data_PR202_123K _audit_creation_date "2016-10-05" _audit_creation_method CRYSTALS_ver_14.61_build_5809 _oxford_structure_analysis_title 'mono in C2/c' _chemical_name_systematic ? _chemical_melting_point ? _publ_contact_author_name 'Alessandro Prescimone' _publ_requested_coeditor_name 'Alessandro.Prescimone@unibas.ch' _publ_contact_author_address 'University of Basel' _chemical_compound_source 'P. Ravat' _exptl_crystal_recrystallization_method ; CDCl3 ; _publ_section_exptl_refinement ; The H atoms were all found in the difference map U~iso~(H) (in the range 1.2 times U~eq~ of the parent atom), the positions were refined with riding constraints. see the bottom part of the file for the full list of the applied restraints. -------------------------------------------------------------------------------- CHECKCIF OUTPUT: -------------------------------------------------------------------------------- 911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.600 10 Report #=============================================================================== 008_ALERT_5_G No _iucr_refine_reflections_details in the CIF Please Do ! 760_ALERT_1_G CIF Contains no Torsion Angles ................. ? Info 808_ALERT_5_G No Parseable SHELXL Style Weighting Scheme Found Please Check 910_ALERT_3_G Missing # of FCF Reflection(s) Below Th(Min) ... 1 Report 912_ALERT_4_G Missing # of FCF Reflections Above STh/L= 0.600 40 Note 913_ALERT_3_G Missing # of Very Strong Reflections in FCF .... 2 Note 929_ALERT_5_G No Weight Pars,Obs and Calc R1,wR2,S not checked ! Info 978_ALERT_2_G Number C-C Bonds with Positive Residual Density 21 Note #=============================================================================== ; _cell_length_a 9.2601(11) _cell_length_b 14.9860(11) _cell_length_c 14.9657(14) _cell_angle_alpha 90 _cell_angle_beta 107.491(4) _cell_angle_gamma 90 _cell_volume 1980.8(3) _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_space_group_name_Hall ' -C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' 'x+1/2,y+1/2,z' '-x+1/2,-y+1/2,-z' 'x,-y,z+1/2' '-x,y,-z+1/2' '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' 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' _cell_formula_units_Z 4 # Given Formula = C30 H22 O2 # Dc = 1.39 Fooo = 872.00 Mu = 6.70 M = 414.50 # Found Formula = C30 H22 O2 # Dc = 1.39 FOOO = 872.00 Mu = 6.70 M = 414.50 _chemical_formula_sum 'C30 H22 O2' _chemical_formula_moiety 'C30 H22 O2' _chemical_formula_weight 414.50 _cell_measurement_reflns_used 9961 _cell_measurement_theta_min 3 _cell_measurement_theta_max 70 _cell_measurement_temperature 123 _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_min 0.040 _exptl_crystal_size_mid 0.080 _exptl_crystal_size_max 0.080 _exptl_crystal_density_diffrn 1.390 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 0.670 # Sheldrick geometric approximatio 0.95 0.97 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 0.97 _diffrn_measurement_device_type 'Bruker Kappa Apex2' _diffrn_measurement_device 'Area' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54178 _diffrn_measurement_method \w/2\q # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _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 123 _diffrn_reflns_number 12679 _reflns_number_total 1855 _diffrn_reflns_av_R_equivalents 0.033 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 1855 # Theoretical number of reflections is about 3778 _diffrn_reflns_theta_min 5.838 _diffrn_reflns_theta_max 70.299 _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 68.000 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 18 _reflns_limit_h_min -11 _reflns_limit_h_max 10 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 18 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary Other #heavy,direct,difmap,geom,iterative # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.17 _refine_diff_density_max 0.22 # 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>-3.0\s(I) _refine_ls_number_reflns 1837 _refine_ls_number_restraints 0 _refine_ls_number_parameters 145 _oxford_refine_ls_R_factor_ref 0.0357 _refine_ls_wR_factor_ref 0.0830 _refine_ls_goodness_of_fit_ref 0.9553 _refine_ls_shift/su_max 0.0005254 _refine_ls_shift/su_mean 0.0000955 # The values computed with all filters except I/sigma _oxford_reflns_number_all 1839 _refine_ls_R_factor_all 0.0357 _refine_ls_wR_factor_all 0.0830 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 1826 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_gt 0.0826 # 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 constr #undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 2.29 3.04 0.819 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Bruker Analytical X-ray Systems, Inc., 2006. Apex2, Version 2 User Manual, M86-E01078, Madison, WI. Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # 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 O1 O 0.41008(10) 0.65433(6) 0.60187(6) 0.0378 1.0000 Uani . . . . . . C2 C 0.44952(11) 0.72159(7) 0.56952(7) 0.0265 1.0000 Uani . . . . . . C3 C 0.49962(11) 0.71858(7) 0.48392(7) 0.0217 1.0000 Uani . . . . . . C4 C 0.55519(10) 0.79826(6) 0.45067(7) 0.0189 1.0000 Uani . . . . . . C5 C 0.57488(10) 0.79801(6) 0.35974(6) 0.0175 1.0000 Uani . . . . . . C6 C 0.51914(10) 0.72091(6) 0.30012(6) 0.0174 1.0000 Uani . . . . . . C7 C 0.50531(11) 0.63871(6) 0.34413(7) 0.0209 1.0000 Uani . . . . . . C8 C 0.49083(11) 0.64071(7) 0.43601(7) 0.0225 1.0000 Uani . . . . . . C9 C 0.49778(11) 0.55686(7) 0.29499(7) 0.0236 1.0000 Uani . . . . . . C10 C 0.65701(10) 0.86953(6) 0.33498(6) 0.0184 1.0000 Uani . . . . . . C11 C 0.69411(11) 0.94210(6) 0.39508(7) 0.0219 1.0000 Uani . . . . . . C12 C 0.66261(11) 0.94544(7) 0.48061(7) 0.0228 1.0000 Uani . . . . . . C13 C 0.59801(11) 0.87268(7) 0.51083(7) 0.0214 1.0000 Uani . . . . . . C14 C 0.58000(12) 0.86934(7) 0.60766(7) 0.0260 1.0000 Uani . . . . . . C15 C 0.44261(12) 0.81344(8) 0.60904(7) 0.0292 1.0000 Uani . . . . . . C16 C 0.71925(11) 0.86765(6) 0.25256(7) 0.0219 1.0000 Uani . . . . . . H81 H 0.4700 0.5852 0.4629 0.0280 1.0000 Uiso R . . . . . H91 H 0.4929 0.4996 0.3247 0.0277 1.0000 Uiso R . . . . . H111 H 0.7473 0.9932 0.3787 0.0257 1.0000 Uiso R . . . . . H121 H 0.6913 0.9982 0.5208 0.0269 1.0000 Uiso R . . . . . H141 H 0.5719 0.9316 0.6310 0.0329 1.0000 Uiso R . . . . . H142 H 0.6760 0.8421 0.6516 0.0316 1.0000 Uiso R . . . . . H152 H 0.4323 0.8085 0.6719 0.0351 1.0000 Uiso R . . . . . H151 H 0.3450 0.8435 0.5690 0.0350 1.0000 Uiso R . . . . . H162 H 0.8208 0.8956 0.2704 0.0347 1.0000 Uiso R . . . . . H161 H 0.7259 0.8052 0.2294 0.0338 1.0000 Uiso R . . . . . H163 H 0.6533 0.9025 0.2000 0.0340 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 O1 0.0398(5) 0.0433(5) 0.0338(4) 0.0120(4) 0.0162(4) -0.0047(4) C2 0.0181(5) 0.0364(6) 0.0226(5) 0.0073(4) 0.0027(4) -0.0016(4) C3 0.0152(4) 0.0258(5) 0.0222(5) 0.0054(4) 0.0029(4) 0.0006(4) C4 0.0126(4) 0.0212(5) 0.0214(4) 0.0028(4) 0.0026(3) 0.0018(3) C5 0.0136(4) 0.0162(4) 0.0210(5) 0.0020(3) 0.0029(3) 0.0024(3) C6 0.0119(4) 0.0161(5) 0.0244(5) 0.0014(4) 0.0056(3) 0.0014(3) C7 0.0139(5) 0.0191(5) 0.0277(5) 0.0027(4) 0.0033(4) -0.0008(3) C8 0.0167(5) 0.0205(5) 0.0283(5) 0.0081(4) 0.0040(4) -0.0010(4) C9 0.0185(5) 0.0150(4) 0.0354(5) 0.0034(4) 0.0054(4) -0.0007(3) C10 0.0150(5) 0.0180(5) 0.0207(5) 0.0008(4) 0.0031(4) 0.0006(3) C11 0.0188(5) 0.0181(5) 0.0273(5) 0.0000(4) 0.0050(4) -0.0018(3) C12 0.0195(5) 0.0214(5) 0.0252(5) -0.0052(4) 0.0031(4) -0.0004(4) C13 0.0155(5) 0.0255(5) 0.0214(5) -0.0004(4) 0.0029(4) 0.0032(4) C14 0.0220(5) 0.0342(6) 0.0208(5) -0.0028(4) 0.0047(4) 0.0009(4) C15 0.0240(5) 0.0441(6) 0.0200(5) 0.0001(5) 0.0073(4) -0.0007(5) C16 0.0203(5) 0.0216(5) 0.0235(5) -0.0002(4) 0.0061(4) -0.0051(4) _refine_ls_extinction_method 'None' _oxford_refine_ls_scale 0.11047(5) 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 O1 . C2 . 1.2207(13) yes C2 . C3 . 1.4885(14) yes C2 . C15 . 1.5070(16) yes C3 . C4 . 1.4465(13) yes C3 . C8 . 1.3591(14) yes C4 . C5 . 1.4262(13) yes C4 . C13 . 1.4132(14) yes C5 . C6 . 1.4563(13) yes C5 . C10 . 1.4261(13) yes C6 . C6 6_655 1.4340(18) yes C6 . C7 . 1.4207(13) yes C7 . C8 . 1.4214(15) yes C7 . C9 . 1.4210(14) yes C8 . H81 . 0.969 no C9 . C9 6_655 1.360(2) yes C9 . H91 . 0.974 no C10 . C11 . 1.3871(14) yes C10 . C16 . 1.5106(13) yes C11 . C12 . 1.3965(14) yes C11 . H111 . 0.981 no C12 . C13 . 1.3835(14) yes C12 . H121 . 0.981 no C13 . C14 . 1.5086(14) yes C14 . C15 . 1.5286(15) yes C14 . H141 . 1.008 no C14 . H142 . 1.019 no C15 . H152 . 0.977 no C15 . H151 . 1.026 no C16 . H162 . 0.990 no C16 . H161 . 1.006 no C16 . H163 . 0.988 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 O1 . C2 . C3 . 121.61(10) yes O1 . C2 . C15 . 123.05(9) yes C3 . C2 . C15 . 115.25(9) yes C2 . C3 . C4 . 120.41(9) yes C2 . C3 . C8 . 119.69(9) yes C4 . C3 . C8 . 119.89(9) yes C3 . C4 . C5 . 119.13(9) yes C3 . C4 . C13 . 119.54(9) yes C5 . C4 . C13 . 121.20(9) yes C4 . C5 . C6 . 117.60(8) yes C4 . C5 . C10 . 118.49(8) yes C6 . C5 . C10 . 123.75(8) yes C5 . C6 . C6 6_655 124.86(6) yes C5 . C6 . C7 . 117.94(9) yes C6 6_655 C6 . C7 . 117.17(6) yes C6 . C7 . C8 . 118.56(9) yes C6 . C7 . C9 . 120.38(9) yes C8 . C7 . C9 . 120.97(9) yes C7 . C8 . C3 . 121.35(9) yes C7 . C8 . H81 . 118.2 no C3 . C8 . H81 . 120.4 no C7 . C9 . C9 6_655 120.08(6) yes C7 . C9 . H91 . 121.7 no C9 6_655 C9 . H91 . 118.1 no C5 . C10 . C11 . 117.93(9) yes C5 . C10 . C16 . 124.21(8) yes C11 . C10 . C16 . 117.59(8) yes C10 . C11 . C12 . 122.89(9) yes C10 . C11 . H111 . 119.7 no C12 . C11 . H111 . 117.4 no C11 . C12 . C13 . 120.09(9) yes C11 . C12 . H121 . 119.9 no C13 . C12 . H121 . 120.0 no C4 . C13 . C12 . 118.67(9) yes C4 . C13 . C14 . 119.67(9) yes C12 . C13 . C14 . 121.59(9) yes C13 . C14 . C15 . 111.34(8) yes C13 . C14 . H141 . 110.1 no C15 . C14 . H141 . 110.7 no C13 . C14 . H142 . 107.8 no C15 . C14 . H142 . 109.9 no H141 . C14 . H142 . 106.8 no C14 . C15 . C2 . 111.19(9) yes C14 . C15 . H152 . 112.1 no C2 . C15 . H152 . 109.7 no C14 . C15 . H151 . 110.0 no C2 . C15 . H151 . 107.8 no H152 . C15 . H151 . 105.8 no C10 . C16 . H162 . 109.7 no C10 . C16 . H161 . 112.2 no H162 . C16 . H161 . 109.5 no C10 . C16 . H163 . 110.1 no H162 . C16 . H163 . 107.5 no H161 . C16 . H163 . 107.7 no 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 C9 . H91 . O1 2_666 157 0.97 2.60 3.5122(14) yes _iucr_refine_instructions_details ; # # Punched on 05/10/16 at 15:24:43 # #LIST 12 BLOCK SCALE X'S U'S RIDE C ( 8,X'S) H ( 81,X'S) RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 11,X'S) H ( 111,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 14,X'S) H ( 141,X'S) H ( 142,X'S) RIDE C ( 15,X'S) H ( 152,X'S) H ( 151,X'S) RIDE C ( 16,X'S) H ( 162,X'S) H ( 161,X'S) H ( 163,X'S) END # # Punched on 05/10/16 at 15:24:43 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) 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 2 2 1 x . 2 0 0 x . 4 4 4 x . -1 1 7 x . -1 7 4 x . -7 11 12 x . -2 6 17 x . -4 4 6 x . -2 6 5 x .