data_mg0007 _audit_creation_date "10-06-21" _audit_creation_method CRYSTALS_ver_14.09 _oxford_structure_analysis_title 'mg0007 in P2(1)/n' _chemical_name_systematic ? _chemical_melting_point ? #looking for refcif _publ_contact_author_name 'Simon Parsons' _publ_contact_author_email 'S.Parsons@ed.ac.uk' _publ_section_exptl_refinement ; H atoms placed geometrically after each cycle Checkcif Alerts: 795_ALERT_4_B C-Atom in CIF Coordinate List out of Sequence .. C9 No action taken. 061_ALERT_4_G Tmax/Tmin Range Test RR' too Large ............. 0.80 Multiscan procedures correct for all systematic errors that lead to disparities in the intensities of symmetry-equivalent data. These may include absorption by the mount, crystal decay, changes in the volume of the crystal illuminated, etc. 911_ALERT_3_G Missing # FCF Refl Between THmin & STh/L= 0.600 3 912_ALERT_4_G Missing # of FCF Reflections Above STh/L= 0.600 71 The data collection strategy used aimed to achieve a complete data set to d = 0.84 Ang. Some higher angle data were collected in the process and these have been included in the refinement. ================================================================================ Resolution & Completeness Statistics (Cumulative) ================================================================================ Theta sin(th)/Lambda Complete Expected Measured Missing -------------------------------------------------------------------------------- 50.43 0.500 0.999 1399 1398 1 57.99 0.550 0.999 1856 1855 1 67.68 0.600 0.999 2421 2418 3 ------------------------------------------------------------ ACTA Min. Res. ---- 73.28 0.621 0.973 2693 2619 74 ; #end of refcif _cell_length_a 11.8879(3) _cell_length_b 9.0693(3) _cell_length_c 12.4154(3) _cell_angle_alpha 90 _cell_angle_beta 92.315(2) _cell_angle_gamma 90 _cell_volume 1337.47(6) _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall '-P 2yn ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0311 0.0180 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 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0727 0.0534 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C18 H14 F1 N1 O1 # Dc = 1.39 Fooo = 584.00 Mu = 7.78 M = 279.31 # Found Formula = C18 H14 F1 N1 O1 # Dc = 1.39 FOOO = 584.00 Mu = 7.78 M = 279.31 _chemical_formula_sum 'C18 H14 F1 N1 O1' _chemical_formula_moiety 'C18 H14 F1 N1 O1' _chemical_compound_source 'Didier Pintori - reaction DP803B' _chemical_formula_weight 279.31 _cell_measurement_reflns_used 7036 _cell_measurement_theta_min 4 _cell_measurement_theta_max 73 _cell_measurement_temperature 100 _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_size_min 0.070 _exptl_crystal_size_mid 0.170 _exptl_crystal_size_max 0.170 _exptl_crystal_density_diffrn 1.387 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 584 _exptl_absorpt_coefficient_mu 0.778 # Sheldrick geometric approximatio 0.88 0.95 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.70 _exptl_absorpt_correction_T_max 0.95 _diffrn_measurement_device_type 'Oxford Diffraction XCALIBUR' _diffrn_measurement_device 'Area' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54178 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'CrysAlis CCD, (Oxford Diffraction, 2002)' _computing_cell_refinement 'CrysAlis RED, (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis RED, (Oxford Diffraction, 2002)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 100 _diffrn_reflns_number 10234 _reflns_number_total 2619 _diffrn_reflns_av_R_equivalents 0.026 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 2619 # Theoretical number of reflections is about 5371 _diffrn_reflns_theta_min 5.050 _diffrn_reflns_theta_max 73.277 _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 68.880 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -14 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 10 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _oxford_diffrn_Wilson_B_factor 2.12 _oxford_diffrn_Wilson_scale 3.28 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.24 _refine_diff_density_max 0.21 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 2617 _refine_ls_number_restraints 0 _refine_ls_number_parameters 190 _oxford_refine_ls_R_factor_ref 0.0429 _refine_ls_wR_factor_ref 0.1024 _refine_ls_goodness_of_fit_ref 0.9536 _refine_ls_shift/su_max 0.0002882 _refine_ls_shift/su_mean 0.0000364 # The values computed from all data _oxford_reflns_number_all 2617 _refine_ls_R_factor_all 0.0429 _refine_ls_wR_factor_all 0.1024 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2191 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_gt 0.0995 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration '.' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.07P)^2^ + 0.43P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Oxford Diffraction, (2002). CrysAlis RED. Oxford Diffraction, (2002). Xcalibur User Manual. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens N1 N 0.63281(9) -0.01830(12) 0.43737(8) 0.0224 1.0000 Uani . . . . . . C2 C 0.59721(10) -0.09912(15) 0.34715(10) 0.0231 1.0000 Uani . . . . . . C3 C 0.56868(11) -0.24779(15) 0.33845(11) 0.0274 1.0000 Uani . . . . . . C4 C 0.53745(11) -0.29932(15) 0.23668(12) 0.0304 1.0000 Uani . . . . . . C5 C 0.53504(11) -0.20676(16) 0.14604(11) 0.0295 1.0000 Uani . . . . . . C6 C 0.56409(11) -0.05950(16) 0.15522(10) 0.0264 1.0000 Uani . . . . . . C7 C 0.59492(10) -0.00361(14) 0.25754(10) 0.0232 1.0000 Uani . . . . . . C8 C 0.63195(10) 0.13900(14) 0.29683(10) 0.0232 1.0000 Uani . . . . . . C81 C 0.64945(11) 0.27133(15) 0.23518(11) 0.0265 1.0000 Uani . . . . . . O82 O 0.61959(9) 0.28698(12) 0.14044(8) 0.0346 1.0000 Uani . . . . . . C9 C 0.65464(10) 0.12340(14) 0.40686(10) 0.0221 1.0000 Uani . . . . . . C10 C 0.69957(10) 0.22920(14) 0.48772(10) 0.0229 1.0000 Uani . . . . . . C11 C 0.65460(11) 0.36942(15) 0.49792(10) 0.0252 1.0000 Uani . . . . . . F11 F 0.56293(7) 0.40598(9) 0.43416(6) 0.0298 1.0000 Uani . . . . . . C12 C 0.69718(12) 0.47289(15) 0.56993(11) 0.0280 1.0000 Uani . . . . . . C13 C 0.78964(12) 0.43384(16) 0.63537(11) 0.0294 1.0000 Uani . . . . . . C14 C 0.83594(11) 0.29348(15) 0.62954(11) 0.0278 1.0000 Uani . . . . . . C15 C 0.79231(10) 0.18981(15) 0.55648(10) 0.0243 1.0000 Uani . . . . . . C16 C 0.84578(11) 0.03980(15) 0.54354(10) 0.0259 1.0000 Uani . . . . . . C17 C 0.77404(11) -0.09163(15) 0.57950(10) 0.0263 1.0000 Uani . . . . . . C18 C 0.64932(11) -0.07174(15) 0.54790(10) 0.0254 1.0000 Uani . . . . . . H3 H 0.5706 -0.3109 0.3996 0.0329 1.0000 Uiso . . . . . . H4 H 0.5171 -0.4000 0.2279 0.0365 1.0000 Uiso . . . . . . H5 H 0.5131 -0.2458 0.0774 0.0354 1.0000 Uiso . . . . . . H6 H 0.5632 0.0025 0.0935 0.0317 1.0000 Uiso . . . . . . H8 H 0.6866 0.3516 0.2705 0.0318 1.0000 Uiso . . . . . . H12 H 0.6642 0.5680 0.5746 0.0336 1.0000 Uiso . . . . . . H13 H 0.8217 0.5037 0.6847 0.0353 1.0000 Uiso . . . . . . H14 H 0.8983 0.2679 0.6761 0.0334 1.0000 Uiso . . . . . . H161 H 0.9176 0.0386 0.5867 0.0311 1.0000 Uiso . . . . . . H162 H 0.8612 0.0262 0.4664 0.0311 1.0000 Uiso . . . . . . H171 H 0.7823 -0.1013 0.6589 0.0315 1.0000 Uiso . . . . . . H172 H 0.8016 -0.1825 0.5452 0.0315 1.0000 Uiso . . . . . . H181 H 0.6163 0.0003 0.5975 0.0305 1.0000 Uiso . . . . . . H182 H 0.6107 -0.1678 0.5544 0.0305 1.0000 Uiso . . . . . . 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 N1 0.0218(5) 0.0211(5) 0.0240(5) 0.0012(4) -0.0016(4) 0.0006(4) C2 0.0186(6) 0.0246(7) 0.0259(6) -0.0015(5) -0.0004(5) 0.0017(5) C3 0.0245(7) 0.0234(7) 0.0341(7) 0.0014(5) -0.0010(5) -0.0003(5) C4 0.0265(7) 0.0239(7) 0.0406(8) -0.0041(6) -0.0025(5) -0.0013(5) C5 0.0241(7) 0.0326(8) 0.0316(7) -0.0074(6) -0.0034(5) 0.0009(5) C6 0.0210(6) 0.0311(7) 0.0271(6) -0.0004(5) -0.0012(5) 0.0005(5) C7 0.0182(6) 0.0239(7) 0.0275(6) 0.0006(5) -0.0002(5) 0.0008(5) C8 0.0190(6) 0.0237(7) 0.0268(6) 0.0007(5) -0.0010(4) 0.0009(5) C81 0.0228(6) 0.0258(7) 0.0309(7) 0.0025(5) -0.0005(5) -0.0010(5) O82 0.0362(6) 0.0362(6) 0.0309(5) 0.0099(4) -0.0041(4) -0.0044(4) C9 0.0176(6) 0.0207(6) 0.0278(6) 0.0005(5) 0.0003(4) 0.0014(4) C10 0.0207(6) 0.0237(7) 0.0243(6) 0.0001(5) 0.0011(5) -0.0005(5) C11 0.0221(6) 0.0250(7) 0.0283(6) 0.0023(5) -0.0011(5) 0.0002(5) F11 0.0276(4) 0.0249(4) 0.0364(4) 0.0004(3) -0.0053(3) 0.0048(3) C12 0.0288(7) 0.0219(7) 0.0335(7) -0.0026(5) 0.0032(5) -0.0005(5) C13 0.0294(7) 0.0292(7) 0.0294(7) -0.0050(5) 0.0004(5) -0.0047(5) C14 0.0239(6) 0.0321(7) 0.0271(6) -0.0010(5) -0.0023(5) -0.0005(5) C15 0.0211(6) 0.0266(7) 0.0252(6) -0.0001(5) 0.0018(5) 0.0007(5) C16 0.0221(6) 0.0283(7) 0.0270(6) -0.0007(5) -0.0019(5) 0.0039(5) C17 0.0265(6) 0.0267(7) 0.0254(6) 0.0024(5) -0.0014(5) 0.0051(5) C18 0.0275(7) 0.0247(7) 0.0239(6) 0.0030(5) -0.0001(5) 0.0016(5) _refine_ls_extinction_method 'None' _oxford_refine_ls_scale 0.5459(14) 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 N1 . C2 . 1.3902(16) yes N1 . C9 . 1.3676(16) yes N1 . C18 . 1.4611(16) yes C2 . C3 . 1.3934(19) yes C2 . C7 . 1.4094(18) yes C3 . C4 . 1.384(2) yes C3 . H3 . 0.950 no C4 . C5 . 1.403(2) yes C4 . H4 . 0.950 no C5 . C6 . 1.383(2) yes C5 . H5 . 0.950 no C6 . C7 . 1.4027(18) yes C6 . H6 . 0.950 no C7 . C8 . 1.4447(18) yes C8 . C81 . 1.4430(18) yes C8 . C9 . 1.3888(17) yes C81 . O82 . 1.2231(17) yes C81 . H8 . 0.950 no C9 . C10 . 1.4733(17) yes C10 . C11 . 1.3873(19) yes C10 . C15 . 1.4128(17) yes C11 . F11 . 1.3617(15) yes C11 . C12 . 1.3782(19) yes C12 . C13 . 1.386(2) yes C12 . H12 . 0.950 no C13 . C14 . 1.390(2) yes C13 . H13 . 0.950 no C14 . C15 . 1.3921(19) yes C14 . H14 . 0.950 no C15 . C16 . 1.5129(18) yes C16 . C17 . 1.5421(19) yes C16 . H161 . 0.990 no C16 . H162 . 0.990 no C17 . C18 . 1.5290(18) yes C17 . H171 . 0.990 no C17 . H172 . 0.990 no C18 . H181 . 0.990 no C18 . H182 . 0.990 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 . N1 . C9 . 109.10(10) yes C2 . N1 . C18 . 127.36(11) yes C9 . N1 . C18 . 123.51(11) yes N1 . C2 . C3 . 129.63(12) yes N1 . C2 . C7 . 107.91(11) yes C3 . C2 . C7 . 122.45(12) yes C2 . C3 . C4 . 116.94(12) yes C2 . C3 . H3 . 121.5 no C4 . C3 . H3 . 121.5 no C3 . C4 . C5 . 121.75(13) yes C3 . C4 . H4 . 119.1 no C5 . C4 . H4 . 119.1 no C4 . C5 . C6 . 120.97(13) yes C4 . C5 . H5 . 119.5 no C6 . C5 . H5 . 119.5 no C5 . C6 . C7 . 118.61(12) yes C5 . C6 . H6 . 120.7 no C7 . C6 . H6 . 120.7 no C2 . C7 . C6 . 119.26(12) yes C2 . C7 . C8 . 106.72(11) yes C6 . C7 . C8 . 133.97(12) yes C7 . C8 . C81 . 127.87(12) yes C7 . C8 . C9 . 106.58(11) yes C81 . C8 . C9 . 125.45(12) yes C8 . C81 . O82 . 124.34(12) yes C8 . C81 . H8 . 117.8 no O82 . C81 . H8 . 117.8 no C8 . C9 . N1 . 109.68(11) yes C8 . C9 . C10 . 130.88(12) yes N1 . C9 . C10 . 119.40(11) yes C9 . C10 . C11 . 121.92(11) yes C9 . C10 . C15 . 119.98(12) yes C11 . C10 . C15 . 118.09(12) yes C10 . C11 . F11 . 118.20(11) yes C10 . C11 . C12 . 123.40(12) yes F11 . C11 . C12 . 118.40(12) yes C11 . C12 . C13 . 117.91(13) yes C11 . C12 . H12 . 121.0 no C13 . C12 . H12 . 121.0 no C12 . C13 . C14 . 120.65(12) yes C12 . C13 . H13 . 119.7 no C14 . C13 . H13 . 119.7 no C13 . C14 . C15 . 120.97(12) yes C13 . C14 . H14 . 119.5 no C15 . C14 . H14 . 119.5 no C10 . C15 . C14 . 118.95(12) yes C10 . C15 . C16 . 118.96(11) yes C14 . C15 . C16 . 121.97(12) yes C15 . C16 . C17 . 115.13(11) yes C15 . C16 . H161 . 108.0 no C17 . C16 . H161 . 108.0 no C15 . C16 . H162 . 108.0 no C17 . C16 . H162 . 108.0 no H161 . C16 . H162 . 109.5 no C16 . C17 . C18 . 112.11(10) yes C16 . C17 . H171 . 108.8 no C18 . C17 . H171 . 108.8 no C16 . C17 . H172 . 108.8 no C18 . C17 . H172 . 108.8 no H171 . C17 . H172 . 109.5 no C17 . C18 . N1 . 111.85(11) yes C17 . C18 . H181 . 108.9 no N1 . C18 . H181 . 108.9 no C17 . C18 . H182 . 108.9 no N1 . C18 . H182 . 108.9 no H181 . C18 . H182 . 109.5 no