# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Wagner, Matthias' _publ_contact_author_email Matthias.Wagner@chemie.uni-frankfurt.de _publ_section_title ; Thermally-induced crystal-to-crystal transformations accompanied by changes in the magnetic properties of a CuII-p-Hydroquinonate Polymer ; loop_ _publ_author_name N.Phan I.Halasz I.Opahle E.Alig L.Fink J.Bats P.Cong ; H.-W.Lerner ; B.Sarkar B.Wolf H.Jeschke M.Lang R.Valenti R.Dinnebier ; M.Wagner ; # Attachment '- Compd2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 780369' #TrackingRef '- Compd2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H34 Cu2 N6 O4, 2(C F3 S O3)' _chemical_formula_sum 'C30 H34 Cu2 F6 N6 O10 S2' _chemical_formula_weight 943.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.8327(16) _cell_length_b 19.556(4) _cell_length_c 12.624(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.82(3) _cell_angle_gamma 90.00 _cell_volume 1915.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 164(2) _cell_measurement_reflns_used 126 _cell_measurement_theta_min 3 _cell_measurement_theta_max 23 _exptl_crystal_description rod _exptl_crystal_colour black _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.636 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 1.309 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.33 _exptl_absorpt_correction_T_max 0.71 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 164(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type SIEMENS_SMART_CCD _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 221 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 1200 _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 23637 _diffrn_reflns_av_R_equivalents 0.1415 _diffrn_reflns_av_sigmaI/netI 0.1962 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 26.59 _reflns_number_total 7380 _reflns_number_gt 4256 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SMART (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.055P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.49(3) _refine_ls_number_reflns 7380 _refine_ls_number_parameters 509 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.1413 _refine_ls_R_factor_gt 0.0783 _refine_ls_wR_factor_ref 0.1743 _refine_ls_wR_factor_gt 0.1564 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.5691(5) 0.32613(18) 0.1275(3) 0.0542(9) Uani 1 1 d . . . O5 O 0.6310(11) 0.3354(5) 0.0262(7) 0.074(3) Uani 1 1 d . . . F2 F 0.8873(10) 0.3026(6) 0.2173(8) 0.110(3) Uani 1 1 d . . . F1 F 0.6930(11) 0.2610(7) 0.3022(8) 0.132(5) Uani 1 1 d . . . O6 O 0.4177(12) 0.2817(5) 0.1251(8) 0.075(3) Uani 1 1 d . . . F3 F 0.7526(13) 0.2167(5) 0.1565(12) 0.132(5) Uani 1 1 d . . . C29 C 0.726(2) 0.2748(9) 0.2048(12) 0.072(5) Uani 1 1 d . . . O7 O 0.5683(16) 0.3858(5) 0.1881(9) 0.098(4) Uani 1 1 d . . . S2 S 0.2764(5) 0.6280(2) 0.3363(3) 0.0679(11) Uani 1 1 d . . . O8 O 0.2608(12) 0.6307(5) 0.4462(7) 0.077(3) Uani 1 1 d . . . F4 F 0.3590(12) 0.7243(5) 0.2103(8) 0.103(3) Uani 1 1 d . . . F5 F 0.5086(15) 0.7188(8) 0.3695(10) 0.167(7) Uani 1 1 d . . . F6 F 0.2527(17) 0.7593(6) 0.3472(9) 0.134(4) Uani 1 1 d . . . O9 O 0.419(2) 0.5839(8) 0.3128(13) 0.168(8) Uani 1 1 d . . . C30 C 0.352(2) 0.7084(11) 0.3216(17) 0.096(7) Uani 1 1 d . . . O10 O 0.129(2) 0.6234(10) 0.2590(11) 0.199(9) Uani 1 1 d . . . Cu1 Cu 0.95289(14) 0.45050(6) 0.64413(10) 0.0258(4) Uani 1 1 d . . . N4 N -0.1620(10) 0.5678(4) 0.9594(6) 0.021(2) Uani 1 1 d . . . O1 O 0.8229(7) 0.4664(3) 0.7612(5) 0.0205(18) Uani 1 1 d . . . N2 N 1.1118(10) 0.4287(4) 0.5322(6) 0.025(2) Uani 1 1 d . . . C26 C -0.0568(13) 0.6523(6) 0.6783(9) 0.029(3) Uani 1 1 d . . . H26A H 0.0529 0.6390 0.6612 0.035 Uiso 1 1 calc R . . C23 C 1.0069(14) 0.3436(6) 0.8059(11) 0.043(3) Uani 1 1 d . . . H23A H 0.9041 0.3610 0.8279 0.051 Uiso 1 1 calc R . . N1 N 0.7988(10) 0.5122(4) 0.5499(7) 0.024(2) Uani 1 1 d U . . N3 N 0.1641(10) 0.4952(4) 0.9485(7) 0.027(2) Uani 1 1 d U . . C8 C 0.8584(13) 0.5372(7) 0.4492(9) 0.043(3) Uani 1 1 d . . . H8A H 0.9576 0.5684 0.4672 0.051 Uiso 1 1 calc R . . H8B H 0.7644 0.5631 0.4067 0.051 Uiso 1 1 calc R . . C16 C 0.1229(13) 0.4804(7) 1.0553(11) 0.054(4) Uani 1 1 d . . . H16A H 0.1494 0.5211 1.1014 0.065 Uiso 1 1 calc R . . H16B H 0.1961 0.4422 1.0866 0.065 Uiso 1 1 calc R . . C1 C 0.6519(11) 0.4804(5) 0.7515(8) 0.017(2) Uani 1 1 d U . . C7 C 0.6498(11) 0.5352(5) 0.5690(8) 0.025(3) Uani 1 1 d . . . H7A H 0.5898 0.5656 0.5183 0.029 Uiso 1 1 calc R . . O4 O -0.1062(8) 0.6263(4) 0.7597(6) 0.0321(19) Uani 1 1 d . . . O2 O 1.0571(9) 0.3707(4) 0.7260(6) 0.043(2) Uani 1 1 d . . . C6 C 0.5615(10) 0.4632(5) 0.8339(7) 0.017(2) Uani 1 1 d U . . H6A H 0.6165 0.4371 0.8923 0.021 Uiso 1 1 calc R . . C15 C 0.3119(11) 0.4719(5) 0.9269(8) 0.022(3) Uani 1 1 d . . . H15A H 0.3753 0.4441 0.9801 0.027 Uiso 1 1 calc R . . C4 C 0.3044(11) 0.5187(5) 0.7468(8) 0.018(2) Uani 1 1 d U . . N6 N -0.1437(11) 0.6956(5) 0.6164(8) 0.043(3) Uani 1 1 d . . . C22 C -0.2772(13) 0.6168(7) 0.9399(9) 0.040(3) Uani 1 1 d . . . H22A H -0.2720 0.6459 0.8801 0.048 Uiso 1 1 calc R . . C2 C 0.5680(11) 0.5175(5) 0.6633(7) 0.015(2) Uani 1 1 d U . . C5 C 0.3882(10) 0.4837(5) 0.8329(8) 0.018(2) Uani 1 1 d . . . N5 N 1.0821(13) 0.2945(5) 0.8608(9) 0.054(3) Uani 1 1 d . . . C20 C -0.4219(14) 0.5842(6) 1.0863(10) 0.045(3) Uani 1 1 d . . . H20A H -0.5103 0.5909 1.1298 0.054 Uiso 1 1 calc R . . C3 C 0.3949(10) 0.5368(5) 0.6604(7) 0.021(2) Uani 1 1 d . . . H3A H 0.3386 0.5618 0.6012 0.026 Uiso 1 1 calc R . . C10 C 1.0830(12) 0.4449(7) 0.4288(8) 0.040(3) Uani 1 1 d . . . C21 C -0.4075(13) 0.6276(6) 1.0043(9) 0.035(3) Uani 1 1 d . . . H21A H -0.4847 0.6650 0.9905 0.042 Uiso 1 1 calc R . . C12 C 1.3655(16) 0.4040(7) 0.4018(13) 0.058(4) Uani 1 1 d . . . H12A H 1.4541 0.3974 0.3584 0.069 Uiso 1 1 calc R . . C13 C 1.3882(14) 0.3836(6) 0.5062(11) 0.040(3) Uani 1 1 d . . . H13A H 1.4906 0.3605 0.5352 0.048 Uiso 1 1 calc R . . C18 C -0.1793(15) 0.5218(6) 1.0363(10) 0.043(3) Uani 1 1 d . . . C19 C -0.3106(13) 0.5313(6) 1.1063(9) 0.047(3) Uani 1 1 d . . . H19A H -0.3181 0.5012 1.1645 0.056 Uiso 1 1 calc R . . C14 C 1.2617(14) 0.3968(6) 0.5691(10) 0.039(3) Uani 1 1 d . . . H14A H 1.2804 0.3830 0.6418 0.047 Uiso 1 1 calc R . . C27 C -0.3224(16) 0.7190(8) 0.6384(13) 0.070(5) Uani 1 1 d . . . H27A H -0.3811 0.6809 0.6688 0.105 Uiso 1 1 calc R . . H27B H -0.3903 0.7338 0.5714 0.105 Uiso 1 1 calc R . . H27C H -0.3099 0.7571 0.6892 0.105 Uiso 1 1 calc R . . C28 C -0.0754(17) 0.7293(7) 0.5258(11) 0.061(4) Uani 1 1 d . . . H28A H -0.0751 0.7790 0.5360 0.092 Uiso 1 1 calc R . . H28B H -0.1483 0.7177 0.4588 0.092 Uiso 1 1 calc R . . H28C H 0.0425 0.7135 0.5225 0.092 Uiso 1 1 calc R . . C25 C 1.0130(18) 0.2620(8) 0.9527(11) 0.074(5) Uani 1 1 d . . . H25A H 1.0878 0.2731 1.0191 0.111 Uiso 1 1 calc R . . H25B H 1.0092 0.2122 0.9429 0.111 Uiso 1 1 calc R . . H25C H 0.8965 0.2791 0.9566 0.111 Uiso 1 1 calc R . . C9 C 0.9111(14) 0.4780(7) 0.3838(9) 0.052(3) Uani 1 1 d . . . H9A H 0.9192 0.4944 0.3104 0.063 Uiso 1 1 calc R . . H9B H 0.8198 0.4427 0.3787 0.063 Uiso 1 1 calc R . . C17 C -0.0633(12) 0.4616(6) 1.0537(8) 0.040(3) Uani 1 1 d . . . H17A H -0.0962 0.4279 0.9961 0.048 Uiso 1 1 calc R . . H17B H -0.0787 0.4398 1.1225 0.048 Uiso 1 1 calc R . . C11 C 1.2075(16) 0.4352(6) 0.3591(11) 0.061(4) Uani 1 1 d . . . H11A H 1.1862 0.4491 0.2864 0.073 Uiso 1 1 calc R . . C24 C 1.2490(17) 0.2679(8) 0.8354(13) 0.093(7) Uani 1 1 d . . . H24A H 1.2851 0.2944 0.7764 0.140 Uiso 1 1 calc R . . H24B H 1.2361 0.2197 0.8146 0.140 Uiso 1 1 calc R . . H24C H 1.3362 0.2721 0.8985 0.140 Uiso 1 1 calc R . . Cu2 Cu 0.00460(14) 0.54938(6) 0.84928(10) 0.0252(3) Uani 1 1 d . . . O3 O 0.1354(7) 0.5331(3) 0.7337(5) 0.0244(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.062(2) 0.048(2) 0.056(2) 0.0157(18) 0.0227(17) 0.0107(17) O5 0.066(6) 0.127(9) 0.036(5) 0.017(5) 0.033(5) 0.047(6) F2 0.048(5) 0.165(10) 0.114(8) 0.047(7) 0.002(5) -0.020(6) F1 0.071(6) 0.232(13) 0.091(8) 0.098(9) 0.000(5) -0.039(7) O6 0.055(6) 0.077(7) 0.100(8) 0.016(6) 0.031(5) -0.023(5) F3 0.094(8) 0.071(7) 0.219(14) 0.029(8) -0.025(8) 0.014(6) C29 0.079(11) 0.085(13) 0.047(10) 0.023(9) -0.007(8) -0.034(10) O7 0.155(11) 0.048(7) 0.110(9) -0.019(6) 0.085(8) -0.010(6) S2 0.089(3) 0.072(3) 0.049(2) 0.014(2) 0.032(2) 0.000(2) O8 0.088(7) 0.110(8) 0.037(6) 0.032(5) 0.020(5) 0.035(6) F4 0.101(7) 0.125(9) 0.090(7) 0.047(6) 0.031(6) -0.012(6) F5 0.093(8) 0.233(17) 0.160(12) 0.058(11) -0.037(8) -0.075(9) F6 0.204(13) 0.091(8) 0.121(9) 0.035(7) 0.078(9) 0.037(8) O9 0.223(17) 0.141(14) 0.174(15) 0.033(11) 0.151(14) 0.071(12) C30 0.061(11) 0.114(16) 0.121(18) -0.057(14) 0.040(11) -0.021(11) O10 0.176(14) 0.29(2) 0.104(10) 0.109(12) -0.091(11) -0.142(15) Cu1 0.0143(6) 0.0350(8) 0.0305(8) 0.0002(7) 0.0117(5) 0.0022(6) N4 0.022(4) 0.028(6) 0.012(5) -0.006(4) 0.002(3) -0.008(4) O1 0.014(3) 0.033(5) 0.017(4) 0.009(3) 0.008(3) 0.008(3) N2 0.026(5) 0.032(6) 0.019(5) -0.010(4) 0.006(4) -0.002(4) C26 0.025(4) 0.030(4) 0.027(4) -0.001(3) 0.013(3) 0.003(3) C23 0.030(6) 0.025(7) 0.076(10) 0.022(7) 0.014(6) 0.021(5) N1 0.018(3) 0.034(4) 0.025(3) 0.000(3) 0.014(3) 0.000(3) N3 0.027(3) 0.039(4) 0.019(3) -0.002(3) 0.013(3) -0.005(3) C8 0.043(6) 0.061(9) 0.032(7) 0.027(6) 0.032(5) 0.021(6) C16 0.021(6) 0.079(10) 0.065(9) 0.030(7) 0.020(6) 0.017(6) C1 0.013(3) 0.019(4) 0.018(4) -0.008(3) -0.003(3) 0.000(3) C7 0.016(5) 0.023(7) 0.033(6) 0.007(5) -0.002(4) 0.001(4) O4 0.029(4) 0.031(5) 0.039(5) -0.001(4) 0.017(4) 0.005(3) O2 0.036(5) 0.054(6) 0.045(5) 0.019(5) 0.029(4) 0.018(4) C6 0.016(3) 0.016(4) 0.020(4) 0.009(3) 0.001(3) 0.000(3) C15 0.016(5) 0.037(7) 0.013(6) 0.009(5) 0.003(4) 0.008(4) C4 0.013(3) 0.021(4) 0.023(4) 0.000(3) 0.010(3) 0.001(3) N6 0.027(5) 0.052(6) 0.053(7) 0.014(5) 0.017(5) 0.020(5) C22 0.040(7) 0.054(8) 0.028(7) -0.021(6) 0.011(5) 0.002(6) C2 0.011(3) 0.020(4) 0.015(4) 0.003(3) 0.007(3) -0.001(3) C5 0.008(4) 0.026(5) 0.018(5) -0.001(4) -0.004(4) -0.001(4) N5 0.062(7) 0.048(7) 0.059(7) 0.030(6) 0.036(6) 0.031(6) C20 0.038(7) 0.060(8) 0.044(8) 0.008(7) 0.031(6) 0.015(6) C3 0.016(4) 0.033(7) 0.016(5) 0.014(5) 0.000(4) 0.008(4) C10 0.037(6) 0.060(8) 0.024(6) -0.007(6) 0.010(5) 0.007(6) C21 0.032(6) 0.039(7) 0.034(7) -0.015(6) 0.005(5) 0.005(5) C12 0.039(8) 0.061(9) 0.082(12) -0.012(8) 0.039(7) 0.002(7) C13 0.032(6) 0.034(7) 0.062(9) -0.009(7) 0.034(6) 0.004(5) C18 0.051(7) 0.034(7) 0.050(8) 0.011(6) 0.025(6) 0.015(5) C19 0.037(7) 0.064(10) 0.042(7) -0.002(6) 0.017(5) -0.004(6) C14 0.043(7) 0.033(7) 0.044(8) 0.001(6) 0.017(6) -0.004(6) C27 0.044(8) 0.082(11) 0.092(12) 0.023(9) 0.033(8) 0.023(7) C28 0.070(9) 0.056(9) 0.070(10) 0.023(8) 0.052(8) 0.012(7) C25 0.075(10) 0.094(12) 0.062(10) 0.051(9) 0.044(8) 0.054(9) C9 0.044(7) 0.087(10) 0.026(7) 0.002(6) 0.002(5) 0.008(6) C17 0.038(6) 0.049(8) 0.035(6) 0.000(6) 0.016(5) -0.013(6) C11 0.066(9) 0.064(10) 0.062(9) 0.017(7) 0.046(7) 0.000(8) C24 0.073(10) 0.110(13) 0.113(14) 0.084(11) 0.068(10) 0.078(10) Cu2 0.0108(5) 0.0349(8) 0.0323(8) 0.0001(7) 0.0115(5) 0.0021(6) O3 0.019(3) 0.028(5) 0.025(4) 0.008(3) 0.001(3) 0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 O7 1.396(10) . ? S1 O5 1.438(8) . ? S1 O6 1.468(9) . ? S1 C29 1.772(16) . ? F2 C29 1.366(16) . ? F1 C29 1.317(17) . ? F3 C29 1.321(19) . ? S2 O8 1.410(9) . ? S2 O10 1.409(11) . ? S2 O9 1.472(13) . ? S2 C30 1.70(2) . ? F4 C30 1.45(2) . ? F5 C30 1.305(19) . ? F6 C30 1.331(19) . ? Cu1 O1 1.931(6) . ? Cu1 N1 1.984(8) . ? Cu1 O2 1.985(8) . ? Cu1 N2 2.051(8) . ? Cu1 O3 2.343(7) 1_655 ? N4 C22 1.317(13) . ? N4 C18 1.343(13) . ? N4 Cu2 2.063(8) . ? O1 C1 1.356(10) . ? O1 Cu2 2.338(7) 1_655 ? N2 C10 1.332(12) . ? N2 C14 1.354(14) . ? C26 O4 1.254(12) . ? C26 N6 1.283(13) . ? C23 O2 1.249(13) . ? C23 N5 1.280(14) . ? N1 C7 1.304(11) . ? N1 C8 1.495(12) . ? N3 C15 1.307(11) . ? N3 C16 1.457(14) . ? N3 Cu2 1.956(9) . ? C8 C9 1.512(15) . ? C16 C17 1.502(13) . ? C1 C6 1.378(12) . ? C1 C2 1.413(13) . ? C7 C2 1.468(13) . ? O4 Cu2 2.006(7) . ? C6 C5 1.414(12) . ? C15 C5 1.418(13) . ? C4 O3 1.341(10) . ? C4 C5 1.373(13) . ? C4 C3 1.424(12) . ? N6 C28 1.482(15) . ? N6 C27 1.533(14) . ? C22 C21 1.405(14) . ? C2 C3 1.403(12) . ? N5 C24 1.481(14) . ? N5 C25 1.488(14) . ? C20 C19 1.354(15) . ? C20 C21 1.355(16) . ? C10 C11 1.412(14) . ? C10 C9 1.532(14) . ? C12 C13 1.365(18) . ? C12 C11 1.419(17) . ? C13 C14 1.375(14) . ? C18 C19 1.456(14) . ? C18 C17 1.485(15) . ? Cu2 O3 1.920(7) . ? Cu2 O1 2.338(7) 1_455 ? O3 Cu1 2.343(7) 1_455 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 S1 O5 114.2(6) . . ? O7 S1 O6 116.3(6) . . ? O5 S1 O6 115.1(6) . . ? O7 S1 C29 103.0(9) . . ? O5 S1 C29 105.6(7) . . ? O6 S1 C29 100.0(7) . . ? F1 C29 F3 108.5(15) . . ? F1 C29 F2 105.6(11) . . ? F3 C29 F2 101.2(15) . . ? F1 C29 S1 115.0(13) . . ? F3 C29 S1 112.0(11) . . ? F2 C29 S1 113.5(11) . . ? O8 S2 O10 120.7(9) . . ? O8 S2 O9 113.0(8) . . ? O10 S2 O9 113.3(12) . . ? O8 S2 C30 98.7(8) . . ? O10 S2 C30 104.4(10) . . ? O9 S2 C30 103.5(9) . . ? F5 C30 F6 108.4(16) . . ? F5 C30 F4 105.1(14) . . ? F6 C30 F4 100.1(18) . . ? F5 C30 S2 114.4(18) . . ? F6 C30 S2 116.0(12) . . ? F4 C30 S2 111.4(12) . . ? O1 Cu1 N1 91.1(3) . . ? O1 Cu1 O2 87.2(3) . . ? N1 Cu1 O2 164.5(3) . . ? O1 Cu1 N2 173.5(3) . . ? N1 Cu1 N2 95.2(3) . . ? O2 Cu1 N2 87.1(3) . . ? O1 Cu1 O3 82.5(3) . 1_655 ? N1 Cu1 O3 98.7(3) . 1_655 ? O2 Cu1 O3 96.3(3) . 1_655 ? N2 Cu1 O3 95.1(3) . 1_655 ? C22 N4 C18 119.2(10) . . ? C22 N4 Cu2 118.8(7) . . ? C18 N4 Cu2 120.4(7) . . ? C1 O1 Cu1 125.5(6) . . ? C1 O1 Cu2 115.6(5) . 1_655 ? Cu1 O1 Cu2 97.2(2) . 1_655 ? C10 N2 C14 118.0(9) . . ? C10 N2 Cu1 126.0(7) . . ? C14 N2 Cu1 116.0(7) . . ? O4 C26 N6 124.7(10) . . ? O2 C23 N5 125.6(11) . . ? C7 N1 C8 115.8(8) . . ? C7 N1 Cu1 125.9(7) . . ? C8 N1 Cu1 118.3(6) . . ? C15 N3 C16 116.0(8) . . ? C15 N3 Cu2 124.2(7) . . ? C16 N3 Cu2 119.8(7) . . ? N1 C8 C9 110.8(10) . . ? N3 C16 C17 111.9(10) . . ? O1 C1 C6 119.0(8) . . ? O1 C1 C2 121.5(8) . . ? C6 C1 C2 119.2(8) . . ? N1 C7 C2 124.7(9) . . ? C26 O4 Cu2 127.4(7) . . ? C23 O2 Cu1 127.0(7) . . ? C1 C6 C5 121.0(8) . . ? N3 C15 C5 127.2(9) . . ? O3 C4 C5 124.0(8) . . ? O3 C4 C3 116.0(8) . . ? C5 C4 C3 119.7(8) . . ? C26 N6 C28 123.1(9) . . ? C26 N6 C27 120.5(10) . . ? C28 N6 C27 116.3(10) . . ? N4 C22 C21 122.3(12) . . ? C3 C2 C1 120.2(9) . . ? C3 C2 C7 116.2(8) . . ? C1 C2 C7 123.5(8) . . ? C4 C5 C6 120.2(9) . . ? C4 C5 C15 122.2(8) . . ? C6 C5 C15 117.4(8) . . ? C23 N5 C24 120.1(10) . . ? C23 N5 C25 123.6(10) . . ? C24 N5 C25 116.4(9) . . ? C19 C20 C21 120.1(11) . . ? C2 C3 C4 119.5(8) . . ? N2 C10 C11 122.7(10) . . ? N2 C10 C9 119.2(9) . . ? C11 C10 C9 118.1(10) . . ? C20 C21 C22 119.4(11) . . ? C13 C12 C11 119.0(11) . . ? C12 C13 C14 119.5(12) . . ? N4 C18 C19 120.2(10) . . ? N4 C18 C17 121.1(10) . . ? C19 C18 C17 118.7(10) . . ? C20 C19 C18 118.3(11) . . ? N2 C14 C13 123.2(12) . . ? C8 C9 C10 114.3(9) . . ? C18 C17 C16 112.4(10) . . ? C10 C11 C12 117.4(11) . . ? O3 Cu2 N3 92.1(3) . . ? O3 Cu2 O4 86.0(3) . . ? N3 Cu2 O4 163.0(3) . . ? O3 Cu2 N4 173.0(3) . . ? N3 Cu2 N4 94.0(3) . . ? O4 Cu2 N4 89.1(3) . . ? O3 Cu2 O1 82.9(3) . 1_455 ? N3 Cu2 O1 102.9(3) . 1_455 ? O4 Cu2 O1 93.7(2) . 1_455 ? N4 Cu2 O1 92.4(3) . 1_455 ? C4 O3 Cu2 124.1(6) . . ? C4 O3 Cu1 116.2(6) . 1_455 ? Cu2 O3 Cu1 97.3(3) . 1_455 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O7 S1 C29 F1 59.3(13) . . . . ? O5 S1 C29 F1 179.3(12) . . . . ? O6 S1 C29 F1 -60.9(14) . . . . ? O7 S1 C29 F3 -176.3(12) . . . . ? O5 S1 C29 F3 -56.2(13) . . . . ? O6 S1 C29 F3 63.6(13) . . . . ? O7 S1 C29 F2 -62.5(14) . . . . ? O5 S1 C29 F2 57.6(14) . . . . ? O6 S1 C29 F2 177.4(12) . . . . ? O8 S2 C30 F5 69.0(14) . . . . ? O10 S2 C30 F5 -166.1(15) . . . . ? O9 S2 C30 F5 -47.3(16) . . . . ? O8 S2 C30 F6 -58.3(17) . . . . ? O10 S2 C30 F6 66.6(19) . . . . ? O9 S2 C30 F6 -174.7(17) . . . . ? O8 S2 C30 F4 -171.9(11) . . . . ? O10 S2 C30 F4 -47.0(15) . . . . ? O9 S2 C30 F4 71.7(15) . . . . ? N1 Cu1 O1 C1 30.5(7) . . . . ? O2 Cu1 O1 C1 -134.1(7) . . . . ? N2 Cu1 O1 C1 -162(3) . . . . ? O3 Cu1 O1 C1 129.2(7) 1_655 . . . ? N1 Cu1 O1 Cu2 -98.2(3) . . . 1_655 ? O2 Cu1 O1 Cu2 97.2(3) . . . 1_655 ? N2 Cu1 O1 Cu2 69(3) . . . 1_655 ? O3 Cu1 O1 Cu2 0.4(3) 1_655 . . 1_655 ? O1 Cu1 N2 C10 -177(2) . . . . ? N1 Cu1 N2 C10 -10.2(9) . . . . ? O2 Cu1 N2 C10 154.5(9) . . . . ? O3 Cu1 N2 C10 -109.4(9) 1_655 . . . ? O1 Cu1 N2 C14 0(3) . . . . ? N1 Cu1 N2 C14 167.6(8) . . . . ? O2 Cu1 N2 C14 -27.8(8) . . . . ? O3 Cu1 N2 C14 68.3(7) 1_655 . . . ? O1 Cu1 N1 C7 -13.6(8) . . . . ? O2 Cu1 N1 C7 69.9(16) . . . . ? N2 Cu1 N1 C7 167.9(8) . . . . ? O3 Cu1 N1 C7 -96.2(8) 1_655 . . . ? O1 Cu1 N1 C8 164.2(8) . . . . ? O2 Cu1 N1 C8 -112.3(13) . . . . ? N2 Cu1 N1 C8 -14.4(8) . . . . ? O3 Cu1 N1 C8 81.6(8) 1_655 . . . ? C7 N1 C8 C9 -128.9(10) . . . . ? Cu1 N1 C8 C9 53.1(11) . . . . ? C15 N3 C16 C17 -139.6(10) . . . . ? Cu2 N3 C16 C17 42.2(13) . . . . ? Cu1 O1 C1 C6 153.2(7) . . . . ? Cu2 O1 C1 C6 -85.9(9) 1_655 . . . ? Cu1 O1 C1 C2 -32.4(12) . . . . ? Cu2 O1 C1 C2 88.5(9) 1_655 . . . ? C8 N1 C7 C2 -179.7(9) . . . . ? Cu1 N1 C7 C2 -1.8(14) . . . . ? N6 C26 O4 Cu2 170.9(9) . . . . ? N5 C23 O2 Cu1 -175.9(10) . . . . ? O1 Cu1 O2 C23 13.2(10) . . . . ? N1 Cu1 O2 C23 -70.9(17) . . . . ? N2 Cu1 O2 C23 -169.9(10) . . . . ? O3 Cu1 O2 C23 95.3(10) 1_655 . . . ? O1 C1 C6 C5 172.7(8) . . . . ? C2 C1 C6 C5 -1.8(13) . . . . ? C16 N3 C15 C5 -174.7(10) . . . . ? Cu2 N3 C15 C5 3.3(15) . . . . ? O4 C26 N6 C28 175.1(11) . . . . ? O4 C26 N6 C27 -0.5(19) . . . . ? C18 N4 C22 C21 7.2(16) . . . . ? Cu2 N4 C22 C21 172.7(8) . . . . ? O1 C1 C2 C3 -173.9(8) . . . . ? C6 C1 C2 C3 0.4(13) . . . . ? O1 C1 C2 C7 9.0(14) . . . . ? C6 C1 C2 C7 -176.6(9) . . . . ? N1 C7 C2 C3 -168.5(9) . . . . ? N1 C7 C2 C1 8.7(15) . . . . ? O3 C4 C5 C6 172.0(8) . . . . ? C3 C4 C5 C6 -2.7(14) . . . . ? O3 C4 C5 C15 -13.6(16) . . . . ? C3 C4 C5 C15 171.7(9) . . . . ? C1 C6 C5 C4 3.0(14) . . . . ? C1 C6 C5 C15 -171.6(9) . . . . ? N3 C15 C5 C4 -4.9(17) . . . . ? N3 C15 C5 C6 169.6(10) . . . . ? O2 C23 N5 C24 4(2) . . . . ? O2 C23 N5 C25 -177.2(13) . . . . ? C1 C2 C3 C4 -0.1(14) . . . . ? C7 C2 C3 C4 177.1(9) . . . . ? O3 C4 C3 C2 -173.8(8) . . . . ? C5 C4 C3 C2 1.3(14) . . . . ? C14 N2 C10 C11 -5.3(17) . . . . ? Cu1 N2 C10 C11 172.4(9) . . . . ? C14 N2 C10 C9 177.3(10) . . . . ? Cu1 N2 C10 C9 -5.0(15) . . . . ? C19 C20 C21 C22 0.6(17) . . . . ? N4 C22 C21 C20 -3.5(17) . . . . ? C11 C12 C13 C14 -3.3(19) . . . . ? C22 N4 C18 C19 -7.9(16) . . . . ? Cu2 N4 C18 C19 -173.1(8) . . . . ? C22 N4 C18 C17 173.6(10) . . . . ? Cu2 N4 C18 C17 8.5(15) . . . . ? C21 C20 C19 C18 -1.3(18) . . . . ? N4 C18 C19 C20 5.0(17) . . . . ? C17 C18 C19 C20 -176.5(11) . . . . ? C10 N2 C14 C13 3.3(16) . . . . ? Cu1 N2 C14 C13 -174.6(9) . . . . ? C12 C13 C14 N2 1.0(18) . . . . ? N1 C8 C9 C10 -73.6(12) . . . . ? N2 C10 C9 C8 48.0(15) . . . . ? C11 C10 C9 C8 -129.6(11) . . . . ? N4 C18 C17 C16 46.5(15) . . . . ? C19 C18 C17 C16 -132.0(11) . . . . ? N3 C16 C17 C18 -74.5(13) . . . . ? N2 C10 C11 C12 3.0(19) . . . . ? C9 C10 C11 C12 -179.6(11) . . . . ? C13 C12 C11 C10 1.5(19) . . . . ? C15 N3 Cu2 O3 9.2(8) . . . . ? C16 N3 Cu2 O3 -172.8(8) . . . . ? C15 N3 Cu2 O4 -74.0(15) . . . . ? C16 N3 Cu2 O4 104.0(13) . . . . ? C15 N3 Cu2 N4 -174.2(8) . . . . ? C16 N3 Cu2 N4 3.7(9) . . . . ? C15 N3 Cu2 O1 92.4(8) . . . 1_455 ? C16 N3 Cu2 O1 -89.6(9) . . . 1_455 ? C26 O4 Cu2 O3 -13.8(9) . . . . ? C26 O4 Cu2 N3 70.3(15) . . . . ? C26 O4 Cu2 N4 171.3(9) . . . . ? C26 O4 Cu2 O1 -96.4(9) . . . 1_455 ? C22 N4 Cu2 O3 -45(3) . . . . ? C18 N4 Cu2 O3 120(3) . . . . ? C22 N4 Cu2 N3 164.3(8) . . . . ? C18 N4 Cu2 N3 -30.4(8) . . . . ? C22 N4 Cu2 O4 1.1(8) . . . . ? C18 N4 Cu2 O4 166.3(8) . . . . ? C22 N4 Cu2 O1 -92.6(8) . . . 1_455 ? C18 N4 Cu2 O1 72.7(8) . . . 1_455 ? C5 C4 O3 Cu2 31.5(13) . . . . ? C3 C4 O3 Cu2 -153.7(7) . . . . ? C5 C4 O3 Cu1 -88.9(10) . . . 1_455 ? C3 C4 O3 Cu1 85.9(9) . . . 1_455 ? N3 Cu2 O3 C4 -25.6(7) . . . . ? O4 Cu2 O3 C4 137.5(7) . . . . ? N4 Cu2 O3 C4 -176(2) . . . . ? O1 Cu2 O3 C4 -128.3(7) 1_455 . . . ? N3 Cu2 O3 Cu1 103.2(3) . . . 1_455 ? O4 Cu2 O3 Cu1 -93.8(3) . . . 1_455 ? N4 Cu2 O3 Cu1 -48(3) . . . 1_455 ? O1 Cu2 O3 Cu1 0.4(3) 1_455 . . 1_455 ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 25.75 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.058 _refine_diff_density_min -1.100 _refine_diff_density_rms 0.130 # Attachment '- Compd3.CIF' data_TK91-2DMF _database_code_depnum_ccdc_archive 'CCDC 780480' #TrackingRef '- Compd3.CIF' _chemical_formula_moiety 'C24 H20 Cu2 F6 N4 O8 S2' _chemical_formula_sum 'C24 H20 Cu2 F6 N4 O8 S2' _chemical_formula_weight 797.662 _cell_length_a 10.92547(17) _cell_length_b 7.96493(12) _cell_length_c 18.36893(30) _cell_angle_alpha 90 _cell_angle_beta 116.07536(84) _cell_angle_gamma 90 _cell_volume 1435.778(40) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P121/c1 _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz '-x, -y, -z' '-x, y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' 'x, y, z' _diffrn_radiation_type 'Cu K\a_1' _diffrn_measurement_device_type 'Bruker D8 Advance in Debye-Scherrer geometry' _diffrn_radiation_wavelength 1.54059 _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.845 _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max <0.01 _refine_ls_number_parameters 150 _pd_proc_ls_prof_R_factor 0.0242 _pd_proc_ls_prof_wR_factor 0.0317 _refine_ls_R_Fsqd_factor 0.0125 _refine_ls_goodness_of_fit_all 1.78 _cell_measurement_temperature 293 _diffrn_ambient_temperature 293 _exptl_crystal_description 'microcrystalline powder' _exptl_crystal_colour brown _refine_ls_structure_factor_coef Fsqd _exptl_special_details ; The material was obtained by in situ heating of the sample while mounted in a powder diffractometer up to 220 degrees Celsisus. This resulted in the loss of two DMF molecules yielding the given compound. Capillary with the compound was cooled to room temperature prior to data collection of the high quality powder pattern. ; _computing_data_collection Bruker _computing_data_reduction none _computing_cell_refinement 'Topas version 4.1' _computing_structure_solution 'simulated annealing using Topas version 4.1' _computing_structure_refinement 'Topas version 4.1' _computing_publication_material 'PLATON (Spek, 2003)' loop_ _atom_site_label _atom_site_type_symbol _atom_site_symmetry_multiplicity _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_B_iso_or_equiv Cu Cu 4 -0.078252(31) 0.00243(33) 0.050602(25) 1 1.638(62) S21 S 4 0.23032(27) 0.00500(46) 0.21914(14) 1 1.638(62) F21 F 4 0.33742(51) -0.29576(59) 0.22527(31) 1 3.021(89) F22 F 4 0.31127(57) -0.14974(74) 0.12091(25) 1 3.021(89) F23 F 4 0.46233(48) -0.08803(66) 0.24078(34) 1 3.021(89) O1 O 4 0.009682(78) 0.146554(57) 0.004112(53) 1 3.021(89) O21 O 4 0.10149(53) -0.07087(76) 0.17427(35) 1 3.021(89) O22 O 4 0.25112(64) 0.16531(67) 0.19085(37) 1 3.021(89) O23 O 4 0.28548(58) -0.0061(10) 0.30467(26) 1 3.021(89) N2 N 4 -0.24045(46) -0.13193(77) 0.04273(24) 1 3.021(89) N1 N 4 -0.10844(51) 0.18529(62) 0.11061(27) 1 3.021(89) C1 C 4 -0.31859(37) -0.20339(67) -0.02873(21) 1 3.021(89) H1 H 4 -0.28648(70) -0.2079(14) -0.07081(37) 1 3.63(11) C2 C 4 -0.44546(30) -0.26954(63) -0.04344(20) 1 3.021(89) H2 H 4 -0.50558(64) -0.3205(12) -0.09581(34) 1 3.63(11) C3 C 4 -0.48343(37) -0.25898(56) 0.01903(20) 1 3.021(89) H3 H 4 -0.57161(64) -0.3053(12) 0.01131(46) 1 3.63(11) C4 C 4 -0.39795(35) -0.18715(64) 0.09234(20) 1 3.021(89) H4 H 4 -0.42266(73) -0.1801(13) 0.13731(38) 1 3.63(11) C5 C 4 -0.27073(37) -0.12478(70) 0.10546(22) 1 3.021(89) C6 C 4 -0.18408(36) -0.03987(47) 0.18146(22) 1 3.021(89) H6a H 4 -0.21943(72) -0.0545(14) 0.22266(36) 1 3.63(11) H6b H 4 -0.09298(66) -0.0930(11) 0.20292(58) 1 3.63(11) C7 C 4 -0.17192(36) 0.14812(54) 0.16603(20) 1 3.021(89) H7a H 4 -0.1195(11) 0.2020(12) 0.22030(46) 1 3.63(11) H7b H 4 -0.26487(66) 0.1990(13) 0.14237(61) 1 3.63(11) C8 C 4 -0.08267(47) 0.33759(49) 0.10376(23) 1 3.021(89) H8 H 4 -0.10673(89) 0.41784(96) 0.13563(43) 1 3.63(11) C9 C 4 -0.03826(42) 0.41425(11) 0.052016(51) 1 3.021(89) C10 C 4 0.00058(11) 0.322233(85) -0.000111(77) 1 3.021(89) C11 C 4 0.04331(15) 0.41104(11) -0.04936(17) 1 3.021(89) H11 H 4 0.07163(71) 0.3478(10) -0.08447(39) 1 3.63(11) C21 C 4 0.34096(39) -0.14019(52) 0.20035(22) 1 3.021(89) _vrf_ATOM006_TK91-2DMF ; PROBLEM: _atom_site_U_iso_or_equiv is missing RESPONSE: Displacement parameters are reported as Biso. ; _vrf_GEOM001_TK91-2DMF ; PROBLEM: _geom_bond_atom_site_label_1 is missing RESPONSE: Bond lengths and valence angles are not calculated. ; _vrf_GEOM003_TK91-2DMF ; PROBLEM: _geom_bond_distance is missing RESPONSE: Bond lengths and valence angles are reported separately. ; _vrf_GEOM006_TK91-2DMF ; PROBLEM: _geom_angle_atom_site_label_2 is missing RESPONSE: Bond lengths and valence angles are reported separately. ; _vrf_GEOM007_TK91-2DMF ; PROBLEM: _geom_angle_atom_site_label_3 is missing RESPONSE: Bond lengths and valence angles are reported separately. ; _vrf_PLAT761_TK91-2DMF ; PROBLEM: CIF Contains no X-H Bonds ...................... ? RESPONSE: Bond lengths and valence angles are reported separately. ; _vrf_PLAT762_TK91-2DMF ; PROBLEM: CIF Contains no X-Y-H or H-Y-H Angles .......... ? RESPONSE: Bond lengths and valence angles are reported separately. ; # end of file