measured_fraction_theta_full 0.725 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _reflns_limit_h_min -4 _reflns_limit_h_max 4 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _oxford_diffrn_Wilson_B_factor 4.25 _oxford_diffrn_Wilson_scale 3.44 _atom_sites_solution_primary geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.85 _refine_diff_density_max 0.90 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # Explicitly named reflections are ALWAYS excluded from R&wR # The values actually used during refinement # These are labelled "all" for compatibility with PLATON _oxford_refine_reflns_threshold_expression I>-3.0\s(I) _refine_ls_number_restraints 94 _refine_ls_number_parameters 82 _refine_ls_number_reflns 1095 _oxford_refine_ls_R_factor_ref 0.1839 _refine_ls_R_factor_all 0.1839 _refine_ls_wR_factor_ref 0.0626 _refine_ls_wR_factor_all 0.0626 _refine_ls_goodness_of_fit_ref 1.0629 _refine_ls_shift/su_max 0.0001897 _refine_ls_shift/su_mean 0.0000619 # Computed with I/sigma = -10 _oxford_reflns_number_all 1095 _oxford_refine_ls_R_factor_all 0.1839 _oxford_refine_ls_wR_factor_all 0.0626 # Computed with no filters except I/sigma = +2 a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 738 _refine_ls_R_factor_gt 0.1117 _refine_ls_wR_factor_gt 0.0577 _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed #undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ; Method= SQRT(W) = 1/(Data with the key SIGMA(/FO/) in list 6) ; # 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 S1 S 0.7817(4) 0.59321(9) 0.43128(10) 0.0482 1.0000 Uani D U . . . . O1 O 0.4916(10) 0.6243(2) 0.0256(3) 0.0652(14) 1.0000 Uiso D U . . . . O2 O 0.5497(10) 0.6937(2) 0.1348(3) 0.0637(13) 1.0000 Uiso D U . . . . C1 C 0.8947(12) 0.5821(4) 0.2213(4) 0.0503(14) 1.0000 Uiso D U . . . . C2 C 1.0860(12) 0.5205(3) 0.2601(4) 0.0488(14) 1.0000 Uiso D U . . . . C3 C 1.1432(13) 0.4591(3) 0.2123(4) 0.0493(15) 1.0000 Uiso D U . . . . C4 C 1.0185(13) 0.4541(3) 0.1306(4) 0.0502(14) 1.0000 Uiso D U . . . . C5 C 0.8441(12) 0.5130(3) 0.0963(4) 0.0530(15) 1.0000 Uiso D U . . . . C6 C 0.7775(13) 0.5768(4) 0.1401(4) 0.0500(14) 1.0000 Uiso D U . . . . C7 C 0.9127(13) 0.6535(3) 0.3557(5) 0.0487(14) 1.0000 Uiso D U . . . . C8 C 1.0722(13) 0.7142(3) 0.3889(4) 0.0479(14) 1.0000 Uiso D U . . . . C9 C 1.0780(13) 0.7119(3) 0.4764(4) 0.0491(14) 1.0000 Uiso D U . . . . C10 C 0.9308(9) 0.6497(3) 0.5087(4) 0.0513(14) 1.0000 Uiso D U . . . . C11 C 0.9077(9) 0.6332(3) 0.5966(4) 0.0578(16) 1.0000 Uiso D U . . . . C12 C 1.2298(14) 0.7642(4) 0.3367(4) 0.0504(14) 1.0000 Uiso D U . . . . N1 N 0.8452(10) 0.6418(3) 0.2721(4) 0.0503(13) 1.0000 Uiso D U . . . . N2 N 1.3646(11) 0.8059(3) 0.2909(4) 0.0546(14) 1.0000 Uiso D U . . . . N3 N 0.5908(12) 0.6350(3) 0.0975(4) 0.0570(14) 1.0000 Uiso D U . . . . H1 H 0.726(6) 0.6785(16) 0.2477(19) 0.062(3) 1.0000 Uiso D . . . . . H2 H 1.1674 0.5234 0.3146 0.0611 1.0000 Uiso R . . . . . H3 H 1.2714 0.4203 0.2355 0.0630 1.0000 Uiso R . . . . . H4 H 1.0557 0.4110 0.1011 0.0639 1.0000 Uiso R . . . . . H5 H 0.7665 0.5107 0.0417 0.0631 1.0000 Uiso R . . . . . H9 H 1.1788 0.7489 0.5098 0.0621 1.0000 Uiso R . . . . . H111 H 1.0934 0.6001 0.6130 0.1160 1.0000 Uiso DR . . . . . H112 H 0.9321 0.6779 0.6277 0.1160 1.0000 Uiso DR . . . . . H113 H 0.6829 0.6109 0.6066 0.1160 1.0000 Uiso DR . . . . . 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 S1 0.0540(8) 0.0345(14) 0.0555(18) 0.0054(8) -0.0073(8) -0.0030(7) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.523(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 S1 . C7 . 1.727(7) yes S1 . C10 . 1.702(6) yes O1 . N3 . 1.229(6) yes O2 . N3 . 1.237(6) yes C1 . C2 . 1.460(9) yes C1 . C6 . 1.379(7) yes C1 . N1 . 1.377(8) yes C2 . C3 . 1.380(7) yes C2 . H2 . 0.927 no C3 . C4 . 1.393(8) yes C3 . H3 . 0.926 no C4 . C5 . 1.364(7) yes C4 . H4 . 0.931 no C5 . C6 . 1.386(8) yes C5 . H5 . 0.924 no C6 . N3 . 1.432(8) yes C7 . C8 . 1.357(8) yes C7 . N1 . 1.387(8) yes C8 . C9 . 1.420(7) yes C8 . C12 . 1.389(7) yes C9 . C10 . 1.368(7) yes C9 . H9 . 0.936 no C10 . C11 . 1.463(8) yes C11 . H112 . 0.956 no C11 . H113 . 0.958 no C11 . H111 . 0.953 no C12 . N2 . 1.185(7) yes N1 . H1 . 0.89(3) 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 C7 . S1 . C10 . 92.7(3) yes C2 . C1 . C6 . 119.8(6) yes C2 . C1 . N1 . 114.7(7) yes C6 . C1 . N1 . 125.5(5) yes C1 . C2 . C3 . 117.3(7) yes C1 . C2 . H2 . 120.7 no C3 . C2 . H2 . 121.9 no C2 . C3 . C4 . 122.2(5) yes C2 . C3 . H3 . 118.3 no C4 . C3 . H3 . 119.5 no C3 . C4 . C5 . 118.7(6) yes C3 . C4 . H4 . 119.4 no C5 . C4 . H4 . 121.8 no C4 . C5 . C6 . 122.5(7) yes C4 . C5 . H5 . 119.2 no C6 . C5 . H5 . 118.3 no C5 . C6 . C1 . 119.3(5) yes C5 . C6 . N3 . 117.5(7) yes C1 . C6 . N3 . 123.1(6) yes S1 . C7 . C8 . 111.4(6) yes S1 . C7 . N1 . 123.3(4) yes C8 . C7 . N1 . 125.2(6) yes C7 . C8 . C9 . 111.4(5) yes C7 . C8 . C12 . 118.8(7) yes C9 . C8 . C12 . 129.5(6) yes C8 . C9 . C10 . 114.5(5) yes C8 . C9 . H9 . 123.4 no C10 . C9 . H9 . 122.1 no C9 . C10 . S1 . 110.0(5) yes C9 . C10 . C11 . 125.4(4) yes S1 . C10 . C11 . 124.6(2) yes C10 . C11 . H112 . 109.4 no C10 . C11 . H113 . 109.4 no H112 . C11 . H113 . 109.8 no C10 . C11 . H111 . 109.4 no H112 . C11 . H111 . 109.3 no H113 . C11 . H111 . 109.4 no C8 . C12 . N2 . 178.6(8) yes C7 . N1 . C1 . 132.9(6) yes C7 . N1 . H1 . 113(2) no C1 . N1 . H1 . 114(2) no C6 . N3 . O2 . 117.8(7) yes C6 . N3 . O1 . 118.0(5) yes O2 . N3 . O1 . 124.1(5) yes _iucr_refine_instructions_details ; # # Punched on 25/01/21 at 13:00:06 # #LIST 12 BLOCK CONT SCALE CONT S ( 1 ,X'S,U'S) CONT O ( 1 ,X'S,U[ISO]) UNTIL N ( 3 ) CONT H ( 1 ,X'S,U[ISO]) RIDE C ( 2,X'S) H ( 2,X'S) RIDE C ( 3,X'S) H ( 3,X'S) RIDE C ( 4,X'S) H ( 4,X'S) RIDE C ( 5,X'S) H ( 5,X'S) RIDE C ( 9,X'S) H ( 9,X'S) RIDE C ( 11,X'S) H ( 112,X'S) H ( 113,X'S) H ( 111,X'S) END # # Punched on 25/01/21 at 13:00:06 # #LIST 16 NO REM REM NPF NOTE - FIRST UNTIL LAST REM REM HREST START (DO NOT REMOVE THIS LINE) REM NO H NO #H U MULT DIST REM C-H REM >4 1.5 .96 DISORDER REM 1 1 1.2 .93 C C-H (ACETYLENE) REM 1 2 1.2 .93 C-C(H)-C REM 1 3 1.2 .98 (C)3-C-H REM 2 1 1.2 .93 C=C-H(2) REM 2 2 1.2 .97 (C)2-C-(H)2 REM 3 1 1.5 .96 C-C-(H)3 REM N-H REM >4 1.5 .89 DISORDER REM 1 1 1.2 .86 N-N/H REM 1 2 1.2 .86 (C)2-N-H REM 1 3 1.2 .89 (C)3-N-H REM 2 1 1.2 .86 C-N-(H)2 REM 2 2 1.2 .89 (C)2-N-(H)2 REM 3 1 1.2 .89 C-H-(H)3 REM O-H REM 1 1 1.5 .82 O-H REM REM DIST ESD = 0.02 REM VIB ESD = 0.002 REM ANGLE ESD = 2.0 REM REM TO ACTIVATE THE VIB RESTRAINTS, REMOVE LEADING REM REM H1-N-R2 DIST 0.86, 0.02 = CONT N ( 1) TO H(1) REST 0.062, 0.002 = H(1,U[ISO]) ANGLE 0.0, 2.0 = MEAN CONT H(1) TO N ( 1) TO C(7) CONT H(1) TO N ( 1) TO C(1) REM HREST END (DO NOT REMOVE THIS LINE) REM DELU START (DO NOT REMOVE THIS LINE) VIBR .0, 0.00200 = S(1) TO C(10) VIBR .0, 0.00200 = S(1) TO C(7) VIBR .0, 0.00500 = C(7) TO C(10) VIBR .0, 0.00200 = N(2) TO C(12) VIBR .0, 0.00200 = C(10) TO C(9) VIBR .0, 0.00200 = C(10) TO C(11) VIBR .0, 0.00500 = C(9) TO S(1) VIBR .0, 0.00500 = C(11) TO S(1) VIBR .0, 0.00500 = C(11) TO C(9) VIBR .0, 0.00200 = C(12) TO C(8) VIBR .0, 0.00500 = C(8) TO N(2) VIBR .0, 0.00200 = O(1) TO N(3) VIBR .0, 0.00200 = C(2) TO C(1) VIBR .0, 0.00200 = C(2) TO C(3) VIBR .0, 0.00500 = C(3) TO C(1) VIBR .0, 0.00200 = N(1) TO C(7) VIBR .0, 0.00200 = N(1) TO C(1) VIBR .0, 0.00500 = C(1) TO C(7) VIBR .0, 0.00200 = C(7) TO C(8) VIBR .0, 0.00500 = N(1) TO S(1) VIBR .0, 0.00500 = C(8) TO S(1) VIBR .0, 0.00500 = C(8) TO N(1) VIBR .0, 0.00200 = O(2) TO N(3) VIBR .0, 0.00200 = N(3) TO C(6) VIBR .0, 0.00500 = O(1) TO O(2) VIBR .0, 0.00500 = C(6) TO O(2) VIBR .0, 0.00500 = C(6) TO O(1) VIBR .0, 0.00200 = C(5) TO C(4) VIBR .0, 0.00200 = C(5) TO C(6) VIBR .0, 0.00500 = C(6) TO C(4) VIBR .0, 0.00200 = C(4) TO C(3) VIBR .0, 0.00500 = C(3) TO C(5) VIBR .0, 0.00200 = C(1) TO C(6) VIBR .0, 0.00500 = N(1) TO C(2) VIBR .0, 0.00500 = C(6) TO C(2) VIBR .0, 0.00500 = C(6) TO N(1) VIBR .0, 0.00500 = C(5) TO N(3) VIBR .0, 0.00500 = C(1) TO N(3) VIBR .0, 0.00500 = C(1) TO C(5) VIBR .0, 0.00200 = C(9) TO C(8) VIBR .0, 0.00500 = C(8) TO C(10) VIBR .0, 0.00500 = C(2) TO C(4) VIBR .0, 0.00500 = C(12) TO C(9) VIBR .0, 0.00500 = C(7) TO C(9) VIBR .0, 0.00500 = C(7) TO C(12) REM DELU END (DO NOT REMOVE THIS LINE) ANGLE 110.000000 , 0.020000 = C(10) TO C(11) TO H(111) ANGLE 110.000000 , 0.020000 = C(10) TO C(11) TO H(112) ANGLE 110.000000 , 0.020000 = C(10) TO C(11) TO H(113) DISTANCE 1.225000 , 0.050000 = O(2) TO N(3) DISTANCE 1.225000 , 0.050000 = O(1) TO N(3) DISTANCE 1.440000 , 0.050000 = C(6) TO N(3) DISTANCE 1.390000 , 0.050000 = C(5) TO C(6) DISTANCE 1.364000 , 0.050000 = C(4) TO C(5) DISTANCE 1.222000 , 0.050000 = O(1) TO N(3) DISTANCE 1.232000 , 0.050000 = O(2) TO N(3) DISTANCE 1.440000 , 0.050000 = C(6) TO N(3) DISTANCE 1.392000 , 0.050000 = C(5) TO C(6) DISTANCE 1.364000 , 0.050000 = C(4) TO C(5) DISTANCE 1.391000 , 0.050000 = C(3) TO C(4) DISTANCE 1.371000 , 0.050000 = C(2) TO C(3) DISTANCE 1.400000 , 0.050000 = C(1) TO C(2) DISTANCE 1.408000 , 0.050000 = C(1) TO C(6) DISTANCE 1.382000 , 0.050000 = C(1) TO N(1) DISTANCE 1.387000 , 0.050000 = C(7) TO N(1) DISTANCE 1.728000 , 0.050000 = S(1) TO C(7) DISTANCE 1.724000 , 0.050000 = S(1) TO C(10) DISTANCE 1.500000 , 0.050000 = C(10) TO C(11) DISTANCE 1.349000 , 0.050000 = C(9) TO C(10) DISTANCE 1.427000 , 0.050000 = C(8) TO C(9) DISTANCE 1.372000 , 0.050000 = C(7) TO C(8) DISTANCE 1.422000 , 0.050000 = C(8) TO C(12) DISTANCE 1.141000 , 0.050000 = C(12) TO N(2) REM THERMSIM START (DO NOT REMOVE THIS LINE) U(IJ) .0, 0.04000 = S(1) TO C(7) U(IJ) .0, 0.04000 = S(1) TO C(10) U(IJ) .0, 0.08000 = O(1) TO N(3) U(IJ) .0, 0.08000 = O(2) TO N(3) U(IJ) .0, 0.04000 = C(1) TO C(2) U(IJ) .0, 0.04000 = C(1) TO C(6) U(IJ) .0, 0.04000 = C(1) TO N(1) U(IJ) .0, 0.04000 = C(2) TO C(3) U(IJ) .0, 0.04000 = C(3) TO C(4) U(IJ) .0, 0.04000 = C(4) TO C(5) U(IJ) .0, 0.04000 = C(5) TO C(6) U(IJ) .0, 0.04000 = C(6) TO N(3) U(IJ) .0, 0.04000 = C(7) TO C(8) U(IJ) .0, 0.04000 = C(7) TO N(1) U(IJ) .0, 0.04000 = C(8) TO C(9) U(IJ) .0, 0.04000 = C(8) TO C(12) U(IJ) .0, 0.04000 = C(9) TO C(10) U(IJ) .0, 0.08000 = C(10) TO C(11) U(IJ) .0, 0.08000 = C(12) TO N(2) REM THERMSIM END (DO NOT REMOVE THIS LINE) PLANAR 0.010000 C(1) C(6) N(1) H(1) PLANAR 0.010000 C(1) C(2) C(3) C(4) C(5) C(6) N(1) N(3) PLANAR 0.010000 S(1) C(7) C(8) C(9) C(10) N(1) 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 0 2 6 x . 1 5 11 x . # looking for ARCHIVE-HKL.CIF _iucr_refine_reflections_details ; # Data was input as F-squared # punching LIST 6 as LIST 6 with all keys set # NBGNXT= 36 #LIST 6 READ NCOEF= 8 TYPE=FIX, F'S = FSQ UNIT=DATA, CHECK=NO L30=NO ARCH=NO STORE NCOEF= 6 OUTPUT INDICES /FO/ SIGMA(/FO/) RATIO/JCODE CORRECTIONS SERIAL CONT INPUT H K L /FO/ SIGMA(/FO/) JCODE CONT CORRECTIONS SERIAL FOR (I4,I4,I4,F10.2,F8.2,F4.0,F7.4,F7.0) END 0 -1 1 15.70 0.67 0. 1.0000 0. 0 -1 1 16.68 0.69 0. 1.0000 0. 0 1 -1 16.88 0.70 0. 1.0000 0. 0 -1 2 156.97 5.69 0. 1.0000 0. 0 -1 2 163.80 5.74 0. 1.0000 0. 0 -1 3 807.37 28.17 0. 1.0000 0. 0 -2 1 2220.71 75.53 0. 1.0000 0. 0 2 -1 2227.54 75.59 0. 1.0000 0. 0 2 -1 2226.33 75.69 0. 1.0000 0. 0 2 -2 151.87 5.32 0. 1.0000 0. 0 -2 2 157.74 5.31 0. 1.0000 0. 0 2 -2 150.01 5.46 0. 1.0000 0. 0 -2 2 152.99 5.32 0. 1.0000 0. 0 -2 2 157.99 5.48 0. 1.0000 0. 0 2 -2 161.43 5.47 0. 1.0000 0. 0 2 -2 139.71 5.41 0. 1.0000 0. 0 -2 3 1005.54 33.98 0. 1.0000 0. 0 -2 3 1038.79 34.00 0. 1.0000 0. 0 2 -3 966.42 34.01 0. 1.0000 0. 0 -2 3 974.01 33.85 0. 1.0000 0. 0 -2 4 34.27 1.71 0. 1.0000 0. 0 -2 5 563.12 19.83 0. 1.0000 0. 0 -2 6 0.05 0.67 0. 1.0000 0. 0 3 -1 827.38 28.01 0. 1.0000 0. 0 3 -1 790.46 27.73 0. 1.0000 0. 0 3 -2 90.26 3.33 0. 1.0000 0. 0 3 -2 80.13 3.21 0. 1.0000 0. 0 3 -2 92.03 3.31 0. 1.0000 0. 0 3 -2 76.84 3.17 0. 1.0000 0. 0 3 -2 87.03 3.08 0. 1.0000 0. 0 3 -2 92.13 3.39 0. 1.0000 0. 0 3 -3 3.99 0.53 0. 1.0000 0. 0 3 -3 4.29 0.71 0. 1.0000 0. 0 -3 3 3.81 0.65 0. 1.0000 0. 0 3 -3 3.61 0.56 0. 1.0000 0. 0 -3 3 4.51 0.52 0. 1.0000 0. 0 3 -3 5.14 0.81 0. 1.0000 0. 0 3 -3 3.87 0.48 0. 1.0000 0. 0 -3 4 120.78 4.35 0. 1.0000 0. 0 -3 4 120.49 4.61 0. 1.0000 0. 0 -3 5 82.44 3.09 0. 1.0000 0. 0 -3 5 72.50 3.25 0. 1.0000 0. 0 -3 6 26.08 1.74 0. 1.0000 0. 0 -3 7 -0.72 1.23 0. 1.0000 0. 0 -3 8 -0.58 1.01 0. 1.0000 0. 0 4 -2 891.71 31.28 0. 1.0000 0. 0 4 -2 931.43 31.65 0. 1.0000 0. 0 -4 2 913.32 30.78 0. 1.0000 0. 0 4 -2 874.48 31.13 0. 1.0000 0. 0 4 -3 54.30 2.15 0. 1.0000 0. 0 4 -3 56.50 2.18 0. 1.0000 0. 0 4 -3 58.81 2.10 0. 1.0000 0. 0 4 -3 62.43 2.63 0. 1.0000 0. 0 4 -3 54.76 2.40 0. 1.0000 0. 0 -4 4 17.10 0.99 0. 1.0000 0. 0 -4 4 16.42 1.24 0. 1.0000 0. 0 4 -4 16.10 0.94 0. 1.0000 0. 0 -4 5 612.11 21.32 0. 1.0000 0. 0 4 -5 609.46 21.23 0. 1.0000 0. 0 -4 5 637.59 21.27 0. 1.0000 0. 0 -4 6 209.94 7.91 0. 1.0000 0. 0 -4 6 208.51 7.49 0. 1.0000 0. 0 -4 7 110.62 4.78 0. 1.0000 0. 0 -4 7 112.09 4.77 0. 1.0000 0. 0 -4 8 15.13 1.95 0. 1.0000 0. 0 -4 8 13.82 1.71 0. 1.0000 0. 0 -4 9 319.98 12.28 0. 1.0000 0. 0 -4 9 335.55 12.53 0. 1.0000 0. 0 5 -1 235.99 8.94 0. 1.0000 0. 0 5 -2 827.95 29.21 0. 1.0000 0. 0 5 -2 835.19 29.68 0. 1.0000 0. 0 -5 2 840.02 28.53 0. 1.0000 0. 0 5 -3 297.67 10.77 0. 1.0000 0. 0 5 -3 322.97 11.63 0. 1.0000 0. 0 5 -3 339.28 11.38 0. 1.0000 0. 0 5 -4 392.40 13.27 0. 1.0000 0. 0 5 -4 381.85 13.22 0. 1.0000 0. 0 5 -4 408.74 13.96 0. 1.0000 0. 0 5 -4 377.42 13.35 0. 1.0000 0. 0 5 -5 352.85 12.39 0. 1.0000 0. 0 -5 5 346.64 12.30 0. 1.0000 0. 0 5 -5 363.97 13.01 0. 1.0000 0. 0 -5 6 -0.12 1.36 0. 1.0000 0. 0 5 -6 -0.31 0.69 0. 1.0000 0. 0 -5 6 0.31 0.92 0. 1.0000 0. 0 -5 6 -0.26 1.22 0. 1.0000 0. 0 -5 6 -0.10 0.71 0. 1.0000 0. 0 -5 7 514.87 15.33 0. 1.0000 0. 0 -5 7 513.93 15.24 0. 1.0000 0. 0 -5 7 480.07 14.70 0. 1.0000 0. 0 -5 8 1.53 1.59 0. 1.0000 0. 0 -5 8 1.86 1.67 0. 1.0000 0. 0 5 -8 0.24 1.28 0. 1.0000 0. 0 -5 9 175.25 7.40 0. 1.0000 0. 0 -5 9 184.24 7.49 0. 1.0000 0. 0 -5 10 3.41 2.12 0. 1.0000 0. 0 -5 10 2.31 2.08 0. 1.0000 0. 0 -5 11 0.76 1.78 0. 1.0000 0. 0 -5 11 3.81 2.32 0. 1.0000 0. 0 6 -1 203.64 8.10 0. 1.0000 0. 0 6 -2 127.51 6.25 0. 1.0000 0. 0 6 -2 150.91 5.97 0. 1.0000 0. 0 6 -3 112.09 4.46 0. 1.0000 0. 0 -6 3 123.96 4.30 0. 1.0000 0. 0 6 -3 126.58 5.19 0. 1.0000 0. 0 6 -3 139.75 5.77 0. 1.0000 0. 0 6 -4 44.36 1.93 0. 1.0000 0. 0 6 -4 51.15 3.07 0. 1.0000 0. 0 6 -4 46.98 2.00 0. 1.0000 0. 0 6 -4 53.51 2.77 0. 1.0000 0. 0 -6 4 47.36 1.79 0. 1.0000 0. 0 6 -5 122.55 5.32 0. 1.0000 0. 0 6 -5 127.15 4.48 0. 1.0000 0. 0 6 -5 120.12 4.59 0. 1.0000 0. 0 6 -6 27.05 1.99 0. 1.0000 0. 0 6 -6 34.48 2.58 0. 1.0000 0. 0 -6 6 33.80 1.86 0. 1.0000 0. 0 6 -6 34.34 1.37 0. 1.0000 0. 0 6 -6 34.28 1.43 0. 1.0000 0. 0 6 -6 31.49 2.11 0. 1.0000 0. 0 -6 7 169.16 6.68 0. 1.0000 0. 0 -6 7 164.44 6.75 0. 1.0000 0. 0 -6 7 162.43 6.21 0. 1.0000 0. 0 -6 8 477.72 13.73 0. 1.0000 0. 0 -6 8 489.25 14.51 0. 1.0000 0. 0 -6 8 468.91 14.29 0. 1.0000 0. 0 -6 9 50.55 3.26 0. 1.0000 0. 0 -6 9 48.82 2.36 0. 1.0000 0. 0 6 -9 32.14 4.68 0. 1.0000 0. 0 -6 9 46.69 3.00 0. 1.0000 0. 0 -6 10 114.02 5.44 0. 1.0000 0. 0 -6 10 106.60 4.70 0. 1.0000 0. 0 -6 10 111.58 5.44 0. 1.0000 0. 0 -6 11 3.11 2.47 0. 1.0000 0. 0 -6 11 3.97 2.52 0. 1.0000 0. 0 -6 11 4.32 1.99 0. 1.0000 0. 0 -6 12 1.80 2.74 0. 1.0000 0. 0 -6 12 1.38 2.56 0. 1.0000 0. 0 7 -2 9.97 1.64 0. 1.0000 0. 0 -7 3 1536.07 52.67 0. 1.0000 0. 0 7 -3 1578.35 54.33 0. 1.0000 0. 0 -7 3 1555.28 52.63 0. 1.0000 0. 0 7 -4 463.60 15.89 0. 1.0000 0. 0 7 -4 478.52 17.67 0. 1.0000 0. 0 7 -4 464.99 16.98 0. 1.0000 0. 0 7 -5 668.97 22.69 0. 1.0000 0. 0 7 -5 661.98 23.14 0. 1.0000 0. 0 7 -5 613.55 21.70 0. 1.0000 0. 0 7 -6 60.05 3.63 0. 1.0000 0. 0 7 -6 63.59 2.49 0. 1.0000 0. 0 7 -6 60.02 2.71 0. 1.0000 0. 0 7 -7 119.84 5.90 0. 1.0000 0. 0 7 -7 136.95 5.81 0. 1.0000 0. 0 7 -7 145.76 4.88 0. 1.0000 0. 0 7 -7 120.76 4.65 0. 1.0000 0. 0 7 -7 136.63 4.67 0. 1.0000 0. 0 7 -8 20.95 3.00 0. 1.0000 0. 0 -7 8 32.89 2.09 0. 1.0000 0. 0 7 -8 22.31 2.60 0. 1.0000 0. 0 -7 9 82.20 4.53 0. 1.0000 0. 0 -7 9 100.02 4.05 0. 1.0000 0. 0 7 -9 67.19 5.31 0. 1.0000 0. 0 -7 9 90.99 4.77 0. 1.0000 0. 0 7 -10 129.25 7.64 0. 1.0000 0. 0 -7 10 385.49 9.71 0. 1.0000 0. 0 7 -10 200.77 11.24 0. 1.0000 0. 0 -7 10 359.61 9.85 0. 1.0000 0. 0 -7 10 386.74 8.71 0. 1.0000 0. 0 -7 11 325.09 12.13 0. 1.0000 0. 0 -7 11 282.24 11.00 0. 1.0000 0. 0 -7 11 302.70 11.79 0. 1.0000 0. 0 -7 12 65.70 4.66 0. 1.0000 0. 0 -7 12 55.63 4.24 0. 1.0000 0. 0 -7 13 121.59 6.80 0. 1.0000 0. 0 -7 13 123.31 6.51 0. 1.0000 0. 0 8 -2 384.65 14.60 0. 1.0000 0. 0 8 -3 847.04 29.38 0. 1.0000 0. 0 8 -3 776.69 29.99 0. 1.0000 0. 0 -8 3 822.05 28.06 0. 1.0000 0. 0 8 -4 58.22 3.51 0. 1.0000 0. 0 8 -4 56.59 4.17 0. 1.0000 0. 0 8 -5 116.89 4.30 0. 1.0000 0. 0 8 -5 122.18 6.35 0. 1.0000 0. 0 8 -5 117.72 5.70 0. 1.0000 0. 0 8 -5 111.51 4.53 0. 1.0000 0. 0 -8 5 132.48 4.35 0. 1.0000 0. 0 8 -6 92.08 4.64 0. 1.0000 0. 0 8 -6 80.28 3.97 0. 1.0000 0. 0 8 -7 29.02 2.92 0. 1.0000 0. 0 8 -7 29.85 1.58 0. 1.0000 0. 0 8 -7 26.99 2.27 0. 1.0000 0. 0 8 -7 26.30 2.11 0. 1.0000 0. 0 8 -8 10.60 1.27 0. 1.0000 0. 0 8 -8 3.63 2.55 0. 1.0000 0. 0 8 -8 7.13 2.08 0. 1.0000 0. 0 8 -9 10.50 1.09 0. 1.0000 0. 0 -8 9 14.74 1.87 0. 1.0000 0. 0 8 -9 8.29 2.96 0. 1.0000 0. 0 8 -9 12.77 2.81 0. 1.0000 0. 0 8 -9 7.83 0.84 0. 1.0000 0. 0 8 -10 15.53 4.13 0. 1.0000 0. 0 8 -10 9.28 3.34 0. 1.0000 0. 0 8 -11 -0.45 5.35 0. 1.0000 0. 0 -8 11 5.40 2.74 0. 1.0000 0. 0 -8 11 5.65 2.17 0. 1.0000 0. 0 8 -11 -2.86 3.83 0. 1.0000 0. 0 -8 12 141.22 7.02 0. 1.0000 0. 0 -8 12 143.02 7.30 0. 1.0000 0. 0 -8 14 26.88 3.80 0. 1.0000 0. 0 -8 14 37.49 3.89 0. 1.0000 0. 0 9 -2 13.87 2.26 0. 1.0000 0. 0 -9 3 9.95 0.99 0. 1.0000 0. 0 9 -3 8.58 2.20 0. 1.0000 0. 0 9 -4 1581.79 59.67 0. 1.0000 0. 0 -9 4 1682.65 57.34 0. 1.0000 0. 0 9 -4 1780.90 58.90 0. 1.0000 0. 0 9 -5 87.68 5.31 0. 1.0000 0. 0 9 -5 75.02 3.15 0. 1.0000 0. 0 -9 5 75.56 4.22 0. 1.0000 0. 0 -9 5 77.81 2.88 0. 1.0000 0. 0 9 -5 77.89 4.53 0. 1.0000 0. 0 9 -6 140.24 4.98 0. 1.0000 0. 0 9 -6 137.96 5.29 0. 1.0000 0. 0 9 -6 144.87 6.75 0. 1.0000 0. 0 9 -6 138.57 6.00 0. 1.0000 0. 0 9 -6 156.94 7.62 0. 1.0000 0. 0 9 -7 80.89 4.32 0. 1.0000 0. 0 9 -7 96.45 5.68 0. 1.0000 0. 0 9 -7 91.82 3.81 0. 1.0000 0. 0 9 -7 94.27 5.22 0. 1.0000 0. 0 9 -8 69.21 2.82 0. 1.0000 0. 0 9 -8 60.34 3.80 0. 1.0000 0. 0 9 -8 56.93 4.36 0. 1.0000 0. 0 9 -9 -0.35 2.22 0. 1.0000 0. 0 9 -9 -1.25 3.08 0. 1.0000 0. 0 9 -9 -0.51 1.30 0. 1.0000 0. 0 9 -10 260.78 9.76 0. 1.0000 0. 0 9 -10 136.68 8.14 0. 1.0000 0. 0 9 -11 17.11 5.06 0. 1.0000 0. 0 9 -11 5.12 3.56 0. 1.0000 0. 0 9 -12 29.23 4.84 0. 1.0000 0. 0 9 -12 108.67 8.88 0. 1.0000 0. 0 9 -14 1.11 5.09 0. 1.0000 0. 0 9 -15 1.21 4.91 0. 1.0000 0. 0 10 -3 0.10 2.23 0. 1.0000 0. 0 -10 3 0.22 0.94 0. 1.0000 0. 0 -10 4 19.02 2.75 0. 1.0000 0. 0 -10 4 16.37 0.90 0. 1.0000 0. 0 -10 4 18.39 1.20 0. 1.0000 0. 0 10 -4 16.37 2.92 0. 1.0000 0. 0 10 -5 189.81 8.53 0. 1.0000 0. 0 10 -5 182.86 9.31 0. 1.0000 0. 0 -10 5 191.12 7.98 0. 1.0000 0. 0 10 -6 233.92 10.72 0. 1.0000 0. 0 10 -6 219.72 8.93 0. 1.0000 0. 0 10 -6 221.26 8.11 0. 1.0000 0. 0 10 -6 240.62 9.87 0. 1.0000 0. 0 10 -7 7.87 0.83 0. 1.0000 0. 0 10 -7 9.07 1.41 0. 1.0000 0. 0 10 -7 7.72 3.72 0. 1.0000 0. 0 10 -7 6.19 1.81 0. 1.0000 0. 0 10 -7 10.92 3.14 0. 1.0000 0. 0 10 -8 143.92 6.58 0. 1.0000 0. 0 10 -8 162.82 8.19 0. 1.0000 0. 0 10 -8 146.09 6.14 0. 1.0000 0. 0 10 -8 152.09 7.50 0. 1.0000 0. 0 10 -9 7.94 3.49 0. 1.0000 0. 0 10 -9 11.01 2.72 0. 1.0000 0. 0 10 -9 12.78 4.22 0. 1.0000 0. 0 10 -10 4.99 3.57 0. 1.0000 0. 0 10 -10 3.86 2.91 0. 1.0000 0. 0 10 -11 101.66 6.77 0. 1.0000 0. 0 10 -11 44.40 5.24 0. 1.0000 0. 0 10 -12 2.04 4.18 0. 1.0000 0. 0 10 -12 -2.78 6.22 0. 1.0000 0. 0 10 -13 13.01 4.65 0. 1.0000 0. 0 10 -14 4.29 4.83 0. 1.0000 0. 0 10 -15 -1.27 5.11 0. 1.0000 0. 0 11 -3 58.41 4.35 0. 1.0000 0. 0 -11 4 0.11 0.89 0. 1.0000 0. 0 -11 4 2.78 1.00 0. 1.0000 0. 0 -11 4 2.68 2.73 0. 1.0000 0. 0 11 -4 3.47 2.65 0. 1.0000 0. 0 -11 4 2.80 0.70 0. 1.0000 0. 0 11 -5 59.31 5.19 0. 1.0000 0. 0 -11 5 61.62 4.31 0. 1.0000 0. 0 11 -5 60.71 4.65 0. 1.0000 0. 0 -11 5 59.22 4.21 0. 1.0000 0. 0 11 -6 78.31 3.36 0. 1.0000 0. 0 -11 6 77.45 2.98 0. 1.0000 0. 0 -11 6 77.78 4.55 0. 1.0000 0. 0 11 -6 88.85 5.45 0. 1.0000 0. 0 11 -6 83.31 6.22 0. 1.0000 0. 0 11 -7 72.24 3.32 0. 1.0000 0. 0 -11 7 96.20 5.45 0. 1.0000 0. 0 11 -7 83.40 5.32 0. 1.0000 0. 0 11 -7 72.79 4.17 0. 1.0000 0. 0 11 -7 81.96 6.39 0. 1.0000 0. 0 11 -8 26.06 2.72 0. 1.0000 0. 0 11 -8 26.47 4.12 0. 1.0000 0. 0 11 -8 31.89 4.83 0. 1.0000 0. 0 11 -8 27.18 2.31 0. 1.0000 0. 0 11 -9 219.82 10.78 0. 1.0000 0. 0 11 -9 196.42 9.63 0. 1.0000 0. 0 11 -9 198.43 8.79 0. 1.0000 0. 0 11 -10 6.15 4.55 0. 1.0000 0. 0 11 -10 10.59 2.97 0. 1.0000 0. 0 11 -10 5.14 4.23 0. 1.0000 0. 0 11 -11 12.40 5.28 0. 1.0000 0. 0 11 -11 13.19 4.37 0. 1.0000 0. 0 11 -11 24.54 4.34 0. 1.0000 0. 0 11 -12 -2.98 4.47 0. 1.0000 0. 0 11 -12 -0.23 5.46 0. 1.0000 0. 0 11 -13 0.73 4.73 0. 1.0000 0. 0 11 -13 -0.29 7.12 0. 1.0000 0. 0 11 -14 -6.23 5.27 0. 1.0000 0. 0 11 -15 2.94 5.61 0. 1.0000 0. 0 -12 3 1.61 2.67 0. 1.0000 0. 0 -12 3 0.09 2.50 0. 1.0000 0. 0 -12 4 1.54 2.96 0. 1.0000 0. 0 -12 4 0.68 0.78 0. 1.0000 0. 0 -12 4 0.29 3.10 0. 1.0000 0. 0 12 -4 -0.36 2.83 0. 1.0000 0. 0 12 -5 13.63 3.59 0. 1.0000 0. 0 -12 5 13.08 3.40 0. 1.0000 0. 0 12 -6 16.32 1.61 0. 1.0000 0. 0 -12 6 19.73 3.59 0. 1.0000 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0.39 5.05 0. 1.0000 0. 4 4 1 1.43 4.19 0. 1.0000 0. 4 -4 1 6.03 4.21 0. 1.0000 0. -4 -4 -1 0.52 4.59 0. 1.0000 0. 4 4 2 10.94 4.52 0. 1.0000 0. -4 -4 -2 -1.57 4.57 0. 1.0000 0. 4 -4 2 11.96 4.16 0. 1.0000 0. 4 -4 2 7.17 4.12 0. 1.0000 0. 4 4 3 -1.63 4.06 0. 1.0000 0. -4 4 -3 2.52 5.67 0. 1.0000 0. 4 -4 3 7.19 4.18 0. 1.0000 0. -4 5 3 6.78 5.22 0. 1.0000 0. 4 5 -3 3.94 4.84 0. 1.0000 0. 4 5 -3 -1.29 5.15 0. 1.0000 0. -4 5 2 8.43 5.18 0. 1.0000 0. 4 5 -2 11.89 4.85 0. 1.0000 0. 4 -5 -2 5.60 5.15 0. 1.0000 0. 4 5 -2 8.84 4.72 0. 1.0000 0. 4 -5 -2 -3.36 5.06 0. 1.0000 0. 4 -5 -1 6.38 4.81 0. 1.0000 0. 4 5 -1 2.94 4.54 0. 1.0000 0. 4 -5 -1 -3.03 4.56 0. 1.0000 0. 4 -5 0 9.65 4.55 0. 1.0000 0. -4 5 0 17.00 5.40 0. 1.0000 0. 4 -5 0 7.89 4.40 0. 1.0000 0. -4 -5 0 1.81 4.50 0. 1.0000 0. 4 5 1 8.96 4.20 0. 1.0000 0. 4 -5 1 2.11 4.13 0. 1.0000 0. 4 5 1 6.61 4.23 0. 1.0000 0. -4 5 -1 0.26 5.27 0. 1.0000 0. -4 -5 -1 3.33 4.21 0. 1.0000 0. 4 -5 1 4.57 4.30 0. 1.0000 0. 4 5 2 -1.31 4.07 0. 1.0000 0. -4 5 -2 10.87 7.00 0. 1.0000 0. 4 -5 2 6.72 3.95 0. 1.0000 0. 4 -5 2 5.81 4.13 0. 1.0000 0. -512 # 3864 reflections output ; # end of ARCHIVE-HKL.CIF _chemical_name_common ROY _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: acetone' ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_ROY_ON_1p37GPa _database_code_depnum_ccdc_archive 'CCDC 2098638' loop_ _audit_author_name _audit_author_address 'Nicholas Funnell' ;STFC, ISIS Neutron Facility United Kingdom ; _audit_update_record ; 2021-07-22 deposited with the CCDC. 2021-08-27 downloaded from the CCDC. ; _audit_creation_date 2021-01-25 _audit_creation_method 'CRYSTALS_ver_14.61_build_7795 ' _chemical_name_systematic ; 5-methyl-2[(2-nitrophenyl)amino]-3-thiophenecarbonitrile ; #CheckCIF alerts _vrf_THETM01_ROY_ON_1p37GPa ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575 RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT027_ROY_ON_1p37GPa ; PROBLEM: _diffrn_reflns_theta_full value (too) Low ...... 17.43 Degree RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT029_ROY_ON_1p37GPa ; PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.729 Why? RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT201_ROY_ON_1p37GPa ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 17 Report RESPONSE: The model could only be refined isotropically in order to maintain a favourable data-to-parameter ratio, due to numerous unmeasured reflections. The relatively electron-rich sulfur atom has been modelled anisotropically. ; _vrf_PLAT340_ROY_ON_1p37GPa ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.01091 Ang. RESPONSE: These are poor-quality diffraction data. ; _vrf_PLAT911_ROY_ON_1p37GPa ; PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.555 417 Report RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT082_ROY_ON_1p37GPa ; PROBLEM: High R1 Value .................................. 0.12 Report RESPONSE: These are poor-quality diffraction data and the model has only been refined isotropically. ; _vrf_PLAT910_ROY_ON_1p37GPa ; PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 8 Note RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _refine_special_details ; In the absence of significant anomalous scattering, Friedel pairs were merged. Data were collected in a Merrill-Bassett diamond anvil cell, which significantly restricts the regions over which reciprocal space can be sampled. Thus, these data are poor quality/incomplete, reflected in numerous CheckCIF alerts regarding refinement statistics. At all pressures, the atomic connectivity is known. All non-sulfur atoms were refined isotropically; sulfur was refined anisotropically. Hydrogen atoms were constrained to ride on their host atoms. #=============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Total Missing #------------------------------------------------------------------------------- 20.82 0.500 0.714 1116 797 319 23.01 0.550 0.706 1408 994 414 23.25 0.555 0.706 1446 1021 425 ------------------------------------------------------------ ACTA Min. Res. --- Note: The Reported Completeness refers to the Actual H,K,L Index Range ; #end of refcif _cell_length_a 3.68945(2) _cell_length_b 17.85212(5) _cell_length_c 16.13731(5) _cell_angle_alpha 90 _cell_angle_beta 90.452(6) _cell_angle_gamma 90 _cell_volume 1062.843(7) _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' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 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' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C12 H9 N3 O2 S1 # Dc = 1.62 Fooo = 536.00 Mu = 3.01 M = 259.29 # Found Formula = C12 H9 N3 O2 S1 # Dc = 1.62 FOOO = 536.00 Mu = 3.01 M = 259.29 _chemical_formula_sum 'C12 H9 N3 O2 S1' _chemical_formula_moiety 'C12 H9 N3 O2 S1' _chemical_compound_source 'TCI Chemicals' _chemical_formula_weight 259.29 _cell_measurement_reflns_used 1713 _cell_measurement_theta_min 1.68 _cell_measurement_theta_max 23.18 _cell_measurement_temperature 293 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_min 0.050 _exptl_crystal_size_mid 0.072 _exptl_crystal_size_max 0.248 _exptl_crystal_density_diffrn 1.620 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 0.301 # Sheldrick geometric approximatio 0.98 0.99 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North et al., 1968)' _exptl_absorpt_correction_T_min 0.08 _exptl_absorpt_correction_T_max 0.99 _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_device 'four-circle diffractometer' _diffrn_radiation_monochromator mirror _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 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction ; CrysAlisPro (Rigaku Oxford Diffraction, 2017) ; _computing_structure_solution 'Model from previously-determined structure' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 293 _diffrn_ambient_pressure 1370000 _diffrn_reflns_number 3379 _diffrn_reflns_av_unetI/netI 0.072 _reflns_number_total 1045 _diffrn_reflns_av_R_equivalents 0.079 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 1045 # Theoretical number of reflections is about 3050 _diffrn_reflns_theta_min 1.701 _diffrn_reflns_theta_max 23.247 _diffrn_measured_fraction_theta_max 0.690 _diffrn_reflns_theta_full 17.435 _diffrn_measured_fraction_theta_full 0.729 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -4 _reflns_limit_h_max 4 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.93 _refine_diff_density_max 1.09 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # Explicitly named reflections are ALWAYS excluded from R&wR # The values actually used during refinement # These are labelled "all" for compatibility with PLATON _oxford_refine_reflns_threshold_expression I>-3.0\s(I) _refine_ls_number_restraints 94 _refine_ls_number_parameters 82 _refine_ls_number_reflns 1021 _oxford_refine_ls_R_factor_ref 0.1668 _refine_ls_R_factor_all 0.1668 _refine_ls_wR_factor_ref 0.0875 _refine_ls_wR_factor_all 0.0875 _refine_ls_goodness_of_fit_ref 0.9868 _refine_ls_shift/su_max 0.0001072 _refine_ls_shift/su_mean 0.0000328 # Computed with I/sigma = -10 _oxford_reflns_number_all 1021 _oxford_refine_ls_R_factor_all 0.1668 _oxford_refine_ls_wR_factor_all 0.0875 # Computed with no filters except I/sigma = +2 a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 662 _refine_ls_R_factor_gt 0.1187 _refine_ls_wR_factor_gt 0.0796 _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed #undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ; Method= SQRT(W) = 1/(Data with the key SIGMA(/FO/) in list 6) ; # 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 S1 S 0.7364(5) 0.59154(10) 0.43302(15) 0.0389 1.0000 Uani D U . . . . O1 O 0.4850(13) 0.6281(3) 0.0245(4) 0.0512(16) 1.0000 Uiso D U . . . . O2 O 0.5087(13) 0.6960(3) 0.1363(3) 0.0480(15) 1.0000 Uiso D U . . . . C1 C 0.8678(16) 0.5829(4) 0.2229(6) 0.0366(14) 1.0000 Uiso D U . . . . C2 C 1.0626(16) 0.5211(4) 0.2570(5) 0.0371(15) 1.0000 Uiso D U . . . . C3 C 1.1262(15) 0.4589(4) 0.2112(5) 0.0360(16) 1.0000 Uiso D U . . . . C4 C 1.0098(17) 0.4564(4) 0.1281(5) 0.0394(16) 1.0000 Uiso D U . . . . C5 C 0.8329(16) 0.5151(4) 0.0926(5) 0.0385(15) 1.0000 Uiso D U . . . . C6 C 0.7647(17) 0.5774(4) 0.1418(5) 0.0385(14) 1.0000 Uiso D U . . . . C7 C 0.8688(16) 0.6528(4) 0.3577(5) 0.0365(15) 1.0000 Uiso D U . . . . C8 C 1.0304(18) 0.7152(4) 0.3907(6) 0.0379(15) 1.0000 Uiso D U . . . . C9 C 1.0424(17) 0.7144(4) 0.4776(6) 0.0394(16) 1.0000 Uiso D U . . . . C10 C 0.8885(13) 0.6492(3) 0.5111(6) 0.0386(15) 1.0000 Uiso D U . . . . C11 C 0.8593(13) 0.6268(3) 0.6000(5) 0.0473(18) 1.0000 Uiso D U . . . . C12 C 1.2002(17) 0.7678(4) 0.3399(5) 0.0374(15) 1.0000 Uiso D U . . . . N1 N 0.8081(13) 0.6428(3) 0.2722(4) 0.0355(14) 1.0000 Uiso D U . . . . N2 N 1.3372(15) 0.8063(4) 0.2919(4) 0.0428(16) 1.0000 Uiso D U . . . . N3 N 0.5795(15) 0.6366(3) 0.0983(5) 0.0443(15) 1.0000 Uiso D U . . . . H1 H 0.703(5) 0.6784(16) 0.2462(18) 0.042(3) 1.0000 Uiso D . . . . . H2 H 1.1438 0.5235 0.3111 0.0459 1.0000 Uiso R . . . . . H3 H 1.2452 0.4195 0.2342 0.0434 1.0000 Uiso R . . . . . H4 H 1.0535 0.4137 0.0972 0.0475 1.0000 Uiso R . . . . . H5 H 0.7617 0.5126 0.0383 0.0464 1.0000 Uiso R . . . . . H9 H 1.1385 0.7524 0.5090 0.0470 1.0000 Uiso R . . . . . H111 H 1.0746 0.5998 0.6166 0.0713 1.0000 Uiso DR . . . . . H112 H 0.8313 0.6710 0.6340 0.0698 1.0000 Uiso DR . . . . . H113 H 0.6558 0.5947 0.6068 0.0711 1.0000 Uiso DR . . . . . 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 S1 0.0471(11) 0.0358(16) 0.0336(19) 0.0039(8) -0.0073(9) -0.0024(10) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.4499(18) 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 S1 . C7 . 1.709(8) yes S1 . C10 . 1.718(7) yes O1 . N3 . 1.247(8) yes O2 . N3 . 1.254(8) yes C1 . C2 . 1.424(9) yes C1 . C6 . 1.364(10) yes C1 . N1 . 1.352(9) yes C2 . C3 . 1.356(10) yes C2 . H2 . 0.922 no C3 . C4 . 1.405(9) yes C3 . H3 . 0.907 no C4 . C5 . 1.359(10) yes C4 . H4 . 0.926 no C5 . C6 . 1.390(10) yes C5 . H5 . 0.914 no C6 . N3 . 1.438(9) yes C7 . C8 . 1.369(10) yes C7 . N1 . 1.407(8) yes C8 . C9 . 1.403(11) yes C8 . C12 . 1.398(10) yes C9 . C10 . 1.405(9) yes C9 . H9 . 0.915 no C10 . C11 . 1.495(11) yes C11 . H111 . 0.965 no C11 . H112 . 0.967 no C11 . H113 . 0.951 no C12 . N2 . 1.156(9) yes N1 . H1 . 0.85(3) 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 C7 . S1 . C10 . 92.5(4) yes C2 . C1 . C6 . 116.8(6) yes C2 . C1 . N1 . 118.0(8) yes C6 . C1 . N1 . 125.2(7) yes C1 . C2 . C3 . 120.9(8) yes C1 . C2 . H2 . 119.3 no C3 . C2 . H2 . 119.8 no C2 . C3 . C4 . 119.6(7) yes C2 . C3 . H3 . 119.8 no C4 . C3 . H3 . 120.7 no C3 . C4 . C5 . 121.3(7) yes C3 . C4 . H4 . 119.2 no C5 . C4 . H4 . 119.5 no C4 . C5 . C6 . 117.7(8) yes C4 . C5 . H5 . 120.0 no C6 . C5 . H5 . 122.3 no C5 . C6 . C1 . 123.7(7) yes C5 . C6 . N3 . 113.3(8) yes C1 . C6 . N3 . 122.9(6) yes S1 . C7 . C8 . 111.7(7) yes S1 . C7 . N1 . 124.9(5) yes C8 . C7 . N1 . 123.4(7) yes C7 . C8 . C9 . 113.1(7) yes C7 . C8 . C12 . 120.9(8) yes C9 . C8 . C12 . 125.6(6) yes C8 . C9 . C10 . 112.5(6) yes C8 . C9 . H9 . 123.6 no C10 . C9 . H9 . 123.9 no C9 . C10 . S1 . 110.3(6) yes C9 . C10 . C11 . 128.5(5) yes S1 . C10 . C11 . 121.2(3) yes C10 . C11 . H111 . 109.6 no C10 . C11 . H112 . 109.5 no H111 . C11 . H112 . 110.0 no C10 . C11 . H113 . 109.5 no H111 . C11 . H113 . 108.4 no H112 . C11 . H113 . 109.8 no C8 . C12 . N2 . 173.4(10) yes C7 . N1 . C1 . 130.7(6) yes C7 . N1 . H1 . 117(2) no C1 . N1 . H1 . 112(2) no C6 . N3 . O2 . 118.9(8) yes C6 . N3 . O1 . 120.3(6) yes O2 . N3 . O1 . 120.8(7) yes _iucr_refine_instructions_details ; # # Punched on 02/02/21 at 13:56:53 # #LIST 12 BLOCK CONT SCALE CONT S ( 1 ,X'S,U'S) CONT O ( 1 ,X'S,U[ISO]) UNTIL H ( 1 ) RIDE C ( 2,X'S) H ( 2,X'S) RIDE C ( 3,X'S) H ( 3,X'S) RIDE C ( 4,X'S) H ( 4,X'S) RIDE C ( 5,X'S) H ( 5,X'S) RIDE C ( 9,X'S) H ( 9,X'S) RIDE C ( 11,X'S) H ( 111,X'S) H ( 112,X'S) H ( 113,X'S) END # # Punched on 02/02/21 at 13:56:53 # #LIST 16 NO REM REM NPF NOTE - FIRST UNTIL LAST REM REM HREST START (DO NOT REMOVE THIS LINE) REM NO H NO #H U MULT DIST REM C-H REM >4 1.5 .96 DISORDER REM 1 1 1.2 .93 C C-H (ACETYLENE) REM 1 2 1.2 .93 C-C(H)-C REM 1 3 1.2 .98 (C)3-C-H REM 2 1 1.2 .93 C=C-H(2) REM 2 2 1.2 .97 (C)2-C-(H)2 REM 3 1 1.5 .96 C-C-(H)3 REM N-H REM >4 1.5 .89 DISORDER REM 1 1 1.2 .86 N-N/H REM 1 2 1.2 .86 (C)2-N-H REM 1 3 1.2 .89 (C)3-N-H REM 2 1 1.2 .86 C-N-(H)2 REM 2 2 1.2 .89 (C)2-N-(H)2 REM 3 1 1.2 .89 C-H-(H)3 REM O-H REM 1 1 1.5 .82 O-H REM REM DIST ESD = 0.02 REM VIB ESD = 0.002 REM ANGLE ESD = 2.0 REM REM TO ACTIVATE THE VIB RESTRAINTS, REMOVE LEADING REM REM H1-N-R2 DIST 0.86, 0.02 = CONT N ( 1) TO H(1) REST 0.042, 0.002 = H(1,U[ISO]) ANGLE 0.0, 2.0 = MEAN CONT H(1) TO N ( 1) TO C(7) CONT H(1) TO N ( 1) TO C(1) REM HREST END (DO NOT REMOVE THIS LINE) REM DELU START (DO NOT REMOVE THIS LINE) VIBR .0, 0.00200 = S(1) TO C(10) VIBR .0, 0.00200 = S(1) TO C(7) VIBR .0, 0.00500 = C(7) TO C(10) VIBR .0, 0.00200 = N(2) TO C(12) VIBR .0, 0.00200 = C(10) TO C(9) VIBR .0, 0.00200 = C(10) TO C(11) VIBR .0, 0.00500 = C(9) TO S(1) VIBR .0, 0.00500 = C(11) TO S(1) VIBR .0, 0.00500 = C(11) TO C(9) VIBR .0, 0.00200 = C(12) TO C(8) VIBR .0, 0.00500 = C(8) TO N(2) VIBR .0, 0.00200 = O(1) TO N(3) VIBR .0, 0.00200 = C(2) TO C(1) VIBR .0, 0.00200 = C(2) TO C(3) VIBR .0, 0.00500 = C(3) TO C(1) VIBR .0, 0.00200 = N(1) TO C(7) VIBR .0, 0.00200 = N(1) TO C(1) VIBR .0, 0.00500 = C(1) TO C(7) VIBR .0, 0.00200 = C(7) TO C(8) VIBR .0, 0.00500 = N(1) TO S(1) VIBR .0, 0.00500 = C(8) TO S(1) VIBR .0, 0.00500 = C(8) TO N(1) VIBR .0, 0.00200 = O(2) TO N(3) VIBR .0, 0.00200 = N(3) TO C(6) VIBR .0, 0.00500 = O(1) TO O(2) VIBR .0, 0.00500 = C(6) TO O(2) VIBR .0, 0.00500 = C(6) TO O(1) VIBR .0, 0.00200 = C(5) TO C(4) VIBR .0, 0.00200 = C(5) TO C(6) VIBR .0, 0.00500 = C(6) TO C(4) VIBR .0, 0.00200 = C(4) TO C(3) VIBR .0, 0.00500 = C(3) TO C(5) VIBR .0, 0.00200 = C(1) TO C(6) VIBR .0, 0.00500 = N(1) TO C(2) VIBR .0, 0.00500 = C(6) TO C(2) VIBR .0, 0.00500 = C(6) TO N(1) VIBR .0, 0.00500 = C(5) TO N(3) VIBR .0, 0.00500 = C(1) TO N(3) VIBR .0, 0.00500 = C(1) TO C(5) VIBR .0, 0.00200 = C(9) TO C(8) VIBR .0, 0.00500 = C(8) TO C(10) VIBR .0, 0.00500 = C(2) TO C(4) VIBR .0, 0.00500 = C(12) TO C(9) VIBR .0, 0.00500 = C(7) TO C(9) VIBR .0, 0.00500 = C(7) TO C(12) REM DELU END (DO NOT REMOVE THIS LINE) ANGLE 110.000000 , 0.020000 = C(10) TO C(11) TO H(111) ANGLE 110.000000 , 0.020000 = C(10) TO C(11) TO H(112) ANGLE 110.000000 , 0.020000 = C(10) TO C(11) TO H(113) DISTANCE 1.225000 , 0.050000 = O(2) TO N(3) DISTANCE 1.225000 , 0.050000 = O(1) TO N(3) DISTANCE 1.440000 , 0.050000 = C(6) TO N(3) DISTANCE 1.390000 , 0.050000 = C(5) TO C(6) DISTANCE 1.364000 , 0.050000 = C(4) TO C(5) DISTANCE 1.222000 , 0.050000 = O(1) TO N(3) DISTANCE 1.232000 , 0.050000 = O(2) TO N(3) DISTANCE 1.440000 , 0.050000 = C(6) TO N(3) DISTANCE 1.392000 , 0.050000 = C(5) TO C(6) DISTANCE 1.364000 , 0.050000 = C(4) TO C(5) DISTANCE 1.391000 , 0.050000 = C(3) TO C(4) DISTANCE 1.371000 , 0.050000 = C(2) TO C(3) DISTANCE 1.400000 , 0.050000 = C(1) TO C(2) DISTANCE 1.408000 , 0.050000 = C(1) TO C(6) DISTANCE 1.382000 , 0.050000 = C(1) TO N(1) DISTANCE 1.387000 , 0.050000 = C(7) TO N(1) DISTANCE 1.728000 , 0.050000 = S(1) TO C(7) DISTANCE 1.724000 , 0.050000 = S(1) TO C(10) DISTANCE 1.500000 , 0.050000 = C(10) TO C(11) DISTANCE 1.349000 , 0.050000 = C(9) TO C(10) DISTANCE 1.427000 , 0.050000 = C(8) TO C(9) DISTANCE 1.372000 , 0.050000 = C(7) TO C(8) DISTANCE 1.422000 , 0.050000 = C(8) TO C(12) DISTANCE 1.141000 , 0.050000 = C(12) TO N(2) REM THERMSIM START (DO NOT REMOVE THIS LINE) U(IJ) .0, 0.04000 = S(1) TO C(7) U(IJ) .0, 0.04000 = S(1) TO C(10) U(IJ) .0, 0.08000 = O(1) TO N(3) U(IJ) .0, 0.08000 = O(2) TO N(3) U(IJ) .0, 0.04000 = C(1) TO C(2) U(IJ) .0, 0.04000 = C(1) TO C(6) U(IJ) .0, 0.04000 = C(1) TO N(1) U(IJ) .0, 0.04000 = C(2) TO C(3) U(IJ) .0, 0.04000 = C(3) TO C(4) U(IJ) .0, 0.04000 = C(4) TO C(5) U(IJ) .0, 0.04000 = C(5) TO C(6) U(IJ) .0, 0.04000 = C(6) TO N(3) U(IJ) .0, 0.04000 = C(7) TO C(8) U(IJ) .0, 0.04000 = C(7) TO N(1) U(IJ) .0, 0.04000 = C(8) TO C(9) U(IJ) .0, 0.04000 = C(8) TO C(12) U(IJ) .0, 0.04000 = C(9) TO C(10) U(IJ) .0, 0.08000 = C(10) TO C(11) U(IJ) .0, 0.08000 = C(12) TO N(2) REM THERMSIM END (DO NOT REMOVE THIS LINE) PLANAR 0.010000 C(1) C(6) N(1) H(1) PLANAR 0.010000 C(1) C(2) C(3) C(4) C(5) C(6) N(1) N(3) PLANAR 0.010000 S(1) C(7) C(8) C(9) C(10) N(1) 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 1 1 6 x . -1 6 13 x . -1 3 9 x . 1 3 9 x . 0 1 4 x . 3 0 4 x . 1 8 1 x . -2 10 2 x . -1 4 11 x . -2 12 3 x . 2 0 6 x . 0 13 4 x . -2 14 5 x . 0 14 5 x . 0 6 13 x . 2 6 12 x . 0 8 14 x . -3 3 10 x . # looking for ARCHIVE-HKL.CIF _iucr_refine_reflections_details ; # Data was input as F-squared # punching LIST 6 as LIST 6 with all keys set # NBGNXT= 36 #LIST 6 READ NCOEF= 8 TYPE=FIX, F'S = FSQ UNIT=DATA, CHECK=NO L30=NO ARCH=NO STORE NCOEF= 6 OUTPUT INDICES /FO/ SIGMA(/FO/) RATIO/JCODE CORRECTIONS SERIAL CONT INPUT H K L /FO/ SIGMA(/FO/) JCODE CONT CORRECTIONS SERIAL FOR (I4,I4,I4,F10.2,F8.2,F4.0,F7.4,F7.0) END 0 -1 -1 10.74 0.61 0. 1.0000 0. 0 1 1 10.53 0.59 0. 1.0000 0. 0 -1 -1 9.71 0.49 0. 1.0000 0. 0 -1 -2 116.65 4.28 0. 1.0000 0. 0 1 2 95.64 4.27 0. 1.0000 0. 0 1 3 106.75 7.96 0. 1.0000 0. 0 -1 -3 580.48 10.04 0. 1.0000 0. 0 -1 -4 8.04 1.73 0. 1.0000 0. 0 -2 -1 1560.80 57.53 0. 1.0000 0. 0 2 1 1577.52 57.41 0. 1.0000 0. 0 -2 -1 1599.15 57.47 0. 1.0000 0. 0 2 1 1629.08 57.54 0. 1.0000 0. 0 2 1 1605.88 57.46 0. 1.0000 0. 0 -2 -2 105.25 4.35 0. 1.0000 0. 0 2 2 129.91 4.43 0. 1.0000 0. 0 2 2 106.14 4.31 0. 1.0000 0. 0 2 2 116.75 4.42 0. 1.0000 0. 0 2 2 99.04 4.47 0. 1.0000 0. 0 2 2 121.39 4.34 0. 1.0000 0. 0 2 2 118.45 4.50 0. 1.0000 0. 0 -2 -2 115.45 4.36 0. 1.0000 0. 0 -2 -2 111.23 4.29 0. 1.0000 0. 0 2 2 117.05 4.50 0. 1.0000 0. 0 2 3 817.57 28.17 0. 1.0000 0. 0 -2 -3 769.10 28.51 0. 1.0000 0. 0 -2 -3 885.30 28.44 0. 1.0000 0. 0 2 3 712.74 28.08 0. 1.0000 0. 0 -2 -3 894.30 28.57 0. 1.0000 0. 0 2 3 764.38 28.15 0. 1.0000 0. 0 2 3 870.92 28.40 0. 1.0000 0. 0 -2 -4 36.02 3.42 0. 1.0000 0. 0 -2 -4 29.85 1.89 0. 1.0000 0. 0 -2 -4 38.07 4.12 0. 1.0000 0. 0 2 4 18.18 1.85 0. 1.0000 0. 0 -2 -5 0.16 2.73 0. 1.0000 0. 0 -2 -5 559.68 7.64 0. 1.0000 0. 0 -2 -6 1001.41 37.77 0. 1.0000 0. 0 -2 -7 0.75 1.64 0. 1.0000 0. 0 -3 -1 523.68 18.34 0. 1.0000 0. 0 3 1 478.82 18.78 0. 1.0000 0. 0 3 1 499.34 18.27 0. 1.0000 0. 0 3 2 67.10 2.69 0. 1.0000 0. 0 3 2 59.07 2.62 0. 1.0000 0. 0 -3 -2 64.20 2.45 0. 1.0000 0. 0 -3 -2 57.50 2.57 0. 1.0000 0. 0 3 2 57.47 2.56 0. 1.0000 0. 0 -3 -2 54.41 2.46 0. 1.0000 0. 0 3 2 55.25 2.38 0. 1.0000 0. 0 -3 -2 54.72 2.38 0. 1.0000 0. 0 3 2 59.34 2.46 0. 1.0000 0. 0 -3 -3 3.70 0.87 0. 1.0000 0. 0 -3 -3 2.67 0.85 0. 1.0000 0. 0 3 3 2.32 1.02 0. 1.0000 0. 0 3 3 3.09 1.17 0. 1.0000 0. 0 3 3 2.59 0.63 0. 1.0000 0. 0 -3 -3 3.21 0.65 0. 1.0000 0. 0 3 3 2.53 0.98 0. 1.0000 0. 0 -3 -3 2.29 0.82 0. 1.0000 0. 0 -3 -3 2.75 0.66 0. 1.0000 0. 0 3 3 3.10 0.94 0. 1.0000 0. 0 3 3 3.05 0.63 0. 1.0000 0. 0 3 3 2.78 0.73 0. 1.0000 0. 0 3 4 108.83 4.64 0. 1.0000 0. 0 -3 -4 112.51 5.41 0. 1.0000 0. 0 -3 -4 120.33 4.74 0. 1.0000 0. 0 -3 -4 128.41 5.02 0. 1.0000 0. 0 -3 -4 138.59 4.97 0. 1.0000 0. 0 3 4 126.03 4.96 0. 1.0000 0. 0 -3 -4 111.53 4.70 0. 1.0000 0. 0 -3 -5 51.93 4.76 0. 1.0000 0. 0 3 5 48.41 3.10 0. 1.0000 0. 0 -3 -5 73.38 3.62 0. 1.0000 0. 0 -3 -5 61.62 2.87 0. 1.0000 0. 0 3 5 49.95 2.88 0. 1.0000 0. 0 3 6 19.92 2.53 0. 1.0000 0. 0 3 6 -0.16 1.41 0. 1.0000 0. 0 -3 -7 0.12 1.84 0. 1.0000 0. 0 -3 -8 40.93 3.62 0. 1.0000 0. 0 4 1 0.29 0.61 0. 1.0000 0. 0 -4 -1 -0.03 0.63 0. 1.0000 0. 0 4 1 0.55 0.37 0. 1.0000 0. 0 -4 -2 602.92 21.79 0. 1.0000 0. 0 -4 -2 597.00 21.97 0. 1.0000 0. 0 -4 -2 579.43 22.43 0. 1.0000 0. 0 4 2 595.06 22.17 0. 1.0000 0. 0 -4 -2 613.83 21.94 0. 1.0000 0. 0 4 3 49.16 2.29 0. 1.0000 0. 0 -4 -3 52.93 2.58 0. 1.0000 0. 0 4 3 56.21 2.47 0. 1.0000 0. 0 -4 -3 59.82 2.55 0. 1.0000 0. 0 -4 -3 49.03 2.38 0. 1.0000 0. 0 4 3 54.02 2.55 0. 1.0000 0. 0 -4 -3 57.09 2.46 0. 1.0000 0. 0 -4 -4 27.25 1.79 0. 1.0000 0. 0 -4 -4 24.28 1.54 0. 1.0000 0. 0 -4 -4 24.39 1.61 0. 1.0000 0. 0 4 4 20.20 2.11 0. 1.0000 0. 0 4 4 30.18 1.69 0. 1.0000 0. 0 4 4 24.82 1.97 0. 1.0000 0. 0 -4 -4 26.33 1.57 0. 1.0000 0. 0 -4 -5 544.51 19.35 0. 1.0000 0. 0 -4 -5 526.65 20.07 0. 1.0000 0. 0 -4 -5 542.42 19.15 0. 1.0000 0. 0 4 5 573.55 19.50 0. 1.0000 0. 0 -4 -6 122.00 5.29 0. 1.0000 0. 0 -4 -6 105.07 7.45 0. 1.0000 0. 0 4 6 117.06 5.51 0. 1.0000 0. 0 -4 -6 128.82 5.32 0. 1.0000 0. 0 -4 -7 117.30 5.93 0. 1.0000 0. 0 4 7 89.31 4.92 0. 1.0000 0. 0 -4 -7 132.73 5.00 0. 1.0000 0. 0 4 7 70.31 4.97 0. 1.0000 0. 0 4 8 2.08 2.57 0. 1.0000 0. 0 4 8 -0.53 2.34 0. 1.0000 0. 0 4 9 2.10 4.39 0. 1.0000 0. 0 -4 -9 275.93 6.74 0. 1.0000 0. 0 4 10 1.05 3.18 0. 1.0000 0. 0 -4 -10 0.26 2.40 0. 1.0000 0. 0 5 1 263.64 9.76 0. 1.0000 0. 0 5 2 633.12 23.57 0. 1.0000 0. 0 -5 -2 622.28 22.72 0. 1.0000 0. 0 -5 -3 225.63 8.79 0. 1.0000 0. 0 -5 -3 210.04 8.65 0. 1.0000 0. 0 5 3 234.35 8.65 0. 1.0000 0. 0 -5 -3 224.93 9.20 0. 1.0000 0. 0 5 3 248.51 8.95 0. 1.0000 0. 0 -5 -4 341.71 14.15 0. 1.0000 0. 0 5 4 367.32 14.10 0. 1.0000 0. 0 5 4 394.59 14.36 0. 1.0000 0. 0 5 4 420.43 14.37 0. 1.0000 0. 0 5 4 395.26 14.49 0. 1.0000 0. 0 -5 -4 385.62 14.51 0. 1.0000 0. 0 -5 -5 278.04 10.88 0. 1.0000 0. 0 -5 -5 270.32 11.01 0. 1.0000 0. 0 5 5 271.33 11.74 0. 1.0000 0. 0 5 5 247.46 11.23 0. 1.0000 0. 0 5 5 326.73 10.93 0. 1.0000 0. 0 -5 -5 273.66 10.72 0. 1.0000 0. 0 -5 -6 2.64 1.27 0. 1.0000 0. 0 5 6 0.46 3.50 0. 1.0000 0. 0 -5 -6 4.76 2.96 0. 1.0000 0. 0 5 6 3.38 1.52 0. 1.0000 0. 0 -5 -6 2.25 1.27 0. 1.0000 0. 0 -5 -7 411.24 14.70 0. 1.0000 0. 0 5 7 333.95 14.61 0. 1.0000 0. 0 -5 -7 340.01 16.86 0. 1.0000 0. 0 -5 -7 392.34 14.38 0. 1.0000 0. 0 -5 -8 6.54 2.16 0. 1.0000 0. 0 5 8 3.22 2.14 0. 1.0000 0. 0 -5 -9 198.39 8.78 0. 1.0000 0. 0 -5 -9 190.69 7.08 0. 1.0000 0. 0 -5 -9 219.46 7.50 0. 1.0000 0. 0 5 10 0.93 3.33 0. 1.0000 0. 0 -5 -10 0.65 3.82 0. 1.0000 0. 0 -5 -10 0.72 2.28 0. 1.0000 0. 0 -5 -10 0.56 4.60 0. 1.0000 0. 0 5 11 -1.37 3.79 0. 1.0000 0. 0 -5 -11 4.49 5.04 0. 1.0000 0. 0 -5 -11 -0.15 2.35 0. 1.0000 0. 0 6 1 183.89 6.99 0. 1.0000 0. 0 6 2 93.29 4.85 0. 1.0000 0. 0 -6 -3 128.84 6.48 0. 1.0000 0. 0 -6 -3 131.65 5.62 0. 1.0000 0. 0 -6 -3 143.60 5.27 0. 1.0000 0. 0 -6 -3 121.41 5.39 0. 1.0000 0. 0 6 3 140.78 6.02 0. 1.0000 0. 0 6 4 75.93 3.56 0. 1.0000 0. 0 -6 -4 84.64 3.64 0. 1.0000 0. 0 6 4 71.57 3.52 0. 1.0000 0. 0 6 4 68.75 3.20 0. 1.0000 0. 0 -6 -4 69.33 4.00 0. 1.0000 0. 0 -6 -4 72.18 3.34 0. 1.0000 0. 0 6 5 58.98 3.36 0. 1.0000 0. 0 -6 -5 68.81 3.28 0. 1.0000 0. 0 -6 -5 60.94 3.17 0. 1.0000 0. 0 6 5 68.44 3.25 0. 1.0000 0. 0 -6 -5 55.21 3.21 0. 1.0000 0. 0 6 5 63.65 3.75 0. 1.0000 0. 0 -6 -6 35.75 3.24 0. 1.0000 0. 0 6 6 30.52 3.67 0. 1.0000 0. 0 6 6 40.64 2.54 0. 1.0000 0. 0 6 6 32.71 4.73 0. 1.0000 0. 0 -6 -6 38.41 2.69 0. 1.0000 0. 0 -6 -7 156.26 6.63 0. 1.0000 0. 0 -6 -7 160.37 6.45 0. 1.0000 0. 0 -6 -7 154.64 8.28 0. 1.0000 0. 0 6 7 176.91 6.81 0. 1.0000 0. 0 -6 -8 389.36 15.06 0. 1.0000 0. 0 6 8 330.30 14.48 0. 1.0000 0. 0 -6 -8 376.80 14.11 0. 1.0000 0. 0 -6 -8 369.08 14.41 0. 1.0000 0. 0 6 9 24.26 3.20 0. 1.0000 0. 0 -6 -9 46.00 4.30 0. 1.0000 0. 0 -6 -9 40.12 3.11 0. 1.0000 0. 0 -6 -9 44.93 3.27 0. 1.0000 0. 0 -6 -10 110.38 5.04 0. 1.0000 0. 0 -6 -10 128.90 7.15 0. 1.0000 0. 0 -6 -10 114.53 5.21 0. 1.0000 0. 0 -6 -11 -2.84 5.14 0. 1.0000 0. 0 6 11 -3.30 3.34 0. 1.0000 0. 0 -6 -11 -1.07 3.18 0. 1.0000 0. 0 6 12 1.79 3.75 0. 1.0000 0. 0 -6 -12 -1.40 3.71 0. 1.0000 0. 0 -6 -12 1.23 5.55 0. 1.0000 0. 0 -6 -13 1.07 4.84 0. 1.0000 0. 0 7 3 1471.76 53.49 0. 1.0000 0. 0 -7 -3 1398.10 52.28 0. 1.0000 0. 0 -7 -3 1457.76 52.10 0. 1.0000 0. 0 -7 -4 408.57 16.37 0. 1.0000 0. 0 7 4 446.24 17.05 0. 1.0000 0. 0 -7 -4 464.51 16.26 0. 1.0000 0. 0 -7 -4 429.63 16.59 0. 1.0000 0. 0 7 5 463.69 17.26 0. 1.0000 0. 0 -7 -5 419.80 16.86 0. 1.0000 0. 0 7 5 446.85 17.25 0. 1.0000 0. 0 -7 -5 442.92 17.71 0. 1.0000 0. 0 -7 -5 482.00 17.08 0. 1.0000 0. 0 7 6 25.73 3.27 0. 1.0000 0. 0 -7 -6 21.16 2.40 0. 1.0000 0. 0 7 6 20.81 2.59 0. 1.0000 0. 0 -7 -6 27.86 2.66 0. 1.0000 0. 0 -7 -6 26.94 2.14 0. 1.0000 0. 0 -7 -6 31.36 2.81 0. 1.0000 0. 0 7 6 32.51 2.39 0. 1.0000 0. 0 7 7 142.12 10.28 0. 1.0000 0. 0 -7 -7 207.90 9.27 0. 1.0000 0. 0 7 7 131.85 9.22 0. 1.0000 0. 0 -7 -7 188.89 8.34 0. 1.0000 0. 0 7 7 207.03 8.25 0. 1.0000 0. 0 7 8 41.85 3.22 0. 1.0000 0. 0 -7 -8 64.41 5.04 0. 1.0000 0. 0 -7 -8 50.60 3.64 0. 1.0000 0. 0 -7 -9 87.97 4.89 0. 1.0000 0. 0 7 9 68.78 4.81 0. 1.0000 0. 0 -7 -9 102.04 6.06 0. 1.0000 0. 0 -7 -9 94.14 4.72 0. 1.0000 0. 0 -7 -10 350.58 12.35 0. 1.0000 0. 0 -7 -10 325.01 11.78 0. 1.0000 0. 0 -7 -10 358.85 13.24 0. 1.0000 0. 0 -7 -11 324.53 11.65 0. 1.0000 0. 0 -7 -11 316.02 9.88 0. 1.0000 0. 0 -7 -11 334.65 10.57 0. 1.0000 0. 0 -7 -12 52.84 4.24 0. 1.0000 0. 0 -7 -12 55.37 4.44 0. 1.0000 0. 0 -7 -12 55.41 5.85 0. 1.0000 0. 0 -7 -13 74.84 6.86 0. 1.0000 0. 0 -7 -13 41.09 4.11 0. 1.0000 0. 0 -7 -14 0.74 4.66 0. 1.0000 0. 0 -7 -14 1.75 2.98 0. 1.0000 0. 0 8 2 249.65 9.30 0. 1.0000 0. 0 8 3 434.87 17.88 0. 1.0000 0. 0 -8 -4 49.97 2.98 0. 1.0000 0. 0 8 4 49.45 3.67 0. 1.0000 0. 0 -8 -4 47.50 2.69 0. 1.0000 0. 0 -8 -4 47.60 2.48 0. 1.0000 0. 0 8 5 49.01 3.31 0. 1.0000 0. 0 8 5 58.28 3.66 0. 1.0000 0. 0 -8 -5 55.76 4.72 0. 1.0000 0. 0 -8 -5 56.61 2.74 0. 1.0000 0. 0 -8 -5 53.06 4.00 0. 1.0000 0. 0 -8 -5 51.07 2.96 0. 1.0000 0. 0 -8 -5 58.61 3.27 0. 1.0000 0. 0 -8 -6 43.17 3.01 0. 1.0000 0. 0 8 6 42.93 3.00 0. 1.0000 0. 0 -8 -6 38.11 2.61 0. 1.0000 0. 0 -8 -6 36.05 2.86 0. 1.0000 0. 0 8 6 35.45 3.40 0. 1.0000 0. 0 -8 -6 37.46 4.12 0. 1.0000 0. 0 -8 -6 35.16 3.56 0. 1.0000 0. 0 8 6 35.66 2.94 0. 1.0000 0. 0 -8 -7 32.71 3.52 0. 1.0000 0. 0 8 7 30.05 4.15 0. 1.0000 0. 0 8 7 38.48 2.95 0. 1.0000 0. 0 -8 -7 35.52 4.07 0. 1.0000 0. 0 8 7 29.41 4.88 0. 1.0000 0. 0 8 8 0.28 2.20 0. 1.0000 0. 0 -8 -8 -0.40 2.56 0. 1.0000 0. 0 -8 -8 0.82 4.19 0. 1.0000 0. 0 8 8 2.23 4.91 0. 1.0000 0. 0 8 9 7.24 2.61 0. 1.0000 0. 0 -8 -9 15.34 7.05 0. 1.0000 0. 0 -8 -9 0.55 7.01 0. 1.0000 0. 0 -8 -9 6.46 2.78 0. 1.0000 0. 0 -8 -10 20.65 3.35 0. 1.0000 0. 0 8 10 16.22 3.14 0. 1.0000 0. 0 -8 -10 23.91 5.41 0. 1.0000 0. 0 8 11 0.23 3.23 0. 1.0000 0. 0 -8 -11 3.73 3.05 0. 1.0000 0. 0 -8 -11 3.61 4.83 0. 1.0000 0. 0 -8 -11 2.76 3.05 0. 1.0000 0. 0 -8 -12 106.67 5.40 0. 1.0000 0. 0 -8 -12 135.52 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1.0000 0. -3 9 5 13.12 5.79 0. 1.0000 0. -3 9 4 94.41 9.26 0. 1.0000 0. 3 -9 -4 134.72 8.04 0. 1.0000 0. -3 9 3 14.74 5.25 0. 1.0000 0. 3 -9 -3 31.05 4.65 0. 1.0000 0. 3 -9 -2 131.35 7.60 0. 1.0000 0. 3 -9 -1 -0.08 3.66 0. 1.0000 0. -3 -9 1 1.10 2.96 0. 1.0000 0. 3 9 0 96.97 6.85 0. 1.0000 0. -3 -9 0 -0.93 3.77 0. 1.0000 0. 3 9 1 75.31 6.94 0. 1.0000 0. -3 -9 -1 36.29 4.37 0. 1.0000 0. -3 -9 -2 6.90 3.45 0. 1.0000 0. 3 9 2 13.18 5.86 0. 1.0000 0. -3 -9 -3 3.98 3.16 0. 1.0000 0. 3 9 3 15.52 6.76 0. 1.0000 0. 3 9 4 -2.44 7.57 0. 1.0000 0. 3 9 5 5.39 6.94 0. 1.0000 0. 3 9 5 3.15 9.50 0. 1.0000 0. 3 9 6 18.61 8.09 0. 1.0000 0. 3 9 6 19.08 12.53 0. 1.0000 0. 3 9 7 6.80 9.73 0. 1.0000 0. 3 9 7 18.24 13.75 0. 1.0000 0. -3 -9 -7 5.87 6.96 0. 1.0000 0. -3 -9 -8 15.08 7.12 0. 1.0000 0. 3 9 8 8.13 11.34 0. 1.0000 0. -3 -9 -8 10.44 7.30 0. 1.0000 0. 3 9 9 -2.15 12.12 0. 1.0000 0. 3 -10 -8 0.20 10.17 0. 1.0000 0. -3 10 8 3.00 5.53 0. 1.0000 0. 3 -10 -7 27.31 8.01 0. 1.0000 0. -3 10 7 10.40 5.60 0. 1.0000 0. 3 -10 -6 0.28 7.01 0. 1.0000 0. -3 10 6 -2.08 5.27 0. 1.0000 0. 3 -10 -5 0.69 5.71 0. 1.0000 0. -3 10 5 3.04 5.80 0. 1.0000 0. 3 -10 -4 -2.24 4.63 0. 1.0000 0. -3 10 4 1.13 5.30 0. 1.0000 0. -3 10 3 24.11 5.46 0. 1.0000 0. 3 -10 -3 42.32 4.98 0. 1.0000 0. 3 -10 -2 4.89 4.06 0. 1.0000 0. -3 -10 0 -0.10 3.60 0. 1.0000 0. -3 -10 0 0.96 2.37 0. 1.0000 0. -3 -10 -1 -1.05 3.70 0. 1.0000 0. 3 10 1 17.25 5.80 0. 1.0000 0. 3 10 2 34.79 6.75 0. 1.0000 0. -3 -10 -2 41.11 6.87 0. 1.0000 0. -3 -10 -3 2.49 3.71 0. 1.0000 0. 3 10 3 4.37 6.40 0. 1.0000 0. 3 10 4 47.81 7.21 0. 1.0000 0. 3 10 4 49.93 8.76 0. 1.0000 0. -3 -10 -4 26.58 4.17 0. 1.0000 0. 3 10 5 1.86 6.91 0. 1.0000 0. 3 10 5 4.71 9.03 0. 1.0000 0. 3 10 6 5.81 7.34 0. 1.0000 0. 3 10 6 7.57 11.31 0. 1.0000 0. 3 10 7 28.96 9.43 0. 1.0000 0. 3 10 8 -12.45 10.90 0. 1.0000 0. -3 -10 -8 -2.56 7.33 0. 1.0000 0. 3 -11 -7 1.52 7.54 0. 1.0000 0. -3 11 7 1.09 6.27 0. 1.0000 0. 3 -11 -6 1.39 6.19 0. 1.0000 0. -3 11 6 1.42 6.10 0. 1.0000 0. 3 -11 -5 34.26 5.78 0. 1.0000 0. -3 11 5 28.55 6.83 0. 1.0000 0. 3 -11 -4 14.35 4.68 0. 1.0000 0. -3 11 4 13.54 5.53 0. 1.0000 0. 3 -11 -3 25.37 4.71 0. 1.0000 0. -3 -11 -1 -2.79 3.77 0. 1.0000 0. 3 11 1 -1.29 5.61 0. 1.0000 0. -3 -11 -2 0.40 3.83 0. 1.0000 0. -3 -11 -2 4.32 6.11 0. 1.0000 0. 3 11 3 62.28 7.77 0. 1.0000 0. -3 -11 -3 28.13 4.64 0. 1.0000 0. 3 11 4 -0.16 6.16 0. 1.0000 0. -3 -11 -4 -0.18 3.75 0. 1.0000 0. 3 11 4 -2.44 7.30 0. 1.0000 0. 3 11 5 -9.05 6.90 0. 1.0000 0. 3 11 5 2.20 8.11 0. 1.0000 0. 3 11 6 -5.28 7.68 0. 1.0000 0. 3 -12 -5 0.93 5.11 0. 1.0000 0. -3 12 5 -2.06 5.71 0. 1.0000 0. 3 -12 -4 5.96 4.56 0. 1.0000 0. 3 -12 -3 -1.02 3.73 0. 1.0000 0. -3 -12 -2 2.44 3.97 0. 1.0000 0. 3 12 2 -1.74 6.01 0. 1.0000 0. -3 -12 -2 4.72 6.27 0. 1.0000 0. -3 -12 -3 0.43 4.04 0. 1.0000 0. 3 12 3 12.16 6.77 0. 1.0000 0. 3 12 4 16.56 6.85 0. 1.0000 0. -3 -12 -4 10.50 4.34 0. 1.0000 0. 3 12 4 25.12 7.38 0. 1.0000 0. 3 12 5 6.32 6.83 0. 1.0000 0. -3 -12 -5 4.67 3.72 0. 1.0000 0. -3 -13 -3 3.06 4.29 0. 1.0000 0. 3 13 3 0.18 7.15 0. 1.0000 0. -3 -13 -3 -5.31 7.21 0. 1.0000 0. 4 0 -4 -3.32 7.80 0. 1.0000 0. 4 0 -3 4.22 8.55 0. 1.0000 0. 4 0 -2 51.03 10.58 0. 1.0000 0. 4 0 -1 -1.67 9.74 0. 1.0000 0. 4 0 0 1.03 10.77 0. 1.0000 0. 4 0 1 -8.07 11.55 0. 1.0000 0. 4 0 2 0.60 12.19 0. 1.0000 0. 4 -1 -3 -4.72 9.46 0. 1.0000 0. 4 1 -3 3.70 7.35 0. 1.0000 0. 4 -1 -2 -4.88 9.97 0. 1.0000 0. 4 1 -2 -2.44 8.36 0. 1.0000 0. 4 -1 -1 -1.51 10.31 0. 1.0000 0. 4 1 -1 2.50 9.26 0. 1.0000 0. 4 -1 0 -2.47 11.55 0. 1.0000 0. 4 1 0 -0.99 10.54 0. 1.0000 0. 4 -1 1 -1.79 11.93 0. 1.0000 0. 4 1 1 18.58 11.59 0. 1.0000 0. 4 1 2 -1.43 11.88 0. 1.0000 0. -4 1 -3 1.73 7.69 0. 1.0000 0. 4 1 3 -4.64 12.59 0. 1.0000 0. 4 2 -3 13.28 6.11 0. 1.0000 0. -4 2 3 15.10 5.19 0. 1.0000 0. 4 -2 -2 13.93 10.96 0. 1.0000 0. 4 2 -2 15.88 7.22 0. 1.0000 0. -4 2 2 7.85 4.95 0. 1.0000 0. 4 2 -1 8.26 8.71 0. 1.0000 0. 4 2 0 -0.95 10.14 0. 1.0000 0. 4 2 1 13.94 10.91 0. 1.0000 0. -4 2 -2 3.24 7.12 0. 1.0000 0. 4 2 2 4.43 10.96 0. 1.0000 0. -4 2 -3 24.44 7.69 0. 1.0000 0. 4 2 3 -2.08 12.17 0. 1.0000 0. 4 3 -2 3.13 6.33 0. 1.0000 0. 4 3 -2 -0.89 10.91 0. 1.0000 0. -4 3 2 1.28 4.73 0. 1.0000 0. 4 3 -1 -3.81 7.71 0. 1.0000 0. 4 3 0 -4.62 8.54 0. 1.0000 0. 4 3 1 4.09 10.29 0. 1.0000 0. -4 3 -2 30.14 7.54 0. 1.0000 0. 4 3 2 19.60 11.52 0. 1.0000 0. 4 4 -1 -1.12 6.60 0. 1.0000 0. 4 4 -1 -5.86 11.31 0. 1.0000 0. 4 4 0 -3.10 7.96 0. 1.0000 0. 4 4 0 3.41 12.63 0. 1.0000 0. -4 4 -1 8.49 6.30 0. 1.0000 0. 4 4 1 11.60 9.39 0. 1.0000 0. -512 # 3444 reflections output ; # end of ARCHIVE-HKL.CIF _chemical_name_common ROY _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: acetone' ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_ROY_ON_1p91GPa _database_code_depnum_ccdc_archive 'CCDC 2098639' loop_ _audit_author_name _audit_author_address 'Nicholas Funnell' ;STFC, ISIS Neutron Facility United Kingdom ; _audit_update_record ; 2021-07-22 deposited with the CCDC. 2021-08-27 downloaded from the CCDC. ; _audit_creation_date 2021-01-26 _audit_creation_method 'CRYSTALS_ver_14.61_build_7795 ' _chemical_name_systematic ; 5-methyl-2[(2-nitrophenyl)amino]-3-thiophenecarbonitrile ; #CheckCIF alerts _vrf_THETM01_ROY_ON_1p91GPa ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575 RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT027_ROY_ON_1p91GPa ; PROBLEM: _diffrn_reflns_theta_full value (too) Low ...... 17.42 Degree RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT029_ROY_ON_1p91GPa ; PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.730 Why? RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT201_ROY_ON_1p91GPa ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 17 Report RESPONSE: The model could only be refined isotropically in order to maintain a favourable data-to-parameter ratio, due to numerous unmeasured reflections. The relatively electron-rich sulfur atom has been modelled anisotropically. ; _vrf_PLAT340_ROY_ON_1p91GPa ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.01027 Ang. RESPONSE: These are poor-quality diffraction data. ; _vrf_PLAT911_ROY_ON_1p91GPa ; PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.555 403 Report RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT157_ROY_ON_1p91GPa ; PROBLEM: Non-standard Monoclinic Beta Angle less 90 Deg 89.65 Degree RESPONSE: This is a series of high pressure structures where the beta angle decreases, passing through 90 degrees. The non-standard beta angle allows the change in angle to be followed clearly. ; _vrf_PLAT411_ROY_ON_1p91GPa ; PROBLEM: Short Inter H...H Contact H5 ..H5 . 2.13 Ang. RESPONSE: These are high-pressure data - short contacts are expected. ; _vrf_PLAT413_ROY_ON_1p91GPa ; PROBLEM: Short Inter XH3 .. XHn H111 ..H113 . 2.11 Ang. RESPONSE: These are high-pressure data - short contacts are expected. ; _vrf_PLAT910_ROY_ON_1p91GPa ; PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 8 Note RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; # end Validation Reply Form _refine_special_details ; In the absence of significant anomalous scattering, Friedel pairs were merged. Data were collected in a Merrill-Bassett diamond anvil cell, which significantly restricts the regions over which reciprocal space can be sampled. Thus, these data are poor quality/incomplete, reflected in numerous CheckCIF alerts regarding refinement statistics. At all pressures, the atomic connectivity is known. All non-sulfur atoms were refined isotropically; sulfur was refined anisotropically. Hydrogen atoms were constrained to ride on their host atoms. #=============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Total Missing #------------------------------------------------------------------------------- 20.82 0.500 0.714 1078 770 308 23.01 0.550 0.705 1359 958 401 23.22 0.555 0.705 1395 984 411 ------------------------------------------------------------ ACTA Min. Res. --- Note: The Reported Completeness refers to the Actual H,K,L Index Range ; #end of refcif _cell_length_a 3.631200(17) _cell_length_b 17.68860(4) _cell_length_c 16.02610(5) _cell_angle_alpha 90 _cell_angle_beta 89.648(5) _cell_angle_gamma 90 _cell_volume 1029.350(6) _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' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 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' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C12 H9 N3 O2 S1 # Dc = 1.67 Fooo = 536.00 Mu = 3.11 M = 259.29 # Found Formula = C12 H9 N3 O2 S1 # Dc = 1.67 FOOO = 536.00 Mu = 3.11 M = 259.29 _chemical_formula_sum 'C12 H9 N3 O2 S1' _chemical_formula_moiety 'C12 H9 N3 O2 S1' _chemical_compound_source 'TCI Chemicals' _chemical_formula_weight 259.29 _cell_measurement_reflns_used 1893 _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 23.17 _cell_measurement_temperature 293 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_min 0.050 _exptl_crystal_size_mid 0.072 _exptl_crystal_size_max 0.248 _exptl_crystal_density_diffrn 1.673 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 0.311 # Sheldrick geometric approximatio 0.98 0.98 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North et al., 1968)' _exptl_absorpt_correction_T_min 0.15 _exptl_absorpt_correction_T_max 0.98 _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_device 'four-circle diffractometer' _diffrn_radiation_monochromator mirror _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 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction ; CrysAlisPro (Rigaku Oxford Diffraction, 2017) ; _computing_structure_solution 'Model from previously-determined structure' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 293 _diffrn_ambient_pressure 1910000 _diffrn_reflns_number 3093 _diffrn_reflns_av_unetI/netI 0.037 _reflns_number_total 1005 _diffrn_reflns_av_R_equivalents 0.042 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 1005 # Theoretical number of reflections is about 2945 _diffrn_reflns_theta_min 1.715 _diffrn_reflns_theta_max 23.221 _diffrn_measured_fraction_theta_max 0.691 _diffrn_reflns_theta_full 17.416 _diffrn_measured_fraction_theta_full 0.730 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -4 _reflns_limit_h_max 4 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.86 _refine_diff_density_max 0.80 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # Explicitly named reflections are ALWAYS excluded from R&wR # The values actually used during refinement # These are labelled "all" for compatibility with PLATON _oxford_refine_reflns_threshold_expression I>-3.0\s(I) _refine_ls_number_restraints 94 _refine_ls_number_parameters 82 _refine_ls_number_reflns 984 _oxford_refine_ls_R_factor_ref 0.1401 _refine_ls_R_factor_all 0.1401 _refine_ls_wR_factor_ref 0.0407 _refine_ls_wR_factor_all 0.0407 _refine_ls_goodness_of_fit_ref 1.0777 _refine_ls_shift/su_max 0.0001395 _refine_ls_shift/su_mean 0.0000293 # Computed with I/sigma = -10 _oxford_reflns_number_all 984 _oxford_refine_ls_R_factor_all 0.1401 _oxford_refine_ls_wR_factor_all 0.0407 # Computed with no filters except I/sigma = +2 a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 780 _refine_ls_R_factor_gt 0.1038 _refine_ls_wR_factor_gt 0.0384 _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed #undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ; Method= SQRT(W) = 1/(Data with the key SIGMA(/FO/) in list 6) ; # 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 S1 S 0.7043(4) 0.58954(11) 0.43423(11) 0.0317 1.0000 Uani D U . . . . O1 O 0.4713(12) 0.6315(3) 0.0238(4) 0.0460(15) 1.0000 Uiso D U . . . . O2 O 0.4882(11) 0.6991(3) 0.1378(4) 0.0455(16) 1.0000 Uiso D U . . . . C1 C 0.8544(15) 0.5839(4) 0.2229(5) 0.0313(15) 1.0000 Uiso D U . . . . C2 C 1.0392(16) 0.5208(4) 0.2575(6) 0.0318(17) 1.0000 Uiso D U . . . . C3 C 1.1135(15) 0.4603(4) 0.2083(5) 0.0313(17) 1.0000 Uiso D U . . . . C4 C 1.0057(14) 0.4563(4) 0.1258(5) 0.0337(18) 1.0000 Uiso D U . . . . C5 C 0.8249(16) 0.5171(4) 0.0888(5) 0.0287(16) 1.0000 Uiso D U . . . . C6 C 0.7521(15) 0.5792(4) 0.1407(5) 0.0306(15) 1.0000 Uiso D U . . . . C7 C 0.8421(16) 0.6528(4) 0.3591(5) 0.0312(17) 1.0000 Uiso D U . . . . C8 C 1.0032(14) 0.7148(4) 0.3938(5) 0.0295(17) 1.0000 Uiso D U . . . . C9 C 1.0080(15) 0.7125(4) 0.4817(5) 0.0318(18) 1.0000 Uiso D U . . . . C10 C 0.8529(11) 0.6492(3) 0.5136(5) 0.0320(16) 1.0000 Uiso D U . . . . C11 C 0.8098(11) 0.6230(3) 0.6024(4) 0.0378(19) 1.0000 Uiso D U . . . . C12 C 1.1802(15) 0.7691(5) 0.3418(4) 0.0314(16) 1.0000 Uiso D U . . . . N1 N 0.7825(14) 0.6435(4) 0.2737(4) 0.0323(16) 1.0000 Uiso D U . . . . N2 N 1.3230(14) 0.8064(3) 0.2942(4) 0.0370(16) 1.0000 Uiso D U . . . . N3 N 0.5598(14) 0.6404(4) 0.0965(5) 0.0402(16) 1.0000 Uiso D U . . . . H1 H 0.658(8) 0.678(2) 0.251(3) 0.040(5) 1.0000 Uiso D . . . . . H2 H 1.1096 0.5206 0.3129 0.0401 1.0000 Uiso R . . . . . H3 H 1.2429 0.4196 0.2305 0.0409 1.0000 Uiso R . . . . . H4 H 1.0540 0.4131 0.0943 0.0410 1.0000 Uiso R . . . . . H5 H 0.7562 0.5160 0.0330 0.0421 1.0000 Uiso R . . . . . H9 H 1.1091 0.7504 0.5146 0.0420 1.0000 Uiso R . . . . . H111 H 0.9919 0.5851 0.6138 0.0581 1.0000 Uiso DR . . . . . H112 H 0.8418 0.6655 0.6392 0.0581 1.0000 Uiso DR . . . . . H113 H 0.5680 0.6023 0.6100 0.0580 1.0000 Uiso DR . . . . . 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 S1 0.0405(9) 0.0249(16) 0.0296(18) 0.0016(9) -0.0045(9) -0.0024(9) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.554(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 S1 . C7 . 1.715(8) yes S1 . C10 . 1.741(7) yes O1 . N3 . 1.221(7) yes O2 . N3 . 1.258(8) yes C1 . C2 . 1.417(10) yes C1 . C6 . 1.373(9) yes C1 . N1 . 1.358(9) yes C2 . C3 . 1.356(9) yes C2 . H2 . 0.926 no C3 . C4 . 1.382(9) yes C3 . H3 . 0.932 no C4 . C5 . 1.394(9) yes C4 . H4 . 0.932 no C5 . C6 . 1.403(10) yes C5 . H5 . 0.929 no C6 . N3 . 1.472(10) yes C7 . C8 . 1.364(9) yes C7 . N1 . 1.397(9) yes C8 . C9 . 1.410(9) yes C8 . C12 . 1.423(9) yes C9 . C10 . 1.353(8) yes C9 . H9 . 0.930 no C10 . C11 . 1.504(9) yes C11 . H111 . 0.960 no C11 . H112 . 0.962 no C11 . H113 . 0.958 no C12 . N2 . 1.132(7) yes N1 . H1 . 0.84(4) 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 C7 . S1 . C10 . 91.6(4) yes C2 . C1 . C6 . 117.4(6) yes C2 . C1 . N1 . 117.8(8) yes C6 . C1 . N1 . 124.8(7) yes C1 . C2 . C3 . 119.1(9) yes C1 . C2 . H2 . 120.9 no C3 . C2 . H2 . 120.0 no C2 . C3 . C4 . 122.7(7) yes C2 . C3 . H3 . 119.0 no C4 . C3 . H3 . 118.3 no C3 . C4 . C5 . 120.4(8) yes C3 . C4 . H4 . 120.3 no C5 . C4 . H4 . 119.3 no C4 . C5 . C6 . 116.0(8) yes C4 . C5 . H5 . 121.6 no C6 . C5 . H5 . 122.4 no C5 . C6 . C1 . 124.4(7) yes C5 . C6 . N3 . 112.3(8) yes C1 . C6 . N3 . 123.3(7) yes S1 . C7 . C8 . 111.3(7) yes S1 . C7 . N1 . 124.4(5) yes C8 . C7 . N1 . 124.3(6) yes C7 . C8 . C9 . 113.1(6) yes C7 . C8 . C12 . 119.8(8) yes C9 . C8 . C12 . 126.7(6) yes C8 . C9 . C10 . 113.2(6) yes C8 . C9 . H9 . 123.6 no C10 . C9 . H9 . 123.3 no S1 . C10 . C9 . 110.9(6) yes S1 . C10 . C11 . 118.3(3) yes C9 . C10 . C11 . 130.8(4) yes C10 . C11 . H111 . 109.1 no C10 . C11 . H112 . 109.1 no H111 . C11 . H112 . 110.0 no C10 . C11 . H113 . 109.1 no H111 . C11 . H113 . 109.9 no H112 . C11 . H113 . 109.6 no C8 . C12 . N2 . 172.7(10) yes C7 . N1 . C1 . 130.5(7) yes C7 . N1 . H1 . 115(3) no C1 . N1 . H1 . 114(3) no C6 . N3 . O2 . 116.8(7) yes C6 . N3 . O1 . 119.5(7) yes O2 . N3 . O1 . 123.7(7) yes _iucr_refine_instructions_details ; # # Punched on 26/01/21 at 09:47:27 # #LIST 12 BLOCK CONT SCALE CONT S ( 1 ,X'S,U'S) CONT O ( 1 ,X'S,U[ISO]) UNTIL H ( 1 ) RIDE C ( 2,X'S) H ( 2,X'S) RIDE C ( 3,X'S) H ( 3,X'S) RIDE C ( 4,X'S) H ( 4,X'S) RIDE C ( 5,X'S) H ( 5,X'S) RIDE C ( 9,X'S) H ( 9,X'S) RIDE C ( 11,X'S) H ( 111,X'S) H ( 112,X'S) H ( 113,X'S) END # # Punched on 26/01/21 at 09:47:27 # #LIST 16 NO REM REM NPF NOTE - FIRST UNTIL LAST REM REM HREST START (DO NOT REMOVE THIS LINE) REM NO H NO #H U MULT DIST REM C-H REM >4 1.5 .96 DISORDER REM 1 1 1.2 .93 C C-H (ACETYLENE) REM 1 2 1.2 .93 C-C(H)-C REM 1 3 1.2 .98 (C)3-C-H REM 2 1 1.2 .93 C=C-H(2) REM 2 2 1.2 .97 (C)2-C-(H)2 REM 3 1 1.5 .96 C-C-(H)3 REM N-H REM >4 1.5 .89 DISORDER REM 1 1 1.2 .86 N-N/H REM 1 2 1.2 .86 (C)2-N-H REM 1 3 1.2 .89 (C)3-N-H REM 2 1 1.2 .86 C-N-(H)2 REM 2 2 1.2 .89 (C)2-N-(H)2 REM 3 1 1.2 .89 C-H-(H)3 REM O-H REM 1 1 1.5 .82 O-H REM REM DIST ESD = 0.02 REM VIB ESD = 0.002 REM ANGLE ESD = 2.0 REM REM TO ACTIVATE THE VIB RESTRAINTS, REMOVE LEADING REM REM H1-N-R2 DIST 0.86, 0.02 = CONT N ( 1) TO H(1) REST 0.040, 0.002 = H(1,U[ISO]) ANGLE 0.0, 2.0 = MEAN CONT H(1) TO N ( 1) TO C(7) CONT H(1) TO N ( 1) TO C(1) REM HREST END (DO NOT REMOVE THIS LINE) REM DELU START (DO NOT REMOVE THIS LINE) VIBR .0, 0.00200 = S(1) TO C(10) VIBR .0, 0.00200 = S(1) TO C(7) VIBR .0, 0.00500 = C(7) TO C(10) VIBR .0, 0.00200 = N(2) TO C(12) VIBR .0, 0.00200 = C(10) TO C(9) VIBR .0, 0.00200 = C(10) TO C(11) VIBR .0, 0.00500 = C(9) TO S(1) VIBR .0, 0.00500 = C(11) TO S(1) VIBR .0, 0.00500 = C(11) TO C(9) VIBR .0, 0.00200 = C(12) TO C(8) VIBR .0, 0.00500 = C(8) TO N(2) VIBR .0, 0.00200 = O(1) TO N(3) VIBR .0, 0.00200 = C(2) TO C(1) VIBR .0, 0.00200 = C(2) TO C(3) VIBR .0, 0.00500 = C(3) TO C(1) VIBR .0, 0.00200 = N(1) TO C(7) VIBR .0, 0.00200 = N(1) TO C(1) VIBR .0, 0.00500 = C(1) TO C(7) VIBR .0, 0.00200 = C(7) TO C(8) VIBR .0, 0.00500 = N(1) TO S(1) VIBR .0, 0.00500 = C(8) TO S(1) VIBR .0, 0.00500 = C(8) TO N(1) VIBR .0, 0.00200 = O(2) TO N(3) VIBR .0, 0.00200 = N(3) TO C(6) VIBR .0, 0.00500 = O(1) TO O(2) VIBR .0, 0.00500 = C(6) TO O(2) VIBR .0, 0.00500 = C(6) TO O(1) VIBR .0, 0.00200 = C(5) TO C(4) VIBR .0, 0.00200 = C(5) TO C(6) VIBR .0, 0.00500 = C(6) TO C(4) VIBR .0, 0.00200 = C(4) TO C(3) VIBR .0, 0.00500 = C(3) TO C(5) VIBR .0, 0.00200 = C(1) TO C(6) VIBR .0, 0.00500 = N(1) TO C(2) VIBR .0, 0.00500 = C(6) TO C(2) VIBR .0, 0.00500 = C(6) TO N(1) VIBR .0, 0.00500 = C(5) TO N(3) VIBR .0, 0.00500 = C(1) TO N(3) VIBR .0, 0.00500 = C(1) TO C(5) VIBR .0, 0.00200 = C(9) TO C(8) VIBR .0, 0.00500 = C(8) TO C(10) VIBR .0, 0.00500 = C(2) TO C(4) VIBR .0, 0.00500 = C(12) TO C(9) VIBR .0, 0.00500 = C(7) TO C(9) VIBR .0, 0.00500 = C(7) TO C(12) REM DELU END (DO NOT REMOVE THIS LINE) ANGLE 110.000000 , 0.020000 = C(10) TO C(11) TO H(111) ANGLE 110.000000 , 0.020000 = C(10) TO C(11) TO H(112) ANGLE 110.000000 , 0.020000 = C(10) TO C(11) TO H(113) DISTANCE 1.225000 , 0.050000 = O(2) TO N(3) DISTANCE 1.225000 , 0.050000 = O(1) TO N(3) DISTANCE 1.440000 , 0.050000 = C(6) TO N(3) DISTANCE 1.390000 , 0.050000 = C(5) TO C(6) DISTANCE 1.364000 , 0.050000 = C(4) TO C(5) DISTANCE 1.222000 , 0.050000 = O(1) TO N(3) DISTANCE 1.232000 , 0.050000 = O(2) TO N(3) DISTANCE 1.440000 , 0.050000 = C(6) TO N(3) DISTANCE 1.392000 , 0.050000 = C(5) TO C(6) DISTANCE 1.364000 , 0.050000 = C(4) TO C(5) DISTANCE 1.391000 , 0.050000 = C(3) TO C(4) DISTANCE 1.371000 , 0.050000 = C(2) TO C(3) DISTANCE 1.400000 , 0.050000 = C(1) TO C(2) DISTANCE 1.408000 , 0.050000 = C(1) TO C(6) DISTANCE 1.382000 , 0.050000 = C(1) TO N(1) DISTANCE 1.387000 , 0.050000 = C(7) TO N(1) DISTANCE 1.728000 , 0.050000 = S(1) TO C(7) DISTANCE 1.724000 , 0.050000 = S(1) TO C(10) DISTANCE 1.500000 , 0.050000 = C(10) TO C(11) DISTANCE 1.349000 , 0.050000 = C(9) TO C(10) DISTANCE 1.427000 , 0.050000 = C(8) TO C(9) DISTANCE 1.372000 , 0.050000 = C(7) TO C(8) DISTANCE 1.422000 , 0.050000 = C(8) TO C(12) DISTANCE 1.141000 , 0.050000 = C(12) TO N(2) REM THERMSIM START (DO NOT REMOVE THIS LINE) U(IJ) .0, 0.04000 = S(1) TO C(7) U(IJ) .0, 0.04000 = S(1) TO C(10) U(IJ) .0, 0.08000 = O(1) TO N(3) U(IJ) .0, 0.08000 = O(2) TO N(3) U(IJ) .0, 0.04000 = C(1) TO C(2) U(IJ) .0, 0.04000 = C(1) TO C(6) U(IJ) .0, 0.04000 = C(1) TO N(1) U(IJ) .0, 0.04000 = C(2) TO C(3) U(IJ) .0, 0.04000 = C(3) TO C(4) U(IJ) .0, 0.04000 = C(4) TO C(5) U(IJ) .0, 0.04000 = C(5) TO C(6) U(IJ) .0, 0.04000 = C(6) TO N(3) U(IJ) .0, 0.04000 = C(7) TO C(8) U(IJ) .0, 0.04000 = C(7) TO N(1) U(IJ) .0, 0.04000 = C(8) TO C(9) U(IJ) .0, 0.04000 = C(8) TO C(12) U(IJ) .0, 0.04000 = C(9) TO C(10) U(IJ) .0, 0.08000 = C(10) TO C(11) U(IJ) .0, 0.08000 = C(12) TO N(2) REM THERMSIM END (DO NOT REMOVE THIS LINE) PLANAR 0.010000 C(1) C(6) N(1) H(1) PLANAR 0.010000 C(1) C(2) C(3) C(4) C(5) C(6) N(1) N(3) PLANAR 0.010000 S(1) C(7) C(8) C(9) C(10) N(1) 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 1 5 11 x . -1 6 13 x . 1 3 9 x . -2 12 3 x . 1 13 4 x . -2 14 5 x . 3 10 0 x . 3 7 1 x . 0 13 4 x . -1 3 9 x . 2 0 6 x . 2 10 1 x . 0 14 5 x . -3 3 10 x . 3 8 0 x . 1 11 2 x . # looking for ARCHIVE-HKL.CIF _iucr_refine_reflections_details ; # Data was input as F-squared # punching LIST 6 as LIST 6 with all keys set # NBGNXT= 36 #LIST 6 READ NCOEF= 8 TYPE=FIX, F'S = FSQ UNIT=DATA, CHECK=NO L30=NO ARCH=NO STORE NCOEF= 6 OUTPUT INDICES /FO/ SIGMA(/FO/) RATIO/JCODE CORRECTIONS SERIAL CONT INPUT H K L /FO/ SIGMA(/FO/) JCODE CONT CORRECTIONS SERIAL FOR (I4,I4,I4,F10.2,F8.2,F4.0,F7.4,F7.0) END 0 -1 -1 10.18 0.40 0. 1.0000 0. 0 -1 -1 9.65 0.38 0. 1.0000 0. 0 1 1 8.58 0.34 0. 1.0000 0. 0 -1 -3 914.58 15.85 0. 1.0000 0. 0 -1 -4 179.39 4.23 0. 1.0000 0. 0 2 1 2142.72 34.50 0. 1.0000 0. 0 -2 -1 2121.87 34.62 0. 1.0000 0. 0 2 1 2125.87 34.47 0. 1.0000 0. 0 -2 -1 2112.75 34.77 0. 1.0000 0. 0 2 2 133.91 2.73 0. 1.0000 0. 0 2 2 136.41 2.46 0. 1.0000 0. 0 2 2 159.74 2.77 0. 1.0000 0. 0 2 2 141.17 2.76 0. 1.0000 0. 0 2 2 128.09 2.59 0. 1.0000 0. 0 2 2 145.32 2.82 0. 1.0000 0. 0 2 2 147.12 2.62 0. 1.0000 0. 0 -2 -3 1085.13 17.31 0. 1.0000 0. 0 2 3 1060.54 17.58 0. 1.0000 0. 0 2 3 1018.81 17.66 0. 1.0000 0. 0 2 3 1024.43 17.49 0. 1.0000 0. 0 -2 -3 1029.88 17.35 0. 1.0000 0. 0 2 3 1018.91 17.63 0. 1.0000 0. 0 -2 -4 50.49 1.77 0. 1.0000 0. 0 -2 -4 53.65 1.82 0. 1.0000 0. 0 -2 -4 49.09 1.74 0. 1.0000 0. 0 -2 -5 752.68 13.39 0. 1.0000 0. 0 -2 -5 719.09 13.15 0. 1.0000 0. 0 -2 -6 1204.31 21.22 0. 1.0000 0. 0 3 1 683.58 11.56 0. 1.0000 0. 0 -3 -1 661.97 12.24 0. 1.0000 0. 0 3 1 692.01 11.51 0. 1.0000 0. 0 -3 -2 68.30 1.64 0. 1.0000 0. 0 3 2 70.41 1.58 0. 1.0000 0. 0 -3 -2 68.06 1.90 0. 1.0000 0. 0 3 2 71.69 1.71 0. 1.0000 0. 0 -3 -2 72.26 1.64 0. 1.0000 0. 0 3 2 60.56 1.48 0. 1.0000 0. 0 3 2 73.27 1.65 0. 1.0000 0. 0 3 2 70.18 1.79 0. 1.0000 0. 0 -3 -2 82.89 1.76 0. 1.0000 0. 0 -3 -2 72.44 1.59 0. 1.0000 0. 0 -3 -2 69.93 1.39 0. 1.0000 0. 0 3 3 3.21 0.83 0. 1.0000 0. 0 -3 -3 2.41 0.53 0. 1.0000 0. 0 3 3 3.21 0.68 0. 1.0000 0. 0 -3 -3 2.35 0.49 0. 1.0000 0. 0 3 3 3.86 0.81 0. 1.0000 0. 0 3 3 3.16 0.63 0. 1.0000 0. 0 3 3 3.26 0.76 0. 1.0000 0. 0 3 3 2.85 0.53 0. 1.0000 0. 0 -3 -3 4.97 0.86 0. 1.0000 0. 0 3 3 3.07 0.47 0. 1.0000 0. 0 3 3 2.97 0.63 0. 1.0000 0. 0 -3 -4 197.97 3.80 0. 1.0000 0. 0 3 4 206.11 4.16 0. 1.0000 0. 0 3 4 184.03 4.15 0. 1.0000 0. 0 -3 -4 184.24 3.90 0. 1.0000 0. 0 3 5 70.08 2.39 0. 1.0000 0. 0 -3 -5 78.47 2.35 0. 1.0000 0. 0 -3 -5 77.47 2.28 0. 1.0000 0. 0 -3 -5 91.89 2.28 0. 1.0000 0. 0 -3 -6 115.33 3.07 0. 1.0000 0. 0 -3 -6 116.10 3.15 0. 1.0000 0. 0 -3 -7 1.06 1.43 0. 1.0000 0. 0 -3 -7 1.27 1.31 0. 1.0000 0. 0 -3 -8 0.97 1.29 0. 1.0000 0. 0 -3 -8 19.35 1.80 0. 1.0000 0. 0 -4 -1 0.04 1.35 0. 1.0000 0. 0 4 1 0.04 0.66 0. 1.0000 0. 0 -4 -1 0.76 0.74 0. 1.0000 0. 0 -4 -2 787.31 13.80 0. 1.0000 0. 0 -4 -2 802.40 13.65 0. 1.0000 0. 0 4 2 795.67 13.62 0. 1.0000 0. 0 -4 -2 799.78 14.42 0. 1.0000 0. 0 4 2 823.22 13.67 0. 1.0000 0. 0 -4 -2 845.02 13.73 0. 1.0000 0. 0 4 3 75.60 1.92 0. 1.0000 0. 0 4 3 70.42 1.80 0. 1.0000 0. 0 -4 -3 83.47 1.72 0. 1.0000 0. 0 4 3 82.87 2.01 0. 1.0000 0. 0 -4 -3 80.28 2.40 0. 1.0000 0. 0 -4 -3 92.37 2.13 0. 1.0000 0. 0 -4 -3 85.23 2.10 0. 1.0000 0. 0 -4 -3 77.85 1.90 0. 1.0000 0. 0 4 4 44.42 1.16 0. 1.0000 0. 0 4 4 51.65 1.56 0. 1.0000 0. 0 -4 -4 38.70 1.37 0. 1.0000 0. 0 4 4 48.55 1.49 0. 1.0000 0. 0 4 4 53.92 1.75 0. 1.0000 0. 0 4 5 741.73 12.41 0. 1.0000 0. 0 -4 -5 715.59 12.77 0. 1.0000 0. 0 4 5 750.11 13.32 0. 1.0000 0. 0 4 5 738.23 12.97 0. 1.0000 0. 0 4 6 125.07 3.76 0. 1.0000 0. 0 -4 -6 131.82 3.36 0. 1.0000 0. 0 -4 -7 221.96 5.21 0. 1.0000 0. 0 -4 -7 257.37 5.86 0. 1.0000 0. 0 -4 -7 227.37 5.06 0. 1.0000 0. 0 4 8 0.86 2.01 0. 1.0000 0. 0 -4 -8 5.99 1.58 0. 1.0000 0. 0 -4 -8 5.99 1.72 0. 1.0000 0. 0 -4 -9 241.51 5.59 0. 1.0000 0. 0 -4 -9 251.42 4.84 0. 1.0000 0. 0 -4 -9 228.54 4.76 0. 1.0000 0. 0 -4 -10 0.35 1.35 0. 1.0000 0. 0 -4 -10 -0.57 2.05 0. 1.0000 0. 0 4 10 1.60 2.26 0. 1.0000 0. 0 -5 -2 952.75 16.16 0. 1.0000 0. 0 -5 -2 937.53 16.33 0. 1.0000 0. 0 -5 -2 937.01 17.29 0. 1.0000 0. 0 5 3 323.43 6.02 0. 1.0000 0. 0 -5 -3 339.89 6.94 0. 1.0000 0. 0 -5 -3 334.42 6.11 0. 1.0000 0. 0 -5 -3 320.15 5.66 0. 1.0000 0. 0 -5 -3 321.35 6.22 0. 1.0000 0. 0 -5 -4 633.86 11.99 0. 1.0000 0. 0 -5 -4 684.69 11.57 0. 1.0000 0. 0 5 4 645.91 11.28 0. 1.0000 0. 0 5 4 634.79 11.41 0. 1.0000 0. 0 5 5 404.26 7.45 0. 1.0000 0. 0 5 5 363.79 6.54 0. 1.0000 0. 0 5 5 380.72 7.09 0. 1.0000 0. 0 -5 -6 11.85 1.72 0. 1.0000 0. 0 5 6 11.19 1.07 0. 1.0000 0. 0 5 6 13.46 1.56 0. 1.0000 0. 0 -5 -6 11.26 1.27 0. 1.0000 0. 0 5 6 10.58 1.96 0. 1.0000 0. 0 5 7 361.20 8.07 0. 1.0000 0. 0 -5 -7 406.75 6.99 0. 1.0000 0. 0 -5 -8 18.64 2.57 0. 1.0000 0. 0 -5 -8 20.17 2.10 0. 1.0000 0. 0 5 8 10.22 2.32 0. 1.0000 0. 0 -5 -9 314.36 6.97 0. 1.0000 0. 0 -5 -9 330.03 6.44 0. 1.0000 0. 0 -5 -9 298.51 6.59 0. 1.0000 0. 0 -5 -10 1.50 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0. 1.0000 0. 3 10 7 44.86 6.17 0. 1.0000 0. -3 -10 -7 36.03 5.98 0. 1.0000 0. 3 10 6 6.95 5.18 0. 1.0000 0. 3 10 5 9.64 5.27 0. 1.0000 0. 3 10 4 46.71 5.58 0. 1.0000 0. -3 -10 -3 5.18 4.49 0. 1.0000 0. -3 -10 -2 34.66 4.68 0. 1.0000 0. -3 -10 -1 8.41 3.85 0. 1.0000 0. -3 -10 0 2.11 3.92 0. 1.0000 0. -3 10 2 8.84 3.78 0. 1.0000 0. 3 -10 -3 134.99 7.49 0. 1.0000 0. -3 10 3 147.30 5.93 0. 1.0000 0. 3 -10 -4 1.16 5.30 0. 1.0000 0. 3 -10 -4 -1.89 5.48 0. 1.0000 0. -3 10 4 9.47 4.21 0. 1.0000 0. -3 10 4 5.18 3.77 0. 1.0000 0. 3 -10 -5 7.21 5.71 0. 1.0000 0. -3 10 5 11.49 4.27 0. 1.0000 0. -3 10 5 13.66 3.88 0. 1.0000 0. 3 -10 -6 17.08 5.71 0. 1.0000 0. -3 10 6 13.41 4.84 0. 1.0000 0. 3 -10 -7 12.43 5.56 0. 1.0000 0. -3 10 7 7.96 5.12 0. 1.0000 0. 3 11 6 7.53 5.38 0. 1.0000 0. 3 11 5 25.93 5.58 0. 1.0000 0. -3 -11 -4 3.79 4.76 0. 1.0000 0. 3 11 4 5.46 4.79 0. 1.0000 0. -3 -11 -3 109.47 6.12 0. 1.0000 0. -3 -11 -2 9.37 4.24 0. 1.0000 0. -3 -11 -1 -0.06 3.32 0. 1.0000 0. 3 -11 -2 1.17 5.32 0. 1.0000 0. -3 11 2 0.60 3.15 0. 1.0000 0. 3 -11 -3 34.02 6.17 0. 1.0000 0. -3 11 3 77.79 5.11 0. 1.0000 0. 3 -11 -4 -1.05 5.57 0. 1.0000 0. 3 -11 -4 0.60 5.75 0. 1.0000 0. -3 11 4 1.19 4.26 0. 1.0000 0. -3 11 4 1.87 3.88 0. 1.0000 0. -3 11 5 37.96 4.95 0. 1.0000 0. 3 -11 -5 30.04 6.38 0. 1.0000 0. -3 11 5 32.91 4.41 0. 1.0000 0. 3 -11 -6 18.94 6.15 0. 1.0000 0. -3 11 6 15.03 5.13 0. 1.0000 0. -3 11 6 14.59 4.58 0. 1.0000 0. -3 -12 -4 -0.15 5.24 0. 1.0000 0. 3 12 4 13.18 5.28 0. 1.0000 0. -3 -12 -3 1.06 4.50 0. 1.0000 0. -3 -12 -2 0.39 4.07 0. 1.0000 0. -3 -12 -2 1.00 3.95 0. 1.0000 0. 3 -12 -3 2.35 5.22 0. 1.0000 0. -3 12 3 -0.64 3.56 0. 1.0000 0. 3 -12 -4 3.46 5.57 0. 1.0000 0. -3 12 4 16.33 4.62 0. 1.0000 0. -3 12 4 15.60 4.30 0. 1.0000 0. 4 0 2 15.40 8.05 0. 1.0000 0. -4 0 -2 12.10 5.64 0. 1.0000 0. -4 0 -1 -2.02 5.57 0. 1.0000 0. 4 0 1 3.80 7.38 0. 1.0000 0. 4 0 0 38.50 7.02 0. 1.0000 0. 4 0 -1 3.20 6.02 0. 1.0000 0. 4 0 -2 133.27 7.32 0. 1.0000 0. 4 -1 2 6.90 8.03 0. 1.0000 0. -4 1 -2 9.57 5.64 0. 1.0000 0. -4 -1 -2 6.32 5.68 0. 1.0000 0. 4 1 2 13.60 7.29 0. 1.0000 0. 4 -1 1 5.39 7.74 0. 1.0000 0. -4 -1 -1 0.63 5.46 0. 1.0000 0. 4 1 1 11.05 6.37 0. 1.0000 0. 4 -1 0 9.60 7.43 0. 1.0000 0. -4 -1 0 0.62 5.55 0. 1.0000 0. 4 1 0 3.44 5.85 0. 1.0000 0. -4 1 1 1.98 5.60 0. 1.0000 0. 4 -1 -1 -0.94 6.77 0. 1.0000 0. 4 1 -1 5.37 5.51 0. 1.0000 0. -4 -2 -1 29.73 6.22 0. 1.0000 0. 4 2 1 33.49 6.55 0. 1.0000 0. 4 -2 0 4.56 7.38 0. 1.0000 0. -4 2 0 3.24 5.63 0. 1.0000 0. -4 -2 0 1.58 5.81 0. 1.0000 0. 4 2 0 1.90 5.52 0. 1.0000 0. 4 -2 -1 4.40 7.23 0. 1.0000 0. -4 2 1 -5.35 5.65 0. 1.0000 0. -4 -2 1 0.87 6.09 0. 1.0000 0. 4 2 -1 -1.39 5.15 0. 1.0000 0. -512 # 3158 reflections output ; # end of ARCHIVE-HKL.CIF _chemical_name_common ROY _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: acetone' ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_ROY_ON_decompress_0p0GPa _database_code_depnum_ccdc_archive 'CCDC 2098644' loop_ _audit_author_name _audit_author_address 'Nicholas Funnell' ;STFC, ISIS Neutron Facility United Kingdom ; _audit_update_record ; 2021-07-22 deposited with the CCDC. 2021-08-27 downloaded from the CCDC. ; _audit_creation_date 2021-01-26 _audit_creation_method 'CRYSTALS_ver_14.61_build_7795 ' _chemical_name_systematic ; 5-methyl-2[(2-nitrophenyl)amino]-3-thiophenecarbonitrile ; #CheckCIF alerts _vrf_THETM01_ROY_ON_decompress_0p0GPa ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575 RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT027_ROY_ON_decompress_0p0GPa ; PROBLEM: _diffrn_reflns_theta_full value (too) Low ...... 17.44 Degree RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT029_ROY_ON_decompress_0p0GPa ; PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.718 Why? RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT201_ROY_ON_decompress_0p0GPa ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 17 Report RESPONSE: The model could only be refined isotropically in order to maintain a favourable data-to-parameter ratio, due to numerous unmeasured reflections. The relatively electron-rich sulfur atom has been modelled anisotropically. ; _vrf_PLAT911_ROY_ON_decompress_0p0GPa ; PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.555 435 Report RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT082_ROY_ON_decompress_0p0GPa ; PROBLEM: High R1 Value .................................. 0.13 Report RESPONSE: These are poor-quality diffraction data and the model has only been refined isotropically. ; _vrf_PLAT340_ROY_ON_decompress_0p0GPa ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.00745 Ang. RESPONSE: These are poor-quality diffraction data. ; _vrf_PLAT910_ROY_ON_decompress_0p0GPa ; PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 8 Note RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _refine_special_details ; In the absence of significant anomalous scattering, Friedel pairs were merged. Data were collected in a Merrill-Bassett diamond anvil cell, which significantly restricts the regions over which reciprocal space can be sampled. Thus, these data are poor quality/incomplete, reflected in numerous CheckCIF alerts regarding refinement statistics. At all pressures, the atomic connectivity is known. All non-sulfur atoms were refined isotropically; sulfur was refined anisotropically. Hydrogen atoms were constrained to ride on their host atoms. #=============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Total Missing #------------------------------------------------------------------------------- 20.82 0.500 0.723 1223 884 339 23.01 0.550 0.729 1589 1158 431 23.25 0.555 0.728 1631 1188 443 ------------------------------------------------------------ ACTA Min. Res. --- Note: The Reported Completeness refers to the Actual H,K,L Index Range ; #end of refcif _cell_length_a 3.94747(2) _cell_length_b 18.67316(6) _cell_length_c 16.33187(6) _cell_angle_alpha 90 _cell_angle_beta 93.736(7) _cell_angle_gamma 90 _cell_volume 1201.293(13) _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' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 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' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C12 H9 N3 O2 S1 # Dc = 1.43 Fooo = 536.00 Mu = 2.66 M = 259.29 # Found Formula = C12 H9 N3 O2 S1 # Dc = 1.43 FOOO = 536.00 Mu = 2.66 M = 259.29 _chemical_formula_sum 'C12 H9 N3 O2 S1' _chemical_formula_moiety 'C12 H9 N3 O2 S1' _chemical_compound_source 'TCI Chemicals' _chemical_formula_weight 259.29 _cell_measurement_reflns_used 1804 _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 23.14 _cell_measurement_temperature 293 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_min 0.050 _exptl_crystal_size_mid 0.072 _exptl_crystal_size_max 0.248 _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 0.266 # Sheldrick geometric approximatio 0.98 0.99 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North et al., 1968)' _exptl_absorpt_correction_T_min 0.13 _exptl_absorpt_correction_T_max 0.99 _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_device 'four-circle diffractometer' _diffrn_radiation_monochromator mirror _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 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction ; CrysAlisPro (Rigaku Oxford Diffraction, 2017) ; _computing_structure_solution 'Model from previously-determined structure' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 293 _diffrn_reflns_number 4298 _diffrn_reflns_av_unetI/netI 0.055 _reflns_number_total 1204 _diffrn_reflns_av_R_equivalents 0.048 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 1204 # Theoretical number of reflections is about 3450 _diffrn_reflns_theta_min 1.658 _diffrn_reflns_theta_max 23.253 _diffrn_measured_fraction_theta_max 0.692 _diffrn_reflns_theta_full 17.440 _diffrn_measured_fraction_theta_full 0.718 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _reflns_limit_h_min -4 _reflns_limit_h_max 4 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 14 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.77 _refine_diff_density_max 0.80 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # Explicitly named reflections are ALWAYS excluded from R&wR # The values actually used during refinement # These are labelled "all" for compatibility with PLATON _oxford_refine_reflns_threshold_expression I>-3.0\s(I) _refine_ls_number_restraints 94 _refine_ls_number_parameters 82 _refine_ls_number_reflns 1188 _oxford_refine_ls_R_factor_ref 0.1854 _refine_ls_R_factor_all 0.1854 _refine_ls_wR_factor_ref 0.0358 _refine_ls_wR_factor_all 0.0358 _refine_ls_goodness_of_fit_ref 0.9591 _refine_ls_shift/su_max 0.0002518 _refine_ls_shift/su_mean 0.0000792 # Computed with I/sigma = -10 _oxford_reflns_number_all 1188 _oxford_refine_ls_R_factor_all 0.1854 _oxford_refine_ls_wR_factor_all 0.0358 # Computed with no filters except I/sigma = +2 a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 728 _refine_ls_R_factor_gt 0.1251 _refine_ls_wR_factor_gt 0.0325 _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed #undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ; Method= SQRT(W) = 1/(Data with the key SIGMA(/FO/) in list 6) ; # 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 S1 S 0.8550(3) 0.59821(6) 0.42899(10) 0.0656 1.0000 Uani D U . . . . O1 O 0.5066(7) 0.61641(16) 0.0305(3) 0.0870(11) 1.0000 Uiso D U . . . . O2 O 0.5984(8) 0.68595(18) 0.1339(3) 0.0868(11) 1.0000 Uiso D U . . . . N1 N 0.9020(8) 0.64175(18) 0.2711(3) 0.0653(11) 1.0000 Uiso D U . . . . N2 N 1.4095(8) 0.80205(17) 0.2880(3) 0.0685(12) 1.0000 Uiso D U . . . . N3 N 0.6319(9) 0.6270(2) 0.0993(3) 0.0812(11) 1.0000 Uiso D U . . . . C1 C 0.9439(10) 0.5811(2) 0.2229(4) 0.0671(12) 1.0000 Uiso D U . . . . C2 C 1.1253(10) 0.5222(2) 0.2633(4) 0.0675(12) 1.0000 Uiso D U . . . . C3 C 1.1659(9) 0.4618(2) 0.2179(4) 0.0676(12) 1.0000 Uiso D U . . . . C4 C 1.0367(9) 0.4564(3) 0.1391(4) 0.0701(12) 1.0000 Uiso D U . . . . C5 C 0.8605(9) 0.5102(2) 0.0995(3) 0.0692(12) 1.0000 Uiso D U . . . . C6 C 0.8164(9) 0.5728(3) 0.1448(4) 0.0703(11) 1.0000 Uiso D U . . . . C7 C 0.9744(10) 0.6541(2) 0.3524(4) 0.0616(10) 1.0000 Uiso D U . . . . C8 C 1.1334(10) 0.7136(2) 0.3844(4) 0.0625(11) 1.0000 Uiso D U . . . . C9 C 1.1583(9) 0.7134(2) 0.4687(4) 0.0666(12) 1.0000 Uiso D U . . . . C10 C 1.0187(7) 0.65517(18) 0.5029(4) 0.0692(10) 1.0000 Uiso D U . . . . C11 C 0.9858(7) 0.63794(18) 0.5920(4) 0.0766(13) 1.0000 Uiso D U . . . . C12 C 1.2782(10) 0.7656(3) 0.3340(4) 0.0629(11) 1.0000 Uiso D U . . . . H1 H 0.782(4) 0.6744(11) 0.2469(13) 0.067(3) 1.0000 Uiso D . . . . . H2 H 1.2104 0.5258 0.3172 0.0790 1.0000 Uiso R . . . . . H3 H 1.2913 0.4238 0.2421 0.0779 1.0000 Uiso R . . . . . H4 H 1.0651 0.4137 0.1115 0.0868 1.0000 Uiso R . . . . . H5 H 0.7716 0.5060 0.0465 0.0750 1.0000 Uiso R . . . . . H9 H 1.2601 0.7510 0.4992 0.0860 1.0000 Uiso R . . . . . H111 H 1.1646 0.6056 0.6109 0.1259 1.0000 Uiso DR . . . . . H112 H 1.0019 0.6811 0.6237 0.1261 1.0000 Uiso DR . . . . . H113 H 0.7706 0.6156 0.5987 0.1261 1.0000 Uiso DR . . . . . 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 S1 0.0751(7) 0.0622(10) 0.0591(15) 0.0052(7) 0.0015(7) -0.0017(6) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.4233(10) 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 S1 . C7 . 1.719(6) yes S1 . C10 . 1.704(5) yes O1 . N3 . 1.215(6) yes O2 . N3 . 1.247(4) yes N1 . C1 . 1.395(6) yes N1 . C7 . 1.359(6) yes N1 . H1 . 0.85(2) no N2 . C12 . 1.160(6) yes N3 . C6 . 1.428(6) yes C1 . C2 . 1.447(7) yes C1 . C6 . 1.349(7) yes C2 . C3 . 1.364(6) yes C2 . H2 . 0.924 no C3 . C4 . 1.356(8) yes C3 . H3 . 0.938 no C4 . C5 . 1.361(5) yes C4 . H4 . 0.928 no C5 . C6 . 1.399(5) yes C5 . H5 . 0.917 no C7 . C8 . 1.363(6) yes C8 . C9 . 1.375(7) yes C8 . C12 . 1.418(6) yes C9 . C10 . 1.356(5) yes C9 . H9 . 0.936 no C10 . C11 . 1.504(7) yes C11 . H111 . 0.965 no C11 . H112 . 0.959 no C11 . H113 . 0.959 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 C7 . S1 . C10 . 91.6(3) yes C1 . N1 . C7 . 131.6(4) yes C1 . N1 . H1 . 113.7(16) no C7 . N1 . H1 . 113.9(16) no O2 . N3 . O1 . 120.9(4) yes O2 . N3 . C6 . 117.1(5) yes O1 . N3 . C6 . 121.9(5) yes N1 . C1 . C2 . 115.7(6) yes N1 . C1 . C6 . 125.2(5) yes C2 . C1 . C6 . 119.1(5) yes C1 . C2 . C3 . 116.9(6) yes C1 . C2 . H2 . 121.0 no C3 . C2 . H2 . 122.0 no C2 . C3 . C4 . 121.8(5) yes C2 . C3 . H3 . 118.3 no C4 . C3 . H3 . 120.0 no C3 . C4 . C5 . 123.0(5) yes C3 . C4 . H4 . 118.4 no C5 . C4 . H4 . 118.6 no C4 . C5 . C6 . 116.2(6) yes C4 . C5 . H5 . 122.5 no C6 . C5 . H5 . 121.3 no N3 . C6 . C5 . 113.2(6) yes N3 . C6 . C1 . 123.8(5) yes C5 . C6 . C1 . 123.0(5) yes S1 . C7 . N1 . 123.9(3) yes S1 . C7 . C8 . 110.9(5) yes N1 . C7 . C8 . 125.1(4) yes C7 . C8 . C9 . 112.6(4) yes C7 . C8 . C12 . 121.9(6) yes C9 . C8 . C12 . 125.3(5) yes C8 . C9 . C10 . 114.2(5) yes C8 . C9 . H9 . 122.1 no C10 . C9 . H9 . 123.7 no S1 . C10 . C9 . 110.8(5) yes S1 . C10 . C11 . 119.9(2) yes C9 . C10 . C11 . 129.3(4) yes C10 . C11 . H111 . 109.7 no C10 . C11 . H112 . 109.7 no H111 . C11 . H112 . 109.4 no C10 . C11 . H113 . 109.7 no H111 . C11 . H113 . 109.0 no H112 . C11 . H113 . 109.4 no C8 . C12 . N2 . 172.6(6) yes _iucr_refine_instructions_details ; # # Punched on 26/01/21 at 12:47:54 # #LIST 12 BLOCK CONT SCALE CONT S ( 1 ,X'S,U'S) CONT O ( 1 ,X'S,U[ISO]) UNTIL H ( 1 ) RIDE C ( 2,X'S) H ( 2,X'S) RIDE C ( 3,X'S) H ( 3,X'S) RIDE C ( 4,X'S) H ( 4,X'S) RIDE C ( 5,X'S) H ( 5,X'S) RIDE C ( 9,X'S) H ( 9,X'S) RIDE C ( 11,X'S) H ( 111,X'S) H ( 112,X'S) H ( 113,X'S) END # # Punched on 26/01/21 at 12:47:54 # #LIST 16 NO REM REM NPF NOTE - FIRST UNTIL LAST REM REM HREST START (DO NOT REMOVE THIS LINE) REM NO H NO #H U MULT DIST REM C-H REM >4 1.5 .96 DISORDER REM 1 1 1.2 .93 C C-H (ACETYLENE) REM 1 2 1.2 .93 C-C(H)-C REM 1 3 1.2 .98 (C)3-C-H REM 2 1 1.2 .93 C=C-H(2) REM 2 2 1.2 .97 (C)2-C-(H)2 REM 3 1 1.5 .96 C-C-(H)3 REM N-H REM >4 1.5 .89 DISORDER REM 1 1 1.2 .86 N-N/H REM 1 2 1.2 .86 (C)2-N-H REM 1 3 1.2 .89 (C)3-N-H REM 2 1 1.2 .86 C-N-(H)2 REM 2 2 1.2 .89 (C)2-N-(H)2 REM 3 1 1.2 .89 C-H-(H)3 REM O-H REM 1 1 1.5 .82 O-H REM REM DIST ESD = 0.02 REM VIB ESD = 0.002 REM ANGLE ESD = 2.0 REM REM TO ACTIVATE THE VIB RESTRAINTS, REMOVE LEADING REM REM H1-N-R2 DIST 0.86, 0.02 = CONT N ( 1) TO H(1) REST 0.068, 0.002 = H(1,U[ISO]) ANGLE 0.0, 2.0 = MEAN CONT H(1) TO N ( 1) TO C(1) CONT H(1) TO N ( 1) TO C(7) REM HREST END (DO NOT REMOVE THIS LINE) REM DELU START (DO NOT REMOVE THIS LINE) VIBR .0, 0.00200 = S(1) TO C(10) VIBR .0, 0.00200 = S(1) TO C(7) VIBR .0, 0.00500 = C(7) TO C(10) VIBR .0, 0.00200 = N(2) TO C(12) VIBR .0, 0.00200 = C(10) TO C(9) VIBR .0, 0.00200 = C(10) TO C(11) VIBR .0, 0.00500 = C(9) TO S(1) VIBR .0, 0.00500 = C(11) TO S(1) VIBR .0, 0.00500 = C(11) TO C(9) VIBR .0, 0.00200 = C(12) TO C(8) VIBR .0, 0.00500 = C(8) TO N(2) VIBR .0, 0.00200 = O(1) TO N(3) VIBR .0, 0.00200 = C(2) TO C(1) VIBR .0, 0.00200 = C(2) TO C(3) VIBR .0, 0.00500 = C(3) TO C(1) VIBR .0, 0.00200 = N(1) TO C(7) VIBR .0, 0.00200 = N(1) TO C(1) VIBR .0, 0.00500 = C(1) TO C(7) VIBR .0, 0.00200 = C(7) TO C(8) VIBR .0, 0.00500 = N(1) TO S(1) VIBR .0, 0.00500 = C(8) TO S(1) VIBR .0, 0.00500 = C(8) TO N(1) VIBR .0, 0.00200 = O(2) TO N(3) VIBR .0, 0.00200 = N(3) TO C(6) VIBR .0, 0.00500 = O(1) TO O(2) VIBR .0, 0.00500 = C(6) TO O(2) VIBR .0, 0.00500 = C(6) TO O(1) VIBR .0, 0.00200 = C(5) TO C(4) VIBR .0, 0.00200 = C(5) TO C(6) VIBR .0, 0.00500 = C(6) TO C(4) VIBR .0, 0.00200 = C(4) TO C(3) VIBR .0, 0.00500 = C(3) TO C(5) VIBR .0, 0.00200 = C(1) TO C(6) VIBR .0, 0.00500 = N(1) TO C(2) VIBR .0, 0.00500 = C(6) TO C(2) VIBR .0, 0.00500 = C(6) TO N(1) VIBR .0, 0.00500 = C(5) TO N(3) VIBR .0, 0.00500 = C(1) TO N(3) VIBR .0, 0.00500 = C(1) TO C(5) VIBR .0, 0.00200 = C(9) TO C(8) VIBR .0, 0.00500 = C(8) TO C(10) VIBR .0, 0.00500 = C(2) TO C(4) VIBR .0, 0.00500 = C(12) TO C(9) VIBR .0, 0.00500 = C(7) TO C(9) VIBR .0, 0.00500 = C(7) TO C(12) REM DELU END (DO NOT REMOVE THIS LINE) ANGLE 110.000000 , 0.020000 = C(10) TO C(11) TO H(111) ANGLE 110.000000 , 0.020000 = C(10) TO C(11) TO H(112) ANGLE 110.000000 , 0.020000 = C(10) TO C(11) TO H(113) DISTANCE 1.225000 , 0.050000 = O(2) TO N(3) DISTANCE 1.225000 , 0.050000 = O(1) TO N(3) DISTANCE 1.440000 , 0.050000 = C(6) TO N(3) DISTANCE 1.390000 , 0.050000 = C(5) TO C(6) DISTANCE 1.364000 , 0.050000 = C(4) TO C(5) DISTANCE 1.222000 , 0.050000 = O(1) TO N(3) DISTANCE 1.232000 , 0.050000 = O(2) TO N(3) DISTANCE 1.440000 , 0.050000 = C(6) TO N(3) DISTANCE 1.392000 , 0.050000 = C(5) TO C(6) DISTANCE 1.364000 , 0.050000 = C(4) TO C(5) DISTANCE 1.391000 , 0.050000 = C(3) TO C(4) DISTANCE 1.371000 , 0.050000 = C(2) TO C(3) DISTANCE 1.400000 , 0.050000 = C(1) TO C(2) DISTANCE 1.408000 , 0.050000 = C(1) TO C(6) DISTANCE 1.382000 , 0.050000 = C(1) TO N(1) DISTANCE 1.387000 , 0.050000 = C(7) TO N(1) DISTANCE 1.728000 , 0.050000 = S(1) TO C(7) DISTANCE 1.724000 , 0.050000 = S(1) TO C(10) DISTANCE 1.500000 , 0.050000 = C(10) TO C(11) DISTANCE 1.349000 , 0.050000 = C(9) TO C(10) DISTANCE 1.427000 , 0.050000 = C(8) TO C(9) DISTANCE 1.372000 , 0.050000 = C(7) TO C(8) DISTANCE 1.422000 , 0.050000 = C(8) TO C(12) DISTANCE 1.141000 , 0.050000 = C(12) TO N(2) REM THERMSIM START (DO NOT REMOVE THIS LINE) U(IJ) .0, 0.04000 = S(1) TO C(7) U(IJ) .0, 0.04000 = S(1) TO C(10) U(IJ) .0, 0.08000 = O(1) TO N(3) U(IJ) .0, 0.08000 = O(2) TO N(3) U(IJ) .0, 0.04000 = C(1) TO C(2) U(IJ) .0, 0.04000 = C(1) TO C(6) U(IJ) .0, 0.04000 = C(1) TO N(1) U(IJ) .0, 0.04000 = C(2) TO C(3) U(IJ) .0, 0.04000 = C(3) TO C(4) U(IJ) .0, 0.04000 = C(4) TO C(5) U(IJ) .0, 0.04000 = C(5) TO C(6) U(IJ) .0, 0.04000 = C(6) TO N(3) U(IJ) .0, 0.04000 = C(7) TO C(8) U(IJ) .0, 0.04000 = C(7) TO N(1) U(IJ) .0, 0.04000 = C(8) TO C(9) U(IJ) .0, 0.04000 = C(8) TO C(12) U(IJ) .0, 0.04000 = C(9) TO C(10) U(IJ) .0, 0.08000 = C(10) TO C(11) U(IJ) .0, 0.08000 = C(12) TO N(2) REM THERMSIM END (DO NOT REMOVE THIS LINE) PLANAR 0.010000 C(1) C(6) N(1) H(1) PLANAR 0.010000 C(1) C(2) C(3) C(4) C(5) C(6) N(1) N(3) PLANAR 0.010000 S(1) C(7) C(8) C(9) C(10) N(1) 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 1 2 6 x . 1 7 11 x . -1 0 4 x . -2 12 1 x . 3 10 0 x . -1 15 3 x . -2 13 2 x . 1 3 7 x . 0 8 12 x . 0 7 11 x . 0 5 9 x . # looking for ARCHIVE-HKL.CIF _iucr_refine_reflections_details ; # Data was input as F-squared # punching LIST 6 as LIST 6 with all keys set # NBGNXT= 36 #LIST 6 READ NCOEF= 8 TYPE=FIX, F'S = FSQ UNIT=DATA, CHECK=NO L30=NO ARCH=NO STORE NCOEF= 6 OUTPUT INDICES /FO/ SIGMA(/FO/) RATIO/JCODE CORRECTIONS SERIAL CONT INPUT H K L /FO/ SIGMA(/FO/) JCODE CONT CORRECTIONS SERIAL FOR (I4,I4,I4,F10.2,F8.2,F4.0,F7.4,F7.0) END 0 1 1 21.87 0.78 0. 1.0000 0. 0 1 1 20.85 0.78 0. 1.0000 0. 0 1 1 18.11 0.81 0. 1.0000 0. 0 -1 -1 19.20 0.76 0. 1.0000 0. 0 -1 -2 156.63 5.45 0. 1.0000 0. 0 1 2 134.05 5.55 0. 1.0000 0. 0 2 1 1572.99 58.31 0. 1.0000 0. 0 2 1 1624.44 58.22 0. 1.0000 0. 0 2 1 1640.19 58.13 0. 1.0000 0. 0 2 1 1616.35 58.12 0. 1.0000 0. 0 2 2 131.17 5.26 0. 1.0000 0. 0 2 2 141.73 5.36 0. 1.0000 0. 0 2 2 142.89 5.26 0. 1.0000 0. 0 2 2 149.47 5.27 0. 1.0000 0. 0 -2 -2 147.65 5.25 0. 1.0000 0. 0 -2 -2 142.40 5.24 0. 1.0000 0. 0 2 2 154.53 5.28 0. 1.0000 0. 0 2 2 147.60 5.31 0. 1.0000 0. 0 2 3 901.38 29.64 0. 1.0000 0. 0 2 3 728.99 29.83 0. 1.0000 0. 0 2 3 841.60 29.63 0. 1.0000 0. 0 2 3 750.32 29.72 0. 1.0000 0. 0 3 1 584.65 21.52 0. 1.0000 0. 0 3 2 95.32 3.47 0. 1.0000 0. 0 3 2 92.90 3.49 0. 1.0000 0. 0 -3 -2 104.96 3.50 0. 1.0000 0. 0 3 2 95.45 3.49 0. 1.0000 0. 0 3 2 97.56 3.50 0. 1.0000 0. 0 3 2 91.62 3.49 0. 1.0000 0. 0 -3 -2 92.52 3.47 0. 1.0000 0. 0 3 2 94.08 3.54 0. 1.0000 0. 0 3 2 91.09 3.51 0. 1.0000 0. 0 -3 -3 4.13 0.31 0. 1.0000 0. 0 3 3 4.75 0.36 0. 1.0000 0. 0 3 3 3.53 0.31 0. 1.0000 0. 0 3 3 4.05 0.49 0. 1.0000 0. 0 3 3 4.04 0.37 0. 1.0000 0. 0 -3 -3 3.75 0.40 0. 1.0000 0. 0 3 3 5.42 0.42 0. 1.0000 0. 0 3 3 4.17 0.33 0. 1.0000 0. 0 -3 -3 3.51 0.54 0. 1.0000 0. 0 -3 -3 3.83 0.30 0. 1.0000 0. 0 -3 -3 3.90 0.32 0. 1.0000 0. 0 3 3 5.02 0.63 0. 1.0000 0. 0 3 4 67.44 2.61 0. 1.0000 0. 0 -3 -4 63.78 2.48 0. 1.0000 0. 0 -3 -4 63.44 2.52 0. 1.0000 0. 0 3 4 59.99 2.54 0. 1.0000 0. 0 3 5 51.61 2.28 0. 1.0000 0. 0 3 5 51.24 2.50 0. 1.0000 0. 0 4 1 2.92 0.31 0. 1.0000 0. 0 -4 -2 679.31 22.87 0. 1.0000 0. 0 4 2 603.51 22.73 0. 1.0000 0. 0 -4 -2 637.94 22.70 0. 1.0000 0. 0 4 2 647.42 23.00 0. 1.0000 0. 0 -4 -2 627.73 22.74 0. 1.0000 0. 0 -4 -2 624.49 22.72 0. 1.0000 0. 0 4 3 28.39 1.15 0. 1.0000 0. 0 4 3 28.39 1.19 0. 1.0000 0. 0 -4 -3 27.40 1.13 0. 1.0000 0. 0 -4 -3 27.46 1.21 0. 1.0000 0. 0 4 3 28.68 1.18 0. 1.0000 0. 0 4 3 27.21 1.16 0. 1.0000 0. 0 4 3 29.33 1.16 0. 1.0000 0. 0 4 3 29.64 1.22 0. 1.0000 0. 0 4 4 0.65 0.42 0. 1.0000 0. 0 -4 -4 0.65 0.30 0. 1.0000 0. 0 4 4 0.27 0.39 0. 1.0000 0. 0 4 4 1.04 0.37 0. 1.0000 0. 0 -4 -4 0.50 0.30 0. 1.0000 0. 0 -4 -4 0.33 0.31 0. 1.0000 0. 0 -4 -5 410.24 15.59 0. 1.0000 0. 0 -4 -5 453.04 15.62 0. 1.0000 0. 0 4 5 415.55 15.71 0. 1.0000 0. 0 4 5 442.59 15.68 0. 1.0000 0. 0 -4 -6 230.93 2.47 0. 1.0000 0. 0 4 6 249.25 3.07 0. 1.0000 0. 0 4 6 222.20 2.93 0. 1.0000 0. 0 -4 -6 0.67 1.01 0. 1.0000 0. 0 4 6 1.49 1.10 0. 1.0000 0. 0 4 7 42.80 2.61 0. 1.0000 0. 0 -5 -2 502.44 18.69 0. 1.0000 0. 0 -5 -2 574.60 18.72 0. 1.0000 0. 0 5 2 514.86 18.72 0. 1.0000 0. 0 5 2 441.69 19.41 0. 1.0000 0. 0 5 2 505.64 18.66 0. 1.0000 0. 0 5 3 201.89 7.59 0. 1.0000 0. 0 5 3 192.06 7.78 0. 1.0000 0. 0 -5 -3 213.66 7.58 0. 1.0000 0. 0 5 3 211.53 7.56 0. 1.0000 0. 0 -5 -3 203.82 7.57 0. 1.0000 0. 0 5 3 210.44 7.63 0. 1.0000 0. 0 -5 -3 218.02 7.67 0. 1.0000 0. 0 5 3 207.90 7.59 0. 1.0000 0. 0 5 4 125.97 4.85 0. 1.0000 0. 0 5 4 134.34 4.92 0. 1.0000 0. 0 5 4 137.58 4.91 0. 1.0000 0. 0 -5 -4 126.28 4.88 0. 1.0000 0. 0 5 4 124.58 4.87 0. 1.0000 0. 0 5 4 132.95 4.82 0. 1.0000 0. 0 5 5 238.37 8.87 0. 1.0000 0. 0 5 5 242.93 8.75 0. 1.0000 0. 0 -5 -5 236.45 8.62 0. 1.0000 0. 0 -5 -5 240.03 8.78 0. 1.0000 0. 0 -5 -5 239.63 8.70 0. 1.0000 0. 0 5 5 240.50 8.81 0. 1.0000 0. 0 -5 -6 3.27 0.58 0. 1.0000 0. 0 -5 -6 2.96 0.60 0. 1.0000 0. 0 5 6 2.92 0.75 0. 1.0000 0. 0 5 6 3.30 0.96 0. 1.0000 0. 0 -5 -7 375.33 3.79 0. 1.0000 0. 0 5 7 337.68 4.44 0. 1.0000 0. 0 5 7 356.60 4.04 0. 1.0000 0. 0 -5 -8 -0.52 0.81 0. 1.0000 0. 0 5 8 0.86 1.31 0. 1.0000 0. 0 5 9 -0.43 1.74 0. 1.0000 0. 0 6 1 284.18 10.45 0. 1.0000 0. 0 -6 -2 97.35 3.60 0. 1.0000 0. 0 6 2 94.99 3.61 0. 1.0000 0. 0 6 2 92.29 3.53 0. 1.0000 0. 0 -6 -3 36.91 1.63 0. 1.0000 0. 0 6 3 35.84 1.55 0. 1.0000 0. 0 6 3 38.38 1.41 0. 1.0000 0. 0 6 3 39.58 1.49 0. 1.0000 0. 0 6 3 35.21 1.51 0. 1.0000 0. 0 6 4 5.71 0.58 0. 1.0000 0. 0 6 4 5.26 0.52 0. 1.0000 0. 0 6 4 5.77 0.47 0. 1.0000 0. 0 6 4 5.17 0.62 0. 1.0000 0. 0 6 4 6.90 0.80 0. 1.0000 0. 0 -6 -5 132.51 5.08 0. 1.0000 0. 0 6 5 161.52 5.42 0. 1.0000 0. 0 6 5 125.74 5.05 0. 1.0000 0. 0 6 5 128.43 4.95 0. 1.0000 0. 0 6 5 130.70 5.05 0. 1.0000 0. 0 -6 -6 13.14 0.77 0. 1.0000 0. 0 -6 -6 11.02 0.91 0. 1.0000 0. 0 6 6 13.51 0.89 0. 1.0000 0. 0 6 6 12.96 1.14 0. 1.0000 0. 0 -6 -6 12.61 0.61 0. 1.0000 0. 0 6 6 12.63 0.97 0. 1.0000 0. 0 6 7 48.47 2.61 0. 1.0000 0. 0 6 7 56.27 2.48 0. 1.0000 0. 0 -6 -7 56.88 2.19 0. 1.0000 0. 0 6 7 54.67 2.72 0. 1.0000 0. 0 6 7 63.91 2.47 0. 1.0000 0. 0 -6 -7 58.17 2.41 0. 1.0000 0. 0 6 8 346.96 11.73 0. 1.0000 0. 0 -6 -8 319.90 11.61 0. 1.0000 0. 0 6 8 313.51 11.96 0. 1.0000 0. 0 -6 -9 39.30 2.10 0. 1.0000 0. 0 6 9 46.38 2.39 0. 1.0000 0. 0 6 10 0.75 1.51 0. 1.0000 0. 0 7 1 12.49 0.84 0. 1.0000 0. 0 -7 -2 25.45 1.24 0. 1.0000 0. 0 7 2 26.09 1.25 0. 1.0000 0. 0 7 2 26.08 1.15 0. 1.0000 0. 0 7 3 609.26 22.63 0. 1.0000 0. 0 -7 -3 653.28 22.62 0. 1.0000 0. 0 7 3 641.75 22.62 0. 1.0000 0. 0 7 4 213.76 9.37 0. 1.0000 0. 0 7 4 242.87 8.89 0. 1.0000 0. 0 7 4 246.10 8.96 0. 1.0000 0. 0 7 4 242.59 8.85 0. 1.0000 0. 0 -7 -4 251.44 9.01 0. 1.0000 0. 0 7 5 453.17 16.04 0. 1.0000 0. 0 7 5 438.99 16.04 0. 1.0000 0. 0 7 5 435.05 16.23 0. 1.0000 0. 0 7 5 430.05 16.05 0. 1.0000 0. 0 -7 -6 61.63 2.82 0. 1.0000 0. 0 7 6 69.24 2.90 0. 1.0000 0. 0 7 6 65.44 2.85 0. 1.0000 0. 0 7 6 69.88 2.72 0. 1.0000 0. 0 -7 -7 26.49 1.52 0. 1.0000 0. 0 7 7 28.61 1.83 0. 1.0000 0. 0 7 7 26.86 1.39 0. 1.0000 0. 0 -7 -7 25.11 2.61 0. 1.0000 0. 0 7 7 26.18 1.49 0. 1.0000 0. 0 -7 -7 25.88 1.07 0. 1.0000 0. 0 7 8 0.93 1.55 0. 1.0000 0. 0 7 8 2.10 0.91 0. 1.0000 0. 0 7 8 1.81 1.02 0. 1.0000 0. 0 -7 -8 2.31 0.93 0. 1.0000 0. 0 -7 -8 3.74 3.40 0. 1.0000 0. 0 -7 -8 2.40 0.52 0. 1.0000 0. 0 7 9 25.92 1.66 0. 1.0000 0. 0 7 9 24.91 1.63 0. 1.0000 0. 0 -7 -9 7.89 5.15 0. 1.0000 0. 0 -7 -9 23.18 1.18 0. 1.0000 0. 0 7 9 23.09 2.35 0. 1.0000 0. 0 -7 -9 24.06 1.51 0. 1.0000 0. 0 -7 -10 223.42 8.65 0. 1.0000 0. 0 7 10 227.29 8.71 0. 1.0000 0. 0 7 10 236.68 8.81 0. 1.0000 0. 0 7 11 -1.23 1.51 0. 1.0000 0. 0 8 1 4.93 0.71 0. 1.0000 0. 0 8 2 274.21 9.99 0. 1.0000 0. 0 8 2 267.38 9.88 0. 1.0000 0. 0 8 3 638.87 23.42 0. 1.0000 0. 0 -8 -3 662.90 23.50 0. 1.0000 0. 0 8 4 18.40 0.77 0. 1.0000 0. 0 8 4 11.29 1.99 0. 1.0000 0. 0 8 4 18.86 0.94 0. 1.0000 0. 0 -8 -4 18.64 1.27 0. 1.0000 0. 0 8 4 18.81 1.08 0. 1.0000 0. 0 8 4 18.70 0.99 0. 1.0000 0. 0 8 5 127.00 5.65 0. 1.0000 0. 0 8 5 132.72 5.00 0. 1.0000 0. 0 8 5 127.89 4.90 0. 1.0000 0. 0 8 6 118.35 5.40 0. 1.0000 0. 0 8 6 112.67 4.60 0. 1.0000 0. 0 8 6 111.04 4.81 0. 1.0000 0. 0 8 6 109.61 4.57 0. 1.0000 0. 0 8 7 12.57 1.43 0. 1.0000 0. 0 8 7 10.65 1.37 0. 1.0000 0. 0 8 7 11.07 1.75 0. 1.0000 0. 0 8 7 12.32 1.07 0. 1.0000 0. 0 -8 -7 11.74 1.94 0. 1.0000 0. 0 8 8 40.85 2.19 0. 1.0000 0. 0 8 8 40.50 2.42 0. 1.0000 0. 0 8 8 44.06 2.65 0. 1.0000 0. 0 8 8 39.70 1.93 0. 1.0000 0. 0 -8 -8 38.15 2.11 0. 1.0000 0. 0 -8 -8 30.91 3.39 0. 1.0000 0. 0 -8 -9 17.84 1.47 0. 1.0000 0. 0 -8 -9 5.76 5.11 0. 1.0000 0. 0 8 9 19.60 1.41 0. 1.0000 0. 0 -8 -9 17.36 0.88 0. 1.0000 0. 0 8 9 18.67 1.59 0. 1.0000 0. 0 8 9 15.00 2.16 0. 1.0000 0. 0 -8 -10 5.98 5.90 0. 1.0000 0. 0 8 10 18.45 1.53 0. 1.0000 0. 0 8 10 15.71 2.58 0. 1.0000 0. 0 -8 -10 16.71 0.98 0. 1.0000 0. 0 8 10 14.96 1.72 0. 1.0000 0. 0 -8 -10 17.91 1.55 0. 1.0000 0. 0 -8 -11 0.04 1.24 0. 1.0000 0. 0 8 11 1.50 1.61 0. 1.0000 0. 0 -8 -11 1.71 0.80 0. 1.0000 0. 0 8 11 1.36 1.32 0. 1.0000 0. 0 8 12 0.16 1.41 0. 1.0000 0. 0 -8 -12 -0.79 1.13 0. 1.0000 0. 0 8 12 0.05 1.46 0. 1.0000 0. 0 9 1 15.44 1.15 0. 1.0000 0. 0 9 2 0.27 0.69 0. 1.0000 0. 0 9 2 0.21 0.54 0. 1.0000 0. 0 -9 -2 0.04 0.30 0. 1.0000 0. 0 -9 -3 24.92 1.43 0. 1.0000 0. 0 9 3 25.65 1.35 0. 1.0000 0. 0 9 3 23.60 1.19 0. 1.0000 0. 0 -9 -4 772.38 27.70 0. 1.0000 0. 0 9 4 760.04 27.43 0. 1.0000 0. 0 9 4 776.97 27.54 0. 1.0000 0. 0 9 4 751.49 27.66 0. 1.0000 0. 0 -9 -5 64.15 2.88 0. 1.0000 0. 0 9 5 65.33 2.70 0. 1.0000 0. 0 9 5 56.17 3.97 0. 1.0000 0. 0 -9 -5 62.51 3.25 0. 1.0000 0. 0 9 5 62.65 2.55 0. 1.0000 0. 0 9 6 10.60 2.81 0. 1.0000 0. 0 9 6 15.79 1.46 0. 1.0000 0. 0 9 6 13.99 1.23 0. 1.0000 0. 0 9 6 16.55 2.17 0. 1.0000 0. 0 -9 -7 42.31 2.68 0. 1.0000 0. 0 9 7 45.43 2.25 0. 1.0000 0. 0 9 7 37.98 2.12 0. 1.0000 0. 0 9 7 44.40 3.33 0. 1.0000 0. 0 9 7 43.48 2.68 0. 1.0000 0. 0 -9 -8 45.52 3.57 0. 1.0000 0. 0 9 8 45.21 2.55 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1.0000 0. 4 -1 -5 0.95 2.54 0. 1.0000 0. 4 1 -5 4.77 2.59 0. 1.0000 0. -4 -1 5 -0.62 2.28 0. 1.0000 0. 4 -1 -4 5.33 2.69 0. 1.0000 0. 4 1 -4 11.71 2.78 0. 1.0000 0. 4 -1 -3 10.47 2.75 0. 1.0000 0. 4 1 -3 11.94 2.84 0. 1.0000 0. 4 -1 -2 -4.56 3.15 0. 1.0000 0. 4 1 -2 -1.06 2.75 0. 1.0000 0. 4 -1 -1 -1.54 3.46 0. 1.0000 0. 4 1 -1 1.78 2.96 0. 1.0000 0. 4 -1 0 -1.02 3.89 0. 1.0000 0. 4 1 0 -0.17 3.23 0. 1.0000 0. 4 -1 1 3.69 3.96 0. 1.0000 0. 4 1 1 -3.77 3.56 0. 1.0000 0. -4 1 -1 -3.59 2.78 0. 1.0000 0. 4 -1 2 6.27 4.85 0. 1.0000 0. 4 1 2 8.47 4.20 0. 1.0000 0. -4 1 -2 6.20 2.98 0. 1.0000 0. 4 -1 3 8.02 6.16 0. 1.0000 0. 4 1 3 9.98 4.59 0. 1.0000 0. -4 1 -3 4.34 2.89 0. 1.0000 0. -4 -1 -3 4.89 2.85 0. 1.0000 0. 4 -1 4 0.46 7.83 0. 1.0000 0. 4 1 4 -1.00 5.86 0. 1.0000 0. -4 1 -4 -0.80 3.02 0. 1.0000 0. -4 -1 -4 1.48 2.90 0. 1.0000 0. 4 1 5 0.40 6.98 0. 1.0000 0. -4 1 -5 0.25 2.96 0. 1.0000 0. -4 1 -5 0.12 3.32 0. 1.0000 0. 4 1 6 5.29 8.66 0. 1.0000 0. 4 -2 -8 6.19 2.37 0. 1.0000 0. -4 2 8 2.72 2.64 0. 1.0000 0. 4 -2 -7 3.11 2.46 0. 1.0000 0. -4 2 7 4.76 2.95 0. 1.0000 0. 4 -2 -6 2.34 2.51 0. 1.0000 0. 4 2 -6 -1.81 2.51 0. 1.0000 0. -4 -2 6 0.62 2.06 0. 1.0000 0. -4 -2 5 7.09 2.39 0. 1.0000 0. 4 -2 -5 6.00 2.62 0. 1.0000 0. 4 2 -5 11.01 2.78 0. 1.0000 0. 4 -2 -4 -0.74 2.53 0. 1.0000 0. 4 2 -4 0.15 2.82 0. 1.0000 0. 4 -2 -3 2.37 2.86 0. 1.0000 0. 4 2 -3 5.34 2.85 0. 1.0000 0. -4 2 3 2.74 2.32 0. 1.0000 0. 4 -2 -2 2.86 3.21 0. 1.0000 0. 4 2 -2 1.09 2.88 0. 1.0000 0. 4 -2 -1 -1.07 3.69 0. 1.0000 0. 4 2 -1 -0.32 2.82 0. 1.0000 0. 4 -2 0 0.10 3.77 0. 1.0000 0. 4 2 0 2.18 2.98 0. 1.0000 0. 4 -2 1 -0.65 4.73 0. 1.0000 0. 4 2 1 4.67 3.44 0. 1.0000 0. -4 2 -1 4.53 2.74 0. 1.0000 0. 4 2 1 -3.04 2.53 0. 1.0000 0. 4 -2 2 -1.40 5.81 0. 1.0000 0. 4 2 2 3.54 3.93 0. 1.0000 0. -4 2 -2 0.59 2.73 0. 1.0000 0. 4 -2 3 16.98 7.52 0. 1.0000 0. 4 2 3 17.28 4.46 0. 1.0000 0. -4 2 -3 18.38 3.30 0. 1.0000 0. 4 2 4 0.41 4.99 0. 1.0000 0. -4 2 -4 1.03 1.70 0. 1.0000 0. -4 2 -4 2.82 3.03 0. 1.0000 0. -4 2 -4 1.84 3.20 0. 1.0000 0. 4 2 5 7.34 6.20 0. 1.0000 0. -4 2 -5 0.51 2.67 0. 1.0000 0. -4 2 -5 -0.47 2.76 0. 1.0000 0. 4 2 6 8.73 8.72 0. 1.0000 0. -4 -2 -6 7.40 3.35 0. 1.0000 0. 4 -3 -8 2.07 2.40 0. 1.0000 0. -4 3 7 2.05 3.75 0. 1.0000 0. 4 -3 -7 0.86 2.45 0. 1.0000 0. 4 3 -6 -0.75 2.36 0. 1.0000 0. -4 -3 6 -0.54 1.87 0. 1.0000 0. 4 -3 -5 -1.22 2.52 0. 1.0000 0. 4 3 -5 1.73 2.60 0. 1.0000 0. -4 -3 5 2.00 2.06 0. 1.0000 0. 4 -3 -4 5.74 3.10 0. 1.0000 0. 4 3 -4 4.28 2.92 0. 1.0000 0. -4 3 4 0.16 2.25 0. 1.0000 0. -4 -3 4 0.66 2.15 0. 1.0000 0. 4 -3 -3 3.94 3.24 0. 1.0000 0. 4 3 -3 1.24 2.86 0. 1.0000 0. -4 3 3 -1.30 2.58 0. 1.0000 0. 4 -3 -2 -0.19 3.56 0. 1.0000 0. 4 3 -2 2.23 2.83 0. 1.0000 0. 4 -3 -1 0.87 4.08 0. 1.0000 0. 4 3 -1 -2.61 3.04 0. 1.0000 0. 4 -3 0 10.44 4.63 0. 1.0000 0. 4 3 0 1.33 3.05 0. 1.0000 0. -4 3 0 3.08 2.74 0. 1.0000 0. 4 -3 1 -4.21 6.08 0. 1.0000 0. 4 3 1 0.42 2.82 0. 1.0000 0. -4 3 -1 -0.50 2.68 0. 1.0000 0. 4 3 1 -0.52 3.05 0. 1.0000 0. 4 -3 2 0.79 9.35 0. 1.0000 0. 4 3 2 7.45 3.94 0. 1.0000 0. -4 3 -2 8.68 2.93 0. 1.0000 0. 4 3 2 -1.14 2.61 0. 1.0000 0. 4 3 3 -1.12 4.03 0. 1.0000 0. -4 3 -3 2.29 1.78 0. 1.0000 0. -4 3 -3 -0.39 2.89 0. 1.0000 0. 4 3 4 0.87 4.44 0. 1.0000 0. -4 3 -4 0.32 1.62 0. 1.0000 0. -4 3 -4 -2.87 2.75 0. 1.0000 0. -4 3 -4 -1.37 2.92 0. 1.0000 0. 4 3 5 3.29 5.53 0. 1.0000 0. -4 -3 -5 1.28 3.01 0. 1.0000 0. -4 4 7 -2.96 5.27 0. 1.0000 0. 4 -4 -6 -2.02 2.73 0. 1.0000 0. 4 -4 -5 4.58 3.08 0. 1.0000 0. 4 4 -5 1.10 2.63 0. 1.0000 0. -4 -4 5 2.40 1.87 0. 1.0000 0. -4 4 5 0.42 2.22 0. 1.0000 0. -4 -4 4 0.33 2.06 0. 1.0000 0. 4 -4 -4 -3.77 3.18 0. 1.0000 0. 4 4 -4 1.33 2.64 0. 1.0000 0. -4 4 4 1.20 2.57 0. 1.0000 0. 4 -4 -3 2.47 3.54 0. 1.0000 0. 4 4 -3 0.81 2.75 0. 1.0000 0. -4 4 3 0.80 2.59 0. 1.0000 0. 4 -4 -2 4.82 4.00 0. 1.0000 0. 4 4 -2 1.88 2.92 0. 1.0000 0. 4 -4 -1 -2.84 4.95 0. 1.0000 0. 4 4 -1 -0.17 3.06 0. 1.0000 0. 4 -4 0 -5.52 5.80 0. 1.0000 0. 4 4 0 0.26 2.93 0. 1.0000 0. -4 4 0 -0.55 2.64 0. 1.0000 0. 4 -4 1 -2.80 7.86 0. 1.0000 0. 4 4 1 4.01 3.24 0. 1.0000 0. -4 4 -1 4.64 2.77 0. 1.0000 0. 4 4 1 -2.29 2.91 0. 1.0000 0. 4 4 2 -1.27 3.41 0. 1.0000 0. -4 4 -2 2.17 1.95 0. 1.0000 0. -4 4 -2 0.30 2.83 0. 1.0000 0. 4 4 2 0.28 3.11 0. 1.0000 0. 4 4 3 1.65 4.09 0. 1.0000 0. -4 4 -3 -0.89 1.82 0. 1.0000 0. -4 4 -3 2.05 2.88 0. 1.0000 0. -4 -4 -3 1.97 1.44 0. 1.0000 0. 4 4 3 0.80 2.35 0. 1.0000 0. -4 4 -3 3.13 2.87 0. 1.0000 0. 4 4 4 9.52 4.57 0. 1.0000 0. -4 4 -4 -1.53 2.47 0. 1.0000 0. 4 -5 -5 -0.90 3.22 0. 1.0000 0. -4 5 5 -0.25 2.68 0. 1.0000 0. 4 -5 -4 -6.90 3.84 0. 1.0000 0. 4 5 -4 0.08 2.72 0. 1.0000 0. -4 5 4 2.39 2.73 0. 1.0000 0. 4 -5 -3 8.75 4.30 0. 1.0000 0. 4 5 -3 6.50 2.79 0. 1.0000 0. -4 5 3 7.41 2.60 0. 1.0000 0. 4 -5 -2 -2.37 5.27 0. 1.0000 0. 4 5 -2 -0.33 2.83 0. 1.0000 0. 4 -5 -1 9.38 6.86 0. 1.0000 0. 4 5 -1 4.81 3.18 0. 1.0000 0. -4 5 1 2.32 2.63 0. 1.0000 0. 4 5 0 1.40 3.19 0. 1.0000 0. -4 5 0 0.55 2.63 0. 1.0000 0. 4 5 1 3.73 3.30 0. 1.0000 0. -4 5 -1 -1.30 2.06 0. 1.0000 0. -4 5 -1 5.19 2.81 0. 1.0000 0. 4 5 1 -1.19 2.75 0. 1.0000 0. 4 5 2 -1.45 3.26 0. 1.0000 0. -4 5 -2 -1.63 2.14 0. 1.0000 0. -4 5 -2 0.53 2.86 0. 1.0000 0. 4 5 2 4.14 3.44 0. 1.0000 0. -4 5 -3 1.35 1.65 0. 1.0000 0. -4 5 -3 0.64 2.58 0. 1.0000 0. -4 -5 -3 -0.22 1.98 0. 1.0000 0. 4 5 3 1.66 3.15 0. 1.0000 0. -4 5 -3 -2.19 2.45 0. 1.0000 0. 4 5 4 1.24 2.23 0. 1.0000 0. -4 6 6 -1.99 2.74 0. 1.0000 0. -4 6 5 3.77 2.79 0. 1.0000 0. 4 -6 -4 1.76 4.98 0. 1.0000 0. 4 6 -4 4.01 2.79 0. 1.0000 0. -4 6 4 -4.05 2.79 0. 1.0000 0. 4 -6 -3 3.94 6.07 0. 1.0000 0. 4 6 -3 0.34 2.83 0. 1.0000 0. -4 6 3 -0.77 2.30 0. 1.0000 0. 4 -6 -2 -2.26 5.38 0. 1.0000 0. 4 6 -2 16.86 3.35 0. 1.0000 0. 4 6 -1 0.44 3.12 0. 1.0000 0. -4 6 1 -1.26 2.63 0. 1.0000 0. 4 6 0 2.41 3.11 0. 1.0000 0. -4 6 0 3.81 2.84 0. 1.0000 0. 4 6 1 3.38 3.25 0. 1.0000 0. -4 6 -1 3.13 2.24 0. 1.0000 0. -4 6 -1 1.03 2.72 0. 1.0000 0. 4 6 1 0.64 2.23 0. 1.0000 0. -4 6 -2 1.25 1.89 0. 1.0000 0. -4 6 -2 1.23 2.68 0. 1.0000 0. 4 6 2 3.61 3.41 0. 1.0000 0. -4 6 -2 0.09 2.59 0. 1.0000 0. -4 -6 -3 0.57 2.26 0. 1.0000 0. 4 6 3 3.64 3.38 0. 1.0000 0. -4 -6 -4 1.41 1.92 0. 1.0000 0. 4 6 4 5.85 2.92 0. 1.0000 0. -4 7 5 7.67 2.63 0. 1.0000 0. -4 7 4 10.35 2.71 0. 1.0000 0. 4 7 -3 2.37 2.89 0. 1.0000 0. 4 7 -2 1.78 3.06 0. 1.0000 0. -4 -7 2 -1.01 2.79 0. 1.0000 0. 4 7 -1 12.91 3.21 0. 1.0000 0. -4 7 1 19.04 2.89 0. 1.0000 0. -4 -7 1 13.77 3.15 0. 1.0000 0. 4 7 0 -3.33 3.31 0. 1.0000 0. -4 7 0 3.38 2.11 0. 1.0000 0. -4 7 0 4.88 2.71 0. 1.0000 0. -4 7 -1 2.96 2.31 0. 1.0000 0. -4 7 -1 5.28 2.83 0. 1.0000 0. 4 7 2 2.95 3.40 0. 1.0000 0. -4 7 -2 2.23 2.12 0. 1.0000 0. 4 7 3 1.07 3.37 0. 1.0000 0. 4 7 3 3.48 3.49 0. 1.0000 0. 4 8 -3 0.64 2.83 0. 1.0000 0. -4 -8 3 1.37 2.43 0. 1.0000 0. 4 8 -2 1.46 3.20 0. 1.0000 0. -4 8 2 3.00 2.53 0. 1.0000 0. -4 -8 2 -1.85 3.05 0. 1.0000 0. 4 8 -1 -1.60 3.28 0. 1.0000 0. -4 8 1 -2.87 2.67 0. 1.0000 0. -4 -8 1 3.36 3.11 0. 1.0000 0. -4 8 0 -0.59 2.36 0. 1.0000 0. -4 8 0 4.11 2.71 0. 1.0000 0. -4 8 -1 -0.26 1.92 0. 1.0000 0. -4 8 -1 -2.68 2.53 0. 1.0000 0. -512 # 4368 reflections output ; # end of ARCHIVE-HKL.CIF _chemical_name_common ROY _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: acetone' ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_ROY_ON_4p18GPa _database_code_depnum_ccdc_archive 'CCDC 2098643' loop_ _audit_author_name _audit_author_address 'Nicholas Funnell' ;STFC, ISIS Neutron Facility United Kingdom ; _audit_update_record ; 2021-07-22 deposited with the CCDC. 2021-08-27 downloaded from the CCDC. ; _audit_creation_date 2021-01-26 _audit_creation_method 'CRYSTALS_ver_14.61_build_7795 ' _chemical_name_systematic ; 5-methyl-2[(2-nitrophenyl)amino]-3-thiophenecarbonitrile ; #CheckCIF alerts _vrf_THETM01_ROY_ON_4p18GPa ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575 RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT027_ROY_ON_4p18GPa ; PROBLEM: _diffrn_reflns_theta_full value (too) Low ...... 17.44 Degree RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT029_ROY_ON_4p18GPa ; PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.698 Why? RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT201_ROY_ON_4p18GPa ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 17 Report RESPONSE: The model could only be refined isotropically in order to maintain a favourable data-to-parameter ratio, due to numerous unmeasured reflections. The relatively electron-rich sulfur atom has been modelled anisotropically. ; _vrf_PLAT340_ROY_ON_4p18GPa ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.01109 Ang. RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT413_ROY_ON_4p18GPa ; PROBLEM: Short Inter XH3 .. XHn H2 ..H111 . 1.93 Ang. RESPONSE: These are high-pressure data - short contacts are expected. ; _vrf_PLAT911_ROY_ON_4p18GPa ; PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.555 397 Report RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT157_ROY_ON_4p18GPa ; PROBLEM: Non-standard Monoclinic Beta Angle less 90 Deg 88.04 Degree RESPONSE: This is a series of high pressure structures where the beta angle decreases, passing through 90 degrees. The non-standard beta angle allows the change in angle to be followed clearly. ; _vrf_PLAT411_ROY_ON_4p18GPa ; PROBLEM: Short Inter H...H Contact H5 ..H5 . 2.11 Ang. RESPONSE: These are high-pressure data - short contacts are expected. ; _vrf_PLAT910_ROY_ON_4p18GPa ; PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 8 Note RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _refine_special_details ; In the absence of significant anomalous scattering, Friedel pairs were merged. Data were collected in a Merrill-Bassett diamond anvil cell, which significantly restricts the regions over which reciprocal space can be sampled. Thus, these data are poor quality/incomplete, reflected in numerous CheckCIF alerts regarding refinement statistics. At all pressures, the atomic connectivity is known. All non-sulfur atoms were refined isotropically; sulfur was refined anisotropically. Hydrogen atoms were constrained to ride on their host atoms. #=============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Total Missing #------------------------------------------------------------------------------- 20.82 0.500 0.696 999 695 304 23.01 0.550 0.688 1263 869 394 23.25 0.555 0.685 1285 880 405 ------------------------------------------------------------ ACTA Min. Res. --- Note: The Reported Completeness refers to the Actual H,K,L Index Range ; #end of refcif _cell_length_a 3.49690(2) _cell_length_b 17.29910(6) _cell_length_c 15.77880(6) _cell_angle_alpha 90 _cell_angle_beta 88.037(7) _cell_angle_gamma 90 _cell_volume 953.950(8) _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' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 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' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C12 H9 N3 O2 S1 # Dc = 1.81 Fooo = 536.00 Mu = 3.35 M = 259.29 # Found Formula = C12 H9 N3 O2 S1 # Dc = 1.81 FOOO = 536.00 Mu = 3.35 M = 259.29 _chemical_formula_sum 'C12 H9 N3 O2 S1' _chemical_formula_moiety 'C12 H9 N3 O2 S1' _chemical_compound_source 'TCI Chemicals' _chemical_formula_weight 259.29 _cell_measurement_reflns_used 1540 _cell_measurement_theta_min 1.74 _cell_measurement_theta_max 23.14 _cell_measurement_temperature 293 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_min 0.050 _exptl_crystal_size_mid 0.072 _exptl_crystal_size_max 0.248 _exptl_crystal_density_diffrn 1.805 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 0.335 # Sheldrick geometric approximatio 0.98 0.98 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North et al., 1968)' _exptl_absorpt_correction_T_min 0.09 _exptl_absorpt_correction_T_max 0.98 _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_device 'four-circle diffractometer' _diffrn_radiation_monochromator mirror _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 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction ; CrysAlisPro (Rigaku Oxford Diffraction, 2017) ; _computing_structure_solution 'Model from previously-determined structure' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 293 _diffrn_ambient_pressure 4180000 _diffrn_reflns_number 2440 _diffrn_reflns_av_unetI/netI 0.055 _reflns_number_total 889 _diffrn_reflns_av_R_equivalents 0.048 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 889 # Theoretical number of reflections is about 2739 _diffrn_reflns_theta_min 1.747 _diffrn_reflns_theta_max 23.251 _diffrn_measured_fraction_theta_max 0.655 _diffrn_reflns_theta_full 17.438 _diffrn_measured_fraction_theta_full 0.698 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_h_max 3 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _reflns_limit_h_min -3 _reflns_limit_h_max 3 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 14 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.91 _refine_diff_density_max 0.82 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # Explicitly named reflections are ALWAYS excluded from R&wR # The values actually used during refinement # These are labelled "all" for compatibility with PLATON _oxford_refine_reflns_threshold_expression I>-3.0\s(I) _refine_ls_number_restraints 94 _refine_ls_number_parameters 82 _refine_ls_number_reflns 880 _oxford_refine_ls_R_factor_ref 0.1211 _refine_ls_R_factor_all 0.1211 _refine_ls_wR_factor_ref 0.0617 _refine_ls_wR_factor_all 0.0617 _refine_ls_goodness_of_fit_ref 1.1493 _refine_ls_shift/su_max 0.0001238 _refine_ls_shift/su_mean 0.0000332 # Computed with I/sigma = -10 _oxford_reflns_number_all 880 _oxford_refine_ls_R_factor_all 0.1211 _oxford_refine_ls_wR_factor_all 0.0617 # Computed with no filters except I/sigma = +2 a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 651 _refine_ls_R_factor_gt 0.0799 _refine_ls_wR_factor_gt 0.0585 _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed #undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ; Method= SQRT(W) = 1/(Data with the key SIGMA(/FO/) in list 6) ; # 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 S1 S 0.6456(4) 0.58588(13) 0.43777(13) 0.0266 1.0000 Uani D U . . . . O1 O 0.4531(11) 0.6379(3) 0.0207(4) 0.0340(14) 1.0000 Uiso D U . . . . O2 O 0.4482(11) 0.7041(3) 0.1391(4) 0.0334(14) 1.0000 Uiso D U . . . . C1 C 0.8181(15) 0.5858(5) 0.2231(5) 0.0259(15) 1.0000 Uiso D U . . . . C2 C 1.0094(15) 0.5196(5) 0.2566(5) 0.0254(15) 1.0000 Uiso D U . . . . C3 C 1.0943(15) 0.4583(5) 0.2072(5) 0.0248(16) 1.0000 Uiso D U . . . . C4 C 0.9960(16) 0.4556(4) 0.1225(5) 0.0257(16) 1.0000 Uiso D U . . . . C5 C 0.8089(15) 0.5186(5) 0.0880(5) 0.0239(16) 1.0000 Uiso D U . . . . C6 C 0.7257(14) 0.5818(5) 0.1391(5) 0.0261(15) 1.0000 Uiso D U . . . . C7 C 0.7972(16) 0.6513(4) 0.3629(5) 0.0246(16) 1.0000 Uiso D U . . . . C8 C 0.9582(17) 0.7150(5) 0.3980(5) 0.0277(16) 1.0000 Uiso D U . . . . C9 C 0.9523(17) 0.7105(5) 0.4894(5) 0.0275(17) 1.0000 Uiso D U . . . . C10 C 0.7885(12) 0.6473(4) 0.5195(5) 0.0263(16) 1.0000 Uiso D U . . . . C11 C 0.7321(12) 0.6188(4) 0.6089(5) 0.0338(19) 1.0000 Uiso D U . . . . C12 C 1.1418(18) 0.7697(5) 0.3447(5) 0.0284(16) 1.0000 Uiso D U . . . . N1 N 0.7377(14) 0.6452(4) 0.2774(4) 0.0270(14) 1.0000 Uiso D U . . . . N2 N 1.3057(14) 0.8087(4) 0.2968(4) 0.0322(16) 1.0000 Uiso D U . . . . N3 N 0.5330(14) 0.6453(4) 0.0976(4) 0.0305(15) 1.0000 Uiso D U . . . . H1 H 0.615(8) 0.682(2) 0.256(2) 0.032(4) 1.0000 Uiso D . . . . . H2 H 1.0802 0.5191 0.3129 0.0322 1.0000 Uiso R . . . . . H3 H 1.2252 0.4166 0.2300 0.0338 1.0000 Uiso R . . . . . H4 H 1.0484 0.4117 0.0894 0.0329 1.0000 Uiso R . . . . . H5 H 0.7437 0.5195 0.0314 0.0291 1.0000 Uiso R . . . . . H111 H 0.8609 0.5700 0.6147 0.0772 1.0000 Uiso DR . . . . . H112 H 0.8342 0.6562 0.6472 0.0769 1.0000 Uiso DR . . . . . H113 H 0.4639 0.6120 0.6214 0.0771 1.0000 Uiso DR . . . . . H114 H 1.0623 0.7481 0.5226 0.0333 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 S1 0.0319(8) 0.0234(18) 0.0248(18) -0.0000(9) -0.0046(8) -0.0027(9) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.453(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 S1 . C7 . 1.707(9) yes S1 . C10 . 1.757(7) yes O1 . N3 . 1.261(7) yes O2 . N3 . 1.240(8) yes C1 . C2 . 1.436(10) yes C1 . C6 . 1.378(9) yes C1 . N1 . 1.361(10) yes C2 . C3 . 1.343(10) yes C2 . H2 . 0.930 no C3 . C4 . 1.392(9) yes C3 . H3 . 0.934 no C4 . C5 . 1.392(10) yes C4 . H4 . 0.937 no C5 . C6 . 1.382(11) yes C5 . H5 . 0.929 no C6 . N3 . 1.456(9) yes C7 . C8 . 1.364(10) yes C7 . N1 . 1.376(9) yes C8 . C9 . 1.444(10) yes C8 . C12 . 1.406(11) yes C9 . C10 . 1.315(9) yes C9 . H114 . 0.926 no C10 . C11 . 1.500(10) yes C11 . H111 . 0.963 no C11 . H112 . 0.962 no C11 . H113 . 0.959 no C12 . N2 . 1.152(9) yes N1 . H1 . 0.85(4) 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 C7 . S1 . C10 . 91.0(4) yes C2 . C1 . C6 . 116.2(7) yes C2 . C1 . N1 . 117.3(8) yes C6 . C1 . N1 . 126.4(8) yes C1 . C2 . C3 . 120.8(8) yes C1 . C2 . H2 . 120.1 no C3 . C2 . H2 . 119.1 no C2 . C3 . C4 . 121.8(8) yes C2 . C3 . H3 . 119.2 no C4 . C3 . H3 . 119.0 no C3 . C4 . C5 . 118.9(8) yes C3 . C4 . H4 . 120.9 no C5 . C4 . H4 . 120.2 no C4 . C5 . C6 . 118.9(9) yes C4 . C5 . H5 . 121.5 no C6 . C5 . H5 . 119.6 no C5 . C6 . C1 . 123.4(8) yes C5 . C6 . N3 . 115.2(8) yes C1 . C6 . N3 . 121.4(7) yes S1 . C7 . C8 . 112.2(6) yes S1 . C7 . N1 . 125.0(5) yes C8 . C7 . N1 . 122.6(7) yes C7 . C8 . C9 . 111.7(7) yes C7 . C8 . C12 . 119.1(8) yes C9 . C8 . C12 . 128.6(7) yes C8 . C9 . C10 . 113.4(7) yes C8 . C9 . H114 . 122.3 no C10 . C9 . H114 . 124.3 no S1 . C10 . C9 . 111.6(6) yes S1 . C10 . C11 . 117.4(3) yes C9 . C10 . C11 . 130.9(5) yes C10 . C11 . H111 . 109.3 no C10 . C11 . H112 . 109.3 no H111 . C11 . H112 . 110.1 no C10 . C11 . H113 . 109.3 no H111 . C11 . H113 . 109.3 no H112 . C11 . H113 . 109.5 no C8 . C12 . N2 . 173.7(10) yes C7 . N1 . C1 . 129.8(7) yes C7 . N1 . H1 . 116(3) no C1 . N1 . H1 . 114(3) no C6 . N3 . O1 . 118.5(6) yes C6 . N3 . O2 . 119.3(7) yes O1 . N3 . O2 . 122.2(6) yes _iucr_refine_instructions_details ; # # Punched on 26/01/21 at 12:22:12 # #LIST 12 BLOCK CONT SCALE CONT S ( 1 ,X'S,U'S) CONT O ( 1 ,X'S,U[ISO]) UNTIL H ( 1 ) RIDE C ( 2,X'S) H ( 2,X'S) RIDE C ( 3,X'S) H ( 3,X'S) RIDE C ( 4,X'S) H ( 4,X'S) RIDE C ( 5,X'S) H ( 5,X'S) RIDE C ( 9,X'S) H ( 114,X'S) RIDE C ( 11,X'S) H ( 111,X'S) H ( 112,X'S) H ( 113,X'S) END # # Punched on 26/01/21 at 12:22:12 # #LIST 16 NO REM REM NPF NOTE - FIRST UNTIL LAST REM REM HREST START (DO NOT REMOVE THIS LINE) REM NO H NO #H U MULT DIST REM C-H REM >4 1.5 .96 DISORDER REM 1 1 1.2 .93 C C-H (ACETYLENE) REM 1 2 1.2 .93 C-C(H)-C REM 1 3 1.2 .98 (C)3-C-H REM 2 1 1.2 .93 C=C-H(2) REM 2 2 1.2 .97 (C)2-C-(H)2 REM 3 1 1.5 .96 C-C-(H)3 REM N-H REM >4 1.5 .89 DISORDER REM 1 1 1.2 .86 N-N/H REM 1 2 1.2 .86 (C)2-N-H REM 1 3 1.2 .89 (C)3-N-H REM 2 1 1.2 .86 C-N-(H)2 REM 2 2 1.2 .89 (C)2-N-(H)2 REM 3 1 1.2 .89 C-H-(H)3 REM O-H REM 1 1 1.5 .82 O-H REM REM DIST ESD = 0.02 REM VIB ESD = 0.002 REM ANGLE ESD = 2.0 REM REM TO ACTIVATE THE VIB RESTRAINTS, REMOVE LEADING REM REM H1-N-R2 DIST 0.86, 0.02 = CONT N ( 1) TO H(1) REST 0.032, 0.002 = H(1,U[ISO]) ANGLE 0.0, 2.0 = MEAN CONT H(1) TO N ( 1) TO C(7) CONT H(1) TO N ( 1) TO C(1) REM HREST END (DO NOT REMOVE THIS LINE) REM DELU START (DO NOT REMOVE THIS LINE) VIBR .0, 0.00200 = S(1) TO C(10) VIBR .0, 0.00200 = S(1) TO C(7) VIBR .0, 0.00500 = C(7) TO C(10) VIBR .0, 0.00200 = N(2) TO C(12) VIBR .0, 0.00200 = C(10) TO C(9) VIBR .0, 0.00200 = C(10) TO C(11) VIBR .0, 0.00500 = C(9) TO S(1) VIBR .0, 0.00500 = C(11) TO S(1) VIBR .0, 0.00500 = C(11) TO C(9) VIBR .0, 0.00200 = C(12) TO C(8) VIBR .0, 0.00500 = C(8) TO N(2) VIBR .0, 0.00200 = O(1) TO N(3) VIBR .0, 0.00200 = C(2) TO C(1) VIBR .0, 0.00200 = C(2) TO C(3) VIBR .0, 0.00500 = C(3) TO C(1) VIBR .0, 0.00200 = N(1) TO C(7) VIBR .0, 0.00200 = N(1) TO C(1) VIBR .0, 0.00500 = C(1) TO C(7) VIBR .0, 0.00200 = C(7) TO C(8) VIBR .0, 0.00500 = N(1) TO S(1) VIBR .0, 0.00500 = C(8) TO S(1) VIBR .0, 0.00500 = C(8) TO N(1) VIBR .0, 0.00200 = O(2) TO N(3) VIBR .0, 0.00200 = N(3) TO C(6) VIBR .0, 0.00500 = O(1) TO O(2) VIBR .0, 0.00500 = C(6) TO O(2) VIBR .0, 0.00500 = C(6) TO O(1) VIBR .0, 0.00200 = C(5) TO C(4) VIBR .0, 0.00200 = C(5) TO C(6) VIBR .0, 0.00500 = C(6) TO C(4) VIBR .0, 0.00200 = C(4) TO C(3) VIBR .0, 0.00500 = C(3) TO C(5) VIBR .0, 0.00200 = C(1) TO C(6) VIBR .0, 0.00500 = N(1) TO C(2) VIBR .0, 0.00500 = C(6) TO C(2) VIBR .0, 0.00500 = C(6) TO N(1) VIBR .0, 0.00500 = C(5) TO N(3) VIBR .0, 0.00500 = C(1) TO N(3) VIBR .0, 0.00500 = C(1) TO C(5) VIBR .0, 0.00200 = C(9) TO C(8) VIBR .0, 0.00500 = C(8) TO C(10) VIBR .0, 0.00500 = C(2) TO C(4) VIBR .0, 0.00500 = C(12) TO C(9) VIBR .0, 0.00500 = C(7) TO C(9) VIBR .0, 0.00500 = C(7) TO C(12) REM DELU END (DO NOT REMOVE THIS LINE) ANGLE 110.000000 , 0.020000 = C(10) TO C(11) TO H(111) ANGLE 110.000000 , 0.020000 = C(10) TO C(11) TO H(112) ANGLE 110.000000 , 0.020000 = C(10) TO C(11) TO H(113) DISTANCE 1.225000 , 0.050000 = O(2) TO N(3) DISTANCE 1.225000 , 0.050000 = O(1) TO N(3) DISTANCE 1.440000 , 0.050000 = C(6) TO N(3) DISTANCE 1.390000 , 0.050000 = C(5) TO C(6) DISTANCE 1.364000 , 0.050000 = C(4) TO C(5) DISTANCE 1.222000 , 0.050000 = O(1) TO N(3) DISTANCE 1.232000 , 0.050000 = O(2) TO N(3) DISTANCE 1.440000 , 0.050000 = C(6) TO N(3) DISTANCE 1.392000 , 0.050000 = C(5) TO C(6) DISTANCE 1.364000 , 0.050000 = C(4) TO C(5) DISTANCE 1.391000 , 0.050000 = C(3) TO C(4) DISTANCE 1.371000 , 0.050000 = C(2) TO C(3) DISTANCE 1.400000 , 0.050000 = C(1) TO C(2) DISTANCE 1.408000 , 0.050000 = C(1) TO C(6) DISTANCE 1.382000 , 0.050000 = C(1) TO N(1) DISTANCE 1.387000 , 0.050000 = C(7) TO N(1) DISTANCE 1.728000 , 0.050000 = S(1) TO C(7) DISTANCE 1.724000 , 0.050000 = S(1) TO C(10) DISTANCE 1.500000 , 0.050000 = C(10) TO C(11) DISTANCE 1.349000 , 0.050000 = C(9) TO C(10) DISTANCE 1.427000 , 0.050000 = C(8) TO C(9) DISTANCE 1.372000 , 0.050000 = C(7) TO C(8) DISTANCE 1.422000 , 0.050000 = C(8) TO C(12) DISTANCE 1.141000 , 0.050000 = C(12) TO N(2) REM THERMSIM START (DO NOT REMOVE THIS LINE) U(IJ) .0, 0.04000 = S(1) TO C(7) U(IJ) .0, 0.04000 = S(1) TO C(10) U(IJ) .0, 0.08000 = O(1) TO N(3) U(IJ) .0, 0.08000 = O(2) TO N(3) U(IJ) .0, 0.04000 = C(1) TO C(2) U(IJ) .0, 0.04000 = C(1) TO C(6) U(IJ) .0, 0.04000 = C(1) TO N(1) U(IJ) .0, 0.04000 = C(2) TO C(3) U(IJ) .0, 0.04000 = C(3) TO C(4) U(IJ) .0, 0.04000 = C(4) TO C(5) U(IJ) .0, 0.04000 = C(5) TO C(6) U(IJ) .0, 0.04000 = C(6) TO N(3) U(IJ) .0, 0.04000 = C(7) TO C(8) U(IJ) .0, 0.04000 = C(7) TO N(1) U(IJ) .0, 0.04000 = C(8) TO C(9) U(IJ) .0, 0.04000 = C(8) TO C(12) U(IJ) .0, 0.04000 = C(9) TO C(10) U(IJ) .0, 0.08000 = C(10) TO C(11) U(IJ) .0, 0.08000 = C(12) TO N(2) REM THERMSIM END (DO NOT REMOVE THIS LINE) PLANAR 0.010000 C(1) C(6) N(1) H(1) PLANAR 0.010000 C(1) C(2) C(3) C(4) C(5) C(6) N(1) N(3) PLANAR 0.010000 S(1) C(7) C(8) C(9) C(10) N(1) 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 0 5 1 x . -2 12 3 x . 2 10 1 x . # looking for ARCHIVE-HKL.CIF _iucr_refine_reflections_details ; # Data was input as F-squared # punching LIST 6 as LIST 6 with all keys set # NBGNXT= 36 #LIST 6 READ NCOEF= 8 TYPE=FIX, F'S = FSQ UNIT=DATA, CHECK=NO L30=NO ARCH=NO STORE NCOEF= 6 OUTPUT INDICES /FO/ SIGMA(/FO/) RATIO/JCODE CORRECTIONS SERIAL CONT INPUT H K L /FO/ SIGMA(/FO/) JCODE CONT CORRECTIONS SERIAL FOR (I4,I4,I4,F10.2,F8.2,F4.0,F7.4,F7.0) END 0 -1 -1 1.99 0.15 0. 1.0000 0. 0 1 1 1.96 0.12 0. 1.0000 0. 0 -1 -1 2.00 0.14 0. 1.0000 0. 0 -1 -1 1.77 0.21 0. 1.0000 0. 0 -1 -2 56.64 1.94 0. 1.0000 0. 0 -1 -3 583.36 18.32 0. 1.0000 0. 0 2 1 1271.23 39.39 0. 1.0000 0. 0 2 2 81.81 2.76 0. 1.0000 0. 0 -2 -2 80.49 2.74 0. 1.0000 0. 0 2 2 83.64 2.66 0. 1.0000 0. 0 2 2 85.30 2.78 0. 1.0000 0. 0 -2 -2 81.42 2.65 0. 1.0000 0. 0 -2 -4 46.35 1.75 0. 1.0000 0. 0 -2 -6 947.91 29.90 0. 1.0000 0. 0 -3 -1 235.45 8.87 0. 1.0000 0. 0 -3 -2 37.68 1.71 0. 1.0000 0. 0 3 2 40.55 1.39 0. 1.0000 0. 0 3 2 38.54 1.50 0. 1.0000 0. 0 -3 -2 42.97 1.70 0. 1.0000 0. 0 3 2 40.21 1.53 0. 1.0000 0. 0 3 2 42.51 2.28 0. 1.0000 0. 0 3 3 1.72 0.54 0. 1.0000 0. 0 3 3 1.79 0.38 0. 1.0000 0. 0 -3 -4 156.10 4.79 0. 1.0000 0. 0 -3 -4 148.43 4.67 0. 1.0000 0. 0 3 4 130.40 4.92 0. 1.0000 0. 0 -3 -4 147.85 4.72 0. 1.0000 0. 0 -3 -5 58.77 2.19 0. 1.0000 0. 0 -3 -6 167.39 5.62 0. 1.0000 0. 0 -3 -7 3.90 1.12 0. 1.0000 0. 0 -3 -7 3.50 0.95 0. 1.0000 0. 0 -3 -8 0.24 1.27 0. 1.0000 0. 0 4 1 0.72 0.26 0. 1.0000 0. 0 -4 -1 1.08 1.22 0. 1.0000 0. 0 4 2 392.31 13.05 0. 1.0000 0. 0 -4 -2 410.59 13.56 0. 1.0000 0. 0 -4 -3 48.80 1.60 0. 1.0000 0. 0 4 3 48.67 2.61 0. 1.0000 0. 0 4 3 50.98 1.68 0. 1.0000 0. 0 4 3 51.34 1.76 0. 1.0000 0. 0 4 3 48.05 1.83 0. 1.0000 0. 0 -4 -3 45.34 2.17 0. 1.0000 0. 0 4 3 51.43 1.93 0. 1.0000 0. 0 4 4 49.39 1.91 0. 1.0000 0. 0 -4 -4 49.24 1.80 0. 1.0000 0. 0 -4 -5 578.78 18.41 0. 1.0000 0. 0 -4 -5 581.78 18.04 0. 1.0000 0. 0 -4 -5 586.19 18.21 0. 1.0000 0. 0 -4 -5 585.33 18.22 0. 1.0000 0. 0 4 5 592.38 18.48 0. 1.0000 0. 0 -4 -5 579.49 18.12 0. 1.0000 0. 0 -4 -6 31.96 1.55 0. 1.0000 0. 0 -4 -6 34.75 1.74 0. 1.0000 0. 0 4 6 29.47 1.95 0. 1.0000 0. 0 -4 -6 32.31 1.43 0. 1.0000 0. 0 -4 -6 30.19 1.29 0. 1.0000 0. 0 -4 -7 283.91 9.11 0. 1.0000 0. 0 -4 -7 275.58 9.30 0. 1.0000 0. 0 -4 -8 -0.59 1.28 0. 1.0000 0. 0 -4 -8 -1.08 1.11 0. 1.0000 0. 0 -4 -9 101.69 2.77 0. 1.0000 0. 0 -4 -9 1.78 1.27 0. 1.0000 0. 0 5 1 0.14 0.20 0. 1.0000 0. 0 -5 -3 228.37 7.27 0. 1.0000 0. 0 -5 -3 194.04 7.72 0. 1.0000 0. 0 5 3 202.27 7.30 0. 1.0000 0. 0 -5 -4 526.40 17.64 0. 1.0000 0. 0 -5 -4 546.93 16.97 0. 1.0000 0. 0 5 4 549.68 17.17 0. 1.0000 0. 0 -5 -4 554.71 17.56 0. 1.0000 0. 0 5 4 561.07 18.43 0. 1.0000 0. 0 5 4 556.59 17.30 0. 1.0000 0. 0 5 4 557.51 17.35 0. 1.0000 0. 0 -5 -5 194.47 6.57 0. 1.0000 0. 0 -5 -5 198.82 6.43 0. 1.0000 0. 0 5 5 204.35 6.76 0. 1.0000 0. 0 5 6 30.23 1.90 0. 1.0000 0. 0 -5 -6 29.34 1.28 0. 1.0000 0. 0 -5 -6 30.37 1.11 0. 1.0000 0. 0 -5 -6 29.91 1.47 0. 1.0000 0. 0 -5 -6 29.50 1.38 0. 1.0000 0. 0 -5 -6 29.22 1.71 0. 1.0000 0. 0 -5 -7 195.97 6.12 0. 1.0000 0. 0 -5 -7 184.28 6.35 0. 1.0000 0. 0 -5 -7 200.96 6.67 0. 1.0000 0. 0 -5 -7 193.53 6.40 0. 1.0000 0. 0 -5 -7 194.34 6.25 0. 1.0000 0. 0 5 7 181.53 6.96 0. 1.0000 0. 0 -5 -8 30.71 1.61 0. 1.0000 0. 0 -5 -8 30.14 1.97 0. 1.0000 0. 0 -5 -8 33.67 1.90 0. 1.0000 0. 0 -5 -8 30.24 1.38 0. 1.0000 0. 0 -5 -8 31.49 1.66 0. 1.0000 0. 0 -5 -9 291.72 9.46 0. 1.0000 0. 0 -5 -9 272.07 9.12 0. 1.0000 0. 0 -5 -9 271.81 9.01 0. 1.0000 0. 0 -5 -10 0.62 1.30 0. 1.0000 0. 0 -5 -10 0.32 1.66 0. 1.0000 0. 0 -5 -11 3.59 1.79 0. 1.0000 0. 0 6 3 193.03 6.27 0. 1.0000 0. 0 -6 -3 181.43 8.69 0. 1.0000 0. 0 -6 -3 195.80 6.18 0. 1.0000 0. 0 -6 -3 217.95 6.56 0. 1.0000 0. 0 6 4 124.23 4.09 0. 1.0000 0. 0 6 4 126.82 4.92 0. 1.0000 0. 0 -6 -4 135.39 4.70 0. 1.0000 0. 0 6 4 125.59 3.99 0. 1.0000 0. 0 6 4 128.96 4.22 0. 1.0000 0. 0 6 5 6.64 0.94 0. 1.0000 0. 0 -6 -5 7.33 1.82 0. 1.0000 0. 0 6 5 6.22 1.27 0. 1.0000 0. 0 6 5 6.14 2.45 0. 1.0000 0. 0 6 6 38.60 1.98 0. 1.0000 0. 0 -6 -6 33.43 2.20 0. 1.0000 0. 0 6 6 39.88 2.74 0. 1.0000 0. 0 6 6 35.07 1.93 0. 1.0000 0. 0 -6 -6 33.30 1.34 0. 1.0000 0. 0 -6 -7 128.27 4.79 0. 1.0000 0. 0 -6 -7 123.59 4.34 0. 1.0000 0. 0 -6 -8 268.63 8.73 0. 1.0000 0. 0 -6 -8 262.08 8.38 0. 1.0000 0. 0 6 8 224.22 9.30 0. 1.0000 0. 0 -6 -8 275.60 8.56 0. 1.0000 0. 0 -6 -8 280.17 9.14 0. 1.0000 0. 0 -6 -8 282.72 8.75 0. 1.0000 0. 0 -6 -9 35.06 1.84 0. 1.0000 0. 0 -6 -9 35.68 1.73 0. 1.0000 0. 0 -6 -9 37.03 2.04 0. 1.0000 0. 0 -6 -9 32.79 1.41 0. 1.0000 0. 0 -6 -9 33.85 2.30 0. 1.0000 0. 0 -6 -10 209.23 6.81 0. 1.0000 0. 0 -6 -10 211.14 7.06 0. 1.0000 0. 0 -6 -10 221.24 7.01 0. 1.0000 0. 0 -6 -10 206.11 7.37 0. 1.0000 0. 0 -6 -10 192.65 6.59 0. 1.0000 0. 0 -6 -11 26.11 1.90 0. 1.0000 0. 0 -6 -11 25.80 1.91 0. 1.0000 0. 0 -6 -11 24.12 2.30 0. 1.0000 0. 0 -6 -11 25.80 2.40 0. 1.0000 0. 0 -6 -12 4.89 2.05 0. 1.0000 0. 0 7 3 2014.22 62.22 0. 1.0000 0. 0 -7 -3 2073.79 62.78 0. 1.0000 0. 0 -7 -4 555.22 16.82 0. 1.0000 0. 0 -7 -4 526.80 16.32 0. 1.0000 0. 0 -7 -5 328.22 11.10 0. 1.0000 0. 0 -7 -5 298.99 11.84 0. 1.0000 0. 0 7 5 328.08 10.69 0. 1.0000 0. 0 7 5 336.60 10.38 0. 1.0000 0. 0 7 5 315.84 11.17 0. 1.0000 0. 0 7 6 1.25 1.54 0. 1.0000 0. 0 7 6 3.42 3.37 0. 1.0000 0. 0 -7 -6 3.34 2.14 0. 1.0000 0. 0 7 6 2.76 1.12 0. 1.0000 0. 0 7 7 277.58 10.28 0. 1.0000 0. 0 -7 -7 276.12 9.39 0. 1.0000 0. 0 -7 -7 254.43 8.25 0. 1.0000 0. 0 7 7 284.72 8.91 0. 1.0000 0. 0 -7 -8 89.29 4.30 0. 1.0000 0. 0 7 8 108.71 5.21 0. 1.0000 0. 0 7 8 98.55 4.36 0. 1.0000 0. 0 -7 -9 105.21 4.04 0. 1.0000 0. 0 -7 -9 117.39 4.75 0. 1.0000 0. 0 -7 -10 302.88 9.89 0. 1.0000 0. 0 -7 -10 296.49 9.86 0. 1.0000 0. 0 -7 -10 299.62 10.45 0. 1.0000 0. 0 -7 -11 470.04 15.04 0. 1.0000 0. 0 -7 -11 454.07 14.46 0. 1.0000 0. 0 -7 -11 448.36 14.44 0. 1.0000 0. 0 -7 -11 433.67 14.20 0. 1.0000 0. 0 -7 -12 53.48 3.37 0. 1.0000 0. 0 -7 -12 41.97 2.37 0. 1.0000 0. 0 -7 -12 48.13 2.54 0. 1.0000 0. 0 -7 -13 3.79 2.37 0. 1.0000 0. 0 -7 -13 -0.07 1.38 0. 1.0000 0. 0 -8 -4 24.24 2.00 0. 1.0000 0. 0 -8 -4 22.90 7.12 0. 1.0000 0. 0 -8 -4 21.94 1.36 0. 1.0000 0. 0 -8 -4 27.35 2.63 0. 1.0000 0. 0 -8 -5 15.05 4.85 0. 1.0000 0. 0 8 5 20.14 1.13 0. 1.0000 0. 0 8 5 19.42 0.83 0. 1.0000 0. 0 8 5 21.25 1.45 0. 1.0000 0. 0 -8 -5 25.44 2.13 0. 1.0000 0. 0 -8 -5 18.59 2.28 0. 1.0000 0. 0 8 6 2.28 1.19 0. 1.0000 0. 0 8 6 2.39 2.45 0. 1.0000 0. 0 -8 -6 1.35 3.25 0. 1.0000 0. 0 -8 -7 75.05 4.60 0. 1.0000 0. 0 8 7 75.23 3.36 0. 1.0000 0. 0 8 7 77.46 3.79 0. 1.0000 0. 0 8 7 59.55 6.00 0. 1.0000 0. 0 -8 -8 55.15 1.98 0. 1.0000 0. 0 8 8 60.37 3.11 0. 1.0000 0. 0 -8 -8 57.51 3.80 0. 1.0000 0. 0 -8 -9 1.14 2.59 0. 1.0000 0. 0 8 9 -1.78 2.10 0. 1.0000 0. 0 8 9 -1.16 2.52 0. 1.0000 0. 0 8 9 -0.43 3.33 0. 1.0000 0. 0 -8 -10 14.90 1.87 0. 1.0000 0. 0 -8 -10 10.52 2.97 0. 1.0000 0. 0 8 10 15.35 3.72 0. 1.0000 0. 0 -8 -11 2.20 2.56 0. 1.0000 0. 0 8 11 -1.01 3.84 0. 1.0000 0. 0 -8 -11 -0.03 1.84 0. 1.0000 0. 0 -8 -12 63.54 3.25 0. 1.0000 0. 0 -8 -12 68.23 4.15 0. 1.0000 0. 0 -8 -13 211.86 8.29 0. 1.0000 0. 0 -8 -14 -1.68 2.43 0. 1.0000 0. 0 -9 -4 1692.36 51.79 0. 1.0000 0. 0 -9 -4 1589.48 52.52 0. 1.0000 0. 0 -9 -5 18.99 1.35 0. 1.0000 0. 0 -9 -5 25.97 2.43 0. 1.0000 0. 0 9 5 18.88 1.19 0. 1.0000 0. 0 9 5 17.72 0.88 0. 1.0000 0. 0 -9 -5 16.34 7.89 0. 1.0000 0. 0 9 6 386.02 12.32 0. 1.0000 0. 0 -9 -6 372.21 15.92 0. 1.0000 0. 0 -9 -6 401.62 13.42 0. 1.0000 0. 0 9 6 396.60 12.75 0. 1.0000 0. 0 -9 -7 49.68 5.45 0. 1.0000 0. 0 9 7 58.95 2.87 0. 1.0000 0. 0 9 8 0.44 4.68 0. 1.0000 0. 0 9 8 1.66 1.82 0. 1.0000 0. 0 9 8 4.68 2.70 0. 1.0000 0. 0 -9 -8 6.16 3.82 0. 1.0000 0. 0 9 9 65.68 7.14 0. 1.0000 0. 0 9 9 69.19 3.98 0. 1.0000 0. 0 9 9 63.04 3.70 0. 1.0000 0. 0 -9 -9 69.47 5.15 0. 1.0000 0. 0 -9 -10 227.19 9.30 0. 1.0000 0. 0 9 10 230.49 8.34 0. 1.0000 0. 0 9 10 221.24 8.92 0. 1.0000 0. 0 9 10 232.35 11.13 0. 1.0000 0. 0 9 11 36.99 5.12 0. 1.0000 0. 0 9 11 39.55 3.28 0. 1.0000 0. 0 -9 -11 40.83 4.11 0. 1.0000 0. 0 9 12 205.71 7.76 0. 1.0000 0. 0 9 12 190.00 9.38 0. 1.0000 0. 0 -9 -12 200.63 8.38 0. 1.0000 0. 0 9 13 59.41 5.78 0. 1.0000 0. 0 -9 -13 62.46 4.61 0. 1.0000 0. 0 9 14 3.97 4.82 0. 1.0000 0. 0 -9 -14 1.04 3.36 0. 1.0000 0. 0 -10 -4 14.71 2.17 0. 1.0000 0. 0 -10 -5 14.33 2.77 0. 1.0000 0. 0 -10 -6 49.09 9.19 0. 1.0000 0. 0 10 6 59.86 2.76 0. 1.0000 0. 0 -10 -6 54.95 2.37 0. 1.0000 0. 0 10 7 18.48 4.64 0. 1.0000 0. 0 -10 -7 28.16 1.51 0. 1.0000 0. 0 10 7 32.62 2.20 0. 1.0000 0. 0 -10 -7 29.16 6.98 0. 1.0000 0. 0 10 8 79.32 5.69 0. 1.0000 0. 0 10 8 100.63 4.26 0. 1.0000 0. 0 -10 -8 87.51 8.01 0. 1.0000 0. 0 10 9 -0.14 3.49 0. 1.0000 0. 0 -10 -9 0.72 5.40 0. 1.0000 0. 0 10 9 -1.46 2.57 0. 1.0000 0. 0 10 10 31.32 7.32 0. 1.0000 0. 0 10 10 39.33 4.01 0. 1.0000 0. 0 -10 -10 47.94 5.59 0. 1.0000 0. 0 10 10 45.82 4.02 0. 1.0000 0. 0 -10 -11 79.45 5.94 0. 1.0000 0. 0 10 11 90.24 8.82 0. 1.0000 0. 0 10 11 78.47 4.78 0. 1.0000 0. 0 10 12 10.32 3.18 0. 1.0000 0. 0 10 12 12.66 6.88 0. 1.0000 0. 0 -10 -12 14.81 4.56 0. 1.0000 0. 0 -10 -13 267.04 10.91 0. 1.0000 0. 0 10 13 245.08 9.43 0. 1.0000 0. 0 10 13 229.44 12.79 0. 1.0000 0. 0 -10 -14 27.47 4.74 0. 1.0000 0. 0 10 14 24.03 3.72 0. 1.0000 0. 0 10 14 20.55 6.40 0. 1.0000 0. 0 -11 -4 9.86 2.34 0. 1.0000 0. 0 -11 -5 82.42 4.63 0. 1.0000 0. 0 -11 -5 67.11 3.95 0. 1.0000 0. 0 -11 -6 62.64 3.68 0. 1.0000 0. 0 11 6 52.88 2.84 0. 1.0000 0. 0 -11 -6 48.02 3.97 0. 1.0000 0. 0 11 7 31.33 2.27 0. 1.0000 0. 0 -11 -7 50.31 13.28 0. 1.0000 0. 0 -11 -7 36.29 2.08 0. 1.0000 0. 0 -11 -7 28.56 4.39 0. 1.0000 0. 0 11 8 -2.68 5.05 0. 1.0000 0. 0 -11 -8 8.78 8.48 0. 1.0000 0. 0 -11 -8 3.22 1.18 0. 1.0000 0. 0 11 8 6.65 1.94 0. 1.0000 0. 0 11 9 194.71 10.32 0. 1.0000 0. 0 -11 -9 211.49 12.01 0. 1.0000 0. 0 11 10 25.57 3.58 0. 1.0000 0. 0 -11 -10 33.09 7.34 0. 1.0000 0. 0 11 11 1.77 4.16 0. 1.0000 0. 0 -11 -11 -0.14 6.00 0. 1.0000 0. 0 11 11 0.89 3.92 0. 1.0000 0. 0 -11 -12 84.60 7.85 0. 1.0000 0. 0 11 12 102.81 5.88 0. 1.0000 0. 0 -11 -13 2.93 5.38 0. 1.0000 0. 0 11 13 -7.09 8.30 0. 1.0000 0. 0 11 13 3.38 4.09 0. 1.0000 0. 0 -11 -14 19.32 5.27 0. 1.0000 0. 0 11 14 18.51 8.74 0. 1.0000 0. 0 11 14 18.93 4.25 0. 1.0000 0. 0 -12 -4 11.42 2.62 0. 1.0000 0. 0 -12 -5 -5.08 3.65 0. 1.0000 0. 0 -12 -5 -0.05 2.67 0. 1.0000 0. 0 -12 -6 129.16 6.12 0. 1.0000 0. 0 -12 -7 16.88 4.43 0. 1.0000 0. 0 12 7 4.02 1.86 0. 1.0000 0. 0 12 8 236.05 8.48 0. 1.0000 0. 0 -12 -8 216.74 16.83 0. 1.0000 0. 0 12 9 17.93 2.78 0. 1.0000 0. 0 12 9 6.85 5.67 0. 1.0000 0. 0 -12 -9 19.77 11.31 0. 1.0000 0. 0 -12 -10 234.75 14.58 0. 1.0000 0. 0 12 10 262.70 9.36 0. 1.0000 0. 0 12 11 87.51 7.46 0. 1.0000 0. 0 -12 -11 98.26 10.16 0. 1.0000 0. 0 -12 -12 5.63 7.06 0. 1.0000 0. 0 12 12 10.31 5.78 0. 1.0000 0. 0 12 13 -0.82 5.17 0. 1.0000 0. 0 -12 -13 6.53 7.11 0. 1.0000 0. 0 -13 -4 -2.11 2.63 0. 1.0000 0. 0 -13 -5 16.96 3.22 0. 1.0000 0. 0 -13 -6 30.13 3.94 0. 1.0000 0. 0 -13 -6 29.98 3.65 0. 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0. 3 5 10 5.62 4.44 0. 1.0000 0. -3 -5 -10 3.42 4.08 0. 1.0000 0. 3 5 9 1.20 5.08 0. 1.0000 0. -3 -5 -9 -3.22 4.64 0. 1.0000 0. 3 5 9 1.13 4.12 0. 1.0000 0. 3 5 8 8.65 4.69 0. 1.0000 0. -3 -5 -8 -1.43 5.36 0. 1.0000 0. 3 5 8 3.21 4.00 0. 1.0000 0. -3 -5 -8 0.62 4.30 0. 1.0000 0. 3 5 7 99.46 6.22 0. 1.0000 0. 3 5 7 111.47 6.01 0. 1.0000 0. -3 -5 -7 85.14 9.17 0. 1.0000 0. 3 5 7 110.34 5.45 0. 1.0000 0. 3 5 6 2.06 3.49 0. 1.0000 0. 3 5 6 1.50 2.79 0. 1.0000 0. 3 5 6 3.15 4.62 0. 1.0000 0. 3 5 5 1.64 3.22 0. 1.0000 0. 3 5 5 3.52 2.30 0. 1.0000 0. 3 5 5 -4.15 5.13 0. 1.0000 0. 3 5 4 75.20 7.52 0. 1.0000 0. 3 5 4 94.00 4.88 0. 1.0000 0. 3 5 3 -0.27 2.94 0. 1.0000 0. 3 5 3 -1.15 2.73 0. 1.0000 0. 3 5 3 2.87 6.67 0. 1.0000 0. -3 5 -3 1.78 2.87 0. 1.0000 0. -3 5 -3 0.60 2.88 0. 1.0000 0. 3 5 2 20.49 2.27 0. 1.0000 0. 3 5 2 20.14 3.09 0. 1.0000 0. -3 5 -2 18.72 3.49 0. 1.0000 0. 3 5 2 24.94 3.24 0. 1.0000 0. 3 -5 1 -0.07 4.03 0. 1.0000 0. 3 5 1 -2.36 2.86 0. 1.0000 0. 3 -5 1 2.36 4.30 0. 1.0000 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0. 3 6 9 39.39 5.28 0. 1.0000 0. -3 -6 -9 21.34 6.49 0. 1.0000 0. 3 6 9 22.48 4.86 0. 1.0000 0. 3 6 8 7.89 4.62 0. 1.0000 0. 3 6 8 10.80 3.17 0. 1.0000 0. -3 -6 -8 10.31 7.03 0. 1.0000 0. 3 6 8 7.05 4.77 0. 1.0000 0. 3 6 7 13.65 4.04 0. 1.0000 0. 3 6 7 13.03 3.12 0. 1.0000 0. 3 6 7 13.73 5.03 0. 1.0000 0. 3 6 6 13.71 3.67 0. 1.0000 0. 3 6 6 15.24 3.07 0. 1.0000 0. 3 6 6 10.54 5.77 0. 1.0000 0. 3 6 5 23.65 3.46 0. 1.0000 0. 3 6 5 20.50 2.70 0. 1.0000 0. 3 6 5 14.63 6.41 0. 1.0000 0. 3 6 4 59.06 3.39 0. 1.0000 0. 3 6 4 47.07 7.94 0. 1.0000 0. 3 6 4 52.59 4.15 0. 1.0000 0. 3 6 3 2.75 3.04 0. 1.0000 0. 3 6 3 0.87 1.44 0. 1.0000 0. 3 6 3 1.13 6.41 0. 1.0000 0. 3 6 3 3.78 2.16 0. 1.0000 0. -3 6 -2 34.12 3.29 0. 1.0000 0. -3 6 -2 38.32 3.49 0. 1.0000 0. 3 6 1 55.78 3.86 0. 1.0000 0. -3 6 -1 43.97 3.42 0. 1.0000 0. 3 -6 1 40.51 3.08 0. 1.0000 0. 3 6 0 87.96 4.89 0. 1.0000 0. -3 6 0 86.71 3.32 0. 1.0000 0. 3 -6 0 72.39 6.10 0. 1.0000 0. -3 6 0 87.11 4.46 0. 1.0000 0. 3 -6 0 80.83 5.49 0. 1.0000 0. 3 -6 0 81.06 4.05 0. 1.0000 0. 3 -6 -1 21.08 2.45 0. 1.0000 0. 3 -6 -1 19.11 4.02 0. 1.0000 0. 3 6 -1 20.67 3.37 0. 1.0000 0. 3 -6 -1 18.85 4.23 0. 1.0000 0. 3 -6 -2 300.91 5.94 0. 1.0000 0. 3 -6 -2 329.63 7.62 0. 1.0000 0. 3 -6 -3 2.33 3.28 0. 1.0000 0. 3 -6 -3 -0.09 1.77 0. 1.0000 0. -3 6 3 -0.33 2.30 0. 1.0000 0. 3 -6 -4 19.01 3.20 0. 1.0000 0. 3 -6 -4 15.88 1.96 0. 1.0000 0. 3 -6 -5 28.99 3.68 0. 1.0000 0. 3 -6 -5 28.31 2.23 0. 1.0000 0. 3 -6 -5 32.80 3.35 0. 1.0000 0. 3 -6 -6 14.88 2.95 0. 1.0000 0. 3 -6 -7 27.81 3.07 0. 1.0000 0. 3 -6 -8 43.13 3.32 0. 1.0000 0. 3 7 9 28.00 5.24 0. 1.0000 0. -3 -7 -9 16.39 8.47 0. 1.0000 0. 3 7 9 21.45 5.52 0. 1.0000 0. 3 7 8 -0.14 4.28 0. 1.0000 0. 3 7 8 -0.31 3.04 0. 1.0000 0. -3 -7 -8 1.45 8.91 0. 1.0000 0. 3 7 8 -3.84 5.70 0. 1.0000 0. 3 7 7 7.94 3.71 0. 1.0000 0. 3 7 7 5.02 3.13 0. 1.0000 0. 3 7 7 4.58 6.27 0. 1.0000 0. 3 7 6 6.68 3.48 0. 1.0000 0. 3 7 6 11.33 2.98 0. 1.0000 0. 3 7 6 0.30 6.59 0. 1.0000 0. 3 7 5 30.40 2.90 0. 1.0000 0. 3 7 5 29.03 3.58 0. 1.0000 0. 3 7 5 25.08 7.72 0. 1.0000 0. 3 7 4 17.15 3.38 0. 1.0000 0. 3 7 4 11.43 2.36 0. 1.0000 0. 3 7 4 8.55 7.30 0. 1.0000 0. 3 7 3 3.39 3.07 0. 1.0000 0. 3 7 3 1.59 2.23 0. 1.0000 0. 3 7 2 4.10 3.08 0. 1.0000 0. 3 7 1 37.57 3.64 0. 1.0000 0. -3 7 -1 39.87 3.16 0. 1.0000 0. -3 7 -1 40.85 3.41 0. 1.0000 0. 3 7 0 1.14 3.22 0. 1.0000 0. 3 -7 0 1.01 2.27 0. 1.0000 0. 3 7 -1 45.41 3.89 0. 1.0000 0. -3 7 1 50.28 2.30 0. 1.0000 0. 3 -7 -1 46.86 2.95 0. 1.0000 0. 3 -7 -2 15.81 3.96 0. 1.0000 0. 3 -7 -2 13.64 2.30 0. 1.0000 0. -3 7 2 19.49 1.97 0. 1.0000 0. 3 -7 -3 5.11 3.62 0. 1.0000 0. 3 -7 -3 3.01 1.93 0. 1.0000 0. 3 -7 -3 3.85 3.78 0. 1.0000 0. -3 7 3 1.78 2.13 0. 1.0000 0. 3 -7 -4 20.35 3.70 0. 1.0000 0. 3 -7 -4 22.53 2.14 0. 1.0000 0. 3 -7 -4 24.31 3.97 0. 1.0000 0. -3 7 4 19.33 2.91 0. 1.0000 0. 3 -7 -5 30.48 3.78 0. 1.0000 0. 3 -7 -5 26.75 2.18 0. 1.0000 0. 3 -7 -5 24.01 3.87 0. 1.0000 0. 3 -7 -6 54.09 4.36 0. 1.0000 0. 3 -7 -6 45.66 2.64 0. 1.0000 0. 3 -7 -7 2.26 2.92 0. 1.0000 0. 3 -7 -7 1.25 1.63 0. 1.0000 0. 3 8 8 1.77 4.08 0. 1.0000 0. 3 8 8 3.11 3.20 0. 1.0000 0. 3 8 8 -1.14 6.44 0. 1.0000 0. 3 8 7 -0.13 3.71 0. 1.0000 0. 3 8 7 -2.48 2.91 0. 1.0000 0. 3 8 7 -3.90 6.89 0. 1.0000 0. 3 8 6 -1.54 3.35 0. 1.0000 0. 3 8 6 1.05 2.59 0. 1.0000 0. 3 8 6 -1.95 7.94 0. 1.0000 0. 3 8 5 -0.94 3.33 0. 1.0000 0. 3 8 5 0.23 2.39 0. 1.0000 0. 3 8 5 5.09 8.09 0. 1.0000 0. 3 8 4 -1.68 3.17 0. 1.0000 0. 3 8 4 2.09 2.41 0. 1.0000 0. 3 8 4 2.83 6.55 0. 1.0000 0. 3 8 3 182.49 7.39 0. 1.0000 0. 3 8 3 169.45 6.74 0. 1.0000 0. 3 8 2 -0.53 3.15 0. 1.0000 0. -3 -8 -2 3.30 4.38 0. 1.0000 0. 3 8 1 172.23 7.45 0. 1.0000 0. 3 8 0 68.12 4.26 0. 1.0000 0. -3 -8 0 3.36 3.47 0. 1.0000 0. -3 8 1 23.61 1.89 0. 1.0000 0. -3 -8 1 0.55 3.00 0. 1.0000 0. -3 8 2 64.27 3.04 0. 1.0000 0. 3 -8 -2 52.88 5.64 0. 1.0000 0. 3 -8 -2 59.87 3.44 0. 1.0000 0. -3 8 3 393.22 12.59 0. 1.0000 0. 3 -8 -3 370.64 14.01 0. 1.0000 0. 3 -8 -3 355.43 12.44 0. 1.0000 0. 3 -8 -4 41.79 2.74 0. 1.0000 0. 3 -8 -4 30.57 3.93 0. 1.0000 0. -3 8 4 43.21 3.27 0. 1.0000 0. 3 -8 -5 2.35 3.61 0. 1.0000 0. 3 -8 -5 1.07 1.75 0. 1.0000 0. 3 -8 -5 3.46 3.83 0. 1.0000 0. -3 8 5 0.93 2.99 0. 1.0000 0. 3 -8 -6 -1.63 3.46 0. 1.0000 0. 3 -8 -6 0.11 1.70 0. 1.0000 0. 3 -8 -6 1.65 3.42 0. 1.0000 0. 3 -8 -7 0.42 3.25 0. 1.0000 0. 3 9 7 7.91 3.75 0. 1.0000 0. 3 9 7 13.54 3.23 0. 1.0000 0. 3 9 6 13.74 3.55 0. 1.0000 0. 3 9 6 -0.23 8.45 0. 1.0000 0. 3 9 5 3.55 3.37 0. 1.0000 0. 3 9 5 7.13 2.47 0. 1.0000 0. 3 9 5 -3.30 7.18 0. 1.0000 0. 3 9 4 50.95 3.32 0. 1.0000 0. 3 9 4 46.84 4.19 0. 1.0000 0. 3 9 3 12.92 3.34 0. 1.0000 0. -3 -9 -3 9.21 5.15 0. 1.0000 0. 3 9 3 9.32 2.47 0. 1.0000 0. 3 9 2 90.49 5.19 0. 1.0000 0. -3 -9 -2 90.52 6.03 0. 1.0000 0. 3 9 1 15.07 3.61 0. 1.0000 0. -3 -9 -1 11.69 3.62 0. 1.0000 0. 3 9 0 -0.83 3.06 0. 1.0000 0. -3 -9 0 -2.25 3.16 0. 1.0000 0. -3 9 1 102.49 4.08 0. 1.0000 0. 3 -9 -1 75.15 6.60 0. 1.0000 0. 3 -9 -2 -5.62 5.00 0. 1.0000 0. -3 9 2 -0.61 1.71 0. 1.0000 0. 3 -9 -3 4.57 2.21 0. 1.0000 0. 3 -9 -3 2.27 4.49 0. 1.0000 0. -3 9 3 5.42 2.02 0. 1.0000 0. 3 -9 -4 15.50 2.29 0. 1.0000 0. 3 -9 -4 13.38 4.01 0. 1.0000 0. -3 9 4 10.49 2.57 0. 1.0000 0. -3 9 5 4.29 3.00 0. 1.0000 0. 3 -9 -6 55.44 4.98 0. 1.0000 0. -3 9 6 53.16 4.52 0. 1.0000 0. 3 10 6 4.43 3.46 0. 1.0000 0. 3 10 6 8.16 2.83 0. 1.0000 0. 3 10 6 6.62 8.23 0. 1.0000 0. 3 10 5 2.82 3.45 0. 1.0000 0. 3 10 5 3.57 2.46 0. 1.0000 0. 3 10 4 4.58 3.30 0. 1.0000 0. 3 10 4 2.37 2.39 0. 1.0000 0. 3 10 3 65.36 4.60 0. 1.0000 0. -3 -10 -3 56.26 6.12 0. 1.0000 0. 3 10 3 62.55 3.63 0. 1.0000 0. 3 10 2 0.32 3.42 0. 1.0000 0. -3 -10 -2 0.47 4.12 0. 1.0000 0. 3 10 1 3.54 3.20 0. 1.0000 0. -3 -10 -1 2.10 3.46 0. 1.0000 0. -3 -10 -1 0.71 3.49 0. 1.0000 0. -3 10 2 152.32 5.66 0. 1.0000 0. 3 -10 -2 118.14 8.04 0. 1.0000 0. -3 10 3 139.92 5.50 0. 1.0000 0. 3 -10 -3 130.77 8.13 0. 1.0000 0. 3 -10 -4 3.54 4.59 0. 1.0000 0. -3 10 4 3.73 2.39 0. 1.0000 0. 3 -10 -5 15.07 4.33 0. 1.0000 0. -3 10 5 13.26 2.95 0. 1.0000 0. 3 11 5 66.40 3.85 0. 1.0000 0. 3 11 5 58.62 4.65 0. 1.0000 0. 3 11 4 1.43 3.38 0. 1.0000 0. -3 -11 -4 -4.08 5.96 0. 1.0000 0. 3 11 4 1.81 2.37 0. 1.0000 0. 3 11 3 34.32 4.08 0. 1.0000 0. -3 -11 -3 30.00 5.44 0. 1.0000 0. 3 11 2 -2.41 3.43 0. 1.0000 0. -3 -11 -2 1.11 3.94 0. 1.0000 0. -3 11 2 -0.28 1.73 0. 1.0000 0. 3 -11 -3 1.09 5.12 0. 1.0000 0. -3 11 3 2.33 2.09 0. 1.0000 0. 3 -11 -4 36.20 5.87 0. 1.0000 0. -3 11 4 35.62 3.02 0. 1.0000 0. 3 12 2 2.29 2.95 0. 1.0000 0. -512 # 2483 reflections output ; # end of ARCHIVE-HKL.CIF _chemical_name_common ROY _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: acetone' ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_ROY_ON_2p41GPa _database_code_depnum_ccdc_archive 'CCDC 2098640' loop_ _audit_author_name _audit_author_address 'Nicholas Funnell' ;STFC, ISIS Neutron Facility United Kingdom ; _audit_update_record ; 2021-07-22 deposited with the CCDC. 2021-08-27 downloaded from the CCDC. ; _audit_creation_date 2021-01-26 _audit_creation_method 'CRYSTALS_ver_14.61_build_7795 ' _chemical_name_systematic ; 5-methyl-2[(2-nitrophenyl)amino]-3-thiophenecarbonitrile ; #CheckCIF alerts _vrf_THETM01_ROY_ON_2p41GPa ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575 RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT027_ROY_ON_2p41GPa ; PROBLEM: _diffrn_reflns_theta_full value (too) Low ...... 17.43 Degree RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT029_ROY_ON_2p41GPa ; PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.727 Why? RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT201_ROY_ON_2p41GPa ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 17 Report RESPONSE: The model could only be refined isotropically in order to maintain a favourable data-to-parameter ratio, due to numerous unmeasured reflections. The relatively electron-rich sulfur atom has been modelled anisotropically. ; _vrf_PLAT911_ROY_ON_2p41GPa ; PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.555 402 Report RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT157_ROY_ON_2p41GPa ; PROBLEM: Non-standard Monoclinic Beta Angle less 90 Deg 89.36 Degree RESPONSE: This is a series of high pressure structures where the beta angle decreases, passing through 90 degrees. The non-standard beta angle allows the change in angle to be followed clearly. ; _vrf_PLAT340_ROY_ON_2p41GPa ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.00809 Ang. RESPONSE: These are poor-quality diffraction data. ; _vrf_PLAT411_ROY_ON_2p41GPa ; PROBLEM: Short Inter H...H Contact H5 ..H5 . 2.11 Ang. RESPONSE: These are high-pressure data - short contacts are expected. ; _vrf_PLAT413_ROY_ON_2p41GPa ; PROBLEM: Short Inter XH3 .. XHn H2 ..H111 . 2.10 Ang. RESPONSE: These are high-pressure data - short contacts are expected. ; _vrf_PLAT910_ROY_ON_2p41GPa ; PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 8 Note RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _refine_special_details ; In the absence of significant anomalous scattering, Friedel pairs were merged. Data were collected in a Merrill-Bassett diamond anvil cell, which significantly restricts the regions over which reciprocal space can be sampled. Thus, these data are poor quality/incomplete, reflected in numerous CheckCIF alerts regarding refinement statistics. At all pressures, the atomic connectivity is known. All non-sulfur atoms were refined isotropically; sulfur was refined anisotropically. Hydrogen atoms were constrained to ride on their host atoms. #=============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Total Missing #------------------------------------------------------------------------------- 20.82 0.500 0.713 1061 756 305 23.01 0.550 0.701 1343 941 402 23.24 0.555 0.700 1366 956 410 ------------------------------------------------------------ ACTA Min. Res. --- Note: The Reported Completeness refers to the Actual H,K,L Index Range ; #end of refcif _cell_length_a 3.59640(2) _cell_length_b 17.60380(6) _cell_length_c 15.95340(6) _cell_angle_alpha 90 _cell_angle_beta 89.358(7) _cell_angle_gamma 90 _cell_volume 1009.951(8) _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' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 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' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C12 H9 N3 O2 S1 # Dc = 1.71 Fooo = 536.00 Mu = 3.17 M = 259.29 # Found Formula = C12 H9 N3 O2 S1 # Dc = 1.71 FOOO = 536.00 Mu = 3.17 M = 259.29 _chemical_formula_sum 'C12 H9 N3 O2 S1' _chemical_formula_moiety 'C12 H9 N3 O2 S1' _chemical_compound_source 'TCI Chemicals' _chemical_formula_weight 259.29 _cell_measurement_reflns_used 1445 _cell_measurement_theta_min 1.71 _cell_measurement_theta_max 23.26 _cell_measurement_temperature 293 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_min 0.050 _exptl_crystal_size_mid 0.072 _exptl_crystal_size_max 0.248 _exptl_crystal_density_diffrn 1.705 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 0.317 # Sheldrick geometric approximatio 0.98 0.98 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North et al., 1968)' _exptl_absorpt_correction_T_min 0.09 _exptl_absorpt_correction_T_max 0.98 _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_device 'four-circle diffractometer' _diffrn_radiation_monochromator mirror _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 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction ; CrysAlisPro (Rigaku Oxford Diffraction, 2017) ; _computing_structure_solution 'Model from previously-determined structure' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 293 _diffrn_ambient_pressure 2410000 _diffrn_reflns_number 2325 _diffrn_reflns_av_unetI/netI 0.045 _reflns_number_total 977 _diffrn_reflns_av_R_equivalents 0.070 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 977 # Theoretical number of reflections is about 2894 _diffrn_reflns_theta_min 1.723 _diffrn_reflns_theta_max 23.236 _diffrn_measured_fraction_theta_max 0.688 _diffrn_reflns_theta_full 17.427 _diffrn_measured_fraction_theta_full 0.727 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_h_max 3 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -3 _reflns_limit_h_max 3 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.77 _refine_diff_density_max 0.74 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # Explicitly named reflections are ALWAYS excluded from R&wR # The values actually used during refinement # These are labelled "all" for compatibility with PLATON _oxford_refine_reflns_threshold_expression I>-3.0\s(I) _refine_ls_number_restraints 94 _refine_ls_number_parameters 82 _refine_ls_number_reflns 956 _oxford_refine_ls_R_factor_ref 0.1507 _refine_ls_R_factor_all 0.1507 _refine_ls_wR_factor_ref 0.0470 _refine_ls_wR_factor_all 0.0470 _refine_ls_goodness_of_fit_ref 1.0101 _refine_ls_shift/su_max 0.0002795 _refine_ls_shift/su_mean 0.0000515 # Computed with I/sigma = -10 _oxford_reflns_number_all 956 _oxford_refine_ls_R_factor_all 0.1507 _oxford_refine_ls_wR_factor_all 0.0470 # Computed with no filters except I/sigma = +2 a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 670 _refine_ls_R_factor_gt 0.1045 _refine_ls_wR_factor_gt 0.0435 _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed #undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ; Method= SQRT(W) = 1/(Data with the key SIGMA(/FO/) in list 6) ; # 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 S1 S 0.6920(3) 0.58857(9) 0.43475(10) 0.0374 1.0000 Uani D U . . . . O1 O 0.4719(9) 0.6333(2) 0.0231(3) 0.0471(12) 1.0000 Uiso D U . . . . O2 O 0.4780(9) 0.7006(2) 0.1379(3) 0.0458(11) 1.0000 Uiso D U . . . . N1 N 0.7757(10) 0.6432(3) 0.2758(3) 0.0371(11) 1.0000 Uiso D U . . . . N2 N 1.3161(11) 0.8078(3) 0.2950(3) 0.0403(13) 1.0000 Uiso D U . . . . N3 N 0.5512(10) 0.6418(3) 0.0964(3) 0.0414(12) 1.0000 Uiso D U . . . . C1 C 0.8414(12) 0.5849(4) 0.2239(4) 0.0367(12) 1.0000 Uiso D U . . . . C2 C 1.0338(14) 0.5217(3) 0.2570(4) 0.0367(13) 1.0000 Uiso D U . . . . C3 C 1.1095(12) 0.4597(3) 0.2068(4) 0.0358(13) 1.0000 Uiso D U . . . . C4 C 0.9997(12) 0.4554(3) 0.1237(4) 0.0359(12) 1.0000 Uiso D U . . . . C5 C 0.8242(12) 0.5175(3) 0.0917(4) 0.0369(12) 1.0000 Uiso D U . . . . C6 C 0.7468(12) 0.5807(3) 0.1403(4) 0.0352(12) 1.0000 Uiso D U . . . . C7 C 0.8338(11) 0.6511(3) 0.3602(4) 0.0354(12) 1.0000 Uiso D U . . . . C8 C 0.9948(12) 0.7161(3) 0.3967(4) 0.0370(13) 1.0000 Uiso D U . . . . C9 C 0.9962(12) 0.7116(3) 0.4829(4) 0.0401(14) 1.0000 Uiso D U . . . . C10 C 0.8407(8) 0.6481(3) 0.5159(4) 0.0412(13) 1.0000 Uiso D U . . . . C11 C 0.8020(8) 0.6215(2) 0.6023(3) 0.0420(15) 1.0000 Uiso D U . . . . C12 C 1.1730(11) 0.7683(4) 0.3416(3) 0.0367(13) 1.0000 Uiso D U . . . . H1 H 0.669(5) 0.6804(15) 0.2528(17) 0.046(3) 1.0000 Uiso D . . . . . H2 H 1.1036 0.5219 0.3127 0.0402 1.0000 Uiso R . . . . . H3 H 1.2448 0.4192 0.2282 0.0450 1.0000 Uiso R . . . . . H4 H 1.0350 0.4108 0.0925 0.0479 1.0000 Uiso R . . . . . H5 H 0.7660 0.5183 0.0351 0.0501 1.0000 Uiso R . . . . . H9 H 1.1022 0.7492 0.5157 0.0480 1.0000 Uiso R . . . . . H111 H 0.9225 0.5734 0.6079 0.0920 1.0000 Uiso DR . . . . . H112 H 0.9119 0.6577 0.6394 0.0920 1.0000 Uiso DR . . . . . H113 H 0.5438 0.6160 0.6163 0.0920 1.0000 Uiso DR . . . . . 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 S1 0.0437(8) 0.0243(14) 0.0444(14) 0.0033(7) -0.0039(7) -0.0025(8) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.4974(15) 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 S1 . C7 . 1.694(6) yes S1 . C10 . 1.754(4) yes O1 . N3 . 1.217(5) yes O2 . N3 . 1.255(5) yes N1 . C1 . 1.338(7) yes N1 . C7 . 1.372(6) yes N1 . H1 . 0.85(3) no N2 . C12 . 1.138(6) yes N3 . C6 . 1.468(7) yes C1 . C2 . 1.415(8) yes C1 . C6 . 1.383(7) yes C2 . C3 . 1.378(6) yes C2 . H2 . 0.927 no C3 . C4 . 1.390(6) yes C3 . H3 . 0.930 no C4 . C5 . 1.365(7) yes C4 . H4 . 0.937 no C5 . C6 . 1.382(7) yes C5 . H5 . 0.930 no C7 . C8 . 1.411(8) yes C8 . C9 . 1.378(6) yes C8 . C12 . 1.419(7) yes C9 . C10 . 1.355(7) yes C9 . H9 . 0.928 no C10 . C11 . 1.459(7) yes C11 . H111 . 0.956 no C11 . H112 . 0.959 no C11 . H113 . 0.957 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 C7 . S1 . C10 . 92.2(3) yes C1 . N1 . C7 . 131.1(6) yes C1 . N1 . H1 . 114(2) no C7 . N1 . H1 . 115.0(20) no O2 . N3 . O1 . 124.0(5) yes O2 . N3 . C6 . 116.9(6) yes O1 . N3 . C6 . 119.1(5) yes N1 . C1 . C2 . 117.2(6) yes N1 . C1 . C6 . 126.5(6) yes C2 . C1 . C6 . 116.3(5) yes C1 . C2 . C3 . 120.0(6) yes C1 . C2 . H2 . 119.5 no C3 . C2 . H2 . 120.5 no C2 . C3 . C4 . 122.8(6) yes C2 . C3 . H3 . 119.7 no C4 . C3 . H3 . 117.5 no C3 . C4 . C5 . 116.7(6) yes C3 . C4 . H4 . 120.9 no C5 . C4 . H4 . 122.3 no C4 . C5 . C6 . 121.8(6) yes C4 . C5 . H5 . 119.0 no C6 . C5 . H5 . 119.1 no N3 . C6 . C1 . 123.0(5) yes N3 . C6 . C5 . 114.7(6) yes C1 . C6 . C5 . 122.3(6) yes N1 . C7 . S1 . 125.1(4) yes N1 . C7 . C8 . 123.7(5) yes S1 . C7 . C8 . 111.1(5) yes C7 . C8 . C9 . 111.8(5) yes C7 . C8 . C12 . 117.0(6) yes C9 . C8 . C12 . 130.4(6) yes C8 . C9 . C10 . 115.5(5) yes C8 . C9 . H9 . 121.9 no C10 . C9 . H9 . 122.6 no S1 . C10 . C9 . 109.5(5) yes S1 . C10 . C11 . 118.6(2) yes C9 . C10 . C11 . 131.8(4) yes C10 . C11 . H111 . 109.5 no C10 . C11 . H112 . 109.6 no H111 . C11 . H112 . 109.9 no C10 . C11 . H113 . 109.5 no H111 . C11 . H113 . 109.2 no H112 . C11 . H113 . 109.1 no C8 . C12 . N2 . 177.2(9) yes _iucr_refine_instructions_details ; # # Punched on 26/01/21 at 11:42:46 # #LIST 12 BLOCK CONT SCALE CONT S ( 1 ,X'S,U'S) CONT O ( 1 ,X'S,U[ISO]) UNTIL H ( 1 ) RIDE C ( 2,X'S) H ( 2,X'S) RIDE C ( 3,X'S) H ( 3,X'S) RIDE C ( 4,X'S) H ( 4,X'S) RIDE C ( 5,X'S) H ( 5,X'S) RIDE C ( 9,X'S) H ( 9,X'S) RIDE C ( 11,X'S) H ( 111,X'S) H ( 112,X'S) H ( 113,X'S) END # # Punched on 26/01/21 at 11:42:46 # #LIST 16 NO REM REM NPF NOTE - FIRST UNTIL LAST REM REM HREST START (DO NOT REMOVE THIS LINE) REM NO H NO #H U MULT DIST REM C-H REM >4 1.5 .96 DISORDER REM 1 1 1.2 .93 C C-H (ACETYLENE) REM 1 2 1.2 .93 C-C(H)-C REM 1 3 1.2 .98 (C)3-C-H REM 2 1 1.2 .93 C=C-H(2) REM 2 2 1.2 .97 (C)2-C-(H)2 REM 3 1 1.5 .96 C-C-(H)3 REM N-H REM >4 1.5 .89 DISORDER REM 1 1 1.2 .86 N-N/H REM 1 2 1.2 .86 (C)2-N-H REM 1 3 1.2 .89 (C)3-N-H REM 2 1 1.2 .86 C-N-(H)2 REM 2 2 1.2 .89 (C)2-N-(H)2 REM 3 1 1.2 .89 C-H-(H)3 REM O-H REM 1 1 1.5 .82 O-H REM REM DIST ESD = 0.02 REM VIB ESD = 0.002 REM ANGLE ESD = 2.0 REM REM TO ACTIVATE THE VIB RESTRAINTS, REMOVE LEADING REM REM H1-N-R2 DIST 0.86, 0.02 = CONT N ( 1) TO H(1) REST 0.046, 0.002 = H(1,U[ISO]) ANGLE 0.0, 2.0 = MEAN CONT H(1) TO N ( 1) TO C(1) CONT H(1) TO N ( 1) TO C(7) REM HREST END (DO NOT REMOVE THIS LINE) REM DELU START (DO NOT REMOVE THIS LINE) VIBR .0, 0.00200 = S(1) TO C(10) VIBR .0, 0.00200 = S(1) TO C(7) VIBR .0, 0.00500 = C(7) TO C(10) VIBR .0, 0.00200 = N(2) TO C(12) VIBR .0, 0.00200 = C(10) TO C(9) VIBR .0, 0.00200 = C(10) TO C(11) VIBR .0, 0.00500 = C(9) TO S(1) VIBR .0, 0.00500 = C(11) TO S(1) VIBR .0, 0.00500 = C(11) TO C(9) VIBR .0, 0.00200 = C(12) TO C(8) VIBR .0, 0.00500 = C(8) TO N(2) VIBR .0, 0.00200 = O(1) TO N(3) VIBR .0, 0.00200 = C(2) TO C(1) VIBR .0, 0.00200 = C(2) TO C(3) VIBR .0, 0.00500 = C(3) TO C(1) VIBR .0, 0.00200 = N(1) TO C(7) VIBR .0, 0.00200 = N(1) TO C(1) VIBR .0, 0.00500 = C(1) TO C(7) VIBR .0, 0.00200 = C(7) TO C(8) VIBR .0, 0.00500 = N(1) TO S(1) VIBR .0, 0.00500 = C(8) TO S(1) VIBR .0, 0.00500 = C(8) TO N(1) VIBR .0, 0.00200 = O(2) TO N(3) VIBR .0, 0.00200 = N(3) TO C(6) VIBR .0, 0.00500 = O(1) TO O(2) VIBR .0, 0.00500 = C(6) TO O(2) VIBR .0, 0.00500 = C(6) TO O(1) VIBR .0, 0.00200 = C(5) TO C(4) VIBR .0, 0.00200 = C(5) TO C(6) VIBR .0, 0.00500 = C(6) TO C(4) VIBR .0, 0.00200 = C(4) TO C(3) VIBR .0, 0.00500 = C(3) TO C(5) VIBR .0, 0.00200 = C(1) TO C(6) VIBR .0, 0.00500 = N(1) TO C(2) VIBR .0, 0.00500 = C(6) TO C(2) VIBR .0, 0.00500 = C(6) TO N(1) VIBR .0, 0.00500 = C(5) TO N(3) VIBR .0, 0.00500 = C(1) TO N(3) VIBR .0, 0.00500 = C(1) TO C(5) VIBR .0, 0.00200 = C(9) TO C(8) VIBR .0, 0.00500 = C(8) TO C(10) VIBR .0, 0.00500 = C(2) TO C(4) VIBR .0, 0.00500 = C(12) TO C(9) VIBR .0, 0.00500 = C(7) TO C(9) VIBR .0, 0.00500 = C(7) TO C(12) REM DELU END (DO NOT REMOVE THIS LINE) ANGLE 110.000000 , 0.020000 = C(10) TO C(11) TO H(111) ANGLE 110.000000 , 0.020000 = C(10) TO C(11) TO H(112) ANGLE 110.000000 , 0.020000 = C(10) TO C(11) TO H(113) DISTANCE 1.225000 , 0.050000 = O(2) TO N(3) DISTANCE 1.225000 , 0.050000 = O(1) TO N(3) DISTANCE 1.440000 , 0.050000 = C(6) TO N(3) DISTANCE 1.390000 , 0.050000 = C(5) TO C(6) DISTANCE 1.364000 , 0.050000 = C(4) TO C(5) DISTANCE 1.222000 , 0.050000 = O(1) TO N(3) DISTANCE 1.232000 , 0.050000 = O(2) TO N(3) DISTANCE 1.440000 , 0.050000 = C(6) TO N(3) DISTANCE 1.392000 , 0.050000 = C(5) TO C(6) DISTANCE 1.364000 , 0.050000 = C(4) TO C(5) DISTANCE 1.391000 , 0.050000 = C(3) TO C(4) DISTANCE 1.371000 , 0.050000 = C(2) TO C(3) DISTANCE 1.400000 , 0.050000 = C(1) TO C(2) DISTANCE 1.408000 , 0.050000 = C(1) TO C(6) DISTANCE 1.382000 , 0.050000 = C(1) TO N(1) DISTANCE 1.387000 , 0.050000 = C(7) TO N(1) DISTANCE 1.728000 , 0.050000 = S(1) TO C(7) DISTANCE 1.724000 , 0.050000 = S(1) TO C(10) DISTANCE 1.500000 , 0.050000 = C(10) TO C(11) DISTANCE 1.349000 , 0.050000 = C(9) TO C(10) DISTANCE 1.427000 , 0.050000 = C(8) TO C(9) DISTANCE 1.372000 , 0.050000 = C(7) TO C(8) DISTANCE 1.422000 , 0.050000 = C(8) TO C(12) DISTANCE 1.141000 , 0.050000 = C(12) TO N(2) REM THERMSIM START (DO NOT REMOVE THIS LINE) U(IJ) .0, 0.04000 = S(1) TO C(7) U(IJ) .0, 0.04000 = S(1) TO C(10) U(IJ) .0, 0.08000 = O(1) TO N(3) U(IJ) .0, 0.08000 = O(2) TO N(3) U(IJ) .0, 0.04000 = C(1) TO C(2) U(IJ) .0, 0.04000 = C(1) TO C(6) U(IJ) .0, 0.04000 = C(1) TO N(1) U(IJ) .0, 0.04000 = C(2) TO C(3) U(IJ) .0, 0.04000 = C(3) TO C(4) U(IJ) .0, 0.04000 = C(4) TO C(5) U(IJ) .0, 0.04000 = C(5) TO C(6) U(IJ) .0, 0.04000 = C(6) TO N(3) U(IJ) .0, 0.04000 = C(7) TO C(8) U(IJ) .0, 0.04000 = C(7) TO N(1) U(IJ) .0, 0.04000 = C(8) TO C(9) U(IJ) .0, 0.04000 = C(8) TO C(12) U(IJ) .0, 0.04000 = C(9) TO C(10) U(IJ) .0, 0.08000 = C(10) TO C(11) U(IJ) .0, 0.08000 = C(12) TO N(2) REM THERMSIM END (DO NOT REMOVE THIS LINE) PLANAR 0.010000 C(1) C(6) N(1) H(1) PLANAR 0.010000 C(1) C(2) C(3) C(4) C(5) C(6) N(1) N(3) PLANAR 0.010000 S(1) C(7) C(8) C(9) C(10) N(1) 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 0 5 1 x . 3 8 0 x . 0 11 3 x . 1 13 4 x . 3 7 1 x . 2 6 12 x . -3 1 7 x . 3 10 0 x . 1 8 1 x . 2 0 6 x . 0 13 4 x . -1 3 9 x . 2 10 1 x . 2 10 1 x . 0 6 1 x . -2 12 3 x . 1 3 9 x . # looking for ARCHIVE-HKL.CIF _iucr_refine_reflections_details ; # Data was input as F-squared # punching LIST 6 as LIST 6 with all keys set # NBGNXT= 36 #LIST 6 READ NCOEF= 8 TYPE=FIX, F'S = FSQ UNIT=DATA, CHECK=NO L30=NO ARCH=NO STORE NCOEF= 6 OUTPUT INDICES /FO/ SIGMA(/FO/) RATIO/JCODE CORRECTIONS SERIAL CONT INPUT H K L /FO/ SIGMA(/FO/) JCODE CONT CORRECTIONS SERIAL FOR (I4,I4,I4,F10.2,F8.2,F4.0,F7.4,F7.0) END 0 1 1 6.31 0.34 0. 1.0000 0. 0 -1 -2 87.18 2.15 0. 1.0000 0. 0 2 1 1657.60 17.62 0. 1.0000 0. 0 2 1 1675.59 17.60 0. 1.0000 0. 0 2 2 120.80 2.11 0. 1.0000 0. 0 -2 -2 109.08 2.38 0. 1.0000 0. 0 2 2 99.99 2.08 0. 1.0000 0. 0 2 2 98.38 1.99 0. 1.0000 0. 0 2 2 110.86 1.97 0. 1.0000 0. 0 -2 -2 106.03 2.27 0. 1.0000 0. 0 -2 -3 736.95 9.91 0. 1.0000 0. 0 -2 -3 706.03 9.37 0. 1.0000 0. 0 2 3 662.20 10.47 0. 1.0000 0. 0 -2 -4 37.90 1.89 0. 1.0000 0. 0 -2 -6 820.86 14.33 0. 1.0000 0. 0 3 1 453.38 6.76 0. 1.0000 0. 0 3 1 474.26 6.94 0. 1.0000 0. 0 3 1 475.39 7.73 0. 1.0000 0. 0 -3 -2 55.50 1.91 0. 1.0000 0. 0 -3 -2 48.99 2.45 0. 1.0000 0. 0 3 2 52.07 1.36 0. 1.0000 0. 0 3 2 33.18 2.49 0. 1.0000 0. 0 3 2 55.43 1.60 0. 1.0000 0. 0 -3 -2 56.97 2.09 0. 1.0000 0. 0 -3 -2 63.35 1.64 0. 1.0000 0. 0 3 2 50.61 1.27 0. 1.0000 0. 0 3 2 53.40 1.42 0. 1.0000 0. 0 3 3 2.20 0.60 0. 1.0000 0. 0 -3 -3 2.44 0.96 0. 1.0000 0. 0 3 3 1.97 0.84 0. 1.0000 0. 0 -3 -3 2.15 0.54 0. 1.0000 0. 0 3 3 2.44 0.60 0. 1.0000 0. 0 -3 -3 2.50 0.69 0. 1.0000 0. 0 3 3 2.01 0.90 0. 1.0000 0. 0 3 3 2.65 0.68 0. 1.0000 0. 0 3 3 1.87 0.77 0. 1.0000 0. 0 3 4 160.09 3.36 0. 1.0000 0. 0 -3 -4 152.73 2.43 0. 1.0000 0. 0 -3 -4 145.22 2.99 0. 1.0000 0. 0 -3 -5 59.30 1.91 0. 1.0000 0. 0 -3 -5 58.01 2.32 0. 1.0000 0. 0 3 5 53.71 2.14 0. 1.0000 0. 0 -3 -6 94.82 2.77 0. 1.0000 0. 0 -3 -6 96.13 3.46 0. 1.0000 0. 0 -3 -7 1.45 1.79 0. 1.0000 0. 0 -3 -7 1.32 1.19 0. 1.0000 0. 0 -3 -8 9.66 2.26 0. 1.0000 0. 0 -4 -1 0.31 0.99 0. 1.0000 0. 0 -4 -1 0.48 0.75 0. 1.0000 0. 0 -4 -2 644.82 12.74 0. 1.0000 0. 0 4 2 620.11 8.79 0. 1.0000 0. 0 -4 -2 641.11 10.37 0. 1.0000 0. 0 -4 -2 569.56 10.39 0. 1.0000 0. 0 -4 -2 632.90 8.55 0. 1.0000 0. 0 -4 -2 619.42 8.62 0. 1.0000 0. 0 4 2 627.72 8.94 0. 1.0000 0. 0 4 3 60.77 1.59 0. 1.0000 0. 0 4 3 61.04 1.87 0. 1.0000 0. 0 4 3 58.71 1.75 0. 1.0000 0. 0 -4 -3 73.25 1.96 0. 1.0000 0. 0 4 3 57.54 1.07 0. 1.0000 0. 0 4 3 59.59 1.70 0. 1.0000 0. 0 4 3 49.67 3.61 0. 1.0000 0. 0 -4 -3 56.23 3.05 0. 1.0000 0. 0 -4 -3 74.37 2.60 0. 1.0000 0. 0 -4 -4 37.03 2.10 0. 1.0000 0. 0 -4 -4 38.51 1.43 0. 1.0000 0. 0 4 4 47.31 1.85 0. 1.0000 0. 0 4 4 48.16 2.45 0. 1.0000 0. 0 4 4 41.21 1.76 0. 1.0000 0. 0 -4 -5 553.44 7.12 0. 1.0000 0. 0 4 5 574.61 8.64 0. 1.0000 0. 0 4 6 77.87 2.86 0. 1.0000 0. 0 -4 -6 84.48 2.59 0. 1.0000 0. 0 -4 -6 85.77 1.95 0. 1.0000 0. 0 -4 -7 176.70 4.85 0. 1.0000 0. 0 -4 -7 172.83 4.67 0. 1.0000 0. 0 4 7 147.67 4.55 0. 1.0000 0. 0 -4 -7 189.37 4.20 0. 1.0000 0. 0 -4 -8 2.42 1.53 0. 1.0000 0. 0 -4 -8 3.20 1.72 0. 1.0000 0. 0 4 8 1.91 1.77 0. 1.0000 0. 0 4 9 11.11 2.35 0. 1.0000 0. 0 -4 -9 157.85 5.28 0. 1.0000 0. 0 4 10 -0.54 1.97 0. 1.0000 0. 0 -4 -10 1.69 2.75 0. 1.0000 0. 0 -5 -1 73.79 2.52 0. 1.0000 0. 0 5 2 685.05 10.53 0. 1.0000 0. 0 -5 -2 711.03 9.94 0. 1.0000 0. 0 -5 -3 291.25 6.12 0. 1.0000 0. 0 -5 -3 232.49 5.49 0. 1.0000 0. 0 -5 -3 285.63 5.89 0. 1.0000 0. 0 5 3 255.04 4.62 0. 1.0000 0. 0 5 3 283.00 5.14 0. 1.0000 0. 0 -5 -4 534.74 8.83 0. 1.0000 0. 0 -5 -4 478.23 10.48 0. 1.0000 0. 0 5 4 511.13 7.68 0. 1.0000 0. 0 5 5 296.72 5.80 0. 1.0000 0. 0 5 5 326.96 8.26 0. 1.0000 0. 0 5 5 279.13 5.86 0. 1.0000 0. 0 -5 -6 12.77 1.78 0. 1.0000 0. 0 5 6 17.12 2.10 0. 1.0000 0. 0 -5 -6 13.44 0.76 0. 1.0000 0. 0 5 6 12.97 1.56 0. 1.0000 0. 0 -5 -7 286.51 5.38 0. 1.0000 0. 0 -5 -7 307.65 4.25 0. 1.0000 0. 0 -5 -8 17.68 2.48 0. 1.0000 0. 0 -5 -8 15.27 1.75 0. 1.0000 0. 0 5 8 8.45 1.91 0. 1.0000 0. 0 -5 -8 12.69 1.18 0. 1.0000 0. 0 -5 -9 241.69 5.95 0. 1.0000 0. 0 5 9 121.49 4.94 0. 1.0000 0. 0 5 10 0.89 2.85 0. 1.0000 0. 0 -5 -10 -0.15 1.94 0. 1.0000 0. 0 5 11 0.38 3.00 0. 1.0000 0. 0 -5 -11 1.91 2.38 0. 1.0000 0. 0 -6 -1 -0.12 0.76 0. 1.0000 0. 0 -6 -2 130.89 3.36 0. 1.0000 0. 0 -6 -3 185.83 2.62 0. 1.0000 0. 0 -6 -3 217.95 6.02 0. 1.0000 0. 0 6 3 192.33 4.42 0. 1.0000 0. 0 6 4 112.06 1.88 0. 1.0000 0. 0 6 4 109.84 3.07 0. 1.0000 0. 0 -6 -4 108.48 3.84 0. 1.0000 0. 0 -6 -5 31.55 2.43 0. 1.0000 0. 0 6 5 16.71 3.03 0. 1.0000 0. 0 6 6 41.96 1.12 0. 1.0000 0. 0 6 6 48.22 4.56 0. 1.0000 0. 0 6 6 43.33 2.60 0. 1.0000 0. 0 -6 -6 40.02 3.30 0. 1.0000 0. 0 -6 -7 159.75 5.40 0. 1.0000 0. 0 -6 -7 147.56 3.80 0. 1.0000 0. 0 6 7 163.92 4.63 0. 1.0000 0. 0 6 8 281.06 6.59 0. 1.0000 0. 0 -6 -8 328.61 4.72 0. 1.0000 0. 0 6 8 326.09 7.84 0. 1.0000 0. 0 -6 -8 365.27 7.24 0. 1.0000 0. 0 -6 -8 321.76 6.24 0. 1.0000 0. 0 -6 -8 386.23 9.06 0. 1.0000 0. 0 -6 -9 44.14 3.69 0. 1.0000 0. 0 -6 -9 38.43 2.27 0. 1.0000 0. 0 -6 -10 132.60 3.89 0. 1.0000 0. 0 -6 -10 143.60 4.87 0. 1.0000 0. 0 -6 -11 4.60 3.16 0. 1.0000 0. 0 6 11 0.47 2.26 0. 1.0000 0. 0 -6 -11 4.62 2.21 0. 1.0000 0. 0 6 12 -0.29 2.30 0. 1.0000 0. 0 -6 -12 1.05 3.28 0. 1.0000 0. 0 -7 -2 2.47 1.54 0. 1.0000 0. 0 -7 -3 1918.85 24.74 0. 1.0000 0. 0 7 3 1867.36 25.98 0. 1.0000 0. 0 7 4 643.19 10.45 0. 1.0000 0. 0 7 4 569.44 9.96 0. 1.0000 0. 0 -7 -4 621.62 11.31 0. 1.0000 0. 0 -7 -5 411.10 8.46 0. 1.0000 0. 0 7 5 403.48 7.00 0. 1.0000 0. 0 7 5 373.91 6.80 0. 1.0000 0. 0 7 6 12.96 1.92 0. 1.0000 0. 0 7 6 12.84 1.98 0. 1.0000 0. 0 -7 -6 12.88 4.09 0. 1.0000 0. 0 7 7 228.38 5.70 0. 1.0000 0. 0 -7 -7 232.28 7.90 0. 1.0000 0. 0 7 7 213.08 2.70 0. 1.0000 0. 0 -7 -8 71.18 4.78 0. 1.0000 0. 0 7 8 66.94 3.55 0. 1.0000 0. 0 -7 -8 66.36 2.99 0. 1.0000 0. 0 -7 -9 93.96 5.04 0. 1.0000 0. 0 -7 -9 95.90 3.34 0. 1.0000 0. 0 7 9 85.05 3.88 0. 1.0000 0. 0 -7 -10 312.41 5.71 0. 1.0000 0. 0 -7 -10 325.83 8.28 0. 1.0000 0. 0 -7 -11 370.32 7.94 0. 1.0000 0. 0 -7 -11 369.91 7.01 0. 1.0000 0. 0 -7 -12 50.75 4.11 0. 1.0000 0. 0 -7 -12 54.50 3.22 0. 1.0000 0. 0 -7 -12 64.19 5.16 0. 1.0000 0. 0 7 13 -0.27 3.08 0. 1.0000 0. 0 -7 -13 1.20 2.07 0. 1.0000 0. 0 -8 -2 140.39 4.26 0. 1.0000 0. 0 -8 -3 504.37 8.58 0. 1.0000 0. 0 -8 -4 53.79 3.72 0. 1.0000 0. 0 8 4 45.72 3.01 0. 1.0000 0. 0 8 4 51.02 2.80 0. 1.0000 0. 0 8 5 33.46 1.11 0. 1.0000 0. 0 8 5 34.26 2.77 0. 1.0000 0. 0 -8 -5 44.03 3.46 0. 1.0000 0. 0 -8 -5 31.83 4.31 0. 1.0000 0. 0 8 5 35.89 2.43 0. 1.0000 0. 0 -8 -6 17.47 2.70 0. 1.0000 0. 0 8 6 17.57 2.21 0. 1.0000 0. 0 -8 -6 5.62 4.20 0. 1.0000 0. 0 -8 -6 13.83 2.94 0. 1.0000 0. 0 8 6 15.12 2.17 0. 1.0000 0. 0 8 7 50.34 2.91 0. 1.0000 0. 0 -8 -7 49.80 6.38 0. 1.0000 0. 0 8 7 57.28 3.45 0. 1.0000 0. 0 -8 -8 13.55 4.67 0. 1.0000 0. 0 8 8 17.10 2.48 0. 1.0000 0. 0 -8 -9 2.06 4.26 0. 1.0000 0. 0 -8 -10 31.27 5.45 0. 1.0000 0. 0 -8 -11 2.91 3.91 0. 1.0000 0. 0 -8 -11 2.13 2.26 0. 1.0000 0. 0 8 11 1.06 3.02 0. 1.0000 0. 0 -8 -12 86.59 3.95 0. 1.0000 0. 0 8 12 31.44 3.90 0. 1.0000 0. 0 -8 -13 178.14 5.50 0. 1.0000 0. 0 8 14 -0.91 3.24 0. 1.0000 0. 0 -8 -14 1.07 2.40 0. 1.0000 0. 0 -9 -2 0.83 1.77 0. 1.0000 0. 0 -9 -3 9.44 2.18 0. 1.0000 0. 0 -9 -4 1828.58 28.27 0. 1.0000 0. 0 9 5 43.48 3.22 0. 1.0000 0. 0 -9 -5 55.51 4.11 0. 1.0000 0. 0 9 5 43.12 1.38 0. 1.0000 0. 0 9 5 49.53 2.88 0. 1.0000 0. 0 9 6 314.80 6.90 0. 1.0000 0. 0 -9 -6 299.02 10.06 0. 1.0000 0. 0 9 6 340.17 7.69 0. 1.0000 0. 0 -9 -6 351.18 8.34 0. 1.0000 0. 0 -9 -7 81.91 5.22 0. 1.0000 0. 0 9 7 79.61 3.69 0. 1.0000 0. 0 9 7 86.17 3.95 0. 1.0000 0. 0 9 8 20.56 3.18 0. 1.0000 0. 0 9 8 21.76 2.74 0. 1.0000 0. 0 -9 -8 15.44 5.71 0. 1.0000 0. 0 -9 -8 21.10 3.43 0. 1.0000 0. 0 9 9 28.91 3.04 0. 1.0000 0. 0 -9 -9 18.99 6.69 0. 1.0000 0. 0 -9 -10 250.47 11.09 0. 1.0000 0. 0 9 10 233.59 6.17 0. 1.0000 0. 0 -9 -11 7.28 5.54 0. 1.0000 0. 0 9 11 6.39 3.24 0. 1.0000 0. 0 -9 -12 213.12 9.64 0. 1.0000 0. 0 9 12 137.88 5.60 0. 1.0000 0. 0 -9 -13 32.78 5.95 0. 1.0000 0. 0 -9 -14 5.37 5.43 0. 1.0000 0. 0 -9 -14 1.39 2.96 0. 1.0000 0. 0 9 14 0.87 3.74 0. 1.0000 0. 0 -9 -15 -0.20 4.28 0. 1.0000 0. 0 -9 -15 1.57 2.59 0. 1.0000 0. 0 -10 -3 23.51 2.76 0. 1.0000 0. 0 -10 -4 18.78 1.01 0. 1.0000 0. 0 -10 -4 24.81 4.27 0. 1.0000 0. 0 10 5 73.65 3.95 0. 1.0000 0. 0 -10 -5 65.25 4.65 0. 1.0000 0. 0 10 6 107.70 3.92 0. 1.0000 0. 0 10 6 108.57 4.81 0. 1.0000 0. 0 10 6 116.09 2.31 0. 1.0000 0. 0 -10 -6 135.71 5.74 0. 1.0000 0. 0 10 7 17.14 2.65 0. 1.0000 0. 0 -10 -7 14.92 5.35 0. 1.0000 0. 0 10 7 17.51 3.40 0. 1.0000 0. 0 10 8 130.09 4.99 0. 1.0000 0. 0 -10 -8 123.45 6.92 0. 1.0000 0. 0 10 8 141.07 5.53 0. 1.0000 0. 0 -10 -9 14.57 4.67 0. 1.0000 0. 0 -10 -9 9.63 6.85 0. 1.0000 0. 0 -10 -10 18.27 6.57 0. 1.0000 0. 0 10 10 25.21 3.38 0. 1.0000 0. 0 -10 -10 30.47 4.24 0. 1.0000 0. 0 -10 -11 116.28 10.81 0. 1.0000 0. 0 10 11 95.32 4.74 0. 1.0000 0. 0 -10 -12 14.32 6.73 0. 1.0000 0. 0 10 12 5.34 3.27 0. 1.0000 0. 0 10 13 111.42 5.35 0. 1.0000 0. 0 -10 -14 23.97 7.42 0. 1.0000 0. 0 10 14 5.60 4.06 0. 1.0000 0. 0 10 15 0.92 3.93 0. 1.0000 0. 0 -10 -15 3.59 6.42 0. 1.0000 0. 0 -11 -3 1.16 2.41 0. 1.0000 0. 0 -11 -4 6.72 3.00 0. 1.0000 0. 0 -11 -4 3.52 4.36 0. 1.0000 0. 0 -11 -4 6.60 1.01 0. 1.0000 0. 0 -11 -5 80.93 5.39 0. 1.0000 0. 0 11 5 75.84 4.18 0. 1.0000 0. 0 11 6 75.59 3.88 0. 1.0000 0. 0 -11 -6 88.80 5.53 0. 1.0000 0. 0 -11 -7 60.20 4.79 0. 1.0000 0. 0 11 7 52.98 4.25 0. 1.0000 0. 0 11 7 58.94 3.80 0. 1.0000 0. 0 -11 -8 8.02 5.79 0. 1.0000 0. 0 11 8 5.49 3.31 0. 1.0000 0. 0 11 8 6.22 3.48 0. 1.0000 0. 0 11 9 252.48 7.93 0. 1.0000 0. 0 -11 -9 260.30 10.37 0. 1.0000 0. 0 11 9 259.87 7.39 0. 1.0000 0. 0 -11 -10 13.56 7.77 0. 1.0000 0. 0 11 10 16.95 3.76 0. 1.0000 0. 0 -11 -10 21.21 5.45 0. 1.0000 0. 0 -11 -11 8.54 4.49 0. 1.0000 0. 0 -11 -11 2.16 7.06 0. 1.0000 0. 0 11 11 6.05 3.41 0. 1.0000 0. 0 -11 -12 46.68 5.40 0. 1.0000 0. 0 -11 -12 29.15 8.08 0. 1.0000 0. 0 11 12 38.69 4.13 0. 1.0000 0. 0 11 13 1.93 3.62 0. 1.0000 0. 0 -11 -13 0.80 8.38 0. 1.0000 0. 0 -11 -14 -4.73 8.40 0. 1.0000 0. 0 11 14 -0.41 4.05 0. 1.0000 0. 0 -12 -3 0.99 2.06 0. 1.0000 0. 0 -12 -4 4.27 1.13 0. 1.0000 0. 0 -12 -4 2.42 4.36 0. 1.0000 0. 0 -12 -4 3.06 3.17 0. 1.0000 0. 0 12 5 2.61 2.62 0. 1.0000 0. 0 -12 -5 3.56 4.08 0. 1.0000 0. 0 12 6 93.37 4.55 0. 1.0000 0. 0 -12 -6 111.31 6.86 0. 1.0000 0. 0 -12 -7 4.60 3.61 0. 1.0000 0. 0 12 7 3.97 2.61 0. 1.0000 0. 0 12 8 210.85 6.73 0. 1.0000 0. 0 12 8 175.16 6.99 0. 1.0000 0. 0 12 9 6.17 3.74 0. 1.0000 0. 0 12 9 2.85 3.74 0. 1.0000 0. 0 -12 -9 8.75 6.42 0. 1.0000 0. 0 12 10 186.46 7.22 0. 1.0000 0. 0 -12 -10 181.44 10.38 0. 1.0000 0. 0 -12 -11 121.51 8.53 0. 1.0000 0. 0 12 11 113.30 5.83 0. 1.0000 0. 0 -12 -12 22.89 6.09 0. 1.0000 0. 0 12 12 23.21 4.25 0. 1.0000 0. 0 12 13 1.45 3.93 0. 1.0000 0. 0 -12 -13 0.93 5.25 0. 1.0000 0. 0 -12 -13 3.36 7.81 0. 1.0000 0. 0 -13 -4 -1.47 4.49 0. 1.0000 0. 0 -13 -4 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-3 6 3 4.41 3.73 0. 1.0000 0. -3 6 3 8.85 6.82 0. 1.0000 0. -3 -6 3 0.09 3.95 0. 1.0000 0. 3 -6 -6 43.37 9.95 0. 1.0000 0. -3 6 6 17.57 6.81 0. 1.0000 0. 3 -6 -7 5.67 9.87 0. 1.0000 0. 3 -6 -7 0.55 3.15 0. 1.0000 0. 3 -6 -8 12.56 8.76 0. 1.0000 0. 3 -6 -9 -1.74 7.73 0. 1.0000 0. 3 -6 -10 6.05 7.04 0. 1.0000 0. 3 7 9 9.22 5.65 0. 1.0000 0. 3 7 8 2.57 5.40 0. 1.0000 0. 3 7 7 2.98 5.09 0. 1.0000 0. 3 7 7 -1.57 5.18 0. 1.0000 0. 3 7 6 34.86 5.20 0. 1.0000 0. 3 7 6 29.93 5.76 0. 1.0000 0. 3 7 5 13.59 4.70 0. 1.0000 0. 3 7 5 12.95 5.72 0. 1.0000 0. 3 7 4 42.86 5.35 0. 1.0000 0. 3 7 4 27.73 5.55 0. 1.0000 0. 3 7 3 62.40 5.06 0. 1.0000 0. 3 7 3 51.46 6.48 0. 1.0000 0. 3 7 2 4.64 4.16 0. 1.0000 0. -3 7 -1 0.40 3.40 0. 1.0000 0. 3 -7 1 0.06 4.38 0. 1.0000 0. 3 7 0 22.93 4.90 0. 1.0000 0. -3 -7 0 10.09 4.78 0. 1.0000 0. 3 -7 0 18.44 5.26 0. 1.0000 0. -3 7 0 26.88 3.77 0. 1.0000 0. -3 7 0 17.69 7.33 0. 1.0000 0. 3 -7 -1 75.26 6.18 0. 1.0000 0. -3 -7 1 0.15 3.20 0. 1.0000 0. -3 7 1 48.59 9.73 0. 1.0000 0. -3 -7 1 2.61 5.20 0. 1.0000 0. -3 7 1 69.86 4.10 0. 1.0000 0. -3 7 2 5.55 7.91 0. 1.0000 0. -3 7 2 7.50 3.34 0. 1.0000 0. -3 -7 2 -1.48 4.64 0. 1.0000 0. 3 -7 -2 7.82 5.13 0. 1.0000 0. -3 7 3 88.97 5.38 0. 1.0000 0. -3 7 4 24.74 4.50 0. 1.0000 0. -3 7 5 0.60 6.86 0. 1.0000 0. -3 7 6 7.08 6.86 0. 1.0000 0. 3 -7 -7 1.44 9.85 0. 1.0000 0. -3 7 7 -1.72 6.77 0. 1.0000 0. 3 -7 -8 20.92 10.35 0. 1.0000 0. -3 7 8 9.42 7.02 0. 1.0000 0. 3 -7 -9 -2.53 9.15 0. 1.0000 0. 3 8 9 5.74 5.92 0. 1.0000 0. 3 8 8 3.23 5.70 0. 1.0000 0. 3 8 7 5.79 4.94 0. 1.0000 0. 3 8 7 5.95 5.80 0. 1.0000 0. 3 8 6 3.87 4.55 0. 1.0000 0. 3 8 6 2.78 5.91 0. 1.0000 0. 3 8 5 18.51 5.41 0. 1.0000 0. 3 8 5 10.27 5.45 0. 1.0000 0. 3 8 4 5.02 4.52 0. 1.0000 0. 3 8 4 6.67 5.56 0. 1.0000 0. 3 8 3 146.03 6.76 0. 1.0000 0. 3 8 2 8.86 4.70 0. 1.0000 0. -3 -8 -2 3.51 4.73 0. 1.0000 0. 3 8 1 19.31 4.73 0. 1.0000 0. -3 -8 -1 4.84 4.89 0. 1.0000 0. 3 -8 0 -0.30 4.45 0. 1.0000 0. -3 -8 0 6.04 5.39 0. 1.0000 0. 3 -8 -1 27.73 5.39 0. 1.0000 0. 3 8 -1 25.09 6.73 0. 1.0000 0. -3 8 1 41.28 4.39 0. 1.0000 0. -3 8 1 18.58 7.54 0. 1.0000 0. -3 8 2 27.46 9.62 0. 1.0000 0. 3 -8 -2 47.37 6.12 0. 1.0000 0. -3 8 2 42.66 4.16 0. 1.0000 0. -3 8 3 446.00 10.96 0. 1.0000 0. -3 8 4 26.35 8.92 0. 1.0000 0. -3 8 4 44.86 5.29 0. 1.0000 0. -3 8 5 0.68 4.32 0. 1.0000 0. -3 8 5 -0.96 8.13 0. 1.0000 0. -3 8 6 -4.12 7.64 0. 1.0000 0. -3 8 7 -1.92 7.26 0. 1.0000 0. -3 8 8 2.41 7.38 0. 1.0000 0. 3 -8 -8 4.42 10.29 0. 1.0000 0. 3 -8 -9 42.19 12.12 0. 1.0000 0. 3 9 8 5.21 6.17 0. 1.0000 0. 3 9 7 10.72 4.86 0. 1.0000 0. 3 9 7 4.79 6.37 0. 1.0000 0. 3 9 6 29.75 5.24 0. 1.0000 0. 3 9 6 22.31 6.12 0. 1.0000 0. 3 9 5 -1.23 5.55 0. 1.0000 0. 3 9 5 1.16 5.73 0. 1.0000 0. 3 9 4 37.48 4.96 0. 1.0000 0. 3 9 3 0.11 4.39 0. 1.0000 0. 3 9 2 18.26 5.16 0. 1.0000 0. -3 -9 -2 4.32 4.99 0. 1.0000 0. 3 9 1 87.86 6.29 0. 1.0000 0. -3 -9 -1 10.71 5.78 0. 1.0000 0. -3 9 0 0.77 3.17 0. 1.0000 0. -3 -9 0 -0.37 5.94 0. 1.0000 0. -3 9 1 137.00 6.36 0. 1.0000 0. 3 -9 -1 1.37 4.76 0. 1.0000 0. 3 -9 -2 86.54 6.89 0. 1.0000 0. -3 9 2 104.14 5.26 0. 1.0000 0. -3 9 3 12.37 4.04 0. 1.0000 0. 3 -9 -3 12.74 5.36 0. 1.0000 0. -3 9 4 27.32 9.88 0. 1.0000 0. -3 9 4 67.77 5.61 0. 1.0000 0. -3 9 5 2.22 8.99 0. 1.0000 0. -3 9 5 1.82 4.71 0. 1.0000 0. -3 9 6 12.96 8.90 0. 1.0000 0. -3 9 7 -0.61 8.38 0. 1.0000 0. -3 9 8 6.43 9.00 0. 1.0000 0. 3 10 7 18.04 5.10 0. 1.0000 0. 3 10 7 13.89 6.40 0. 1.0000 0. 3 10 6 6.47 5.12 0. 1.0000 0. 3 10 6 7.82 6.17 0. 1.0000 0. 3 10 5 7.74 4.99 0. 1.0000 0. 3 10 5 7.20 6.37 0. 1.0000 0. 3 10 4 24.54 4.83 0. 1.0000 0. 3 10 3 13.62 4.98 0. 1.0000 0. -3 -10 -3 0.10 5.29 0. 1.0000 0. 3 10 2 22.73 5.49 0. 1.0000 0. -3 -10 -2 4.80 5.50 0. 1.0000 0. 3 10 1 17.36 5.39 0. 1.0000 0. -3 -10 -1 0.37 5.96 0. 1.0000 0. 3 10 0 0.54 6.68 0. 1.0000 0. -3 10 1 -0.76 3.47 0. 1.0000 0. 3 -10 -2 0.81 5.15 0. 1.0000 0. -3 10 2 43.30 4.46 0. 1.0000 0. 3 -10 -3 108.56 6.85 0. 1.0000 0. -3 10 3 62.78 10.50 0. 1.0000 0. -3 10 4 4.08 4.25 0. 1.0000 0. -3 10 4 0.59 8.28 0. 1.0000 0. -3 10 5 6.42 9.30 0. 1.0000 0. -3 10 5 9.38 5.09 0. 1.0000 0. -3 10 6 3.61 9.07 0. 1.0000 0. -3 10 6 15.76 5.20 0. 1.0000 0. -3 10 7 -3.40 9.69 0. 1.0000 0. 3 11 6 9.63 5.55 0. 1.0000 0. 3 11 6 5.89 6.82 0. 1.0000 0. 3 11 5 35.26 5.45 0. 1.0000 0. 3 11 4 -2.21 4.67 0. 1.0000 0. 3 11 3 102.00 6.78 0. 1.0000 0. -3 -11 -3 22.39 6.51 0. 1.0000 0. 3 11 2 38.46 5.83 0. 1.0000 0. -3 -11 -2 -3.92 6.25 0. 1.0000 0. 3 11 1 0.44 5.83 0. 1.0000 0. -3 -11 -1 -0.72 6.08 0. 1.0000 0. -3 11 2 -0.07 3.60 0. 1.0000 0. 3 -11 -3 0.06 5.09 0. 1.0000 0. -3 11 3 34.57 4.58 0. 1.0000 0. -3 11 4 0.90 4.21 0. 1.0000 0. -3 11 4 0.95 6.82 0. 1.0000 0. -3 11 5 18.52 5.22 0. 1.0000 0. -3 11 5 7.48 8.10 0. 1.0000 0. -3 -12 -4 4.50 6.55 0. 1.0000 0. 3 12 3 -0.41 5.14 0. 1.0000 0. -3 -12 -3 1.96 6.13 0. 1.0000 0. 3 12 2 0.07 4.48 0. 1.0000 0. -3 -12 -2 3.19 6.08 0. 1.0000 0. -3 12 3 2.50 3.47 0. 1.0000 0. -3 12 4 11.17 4.44 0. 1.0000 0. -512 # 2376 reflections output ; # end of ARCHIVE-HKL.CIF _chemical_name_common ROY _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: acetone' ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_ROY_ON_3p00GPa _database_code_depnum_ccdc_archive 'CCDC 2098641' loop_ _audit_author_name _audit_author_address 'Nicholas Funnell' ;STFC, ISIS Neutron Facility United Kingdom ; _audit_update_record ; 2021-07-22 deposited with the CCDC. 2021-08-27 downloaded from the CCDC. ; _audit_creation_date 2021-01-26 _audit_creation_method 'CRYSTALS_ver_14.61_build_7795 ' _chemical_name_systematic ; 5-methyl-2[(2-nitrophenyl)amino]-3-thiophenecarbonitrile ; #CheckCIF alerts _vrf_THETM01_ROY_ON_3p00GPa ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575 RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT027_ROY_ON_3p00GPa ; PROBLEM: _diffrn_reflns_theta_full value (too) Low ...... 17.44 Degree RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT029_ROY_ON_3p00GPa ; PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.700 Why? RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT201_ROY_ON_3p00GPa ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 17 Report RESPONSE: The model could only be refined isotropically in order to maintain a favourable data-to-parameter ratio, due to numerous unmeasured reflections. The relatively electron-rich sulfur atom has been modelled anisotropically. ; _vrf_PLAT911_ROY_ON_3p00GPa ; PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.555 471 Report RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT157_ROY_ON_3p00GPa ; PROBLEM: Non-standard Monoclinic Beta Angle less 90 Deg 88.80 Degree RESPONSE: This is a series of high pressure structures where the beta angle decreases, passing through 90 degrees. The non-standard beta angle allows the change in angle to be followed clearly. ; _vrf_PLAT340_ROY_ON_3p00GPa ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.00745 Ang. RESPONSE: These are poor-quality diffraction data. ; _vrf_PLAT413_ROY_ON_3p00GPa ; PROBLEM: Short Inter XH3 .. XHn H2 ..H111 . 2.03 Ang. RESPONSE: These are high-pressure data - short contacts are expected. ; _vrf_PLAT910_ROY_ON_3p00GPa ; PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 8 Note RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _refine_special_details ; In the absence of significant anomalous scattering, Friedel pairs were merged. Data were collected in a Merrill-Bassett diamond anvil cell, which significantly restricts the regions over which reciprocal space can be sampled. Thus, these data are poor quality/incomplete, reflected in numerous CheckCIF alerts regarding refinement statistics. At all pressures, the atomic connectivity is known. All non-sulfur atoms were refined isotropically; sulfur was refined anisotropically. Hydrogen atoms were constrained to ride on their host atoms. #=============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Total Missing #------------------------------------------------------------------------------- 20.82 0.500 0.684 1049 717 332 23.01 0.550 0.653 1326 866 460 23.25 0.555 0.646 1355 876 479 ------------------------------------------------------------ ACTA Min. Res. --- Note: The Reported Completeness refers to the Actual H,K,L Index Range ; #end of refcif _cell_length_a 3.565200(17) _cell_length_b 17.43660(5) _cell_length_c 15.97730(5) _cell_angle_alpha 90 _cell_angle_beta 88.803(6) _cell_angle_gamma 90 _cell_volume 993.012(7) _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' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 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' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C12 H9 N3 O2 S1 # Dc = 1.73 Fooo = 536.00 Mu = 3.22 M = 259.29 # Found Formula = C12 H9 N3 O2 S1 # Dc = 1.73 FOOO = 536.00 Mu = 3.22 M = 259.29 _chemical_formula_sum 'C12 H9 N3 O2 S1' _chemical_formula_moiety 'C12 H9 N3 O2 S1' _chemical_compound_source 'TCI Chemicals' _chemical_formula_weight 259.29 _cell_measurement_reflns_used 1445 _cell_measurement_theta_min 1.71 _cell_measurement_theta_max 23.26 _cell_measurement_temperature 293 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_min 0.050 _exptl_crystal_size_mid 0.072 _exptl_crystal_size_max 0.248 _exptl_crystal_density_diffrn 1.734 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 0.322 # Sheldrick geometric approximatio 0.98 0.98 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North et al., 1968)' _exptl_absorpt_correction_T_min 0.09 _exptl_absorpt_correction_T_max 0.98 _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_device 'four-circle diffractometer' _diffrn_radiation_monochromator mirror _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 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction ; CrysAlisPro (Rigaku Oxford Diffraction, 2017) ; _computing_structure_solution 'Model from previously-determined structure' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 293 _diffrn_ambient_pressure 3000000 _diffrn_reflns_number 2277 _diffrn_reflns_av_unetI/netI 0.036 _reflns_number_total 898 _diffrn_reflns_av_R_equivalents 0.036 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 898 # Theoretical number of reflections is about 2852 _diffrn_reflns_theta_min 1.729 _diffrn_reflns_theta_max 23.253 _diffrn_measured_fraction_theta_max 0.638 _diffrn_reflns_theta_full 17.440 _diffrn_measured_fraction_theta_full 0.700 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_h_max 3 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -3 _reflns_limit_h_max 3 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.78 _refine_diff_density_max 0.61 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # Explicitly named reflections are ALWAYS excluded from R&wR # The values actually used during refinement # These are labelled "all" for compatibility with PLATON _oxford_refine_reflns_threshold_expression I>-3.0\s(I) _refine_ls_number_restraints 94 _refine_ls_number_parameters 82 _refine_ls_number_reflns 876 _oxford_refine_ls_R_factor_ref 0.1234 _refine_ls_R_factor_all 0.1234 _refine_ls_wR_factor_ref 0.0481 _refine_ls_wR_factor_all 0.0481 _refine_ls_goodness_of_fit_ref 1.0701 _refine_ls_shift/su_max 0.0002431 _refine_ls_shift/su_mean 0.0000576 # Computed with I/sigma = -10 _oxford_reflns_number_all 876 _oxford_refine_ls_R_factor_all 0.1234 _oxford_refine_ls_wR_factor_all 0.0481 # Computed with no filters except I/sigma = +2 a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 681 _refine_ls_R_factor_gt 0.0885 _refine_ls_wR_factor_gt 0.0448 _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed #undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ; Method= SQRT(W) = 1/(Data with the key SIGMA(/FO/) in list 6) ; # 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 S1 S 0.6740(3) 0.58757(8) 0.43609(9) 0.0301 1.0000 Uani D U . . . . O1 O 0.4653(8) 0.6347(2) 0.0224(3) 0.0373(10) 1.0000 Uiso D U . . . . O2 O 0.4682(8) 0.7018(2) 0.1379(3) 0.0363(9) 1.0000 Uiso D U . . . . C1 C 0.8370(10) 0.5855(3) 0.2231(3) 0.0293(11) 1.0000 Uiso D U . . . . C2 C 1.0264(11) 0.5210(3) 0.2566(4) 0.0277(11) 1.0000 Uiso D U . . . . C3 C 1.1048(9) 0.4586(3) 0.2068(3) 0.0274(12) 1.0000 Uiso D U . . . . C4 C 0.9988(11) 0.4556(3) 0.1237(4) 0.0297(11) 1.0000 Uiso D U . . . . C5 C 0.8164(11) 0.5182(3) 0.0902(4) 0.0295(11) 1.0000 Uiso D U . . . . C6 C 0.7391(10) 0.5811(3) 0.1394(3) 0.0291(10) 1.0000 Uiso D U . . . . C7 C 0.8202(11) 0.6524(3) 0.3598(4) 0.0282(11) 1.0000 Uiso D U . . . . C8 C 0.9806(11) 0.7149(3) 0.3962(4) 0.0295(11) 1.0000 Uiso D U . . . . C9 C 0.9762(10) 0.7105(3) 0.4846(3) 0.0292(11) 1.0000 Uiso D U . . . . C10 C 0.8220(8) 0.6476(2) 0.5155(4) 0.0293(11) 1.0000 Uiso D U . . . . C11 C 0.7743(8) 0.6222(2) 0.6053(3) 0.0342(13) 1.0000 Uiso D U . . . . C12 C 1.1600(11) 0.7699(3) 0.3435(4) 0.0327(11) 1.0000 Uiso D U . . . . N1 N 0.7625(9) 0.6445(3) 0.2748(3) 0.0289(10) 1.0000 Uiso D U . . . . N2 N 1.3164(10) 0.8075(3) 0.2952(3) 0.0351(11) 1.0000 Uiso D U . . . . N3 N 0.5459(9) 0.6432(3) 0.0967(3) 0.0337(10) 1.0000 Uiso D U . . . . H1 H 0.641(5) 0.6797(13) 0.2523(16) 0.034(3) 1.0000 Uiso D . . . . . H2 H 1.0966 0.5206 0.3123 0.0371 1.0000 Uiso R . . . . . H3 H 1.2342 0.4171 0.2291 0.0378 1.0000 Uiso R . . . . . H4 H 1.0459 0.4124 0.0911 0.0379 1.0000 Uiso R . . . . . H5 H 0.7519 0.5195 0.0342 0.0381 1.0000 Uiso R . . . . . H9 H 1.0777 0.7488 0.5177 0.0401 1.0000 Uiso R . . . . . H111 H 0.8973 0.5738 0.6129 0.0522 1.0000 Uiso DR . . . . . H112 H 0.8815 0.6596 0.6414 0.0520 1.0000 Uiso DR . . . . . H113 H 0.5138 0.6167 0.6188 0.0520 1.0000 Uiso DR . . . . . 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 S1 0.0376(7) 0.0301(13) 0.0229(13) 0.0015(6) -0.0044(6) -0.0030(7) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.5061(15) 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 S1 . C7 . 1.735(6) yes S1 . C10 . 1.735(5) yes O1 . N3 . 1.236(5) yes O2 . N3 . 1.243(5) yes C1 . C2 . 1.422(7) yes C1 . C6 . 1.391(7) yes C1 . N1 . 1.343(6) yes C2 . C3 . 1.374(7) yes C2 . H2 . 0.929 no C3 . C4 . 1.390(7) yes C3 . H3 . 0.932 no C4 . C5 . 1.385(7) yes C4 . H4 . 0.928 no C5 . C6 . 1.374(7) yes C5 . H5 . 0.929 no C6 . N3 . 1.461(6) yes C7 . C8 . 1.367(7) yes C7 . N1 . 1.383(6) yes C8 . C9 . 1.414(7) yes C8 . C12 . 1.420(7) yes C9 . C10 . 1.318(7) yes C9 . H9 . 0.931 no C10 . C11 . 1.507(7) yes C11 . H111 . 0.960 no C11 . H112 . 0.956 no C11 . H113 . 0.954 no C12 . N2 . 1.148(6) yes N1 . H1 . 0.84(2) 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 C7 . S1 . C10 . 91.7(3) yes C2 . C1 . C6 . 116.7(5) yes C2 . C1 . N1 . 117.6(6) yes C6 . C1 . N1 . 125.7(5) yes C1 . C2 . C3 . 120.1(6) yes C1 . C2 . H2 . 120.4 no C3 . C2 . H2 . 119.6 no C2 . C3 . C4 . 121.8(5) yes C2 . C3 . H3 . 119.3 no C4 . C3 . H3 . 118.8 no C3 . C4 . C5 . 118.6(5) yes C3 . C4 . H4 . 121.1 no C5 . C4 . H4 . 120.3 no C4 . C5 . C6 . 119.9(6) yes C4 . C5 . H5 . 121.2 no C6 . C5 . H5 . 118.8 no C1 . C6 . C5 . 122.9(5) yes C1 . C6 . N3 . 122.6(4) yes C5 . C6 . N3 . 114.5(5) yes S1 . C7 . C8 . 110.0(4) yes S1 . C7 . N1 . 125.2(4) yes C8 . C7 . N1 . 124.7(5) yes C7 . C8 . C9 . 112.7(5) yes C7 . C8 . C12 . 118.3(5) yes C9 . C8 . C12 . 128.6(4) yes C8 . C9 . C10 . 114.5(5) yes C8 . C9 . H9 . 122.1 no C10 . C9 . H9 . 123.3 no S1 . C10 . C9 . 111.0(5) yes S1 . C10 . C11 . 119.3(2) yes C9 . C10 . C11 . 129.7(3) yes C10 . C11 . H111 . 109.6 no C10 . C11 . H112 . 109.6 no H111 . C11 . H112 . 109.5 no C10 . C11 . H113 . 109.6 no H111 . C11 . H113 . 109.1 no H112 . C11 . H113 . 109.3 no C8 . C12 . N2 . 172.3(7) yes C7 . N1 . C1 . 130.4(5) yes C7 . N1 . H1 . 116.0(18) no C1 . N1 . H1 . 113.2(18) no C6 . N3 . O2 . 117.6(5) yes C6 . N3 . O1 . 118.7(4) yes O2 . N3 . O1 . 123.6(4) yes _iucr_refine_instructions_details ; # # Punched on 26/01/21 at 11:54:12 # #LIST 12 BLOCK CONT SCALE CONT S ( 1 ,X'S,U'S) CONT O ( 1 ,X'S,U[ISO]) UNTIL H ( 1 ) RIDE C ( 2,X'S) H ( 2,X'S) RIDE C ( 3,X'S) H ( 3,X'S) RIDE C ( 4,X'S) H ( 4,X'S) RIDE C ( 5,X'S) H ( 5,X'S) RIDE C ( 9,X'S) H ( 9,X'S) RIDE C ( 11,X'S) H ( 111,X'S) H ( 112,X'S) H ( 113,X'S) END # # Punched on 26/01/21 at 11:54:12 # #LIST 16 NO REM REM NPF NOTE - FIRST UNTIL LAST REM REM HREST START (DO NOT REMOVE THIS LINE) REM NO H NO #H U MULT DIST REM C-H REM >4 1.5 .96 DISORDER REM 1 1 1.2 .93 C C-H (ACETYLENE) REM 1 2 1.2 .93 C-C(H)-C REM 1 3 1.2 .98 (C)3-C-H REM 2 1 1.2 .93 C=C-H(2) REM 2 2 1.2 .97 (C)2-C-(H)2 REM 3 1 1.5 .96 C-C-(H)3 REM N-H REM >4 1.5 .89 DISORDER REM 1 1 1.2 .86 N-N/H REM 1 2 1.2 .86 (C)2-N-H REM 1 3 1.2 .89 (C)3-N-H REM 2 1 1.2 .86 C-N-(H)2 REM 2 2 1.2 .89 (C)2-N-(H)2 REM 3 1 1.2 .89 C-H-(H)3 REM O-H REM 1 1 1.5 .82 O-H REM REM DIST ESD = 0.02 REM VIB ESD = 0.002 REM ANGLE ESD = 2.0 REM REM TO ACTIVATE THE VIB RESTRAINTS, REMOVE LEADING REM REM H1-N-R2 DIST 0.86, 0.02 = CONT N ( 1) TO H(1) REST 0.034, 0.002 = H(1,U[ISO]) ANGLE 0.0, 2.0 = MEAN CONT H(1) TO N ( 1) TO C(7) CONT H(1) TO N ( 1) TO C(1) REM HREST END (DO NOT REMOVE THIS LINE) REM DELU START (DO NOT REMOVE THIS LINE) VIBR .0, 0.00200 = S(1) TO C(10) VIBR .0, 0.00200 = S(1) TO C(7) VIBR .0, 0.00500 = C(7) TO C(10) VIBR .0, 0.00200 = N(2) TO C(12) VIBR .0, 0.00200 = C(10) TO C(9) VIBR .0, 0.00200 = C(10) TO C(11) VIBR .0, 0.00500 = C(9) TO S(1) VIBR .0, 0.00500 = C(11) TO S(1) VIBR .0, 0.00500 = C(11) TO C(9) VIBR .0, 0.00200 = C(12) TO C(8) VIBR .0, 0.00500 = C(8) TO N(2) VIBR .0, 0.00200 = O(1) TO N(3) VIBR .0, 0.00200 = C(2) TO C(1) VIBR .0, 0.00200 = C(2) TO C(3) VIBR .0, 0.00500 = C(3) TO C(1) VIBR .0, 0.00200 = N(1) TO C(7) VIBR .0, 0.00200 = N(1) TO C(1) VIBR .0, 0.00500 = C(1) TO C(7) VIBR .0, 0.00200 = C(7) TO C(8) VIBR .0, 0.00500 = N(1) TO S(1) VIBR .0, 0.00500 = C(8) TO S(1) VIBR .0, 0.00500 = C(8) TO N(1) VIBR .0, 0.00200 = O(2) TO N(3) VIBR .0, 0.00200 = N(3) TO C(6) VIBR .0, 0.00500 = O(1) TO O(2) VIBR .0, 0.00500 = C(6) TO O(2) VIBR .0, 0.00500 = C(6) TO O(1) VIBR .0, 0.00200 = C(5) TO C(4) VIBR .0, 0.00200 = C(5) TO C(6) VIBR .0, 0.00500 = C(6) TO C(4) VIBR .0, 0.00200 = C(4) TO C(3) VIBR .0, 0.00500 = C(3) TO C(5) VIBR .0, 0.00200 = C(1) TO C(6) VIBR .0, 0.00500 = N(1) TO C(2) VIBR .0, 0.00500 = C(6) TO C(2) VIBR .0, 0.00500 = C(6) TO N(1) VIBR .0, 0.00500 = C(5) TO N(3) VIBR .0, 0.00500 = C(1) TO N(3) VIBR .0, 0.00500 = C(1) TO C(5) VIBR .0, 0.00200 = C(9) TO C(8) VIBR .0, 0.00500 = C(8) TO C(10) VIBR .0, 0.00500 = C(2) TO C(4) VIBR .0, 0.00500 = C(12) TO C(9) VIBR .0, 0.00500 = C(7) TO C(9) VIBR .0, 0.00500 = C(7) TO C(12) REM DELU END (DO NOT REMOVE THIS LINE) ANGLE 110.000000 , 0.020000 = C(10) TO C(11) TO H(111) ANGLE 110.000000 , 0.020000 = C(10) TO C(11) TO H(112) ANGLE 110.000000 , 0.020000 = C(10) TO C(11) TO H(113) DISTANCE 1.225000 , 0.050000 = O(2) TO N(3) DISTANCE 1.225000 , 0.050000 = O(1) TO N(3) DISTANCE 1.440000 , 0.050000 = C(6) TO N(3) DISTANCE 1.390000 , 0.050000 = C(5) TO C(6) DISTANCE 1.364000 , 0.050000 = C(4) TO C(5) DISTANCE 1.222000 , 0.050000 = O(1) TO N(3) DISTANCE 1.232000 , 0.050000 = O(2) TO N(3) DISTANCE 1.440000 , 0.050000 = C(6) TO N(3) DISTANCE 1.392000 , 0.050000 = C(5) TO C(6) DISTANCE 1.364000 , 0.050000 = C(4) TO C(5) DISTANCE 1.391000 , 0.050000 = C(3) TO C(4) DISTANCE 1.371000 , 0.050000 = C(2) TO C(3) DISTANCE 1.400000 , 0.050000 = C(1) TO C(2) DISTANCE 1.408000 , 0.050000 = C(1) TO C(6) DISTANCE 1.382000 , 0.050000 = C(1) TO N(1) DISTANCE 1.387000 , 0.050000 = C(7) TO N(1) DISTANCE 1.728000 , 0.050000 = S(1) TO C(7) DISTANCE 1.724000 , 0.050000 = S(1) TO C(10) DISTANCE 1.500000 , 0.050000 = C(10) TO C(11) DISTANCE 1.349000 , 0.050000 = C(9) TO C(10) DISTANCE 1.427000 , 0.050000 = C(8) TO C(9) DISTANCE 1.372000 , 0.050000 = C(7) TO C(8) DISTANCE 1.422000 , 0.050000 = C(8) TO C(12) DISTANCE 1.141000 , 0.050000 = C(12) TO N(2) REM THERMSIM START (DO NOT REMOVE THIS LINE) U(IJ) .0, 0.04000 = S(1) TO C(7) U(IJ) .0, 0.04000 = S(1) TO C(10) U(IJ) .0, 0.08000 = O(1) TO N(3) U(IJ) .0, 0.08000 = O(2) TO N(3) U(IJ) .0, 0.04000 = C(1) TO C(2) U(IJ) .0, 0.04000 = C(1) TO C(6) U(IJ) .0, 0.04000 = C(1) TO N(1) U(IJ) .0, 0.04000 = C(2) TO C(3) U(IJ) .0, 0.04000 = C(3) TO C(4) U(IJ) .0, 0.04000 = C(4) TO C(5) U(IJ) .0, 0.04000 = C(5) TO C(6) U(IJ) .0, 0.04000 = C(6) TO N(3) U(IJ) .0, 0.04000 = C(7) TO C(8) U(IJ) .0, 0.04000 = C(7) TO N(1) U(IJ) .0, 0.04000 = C(8) TO C(9) U(IJ) .0, 0.04000 = C(8) TO C(12) U(IJ) .0, 0.04000 = C(9) TO C(10) U(IJ) .0, 0.08000 = C(10) TO C(11) U(IJ) .0, 0.08000 = C(12) TO N(2) REM THERMSIM END (DO NOT REMOVE THIS LINE) PLANAR 0.010000 C(1) C(6) N(1) H(1) PLANAR 0.010000 C(1) C(2) C(3) C(4) C(5) C(6) N(1) N(3) PLANAR 0.010000 S(1) C(7) C(8) C(9) C(10) N(1) 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 -1 9 2 x . 1 3 9 x . 2 10 1 x . -2 12 3 x . 0 8 2 x . 0 7 1 x . 0 14 5 x . 2 0 6 x . -2 10 2 x . -3 9 1 x . 3 8 0 x . 0 13 4 x . 1 8 1 x . -2 1 8 x . 3 7 1 x . 1 17 7 x . 1 13 4 x . # looking for ARCHIVE-HKL.CIF _iucr_refine_reflections_details ; # Data was input as F-squared # punching LIST 6 as LIST 6 with all keys set # NBGNXT= 36 #LIST 6 READ NCOEF= 8 TYPE=FIX, F'S = FSQ UNIT=DATA, CHECK=NO L30=NO ARCH=NO STORE NCOEF= 6 OUTPUT INDICES /FO/ SIGMA(/FO/) RATIO/JCODE CORRECTIONS SERIAL CONT INPUT H K L /FO/ SIGMA(/FO/) JCODE CONT CORRECTIONS SERIAL FOR (I4,I4,I4,F10.2,F8.2,F4.0,F7.4,F7.0) END 0 -1 1 5.26 0.28 0. 1.0000 0. 0 1 -1 4.81 0.25 0. 1.0000 0. 0 1 -2 79.31 1.94 0. 1.0000 0. 0 2 -1 1787.90 31.50 0. 1.0000 0. 0 2 -2 110.76 2.40 0. 1.0000 0. 0 2 -2 121.36 2.41 0. 1.0000 0. 0 -2 2 114.16 2.45 0. 1.0000 0. 0 -2 2 109.03 2.17 0. 1.0000 0. 0 2 -2 110.83 2.25 0. 1.0000 0. 0 2 -3 885.94 15.32 0. 1.0000 0. 0 2 -3 783.32 15.63 0. 1.0000 0. 0 2 -3 824.74 15.29 0. 1.0000 0. 0 -2 6 995.45 18.88 0. 1.0000 0. 0 3 -1 457.89 8.13 0. 1.0000 0. 0 -3 1 459.85 8.15 0. 1.0000 0. 0 3 -2 52.59 1.24 0. 1.0000 0. 0 3 -2 52.62 1.39 0. 1.0000 0. 0 3 -2 55.46 1.45 0. 1.0000 0. 0 3 -2 59.74 1.47 0. 1.0000 0. 0 -3 2 58.47 2.00 0. 1.0000 0. 0 -3 3 2.72 0.48 0. 1.0000 0. 0 3 -3 1.58 0.70 0. 1.0000 0. 0 3 -3 2.14 0.48 0. 1.0000 0. 0 3 -3 2.67 0.73 0. 1.0000 0. 0 -3 3 2.66 0.77 0. 1.0000 0. 0 3 -3 2.85 0.86 0. 1.0000 0. 0 3 -3 2.29 0.52 0. 1.0000 0. 0 -3 4 164.82 3.58 0. 1.0000 0. 0 -3 4 159.78 3.02 0. 1.0000 0. 0 -3 4 163.08 4.24 0. 1.0000 0. 0 -3 5 72.17 2.03 0. 1.0000 0. 0 -3 6 153.40 3.75 0. 1.0000 0. 0 -3 7 1.92 2.50 0. 1.0000 0. 0 -3 7 2.05 1.40 0. 1.0000 0. 0 -3 8 6.14 1.75 0. 1.0000 0. 0 4 -1 0.29 0.26 0. 1.0000 0. 0 -4 1 -0.02 0.12 0. 1.0000 0. 0 -4 2 557.00 12.96 0. 1.0000 0. 0 -4 2 597.50 10.46 0. 1.0000 0. 0 4 -2 552.55 11.25 0. 1.0000 0. 0 4 -3 49.93 3.11 0. 1.0000 0. 0 4 -3 65.82 1.51 0. 1.0000 0. 0 4 -3 64.22 1.79 0. 1.0000 0. 0 -4 4 52.72 1.77 0. 1.0000 0. 0 -4 4 53.57 1.45 0. 1.0000 0. 0 -4 4 53.01 2.10 0. 1.0000 0. 0 -4 4 54.30 2.28 0. 1.0000 0. 0 -4 5 696.75 12.39 0. 1.0000 0. 0 -4 5 696.88 12.69 0. 1.0000 0. 0 -4 5 721.86 13.32 0. 1.0000 0. 0 -4 5 674.69 13.94 0. 1.0000 0. 0 -4 6 66.81 2.37 0. 1.0000 0. 0 -4 6 63.88 2.47 0. 1.0000 0. 0 -4 6 73.31 2.16 0. 1.0000 0. 0 -4 6 68.87 1.58 0. 1.0000 0. 0 -4 7 264.21 6.26 0. 1.0000 0. 0 -4 7 247.37 5.84 0. 1.0000 0. 0 -4 7 254.08 5.51 0. 1.0000 0. 0 -4 8 1.19 1.37 0. 1.0000 0. 0 -4 9 175.29 4.64 0. 1.0000 0. 0 -4 9 177.13 5.79 0. 1.0000 0. 0 -4 10 -0.19 1.56 0. 1.0000 0. 0 -4 10 0.08 2.82 0. 1.0000 0. 0 5 -1 486.76 8.73 0. 1.0000 0. 0 -5 2 765.86 13.62 0. 1.0000 0. 0 -5 3 271.77 5.06 0. 1.0000 0. 0 5 -3 271.22 5.25 0. 1.0000 0. 0 -5 3 280.98 6.71 0. 1.0000 0. 0 5 -4 642.28 11.42 0. 1.0000 0. 0 -5 4 658.04 12.41 0. 1.0000 0. 0 -5 5 308.26 6.89 0. 1.0000 0. 0 -5 5 292.74 5.86 0. 1.0000 0. 0 -5 5 294.67 6.31 0. 1.0000 0. 0 -5 6 21.88 1.23 0. 1.0000 0. 0 -5 6 22.82 1.80 0. 1.0000 0. 0 -5 6 20.36 2.95 0. 1.0000 0. 0 -5 6 22.20 1.91 0. 1.0000 0. 0 -5 7 339.85 6.17 0. 1.0000 0. 0 -5 7 334.73 6.59 0. 1.0000 0. 0 -5 7 333.32 7.36 0. 1.0000 0. 0 -5 7 314.31 6.90 0. 1.0000 0. 0 -5 8 22.26 1.51 0. 1.0000 0. 0 -5 8 23.47 1.07 0. 1.0000 0. 0 -5 8 24.46 1.88 0. 1.0000 0. 0 -5 8 24.16 2.33 0. 1.0000 0. 0 -5 8 22.85 1.69 0. 1.0000 0. 0 -5 9 298.45 7.25 0. 1.0000 0. 0 -5 9 328.48 6.95 0. 1.0000 0. 0 -5 9 310.79 7.58 0. 1.0000 0. 0 -5 10 1.06 2.84 0. 1.0000 0. 0 -5 10 -0.44 1.94 0. 1.0000 0. 0 -5 10 0.37 1.73 0. 1.0000 0. 0 -5 11 2.09 1.80 0. 1.0000 0. 0 -5 11 6.43 3.13 0. 1.0000 0. 0 -5 11 1.63 1.90 0. 1.0000 0. 0 6 -1 161.42 3.11 0. 1.0000 0. 0 -6 3 226.35 4.13 0. 1.0000 0. 0 -6 3 229.44 4.33 0. 1.0000 0. 0 6 -3 225.42 4.66 0. 1.0000 0. 0 -6 3 239.72 7.20 0. 1.0000 0. 0 6 -4 129.33 2.61 0. 1.0000 0. 0 -6 4 140.90 2.82 0. 1.0000 0. 0 6 -4 141.18 2.96 0. 1.0000 0. 0 -6 4 139.04 3.82 0. 1.0000 0. 0 -6 4 160.41 4.64 0. 1.0000 0. 0 -6 5 21.54 1.77 0. 1.0000 0. 0 -6 5 20.86 1.97 0. 1.0000 0. 0 -6 6 48.35 2.62 0. 1.0000 0. 0 6 -6 49.68 1.23 0. 1.0000 0. 0 -6 6 53.44 2.42 0. 1.0000 0. 0 -6 6 53.85 3.35 0. 1.0000 0. 0 -6 7 187.82 5.87 0. 1.0000 0. 0 -6 7 180.79 4.09 0. 1.0000 0. 0 -6 7 179.30 4.69 0. 1.0000 0. 0 -6 8 401.80 8.53 0. 1.0000 0. 0 -6 8 406.36 9.27 0. 1.0000 0. 0 -6 8 395.89 7.93 0. 1.0000 0. 0 -6 8 415.26 8.89 0. 1.0000 0. 0 -6 9 44.71 2.04 0. 1.0000 0. 0 -6 9 45.44 1.42 0. 1.0000 0. 0 -6 9 44.36 2.85 0. 1.0000 0. 0 -6 9 45.78 3.01 0. 1.0000 0. 0 -6 9 44.76 2.28 0. 1.0000 0. 0 -6 10 185.61 3.92 0. 1.0000 0. 0 -6 10 182.38 5.44 0. 1.0000 0. 0 -6 10 201.36 5.73 0. 1.0000 0. 0 -6 10 197.90 4.58 0. 1.0000 0. 0 -6 10 207.12 5.07 0. 1.0000 0. 0 -6 11 11.48 2.11 0. 1.0000 0. 0 -6 11 12.34 3.10 0. 1.0000 0. 0 -6 11 7.92 1.87 0. 1.0000 0. 0 -6 12 2.03 2.12 0. 1.0000 0. 0 -6 12 1.24 1.94 0. 1.0000 0. 0 -6 12 4.14 3.07 0. 1.0000 0. 0 -6 12 1.29 1.85 0. 1.0000 0. 0 7 -1 0.30 0.27 0. 1.0000 0. 0 7 -2 7.38 0.54 0. 1.0000 0. 0 -7 3 2075.29 41.45 0. 1.0000 0. 0 -7 4 654.02 13.52 0. 1.0000 0. 0 -7 4 601.74 11.27 0. 1.0000 0. 0 -7 4 631.89 12.18 0. 1.0000 0. 0 7 -4 633.03 11.13 0. 1.0000 0. 0 -7 5 454.56 8.56 0. 1.0000 0. 0 7 -5 465.28 8.29 0. 1.0000 0. 0 -7 5 482.49 9.87 0. 1.0000 0. 0 -7 5 450.86 9.60 0. 1.0000 0. 0 -7 6 8.62 2.46 0. 1.0000 0. 0 -7 7 289.70 7.73 0. 1.0000 0. 0 -7 7 334.20 7.18 0. 1.0000 0. 0 7 -7 300.41 5.56 0. 1.0000 0. 0 -7 7 313.06 8.30 0. 1.0000 0. 0 -7 8 93.20 3.93 0. 1.0000 0. 0 -7 8 106.84 3.81 0. 1.0000 0. 0 -7 8 102.85 3.05 0. 1.0000 0. 0 -7 9 143.96 5.93 0. 1.0000 0. 0 -7 9 137.32 3.66 0. 1.0000 0. 0 -7 9 141.15 4.69 0. 1.0000 0. 0 -7 9 136.16 4.59 0. 1.0000 0. 0 -7 10 392.88 8.92 0. 1.0000 0. 0 -7 10 377.65 8.00 0. 1.0000 0. 0 -7 10 392.82 10.12 0. 1.0000 0. 0 -7 10 420.84 9.40 0. 1.0000 0. 0 -7 11 505.90 10.01 0. 1.0000 0. 0 -7 11 500.61 11.74 0. 1.0000 0. 0 -7 11 477.02 11.19 0. 1.0000 0. 0 -7 11 504.47 10.80 0. 1.0000 0. 0 -7 12 67.54 4.15 0. 1.0000 0. 0 -7 12 59.56 3.27 0. 1.0000 0. 0 -7 12 71.06 4.25 0. 1.0000 0. 0 -7 12 62.72 2.86 0. 1.0000 0. 0 -7 13 28.73 3.70 0. 1.0000 0. 0 -7 13 25.36 2.54 0. 1.0000 0. 0 -7 13 25.98 3.17 0. 1.0000 0. 0 8 -2 0.34 0.47 0. 1.0000 0. 0 -8 3 362.57 13.32 0. 1.0000 0. 0 -8 3 491.26 9.66 0. 1.0000 0. 0 -8 4 41.38 2.32 0. 1.0000 0. 0 -8 4 47.72 3.66 0. 1.0000 0. 0 -8 4 43.81 1.38 0. 1.0000 0. 0 8 -5 29.37 0.94 0. 1.0000 0. 0 -8 5 32.58 2.63 0. 1.0000 0. 0 -8 5 29.68 1.20 0. 1.0000 0. 0 -8 5 29.93 2.28 0. 1.0000 0. 0 8 -5 34.73 1.01 0. 1.0000 0. 0 -8 6 10.50 2.47 0. 1.0000 0. 0 -8 6 10.43 2.48 0. 1.0000 0. 0 -8 6 11.92 1.08 0. 1.0000 0. 0 -8 7 81.96 4.57 0. 1.0000 0. 0 -8 7 77.71 3.59 0. 1.0000 0. 0 -8 8 37.28 3.02 0. 1.0000 0. 0 -8 8 37.99 4.97 0. 1.0000 0. 0 -8 9 0.56 2.74 0. 1.0000 0. 0 -8 10 34.96 3.82 0. 1.0000 0. 0 -8 10 25.63 3.34 0. 1.0000 0. 0 -8 10 22.25 2.45 0. 1.0000 0. 0 -8 11 1.12 3.26 0. 1.0000 0. 0 -8 11 0.12 4.34 0. 1.0000 0. 0 -8 11 -1.95 3.05 0. 1.0000 0. 0 -8 11 1.10 2.16 0. 1.0000 0. 0 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-1 20.29 3.32 0. 1.0000 0. 3 -5 -1 16.11 3.17 0. 1.0000 0. -3 -5 1 14.99 3.13 0. 1.0000 0. -3 -5 2 41.45 3.37 0. 1.0000 0. 3 5 -2 36.40 3.48 0. 1.0000 0. 3 -5 -3 2.27 4.62 0. 1.0000 0. -3 -5 3 0.56 2.67 0. 1.0000 0. 3 5 -4 5.24 3.16 0. 1.0000 0. -3 -5 4 5.61 2.65 0. 1.0000 0. -3 -5 5 5.74 2.75 0. 1.0000 0. -3 -5 6 17.06 2.84 0. 1.0000 0. -3 -5 7 206.19 5.71 0. 1.0000 0. -3 -5 8 12.43 2.73 0. 1.0000 0. 3 -6 10 23.43 5.80 0. 1.0000 0. 3 -6 10 23.81 5.06 0. 1.0000 0. 3 -6 9 28.73 5.93 0. 1.0000 0. -3 6 -9 34.40 4.29 0. 1.0000 0. 3 -6 9 36.04 5.04 0. 1.0000 0. -3 6 -8 13.68 3.80 0. 1.0000 0. -3 6 -7 0.92 3.32 0. 1.0000 0. -3 6 -6 4.68 3.29 0. 1.0000 0. -3 6 -5 23.53 3.56 0. 1.0000 0. 3 -6 4 0.61 2.18 0. 1.0000 0. -3 6 -4 9.01 3.17 0. 1.0000 0. 3 -6 3 14.41 5.52 0. 1.0000 0. -3 6 -3 16.39 3.39 0. 1.0000 0. 3 -6 2 135.00 3.73 0. 1.0000 0. -3 -6 -2 -0.06 2.86 0. 1.0000 0. 3 6 2 0.73 1.60 0. 1.0000 0. 3 -6 2 150.43 6.09 0. 1.0000 0. 3 6 2 -0.70 2.85 0. 1.0000 0. -3 6 -2 161.57 5.01 0. 1.0000 0. 3 -6 1 21.49 2.74 0. 1.0000 0. 3 6 1 22.74 3.35 0. 1.0000 0. 3 -6 1 18.67 4.02 0. 1.0000 0. 3 6 0 124.48 4.81 0. 1.0000 0. 3 -6 0 120.12 5.05 0. 1.0000 0. 3 6 0 124.73 4.79 0. 1.0000 0. 3 6 -1 11.75 3.29 0. 1.0000 0. 3 -6 -1 1.77 3.90 0. 1.0000 0. -3 -6 1 11.29 3.75 0. 1.0000 0. 3 6 -1 11.94 3.02 0. 1.0000 0. -3 -6 1 6.54 3.13 0. 1.0000 0. -3 -6 2 263.50 5.95 0. 1.0000 0. 3 6 -2 269.82 6.32 0. 1.0000 0. -3 -6 2 251.12 6.80 0. 1.0000 0. 3 6 -3 -1.65 3.20 0. 1.0000 0. -3 -6 3 4.64 2.94 0. 1.0000 0. 3 6 -4 55.55 3.92 0. 1.0000 0. -3 -6 4 59.64 3.51 0. 1.0000 0. 3 6 -5 36.98 3.86 0. 1.0000 0. -3 -6 5 37.77 3.15 0. 1.0000 0. -3 -6 6 43.88 3.11 0. 1.0000 0. -3 -6 7 3.77 2.65 0. 1.0000 0. -3 -6 8 34.15 3.01 0. 1.0000 0. 3 -7 9 21.64 4.08 0. 1.0000 0. 3 -7 9 27.89 6.18 0. 1.0000 0. -3 7 -9 26.66 4.10 0. 1.0000 0. -3 7 -8 -3.47 3.74 0. 1.0000 0. -3 7 -7 -0.25 3.43 0. 1.0000 0. -3 7 -6 27.47 3.66 0. 1.0000 0. 3 -7 5 20.27 7.11 0. 1.0000 0. -3 7 -5 21.56 3.47 0. 1.0000 0. 3 -7 4 33.39 6.29 0. 1.0000 0. -3 7 -4 35.72 3.63 0. 1.0000 0. 3 -7 3 36.93 5.60 0. 1.0000 0. -3 7 -3 32.73 3.66 0. 1.0000 0. 3 -7 2 -1.85 2.43 0. 1.0000 0. 3 -7 2 -0.93 4.37 0. 1.0000 0. -3 7 -2 1.30 3.26 0. 1.0000 0. 3 7 1 -3.74 2.95 0. 1.0000 0. 3 -7 1 7.43 2.61 0. 1.0000 0. 3 -7 0 5.50 4.32 0. 1.0000 0. -3 -7 0 8.59 3.81 0. 1.0000 0. 3 7 0 9.06 3.02 0. 1.0000 0. 3 7 0 10.32 3.15 0. 1.0000 0. 3 -7 0 12.63 3.50 0. 1.0000 0. 3 7 -1 83.73 4.24 0. 1.0000 0. -3 -7 1 78.56 4.79 0. 1.0000 0. 3 -7 -2 5.67 5.21 0. 1.0000 0. 3 7 -2 1.05 3.32 0. 1.0000 0. -3 -7 2 0.51 3.81 0. 1.0000 0. -3 -7 3 29.51 3.43 0. 1.0000 0. 3 7 -3 30.01 3.72 0. 1.0000 0. 3 7 -4 27.40 3.64 0. 1.0000 0. -3 -7 4 29.28 3.23 0. 1.0000 0. 3 7 -5 15.72 3.62 0. 1.0000 0. -3 -7 5 14.79 3.05 0. 1.0000 0. 3 7 -6 44.07 4.05 0. 1.0000 0. -3 -7 6 48.51 3.34 0. 1.0000 0. -3 -7 7 6.85 2.66 0. 1.0000 0. 3 -8 9 8.13 3.98 0. 1.0000 0. -3 8 -9 4.96 3.97 0. 1.0000 0. -3 8 -8 2.03 3.48 0. 1.0000 0. -3 8 -7 5.26 3.42 0. 1.0000 0. -3 8 -6 0.56 3.42 0. 1.0000 0. 3 -8 5 9.74 6.86 0. 1.0000 0. -3 8 -5 13.08 3.40 0. 1.0000 0. 3 -8 4 -0.32 6.15 0. 1.0000 0. -3 8 -4 1.54 3.22 0. 1.0000 0. 3 -8 3 181.72 6.96 0. 1.0000 0. -3 8 -3 192.60 5.43 0. 1.0000 0. 3 -8 2 2.41 2.11 0. 1.0000 0. 3 -8 2 8.85 4.44 0. 1.0000 0. 3 -8 1 29.77 5.40 0. 1.0000 0. 3 -8 1 54.62 4.35 0. 1.0000 0. 3 -8 0 -0.70 4.40 0. 1.0000 0. -3 -8 0 -2.22 3.40 0. 1.0000 0. 3 -8 -1 -3.37 4.88 0. 1.0000 0. -3 -8 1 2.12 3.72 0. 1.0000 0. 3 8 -1 3.17 3.18 0. 1.0000 0. 3 8 -2 56.61 4.07 0. 1.0000 0. -3 -8 2 53.56 4.55 0. 1.0000 0. 3 8 -5 4.72 3.48 0. 1.0000 0. 3 8 -6 2.40 3.58 0. 1.0000 0. -3 -8 6 0.50 2.88 0. 1.0000 0. 3 8 -7 -4.34 3.67 0. 1.0000 0. -3 9 -8 -0.57 3.52 0. 1.0000 0. -3 9 -7 13.07 3.61 0. 1.0000 0. 3 -9 6 38.59 8.03 0. 1.0000 0. -3 9 -6 28.62 3.74 0. 1.0000 0. 3 -9 5 0.49 6.61 0. 1.0000 0. -3 9 -5 1.39 3.35 0. 1.0000 0. 3 -9 4 46.92 6.16 0. 1.0000 0. -3 9 -4 47.40 4.04 0. 1.0000 0. 3 -9 3 5.81 5.15 0. 1.0000 0. -3 9 -3 1.16 3.36 0. 1.0000 0. 3 -9 2 38.91 4.68 0. 1.0000 0. 3 -9 2 37.65 4.95 0. 1.0000 0. 3 -9 1 3.30 4.73 0. 1.0000 0. 3 -9 1 41.97 4.35 0. 1.0000 0. 3 -9 0 -2.78 4.70 0. 1.0000 0. -3 -9 1 0.52 3.65 0. 1.0000 0. 3 9 -2 46.26 3.87 0. 1.0000 0. -3 -9 2 48.85 4.57 0. 1.0000 0. 3 9 -3 9.81 3.56 0. 1.0000 0. 3 9 -4 30.41 3.86 0. 1.0000 0. 3 9 -5 0.61 3.47 0. 1.0000 0. 3 9 -6 39.52 4.01 0. 1.0000 0. 3 9 -7 10.20 3.81 0. 1.0000 0. 3 -10 7 6.00 8.45 0. 1.0000 0. -3 10 -7 8.90 3.63 0. 1.0000 0. 3 -10 6 13.71 7.42 0. 1.0000 0. -3 10 -6 5.73 3.55 0. 1.0000 0. 3 -10 5 3.92 6.58 0. 1.0000 0. -3 10 -5 4.10 3.45 0. 1.0000 0. 3 -10 4 12.70 5.66 0. 1.0000 0. -3 10 -4 11.89 3.61 0. 1.0000 0. 3 -10 3 22.52 5.23 0. 1.0000 0. 3 -10 2 7.74 4.44 0. 1.0000 0. 3 -10 2 8.15 4.34 0. 1.0000 0. 3 -10 1 -1.93 4.80 0. 1.0000 0. 3 -10 1 -0.07 4.02 0. 1.0000 0. -3 -10 1 1.10 2.99 0. 1.0000 0. -3 -10 2 -0.34 4.04 0. 1.0000 0. 3 10 -2 88.82 4.17 0. 1.0000 0. -3 -10 3 137.83 6.02 0. 1.0000 0. 3 10 -4 6.37 3.56 0. 1.0000 0. 3 10 -5 15.33 3.70 0. 1.0000 0. 3 10 -6 13.45 3.81 0. 1.0000 0. -3 11 -6 6.55 3.61 0. 1.0000 0. 3 -11 5 42.58 7.03 0. 1.0000 0. -3 11 -5 51.46 4.24 0. 1.0000 0. 3 -11 4 -3.36 5.65 0. 1.0000 0. -3 11 -4 4.20 3.55 0. 1.0000 0. 3 -11 3 70.23 6.01 0. 1.0000 0. 3 -11 3 73.14 5.64 0. 1.0000 0. 3 -11 2 10.60 5.70 0. 1.0000 0. 3 -11 2 -3.43 4.49 0. 1.0000 0. 3 -11 2 1.25 4.06 0. 1.0000 0. -3 -11 2 4.72 3.34 0. 1.0000 0. -3 -11 3 1.67 4.05 0. 1.0000 0. 3 11 -3 4.62 3.29 0. 1.0000 0. 3 11 -4 14.29 3.59 0. 1.0000 0. 3 11 -5 5.88 3.66 0. 1.0000 0. 3 -12 3 3.76 4.87 0. 1.0000 0. 3 -12 3 -0.29 4.86 0. 1.0000 0. 3 -12 2 -1.55 4.88 0. 1.0000 0. 3 -12 2 6.34 4.01 0. 1.0000 0. 3 -12 2 -4.73 3.93 0. 1.0000 0. -3 -12 3 -0.99 3.44 0. 1.0000 0. -512 # 2329 reflections output ; # end of ARCHIVE-HKL.CIF _chemical_name_common ROY _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: acetone' ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_ROY_ON_3p53GPa _database_code_depnum_ccdc_archive 'CCDC 2098642' loop_ _audit_author_name _audit_author_address 'Nicholas Funnell' ;STFC, ISIS Neutron Facility United Kingdom ; _audit_update_record ; 2021-07-22 deposited with the CCDC. 2021-08-27 downloaded from the CCDC. ; _audit_creation_date 2021-01-26 _audit_creation_method 'CRYSTALS_ver_14.61_build_7795 ' _chemical_name_systematic ; 5-methyl-2[(2-nitrophenyl)amino]-3-thiophenecarbonitrile ; #CheckCIF alerts _vrf_THETM01_ROY_ON_3p53GPa ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575 RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT027_ROY_ON_3p53GPa ; PROBLEM: _diffrn_reflns_theta_full value (too) Low ...... 17.67 Degree RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT029_ROY_ON_3p53GPa ; PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.718 Why? RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT201_ROY_ON_3p53GPa ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 17 Report RESPONSE: The model could only be refined isotropically in order to maintain a favourable data-to-parameter ratio, due to numerous unmeasured reflections. The relatively electron-rich sulfur atom has been modelled anisotropically. ; _vrf_PLAT911_ROY_ON_3p53GPa ; PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.555 399 Report RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _vrf_PLAT157_ROY_ON_3p53GPa ; PROBLEM: Non-standard Monoclinic Beta Angle less 90 Deg 88.36 Degree RESPONSE: This is a series of high pressure structures where the beta angle decreases, passing through 90 degrees. The non-standard beta angle allows the change in angle to be followed clearly. ; _vrf_PLAT340_ROY_ON_3p53GPa ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.00709 Ang. RESPONSE: These are poor-quality diffraction data. ; _vrf_PLAT411_ROY_ON_3p53GPa ; PROBLEM: Short Inter H...H Contact H5 ..H5 . 2.07 Ang. RESPONSE: These are high-pressure data - short contacts are expected. ; _vrf_PLAT413_ROY_ON_3p53GPa ; PROBLEM: Short Inter XH3 .. XHn H2 ..H111 . 2.03 Ang. RESPONSE: These are high-pressure data - short contacts are expected. ; _vrf_PLAT910_ROY_ON_3p53GPa ; PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 8 Note RESPONSE: Data are highly incomplete owing to shading of recripocal space by the pressure cell. Resolution and completeness statistics are given below. ; _refine_special_details ; In the absence of significant anomalous scattering, Friedel pairs were merged. Data were collected in a Merrill-Bassett diamond anvil cell, which significantly restricts the regions over which reciprocal space can be sampled. Thus, these data are poor quality/incomplete, reflected in numerous CheckCIF alerts regarding refinement statistics. At all pressures, the atomic connectivity is known. All non-sulfur atoms were refined isotropically; sulfur was refined anisotropically. Hydrogen atoms were constrained to ride on their host atoms. #=============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Total Missing #------------------------------------------------------------------------------- 20.82 0.500 0.713 1025 731 294 23.01 0.550 0.693 1301 902 399 23.24 0.555 0.694 1332 925 407 ------------------------------------------------------------ ACTA Min. Res. --- Note: The Reported Completeness refers to the Actual H,K,L Index Range ; #end of refcif _cell_length_a 3.52400(2) _cell_length_b 17.38790(7) _cell_length_c 15.81840(7) _cell_angle_alpha 90 _cell_angle_beta 88.361(8) _cell_angle_gamma 90 _cell_volume 968.875(10) _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' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 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' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C12 H9 N3 O2 S1 # Dc = 1.78 Fooo = 536.00 Mu = 3.30 M = 259.29 # Found Formula = C12 H9 N3 O2 S1 # Dc = 1.78 FOOO = 536.00 Mu = 3.30 M = 259.29 _chemical_formula_sum 'C12 H9 N3 O2 S1' _chemical_formula_moiety 'C12 H9 N3 O2 S1' _chemical_compound_source 'TCI Chemicals' _chemical_formula_weight 259.29 _cell_measurement_reflns_used 1358 _cell_measurement_theta_min 1.74 _cell_measurement_theta_max 23.34 _cell_measurement_temperature 293 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_min 0.050 _exptl_crystal_size_mid 0.072 _exptl_crystal_size_max 0.248 _exptl_crystal_density_diffrn 1.777 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 0.330 # Sheldrick geometric approximatio 0.98 0.98 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North et al., 1968)' _exptl_absorpt_correction_T_min 0.07 _exptl_absorpt_correction_T_max 0.98 _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_device 'four-circle diffractometer' _diffrn_radiation_monochromator mirror _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 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction ; CrysAlisPro (Rigaku Oxford Diffraction, 2017) ; _computing_structure_solution 'Model from previously-determined structure' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 293 _diffrn_ambient_pressure 3530000 _diffrn_reflns_number 2425 _diffrn_reflns_av_unetI/netI 0.058 _reflns_number_total 936 _diffrn_reflns_av_R_equivalents 0.057 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 936 # Theoretical number of reflections is about 2779 _diffrn_reflns_theta_min 1.741 _diffrn_reflns_theta_max 23.243 _diffrn_measured_fraction_theta_max 0.679 _diffrn_reflns_theta_full 17.665 _diffrn_measured_fraction_theta_full 0.718 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_h_max 3 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -3 _reflns_limit_h_max 3 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.83 _refine_diff_density_max 0.95 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # Explicitly named reflections are ALWAYS excluded from R&wR # The values actually used during refinement # These are labelled "all" for compatibility with PLATON _oxford_refine_reflns_threshold_expression I>-3.0\s(I) _refine_ls_number_restraints 94 _refine_ls_number_parameters 82 _refine_ls_number_reflns 925 _oxford_refine_ls_R_factor_ref 0.1378 _refine_ls_R_factor_all 0.1378 _refine_ls_wR_factor_ref 0.0598 _refine_ls_wR_factor_all 0.0598 _refine_ls_goodness_of_fit_ref 1.0826 _refine_ls_shift/su_max 0.0001479 _refine_ls_shift/su_mean 0.0000479 # Computed with I/sigma = -10 _oxford_reflns_number_all 925 _oxford_refine_ls_R_factor_all 0.1378 _oxford_refine_ls_wR_factor_all 0.0598 # Computed with no filters except I/sigma = +2 a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 643 _refine_ls_R_factor_gt 0.0799 _refine_ls_wR_factor_gt 0.0553 _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed #undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ; Method= SQRT(W) = 1/(Data with the key SIGMA(/FO/) in list 6) ; # 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 S1 S 0.6586(3) 0.58693(7) 0.43699(9) 0.0284 1.0000 Uani D U . . . . O1 O 0.4578(7) 0.6371(2) 0.0222(2) 0.0378(9) 1.0000 Uiso D U . . . . O2 O 0.4560(7) 0.7026(2) 0.1390(2) 0.0352(9) 1.0000 Uiso D U . . . . N1 N 0.7496(8) 0.6457(2) 0.2768(3) 0.0269(9) 1.0000 Uiso D U . . . . N2 N 1.3063(9) 0.8078(2) 0.2947(3) 0.0334(10) 1.0000 Uiso D U . . . . N3 N 0.5412(9) 0.6448(2) 0.0968(3) 0.0336(9) 1.0000 Uiso D U . . . . C1 C 0.8244(10) 0.5860(3) 0.2222(3) 0.0272(10) 1.0000 Uiso D U . . . . C2 C 1.0172(9) 0.5206(3) 0.2569(3) 0.0265(10) 1.0000 Uiso D U . . . . C3 C 1.1001(9) 0.4581(3) 0.2072(3) 0.0274(10) 1.0000 Uiso D U . . . . C4 C 1.0011(10) 0.4556(3) 0.1232(3) 0.0290(10) 1.0000 Uiso D U . . . . C5 C 0.8162(9) 0.5166(3) 0.0890(3) 0.0276(10) 1.0000 Uiso D U . . . . C6 C 0.7314(10) 0.5819(3) 0.1380(3) 0.0280(10) 1.0000 Uiso D U . . . . C7 C 0.8067(10) 0.6512(3) 0.3628(3) 0.0243(10) 1.0000 Uiso D U . . . . C8 C 0.9691(11) 0.7152(3) 0.3978(4) 0.0272(9) 1.0000 Uiso D U . . . . C9 C 0.9676(10) 0.7118(3) 0.4875(3) 0.0297(10) 1.0000 Uiso D U . . . . C10 C 0.8068(7) 0.6462(2) 0.5184(3) 0.0281(10) 1.0000 Uiso D U . . . . C11 C 0.7564(8) 0.6211(2) 0.6069(4) 0.0377(12) 1.0000 Uiso D U . . . . C12 C 1.1474(11) 0.7704(3) 0.3444(3) 0.0266(10) 1.0000 Uiso D U . . . . H1 H 0.634(4) 0.6832(12) 0.2553(14) 0.034(3) 1.0000 Uiso D . . . . . H2 H 1.0845 0.5203 0.3130 0.0311 1.0000 Uiso R . . . . . H3 H 1.2297 0.4166 0.2294 0.0319 1.0000 Uiso R . . . . . H4 H 1.0529 0.4120 0.0906 0.0360 1.0000 Uiso R . . . . . H5 H 0.7535 0.5167 0.0321 0.0361 1.0000 Uiso R . . . . . H9 H 1.0619 0.7511 0.5208 0.0401 1.0000 Uiso R . . . . . H111 H 0.9136 0.5773 0.6168 0.0820 1.0000 Uiso DR . . . . . H112 H 0.8267 0.6619 0.6440 0.0819 1.0000 Uiso DR . . . . . H113 H 0.4958 0.6078 0.6181 0.0821 1.0000 Uiso DR . . . . . 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 S1 0.0359(6) 0.0180(10) 0.0316(11) 0.0016(6) -0.0060(5) -0.0021(6) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.3906(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 S1 . C7 . 1.693(5) yes S1 . C10 . 1.741(5) yes O1 . N3 . 1.231(5) yes O2 . N3 . 1.239(5) yes N1 . C1 . 1.371(6) yes N1 . C7 . 1.385(5) yes N1 . H1 . 0.85(2) no N2 . C12 . 1.153(5) yes N3 . C6 . 1.446(6) yes C1 . C2 . 1.442(6) yes C1 . C6 . 1.382(6) yes C2 . C3 . 1.367(6) yes C2 . H2 . 0.926 no C3 . C4 . 1.385(6) yes C3 . H3 . 0.929 no C4 . C5 . 1.365(6) yes C4 . H4 . 0.932 no C5 . C6 . 1.402(6) yes C5 . H5 . 0.934 no C7 . C8 . 1.375(7) yes C8 . C9 . 1.420(6) yes C8 . C12 . 1.413(6) yes C9 . C10 . 1.359(6) yes C9 . H9 . 0.930 no C10 . C11 . 1.472(6) yes C11 . H111 . 0.958 no C11 . H112 . 0.958 no C11 . H113 . 0.959 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 C7 . S1 . C10 . 91.6(3) yes C1 . N1 . C7 . 129.8(5) yes C1 . N1 . H1 . 114.7(16) no C7 . N1 . H1 . 115.3(16) no O2 . N3 . O1 . 122.9(4) yes O2 . N3 . C6 . 118.6(5) yes O1 . N3 . C6 . 118.4(4) yes N1 . C1 . C2 . 116.3(5) yes N1 . C1 . C6 . 126.8(5) yes C2 . C1 . C6 . 116.9(5) yes C1 . C2 . C3 . 120.3(5) yes C1 . C2 . H2 . 120.3 no C3 . C2 . H2 . 119.4 no C2 . C3 . C4 . 121.4(5) yes C2 . C3 . H3 . 120.0 no C4 . C3 . H3 . 118.6 no C3 . C4 . C5 . 119.4(5) yes C3 . C4 . H4 . 120.4 no C5 . C4 . H4 . 120.1 no C4 . C5 . C6 . 120.5(5) yes C4 . C5 . H5 . 120.8 no C6 . C5 . H5 . 118.6 no N3 . C6 . C5 . 117.2(5) yes N3 . C6 . C1 . 121.4(5) yes C5 . C6 . C1 . 121.4(5) yes N1 . C7 . S1 . 125.8(4) yes N1 . C7 . C8 . 121.7(5) yes S1 . C7 . C8 . 112.3(4) yes C7 . C8 . C9 . 112.3(5) yes C7 . C8 . C12 . 119.4(5) yes C9 . C8 . C12 . 127.9(4) yes C8 . C9 . C10 . 112.6(4) yes C8 . C9 . H9 . 123.0 no C10 . C9 . H9 . 124.4 no S1 . C10 . C9 . 111.2(4) yes S1 . C10 . C11 . 119.82(17) yes C9 . C10 . C11 . 129.0(3) yes C10 . C11 . H111 . 109.7 no C10 . C11 . H112 . 109.7 no H111 . C11 . H112 . 109.1 no C10 . C11 . H113 . 109.7 no H111 . C11 . H113 . 109.4 no H112 . C11 . H113 . 109.2 no C8 . C12 . N2 . 171.6(6) yes _iucr_refine_instructions_details ; # # Punched on 26/01/21 at 12:05:20 # #LIST 12 BLOCK CONT SCALE CONT S ( 1 ,X'S,U'S) CONT O ( 1 ,X'S,U[ISO]) UNTIL H ( 1 ) RIDE C ( 2,X'S) H ( 2,X'S) RIDE C ( 3,X'S) H ( 3,X'S) RIDE C ( 4,X'S) H ( 4,X'S) RIDE C ( 5,X'S) H ( 5,X'S) RIDE C ( 9,X'S) H ( 9,X'S) RIDE C ( 11,X'S) H ( 111,X'S) H ( 112,X'S) H ( 113,X'S) END # # Punched on 26/01/21 at 12:05:20 # #LIST 16 NO REM REM NPF NOTE - FIRST UNTIL LAST REM REM HREST START (DO NOT REMOVE THIS LINE) REM NO H NO #H U MULT DIST REM C-H REM >4 1.5 .96 DISORDER REM 1 1 1.2 .93 C C-H (ACETYLENE) REM 1 2 1.2 .93 C-C(H)-C REM 1 3 1.2 .98 (C)3-C-H REM 2 1 1.2 .93 C=C-H(2) REM 2 2 1.2 .97 (C)2-C-(H)2 REM 3 1 1.5 .96 C-C-(H)3 REM N-H REM >4 1.5 .89 DISORDER REM 1 1 1.2 .86 N-N/H REM 1 2 1.2 .86 (C)2-N-H REM 1 3 1.2 .89 (C)3-N-H REM 2 1 1.2 .86 C-N-(H)2 REM 2 2 1.2 .89 (C)2-N-(H)2 REM 3 1 1.2 .89 C-H-(H)3 REM O-H REM 1 1 1.5 .82 O-H REM REM DIST ESD = 0.02 REM VIB ESD = 0.002 REM ANGLE ESD = 2.0 REM REM TO ACTIVATE THE VIB RESTRAINTS, REMOVE LEADING REM REM H1-N-R2 DIST 0.86, 0.02 = CONT N ( 1) TO H(1) REST 0.034, 0.002 = H(1,U[ISO]) ANGLE 0.0, 2.0 = MEAN CONT H(1) TO N ( 1) TO C(1) CONT H(1) TO N ( 1) TO C(7) REM HREST END (DO NOT REMOVE THIS LINE) REM DELU START (DO NOT REMOVE THIS LINE) VIBR .0, 0.00200 = S(1) TO C(10) VIBR .0, 0.00200 = S(1) TO C(7) VIBR .0, 0.00500 = C(7) TO C(10) VIBR .0, 0.00200 = N(2) TO C(12) VIBR .0, 0.00200 = C(10) TO C(9) VIBR .0, 0.00200 = C(10) TO C(11) VIBR .0, 0.00500 = C(9) TO S(1) VIBR .0, 0.00500 = C(11) TO S(1) VIBR .0, 0.00500 = C(11) TO C(9) VIBR .0, 0.00200 = C(12) TO C(8) VIBR .0, 0.00500 = C(8) TO N(2) VIBR .0, 0.00200 = O(1) TO N(3) VIBR .0, 0.00200 = C(2) TO C(1) VIBR .0, 0.00200 = C(2) TO C(3) VIBR .0, 0.00500 = C(3) TO C(1) VIBR .0, 0.00200 = N(1) TO C(7) VIBR .0, 0.00200 = N(1) TO C(1) VIBR .0, 0.00500 = C(1) TO C(7) VIBR .0, 0.00200 = C(7) TO C(8) VIBR .0, 0.00500 = N(1) TO S(1) VIBR .0, 0.00500 = C(8) TO S(1) VIBR .0, 0.00500 = C(8) TO N(1) VIBR .0, 0.00200 = O(2) TO N(3) VIBR .0, 0.00200 = N(3) TO C(6) VIBR .0, 0.00500 = O(1) TO O(2) VIBR .0, 0.00500 = C(6) TO O(2) VIBR .0, 0.00500 = C(6) TO O(1) VIBR .0, 0.00200 = C(5) TO C(4) VIBR .0, 0.00200 = C(5) TO C(6) VIBR .0, 0.00500 = C(6) TO C(4) VIBR .0, 0.00200 = C(4) TO C(3) VIBR .0, 0.00500 = C(3) TO C(5) VIBR .0, 0.00200 = C(1) TO C(6) VIBR .0, 0.00500 = N(1) TO C(2) VIBR .0, 0.00500 = C(6) TO C(2) VIBR .0, 0.00500 = C(6) TO N(1) VIBR .0, 0.00500 = C(5) TO N(3) VIBR .0, 0.00500 = C(1) TO N(3) VIBR .0, 0.00500 = C(1) TO C(5) VIBR .0, 0.00200 = C(9) TO C(8) VIBR .0, 0.00500 = C(8) TO C(10) VIBR .0, 0.00500 = C(2) TO C(4) VIBR .0, 0.00500 = C(12) TO C(9) VIBR .0, 0.00500 = C(7) TO C(9) VIBR .0, 0.00500 = C(7) TO C(12) REM DELU END (DO NOT REMOVE THIS LINE) ANGLE 110.000000 , 0.020000 = C(10) TO C(11) TO H(111) ANGLE 110.000000 , 0.020000 = C(10) TO C(11) TO H(112) ANGLE 110.000000 , 0.020000 = C(10) TO C(11) TO H(113) DISTANCE 1.225000 , 0.050000 = O(2) TO N(3) DISTANCE 1.225000 , 0.050000 = O(1) TO N(3) DISTANCE 1.440000 , 0.050000 = C(6) TO N(3) DISTANCE 1.390000 , 0.050000 = C(5) TO C(6) DISTANCE 1.364000 , 0.050000 = C(4) TO C(5) DISTANCE 1.222000 , 0.050000 = O(1) TO N(3) DISTANCE 1.232000 , 0.050000 = O(2) TO N(3) DISTANCE 1.440000 , 0.050000 = C(6) TO N(3) DISTANCE 1.392000 , 0.050000 = C(5) TO C(6) DISTANCE 1.364000 , 0.050000 = C(4) TO C(5) DISTANCE 1.391000 , 0.050000 = C(3) TO C(4) DISTANCE 1.371000 , 0.050000 = C(2) TO C(3) DISTANCE 1.400000 , 0.050000 = C(1) TO C(2) DISTANCE 1.408000 , 0.050000 = C(1) TO C(6) DISTANCE 1.382000 , 0.050000 = C(1) TO N(1) DISTANCE 1.387000 , 0.050000 = C(7) TO N(1) DISTANCE 1.728000 , 0.050000 = S(1) TO C(7) DISTANCE 1.724000 , 0.050000 = S(1) TO C(10) DISTANCE 1.500000 , 0.050000 = C(10) TO C(11) DISTANCE 1.349000 , 0.050000 = C(9) TO C(10) DISTANCE 1.427000 , 0.050000 = C(8) TO C(9) DISTANCE 1.372000 , 0.050000 = C(7) TO C(8) DISTANCE 1.422000 , 0.050000 = C(8) TO C(12) DISTANCE 1.141000 , 0.050000 = C(12) TO N(2) REM THERMSIM START (DO NOT REMOVE THIS LINE) U(IJ) .0, 0.04000 = S(1) TO C(7) U(IJ) .0, 0.04000 = S(1) TO C(10) U(IJ) .0, 0.08000 = O(1) TO N(3) U(IJ) .0, 0.08000 = O(2) TO N(3) U(IJ) .0, 0.04000 = C(1) TO C(2) U(IJ) .0, 0.04000 = C(1) TO C(6) U(IJ) .0, 0.04000 = C(1) TO N(1) U(IJ) .0, 0.04000 = C(2) TO C(3) U(IJ) .0, 0.04000 = C(3) TO C(4) U(IJ) .0, 0.04000 = C(4) TO C(5) U(IJ) .0, 0.04000 = C(5) TO C(6) U(IJ) .0, 0.04000 = C(6) TO N(3) U(IJ) .0, 0.04000 = C(7) TO C(8) U(IJ) .0, 0.04000 = C(7) TO N(1) U(IJ) .0, 0.04000 = C(8) TO C(9) U(IJ) .0, 0.04000 = C(8) TO C(12) U(IJ) .0, 0.04000 = C(9) TO C(10) U(IJ) .0, 0.08000 = C(10) TO C(11) U(IJ) .0, 0.08000 = C(12) TO N(2) REM THERMSIM END (DO NOT REMOVE THIS LINE) PLANAR 0.010000 C(1) C(6) N(1) H(1) PLANAR 0.010000 C(1) C(2) C(3) C(4) C(5) C(6) N(1) N(3) PLANAR 0.010000 S(1) C(7) C(8) C(9) C(10) N(1) 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 1 1 6 x . -2 13 3 x . 1 5 11 x . 2 10 1 x . 0 7 1 x . # looking for ARCHIVE-HKL.CIF _iucr_refine_reflections_details ; # Data was input as F-squared # punching LIST 6 as LIST 6 with all keys set # NBGNXT= 36 #LIST 6 READ NCOEF= 8 TYPE=FIX, F'S = FSQ UNIT=DATA, CHECK=NO L30=NO ARCH=NO STORE NCOEF= 6 OUTPUT INDICES /FO/ SIGMA(/FO/) RATIO/JCODE CORRECTIONS SERIAL CONT INPUT H K L /FO/ SIGMA(/FO/) JCODE CONT CORRECTIONS SERIAL FOR (I4,I4,I4,F10.2,F8.2,F4.0,F7.4,F7.0) END 0 1 -1 1.98 0.13 0. 1.0000 0. 0 -1 1 2.03 0.14 0. 1.0000 0. 0 -1 1 2.08 0.17 0. 1.0000 0. 0 -1 2 41.15 1.35 0. 1.0000 0. 0 -1 3 283.47 7.86 0. 1.0000 0. 0 2 -1 1026.02 27.14 0. 1.0000 0. 0 -2 1 985.75 27.99 0. 1.0000 0. 0 -2 1 1031.06 27.09 0. 1.0000 0. 0 -2 1 1034.20 27.70 0. 1.0000 0. 0 2 -1 1026.50 27.25 0. 1.0000 0. 0 -2 2 64.62 1.82 0. 1.0000 0. 0 2 -2 58.69 1.79 0. 1.0000 0. 0 2 -2 64.06 1.82 0. 1.0000 0. 0 -2 2 61.98 2.74 0. 1.0000 0. 0 2 -2 60.72 1.77 0. 1.0000 0. 0 -2 2 58.73 1.90 0. 1.0000 0. 0 2 -2 61.56 2.22 0. 1.0000 0. 0 2 -3 443.12 12.47 0. 1.0000 0. 0 2 -3 477.91 12.44 0. 1.0000 0. 0 2 -4 26.37 1.38 0. 1.0000 0. 0 -2 5 303.73 8.69 0. 1.0000 0. 0 -2 6 482.63 13.55 0. 1.0000 0. 0 -3 1 305.57 8.10 0. 1.0000 0. 0 -3 1 297.77 8.00 0. 1.0000 0. 0 -3 1 255.98 9.82 0. 1.0000 0. 0 3 -2 30.76 1.04 0. 1.0000 0. 0 3 -2 30.66 0.94 0. 1.0000 0. 0 3 -2 26.58 1.44 0. 1.0000 0. 0 -3 2 32.18 1.59 0. 1.0000 0. 0 -3 2 29.33 1.12 0. 1.0000 0. 0 -3 2 31.30 1.45 0. 1.0000 0. 0 3 -2 30.16 1.05 0. 1.0000 0. 0 3 -2 28.50 1.84 0. 1.0000 0. 0 -3 2 32.90 1.13 0. 1.0000 0. 0 3 -3 1.54 0.34 0. 1.0000 0. 0 -3 3 1.24 0.42 0. 1.0000 0. 0 3 -4 119.87 3.27 0. 1.0000 0. 0 -3 4 100.51 3.34 0. 1.0000 0. 0 3 -4 103.90 4.12 0. 1.0000 0. 0 3 -4 103.14 3.27 0. 1.0000 0. 0 3 -5 35.52 1.47 0. 1.0000 0. 0 3 -5 39.84 1.85 0. 1.0000 0. 0 -3 5 35.44 1.57 0. 1.0000 0. 0 -3 6 103.47 3.57 0. 1.0000 0. 0 -3 7 0.94 1.07 0. 1.0000 0. 0 -3 8 0.03 1.12 0. 1.0000 0. 0 -4 2 386.83 10.24 0. 1.0000 0. 0 -4 2 371.22 10.86 0. 1.0000 0. 0 4 -2 386.74 10.43 0. 1.0000 0. 0 -4 2 378.30 11.67 0. 1.0000 0. 0 -4 2 366.97 11.80 0. 1.0000 0. 0 4 -3 37.68 1.85 0. 1.0000 0. 0 -4 3 42.08 1.40 0. 1.0000 0. 0 4 -3 38.28 1.37 0. 1.0000 0. 0 -4 3 38.43 1.83 0. 1.0000 0. 0 4 -3 33.68 2.31 0. 1.0000 0. 0 -4 3 39.16 2.14 0. 1.0000 0. 0 4 -3 38.20 1.20 0. 1.0000 0. 0 4 -3 42.10 2.68 0. 1.0000 0. 0 4 -4 36.85 1.43 0. 1.0000 0. 0 -4 4 27.33 2.81 0. 1.0000 0. 0 -4 4 30.49 1.52 0. 1.0000 0. 0 -4 5 411.66 12.02 0. 1.0000 0. 0 4 -5 440.61 11.78 0. 1.0000 0. 0 -4 5 409.53 14.13 0. 1.0000 0. 0 4 -5 436.53 11.94 0. 1.0000 0. 0 4 -6 32.31 1.48 0. 1.0000 0. 0 -4 6 28.12 1.64 0. 1.0000 0. 0 -4 6 30.76 1.00 0. 1.0000 0. 0 -4 7 159.48 5.02 0. 1.0000 0. 0 4 -7 149.30 4.73 0. 1.0000 0. 0 -4 8 0.30 1.15 0. 1.0000 0. 0 4 -8 0.30 1.10 0. 1.0000 0. 0 4 -9 -0.30 1.36 0. 1.0000 0. 0 -4 9 79.11 2.62 0. 1.0000 0. 0 5 -1 341.90 9.23 0. 1.0000 0. 0 5 -2 476.07 13.24 0. 1.0000 0. 0 -5 2 491.69 12.84 0. 1.0000 0. 0 5 -3 166.53 4.66 0. 1.0000 0. 0 5 -3 156.73 4.54 0. 1.0000 0. 0 -5 3 151.47 5.84 0. 1.0000 0. 0 -5 3 161.34 5.70 0. 1.0000 0. 0 -5 4 368.23 11.20 0. 1.0000 0. 0 5 -4 390.49 10.37 0. 1.0000 0. 0 5 -4 374.28 11.35 0. 1.0000 0. 0 -5 4 388.15 10.61 0. 1.0000 0. 0 -5 4 418.25 12.28 0. 1.0000 0. 0 5 -4 384.98 10.28 0. 1.0000 0. 0 5 -5 155.59 4.92 0. 1.0000 0. 0 5 -5 155.18 4.75 0. 1.0000 0. 0 5 -5 167.31 4.80 0. 1.0000 0. 0 5 -6 15.56 1.28 0. 1.0000 0. 0 5 -6 18.03 1.24 0. 1.0000 0. 0 -5 7 172.07 5.45 0. 1.0000 0. 0 -5 7 170.45 8.30 0. 1.0000 0. 0 5 -7 158.90 5.03 0. 1.0000 0. 0 5 -7 171.51 5.61 0. 1.0000 0. 0 -5 8 14.17 3.83 0. 1.0000 0. 0 -5 8 17.60 0.74 0. 1.0000 0. 0 5 -8 17.63 1.49 0. 1.0000 0. 0 5 -9 168.90 5.72 0. 1.0000 0. 0 -5 9 184.81 5.10 0. 1.0000 0. 0 -5 9 197.77 6.16 0. 1.0000 0. 0 -5 10 0.46 0.88 0. 1.0000 0. 0 -5 10 0.11 1.53 0. 1.0000 0. 0 5 -10 0.89 1.49 0. 1.0000 0. 0 -5 11 -0.99 1.51 0. 1.0000 0. 0 6 -1 101.73 3.01 0. 1.0000 0. 0 6 -2 84.64 3.03 0. 1.0000 0. 0 6 -3 141.16 4.53 0. 1.0000 0. 0 -6 3 141.36 4.15 0. 1.0000 0. 0 -6 3 124.69 6.64 0. 1.0000 0. 0 -6 3 156.49 4.35 0. 1.0000 0. 0 6 -3 152.00 4.43 0. 1.0000 0. 0 -6 3 151.14 5.78 0. 1.0000 0. 0 6 -4 92.74 2.86 0. 1.0000 0. 0 6 -4 92.21 2.99 0. 1.0000 0. 0 -6 4 97.85 3.01 0. 1.0000 0. 0 -6 4 100.41 4.42 0. 1.0000 0. 0 6 -5 8.36 0.85 0. 1.0000 0. 0 -6 5 8.60 1.76 0. 1.0000 0. 0 6 -5 8.77 0.65 0. 1.0000 0. 0 6 -5 7.09 1.47 0. 1.0000 0. 0 -6 5 9.21 3.13 0. 1.0000 0. 0 -6 6 26.57 2.05 0. 1.0000 0. 0 6 -6 29.21 1.56 0. 1.0000 0. 0 6 -6 27.67 1.84 0. 1.0000 0. 0 6 -6 29.63 1.58 0. 1.0000 0. 0 6 -7 103.36 3.79 0. 1.0000 0. 0 6 -7 103.65 3.63 0. 1.0000 0. 0 -6 7 101.99 3.96 0. 1.0000 0. 0 6 -8 231.39 7.43 0. 1.0000 0. 0 6 -8 214.78 6.71 0. 1.0000 0. 0 6 -9 21.66 1.62 0. 1.0000 0. 0 -6 9 24.82 2.19 0. 1.0000 0. 0 -6 9 26.09 5.45 0. 1.0000 0. 0 -6 10 133.68 8.88 0. 1.0000 0. 0 6 -10 109.44 4.17 0. 1.0000 0. 0 -6 10 129.50 4.75 0. 1.0000 0. 0 6 -11 8.31 1.82 0. 1.0000 0. 0 -6 11 16.06 2.36 0. 1.0000 0. 0 -6 11 16.16 6.48 0. 1.0000 0. 0 6 -12 0.10 1.70 0. 1.0000 0. 0 -6 12 -1.66 4.38 0. 1.0000 0. 0 -6 12 0.76 1.75 0. 1.0000 0. 0 7 -1 -0.26 0.32 0. 1.0000 0. 0 7 -2 6.65 1.05 0. 1.0000 0. 0 -7 3 1538.75 40.50 0. 1.0000 0. 0 7 -3 1518.06 40.66 0. 1.0000 0. 0 -7 3 1577.13 43.00 0. 1.0000 0. 0 7 -4 399.53 11.55 0. 1.0000 0. 0 7 -4 402.72 11.45 0. 1.0000 0. 0 -7 4 423.50 11.40 0. 1.0000 0. 0 -7 4 446.08 13.18 0. 1.0000 0. 0 -7 5 280.20 9.77 0. 1.0000 0. 0 7 -5 266.32 7.21 0. 1.0000 0. 0 -7 5 247.81 9.28 0. 1.0000 0. 0 7 -5 270.75 7.47 0. 1.0000 0. 0 -7 5 271.10 7.70 0. 1.0000 0. 0 7 -5 264.04 7.65 0. 1.0000 0. 0 -7 6 3.60 3.81 0. 1.0000 0. 0 7 -6 2.98 1.85 0. 1.0000 0. 0 7 -6 4.23 1.02 0. 1.0000 0. 0 7 -6 4.88 0.70 0. 1.0000 0. 0 7 -6 3.19 0.99 0. 1.0000 0. 0 7 -7 197.68 6.03 0. 1.0000 0. 0 7 -7 180.41 6.50 0. 1.0000 0. 0 -7 7 177.16 6.53 0. 1.0000 0. 0 7 -7 196.52 5.40 0. 1.0000 0. 0 7 -8 60.38 2.99 0. 1.0000 0. 0 7 -8 71.53 3.32 0. 1.0000 0. 0 7 -9 84.59 4.25 0. 1.0000 0. 0 7 -9 74.50 3.33 0. 1.0000 0. 0 -7 9 79.62 3.82 0. 1.0000 0. 0 -7 10 207.75 6.85 0. 1.0000 0. 0 7 -10 185.74 6.33 0. 1.0000 0. 0 -7 11 301.95 13.97 0. 1.0000 0. 0 -7 11 312.82 8.83 0. 1.0000 0. 0 -7 12 35.90 2.98 0. 1.0000 0. 0 -7 12 34.47 7.19 0. 1.0000 0. 0 7 -12 19.60 2.16 0. 1.0000 0. 0 7 -13 -1.17 1.75 0. 1.0000 0. 0 -7 13 -0.68 5.13 0. 1.0000 0. 0 -7 13 1.76 2.15 0. 1.0000 0. 0 -8 2 133.53 4.58 0. 1.0000 0. 0 -8 3 297.61 8.66 0. 1.0000 0. 0 -8 3 297.84 11.96 0. 1.0000 0. 0 8 -3 311.96 9.00 0. 1.0000 0. 0 -8 4 15.43 5.60 0. 1.0000 0. 0 -8 4 24.02 3.17 0. 1.0000 0. 0 -8 5 15.36 2.84 0. 1.0000 0. 0 8 -5 18.50 1.31 0. 1.0000 0. 0 -8 5 18.11 1.44 0. 1.0000 0. 0 -8 5 16.29 4.26 0. 1.0000 0. 0 8 -5 14.18 1.43 0. 1.0000 0. 0 -8 6 3.61 3.27 0. 1.0000 0. 0 8 -6 2.82 1.00 0. 1.0000 0. 0 -8 6 3.37 3.57 0. 1.0000 0. 0 8 -6 6.74 1.07 0. 1.0000 0. 0 -8 7 47.11 3.93 0. 1.0000 0. 0 8 -7 54.97 2.47 0. 1.0000 0. 0 8 -7 51.17 1.86 0. 1.0000 0. 0 8 -7 51.55 2.41 0. 1.0000 0. 0 8 -7 42.10 3.66 0. 1.0000 0. 0 8 -8 33.61 3.08 0. 1.0000 0. 0 8 -8 29.88 1.34 0. 1.0000 0. 0 8 -8 32.02 2.27 0. 1.0000 0. 0 -8 8 27.74 3.05 0. 1.0000 0. 0 8 -9 1.84 1.99 0. 1.0000 0. 0 8 -9 0.22 0.87 0. 1.0000 0. 0 8 -9 -0.21 2.28 0. 1.0000 0. 0 8 -10 13.75 3.29 0. 1.0000 0. 0 -8 10 13.80 2.79 0. 1.0000 0. 0 8 -10 10.23 2.26 0. 1.0000 0. 0 8 -11 -0.04 2.04 0. 1.0000 0. 0 -8 11 -0.16 2.40 0. 1.0000 0. 0 8 -12 36.06 2.95 0. 1.0000 0. 0 -8 12 58.22 3.82 0. 1.0000 0. 0 8 -13 46.29 3.60 0. 1.0000 0. 0 -8 13 154.78 5.38 0. 1.0000 0. 0 8 -14 -0.18 2.15 0. 1.0000 0. 0 -8 14 -1.04 2.33 0. 1.0000 0. 0 -9 2 0.38 1.43 0. 1.0000 0. 0 9 -3 19.02 1.70 0. 1.0000 0. 0 -9 3 15.09 4.90 0. 1.0000 0. 0 -9 3 16.92 1.66 0. 1.0000 0. 0 -9 4 1296.18 34.94 0. 1.0000 0. 0 9 -4 1298.20 35.06 0. 1.0000 0. 0 -9 4 1333.46 37.30 0. 1.0000 0. 0 -9 5 21.63 3.46 0. 1.0000 0. 0 9 -5 20.73 1.41 0. 1.0000 0. 0 -9 5 19.85 1.24 0. 1.0000 0. 0 -9 5 12.48 6.26 0. 1.0000 0. 0 -9 5 18.02 1.59 0. 1.0000 0. 0 9 -6 282.54 7.73 0. 1.0000 0. 0 9 -6 295.58 8.36 0. 1.0000 0. 0 -9 6 270.47 11.01 0. 1.0000 0. 0 -9 6 287.97 8.39 0. 1.0000 0. 0 -9 6 250.36 11.68 0. 1.0000 0. 0 9 -7 48.77 2.39 0. 1.0000 0. 0 9 -7 51.74 2.44 0. 1.0000 0. 0 -9 7 39.37 6.25 0. 1.0000 0. 0 -9 7 45.79 4.98 0. 1.0000 0. 0 9 -7 51.80 2.23 0. 1.0000 0. 0 9 -8 2.38 1.58 0. 1.0000 0. 0 9 -8 2.90 1.62 0. 1.0000 0. 0 9 -8 4.65 1.10 0. 1.0000 0. 0 -9 8 2.12 3.37 0. 1.0000 0. 0 -9 9 36.83 4.45 0. 1.0000 0. 0 9 -9 33.20 3.91 0. 1.0000 0. 0 9 -9 35.51 1.64 0. 1.0000 0. 0 9 -9 45.03 3.02 0. 1.0000 0. 0 9 -10 170.44 5.00 0. 1.0000 0. 0 -9 10 176.30 7.35 0. 1.0000 0. 0 9 -10 202.46 7.26 0. 1.0000 0. 0 9 -11 13.77 2.94 0. 1.0000 0. 0 9 -11 17.67 3.97 0. 1.0000 0. 0 -9 11 16.40 3.17 0. 1.0000 0. 0 9 -12 104.90 5.55 0. 1.0000 0. 0 -9 12 145.90 6.35 0. 1.0000 0. 0 -9 13 45.62 4.17 0. 1.0000 0. 0 9 -13 26.19 3.22 0. 1.0000 0. 0 9 -14 0.11 2.65 0. 1.0000 0. 0 -9 14 2.62 3.21 0. 1.0000 0. 0 -10 2 0.40 1.23 0. 1.0000 0. 0 -10 3 26.16 5.70 0. 1.0000 0. 0 -10 3 35.63 2.21 0. 1.0000 0. 0 10 -3 34.76 2.31 0. 1.0000 0. 0 -10 4 12.62 1.59 0. 1.0000 0. 0 10 -4 11.64 1.45 0. 1.0000 0. 0 -10 4 12.86 3.78 0. 1.0000 0. 0 -10 5 21.87 3.78 0. 1.0000 0. 0 -10 5 16.33 1.19 0. 1.0000 0. 0 -10 5 20.91 1.73 0. 1.0000 0. 0 10 -5 18.37 1.46 0. 1.0000 0. 0 -10 6 51.64 7.96 0. 1.0000 0. 0 10 -6 50.71 1.72 0. 1.0000 0. 0 -10 6 54.86 5.23 0. 1.0000 0. 0 10 -6 56.62 2.46 0. 1.0000 0. 0 10 -7 21.58 1.75 0. 1.0000 0. 0 -10 7 11.09 5.33 0. 1.0000 0. 0 -10 7 20.05 5.94 0. 1.0000 0. 0 10 -7 16.67 2.01 0. 1.0000 0. 0 10 -7 22.44 1.81 0. 1.0000 0. 0 10 -8 88.86 3.53 0. 1.0000 0. 0 10 -8 74.09 3.15 0. 1.0000 0. 0 -10 8 56.47 6.56 0. 1.0000 0. 0 10 -8 82.53 3.43 0. 1.0000 0. 0 10 -9 0.75 2.11 0. 1.0000 0. 0 -10 9 3.72 4.74 0. 1.0000 0. 0 10 -9 0.26 1.37 0. 1.0000 0. 0 10 -10 29.16 3.40 0. 1.0000 0. 0 -10 10 30.84 4.87 0. 1.0000 0. 0 10 -11 48.45 5.07 0. 1.0000 0. 0 -10 11 69.58 5.63 0. 1.0000 0. 0 10 -11 77.34 5.02 0. 1.0000 0. 0 -10 12 7.74 3.88 0. 1.0000 0. 0 10 -12 1.85 3.33 0. 1.0000 0. 0 -10 13 186.81 7.78 0. 1.0000 0. 0 10 -13 106.97 6.63 0. 1.0000 0. 0 -10 14 18.72 4.13 0. 1.0000 0. 0 10 -14 8.02 3.47 0. 1.0000 0. 0 -10 15 2.24 3.54 0. 1.0000 0. 0 -11 3 4.62 5.03 0. 1.0000 0. 0 -11 3 3.35 1.80 0. 1.0000 0. 0 11 -4 7.50 1.46 0. 1.0000 0. 0 -11 4 8.28 1.79 0. 1.0000 0. 0 -11 4 7.74 4.17 0. 1.0000 0. 0 -11 5 56.77 2.67 0. 1.0000 0. 0 -11 5 56.55 5.21 0. 1.0000 0. 0 11 -5 49.16 2.53 0. 1.0000 0. 0 11 -6 47.89 2.42 0. 1.0000 0. 0 -11 6 47.31 2.62 0. 1.0000 0. 0 -11 6 41.46 5.02 0. 1.0000 0. 0 -11 6 36.77 10.80 0. 1.0000 0. 0 -11 7 30.12 10.88 0. 1.0000 0. 0 11 -7 27.55 2.06 0. 1.0000 0. 0 -11 7 32.69 6.31 0. 1.0000 0. 0 -11 7 26.89 1.70 0. 1.0000 0. 0 11 -8 3.63 1.77 0. 1.0000 0. 0 -11 8 1.50 6.38 0. 1.0000 0. 0 11 -8 3.12 1.74 0. 1.0000 0. 0 11 -8 2.49 1.75 0. 1.0000 0. 0 -11 8 2.75 7.12 0. 1.0000 0. 0 -11 8 2.82 1.34 0. 1.0000 0. 0 -11 9 184.93 11.10 0. 1.0000 0. 0 11 -9 194.19 6.62 0. 1.0000 0. 0 -11 10 27.40 6.46 0. 1.0000 0. 0 11 -10 17.43 2.95 0. 1.0000 0. 0 11 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8.95 3.78 0. 1.0000 0. 3 -6 -1 8.43 4.57 0. 1.0000 0. 3 -6 -1 7.30 1.82 0. 1.0000 0. -3 -6 2 203.07 3.58 0. 1.0000 0. 3 6 -2 218.14 4.48 0. 1.0000 0. 3 6 -3 1.80 2.13 0. 1.0000 0. 3 6 -5 25.63 2.08 0. 1.0000 0. 3 6 -6 20.23 2.25 0. 1.0000 0. 3 6 -7 1.15 5.74 0. 1.0000 0. 3 6 -7 8.39 2.33 0. 1.0000 0. 3 6 -8 32.88 3.38 0. 1.0000 0. 3 6 -8 17.56 5.98 0. 1.0000 0. 3 6 -9 -0.67 5.65 0. 1.0000 0. 3 6 -9 1.22 3.80 0. 1.0000 0. -3 7 -9 15.09 2.60 0. 1.0000 0. 3 -7 9 19.79 6.89 0. 1.0000 0. 3 -7 9 14.83 4.34 0. 1.0000 0. -3 7 -8 -0.54 2.44 0. 1.0000 0. 3 -7 8 -6.88 7.03 0. 1.0000 0. 3 -7 8 3.08 4.02 0. 1.0000 0. -3 7 -7 3.70 2.47 0. 1.0000 0. 3 -7 7 2.34 7.62 0. 1.0000 0. 3 -7 7 -0.35 3.45 0. 1.0000 0. -3 7 -6 10.33 2.53 0. 1.0000 0. -3 7 -5 21.98 3.01 0. 1.0000 0. 3 -7 5 13.42 8.83 0. 1.0000 0. 3 -7 4 10.73 8.14 0. 1.0000 0. -3 7 -3 5.66 4.01 0. 1.0000 0. 3 -7 3 0.76 6.07 0. 1.0000 0. -3 7 -2 0.27 3.31 0. 1.0000 0. 3 7 2 -1.36 1.23 0. 1.0000 0. -3 7 -2 2.94 3.59 0. 1.0000 0. 3 -7 2 1.77 5.43 0. 1.0000 0. 3 7 1 52.54 2.76 0. 1.0000 0. -3 7 -1 47.97 4.68 0. 1.0000 0. -3 7 -1 53.54 4.19 0. 1.0000 0. 3 -7 1 36.45 5.97 0. 1.0000 0. -3 7 0 1.62 3.98 0. 1.0000 0. 3 7 0 3.40 1.78 0. 1.0000 0. -3 7 0 3.18 2.74 0. 1.0000 0. 3 -7 0 1.14 4.77 0. 1.0000 0. -3 -7 1 48.60 2.36 0. 1.0000 0. 3 7 -1 53.18 2.87 0. 1.0000 0. -3 7 1 51.14 3.47 0. 1.0000 0. 3 7 -2 3.97 1.88 0. 1.0000 0. 3 7 -3 1.19 2.16 0. 1.0000 0. 3 7 -4 17.99 2.60 0. 1.0000 0. 3 7 -6 36.02 2.61 0. 1.0000 0. 3 7 -7 -1.52 2.13 0. 1.0000 0. 3 7 -8 -1.09 2.65 0. 1.0000 0. 3 -8 9 -5.14 7.72 0. 1.0000 0. 3 -8 9 2.40 4.21 0. 1.0000 0. -3 8 -8 0.23 2.53 0. 1.0000 0. 3 -8 8 0.26 8.43 0. 1.0000 0. 3 -8 8 -1.76 3.60 0. 1.0000 0. -3 8 -7 2.07 2.65 0. 1.0000 0. 3 -8 7 -0.98 9.71 0. 1.0000 0. 3 -8 7 0.88 3.56 0. 1.0000 0. -3 8 -5 7.74 2.97 0. 1.0000 0. 3 -8 5 3.47 8.62 0. 1.0000 0. -3 8 -4 2.90 3.24 0. 1.0000 0. -3 8 -4 2.30 4.63 0. 1.0000 0. 3 -8 4 3.83 7.59 0. 1.0000 0. -3 8 -3 145.77 6.93 0. 1.0000 0. 3 -8 3 96.42 9.24 0. 1.0000 0. -3 8 -2 2.54 3.55 0. 1.0000 0. 3 -8 2 3.07 5.46 0. 1.0000 0. -3 8 -1 67.86 5.32 0. 1.0000 0. 3 -8 1 44.44 6.46 0. 1.0000 0. 3 8 0 61.51 3.02 0. 1.0000 0. -3 8 0 42.55 4.55 0. 1.0000 0. -3 8 0 62.10 3.79 0. 1.0000 0. 3 8 -1 3.57 1.96 0. 1.0000 0. 3 8 -2 43.55 2.98 0. 1.0000 0. 3 8 -3 307.31 9.74 0. 1.0000 0. 3 8 -4 35.19 3.02 0. 1.0000 0. 3 8 -5 1.24 2.61 0. 1.0000 0. 3 8 -6 3.01 1.85 0. 1.0000 0. 3 8 -7 1.23 2.19 0. 1.0000 0. 3 8 -8 6.45 2.68 0. 1.0000 0. -3 9 -8 1.56 2.82 0. 1.0000 0. 3 -9 8 -6.88 10.75 0. 1.0000 0. 3 -9 8 1.94 3.64 0. 1.0000 0. -3 9 -7 9.10 3.02 0. 1.0000 0. -3 9 -6 15.24 3.32 0. 1.0000 0. 3 -9 6 16.55 10.10 0. 1.0000 0. -3 9 -5 4.66 3.38 0. 1.0000 0. -3 9 -5 5.10 4.48 0. 1.0000 0. 3 -9 5 -1.43 8.75 0. 1.0000 0. -3 9 -4 34.34 4.08 0. 1.0000 0. -3 9 -4 31.49 4.84 0. 1.0000 0. 3 -9 4 31.51 8.07 0. 1.0000 0. -3 9 -3 4.01 3.87 0. 1.0000 0. -3 9 -3 7.62 4.12 0. 1.0000 0. 3 -9 3 0.76 6.13 0. 1.0000 0. -3 9 -2 55.93 4.38 0. 1.0000 0. 3 -9 2 36.21 6.72 0. 1.0000 0. 3 -9 1 1.01 5.63 0. 1.0000 0. 3 -9 1 6.26 2.17 0. 1.0000 0. 3 9 0 -0.40 1.60 0. 1.0000 0. 3 -9 0 -3.29 4.87 0. 1.0000 0. 3 9 -1 92.13 4.16 0. 1.0000 0. 3 9 -2 8.29 2.17 0. 1.0000 0. 3 9 -3 3.29 2.11 0. 1.0000 0. 3 9 -4 14.93 2.70 0. 1.0000 0. 3 9 -5 2.01 2.61 0. 1.0000 0. 3 9 -7 4.63 2.20 0. 1.0000 0. -3 10 -6 2.74 3.46 0. 1.0000 0. 3 -10 6 1.34 10.21 0. 1.0000 0. -3 10 -5 0.74 3.73 0. 1.0000 0. -3 10 -5 -1.78 4.58 0. 1.0000 0. 3 -10 5 -4.74 8.74 0. 1.0000 0. -3 10 -4 -1.30 4.05 0. 1.0000 0. -3 10 -4 1.65 4.39 0. 1.0000 0. 3 -10 4 3.59 7.44 0. 1.0000 0. -3 10 -3 31.43 4.83 0. 1.0000 0. -3 10 -3 42.34 4.41 0. 1.0000 0. 3 -10 3 21.17 6.88 0. 1.0000 0. -3 10 -2 3.28 4.46 0. 1.0000 0. -3 10 -2 -2.54 3.19 0. 1.0000 0. 3 -10 2 2.06 2.23 0. 1.0000 0. 3 -10 2 2.95 5.95 0. 1.0000 0. -3 10 -1 -0.29 2.78 0. 1.0000 0. 3 -10 1 0.91 5.51 0. 1.0000 0. 3 -10 1 2.33 2.02 0. 1.0000 0. 3 10 -1 0.33 1.82 0. 1.0000 0. 3 10 -2 104.25 4.60 0. 1.0000 0. 3 10 -3 120.64 5.13 0. 1.0000 0. 3 10 -4 4.25 2.60 0. 1.0000 0. 3 10 -5 10.42 3.00 0. 1.0000 0. 3 10 -6 7.48 3.10 0. 1.0000 0. -3 11 -5 41.11 5.27 0. 1.0000 0. -3 11 -5 26.33 4.58 0. 1.0000 0. 3 -11 5 28.92 9.69 0. 1.0000 0. -3 11 -4 2.62 4.17 0. 1.0000 0. -3 11 -4 -1.17 4.85 0. 1.0000 0. 3 -11 4 5.26 7.57 0. 1.0000 0. -3 11 -3 38.22 4.28 0. 1.0000 0. -3 11 -3 30.99 5.36 0. 1.0000 0. -3 11 -2 -0.91 2.43 0. 1.0000 0. -3 11 -2 0.58 3.08 0. 1.0000 0. 3 -11 2 0.35 2.33 0. 1.0000 0. 3 -11 2 -0.20 5.80 0. 1.0000 0. 3 11 -2 -0.14 2.17 0. 1.0000 0. 3 11 -3 -1.86 2.52 0. 1.0000 0. 3 11 -4 15.21 2.80 0. 1.0000 0. -3 12 -3 -1.98 2.79 0. 1.0000 0. -3 12 -3 -1.82 3.36 0. 1.0000 0. 3 12 -2 0.30 1.87 0. 1.0000 0. -512 # 2472 reflections output ; # end of ARCHIVE-HKL.CIF _chemical_name_common ROY _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: acetone'