# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_address _publ_author_footnote ; ? # Address for author 1 ; ; ? # Footnote for author 1 ; ; ? # Address 2 ; ; ? # Footnote 2 ; _publ_contact_author_name 'Robertson, Neil' _publ_contact_author_email neil.robertson@ed.ac.uk _publ_section_title ; Substituted [Cu(I)(POP)(bipyridyl)] and related complexes: Synthesis, structure, properties and applications to dye-sensitised solar cells ; _publ_contact_author_address ; Department of Chemistry, Joseph Black Builing, West Mains Road, University of Edinburgh, Edinburgh, EH9 3JJ, UK. ; _publ_contact_author_phone '+44 131 650 4806' _publ_contact_letter ; ; _publ_author_name N.Robertson # Attachment '- 771439.cif' data_nr0006 _database_code_depnum_ccdc_archive 'CCDC 771439' #TrackingRef '- 771439.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_compound_source 'Charlotte Linfoot' _exptl_crystal_recrystallization_method 'slow diffusion of diethyl ether into MeCN solution' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H44 Cu N2 O5 P2, C2 H3 N, B F4' _chemical_formula_sum 'C54 H47 B Cu F4 N3 O5 P2' _chemical_formula_weight 1030.24 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' B B 0.0013 0.0007 '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' P P 0.1023 0.0942 '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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.3345(3) _cell_length_b 12.6111(3) _cell_length_c 18.0200(4) _cell_angle_alpha 98.4411(13) _cell_angle_beta 100.4738(12) _cell_angle_gamma 113.2549(12) _cell_volume 2457.18(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9883 _cell_measurement_theta_min 2.2595 _cell_measurement_theta_max 26.7975 _exptl_crystal_description tablet _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.392 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 0.577 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8106 _exptl_absorpt_correction_T_max 0.9542 _exptl_absorpt_process_details 'SADABS 2007/2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex II CCD on D8' _diffrn_measurement_method 'Phi and Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 49789 _diffrn_reflns_av_R_equivalents 0.0606 _diffrn_reflns_av_sigmaI/netI 0.0557 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 27.05 _reflns_number_total 10570 _reflns_number_gt 7712 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution 'Superflip - WinGX' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Shelxp _computing_publication_material 'Platon, encifer' _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. #============================================================================== The Following Model and Quality ALERTS were generated - (Acta-Mode) <<< #============================================================================== Format: alert-number_ALERT_alert-type_alert-level text 213_ALERT_2_C Atom C15' has ADP max/min Ratio ............. 3.40 oblat This atom is part of a disordered group, some abnormal behavior in its ADP's is not unexpected. Restraints were applied to control this. 220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.02 Ratio 222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.62 Ratio This carbon is expected to have higher thermal motion. 911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.600 39 912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 174 Completeness is better than 99% to acta minimum resolution. See below... #============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 1.000 5148 5147 1 23.01 0.550 0.998 6840 6828 12 25.24 0.600 0.996 8894 8855 39 #----------------------------------------------------------- ACTA Min. Res. --- 27.05 0.640 0.980 10783 10570 213 061_ALERT_4_C Tmax/Tmin Range Test RR' too Large ............. 0.88 Sadabs corrects for all systematic errors that lead to disparities in the intensities of symmetry-equivalent data. These may include absorption by the mount, crystal decay etc. The crystal was a plate and accurate measurement of its dimensions was difficult. 244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbours of B1S This is a BF4 anion. Rotational motion about B1S is expected to an extent. 301_ALERT_3_G Note Main Residue Disorder .................... 3.00 Perc. 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 63 302_ALERT_4_G Note Anion/Solvent Disorder .................... 27.00 Perc. 720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 6 760_ALERT_1_G CIF Contains no Torsion Angles ................. ? 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 24.60 Deg. C15 -O5 -C15' 1.555 1.555 1.555 Confirmed, no action taken ; _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^)+(0.0424P)^2^+1.5064P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'charge flipping' _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_number_reflns 10570 _refine_ls_number_parameters 680 _refine_ls_number_restraints 63 _refine_ls_R_factor_all 0.0685 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.1040 _refine_ls_wR_factor_gt 0.0937 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Cu1 Cu 0.35373(3) 0.62887(2) 0.276302(16) 0.01639(8) Uani 1 1 d . . . N1 N 0.28402(17) 0.64940(16) 0.37030(11) 0.0163(4) Uani 1 1 d . A . C1 C 0.6000(2) 0.8459(2) 0.32890(14) 0.0202(5) Uani 1 1 d . . . H1 H 0.6072 0.8269 0.2776 0.024 Uiso 1 1 calc R . . P1 P 0.22207(6) 0.60217(5) 0.16542(3) 0.01713(14) Uani 1 1 d . . . O1 O 0.13441(14) 0.37808(14) 0.21356(9) 0.0185(4) Uani 1 1 d . . . C2 C 0.6985(2) 0.9373(2) 0.38336(14) 0.0202(5) Uani 1 1 d . . . H2 H 0.7713 0.9811 0.3696 0.024 Uiso 1 1 calc R . . N2 N 0.49441(18) 0.78237(17) 0.34473(11) 0.0173(4) Uani 1 1 d . . . O2 O 0.79381(16) 1.07067(16) 0.59050(10) 0.0283(4) Uani 1 1 d . . . P2 P 0.41122(6) 0.48022(5) 0.27022(3) 0.01604(13) Uani 1 1 d . . . C3 C 0.6891(2) 0.9641(2) 0.45896(13) 0.0182(5) Uani 1 1 d . . . O3 O 0.88732(15) 1.11774(15) 0.49579(9) 0.0232(4) Uani 1 1 d . . . C4 C 0.5800(2) 0.9013(2) 0.47632(14) 0.0186(5) Uani 1 1 d . . . H4 H 0.5710 0.9191 0.5273 0.022 Uiso 1 1 calc R . . O4 O 0.07868(17) 0.65995(16) 0.58626(10) 0.0273(4) Uani 1 1 d . . . C5 C 0.4837(2) 0.8115(2) 0.41768(13) 0.0169(5) Uani 1 1 d . . . O5 O 0.27606(17) 0.79195(17) 0.63875(10) 0.0326(4) Uani 1 1 d DU . . C6 C 0.3642(2) 0.7397(2) 0.43116(13) 0.0174(5) Uani 1 1 d . . . C7 C 0.3354(2) 0.7626(2) 0.50136(13) 0.0188(5) Uani 1 1 d . A . H7 H 0.3941 0.8249 0.5440 0.023 Uiso 1 1 calc R . . C8 C 0.2196(2) 0.6927(2) 0.50779(13) 0.0195(5) Uani 1 1 d . . . C9 C 0.1363(2) 0.6029(2) 0.44449(13) 0.0193(5) Uani 1 1 d . A . H9 H 0.0558 0.5555 0.4471 0.023 Uiso 1 1 calc R . . C10 C 0.1722(2) 0.5832(2) 0.37743(13) 0.0177(5) Uani 1 1 d . . . H10 H 0.1153 0.5201 0.3346 0.021 Uiso 1 1 calc R A . C11 C 0.7941(2) 1.0556(2) 0.52318(14) 0.0203(5) Uani 1 1 d . . . C12 C 0.9972(2) 1.2080(2) 0.55302(15) 0.0257(6) Uani 1 1 d . . . H12A H 0.9748 1.2380 0.5990 0.031 Uiso 1 1 calc R . . H12B H 1.0367 1.2758 0.5304 0.031 Uiso 1 1 calc R . . C13 C 1.0854(2) 1.1568(2) 0.57756(17) 0.0331(7) Uani 1 1 d . . . H13A H 1.1587 1.2183 0.6161 0.050 Uiso 1 1 calc R . . H13B H 1.1086 1.1284 0.5321 0.050 Uiso 1 1 calc R . . H13C H 1.0466 1.0903 0.6005 0.050 Uiso 1 1 calc R . . C14 C 0.1821(2) 0.7119(2) 0.58129(14) 0.0227(5) Uani 1 1 d . A . C15 C 0.2517(5) 0.8332(4) 0.7122(2) 0.0298(11) Uani 0.767(8) 1 d PDU A 1 H15A H 0.1711 0.8354 0.7016 0.036 Uiso 0.767(8) 1 calc PR A 1 H15B H 0.3154 0.9142 0.7394 0.036 Uiso 0.767(8) 1 calc PR A 1 C16 C 0.2531(5) 0.7472(4) 0.7614(2) 0.0458(15) Uani 0.767(8) 1 d PU A 1 H16A H 0.2375 0.7722 0.8109 0.069 Uiso 0.767(8) 1 calc PR A 1 H16B H 0.3333 0.7458 0.7714 0.069 Uiso 0.767(8) 1 calc PR A 1 H16C H 0.1895 0.6675 0.7340 0.069 Uiso 0.767(8) 1 calc PR A 1 C15' C 0.2415(15) 0.7813(16) 0.7140(6) 0.029(3) Uani 0.233(8) 1 d PDU A 2 H15C H 0.1930 0.6964 0.7119 0.035 Uiso 0.233(8) 1 calc PR A 2 H15D H 0.1898 0.8233 0.7210 0.035 Uiso 0.233(8) 1 calc PR A 2 C16' C 0.3530(15) 0.8333(16) 0.7824(7) 0.052(5) Uani 0.233(8) 1 d PU A 2 H16D H 0.3273 0.8262 0.8305 0.077 Uiso 0.233(8) 1 calc PR A 2 H16E H 0.4011 0.9174 0.7847 0.077 Uiso 0.233(8) 1 calc PR A 2 H16F H 0.4030 0.7901 0.7765 0.077 Uiso 0.233(8) 1 calc PR A 2 C17 C 0.5477(2) 0.5110(2) 0.34564(13) 0.0182(5) Uani 1 1 d . . . C18 C 0.5557(2) 0.5633(2) 0.42132(14) 0.0243(6) Uani 1 1 d . . . H18 H 0.4913 0.5813 0.4318 0.029 Uiso 1 1 calc R . . C19 C 0.6569(3) 0.5892(2) 0.48138(15) 0.0284(6) Uani 1 1 d . . . H19 H 0.6611 0.6239 0.5329 0.034 Uiso 1 1 calc R . . C20 C 0.7515(2) 0.5649(2) 0.46680(15) 0.0281(6) Uani 1 1 d . . . H20 H 0.8207 0.5827 0.5082 0.034 Uiso 1 1 calc R . . C21 C 0.7456(2) 0.5145(2) 0.39180(16) 0.0275(6) Uani 1 1 d . . . H21 H 0.8113 0.4984 0.3817 0.033 Uiso 1 1 calc R . . C22 C 0.6438(2) 0.4870(2) 0.33089(15) 0.0226(5) Uani 1 1 d . . . H22 H 0.6400 0.4520 0.2795 0.027 Uiso 1 1 calc R . . C23 C 0.4512(2) 0.4387(2) 0.18169(13) 0.0181(5) Uani 1 1 d . . . C24 C 0.4118(2) 0.3218(2) 0.14112(14) 0.0257(6) Uani 1 1 d . . . H24 H 0.3574 0.2582 0.1578 0.031 Uiso 1 1 calc R . . C25 C 0.4520(3) 0.2981(3) 0.07634(16) 0.0334(7) Uani 1 1 d . . . H25 H 0.4243 0.2182 0.0484 0.040 Uiso 1 1 calc R . . C26 C 0.5323(3) 0.3902(3) 0.05228(15) 0.0311(6) Uani 1 1 d . . . H26 H 0.5605 0.3732 0.0084 0.037 Uiso 1 1 calc R . . C27 C 0.5715(2) 0.5069(2) 0.09195(14) 0.0259(6) Uani 1 1 d . . . H27 H 0.6266 0.5702 0.0754 0.031 Uiso 1 1 calc R . . C28 C 0.5299(2) 0.5310(2) 0.15587(14) 0.0214(5) Uani 1 1 d . . . H28 H 0.5551 0.6112 0.1824 0.026 Uiso 1 1 calc R . . C29 C 0.2986(2) 0.3420(2) 0.28346(13) 0.0176(5) Uani 1 1 d . . . C30 C 0.3322(2) 0.2692(2) 0.32432(14) 0.0217(5) Uani 1 1 d . . . H30 H 0.4164 0.2878 0.3425 0.026 Uiso 1 1 calc R . . C31 C 0.2451(2) 0.1700(2) 0.33889(15) 0.0266(6) Uani 1 1 d . . . H31 H 0.2701 0.1216 0.3668 0.032 Uiso 1 1 calc R . . C32 C 0.1214(3) 0.1412(2) 0.31287(15) 0.0281(6) Uani 1 1 d . . . H32 H 0.0617 0.0740 0.3234 0.034 Uiso 1 1 calc R . . C33 C 0.0861(2) 0.2120(2) 0.27121(15) 0.0248(6) Uani 1 1 d . . . H33 H 0.0018 0.1931 0.2529 0.030 Uiso 1 1 calc R . . C34 C 0.1733(2) 0.3094(2) 0.25653(13) 0.0184(5) Uani 1 1 d . . . C35 C 0.1345(2) 0.3560(2) 0.13504(13) 0.0189(5) Uani 1 1 d . . . C36 C 0.0992(2) 0.2421(2) 0.09189(14) 0.0237(5) Uani 1 1 d . . . H36 H 0.0725 0.1762 0.1148 0.028 Uiso 1 1 calc R . . C37 C 0.1033(2) 0.2251(2) 0.01498(15) 0.0283(6) Uani 1 1 d . . . H37 H 0.0805 0.1474 -0.0149 0.034 Uiso 1 1 calc R . . C38 C 0.1403(2) 0.3211(2) -0.01842(14) 0.0265(6) Uani 1 1 d . . . H38 H 0.1442 0.3094 -0.0710 0.032 Uiso 1 1 calc R . . C39 C 0.1718(2) 0.4344(2) 0.02469(14) 0.0227(5) Uani 1 1 d . . . H39 H 0.1954 0.4995 0.0009 0.027 Uiso 1 1 calc R . . C40 C 0.1693(2) 0.4544(2) 0.10264(13) 0.0195(5) Uani 1 1 d . . . C41 C 0.0835(2) 0.6102(2) 0.18234(13) 0.0194(5) Uani 1 1 d . . . C42 C 0.0971(2) 0.7182(2) 0.22551(14) 0.0261(6) Uani 1 1 d . . . H42 H 0.1762 0.7830 0.2444 0.031 Uiso 1 1 calc R . . C43 C -0.0026(3) 0.7322(3) 0.24116(15) 0.0297(6) Uani 1 1 d . . . H43 H 0.0075 0.8071 0.2689 0.036 Uiso 1 1 calc R . . C44 C -0.1170(2) 0.6372(3) 0.21638(14) 0.0283(6) Uani 1 1 d . . . H44 H -0.1858 0.6464 0.2274 0.034 Uiso 1 1 calc R . . C45 C -0.1314(2) 0.5285(2) 0.17549(15) 0.0267(6) Uani 1 1 d . . . H45 H -0.2098 0.4625 0.1595 0.032 Uiso 1 1 calc R . . C46 C -0.0316(2) 0.5157(2) 0.15783(14) 0.0223(5) Uani 1 1 d . . . H46 H -0.0425 0.4414 0.1287 0.027 Uiso 1 1 calc R . . C47 C 0.2693(2) 0.7036(2) 0.10250(13) 0.0193(5) Uani 1 1 d . . . C48 C 0.3933(2) 0.7690(2) 0.11182(14) 0.0220(5) Uani 1 1 d . . . H48 H 0.4506 0.7600 0.1503 0.026 Uiso 1 1 calc R . . C49 C 0.4354(2) 0.8478(2) 0.06579(15) 0.0264(6) Uani 1 1 d . . . H49 H 0.5207 0.8923 0.0727 0.032 Uiso 1 1 calc R . . C50 C 0.3514(3) 0.8605(2) 0.00978(15) 0.0284(6) Uani 1 1 d . . . H50 H 0.3793 0.9139 -0.0220 0.034 Uiso 1 1 calc R . . C51 C 0.2276(3) 0.7962(2) -0.00021(15) 0.0294(6) Uani 1 1 d . . . H51 H 0.1707 0.8062 -0.0384 0.035 Uiso 1 1 calc R . . C52 C 0.1856(2) 0.7169(2) 0.04529(14) 0.0248(6) Uani 1 1 d . . . H52 H 0.1002 0.6719 0.0376 0.030 Uiso 1 1 calc R . . B1S B 0.7939(3) 0.9227(3) 0.17122(19) 0.0307(7) Uani 1 1 d . . . F1S F 0.83388(17) 0.96028(18) 0.25220(10) 0.0533(5) Uani 1 1 d . . . F2S F 0.88930(18) 0.91733(19) 0.14419(11) 0.0568(5) Uani 1 1 d . . . F3S F 0.69416(18) 0.81341(17) 0.15094(12) 0.0636(6) Uani 1 1 d . . . F4S F 0.7609(2) 1.00416(18) 0.14290(12) 0.0626(6) Uani 1 1 d . . . N1T N 0.5568(3) 0.9808(2) 0.66643(19) 0.0329(7) Uani 0.80 1 d PU B 1 C2T C 0.6097(4) 0.9844(3) 0.7288(2) 0.0396(9) Uani 0.80 1 d PU B 1 C3T C 0.6869(7) 0.9931(6) 0.8053(4) 0.0608(19) Uani 0.80 1 d PU B 1 H3T1 H 0.7576 0.9800 0.7976 0.091 Uiso 0.80 1 calc PR B 1 H3T2 H 0.6386 0.9327 0.8296 0.091 Uiso 0.80 1 calc PR B 1 H3T3 H 0.7151 1.0723 0.8392 0.091 Uiso 0.80 1 calc PR B 1 C3U C 0.8340(18) 1.0135(17) 0.8823(12) 0.063(5) Uani 0.20 1 d PU C 2 H3U1 H 0.8723 0.9735 0.8527 0.095 Uiso 0.20 1 calc PR C 2 H3U2 H 0.8310 0.9890 0.9313 0.095 Uiso 0.20 1 calc PR C 2 H3U3 H 0.8820 1.0998 0.8933 0.095 Uiso 0.20 1 calc PR C 2 C2U C 0.715(2) 0.982(2) 0.8386(14) 0.059(5) Uani 0.20 1 d PU C 2 N1U N 0.6190(17) 0.9605(18) 0.8019(13) 0.048(4) Uani 0.20 1 d PU C 2 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 Cu1 0.01544(16) 0.01928(16) 0.01323(15) 0.00212(11) 0.00139(11) 0.00794(12) N1 0.0148(10) 0.0160(10) 0.0166(10) 0.0040(8) 0.0009(8) 0.0066(8) C1 0.0189(13) 0.0234(13) 0.0177(12) 0.0049(10) 0.0050(10) 0.0087(11) P1 0.0154(3) 0.0213(3) 0.0137(3) 0.0042(2) 0.0019(2) 0.0079(3) O1 0.0189(9) 0.0223(9) 0.0149(8) 0.0044(7) 0.0036(7) 0.0100(7) C2 0.0161(13) 0.0207(13) 0.0214(13) 0.0057(10) 0.0035(10) 0.0062(10) N2 0.0156(11) 0.0197(11) 0.0169(10) 0.0036(8) 0.0035(8) 0.0087(9) O2 0.0281(10) 0.0288(10) 0.0172(10) 0.0031(8) 0.0015(8) 0.0043(8) P2 0.0153(3) 0.0185(3) 0.0145(3) 0.0034(2) 0.0028(2) 0.0081(3) C3 0.0169(13) 0.0174(12) 0.0182(12) 0.0050(10) 0.0009(9) 0.0068(10) O3 0.0143(9) 0.0245(9) 0.0226(9) 0.0026(7) 0.0009(7) 0.0028(7) C4 0.0207(13) 0.0193(12) 0.0157(12) 0.0041(10) 0.0044(10) 0.0089(10) O4 0.0257(10) 0.0291(10) 0.0286(10) 0.0085(8) 0.0138(8) 0.0098(8) C5 0.0171(12) 0.0172(12) 0.0182(12) 0.0043(10) 0.0035(9) 0.0098(10) O5 0.0269(11) 0.0453(12) 0.0192(9) -0.0048(8) 0.0066(8) 0.0134(9) C6 0.0189(13) 0.0162(12) 0.0187(12) 0.0054(10) 0.0031(10) 0.0097(10) C7 0.0193(13) 0.0192(13) 0.0176(12) 0.0038(10) 0.0025(10) 0.0094(10) C8 0.0221(13) 0.0229(13) 0.0190(12) 0.0076(10) 0.0064(10) 0.0140(11) C9 0.0154(12) 0.0227(13) 0.0216(13) 0.0075(10) 0.0058(10) 0.0089(10) C10 0.0150(12) 0.0181(12) 0.0176(12) 0.0038(10) 0.0008(9) 0.0064(10) C11 0.0199(13) 0.0184(13) 0.0229(14) 0.0060(10) 0.0030(10) 0.0094(11) C12 0.0165(13) 0.0219(14) 0.0286(14) 0.0008(11) -0.0028(10) 0.0039(11) C13 0.0233(15) 0.0284(15) 0.0414(17) 0.0028(13) -0.0014(12) 0.0113(12) C14 0.0254(15) 0.0240(14) 0.0231(13) 0.0085(11) 0.0084(11) 0.0134(12) C15 0.047(3) 0.030(2) 0.0193(19) 0.0016(18) 0.0165(16) 0.022(2) C16 0.079(4) 0.043(3) 0.026(2) 0.012(2) 0.022(2) 0.032(3) C15' 0.032(5) 0.035(6) 0.026(5) -0.007(5) 0.009(4) 0.025(5) C16' 0.055(9) 0.072(11) 0.021(7) -0.002(6) 0.008(5) 0.027(8) C17 0.0182(13) 0.0160(12) 0.0183(12) 0.0047(10) 0.0015(10) 0.0066(10) C18 0.0246(14) 0.0269(14) 0.0202(13) 0.0062(11) 0.0047(10) 0.0103(12) C19 0.0333(16) 0.0289(15) 0.0169(13) 0.0063(11) 0.0007(11) 0.0097(13) C20 0.0227(14) 0.0260(14) 0.0268(15) 0.0112(12) -0.0043(11) 0.0048(11) C21 0.0212(14) 0.0270(14) 0.0352(16) 0.0124(12) 0.0031(11) 0.0116(12) C22 0.0224(14) 0.0231(13) 0.0234(13) 0.0058(11) 0.0032(10) 0.0121(11) C23 0.0152(12) 0.0269(13) 0.0155(12) 0.0059(10) 0.0032(9) 0.0125(11) C24 0.0307(15) 0.0259(14) 0.0223(13) 0.0050(11) 0.0099(11) 0.0132(12) C25 0.0407(18) 0.0302(16) 0.0319(16) 0.0019(12) 0.0145(13) 0.0178(14) C26 0.0325(16) 0.0445(18) 0.0221(14) 0.0059(12) 0.0122(12) 0.0213(14) C27 0.0210(14) 0.0376(16) 0.0230(14) 0.0133(12) 0.0089(11) 0.0134(12) C28 0.0197(13) 0.0258(14) 0.0180(12) 0.0056(10) 0.0020(10) 0.0102(11) C29 0.0213(13) 0.0183(12) 0.0128(11) 0.0017(9) 0.0049(9) 0.0085(10) C30 0.0229(14) 0.0240(14) 0.0182(12) 0.0044(10) 0.0036(10) 0.0112(11) C31 0.0327(16) 0.0254(14) 0.0250(14) 0.0095(11) 0.0075(11) 0.0149(12) C32 0.0292(15) 0.0258(14) 0.0288(15) 0.0102(12) 0.0134(12) 0.0080(12) C33 0.0194(14) 0.0252(14) 0.0280(14) 0.0064(11) 0.0070(11) 0.0075(11) C34 0.0224(13) 0.0209(13) 0.0130(12) 0.0031(10) 0.0036(10) 0.0112(11) C35 0.0134(12) 0.0258(13) 0.0154(12) 0.0020(10) 0.0012(9) 0.0085(10) C36 0.0214(14) 0.0222(13) 0.0233(13) 0.0029(11) 0.0010(10) 0.0082(11) C37 0.0297(15) 0.0273(15) 0.0226(14) -0.0032(11) 0.0011(11) 0.0127(12) C38 0.0253(14) 0.0340(15) 0.0152(13) -0.0006(11) 0.0029(10) 0.0111(12) C39 0.0184(13) 0.0312(15) 0.0178(13) 0.0068(11) 0.0026(10) 0.0107(11) C40 0.0117(12) 0.0239(13) 0.0181(12) 0.0002(10) 0.0001(9) 0.0064(10) C41 0.0192(13) 0.0290(14) 0.0123(12) 0.0076(10) 0.0038(9) 0.0121(11) C42 0.0218(14) 0.0315(15) 0.0223(13) 0.0006(11) 0.0011(11) 0.0128(12) C43 0.0325(16) 0.0380(16) 0.0219(14) 0.0018(12) 0.0044(11) 0.0216(14) C44 0.0244(15) 0.0494(18) 0.0203(13) 0.0107(12) 0.0067(11) 0.0240(14) C45 0.0156(13) 0.0395(16) 0.0250(14) 0.0122(12) 0.0049(10) 0.0106(12) C46 0.0227(14) 0.0285(14) 0.0157(12) 0.0079(10) 0.0031(10) 0.0111(11) C47 0.0207(13) 0.0219(13) 0.0145(12) 0.0035(10) 0.0030(10) 0.0093(11) C48 0.0199(13) 0.0254(14) 0.0194(13) 0.0035(10) 0.0026(10) 0.0102(11) C49 0.0225(14) 0.0266(14) 0.0276(14) 0.0065(11) 0.0075(11) 0.0076(12) C50 0.0334(16) 0.0276(15) 0.0234(14) 0.0121(11) 0.0103(12) 0.0092(12) C51 0.0322(16) 0.0367(16) 0.0215(14) 0.0130(12) 0.0030(11) 0.0167(13) C52 0.0196(14) 0.0304(15) 0.0208(13) 0.0077(11) 0.0010(10) 0.0087(11) B1S 0.0287(18) 0.0271(17) 0.0323(18) -0.0003(14) 0.0100(14) 0.0100(14) F1S 0.0422(11) 0.0703(13) 0.0311(10) -0.0008(9) 0.0153(8) 0.0102(10) F2S 0.0517(12) 0.0791(14) 0.0444(11) -0.0045(10) 0.0209(9) 0.0365(11) F3S 0.0479(12) 0.0406(11) 0.0692(14) 0.0046(10) -0.0023(10) -0.0033(10) F4S 0.0723(15) 0.0568(13) 0.0723(14) 0.0226(11) 0.0175(12) 0.0398(12) N1T 0.0207(15) 0.0264(16) 0.0462(19) -0.0042(14) 0.0030(13) 0.0117(13) C2T 0.059(3) 0.0210(18) 0.046(2) 0.0045(17) 0.025(2) 0.0214(19) C3T 0.105(6) 0.039(4) 0.041(3) -0.002(3) 0.011(4) 0.041(4) C3U 0.062(10) 0.053(10) 0.069(12) 0.013(9) -0.003(9) 0.030(9) C2U 0.060(9) 0.055(10) 0.061(12) 0.011(10) 0.009(9) 0.029(9) N1U 0.061(10) 0.046(10) 0.046(9) 0.027(7) 0.020(9) 0.024(9) _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 Cu1 N2 2.037(2) . ? Cu1 N1 2.0621(19) . ? Cu1 P1 2.2213(6) . ? Cu1 P2 2.2465(6) . ? N1 C10 1.343(3) . ? N1 C6 1.352(3) . ? C1 N2 1.341(3) . ? C1 C2 1.377(3) . ? C1 H1 0.9500 . ? P1 C40 1.826(2) . ? P1 C47 1.827(2) . ? P1 C41 1.828(2) . ? O1 C35 1.402(3) . ? O1 C34 1.404(3) . ? C2 C3 1.392(3) . ? C2 H2 0.9500 . ? N2 C5 1.356(3) . ? O2 C11 1.201(3) . ? P2 C23 1.818(2) . ? P2 C17 1.824(2) . ? P2 C29 1.832(2) . ? C3 C4 1.386(3) . ? C3 C11 1.494(3) . ? O3 C11 1.337(3) . ? O3 C12 1.458(3) . ? C4 C5 1.392(3) . ? C4 H4 0.9500 . ? O4 C14 1.210(3) . ? C5 C6 1.480(3) . ? O5 C14 1.329(3) . ? O5 C15 1.476(4) . ? O5 C15' 1.502(9) . ? C6 C7 1.395(3) . ? C7 C8 1.388(3) . ? C7 H7 0.9500 . ? C8 C9 1.384(3) . ? C8 C14 1.498(3) . ? C9 C10 1.382(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C12 C13 1.504(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C15 C16 1.501(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C15' C16' 1.51(2) . ? C15' H15C 0.9900 . ? C15' H15D 0.9900 . ? C16' H16D 0.9800 . ? C16' H16E 0.9800 . ? C16' H16F 0.9800 . ? C17 C18 1.393(3) . ? C17 C22 1.394(3) . ? C18 C19 1.386(3) . ? C18 H18 0.9500 . ? C19 C20 1.377(4) . ? C19 H19 0.9500 . ? C20 C21 1.382(4) . ? C20 H20 0.9500 . ? C21 C22 1.394(3) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.390(3) . ? C23 C28 1.395(3) . ? C24 C25 1.387(4) . ? C24 H24 0.9500 . ? C25 C26 1.383(4) . ? C25 H25 0.9500 . ? C26 C27 1.384(4) . ? C26 H26 0.9500 . ? C27 C28 1.385(3) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.395(3) . ? C29 C34 1.401(3) . ? C30 C31 1.387(4) . ? C30 H30 0.9500 . ? C31 C32 1.390(4) . ? C31 H31 0.9500 . ? C32 C33 1.391(4) . ? C32 H32 0.9500 . ? C33 C34 1.375(3) . ? C33 H33 0.9500 . ? C35 C36 1.383(3) . ? C35 C40 1.396(3) . ? C36 C37 1.384(4) . ? C36 H36 0.9500 . ? C37 C38 1.383(4) . ? C37 H37 0.9500 . ? C38 C39 1.386(4) . ? C38 H38 0.9500 . ? C39 C40 1.398(3) . ? C39 H39 0.9500 . ? C41 C46 1.384(3) . ? C41 C42 1.396(3) . ? C42 C43 1.381(4) . ? C42 H42 0.9500 . ? C43 C44 1.381(4) . ? C43 H43 0.9500 . ? C44 C45 1.385(4) . ? C44 H44 0.9500 . ? C45 C46 1.388(4) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C48 1.385(3) . ? C47 C52 1.399(3) . ? C48 C49 1.391(3) . ? C48 H48 0.9500 . ? C49 C50 1.384(4) . ? C49 H49 0.9500 . ? C50 C51 1.379(4) . ? C50 H50 0.9500 . ? C51 C52 1.387(4) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? B1S F2S 1.374(4) . ? B1S F4S 1.375(4) . ? B1S F3S 1.377(4) . ? B1S F1S 1.396(4) . ? N1T C2T 1.176(5) . ? C2T C3T 1.489(8) . ? C3T H3T1 0.9800 . ? C3T H3T2 0.9800 . ? C3T H3T3 0.9800 . ? C3U C2U 1.40(3) . ? C3U H3U1 0.9800 . ? C3U H3U2 0.9800 . ? C3U H3U3 0.9800 . ? C2U N1U 1.15(3) . ? 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 N2 Cu1 N1 80.30(8) . . ? N2 Cu1 P1 128.87(6) . . ? N1 Cu1 P1 111.47(5) . . ? N2 Cu1 P2 109.74(6) . . ? N1 Cu1 P2 112.26(5) . . ? P1 Cu1 P2 110.40(2) . . ? C10 N1 C6 118.4(2) . . ? C10 N1 Cu1 127.68(16) . . ? C6 N1 Cu1 113.89(15) . . ? N2 C1 C2 123.2(2) . . ? N2 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C40 P1 C47 104.52(11) . . ? C40 P1 C41 105.09(11) . . ? C47 P1 C41 103.78(11) . . ? C40 P1 Cu1 111.56(8) . . ? C47 P1 Cu1 119.24(8) . . ? C41 P1 Cu1 111.44(8) . . ? C35 O1 C34 114.82(17) . . ? C1 C2 C3 118.6(2) . . ? C1 C2 H2 120.7 . . ? C3 C2 H2 120.7 . . ? C1 N2 C5 118.1(2) . . ? C1 N2 Cu1 127.14(16) . . ? C5 N2 Cu1 114.08(15) . . ? C23 P2 C17 102.33(11) . . ? C23 P2 C29 105.94(11) . . ? C17 P2 C29 102.36(11) . . ? C23 P2 Cu1 115.90(8) . . ? C17 P2 Cu1 114.38(8) . . ? C29 P2 Cu1 114.34(8) . . ? C4 C3 C2 119.2(2) . . ? C4 C3 C11 118.4(2) . . ? C2 C3 C11 122.3(2) . . ? C11 O3 C12 116.69(19) . . ? C3 C4 C5 118.8(2) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N2 C5 C4 122.0(2) . . ? N2 C5 C6 115.6(2) . . ? C4 C5 C6 122.4(2) . . ? C14 O5 C15 118.4(3) . . ? C14 O5 C15' 108.1(7) . . ? C15 O5 C15' 24.1(5) . . ? N1 C6 C7 121.9(2) . . ? N1 C6 C5 115.2(2) . . ? C7 C6 C5 122.9(2) . . ? C8 C7 C6 118.8(2) . . ? C8 C7 H7 120.6 . . ? C6 C7 H7 120.6 . . ? C9 C8 C7 119.1(2) . . ? C9 C8 C14 119.0(2) . . ? C7 C8 C14 121.9(2) . . ? C10 C9 C8 119.0(2) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? N1 C10 C9 122.7(2) . . ? N1 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? O2 C11 O3 124.9(2) . . ? O2 C11 C3 123.9(2) . . ? O3 C11 C3 111.2(2) . . ? O3 C12 C13 110.4(2) . . ? O3 C12 H12A 109.6 . . ? C13 C12 H12A 109.6 . . ? O3 C12 H12B 109.6 . . ? C13 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O4 C14 O5 125.4(2) . . ? O4 C14 C8 123.2(2) . . ? O5 C14 C8 111.5(2) . . ? O5 C15 C16 107.3(3) . . ? O5 C15 H15A 110.3 . . ? C16 C15 H15A 110.3 . . ? O5 C15 H15B 110.3 . . ? C16 C15 H15B 110.3 . . ? H15A C15 H15B 108.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O5 C15' C16' 111.5(11) . . ? O5 C15' H15C 109.3 . . ? C16' C15' H15C 109.3 . . ? O5 C15' H15D 109.3 . . ? C16' C15' H15D 109.3 . . ? H15C C15' H15D 108.0 . . ? C15' C16' H16D 109.5 . . ? C15' C16' H16E 109.5 . . ? H16D C16' H16E 109.5 . . ? C15' C16' H16F 109.5 . . ? H16D C16' H16F 109.5 . . ? H16E C16' H16F 109.5 . . ? C18 C17 C22 119.1(2) . . ? C18 C17 P2 117.45(18) . . ? C22 C17 P2 123.42(18) . . ? C19 C18 C17 120.4(2) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C20 C19 C18 120.4(2) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C19 C20 C21 119.8(2) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C20 C21 C22 120.4(2) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C17 C22 C21 119.8(2) . . ? C17 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C24 C23 C28 119.2(2) . . ? C24 C23 P2 123.86(19) . . ? C28 C23 P2 116.87(18) . . ? C25 C24 C23 120.0(2) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C26 C25 C24 120.3(3) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C25 C26 C27 120.2(2) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C26 C27 C28 119.6(2) . . ? C26 C27 H27 120.2 . . ? C28 C27 H27 120.2 . . ? C27 C28 C23 120.6(2) . . ? C27 C28 H28 119.7 . . ? C23 C28 H28 119.7 . . ? C30 C29 C34 117.1(2) . . ? C30 C29 P2 122.46(19) . . ? C34 C29 P2 120.28(17) . . ? C31 C30 C29 121.3(2) . . ? C31 C30 H30 119.3 . . ? C29 C30 H30 119.3 . . ? C30 C31 C32 120.3(2) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C31 C32 C33 119.2(2) . . ? C31 C32 H32 120.4 . . ? C33 C32 H32 120.4 . . ? C34 C33 C32 119.9(2) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C29 122.1(2) . . ? C33 C34 O1 118.4(2) . . ? C29 C34 O1 119.5(2) . . ? C36 C35 C40 122.1(2) . . ? C36 C35 O1 121.4(2) . . ? C40 C35 O1 116.5(2) . . ? C35 C36 C37 119.2(2) . . ? C35 C36 H36 120.4 . . ? C37 C36 H36 120.4 . . ? C38 C37 C36 120.1(2) . . ? C38 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? C37 C38 C39 120.1(2) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C38 C39 C40 121.0(2) . . ? C38 C39 H39 119.5 . . ? C40 C39 H39 119.5 . . ? C35 C40 C39 117.3(2) . . ? C35 C40 P1 118.90(18) . . ? C39 C40 P1 123.53(19) . . ? C46 C41 C42 118.6(2) . . ? C46 C41 P1 124.30(19) . . ? C42 C41 P1 117.05(19) . . ? C43 C42 C41 121.0(3) . . ? C43 C42 H42 119.5 . . ? C41 C42 H42 119.5 . . ? C44 C43 C42 119.9(2) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C43 C44 C45 119.8(2) . . ? C43 C44 H44 120.1 . . ? C45 C44 H44 120.1 . . ? C44 C45 C46 120.2(2) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? C41 C46 C45 120.5(2) . . ? C41 C46 H46 119.7 . . ? C45 C46 H46 119.7 . . ? C48 C47 C52 119.0(2) . . ? C48 C47 P1 118.22(18) . . ? C52 C47 P1 122.76(19) . . ? C47 C48 C49 121.1(2) . . ? C47 C48 H48 119.4 . . ? C49 C48 H48 119.4 . . ? C50 C49 C48 119.1(2) . . ? C50 C49 H49 120.4 . . ? C48 C49 H49 120.4 . . ? C51 C50 C49 120.5(2) . . ? C51 C50 H50 119.8 . . ? C49 C50 H50 119.8 . . ? C50 C51 C52 120.4(2) . . ? C50 C51 H51 119.8 . . ? C52 C51 H51 119.8 . . ? C51 C52 C47 119.8(2) . . ? C51 C52 H52 120.1 . . ? C47 C52 H52 120.1 . . ? F2S B1S F4S 110.0(3) . . ? F2S B1S F3S 111.8(2) . . ? F4S B1S F3S 109.8(3) . . ? F2S B1S F1S 107.9(3) . . ? F4S B1S F1S 108.6(2) . . ? F3S B1S F1S 108.7(3) . . ? N1T C2T C3T 174.9(5) . . ? C2U C3U H3U1 109.5 . . ? C2U C3U H3U2 109.5 . . ? H3U1 C3U H3U2 109.5 . . ? C2U C3U H3U3 109.5 . . ? H3U1 C3U H3U3 109.5 . . ? H3U2 C3U H3U3 109.5 . . ? N1U C2U C3U 177(3) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.05 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.596 _refine_diff_density_min -0.565 _refine_diff_density_rms 0.070 # Attachment '- nr7004_2.cif' data_NR7004 _database_code_depnum_ccdc_archive 'CCDC 771440' #TrackingRef '- nr7004_2.cif' _audit_creation_date 07-12-14 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'nr7004 in P2(1)/c' _chemical_name_systematic ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H34 Cu1 N4 O1 P2, (B F4)' _chemical_compound_source Moudam _exptl_crystal_recrystallization_method ; ; _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_related_literature # Not in version 2.3.1 ############################################################### # Essential references (e.g. to the origin of the material studied, related # structural studies, and to information supporting the reported structure) # should be cited in this section, with appropriate very brief explanatory # text, for example `The synthesis of the complex is described by Jones # (2001). The anhydrous complex has essentially the same coordination # geometry (Smith, 2003).' In addition, all references included in the # supplementary materials, but not elsewhere in the published article, # should be given here. The simple text `For related literature, see:...' # may be used, but further details should be provided in the Comment # section, which forms part of the supplementary material. ############################################################### ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fig. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. 912_ALERT_3_B # Missing FCF Reflections Above STh/L= 0.600 737 910_ALERT_3_C # Missing FCF Reflections Below Th(Min) ........ 1 911_ALERT_3_C # Missing FCF Refl Between THmin & STh/L= 0.600 1 913_ALERT_3_C # Missing Very Strong Reflections in FCF ....... 1 #============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 1.000 4046 4044 2 23.01 0.550 1.000 5380 5378 2 25.24 0.600 1.000 6978 6976 2 #----------------------------------------------------------- ACTA Min. Res. --- 27.51 0.650 1.000 8869 8865 4 29.74 0.698 0.933 10978 10239 739 061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.85 Sadabs corrects 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. 244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for B53 No action taken. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # # End of 'script/refcif-b.dat' #end of refcif _cell_length_a 9.5405(2) _cell_length_b 19.8580(4) _cell_length_c 20.4442(4) _cell_angle_alpha 90 _cell_angle_beta 95.4810(10) _cell_angle_gamma 90 _cell_volume 3855.55(14) _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' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cu 0.3201 1.2651 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126 1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 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' 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' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C44 H34 B1 Cu1 F4 N4 O1 P2 # Dc = 1.46 Fooo = 1736.00 Mu = 7.11 M = 847.08 # Found Formula = C44 H34 B1 Cu1 F4 N4 O1 P2 # Dc = 1.46 FOOO = 1736.00 Mu = 7.11 M = 847.08 _chemical_formula_sum 'C44 H34 B1 Cu1 F4 N4 O1 P2' _chemical_formula_weight 847.08 _cell_measurement_reflns_used 9876 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_min 0.22 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_max 0.36 _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 0.711 # Sheldrick geometric approximatio 0.79 0.86 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.66 _exptl_absorpt_correction_T_max 0.86 _diffrn_measurement_device 'Bruker SMART' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction 'SAINT (Siemens ,1995)' _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 150 _diffrn_reflns_number 31367 _reflns_number_total 10239 _diffrn_reflns_av_R_equivalents 0.038 # Number of reflections with Friedels Law is 10239 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 10985 _diffrn_reflns_theta_min 2.001 _diffrn_reflns_theta_max 29.743 _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 28.255 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _reflns_limit_h_min -13 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 27 _reflns_limit_l_min 0 _reflns_limit_l_max 27 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.64 _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 # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 10239 _refine_ls_number_restraints 0 _refine_ls_number_parameters 514 _oxford_refine_ls_R_factor_ref 0.0667 _refine_ls_wR_factor_ref 0.1168 _refine_ls_goodness_of_fit_ref 1.0387 _refine_ls_shift/su_max 0.001334 # The values computed from all data _oxford_reflns_number_all 10239 _refine_ls_R_factor_all 0.0667 _refine_ls_wR_factor_all 0.1168 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 8089 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_gt 0.1071 # 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 # 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^) + ( 0.03P)^2^ + 0.00P] ,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, G., 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. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. 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 _oxford_atom_site_special_shape _atom_site_attached_hydrogens Cu1 Cu 0.59097(3) 0.626227(15) 0.760628(15) 0.0179 1.0000 Uani . . . . . . . P1 P 0.55531(6) 0.56458(3) 0.66830(3) 0.0173 1.0000 Uani . . . . . . . P2 P 0.82324(6) 0.63173(3) 0.79779(3) 0.0178 1.0000 Uani . . . . . . . O1 O 0.76245(18) 0.48851(9) 0.74804(9) 0.0215 1.0000 Uani . . . . . . . C27 C 0.8149(3) 0.50346(12) 0.68827(12) 0.0206 1.0000 Uani . . . . . . . C32 C 0.7249(2) 0.53812(12) 0.64252(12) 0.0192 1.0000 Uani . . . . . . . C31 C 0.7727(3) 0.55298(14) 0.58201(13) 0.0256 1.0000 Uani . . . . . . . C30 C 0.9069(3) 0.53381(15) 0.56821(15) 0.0318 1.0000 Uani . . . . . . . C29 C 0.9929(3) 0.49830(16) 0.61402(15) 0.0340 1.0000 Uani . . . . . . . C28 C 0.9481(3) 0.48254(14) 0.67450(14) 0.0278 1.0000 Uani . . . . . . . C26 C 0.8571(3) 0.49115(13) 0.80462(13) 0.0229 1.0000 Uani . . . . . . . C21 C 0.8955(3) 0.55279(13) 0.83367(12) 0.0209 1.0000 Uani . . . . . . . C22 C 0.9876(3) 0.55186(14) 0.89128(13) 0.0269 1.0000 Uani . . . . . . . C23 C 1.0372(3) 0.49160(16) 0.91845(15) 0.0338 1.0000 Uani . . . . . . . C24 C 0.9962(3) 0.43120(16) 0.88945(17) 0.0394 1.0000 Uani . . . . . . . C25 C 0.9050(3) 0.43040(15) 0.83252(15) 0.0341 1.0000 Uani . . . . . . . C33 C 0.4727(3) 0.60952(12) 0.59681(12) 0.0192 1.0000 Uani . . . . . . . C34 C 0.5231(3) 0.67377(13) 0.58396(13) 0.0237 1.0000 Uani . . . . . . . C35 C 0.4600(3) 0.71240(14) 0.53286(13) 0.0270 1.0000 Uani . . . . . . . C36 C 0.3448(3) 0.68719(14) 0.49381(13) 0.0268 1.0000 Uani . . . . . . . C37 C 0.2938(3) 0.62363(14) 0.50630(13) 0.0269 1.0000 Uani . . . . . . . C38 C 0.3572(3) 0.58477(14) 0.55750(13) 0.0239 1.0000 Uani . . . . . . . C39 C 0.4592(3) 0.48509(12) 0.66660(12) 0.0192 1.0000 Uani . . . . . . . C40 C 0.4711(3) 0.43882(13) 0.61550(13) 0.0247 1.0000 Uani . . . . . . . C41 C 0.3933(3) 0.38011(14) 0.61266(14) 0.0312 1.0000 Uani . . . . . . . C42 C 0.3049(3) 0.36580(14) 0.66073(15) 0.0314 1.0000 Uani . . . . . . . C43 C 0.2942(3) 0.41044(15) 0.71182(14) 0.0281 1.0000 Uani . . . . . . . C44 C 0.3702(3) 0.47033(14) 0.71457(13) 0.0230 1.0000 Uani . . . . . . . C9 C 0.8685(2) 0.69235(12) 0.86352(12) 0.0189 1.0000 Uani . . . . . . . C10 C 0.9772(3) 0.73900(14) 0.86130(13) 0.0248 1.0000 Uani . . . . . . . C11 C 1.0054(3) 0.78489(14) 0.91180(14) 0.0288 1.0000 Uani . . . . . . . C12 C 0.9289(3) 0.78400(15) 0.96591(14) 0.0307 1.0000 Uani . . . . . . . C13 C 0.8223(3) 0.73706(15) 0.96933(13) 0.0301 1.0000 Uani . . . . . . . C14 C 0.7914(3) 0.69205(14) 0.91829(13) 0.0259 1.0000 Uani . . . . . . . C15 C 0.9448(3) 0.65518(13) 0.73795(12) 0.0205 1.0000 Uani . . . . . . . C16 C 0.9029(3) 0.70551(14) 0.69337(13) 0.0270 1.0000 Uani . . . . . . . C17 C 0.9950(3) 0.72944(16) 0.64983(14) 0.0345 1.0000 Uani . . . . . . . C18 C 1.1291(3) 0.70246(17) 0.65077(15) 0.0370 1.0000 Uani . . . . . . . C19 C 1.1710(3) 0.65188(16) 0.69460(14) 0.0324 1.0000 Uani . . . . . . . C20 C 1.0799(3) 0.62834(14) 0.73857(13) 0.0256 1.0000 Uani . . . . . . . C5 C 0.4034(3) 0.66212(13) 0.85838(12) 0.0197 1.0000 Uani . . . . . . . N1 N 0.4766(2) 0.60854(10) 0.83985(10) 0.0195 1.0000 Uani . . . . . . . C8 C 0.4754(3) 0.55359(14) 0.87815(13) 0.0253 1.0000 Uani . . . . . . . C7 C 0.4042(3) 0.55287(14) 0.93373(13) 0.0295 1.0000 Uani . . . . . . . C6 C 0.3363(3) 0.61109(15) 0.94923(13) 0.0303 1.0000 Uani . . . . . . . N4 N 0.3334(2) 0.66601(12) 0.91138(11) 0.0265 1.0000 Uani . . . . . . . C4 C 0.4028(3) 0.72199(13) 0.81471(12) 0.0193 1.0000 Uani . . . . . . . N2 N 0.4854(2) 0.71824(10) 0.76508(10) 0.0184 1.0000 Uani . . . . . . . C1 C 0.4834(3) 0.77196(13) 0.72542(13) 0.0229 1.0000 Uani . . . . . . . C2 C 0.4016(3) 0.82779(14) 0.73445(14) 0.0270 1.0000 Uani . . . . . . . C3 C 0.3219(3) 0.82622(14) 0.78716(14) 0.0269 1.0000 Uani . . . . . . . N3 N 0.3213(2) 0.77355(11) 0.82793(11) 0.0247 1.0000 Uani . . . . . . . B53 B 0.6339(4) 0.62281(18) 1.09532(16) 0.0307 1.0000 Uani . . . . . . . F54 F 0.4885(2) 0.62269(13) 1.09589(11) 0.0594 1.0000 Uani . . . . . . . F55 F 0.6884(2) 0.68533(9) 1.11329(9) 0.0387 1.0000 Uani . . . . . . . F56 F 0.6898(2) 0.57463(10) 1.13926(9) 0.0506 1.0000 Uani . . . . . . . F57 F 0.6676(2) 0.60640(9) 1.03252(8) 0.0409 1.0000 Uani . . . . . . . H241 H 0.5317 0.4481 0.5834 0.0300 1.0000 Uiso R . . . . . . H251 H 0.4007 0.3497 0.5788 0.0369 1.0000 Uiso R . . . . . . H261 H 0.2515 0.3264 0.6591 0.0366 1.0000 Uiso R . . . . . . H271 H 0.2383 0.4007 0.7451 0.0337 1.0000 Uiso R . . . . . . H281 H 0.3617 0.5008 0.7490 0.0270 1.0000 Uiso R . . . . . . H221 H 0.3220 0.5428 0.5656 0.0288 1.0000 Uiso R . . . . . . H211 H 0.2163 0.6066 0.4800 0.0317 1.0000 Uiso R . . . . . . H201 H 0.3018 0.7135 0.4594 0.0319 1.0000 Uiso R . . . . . . H191 H 0.4937 0.7557 0.5252 0.0323 1.0000 Uiso R . . . . . . H181 H 0.6008 0.6911 0.6101 0.0281 1.0000 Uiso R . . . . . . H101 H 1.0057 0.4588 0.7049 0.0329 1.0000 Uiso R . . . . . . H91 H 1.0813 0.4851 0.6046 0.0411 1.0000 Uiso R . . . . . . H81 H 0.9369 0.5458 0.5280 0.0390 1.0000 Uiso R . . . . . . H71 H 0.7155 0.5762 0.5509 0.0308 1.0000 Uiso R . . . . . . H131 H 1.0159 0.5932 0.9111 0.0318 1.0000 Uiso R . . . . . . H141 H 1.0991 0.4914 0.9568 0.0400 1.0000 Uiso R . . . . . . H151 H 1.0296 0.3909 0.9082 0.0461 1.0000 Uiso R . . . . . . H161 H 0.8771 0.3904 0.8128 0.0398 1.0000 Uiso R . . . . . . H301 H 1.0314 0.7396 0.8259 0.0301 1.0000 Uiso R . . . . . . H311 H 1.0756 0.8164 0.9089 0.0342 1.0000 Uiso R . . . . . . H321 H 0.9476 0.8149 0.9999 0.0359 1.0000 Uiso R . . . . . . H331 H 0.7722 0.7356 1.0057 0.0361 1.0000 Uiso R . . . . . . H341 H 0.7198 0.6603 0.9208 0.0301 1.0000 Uiso R . . . . . . H361 H 0.8140 0.7233 0.6928 0.0316 1.0000 Uiso R . . . . . . H371 H 0.9662 0.7639 0.6199 0.0411 1.0000 Uiso R . . . . . . H381 H 1.1891 0.7188 0.6215 0.0449 1.0000 Uiso R . . . . . . H391 H 1.2611 0.6333 0.6957 0.0394 1.0000 Uiso R . . . . . . H401 H 1.1085 0.5944 0.7684 0.0311 1.0000 Uiso R . . . . . . H431 H 0.5246 0.5152 0.8662 0.0298 1.0000 Uiso R . . . . . . H441 H 0.4020 0.5150 0.9594 0.0345 1.0000 Uiso R . . . . . . H451 H 0.2924 0.6130 0.9883 0.0370 1.0000 Uiso R . . . . . . H511 H 0.2672 0.8633 0.7960 0.0318 1.0000 Uiso R . . . . . . H501 H 0.4002 0.8646 0.7057 0.0314 1.0000 Uiso R . . . . . . H491 H 0.5395 0.7707 0.6912 0.0280 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 Cu1 0.01519(14) 0.01852(15) 0.02024(14) -0.00167(12) 0.00285(11) 0.00144(11) P1 0.0156(3) 0.0176(3) 0.0188(3) -0.0012(2) 0.0017(2) 0.0003(2) P2 0.0158(3) 0.0177(3) 0.0198(3) -0.0014(2) 0.0017(2) 0.0007(2) O1 0.0188(8) 0.0200(9) 0.0252(9) -0.0021(7) -0.0005(7) 0.0001(7) C27 0.0186(11) 0.0173(11) 0.0259(12) -0.0055(10) 0.0023(10) -0.0012(9) C32 0.0159(11) 0.0188(11) 0.0233(11) -0.0062(9) 0.0039(9) -0.0010(9) C31 0.0263(13) 0.0252(13) 0.0259(12) -0.0025(10) 0.0048(11) 0.0003(11) C30 0.0314(15) 0.0319(15) 0.0345(15) -0.0060(12) 0.0151(13) 0.0007(12) C29 0.0206(13) 0.0378(16) 0.0453(17) -0.0131(14) 0.0119(13) 0.0010(12) C28 0.0206(12) 0.0260(14) 0.0363(15) -0.0061(11) 0.0005(11) 0.0053(10) C26 0.0188(11) 0.0235(13) 0.0258(12) 0.0015(10) -0.0014(10) 0.0019(10) C21 0.0189(11) 0.0211(12) 0.0228(11) 0.0009(10) 0.0021(9) 0.0002(9) C22 0.0249(13) 0.0276(14) 0.0272(13) -0.0021(11) -0.0036(11) 0.0027(11) C23 0.0323(15) 0.0343(16) 0.0322(15) 0.0074(12) -0.0110(12) 0.0047(13) C24 0.0376(17) 0.0296(16) 0.0481(19) 0.0103(14) -0.0108(15) 0.0046(13) C25 0.0353(16) 0.0210(14) 0.0438(17) 0.0022(12) -0.0076(14) 0.0022(12) C33 0.0195(11) 0.0196(11) 0.0189(11) -0.0003(9) 0.0033(9) 0.0012(9) C34 0.0232(12) 0.0229(13) 0.0250(12) -0.0013(10) 0.0015(10) -0.0003(10) C35 0.0277(13) 0.0258(13) 0.0278(13) 0.0032(11) 0.0034(11) -0.0032(11) C36 0.0272(13) 0.0294(14) 0.0239(12) 0.0061(11) 0.0020(11) 0.0023(11) C37 0.0220(12) 0.0315(14) 0.0256(12) 0.0014(11) -0.0055(10) -0.0012(11) C38 0.0221(12) 0.0239(13) 0.0254(12) 0.0004(10) 0.0016(10) -0.0023(10) C39 0.0184(11) 0.0179(11) 0.0208(11) -0.0007(9) -0.0008(9) -0.0015(9) C40 0.0246(12) 0.0230(13) 0.0266(12) -0.0022(10) 0.0032(10) 0.0002(10) C41 0.0357(15) 0.0250(14) 0.0323(14) -0.0063(12) 0.0001(12) -0.0029(12) C42 0.0251(13) 0.0246(14) 0.0430(16) 0.0043(12) -0.0055(12) -0.0069(11) C43 0.0207(12) 0.0319(15) 0.0314(14) 0.0081(12) 0.0008(11) -0.0028(11) C44 0.0186(11) 0.0268(13) 0.0233(12) 0.0019(10) 0.0000(10) 0.0007(10) C9 0.0164(11) 0.0192(11) 0.0201(11) -0.0049(9) -0.0030(9) 0.0004(9) C10 0.0180(11) 0.0284(14) 0.0280(13) -0.0042(11) 0.0014(10) 0.0006(10) C11 0.0242(13) 0.0264(14) 0.0348(15) -0.0066(12) -0.0020(11) -0.0042(11) C12 0.0349(15) 0.0292(14) 0.0267(13) -0.0088(11) -0.0034(12) 0.0031(12) C13 0.0326(14) 0.0351(15) 0.0231(13) -0.0043(11) 0.0049(11) 0.0029(12) C14 0.0244(13) 0.0289(14) 0.0246(12) -0.0015(11) 0.0040(10) -0.0010(11) C15 0.0203(11) 0.0215(12) 0.0201(11) -0.0022(9) 0.0035(9) -0.0034(9) C16 0.0238(13) 0.0303(14) 0.0267(13) 0.0001(11) 0.0004(11) -0.0028(11) C17 0.0408(17) 0.0345(16) 0.0281(14) 0.0061(12) 0.0032(13) -0.0100(13) C18 0.0381(17) 0.0449(18) 0.0304(15) -0.0081(13) 0.0153(13) -0.0164(14) C19 0.0221(13) 0.0404(17) 0.0364(15) -0.0142(13) 0.0121(12) -0.0054(12) C20 0.0197(12) 0.0287(14) 0.0290(13) -0.0052(11) 0.0056(10) -0.0008(10) C5 0.0193(11) 0.0195(12) 0.0202(11) -0.0032(9) 0.0019(9) -0.0018(9) N1 0.0187(10) 0.0188(10) 0.0209(10) -0.0001(8) 0.0010(8) -0.0007(8) C8 0.0274(13) 0.0224(13) 0.0257(12) 0.0014(10) -0.0001(11) 0.0008(10) C7 0.0373(15) 0.0268(14) 0.0239(13) 0.0070(11) 0.0009(12) -0.0020(12) C6 0.0366(15) 0.0336(15) 0.0216(12) -0.0002(11) 0.0072(12) -0.0050(12) N4 0.0311(12) 0.0275(12) 0.0221(10) -0.0028(9) 0.0082(9) -0.0002(10) C4 0.0171(11) 0.0203(12) 0.0204(11) -0.0026(9) 0.0006(9) -0.0016(9) N2 0.0163(9) 0.0178(10) 0.0210(10) -0.0010(8) 0.0013(8) -0.0012(8) C1 0.0218(12) 0.0233(12) 0.0238(12) 0.0010(10) 0.0033(10) -0.0004(10) C2 0.0299(14) 0.0199(12) 0.0310(14) 0.0018(11) 0.0019(11) 0.0006(11) C3 0.0269(13) 0.0203(12) 0.0333(14) -0.0035(11) 0.0026(11) 0.0054(10) N3 0.0240(11) 0.0229(11) 0.0279(11) -0.0027(9) 0.0051(9) 0.0039(9) B53 0.0333(17) 0.0309(17) 0.0290(15) -0.0041(13) 0.0087(13) -0.0022(14) F54 0.0342(11) 0.0843(18) 0.0611(14) -0.0184(13) 0.0117(10) -0.0093(11) F55 0.0445(11) 0.0287(9) 0.0437(10) -0.0073(8) 0.0078(9) -0.0012(8) F56 0.0816(16) 0.0373(11) 0.0331(10) 0.0067(8) 0.0058(10) -0.0034(11) F57 0.0577(12) 0.0382(10) 0.0284(9) -0.0029(8) 0.0130(9) -0.0071(9) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.3493(3) 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 Cu1 . P1 . 2.2482(7) yes Cu1 . P2 . 2.2756(7) yes Cu1 . N1 . 2.068(2) yes Cu1 . N2 . 2.093(2) yes P1 . C32 . 1.826(2) yes P1 . C33 . 1.826(3) yes P1 . C39 . 1.824(2) yes P2 . C21 . 1.837(3) yes P2 . C9 . 1.825(2) yes P2 . C15 . 1.825(2) yes O1 . C27 . 1.396(3) yes O1 . C26 . 1.399(3) yes C27 . C32 . 1.390(3) yes C27 . C28 . 1.392(3) yes C32 . C31 . 1.390(3) yes C31 . C30 . 1.390(4) yes C31 . H71 . 0.922 no C30 . C29 . 1.378(4) yes C30 . H81 . 0.928 no C29 . C28 . 1.382(4) yes C29 . H91 . 0.921 no C28 . H101 . 0.919 no C26 . C21 . 1.394(4) yes C26 . C25 . 1.393(4) yes C21 . C22 . 1.401(3) yes C22 . C23 . 1.384(4) yes C22 . H131 . 0.943 no C23 . C24 . 1.378(4) yes C23 . H141 . 0.935 no C24 . C25 . 1.385(4) yes C24 . H151 . 0.931 no C25 . H161 . 0.919 no C33 . C34 . 1.397(3) yes C33 . C38 . 1.391(3) yes C34 . C35 . 1.386(4) yes C34 . H181 . 0.936 no C35 . C36 . 1.389(4) yes C35 . H191 . 0.936 no C36 . C37 . 1.385(4) yes C36 . H201 . 0.938 no C37 . C38 . 1.391(4) yes C37 . H211 . 0.935 no C38 . H221 . 0.920 no C39 . C40 . 1.404(3) yes C39 . C44 . 1.389(3) yes C40 . C41 . 1.381(4) yes C40 . H241 . 0.934 no C41 . C42 . 1.384(4) yes C41 . H251 . 0.928 no C42 . C43 . 1.381(4) yes C42 . H261 . 0.932 no C43 . C44 . 1.391(4) yes C43 . H271 . 0.925 no C44 . H281 . 0.937 no C9 . C10 . 1.395(3) yes C9 . C14 . 1.397(3) yes C10 . C11 . 1.384(4) yes C10 . H301 . 0.929 no C11 . C12 . 1.383(4) yes C11 . H311 . 0.922 no C12 . C13 . 1.386(4) yes C12 . H321 . 0.932 no C13 . C14 . 1.384(4) yes C13 . H331 . 0.922 no C14 . H341 . 0.935 no C15 . C16 . 1.386(4) yes C15 . C20 . 1.394(3) yes C16 . C17 . 1.392(4) yes C16 . H361 . 0.917 no C17 . C18 . 1.386(4) yes C17 . H371 . 0.941 no C18 . C19 . 1.380(5) yes C18 . H381 . 0.925 no C19 . C20 . 1.390(4) yes C19 . H391 . 0.933 no C20 . H401 . 0.931 no C5 . N1 . 1.346(3) yes C5 . N4 . 1.328(3) yes C5 . C4 . 1.487(3) yes N1 . C8 . 1.344(3) yes C8 . C7 . 1.379(4) yes C8 . H431 . 0.940 no C7 . C6 . 1.377(4) yes C7 . H441 . 0.918 no C6 . N4 . 1.336(4) yes C6 . H451 . 0.937 no C4 . N2 . 1.345(3) yes C4 . N3 . 1.329(3) yes N2 . C1 . 1.339(3) yes C1 . C2 . 1.378(4) yes C1 . H491 . 0.921 no C2 . C3 . 1.377(4) yes C2 . H501 . 0.937 no C3 . N3 . 1.338(3) yes C3 . H511 . 0.930 no B53 . F54 . 1.389(4) yes B53 . F55 . 1.382(4) yes B53 . F56 . 1.384(4) yes B53 . F57 . 1.392(3) yes 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 P1 . Cu1 . P2 . 111.77(2) yes P1 . Cu1 . N1 . 121.08(6) yes P2 . Cu1 . N1 . 108.47(6) yes P1 . Cu1 . N2 . 118.49(6) yes P2 . Cu1 . N2 . 113.65(6) yes N1 . Cu1 . N2 . 79.74(8) yes Cu1 . P1 . C32 . 109.38(8) yes Cu1 . P1 . C33 . 115.16(8) yes C32 . P1 . C33 . 103.66(11) yes Cu1 . P1 . C39 . 121.51(8) yes C32 . P1 . C39 . 101.72(11) yes C33 . P1 . C39 . 103.29(11) yes Cu1 . P2 . C21 . 114.11(8) yes Cu1 . P2 . C9 . 115.58(8) yes C21 . P2 . C9 . 102.45(11) yes Cu1 . P2 . C15 . 116.72(8) yes C21 . P2 . C15 . 104.31(11) yes C9 . P2 . C15 . 101.80(11) yes C27 . O1 . C26 . 117.31(19) yes O1 . C27 . C32 . 116.4(2) yes O1 . C27 . C28 . 121.6(2) yes C32 . C27 . C28 . 121.9(2) yes P1 . C32 . C27 . 117.09(18) yes P1 . C32 . C31 . 124.8(2) yes C27 . C32 . C31 . 118.0(2) yes C32 . C31 . C30 . 120.6(3) yes C32 . C31 . H71 . 119.8 no C30 . C31 . H71 . 119.5 no C31 . C30 . C29 . 120.1(3) yes C31 . C30 . H81 . 118.5 no C29 . C30 . H81 . 121.4 no C30 . C29 . C28 . 120.6(3) yes C30 . C29 . H91 . 120.0 no C28 . C29 . H91 . 119.4 no C27 . C28 . C29 . 118.7(3) yes C27 . C28 . H101 . 121.0 no C29 . C28 . H101 . 120.3 no O1 . C26 . C21 . 120.5(2) yes O1 . C26 . C25 . 117.8(2) yes C21 . C26 . C25 . 121.6(2) yes P2 . C21 . C26 . 120.41(19) yes P2 . C21 . C22 . 121.9(2) yes C26 . C21 . C22 . 117.7(2) yes C21 . C22 . C23 . 120.8(3) yes C21 . C22 . H131 . 118.7 no C23 . C22 . H131 . 120.5 no C22 . C23 . C24 . 120.5(3) yes C22 . C23 . H141 . 120.3 no C24 . C23 . H141 . 119.2 no C23 . C24 . C25 . 120.1(3) yes C23 . C24 . H151 . 120.0 no C25 . C24 . H151 . 119.9 no C26 . C25 . C24 . 119.3(3) yes C26 . C25 . H161 . 120.0 no C24 . C25 . H161 . 120.7 no P1 . C33 . C34 . 117.82(19) yes P1 . C33 . C38 . 123.21(19) yes C34 . C33 . C38 . 118.8(2) yes C33 . C34 . C35 . 121.0(2) yes C33 . C34 . H181 . 119.8 no C35 . C34 . H181 . 119.3 no C34 . C35 . C36 . 119.8(3) yes C34 . C35 . H191 . 120.2 no C36 . C35 . H191 . 120.0 no C35 . C36 . C37 . 119.7(3) yes C35 . C36 . H201 . 119.7 no C37 . C36 . H201 . 120.6 no C36 . C37 . C38 . 120.6(3) yes C36 . C37 . H211 . 119.7 no C38 . C37 . H211 . 119.7 no C37 . C38 . C33 . 120.2(2) yes C37 . C38 . H221 . 119.9 no C33 . C38 . H221 . 120.0 no P1 . C39 . C40 . 120.29(19) yes P1 . C39 . C44 . 120.63(19) yes C40 . C39 . C44 . 119.1(2) yes C39 . C40 . C41 . 120.2(2) yes C39 . C40 . H241 . 119.6 no C41 . C40 . H241 . 120.3 no C40 . C41 . C42 . 120.3(3) yes C40 . C41 . H251 . 120.2 no C42 . C41 . H251 . 119.5 no C41 . C42 . C43 . 119.9(3) yes C41 . C42 . H261 . 120.9 no C43 . C42 . H261 . 119.1 no C42 . C43 . C44 . 120.2(3) yes C42 . C43 . H271 . 120.7 no C44 . C43 . H271 . 119.0 no C43 . C44 . C39 . 120.2(3) yes C43 . C44 . H281 . 120.0 no C39 . C44 . H281 . 119.7 no P2 . C9 . C10 . 122.58(19) yes P2 . C9 . C14 . 118.81(19) yes C10 . C9 . C14 . 118.6(2) yes C9 . C10 . C11 . 120.3(2) yes C9 . C10 . H301 . 120.3 no C11 . C10 . H301 . 119.4 no C10 . C11 . C12 . 120.6(3) yes C10 . C11 . H311 . 119.2 no C12 . C11 . H311 . 120.2 no C11 . C12 . C13 . 119.7(3) yes C11 . C12 . H321 . 120.6 no C13 . C12 . H321 . 119.7 no C12 . C13 . C14 . 120.0(3) yes C12 . C13 . H331 . 120.1 no C14 . C13 . H331 . 119.9 no C9 . C14 . C13 . 120.8(3) yes C9 . C14 . H341 . 119.4 no C13 . C14 . H341 . 119.8 no P2 . C15 . C16 . 117.6(2) yes P2 . C15 . C20 . 122.9(2) yes C16 . C15 . C20 . 119.4(2) yes C15 . C16 . C17 . 120.4(3) yes C15 . C16 . H361 . 119.6 no C17 . C16 . H361 . 119.9 no C16 . C17 . C18 . 119.8(3) yes C16 . C17 . H371 . 120.1 no C18 . C17 . H371 . 120.1 no C17 . C18 . C19 . 120.0(3) yes C17 . C18 . H381 . 118.9 no C19 . C18 . H381 . 121.1 no C18 . C19 . C20 . 120.3(3) yes C18 . C19 . H391 . 120.8 no C20 . C19 . H391 . 118.8 no C15 . C20 . C19 . 120.0(3) yes C15 . C20 . H401 . 119.7 no C19 . C20 . H401 . 120.3 no N1 . C5 . N4 . 126.2(2) yes N1 . C5 . C4 . 115.8(2) yes N4 . C5 . C4 . 118.0(2) yes C5 . N1 . Cu1 . 114.38(16) yes C5 . N1 . C8 . 116.4(2) yes Cu1 . N1 . C8 . 128.96(18) yes N1 . C8 . C7 . 121.4(3) yes N1 . C8 . H431 . 118.4 no C7 . C8 . H431 . 120.2 no C8 . C7 . C6 . 117.4(3) yes C8 . C7 . H441 . 121.3 no C6 . C7 . H441 . 121.3 no C7 . C6 . N4 . 122.4(3) yes C7 . C6 . H451 . 119.3 no N4 . C6 . H451 . 118.3 no C6 . N4 . C5 . 116.2(2) yes C5 . C4 . N2 . 116.1(2) yes C5 . C4 . N3 . 117.6(2) yes N2 . C4 . N3 . 126.3(2) yes C4 . N2 . Cu1 . 113.60(16) yes C4 . N2 . C1 . 115.9(2) yes Cu1 . N2 . C1 . 130.42(17) yes N2 . C1 . C2 . 122.4(2) yes N2 . C1 . H491 . 117.5 no C2 . C1 . H491 . 120.1 no C1 . C2 . C3 . 116.7(2) yes C1 . C2 . H501 . 121.2 no C3 . C2 . H501 . 122.1 no C2 . C3 . N3 . 122.7(2) yes C2 . C3 . H511 . 119.8 no N3 . C3 . H511 . 117.5 no C3 . N3 . C4 . 116.0(2) yes F54 . B53 . F55 . 110.5(3) yes F54 . B53 . F56 . 108.5(3) yes F55 . B53 . F56 . 109.7(3) yes F54 . B53 . F57 . 109.0(3) yes F55 . B53 . F57 . 110.0(3) yes F56 . B53 . F57 . 109.2(3) yes # Attachment '- nr8006_2.cif' data_NR8006 _database_code_depnum_ccdc_archive 'CCDC 771441' #TrackingRef '- nr8006_2.cif' _audit_creation_date 08-03-25 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'nr8006 in P-1' _chemical_name_systematic ? _chemical_melting_point ? _exptl_crystal_recrystallization_method ; ? ; _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_related_literature # Not in version 2.3.1 ############################################################### # Essential references (e.g. to the origin of the material studied, related # structural studies, and to information supporting the reported structure) # should be cited in this section, with appropriate very brief explanatory # text, for example `The synthesis of the complex is described by Jones # (2001). The anhydrous complex has essentially the same coordination # geometry (Smith, 2003).' In addition, all references included in the # supplementary materials, but not elsewhere in the published article, # should be given here. The simple text `For related literature, see:...' # may be used, but further details should be provided in the Comment # section, which forms part of the supplementary material. ############################################################### ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fig. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98\%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. 912_ALERT_3_B # Missing FCF Reflections Above STh/L= 0.600 814 910_ALERT_3_C # Missing FCF Reflections Below Th(Min) ........ 3 911_ALERT_3_C # Missing FCF Refl Between THmin & STh/L= 0.600 4 913_ALERT_3_C # Missing Very Strong Reflections in FCF ....... 1 The data collection strategy used aimed to achieve a complete data set to 2\q = 54 deg. Some higher angle data were collected in the process and these have been included in the refinement. Reflections with [sin(\q/\l)]^2^ less than 0.01 have been excluded from the refinement as they may be partially obscured by the beamstop. 061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.88 Sadabs corrects 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. 154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 100 Deg. Checked 220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.59 Ratio No action taken. The largest adps occur at the apex of Ph groups. 244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C52 244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for B47 These are the central atoms of the two solvent molecules. No action. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # # End of 'script/refcif-b.dat' #end of refcif _cell_length_a 11.3321(2) _cell_length_b 13.2821(3) _cell_length_c 14.2188(3) _cell_angle_alpha 108.665(1) _cell_angle_beta 105.605(1) _cell_angle_gamma 97.186(1) _cell_volume 1899.81(7) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z 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' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cu 0.3201 1.2651 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126 1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 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' 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' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 1 # Given Formula = C86 H74 B2 Cu2 F8 N4 O4 P4 # Dc = 1.44 Fooo = 850.00 Mu = 7.19 M = 826.08 # Found Formula = C86 H74 B2 Cu2 F8 N4 O4 P4 # Dc = 1.44 FOOO = 850.00 Mu = 7.19 M = 826.08 _chemical_formula_sum 'C86 H74 B2 Cu2 F8 N4 O4 P4' _chemical_formula_moiety 'C80 H62 Cu2 N4 O2 P4, 2(C3 H6 O), 2(B F4)' _chemical_compound_source 'Omar Moudam, MO66' _chemical_formula_weight 1652.15 _cell_measurement_reflns_used 9919 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _cell_measurement_temperature 150 _exptl_crystal_description rhomb _exptl_crystal_colour orange-yellow _exptl_crystal_size_min 0.15 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_max 0.25 _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 850 _exptl_absorpt_coefficient_mu 0.719 # Sheldrick geometric approximatio 0.86 0.90 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.74 _exptl_absorpt_correction_T_max 0.90 _diffrn_measurement_device 'Bruker SMART' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction 'SAINT (Siemens ,1995)' _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 150 _diffrn_reflns_number 27104 _reflns_number_total 10287 _diffrn_reflns_av_R_equivalents 0.037 # Number of reflections with Friedels Law is 10287 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 11139 _diffrn_reflns_theta_min 1.918 _diffrn_reflns_theta_max 30.056 _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 27.651 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 20 _reflns_limit_h_min -15 _reflns_limit_h_max 14 _reflns_limit_k_min -18 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.76 _refine_diff_density_max 0.73 # 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 10259 _refine_ls_number_restraints 0 _refine_ls_number_parameters 496 _oxford_refine_ls_R_factor_ref 0.0715 _refine_ls_wR_factor_ref 0.1255 _refine_ls_goodness_of_fit_ref 1.0479 _refine_ls_shift/su_max 0.000708 # The values computed from all data _oxford_reflns_number_all 10259 _refine_ls_R_factor_all 0.0715 _refine_ls_wR_factor_all 0.1255 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 8417 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_gt 0.1160 # 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 # 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^) + ( 0.03P)^2^ + 1.31P] ,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, G., 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. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. 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 _oxford_atom_site_special_shape _atom_site_attached_hydrogens Cu1 Cu 0.08908(3) 0.67957(3) 0.68851(2) 0.0175 1.0000 Uani . . . . . . . P1 P 0.15759(6) 0.71957(5) 0.86051(5) 0.0178 1.0000 Uani . . . . . . . P2 P 0.05166(6) 0.82101(5) 0.63520(5) 0.0185 1.0000 Uani . . . . . . . C5 C 0.2976(2) 0.6789(2) 0.9205(2) 0.0205 1.0000 Uani . . . . . . . C6 C 0.3855(3) 0.6610(2) 0.8682(2) 0.0285 1.0000 Uani . . . . . . . C7 C 0.4982(3) 0.6377(3) 0.9139(3) 0.0354 1.0000 Uani . . . . . . . C8 C 0.5226(3) 0.6313(3) 1.0127(3) 0.0377 1.0000 Uani . . . . . . . C9 C 0.4351(3) 0.6468(3) 1.0640(3) 0.0365 1.0000 Uani . . . . . . . C10 C 0.3231(3) 0.6711(2) 1.0190(2) 0.0275 1.0000 Uani . . . . . . . C11 C 0.0399(2) 0.6697(2) 0.91033(19) 0.0193 1.0000 Uani . . . . . . . C12 C -0.0322(3) 0.5631(2) 0.8536(2) 0.0245 1.0000 Uani . . . . . . . C13 C -0.1238(3) 0.5193(2) 0.8873(2) 0.0307 1.0000 Uani . . . . . . . C14 C -0.1443(3) 0.5829(3) 0.9773(3) 0.0330 1.0000 Uani . . . . . . . C15 C -0.0737(3) 0.6886(3) 1.0335(3) 0.0329 1.0000 Uani . . . . . . . C16 C 0.0182(3) 0.7320(2) 1.0008(2) 0.0274 1.0000 Uani . . . . . . . C17 C 0.2010(2) 0.8674(2) 0.92712(19) 0.0181 1.0000 Uani . . . . . . . C18 C 0.3231(3) 0.9258(2) 0.9941(2) 0.0216 1.0000 Uani . . . . . . . C19 C 0.3562(3) 1.0392(2) 1.0289(2) 0.0253 1.0000 Uani . . . . . . . C20 C 0.2689(3) 1.0956(2) 0.9976(2) 0.0266 1.0000 Uani . . . . . . . C21 C 0.1470(3) 1.0400(2) 0.9325(2) 0.0241 1.0000 Uani . . . . . . . C22 C 0.1143(2) 0.9271(2) 0.89819(18) 0.0180 1.0000 Uani . . . . . . . C35 C -0.0126(3) 0.7652(2) 0.49197(19) 0.0216 1.0000 Uani . . . . . . . C36 C 0.0618(3) 0.7711(3) 0.4294(2) 0.0304 1.0000 Uani . . . . . . . C37 C 0.0136(3) 0.7138(3) 0.3210(2) 0.0403 1.0000 Uani . . . . . . . C38 C -0.1072(3) 0.6495(3) 0.2758(2) 0.0384 1.0000 Uani . . . . . . . C39 C -0.1822(3) 0.6426(3) 0.3365(2) 0.0316 1.0000 Uani . . . . . . . C40 C -0.1352(3) 0.7007(2) 0.4447(2) 0.0267 1.0000 Uani . . . . . . . C29 C 0.1917(3) 0.9267(2) 0.66959(19) 0.0204 1.0000 Uani . . . . . . . C30 C 0.3083(3) 0.9038(2) 0.7037(2) 0.0270 1.0000 Uani . . . . . . . C31 C 0.4193(3) 0.9804(3) 0.7313(2) 0.0317 1.0000 Uani . . . . . . . C32 C 0.4140(3) 1.0823(3) 0.7283(3) 0.0362 1.0000 Uani . . . . . . . C33 C 0.2984(3) 1.1072(3) 0.6964(3) 0.0441 1.0000 Uani . . . . . . . C34 C 0.1877(3) 1.0302(3) 0.6668(3) 0.0340 1.0000 Uani . . . . . . . C28 C -0.0617(2) 0.8969(2) 0.6733(2) 0.0199 1.0000 Uani . . . . . . . C27 C -0.1329(3) 0.9444(2) 0.6103(2) 0.0252 1.0000 Uani . . . . . . . C26 C -0.2145(3) 1.0053(2) 0.6438(2) 0.0287 1.0000 Uani . . . . . . . C25 C -0.2298(3) 1.0171(3) 0.7403(2) 0.0304 1.0000 Uani . . . . . . . C24 C -0.1615(3) 0.9691(2) 0.8040(2) 0.0257 1.0000 Uani . . . . . . . C23 C -0.0768(2) 0.9119(2) 0.7704(2) 0.0201 1.0000 Uani . . . . . . . O1 O -0.00616(17) 0.86646(15) 0.83530(13) 0.0196 1.0000 Uani . . . . . . . C1 C 0.0624(2) 0.5080(2) 0.49340(19) 0.0171 1.0000 Uani . . . . . . . N1 N 0.1555(2) 0.58547(17) 0.57275(16) 0.0177 1.0000 Uani . . . . . . . C4 C 0.2694(3) 0.5955(2) 0.5607(2) 0.0242 1.0000 Uani . . . . . . . C3 C 0.2890(3) 0.5292(2) 0.4717(2) 0.0254 1.0000 Uani . . . . . . . C2 C 0.1869(3) 0.4536(2) 0.3935(2) 0.0220 1.0000 Uani . . . . . . . N2 N 0.0723(2) 0.44189(17) 0.40362(16) 0.0176 1.0000 Uani . . . . . . . B47 B 0.3932(3) 0.3054(3) 0.3035(3) 0.0311 1.0000 Uani . . . . . . . F48 F 0.4610(2) 0.41189(17) 0.3355(2) 0.0606 1.0000 Uani . . . . . . . F49 F 0.28621(18) 0.28649(18) 0.22133(15) 0.0429 1.0000 Uani . . . . . . . F50 F 0.46898(18) 0.23416(15) 0.27407(16) 0.0409 1.0000 Uani . . . . . . . F51 F 0.3612(3) 0.2935(2) 0.38738(18) 0.0638 1.0000 Uani . . . . . . . C52 C 0.5861(3) 0.2552(3) 0.6232(3) 0.0367 1.0000 Uani . . . . . . . C53 C 0.5085(4) 0.3369(3) 0.6437(3) 0.0509 1.0000 Uani . . . . . . . C54 C 0.5396(5) 0.1670(4) 0.5171(3) 0.0622 1.0000 Uani . . . . . . . O55 O 0.6804(3) 0.2589(3) 0.6891(2) 0.0665 1.0000 Uani . . . . . . . H291 H 0.3134 0.8359 0.7072 0.0310 1.0000 Uiso R . . . . . . H301 H 0.4972 0.9621 0.7513 0.0373 1.0000 Uiso R . . . . . . H311 H 0.4878 1.1332 0.7464 0.0423 1.0000 Uiso R . . . . . . H321 H 0.2944 1.1759 0.6951 0.0542 1.0000 Uiso R . . . . . . H331 H 0.1098 1.0483 0.6455 0.0442 1.0000 Uiso R . . . . . . H271 H -0.1868 0.6970 0.4852 0.0328 1.0000 Uiso R . . . . . . H261 H -0.2640 0.5988 0.3056 0.0337 1.0000 Uiso R . . . . . . H251 H -0.1384 0.6103 0.2037 0.0441 1.0000 Uiso R . . . . . . H241 H 0.0637 0.7189 0.2801 0.0491 1.0000 Uiso R . . . . . . H231 H 0.1448 0.8136 0.4603 0.0356 1.0000 Uiso R . . . . . . H351 H -0.1255 0.9360 0.5455 0.0317 1.0000 Uiso R . . . . . . H361 H -0.2607 1.0373 0.6005 0.0347 1.0000 Uiso R . . . . . . H371 H -0.2870 1.0567 0.7616 0.0367 1.0000 Uiso R . . . . . . H381 H -0.1732 0.9746 0.8671 0.0313 1.0000 Uiso R . . . . . . H111 H -0.0171 0.5221 0.7939 0.0282 1.0000 Uiso R . . . . . . H121 H -0.1708 0.4488 0.8490 0.0352 1.0000 Uiso R . . . . . . H131 H -0.2057 0.5543 1.0005 0.0429 1.0000 Uiso R . . . . . . H141 H -0.0885 0.7301 1.0934 0.0440 1.0000 Uiso R . . . . . . H151 H 0.0655 0.8040 1.0385 0.0344 1.0000 Uiso R . . . . . . H51 H 0.3703 0.6665 0.8028 0.0339 1.0000 Uiso R . . . . . . H61 H 0.5570 0.6264 0.8787 0.0416 1.0000 Uiso R . . . . . . H71 H 0.5987 0.6160 1.0444 0.0434 1.0000 Uiso R . . . . . . H81 H 0.4513 0.6403 1.1294 0.0442 1.0000 Uiso R . . . . . . H91 H 0.2657 0.6812 1.0538 0.0338 1.0000 Uiso R . . . . . . H171 H 0.3830 0.8880 1.0153 0.0250 1.0000 Uiso R . . . . . . H181 H 0.4383 1.0758 1.0733 0.0282 1.0000 Uiso R . . . . . . H191 H 0.2901 1.1716 1.0213 0.0299 1.0000 Uiso R . . . . . . H201 H 0.0876 1.0781 0.9124 0.0278 1.0000 Uiso R . . . . . . H431 H 0.3369 0.6483 0.6142 0.0269 1.0000 Uiso R . . . . . . H441 H 0.3686 0.5350 0.4654 0.0294 1.0000 Uiso R . . . . . . H451 H 0.1970 0.4087 0.3337 0.0264 1.0000 Uiso R . . . . . . H531 H 0.4745 0.3520 0.5822 0.0868 1.0000 Uiso R . . . . . . H533 H 0.4407 0.3071 0.6608 0.0870 1.0000 Uiso R . . . . . . H532 H 0.5579 0.4017 0.7000 0.0871 1.0000 Uiso R . . . . . . H542 H 0.5272 0.1974 0.4639 0.0852 1.0000 Uiso R . . . . . . H541 H 0.4607 0.1253 0.5098 0.0855 1.0000 Uiso R . . . . . . H543 H 0.5971 0.1215 0.5104 0.0849 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 Cu1 0.02123(16) 0.01548(15) 0.01315(14) 0.00238(11) 0.00521(11) 0.00344(11) P1 0.0211(3) 0.0162(3) 0.0146(3) 0.0044(2) 0.0056(2) 0.0034(2) P2 0.0215(3) 0.0189(3) 0.0160(3) 0.0065(2) 0.0069(2) 0.0054(2) C5 0.0214(13) 0.0176(11) 0.0188(11) 0.0052(9) 0.0030(10) 0.0042(10) C6 0.0295(15) 0.0283(15) 0.0275(14) 0.0083(12) 0.0103(12) 0.0089(12) C7 0.0274(16) 0.0336(17) 0.0446(18) 0.0115(14) 0.0128(14) 0.0111(13) C8 0.0282(16) 0.0328(17) 0.0469(19) 0.0164(15) 0.0010(14) 0.0095(13) C9 0.0405(19) 0.0367(17) 0.0337(16) 0.0203(14) 0.0037(14) 0.0127(14) C10 0.0315(15) 0.0281(14) 0.0248(13) 0.0126(11) 0.0083(12) 0.0084(12) C11 0.0216(12) 0.0199(12) 0.0175(11) 0.0074(9) 0.0073(10) 0.0054(10) C12 0.0292(14) 0.0216(13) 0.0201(12) 0.0062(10) 0.0062(11) 0.0047(11) C13 0.0324(16) 0.0255(14) 0.0295(14) 0.0113(12) 0.0051(12) -0.0017(12) C14 0.0321(16) 0.0356(17) 0.0408(17) 0.0231(14) 0.0164(14) 0.0076(13) C15 0.0442(19) 0.0300(16) 0.0349(16) 0.0132(13) 0.0261(14) 0.0117(14) C16 0.0364(16) 0.0212(13) 0.0268(14) 0.0079(11) 0.0155(12) 0.0055(12) C17 0.0227(12) 0.0154(11) 0.0156(10) 0.0031(9) 0.0089(9) 0.0042(9) C18 0.0216(13) 0.0226(13) 0.0190(11) 0.0062(10) 0.0062(10) 0.0044(10) C19 0.0238(14) 0.0222(13) 0.0240(13) 0.0056(10) 0.0052(11) -0.0009(11) C20 0.0324(15) 0.0169(12) 0.0254(13) 0.0031(10) 0.0092(12) 0.0008(11) C21 0.0296(14) 0.0184(12) 0.0224(12) 0.0052(10) 0.0080(11) 0.0062(11) C22 0.0205(12) 0.0175(11) 0.0138(10) 0.0028(9) 0.0067(9) 0.0026(9) C35 0.0281(14) 0.0229(13) 0.0152(11) 0.0078(10) 0.0074(10) 0.0084(11) C36 0.0316(16) 0.0379(17) 0.0211(13) 0.0100(12) 0.0088(12) 0.0085(13) C37 0.047(2) 0.053(2) 0.0225(14) 0.0100(14) 0.0172(14) 0.0148(17) C38 0.048(2) 0.0442(19) 0.0180(13) 0.0046(13) 0.0068(13) 0.0191(16) C39 0.0333(16) 0.0301(15) 0.0224(13) 0.0054(11) 0.0003(12) 0.0079(13) C40 0.0308(15) 0.0291(14) 0.0225(13) 0.0120(11) 0.0077(11) 0.0110(12) C29 0.0234(13) 0.0216(12) 0.0171(11) 0.0068(9) 0.0088(10) 0.0045(10) C30 0.0252(14) 0.0224(13) 0.0299(14) 0.0087(11) 0.0047(11) 0.0056(11) C31 0.0248(15) 0.0297(15) 0.0373(16) 0.0119(13) 0.0071(13) 0.0032(12) C32 0.0318(17) 0.0314(16) 0.0409(18) 0.0139(14) 0.0083(14) -0.0020(13) C33 0.041(2) 0.0281(17) 0.067(2) 0.0270(17) 0.0135(18) 0.0046(14) C34 0.0301(16) 0.0302(16) 0.0497(19) 0.0235(15) 0.0141(14) 0.0094(13) C28 0.0212(12) 0.0198(12) 0.0194(11) 0.0076(9) 0.0072(10) 0.0047(10) C27 0.0273(14) 0.0285(14) 0.0231(12) 0.0119(11) 0.0089(11) 0.0100(11) C26 0.0263(14) 0.0303(15) 0.0320(15) 0.0158(12) 0.0061(12) 0.0112(12) C25 0.0234(14) 0.0329(16) 0.0364(16) 0.0113(13) 0.0116(12) 0.0115(12) C24 0.0257(14) 0.0257(14) 0.0268(13) 0.0071(11) 0.0134(11) 0.0055(11) C23 0.0189(12) 0.0186(12) 0.0210(12) 0.0074(10) 0.0047(10) 0.0024(9) O1 0.0214(9) 0.0195(9) 0.0161(8) 0.0066(7) 0.0038(7) 0.0036(7) C1 0.0187(12) 0.0164(11) 0.0150(10) 0.0031(9) 0.0065(9) 0.0051(9) N1 0.0165(10) 0.0158(10) 0.0181(10) 0.0040(8) 0.0047(8) 0.0026(8) C4 0.0201(13) 0.0233(13) 0.0233(13) 0.0039(10) 0.0056(10) 0.0010(10) C3 0.0174(13) 0.0302(15) 0.0280(14) 0.0071(11) 0.0112(11) 0.0049(11) C2 0.0237(13) 0.0257(13) 0.0168(11) 0.0043(10) 0.0104(10) 0.0081(11) N2 0.0204(11) 0.0164(10) 0.0149(9) 0.0025(8) 0.0081(8) 0.0044(8) B47 0.0285(17) 0.0279(17) 0.0291(16) 0.0023(13) 0.0063(14) 0.0093(14) F48 0.0416(13) 0.0251(11) 0.0884(18) -0.0001(11) 0.0075(12) 0.0037(9) F49 0.0342(11) 0.0521(13) 0.0286(9) 0.0033(9) 0.0006(8) 0.0154(9) F50 0.0288(10) 0.0299(10) 0.0513(12) 0.0004(9) 0.0091(9) 0.0108(8) F51 0.0903(19) 0.0835(19) 0.0431(13) 0.0354(13) 0.0318(13) 0.0543(16) C52 0.0321(17) 0.0361(18) 0.0438(19) 0.0208(15) 0.0099(14) 0.0037(14) C53 0.066(3) 0.055(2) 0.052(2) 0.032(2) 0.032(2) 0.025(2) C54 0.069(3) 0.052(3) 0.049(2) 0.012(2) -0.003(2) 0.023(2) O55 0.0522(18) 0.062(2) 0.0604(19) 0.0125(16) -0.0090(15) 0.0130(15) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.4614(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 Cu1 . N2 2_566 2.070(2) yes Cu1 . P1 . 2.2158(7) yes Cu1 . P2 . 2.2851(7) yes Cu1 . N1 . 2.103(2) yes P1 . C5 . 1.821(3) yes P1 . C11 . 1.819(3) yes P1 . C17 . 1.820(3) yes P2 . C35 . 1.824(3) yes P2 . C29 . 1.821(3) yes P2 . C28 . 1.819(3) yes C5 . C6 . 1.395(4) yes C5 . C10 . 1.393(4) yes C6 . C7 . 1.390(4) yes C6 . H51 . 0.927 no C7 . C8 . 1.389(5) yes C7 . H61 . 0.935 no C8 . C9 . 1.379(5) yes C8 . H71 . 0.939 no C9 . C10 . 1.387(4) yes C9 . H81 . 0.932 no C10 . H91 . 0.916 no C11 . C12 . 1.395(4) yes C11 . C16 . 1.393(4) yes C12 . C13 . 1.392(4) yes C12 . H111 . 0.923 no C13 . C14 . 1.386(4) yes C13 . H121 . 0.923 no C14 . C15 . 1.381(4) yes C14 . H131 . 0.936 no C15 . C16 . 1.384(4) yes C15 . H141 . 0.925 no C16 . H151 . 0.937 no C17 . C18 . 1.405(4) yes C17 . C22 . 1.396(3) yes C18 . C19 . 1.391(4) yes C18 . H171 . 0.936 no C19 . C20 . 1.379(4) yes C19 . H181 . 0.935 no C20 . C21 . 1.389(4) yes C20 . H191 . 0.931 no C21 . C22 . 1.385(4) yes C21 . H201 . 0.931 no C22 . O1 . 1.385(3) yes C35 . C36 . 1.393(4) yes C35 . C40 . 1.395(4) yes C36 . C37 . 1.394(4) yes C36 . H231 . 0.939 no C37 . C38 . 1.379(5) yes C37 . H241 . 0.927 no C38 . C39 . 1.380(5) yes C38 . H251 . 0.929 no C39 . C40 . 1.393(4) yes C39 . H261 . 0.935 no C40 . H271 . 0.933 no C29 . C30 . 1.387(4) yes C29 . C34 . 1.393(4) yes C30 . C31 . 1.390(4) yes C30 . H291 . 0.927 no C31 . C32 . 1.375(4) yes C31 . H301 . 0.939 no C32 . C33 . 1.384(5) yes C32 . H311 . 0.924 no C33 . C34 . 1.385(4) yes C33 . H321 . 0.925 no C34 . H331 . 0.941 no C28 . C27 . 1.398(3) yes C28 . C23 . 1.391(3) yes C27 . C26 . 1.382(4) yes C27 . H351 . 0.920 no C26 . C25 . 1.391(4) yes C26 . H361 . 0.940 no C25 . C24 . 1.393(4) yes C25 . H371 . 0.936 no C24 . C23 . 1.387(4) yes C24 . H381 . 0.924 no C23 . O1 . 1.392(3) yes C1 . C1 2_566 1.474(5) yes C1 . N1 . 1.338(3) yes C1 . N2 . 1.341(3) yes N1 . C4 . 1.343(3) yes C4 . C3 . 1.382(4) yes C4 . H431 . 0.931 no C3 . C2 . 1.373(4) yes C3 . H441 . 0.927 no C2 . N2 . 1.339(3) yes C2 . H451 . 0.915 no B47 . F48 . 1.389(4) yes B47 . F49 . 1.368(4) yes B47 . F50 . 1.397(4) yes B47 . F51 . 1.384(4) yes C52 . C53 . 1.487(5) yes C52 . C54 . 1.487(5) yes C52 . O55 . 1.201(4) yes C53 . H531 . 0.951 no C53 . H533 . 0.945 no C53 . H532 . 0.945 no C54 . H542 . 0.953 no C54 . H541 . 0.952 no C54 . H543 . 0.946 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 N2 2_566 Cu1 . P1 . 119.24(6) yes N2 2_566 Cu1 . P2 . 102.75(6) yes P1 . Cu1 . P2 . 116.30(3) yes N2 2_566 Cu1 . N1 . 80.18(8) yes P1 . Cu1 . N1 . 128.91(6) yes P2 . Cu1 . N1 . 102.14(6) yes Cu1 . P1 . C5 . 120.24(9) yes Cu1 . P1 . C11 . 113.79(9) yes C5 . P1 . C11 . 104.08(12) yes Cu1 . P1 . C17 . 108.78(8) yes C5 . P1 . C17 . 102.52(12) yes C11 . P1 . C17 . 106.08(12) yes Cu1 . P2 . C35 . 107.54(9) yes Cu1 . P2 . C29 . 114.44(9) yes C35 . P2 . C29 . 106.10(12) yes Cu1 . P2 . C28 . 120.35(9) yes C35 . P2 . C28 . 103.14(12) yes C29 . P2 . C28 . 103.93(12) yes P1 . C5 . C6 . 118.6(2) yes P1 . C5 . C10 . 122.3(2) yes C6 . C5 . C10 . 119.0(3) yes C5 . C6 . C7 . 120.9(3) yes C5 . C6 . H51 . 120.2 no C7 . C6 . H51 . 118.9 no C6 . C7 . C8 . 119.2(3) yes C6 . C7 . H61 . 120.5 no C8 . C7 . H61 . 120.3 no C7 . C8 . C9 . 120.2(3) yes C7 . C8 . H71 . 119.8 no C9 . C8 . H71 . 119.9 no C8 . C9 . C10 . 120.6(3) yes C8 . C9 . H81 . 119.6 no C10 . C9 . H81 . 119.7 no C5 . C10 . C9 . 119.9(3) yes C5 . C10 . H91 . 120.2 no C9 . C10 . H91 . 119.9 no P1 . C11 . C12 . 117.4(2) yes P1 . C11 . C16 . 123.6(2) yes C12 . C11 . C16 . 119.0(2) yes C11 . C12 . C13 . 120.6(3) yes C11 . C12 . H111 . 118.6 no C13 . C12 . H111 . 120.8 no C12 . C13 . C14 . 119.5(3) yes C12 . C13 . H121 . 119.7 no C14 . C13 . H121 . 120.7 no C13 . C14 . C15 . 120.2(3) yes C13 . C14 . H131 . 120.2 no C15 . C14 . H131 . 119.6 no C14 . C15 . C16 . 120.4(3) yes C14 . C15 . H141 . 119.3 no C16 . C15 . H141 . 120.4 no C11 . C16 . C15 . 120.3(3) yes C11 . C16 . H151 . 119.2 no C15 . C16 . H151 . 120.4 no P1 . C17 . C18 . 123.3(2) yes P1 . C17 . C22 . 118.15(19) yes C18 . C17 . C22 . 117.8(2) yes C17 . C18 . C19 . 120.7(3) yes C17 . C18 . H171 . 119.7 no C19 . C18 . H171 . 119.6 no C18 . C19 . C20 . 120.1(3) yes C18 . C19 . H181 . 118.8 no C20 . C19 . H181 . 121.1 no C19 . C20 . C21 . 120.3(3) yes C19 . C20 . H191 . 120.6 no C21 . C20 . H191 . 119.1 no C20 . C21 . C22 . 119.4(3) yes C20 . C21 . H201 . 120.4 no C22 . C21 . H201 . 120.2 no C17 . C22 . C21 . 121.6(2) yes C17 . C22 . O1 . 115.8(2) yes C21 . C22 . O1 . 122.6(2) yes P2 . C35 . C36 . 122.2(2) yes P2 . C35 . C40 . 118.1(2) yes C36 . C35 . C40 . 119.0(3) yes C35 . C36 . C37 . 120.2(3) yes C35 . C36 . H231 . 119.9 no C37 . C36 . H231 . 119.9 no C36 . C37 . C38 . 120.0(3) yes C36 . C37 . H241 . 119.4 no C38 . C37 . H241 . 120.5 no C37 . C38 . C39 . 120.6(3) yes C37 . C38 . H251 . 119.7 no C39 . C38 . H251 . 119.7 no C38 . C39 . C40 . 119.7(3) yes C38 . C39 . H261 . 120.3 no C40 . C39 . H261 . 119.9 no C35 . C40 . C39 . 120.5(3) yes C35 . C40 . H271 . 120.1 no C39 . C40 . H271 . 119.4 no P2 . C29 . C30 . 117.9(2) yes P2 . C29 . C34 . 123.5(2) yes C30 . C29 . C34 . 118.6(3) yes C29 . C30 . C31 . 121.2(3) yes C29 . C30 . H291 . 120.2 no C31 . C30 . H291 . 118.6 no C30 . C31 . C32 . 119.6(3) yes C30 . C31 . H301 . 119.8 no C32 . C31 . H301 . 120.6 no C31 . C32 . C33 . 119.9(3) yes C31 . C32 . H311 . 119.7 no C33 . C32 . H311 . 120.4 no C32 . C33 . C34 . 120.6(3) yes C32 . C33 . H321 . 120.2 no C34 . C33 . H321 . 119.2 no C29 . C34 . C33 . 120.1(3) yes C29 . C34 . H331 . 120.2 no C33 . C34 . H331 . 119.7 no P2 . C28 . C27 . 122.8(2) yes P2 . C28 . C23 . 119.49(19) yes C27 . C28 . C23 . 117.7(2) yes C28 . C27 . C26 . 121.1(3) yes C28 . C27 . H351 . 120.0 no C26 . C27 . H351 . 118.8 no C27 . C26 . C25 . 120.0(3) yes C27 . C26 . H361 . 119.7 no C25 . C26 . H361 . 120.2 no C26 . C25 . C24 . 120.0(3) yes C26 . C25 . H371 . 119.5 no C24 . C25 . H371 . 120.4 no C25 . C24 . C23 . 118.9(3) yes C25 . C24 . H381 . 120.5 no C23 . C24 . H381 . 120.6 no C28 . C23 . C24 . 122.2(2) yes C28 . C23 . O1 . 118.9(2) yes C24 . C23 . O1 . 118.9(2) yes C23 . O1 . C22 . 116.42(19) yes C1 2_566 C1 . N1 . 117.1(3) yes C1 2_566 C1 . N2 . 116.8(3) yes N1 . C1 . N2 . 126.1(2) yes C1 . N1 . Cu1 . 111.86(16) yes C1 . N1 . C4 . 116.0(2) yes Cu1 . N1 . C4 . 131.86(18) yes N1 . C4 . C3 . 121.8(2) yes N1 . C4 . H431 . 118.7 no C3 . C4 . H431 . 119.4 no C4 . C3 . C2 . 117.8(2) yes C4 . C3 . H441 . 121.1 no C2 . C3 . H441 . 121.1 no C3 . C2 . N2 . 121.5(2) yes C3 . C2 . H451 . 119.7 no N2 . C2 . H451 . 118.7 no C1 . N2 . C2 . 116.7(2) yes C1 . N2 . Cu1 2_566 113.09(16) yes C2 . N2 . Cu1 2_566 129.47(17) yes F48 . B47 . F49 . 109.2(3) yes F48 . B47 . F50 . 108.7(3) yes F49 . B47 . F50 . 111.0(3) yes F48 . B47 . F51 . 108.2(3) yes F49 . B47 . F51 . 109.7(3) yes F50 . B47 . F51 . 110.1(3) yes C53 . C52 . C54 . 116.5(3) yes C53 . C52 . O55 . 122.0(4) yes C54 . C52 . O55 . 121.5(4) yes C52 . C53 . H531 . 110.0 no C52 . C53 . H533 . 108.6 no H531 . C53 . H533 . 108.0 no C52 . C53 . H532 . 110.0 no H531 . C53 . H532 . 110.3 no H533 . C53 . H532 . 109.9 no C52 . C54 . H542 . 110.4 no C52 . C54 . H541 . 107.5 no H542 . C54 . H541 . 108.7 no C52 . C54 . H543 . 110.3 no H542 . C54 . H543 . 110.3 no H541 . C54 . H543 . 109.6 no # Attachment '- nr9001.cif' data_nr9001 _database_code_depnum_ccdc_archive 'CCDC 771442' #TrackingRef '- nr9001.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_compound_source 'Tracy Hewat' _exptl_crystal_recrystallization_method 'Slow evaporation of DCM/Et2O solution' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2[Cu (C12 H12 N2)2], 2BF4, CH2Cl2' _chemical_formula_sum 'C24.50 H25 B Cl2 Cu F4 N4' _chemical_formula_weight 596.73 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' F F 0.0171 0.0103 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8528(3) _cell_length_b 14.4072(4) _cell_length_c 17.6085(5) _cell_angle_alpha 83.9868(16) _cell_angle_beta 74.9744(14) _cell_angle_gamma 73.3850(14) _cell_volume 2546.69(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9477 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 24.87 _exptl_crystal_description block _exptl_crystal_colour cyan _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 1.119 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6209 _exptl_absorpt_correction_T_max 0.7154 _exptl_absorpt_process_details 'SADABS 2008/1' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'Phi and Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 36169 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0383 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.08 _reflns_number_total 8998 _reflns_number_gt 7635 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution Sir92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Shelxp _computing_publication_material 'Platon, encifer' _refine_special_details ; #============================================================ >>> The Following Model and Quality ALERTS were generated <<< #============================================================ Format: alert-number_ALERT_alert-type_alert-level text 910_ALERT_3_G Missing # of FCF Reflections Below Th(Min) ..... 2 911_ALERT_3_G Missing # FCF Refl Between THmin & STh/L= 0.596 44 The data collection strategy was refined using Cosmo and aimed to get 100perc completeness to 53% in 2TH. Completeness is better than 99perc to 50 deg in 2TH #============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 1.000 5339 5337 2 23.01 0.550 1.000 7096 7094 2 25.08 0.596 0.995 9044 8998 46 #----------------------------------------------------------- ACTA Min. Res. --- #================================================================ >>> The Following Improvement and Query ALERTS were generated <<< #================================================================ 180_ALERT_4_B Check Cell Rounding: # of Values Ending with 0 = 1 Surprising error given the following is from the very same checkcif report # UCL 10.8528(3) 14.4072(4) 17.6085(5) 83.987(2) 74.974(1) 73.385(1) # WaveLength 0.71073 Volume Reported 2546.68(12) Calculated 2546.68(12) 041_ALERT_1_C Calc. and Reported SumFormula Strings Differ ? 042_ALERT_1_C Calc. and Reported MoietyFormula Strings Differ ? 045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.50 Ratio Z is incorrectly calculated by Platon. Visual inspection confirms z=4 The given formula is intended to identify separate ligands 244_ALERT_4_G Low 'Solvent' Ueq as Compared to Neighbors for C1G 244_ALERT_4_G Low 'Solvent' Ueq as Compared to Neighbors for B1E 244_ALERT_4_G Low 'Solvent' Ueq as Compared to Neighbors for B1F These are the central atoms in DCM and BF4 solvent molecules 720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 2 No action taken ; _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^)+(0.0510P)^2^+1.3566P] 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_number_reflns 8998 _refine_ls_number_parameters 666 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0450 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0981 _refine_ls_wR_factor_gt 0.0933 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Cu1 Cu 0.31114(3) 0.57883(2) 0.886564(17) 0.02168(9) Uani 1 1 d . . . N1A N 0.2633(2) 0.58198(14) 0.77483(12) 0.0201(4) Uani 1 1 d . . . C1A C 0.1530(2) 0.63096(17) 0.75193(15) 0.0232(5) Uani 1 1 d . . . H1A H 0.0797 0.6660 0.7900 0.028 Uiso 1 1 calc R . . C2A C 0.1411(2) 0.63281(18) 0.67524(15) 0.0245(6) Uani 1 1 d . . . H2A H 0.0608 0.6679 0.6617 0.029 Uiso 1 1 calc R . . C3A C 0.2468(3) 0.58333(18) 0.61875(15) 0.0242(6) Uani 1 1 d . . . C4A C 0.2424(3) 0.5840(2) 0.53449(16) 0.0353(7) Uani 1 1 d . . . H4C H 0.3123 0.6110 0.5012 0.053 Uiso 1 1 calc R . . H4B H 0.1559 0.6238 0.5278 0.053 Uiso 1 1 calc R . . H4A H 0.2563 0.5176 0.5193 0.053 Uiso 1 1 calc R . . C5A C 0.3613(2) 0.53227(18) 0.64251(14) 0.0234(5) Uani 1 1 d . . . H5A H 0.4360 0.4970 0.6053 0.028 Uiso 1 1 calc R . . C6A C 0.3663(2) 0.53285(16) 0.71978(14) 0.0193(5) Uani 1 1 d . . . C7A C 0.4854(2) 0.48075(17) 0.74876(14) 0.0201(5) Uani 1 1 d . . . N2A N 0.4799(2) 0.49434(14) 0.82423(12) 0.0216(4) Uani 1 1 d . . . C12A C 0.5854(3) 0.44821(18) 0.85336(15) 0.0253(6) Uani 1 1 d . . . H12A H 0.5813 0.4569 0.9068 0.030 Uiso 1 1 calc R . . C11A C 0.6988(3) 0.38903(18) 0.80895(16) 0.0265(6) Uani 1 1 d . . . H11A H 0.7714 0.3580 0.8316 0.032 Uiso 1 1 calc R . . C9A C 0.7065(2) 0.37491(18) 0.73092(15) 0.0245(6) Uani 1 1 d . . . C10A C 0.8283(3) 0.3142(2) 0.67801(17) 0.0334(6) Uani 1 1 d . . . H10C H 0.8024 0.2754 0.6455 0.050 Uiso 1 1 calc R . . H10B H 0.8843 0.2711 0.7100 0.050 Uiso 1 1 calc R . . H10A H 0.8776 0.3564 0.6440 0.050 Uiso 1 1 calc R . . C8A C 0.5959(2) 0.42139(18) 0.70197(15) 0.0243(6) Uani 1 1 d . . . H8A H 0.5965 0.4121 0.6492 0.029 Uiso 1 1 calc R . . N1B N 0.3751(2) 0.70382(14) 0.87549(12) 0.0226(5) Uani 1 1 d . . . C1B C 0.4998(3) 0.71212(19) 0.85111(15) 0.0274(6) Uani 1 1 d . . . H1B H 0.5709 0.6548 0.8425 0.033 Uiso 1 1 calc R . . C2B C 0.5283(3) 0.80015(19) 0.83815(15) 0.0282(6) Uani 1 1 d . . . H2B H 0.6176 0.8030 0.8199 0.034 Uiso 1 1 calc R . . C3B C 0.4265(3) 0.88485(18) 0.85185(14) 0.0245(6) Uani 1 1 d . . . C4B C 0.4538(3) 0.98258(19) 0.84031(17) 0.0315(6) Uani 1 1 d . . . H4F H 0.4933 0.9919 0.8821 0.047 Uiso 1 1 calc R . . H4E H 0.3706 1.0332 0.8423 0.047 Uiso 1 1 calc R . . H4D H 0.5152 0.9863 0.7891 0.047 Uiso 1 1 calc R . . C5B C 0.2971(3) 0.87629(18) 0.87704(14) 0.0217(5) Uani 1 1 d . . . H5B H 0.2245 0.9326 0.8866 0.026 Uiso 1 1 calc R . . C6B C 0.2752(2) 0.78510(17) 0.88808(13) 0.0200(5) Uani 1 1 d . . . C7B C 0.1409(2) 0.76952(17) 0.91439(13) 0.0199(5) Uani 1 1 d . . . N2B N 0.1413(2) 0.67512(14) 0.92927(11) 0.0218(5) Uani 1 1 d . . . C12B C 0.0246(3) 0.65443(19) 0.95540(15) 0.0260(6) Uani 1 1 d . . . H12B H 0.0241 0.5889 0.9685 0.031 Uiso 1 1 calc R . . C11B C -0.0938(3) 0.72359(19) 0.96408(15) 0.0279(6) Uani 1 1 d . . . H11B H -0.1743 0.7055 0.9818 0.034 Uiso 1 1 calc R . . C9B C -0.0965(3) 0.8201(2) 0.94712(15) 0.0277(6) Uani 1 1 d . . . C10B C -0.2233(3) 0.8985(2) 0.95398(19) 0.0402(7) Uani 1 1 d . . . H10F H -0.2385 0.9181 0.9014 0.060 Uiso 1 1 calc R . . H10E H -0.2177 0.9544 0.9789 0.060 Uiso 1 1 calc R . . H10D H -0.2968 0.8743 0.9861 0.060 Uiso 1 1 calc R . . C8B C 0.0252(3) 0.84215(18) 0.92296(14) 0.0241(6) Uani 1 1 d . . . H8B H 0.0279 0.9077 0.9124 0.029 Uiso 1 1 calc R . . Cu2 Cu 0.47756(3) 0.19970(2) 0.616213(16) 0.01927(9) Uani 1 1 d . . . N1C N 0.39979(19) 0.07937(14) 0.64039(11) 0.0189(4) Uani 1 1 d . . . C1C C 0.2816(2) 0.07482(18) 0.68584(14) 0.0224(5) Uani 1 1 d . . . H1C H 0.2216 0.1324 0.7089 0.027 Uiso 1 1 calc R . . C2C C 0.2434(3) -0.01007(18) 0.70051(14) 0.0247(6) Uani 1 1 d . . . H2C H 0.1583 -0.0102 0.7326 0.030 Uiso 1 1 calc R . . C3C C 0.3299(3) -0.09531(18) 0.66817(14) 0.0238(6) Uani 1 1 d . . . C4C C 0.2924(3) -0.18896(19) 0.68191(16) 0.0332(6) Uani 1 1 d . . . H4I H 0.3339 -0.2286 0.7220 0.050 Uiso 1 1 calc R . . H4H H 0.3227 -0.2239 0.6327 0.050 Uiso 1 1 calc R . . H4G H 0.1958 -0.1757 0.7000 0.050 Uiso 1 1 calc R . . C5C C 0.4531(3) -0.09052(17) 0.62184(14) 0.0227(5) Uani 1 1 d . . . H5C H 0.5153 -0.1474 0.5988 0.027 Uiso 1 1 calc R . . C6C C 0.4853(2) -0.00259(17) 0.60918(13) 0.0197(5) Uani 1 1 d . . . C7C C 0.6143(2) 0.00896(17) 0.56075(13) 0.0197(5) Uani 1 1 d . . . N2C N 0.62926(19) 0.09905(14) 0.55839(11) 0.0195(4) Uani 1 1 d . . . C12C C 0.7431(2) 0.11569(19) 0.51525(14) 0.0234(5) Uani 1 1 d . . . H12C H 0.7534 0.1793 0.5131 0.028 Uiso 1 1 calc R . . C11C C 0.8450(2) 0.04478(19) 0.47419(15) 0.0259(6) Uani 1 1 d . . . H11C H 0.9243 0.0593 0.4448 0.031 Uiso 1 1 calc R . . C9C C 0.8312(2) -0.04858(19) 0.47584(14) 0.0247(6) Uani 1 1 d . . . C10C C 0.9402(3) -0.1284(2) 0.43280(16) 0.0326(6) Uani 1 1 d . . . H10I H 0.9925 -0.1657 0.4690 0.049 Uiso 1 1 calc R . . H10H H 0.9973 -0.1006 0.3894 0.049 Uiso 1 1 calc R . . H10G H 0.9021 -0.1711 0.4117 0.049 Uiso 1 1 calc R . . C8C C 0.7128(2) -0.06460(18) 0.51992(14) 0.0227(5) Uani 1 1 d . . . H8C H 0.6994 -0.1272 0.5220 0.027 Uiso 1 1 calc R . . N1D N 0.54451(19) 0.19107(14) 0.71862(11) 0.0194(4) Uani 1 1 d . . . C1D C 0.6602(2) 0.13874(17) 0.73298(15) 0.0226(5) Uani 1 1 d . . . H1D H 0.7249 0.1026 0.6915 0.027 Uiso 1 1 calc R . . C2D C 0.6902(3) 0.13460(18) 0.80465(15) 0.0247(6) Uani 1 1 d . . . H2D H 0.7741 0.0970 0.8120 0.030 Uiso 1 1 calc R . . C3D C 0.5964(3) 0.18611(19) 0.86611(15) 0.0259(6) Uani 1 1 d . . . C4D C 0.6231(3) 0.1849(2) 0.94563(16) 0.0393(7) Uani 1 1 d . . . H4L H 0.5733 0.2466 0.9707 0.059 Uiso 1 1 calc R . . H4K H 0.7181 0.1758 0.9399 0.059 Uiso 1 1 calc R . . H4J H 0.5954 0.1317 0.9783 0.059 Uiso 1 1 calc R . . C5D C 0.4752(2) 0.23916(18) 0.85201(14) 0.0229(5) Uani 1 1 d . . . H5D H 0.4082 0.2745 0.8931 0.027 Uiso 1 1 calc R . . C6D C 0.4519(2) 0.24059(17) 0.77818(14) 0.0194(5) Uani 1 1 d . . . C7D C 0.3265(2) 0.29576(17) 0.75786(14) 0.0193(5) Uani 1 1 d . . . N2D N 0.32304(19) 0.28904(14) 0.68263(11) 0.0197(4) Uani 1 1 d . . . C12D C 0.2138(2) 0.33815(18) 0.65913(15) 0.0243(6) Uani 1 1 d . . . H12D H 0.2118 0.3342 0.6060 0.029 Uiso 1 1 calc R . . C11D C 0.1045(2) 0.39405(18) 0.70890(15) 0.0246(6) Uani 1 1 d . . . H11D H 0.0290 0.4281 0.6899 0.029 Uiso 1 1 calc R . . C9D C 0.1045(2) 0.40066(17) 0.78657(15) 0.0228(5) Uani 1 1 d . . . C10D C -0.0131(3) 0.4587(2) 0.84361(16) 0.0310(6) Uani 1 1 d . . . H10L H -0.0705 0.5060 0.8147 0.046 Uiso 1 1 calc R . . H10K H 0.0168 0.4929 0.8777 0.046 Uiso 1 1 calc R . . H10J H -0.0626 0.4154 0.8758 0.046 Uiso 1 1 calc R . . C8D C 0.2195(2) 0.35073(17) 0.81044(15) 0.0226(5) Uani 1 1 d . . . H8D H 0.2242 0.3546 0.8631 0.027 Uiso 1 1 calc R . . B1E B 0.8692(3) 0.8738(2) 0.69417(19) 0.0313(7) Uani 1 1 d . . . F1E F 0.8961(2) 0.81427(16) 0.75701(11) 0.0752(7) Uani 1 1 d . . . F2E F 0.9109(2) 0.95567(15) 0.69074(15) 0.0776(7) Uani 1 1 d . . . F3E F 0.73484(17) 0.89993(15) 0.70036(11) 0.0545(5) Uani 1 1 d . . . F4E F 0.93443(17) 0.82353(12) 0.62482(9) 0.0406(4) Uani 1 1 d . . . B1F B 0.9908(3) 0.8443(2) 0.13573(18) 0.0288(7) Uani 1 1 d . . . F1F F 0.86024(16) 0.85754(14) 0.13245(11) 0.0511(5) Uani 1 1 d . . . F2F F 0.99788(17) 0.83898(15) 0.21310(10) 0.0558(5) Uani 1 1 d . . . F3F F 1.0332(2) 0.92120(13) 0.09793(14) 0.0692(6) Uani 1 1 d . . . F4F F 1.07004(17) 0.75995(11) 0.09972(10) 0.0406(4) Uani 1 1 d . . . C1G C 0.2332(3) 0.3272(2) 0.3878(2) 0.0464(8) Uani 1 1 d . . . H1G1 H 0.3211 0.3176 0.3987 0.056 Uiso 1 1 calc R . . H1G2 H 0.2228 0.2628 0.3809 0.056 Uiso 1 1 calc R . . Cl1G Cl 0.22444(10) 0.39850(7) 0.30131(6) 0.0647(3) Uani 1 1 d . . . Cl2G Cl 0.10868(10) 0.38349(9) 0.46743(6) 0.0722(3) Uani 1 1 d . . . Cl2 Cl 0.47586(7) 0.30437(5) 0.50910(4) 0.03151(16) Uani 1 1 d . . . Cl1 Cl 0.28449(7) 0.46181(4) 0.98202(4) 0.03132(16) 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 Cu1 0.02301(17) 0.01808(16) 0.02116(17) -0.00229(12) -0.00044(13) -0.00499(13) N1A 0.0203(11) 0.0164(10) 0.0230(11) -0.0006(8) -0.0024(9) -0.0064(9) C1A 0.0205(13) 0.0188(12) 0.0290(14) -0.0019(10) -0.0032(11) -0.0053(11) C2A 0.0204(13) 0.0205(13) 0.0343(15) -0.0005(11) -0.0089(11) -0.0061(11) C3A 0.0259(14) 0.0232(13) 0.0279(14) 0.0009(11) -0.0081(11) -0.0125(11) C4A 0.0338(16) 0.0477(18) 0.0284(15) -0.0011(13) -0.0131(13) -0.0122(14) C5A 0.0211(13) 0.0254(13) 0.0237(13) -0.0042(10) -0.0022(10) -0.0082(11) C6A 0.0193(12) 0.0154(12) 0.0220(13) -0.0018(10) -0.0015(10) -0.0056(10) C7A 0.0220(13) 0.0179(12) 0.0216(13) 0.0003(10) -0.0038(10) -0.0087(10) N2A 0.0228(11) 0.0186(10) 0.0221(11) -0.0004(8) -0.0040(9) -0.0049(9) C12A 0.0284(14) 0.0225(13) 0.0263(14) -0.0005(11) -0.0096(11) -0.0066(11) C11A 0.0216(14) 0.0238(13) 0.0356(15) 0.0047(11) -0.0107(12) -0.0070(11) C9A 0.0193(13) 0.0207(13) 0.0319(14) 0.0005(11) -0.0031(11) -0.0058(11) C10A 0.0225(14) 0.0341(15) 0.0389(16) -0.0030(13) -0.0028(12) -0.0038(12) C8A 0.0236(14) 0.0231(13) 0.0236(13) -0.0008(10) -0.0017(11) -0.0060(11) N1B 0.0252(12) 0.0209(11) 0.0205(11) -0.0031(8) -0.0011(9) -0.0073(9) C1B 0.0216(14) 0.0272(14) 0.0309(14) -0.0040(11) -0.0006(11) -0.0070(11) C2B 0.0239(14) 0.0330(15) 0.0265(14) -0.0015(11) 0.0016(11) -0.0127(12) C3B 0.0313(15) 0.0266(14) 0.0189(12) 0.0003(10) -0.0050(11) -0.0144(12) C4B 0.0316(15) 0.0271(14) 0.0395(16) 0.0021(12) -0.0068(13) -0.0164(12) C5B 0.0260(14) 0.0215(13) 0.0181(12) -0.0001(10) -0.0050(10) -0.0074(11) C6B 0.0245(13) 0.0212(13) 0.0149(12) -0.0009(10) -0.0041(10) -0.0078(11) C7B 0.0245(13) 0.0213(13) 0.0145(12) -0.0026(10) -0.0028(10) -0.0082(11) N2B 0.0238(11) 0.0213(11) 0.0184(10) -0.0034(8) 0.0008(9) -0.0073(9) C12B 0.0310(15) 0.0241(13) 0.0230(13) -0.0030(10) 0.0004(11) -0.0132(12) C11B 0.0260(14) 0.0336(15) 0.0258(14) -0.0038(11) -0.0003(11) -0.0151(12) C9B 0.0252(14) 0.0335(15) 0.0226(13) -0.0038(11) -0.0021(11) -0.0072(12) C10B 0.0255(15) 0.0386(17) 0.0505(19) 0.0011(14) -0.0041(14) -0.0047(13) C8B 0.0285(14) 0.0208(13) 0.0226(13) -0.0024(10) -0.0048(11) -0.0066(11) Cu2 0.01771(16) 0.01904(16) 0.01956(16) -0.00493(12) -0.00227(12) -0.00307(12) N1C 0.0190(10) 0.0195(10) 0.0194(10) -0.0037(8) -0.0049(8) -0.0056(9) C1C 0.0197(13) 0.0253(13) 0.0217(13) -0.0038(10) -0.0044(10) -0.0046(11) C2C 0.0244(14) 0.0298(14) 0.0205(13) 0.0007(11) -0.0035(11) -0.0108(12) C3C 0.0292(14) 0.0253(13) 0.0203(13) 0.0015(10) -0.0082(11) -0.0115(11) C4C 0.0436(17) 0.0292(15) 0.0299(15) 0.0006(12) -0.0059(13) -0.0180(13) C5C 0.0290(14) 0.0181(12) 0.0208(13) -0.0013(10) -0.0083(11) -0.0038(11) C6C 0.0211(13) 0.0226(13) 0.0169(12) -0.0018(10) -0.0079(10) -0.0047(11) C7C 0.0196(13) 0.0234(13) 0.0158(12) -0.0001(10) -0.0070(10) -0.0032(10) N2C 0.0184(11) 0.0204(10) 0.0188(10) -0.0040(8) -0.0039(8) -0.0032(9) C12C 0.0224(13) 0.0261(13) 0.0224(13) -0.0035(10) -0.0046(11) -0.0076(11) C11C 0.0191(13) 0.0344(15) 0.0230(13) -0.0021(11) -0.0040(11) -0.0061(12) C9C 0.0216(13) 0.0304(14) 0.0192(13) -0.0047(11) -0.0081(10) 0.0017(11) C10C 0.0242(14) 0.0353(16) 0.0319(15) -0.0099(12) -0.0025(12) 0.0012(12) C8C 0.0259(14) 0.0197(12) 0.0220(13) -0.0012(10) -0.0093(11) -0.0023(11) N1D 0.0205(11) 0.0185(10) 0.0203(10) -0.0027(8) -0.0046(9) -0.0063(9) C1D 0.0211(13) 0.0193(12) 0.0266(13) -0.0049(10) -0.0026(11) -0.0058(11) C2D 0.0223(13) 0.0228(13) 0.0304(14) 0.0008(11) -0.0086(11) -0.0067(11) C3D 0.0291(14) 0.0279(14) 0.0229(13) 0.0011(11) -0.0064(11) -0.0118(12) C4D 0.0366(17) 0.0539(19) 0.0255(15) -0.0036(13) -0.0107(13) -0.0057(15) C5D 0.0242(14) 0.0247(13) 0.0204(13) -0.0019(10) -0.0033(10) -0.0091(11) C6D 0.0205(13) 0.0163(12) 0.0217(13) -0.0015(10) -0.0017(10) -0.0084(10) C7D 0.0219(13) 0.0167(12) 0.0214(12) -0.0032(10) -0.0030(10) -0.0096(10) N2D 0.0188(11) 0.0177(10) 0.0221(11) -0.0059(8) -0.0035(9) -0.0034(9) C12D 0.0239(14) 0.0226(13) 0.0269(14) -0.0034(11) -0.0080(11) -0.0044(11) C11D 0.0187(13) 0.0225(13) 0.0315(14) -0.0027(11) -0.0059(11) -0.0034(11) C9D 0.0212(13) 0.0189(12) 0.0284(14) -0.0053(10) 0.0000(11) -0.0093(11) C10D 0.0239(14) 0.0312(15) 0.0332(15) -0.0111(12) 0.0019(12) -0.0045(12) C8D 0.0237(13) 0.0230(13) 0.0214(13) -0.0039(10) -0.0017(10) -0.0092(11) B1E 0.0270(17) 0.0280(16) 0.0340(18) -0.0021(14) -0.0044(14) -0.0021(14) F1E 0.0862(17) 0.0740(15) 0.0354(11) -0.0023(10) -0.0200(11) 0.0304(13) F2E 0.0522(13) 0.0511(13) 0.119(2) -0.0377(13) 0.0213(13) -0.0231(11) F3E 0.0274(9) 0.0740(14) 0.0537(12) 0.0052(10) -0.0028(8) -0.0094(9) F4E 0.0434(10) 0.0381(9) 0.0340(9) -0.0029(7) -0.0076(8) -0.0020(8) B1F 0.0259(16) 0.0269(16) 0.0294(16) -0.0036(13) -0.0056(13) -0.0008(13) F1F 0.0275(9) 0.0714(13) 0.0518(11) -0.0158(10) -0.0160(8) 0.0015(9) F2F 0.0338(10) 0.0901(15) 0.0325(10) -0.0158(9) -0.0111(8) 0.0081(10) F3F 0.0721(15) 0.0309(10) 0.0997(17) 0.0119(11) -0.0143(13) -0.0168(10) F4F 0.0408(10) 0.0311(9) 0.0434(10) -0.0108(7) -0.0095(8) 0.0035(8) C1G 0.0433(19) 0.0363(17) 0.065(2) 0.0017(16) -0.0251(17) -0.0092(15) Cl1G 0.0579(6) 0.0512(5) 0.0632(6) 0.0142(4) 0.0087(5) -0.0075(4) Cl2G 0.0509(6) 0.1268(10) 0.0473(5) -0.0102(6) -0.0141(4) -0.0322(6) Cl2 0.0298(4) 0.0294(3) 0.0264(3) 0.0038(3) -0.0001(3) -0.0017(3) Cl1 0.0386(4) 0.0231(3) 0.0261(3) 0.0024(3) 0.0014(3) -0.0083(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 Cu1 N2B 1.981(2) . ? Cu1 N2A 2.001(2) . ? Cu1 N1B 2.082(2) . ? Cu1 N1A 2.154(2) . ? Cu1 Cl1 2.2770(7) . ? N1A C1A 1.341(3) . ? N1A C6A 1.349(3) . ? C1A C2A 1.386(4) . ? C1A H1A 0.9500 . ? C2A C3A 1.379(4) . ? C2A H2A 0.9500 . ? C3A C5A 1.394(4) . ? C3A C4A 1.496(4) . ? C4A H4C 0.9800 . ? C4A H4B 0.9800 . ? C4A H4A 0.9800 . ? C5A C6A 1.376(3) . ? C5A H5A 0.9500 . ? C6A C7A 1.484(3) . ? C7A N2A 1.347(3) . ? C7A C8A 1.377(3) . ? N2A C12A 1.347(3) . ? C12A C11A 1.376(4) . ? C12A H12A 0.9500 . ? C11A C9A 1.388(4) . ? C11A H11A 0.9500 . ? C9A C8A 1.392(4) . ? C9A C10A 1.500(4) . ? C10A H10C 0.9800 . ? C10A H10B 0.9800 . ? C10A H10A 0.9800 . ? C8A H8A 0.9500 . ? N1B C6B 1.342(3) . ? N1B C1B 1.346(3) . ? C1B C2B 1.373(4) . ? C1B H1B 0.9500 . ? C2B C3B 1.386(4) . ? C2B H2B 0.9500 . ? C3B C5B 1.395(4) . ? C3B C4B 1.503(3) . ? C4B H4F 0.9800 . ? C4B H4E 0.9800 . ? C4B H4D 0.9800 . ? C5B C6B 1.386(3) . ? C5B H5B 0.9500 . ? C6B C7B 1.485(3) . ? C7B N2B 1.357(3) . ? C7B C8B 1.370(3) . ? N2B C12B 1.338(3) . ? C12B C11B 1.365(4) . ? C12B H12B 0.9500 . ? C11B C9B 1.385(4) . ? C11B H11B 0.9500 . ? C9B C8B 1.396(4) . ? C9B C10B 1.495(4) . ? C10B H10F 0.9800 . ? C10B H10E 0.9800 . ? C10B H10D 0.9800 . ? C8B H8B 0.9500 . ? Cu2 N2D 1.9750(19) . ? Cu2 N2C 1.9811(19) . ? Cu2 N1D 2.0917(19) . ? Cu2 N1C 2.096(2) . ? Cu2 Cl2 2.2887(7) . ? N1C C1C 1.340(3) . ? N1C C6C 1.343(3) . ? C1C C2C 1.379(4) . ? C1C H1C 0.9500 . ? C2C C3C 1.387(4) . ? C2C H2C 0.9500 . ? C3C C5C 1.391(4) . ? C3C C4C 1.497(3) . ? C4C H4I 0.9800 . ? C4C H4H 0.9800 . ? C4C H4G 0.9800 . ? C5C C6C 1.389(3) . ? C5C H5C 0.9500 . ? C6C C7C 1.483(3) . ? C7C N2C 1.348(3) . ? C7C C8C 1.377(3) . ? N2C C12C 1.343(3) . ? C12C C11C 1.372(3) . ? C12C H12C 0.9500 . ? C11C C9C 1.392(4) . ? C11C H11C 0.9500 . ? C9C C8C 1.387(4) . ? C9C C10C 1.495(3) . ? C10C H10I 0.9800 . ? C10C H10H 0.9800 . ? C10C H10G 0.9800 . ? C8C H8C 0.9500 . ? N1D C1D 1.339(3) . ? N1D C6D 1.349(3) . ? C1D C2D 1.375(4) . ? C1D H1D 0.9500 . ? C2D C3D 1.387(4) . ? C2D H2D 0.9500 . ? C3D C5D 1.390(4) . ? C3D C4D 1.499(4) . ? C4D H4L 0.9800 . ? C4D H4K 0.9800 . ? C4D H4J 0.9800 . ? C5D C6D 1.384(3) . ? C5D H5D 0.9500 . ? C6D C7D 1.478(3) . ? C7D N2D 1.349(3) . ? C7D C8D 1.380(3) . ? N2D C12D 1.338(3) . ? C12D C11D 1.373(3) . ? C12D H12D 0.9500 . ? C11D C9D 1.381(4) . ? C11D H11D 0.9500 . ? C9D C8D 1.396(4) . ? C9D C10D 1.496(3) . ? C10D H10L 0.9800 . ? C10D H10K 0.9800 . ? C10D H10J 0.9800 . ? C8D H8D 0.9500 . ? B1E F1E 1.367(4) . ? B1E F2E 1.370(4) . ? B1E F3E 1.376(4) . ? B1E F4E 1.400(4) . ? B1F F3F 1.364(4) . ? B1F F2F 1.377(4) . ? B1F F4F 1.378(3) . ? B1F F1F 1.390(4) . ? C1G Cl1G 1.754(3) . ? C1G Cl2G 1.755(4) . ? C1G H1G1 0.9900 . ? C1G H1G2 0.9900 . ? 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 N2B Cu1 N2A 169.34(8) . . ? N2B Cu1 N1B 79.64(8) . . ? N2A Cu1 N1B 96.60(8) . . ? N2B Cu1 N1A 91.78(8) . . ? N2A Cu1 N1A 79.07(8) . . ? N1B Cu1 N1A 100.97(8) . . ? N2B Cu1 Cl1 96.57(6) . . ? N2A Cu1 Cl1 93.08(6) . . ? N1B Cu1 Cl1 135.48(6) . . ? N1A Cu1 Cl1 123.54(6) . . ? C1A N1A C6A 117.5(2) . . ? C1A N1A Cu1 129.64(16) . . ? C6A N1A Cu1 112.56(15) . . ? N1A C1A C2A 123.0(2) . . ? N1A C1A H1A 118.5 . . ? C2A C1A H1A 118.5 . . ? C3A C2A C1A 119.5(2) . . ? C3A C2A H2A 120.3 . . ? C1A C2A H2A 120.3 . . ? C2A C3A C5A 117.5(2) . . ? C2A C3A C4A 122.5(2) . . ? C5A C3A C4A 120.0(2) . . ? C3A C4A H4C 109.5 . . ? C3A C4A H4B 109.5 . . ? H4C C4A H4B 109.5 . . ? C3A C4A H4A 109.5 . . ? H4C C4A H4A 109.5 . . ? H4B C4A H4A 109.5 . . ? C6A C5A C3A 120.1(2) . . ? C6A C5A H5A 120.0 . . ? C3A C5A H5A 120.0 . . ? N1A C6A C5A 122.4(2) . . ? N1A C6A C7A 114.9(2) . . ? C5A C6A C7A 122.8(2) . . ? N2A C7A C8A 121.3(2) . . ? N2A C7A C6A 116.2(2) . . ? C8A C7A C6A 122.5(2) . . ? C7A N2A C12A 118.4(2) . . ? C7A N2A Cu1 117.10(16) . . ? C12A N2A Cu1 124.47(17) . . ? N2A C12A C11A 122.7(2) . . ? N2A C12A H12A 118.6 . . ? C11A C12A H12A 118.6 . . ? C12A C11A C9A 119.6(2) . . ? C12A C11A H11A 120.2 . . ? C9A C11A H11A 120.2 . . ? C11A C9A C8A 117.1(2) . . ? C11A C9A C10A 122.7(2) . . ? C8A C9A C10A 120.1(2) . . ? C9A C10A H10C 109.5 . . ? C9A C10A H10B 109.5 . . ? H10C C10A H10B 109.5 . . ? C9A C10A H10A 109.5 . . ? H10C C10A H10A 109.5 . . ? H10B C10A H10A 109.5 . . ? C7A C8A C9A 120.9(2) . . ? C7A C8A H8A 119.6 . . ? C9A C8A H8A 119.6 . . ? C6B N1B C1B 118.4(2) . . ? C6B N1B Cu1 113.19(16) . . ? C1B N1B Cu1 128.13(17) . . ? N1B C1B C2B 122.6(2) . . ? N1B C1B H1B 118.7 . . ? C2B C1B H1B 118.7 . . ? C1B C2B C3B 119.8(2) . . ? C1B C2B H2B 120.1 . . ? C3B C2B H2B 120.1 . . ? C2B C3B C5B 117.6(2) . . ? C2B C3B C4B 121.4(2) . . ? C5B C3B C4B 121.0(2) . . ? C3B C4B H4F 109.5 . . ? C3B C4B H4E 109.5 . . ? H4F C4B H4E 109.5 . . ? C3B C4B H4D 109.5 . . ? H4F C4B H4D 109.5 . . ? H4E C4B H4D 109.5 . . ? C6B C5B C3B 119.7(2) . . ? C6B C5B H5B 120.2 . . ? C3B C5B H5B 120.2 . . ? N1B C6B C5B 122.0(2) . . ? N1B C6B C7B 114.9(2) . . ? C5B C6B C7B 123.1(2) . . ? N2B C7B C8B 121.8(2) . . ? N2B C7B C6B 113.9(2) . . ? C8B C7B C6B 124.4(2) . . ? C12B N2B C7B 118.0(2) . . ? C12B N2B Cu1 124.42(17) . . ? C7B N2B Cu1 115.90(16) . . ? N2B C12B C11B 122.8(2) . . ? N2B C12B H12B 118.6 . . ? C11B C12B H12B 118.6 . . ? C12B C11B C9B 120.1(2) . . ? C12B C11B H11B 119.9 . . ? C9B C11B H11B 119.9 . . ? C11B C9B C8B 117.1(2) . . ? C11B C9B C10B 122.3(2) . . ? C8B C9B C10B 120.6(2) . . ? C9B C10B H10F 109.5 . . ? C9B C10B H10E 109.5 . . ? H10F C10B H10E 109.5 . . ? C9B C10B H10D 109.5 . . ? H10F C10B H10D 109.5 . . ? H10E C10B H10D 109.5 . . ? C7B C8B C9B 120.2(2) . . ? C7B C8B H8B 119.9 . . ? C9B C8B H8B 119.9 . . ? N2D Cu2 N2C 173.81(8) . . ? N2D Cu2 N1D 79.94(8) . . ? N2C Cu2 N1D 96.96(8) . . ? N2D Cu2 N1C 95.45(8) . . ? N2C Cu2 N1C 79.60(8) . . ? N1D Cu2 N1C 97.96(8) . . ? N2D Cu2 Cl2 92.77(6) . . ? N2C Cu2 Cl2 93.21(6) . . ? N1D Cu2 Cl2 134.28(6) . . ? N1C Cu2 Cl2 127.73(6) . . ? C1C N1C C6C 118.5(2) . . ? C1C N1C Cu2 127.86(17) . . ? C6C N1C Cu2 113.53(16) . . ? N1C C1C C2C 122.7(2) . . ? N1C C1C H1C 118.6 . . ? C2C C1C H1C 118.6 . . ? C1C C2C C3C 119.7(2) . . ? C1C C2C H2C 120.2 . . ? C3C C2C H2C 120.2 . . ? C2C C3C C5C 117.4(2) . . ? C2C C3C C4C 121.5(2) . . ? C5C C3C C4C 121.0(2) . . ? C3C C4C H4I 109.5 . . ? C3C C4C H4H 109.5 . . ? H4I C4C H4H 109.5 . . ? C3C C4C H4G 109.5 . . ? H4I C4C H4G 109.5 . . ? H4H C4C H4G 109.5 . . ? C6C C5C C3C 120.0(2) . . ? C6C C5C H5C 120.0 . . ? C3C C5C H5C 120.0 . . ? N1C C6C C5C 121.7(2) . . ? N1C C6C C7C 114.8(2) . . ? C5C C6C C7C 123.5(2) . . ? N2C C7C C8C 121.1(2) . . ? N2C C7C C6C 114.8(2) . . ? C8C C7C C6C 124.1(2) . . ? C12C N2C C7C 118.5(2) . . ? C12C N2C Cu2 124.29(17) . . ? C7C N2C Cu2 117.21(16) . . ? N2C C12C C11C 122.8(2) . . ? N2C C12C H12C 118.6 . . ? C11C C12C H12C 118.6 . . ? C12C C11C C9C 119.5(2) . . ? C12C C11C H11C 120.2 . . ? C9C C11C H11C 120.2 . . ? C8C C9C C11C 117.1(2) . . ? C8C C9C C10C 121.5(2) . . ? C11C C9C C10C 121.4(2) . . ? C9C C10C H10I 109.5 . . ? C9C C10C H10H 109.5 . . ? H10I C10C H10H 109.5 . . ? C9C C10C H10G 109.5 . . ? H10I C10C H10G 109.5 . . ? H10H C10C H10G 109.5 . . ? C7C C8C C9C 121.0(2) . . ? C7C C8C H8C 119.5 . . ? C9C C8C H8C 119.5 . . ? C1D N1D C6D 118.1(2) . . ? C1D N1D Cu2 128.67(16) . . ? C6D N1D Cu2 113.05(15) . . ? N1D C1D C2D 123.4(2) . . ? N1D C1D H1D 118.3 . . ? C2D C1D H1D 118.3 . . ? C1D C2D C3D 119.0(2) . . ? C1D C2D H2D 120.5 . . ? C3D C2D H2D 120.5 . . ? C2D C3D C5D 117.8(2) . . ? C2D C3D C4D 121.7(2) . . ? C5D C3D C4D 120.4(2) . . ? C3D C4D H4L 109.5 . . ? C3D C4D H4K 109.5 . . ? H4L C4D H4K 109.5 . . ? C3D C4D H4J 109.5 . . ? H4L C4D H4J 109.5 . . ? H4K C4D H4J 109.5 . . ? C6D C5D C3D 120.0(2) . . ? C6D C5D H5D 120.0 . . ? C3D C5D H5D 120.0 . . ? N1D C6D C5D 121.5(2) . . ? N1D C6D C7D 114.8(2) . . ? C5D C6D C7D 123.6(2) . . ? N2D C7D C8D 121.2(2) . . ? N2D C7D C6D 115.0(2) . . ? C8D C7D C6D 123.8(2) . . ? C12D N2D C7D 118.7(2) . . ? C12D N2D Cu2 124.34(17) . . ? C7D N2D Cu2 116.86(16) . . ? N2D C12D C11D 122.5(2) . . ? N2D C12D H12D 118.7 . . ? C11D C12D H12D 118.7 . . ? C12D C11D C9D 119.9(2) . . ? C12D C11D H11D 120.0 . . ? C9D C11D H11D 120.0 . . ? C11D C9D C8D 117.3(2) . . ? C11D C9D C10D 122.1(2) . . ? C8D C9D C10D 120.6(2) . . ? C9D C10D H10L 109.5 . . ? C9D C10D H10K 109.5 . . ? H10L C10D H10K 109.5 . . ? C9D C10D H10J 109.5 . . ? H10L C10D H10J 109.5 . . ? H10K C10D H10J 109.5 . . ? C7D C8D C9D 120.3(2) . . ? C7D C8D H8D 119.9 . . ? C9D C8D H8D 119.9 . . ? F1E B1E F2E 111.7(3) . . ? F1E B1E F3E 109.1(3) . . ? F2E B1E F3E 109.1(2) . . ? F1E B1E F4E 109.0(2) . . ? F2E B1E F4E 108.7(3) . . ? F3E B1E F4E 109.2(3) . . ? F3F B1F F2F 109.6(3) . . ? F3F B1F F4F 109.5(2) . . ? F2F B1F F4F 109.3(2) . . ? F3F B1F F1F 108.7(2) . . ? F2F B1F F1F 109.6(2) . . ? F4F B1F F1F 110.2(2) . . ? Cl1G C1G Cl2G 110.41(17) . . ? Cl1G C1G H1G1 109.6 . . ? Cl2G C1G H1G1 109.6 . . ? Cl1G C1G H1G2 109.6 . . ? Cl2G C1G H1G2 109.6 . . ? H1G1 C1G H1G2 108.1 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.08 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.676 _refine_diff_density_min -0.428 _refine_diff_density_rms 0.071 # Attachment '- nr9002.cif' data_nr9002 _database_code_depnum_ccdc_archive 'CCDC 771443' #TrackingRef '- nr9002.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_compound_source 'Tracy Hewat' _exptl_crystal_recrystallization_method 'Diffusion of Et2O into DCM solution' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2[Cu (C14 H16 N2)2], 2BF4, CH2Cl2' _chemical_formula_sum 'C28 H32 B Cu F4 N4' _chemical_formula_weight 574.93 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' _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+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.8531(14) _cell_length_b 16.4771(14) _cell_length_c 13.5039(19) _cell_angle_alpha 90.00 _cell_angle_beta 119.730(7) _cell_angle_gamma 90.00 _cell_volume 2676.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5429 _cell_measurement_theta_min 2.472 _cell_measurement_theta_max 26.3515 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.90 _exptl_crystal_size_mid 0.59 _exptl_crystal_size_min 0.43 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 0.869 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5519 _exptl_absorpt_correction_T_max 0.6858 _exptl_absorpt_process_details 'SADABS 2007/2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 13995 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 26.42 _reflns_number_total 2747 _reflns_number_gt 2276 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution 'Shelxs Sheldrick' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Shelxp _computing_publication_material 'Platon, encifer' _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. #========================================================================== The Following Model and Quality ALERTS were generated - (Acta-Mode) <<< #========================================================================== Format: alert-number_ALERT_alert-type_alert-level text 083_ALERT_2_G SHELXL Second Parameter in WGHT Unusually Large. 5.84 This is likely due to noise in the difference map in the region of the BF4 911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.600 3 912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 12 A sphere of data was collected. Completeness stats below... #============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 1.000 1409 1409 0 23.01 0.550 0.999 1869 1868 1 25.24 0.600 0.999 2423 2420 3 #----------------------------------------------------------- ACTA Min. Res. --- 26.42 0.626 0.995 2762 2747 15 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 184 Confirmed 063_ALERT_4_B Crystal Probably too Large for Beam Size ....... 0.90 mm Gorbitz has shown that use of a large crystal does not appear to matter. See C. H. Gorbitz Acta Cryst. (1999). B55, 1090-1098 042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? The formula given is intended to be more chemically meaningful. 221_ALERT_4_C Large Solvent/Anion F Ueq(max)/Ueq(min) ... 3.31 Ratio 244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for B1 302_ALERT_4_G Note Anion/Solvent Disorder .................... 24.00 Perc. 764_ALERT_4_G Overcomplete CIF Bond List Detected (Rep/Expd) . 1.13 Ratio 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 33.50 Deg. F2' -B1 -F2A 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 33.50 Deg. F2' -B1 -F2A 2.656 1.555 2.656 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 24.00 Deg. F2 -B1 -F2" 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 24.00 Deg. F2 -B1 -F2" 2.656 1.555 2.656 There is disordered BF4- in the structure. It has been modelled as best as possible using isotropic thermal parameters, DFIX restraints on 1,2 and 1,3 distances and thermal similarity restraints. Occupancies were initially refined using free variables and a sump to sum the 4 components occupancies to 1. These were then used as a guide to fix the occupancies. 720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 4 760_ALERT_1_G CIF Contains no Torsion Angles ................. ? No action taken. 811_ALERT_5_G No ADDSYM Analysis: Too Many Excluded Atoms .... ! Addsym is missed out due to BF4 disorder. Removing it confirms C2/c symmetry. C2/c with disorder in the BF4 is therefore the most appropriate solution. ; _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^)+(0.0929P)^2^+5.8420P] 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_number_reflns 2747 _refine_ls_number_parameters 190 _refine_ls_number_restraints 184 _refine_ls_R_factor_all 0.0617 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1560 _refine_ls_wR_factor_gt 0.1470 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.120 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Cu1 Cu 0.5000 0.74919(3) 0.7500 0.0237(2) Uani 1 2 d S . . N1A N 0.56299(19) 0.65406(14) 0.8629(2) 0.0221(5) Uani 1 1 d U . . C2A C 0.5336(2) 0.57968(17) 0.8135(2) 0.0225(6) Uani 1 1 d U . . C3A C 0.5645(3) 0.50821(18) 0.8760(3) 0.0273(6) Uani 1 1 d U . . H3AA H 0.5429 0.4573 0.8383 0.033 Uiso 1 1 calc R . . C4A C 0.6274(3) 0.51166(19) 0.9947(3) 0.0289(7) Uani 1 1 d U . . C5A C 0.6548(3) 0.58773(19) 1.0449(3) 0.0287(7) Uani 1 1 d U . . H5AA H 0.6968 0.5923 1.1256 0.034 Uiso 1 1 calc R . . C6A C 0.6212(2) 0.65765(18) 0.9781(2) 0.0252(6) Uani 1 1 d U . . C41A C 0.6635(3) 0.4350(2) 1.0639(3) 0.0396(8) Uani 1 1 d U . . H41A H 0.7087 0.4486 1.1450 0.059 Uiso 1 1 calc R . . H41B H 0.7075 0.4020 1.0404 0.059 Uiso 1 1 calc R . . H41C H 0.5978 0.4043 1.0516 0.059 Uiso 1 1 calc R . . C61A C 0.6466(3) 0.73987(18) 1.0316(3) 0.0325(7) Uani 1 1 d U . . H61A H 0.6192 0.7814 0.9719 0.049 Uiso 1 1 calc R . . H61B H 0.7271 0.7458 1.0807 0.049 Uiso 1 1 calc R . . H61C H 0.6101 0.7463 1.0774 0.049 Uiso 1 1 calc R . . N1B N 0.56946(19) 0.84434(14) 0.70868(19) 0.0218(5) Uani 1 1 d U . . C2B C 0.5353(2) 0.91860(17) 0.7225(2) 0.0227(6) Uani 1 1 d U . . C3B C 0.5639(3) 0.98959(17) 0.6884(2) 0.0256(6) Uani 1 1 d U . . H3BA H 0.5386 1.0404 0.6999 0.031 Uiso 1 1 calc R . . C4B C 0.6294(3) 0.98627(18) 0.6376(3) 0.0279(6) Uani 1 1 d U . . C5B C 0.6640(3) 0.91025(19) 0.6227(3) 0.0291(7) Uani 1 1 d U . . H5BA H 0.7092 0.9058 0.5883 0.035 Uiso 1 1 calc R . . C6B C 0.6323(2) 0.84036(18) 0.6583(2) 0.0253(6) Uani 1 1 d U . . C41B C 0.6609(3) 1.0628(2) 0.5992(3) 0.0360(8) Uani 1 1 d U . . H41D H 0.7025 1.0488 0.5604 0.054 Uiso 1 1 calc R . . H41E H 0.7072 1.0969 0.6657 0.054 Uiso 1 1 calc R . . H41F H 0.5934 1.0926 0.5466 0.054 Uiso 1 1 calc R . . C61B C 0.6667(3) 0.75817(18) 0.6401(3) 0.0330(7) Uani 1 1 d U . . H61D H 0.6353 0.7166 0.6678 0.049 Uiso 1 1 calc R . . H61E H 0.7479 0.7542 0.6819 0.049 Uiso 1 1 calc R . . H61F H 0.6392 0.7499 0.5585 0.049 Uiso 1 1 calc R . . B1 B 0.5000 0.2526(3) 0.7500 0.055(2) Uani 1 2 d SD . . F1 F 0.4311(6) 0.1967(5) 0.7685(9) 0.058(2) Uiso 0.30 1 d PD A 1 F2 F 0.5621(8) 0.2921(5) 0.8443(5) 0.095(4) Uiso 0.30 1 d PD B 1 F1' F 0.5731(8) 0.3091(6) 0.7384(13) 0.086(3) Uiso 0.27 1 d PD C 2 F2' F 0.4452(11) 0.2130(7) 0.6557(5) 0.192(11) Uiso 0.27 1 d PD B 2 F1" F 0.4678(10) 0.2075(6) 0.8111(9) 0.077(4) Uiso 0.26 1 d PD B 3 F2" F 0.5869(5) 0.3033(6) 0.8237(8) 0.077(4) Uiso 0.26 1 d PD B 3 F1A F 0.5223(19) 0.2956(7) 0.6815(14) 0.096(5) Uiso 0.17 1 d PD B 4 F2A F 0.4113(6) 0.2006(7) 0.6854(15) 0.096(5) Uiso 0.17 1 d PD B 4 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 Cu1 0.0308(3) 0.0156(3) 0.0270(3) 0.000 0.0160(2) 0.000 N1A 0.0240(12) 0.0188(11) 0.0243(11) -0.0012(9) 0.0125(10) -0.0007(9) C2A 0.0239(14) 0.0209(13) 0.0250(15) 0.0001(11) 0.0140(12) -0.0004(11) C3A 0.0315(16) 0.0200(14) 0.0298(15) 0.0010(11) 0.0148(13) -0.0017(11) C4A 0.0310(16) 0.0244(15) 0.0312(15) 0.0053(12) 0.0154(13) 0.0001(12) C5A 0.0304(16) 0.0292(15) 0.0241(14) 0.0021(11) 0.0117(12) -0.0017(12) C6A 0.0262(14) 0.0235(14) 0.0270(14) -0.0010(11) 0.0139(12) -0.0004(11) C41A 0.049(2) 0.0281(17) 0.0335(17) 0.0094(13) 0.0142(16) 0.0004(14) C61A 0.0398(19) 0.0266(16) 0.0279(16) -0.0043(12) 0.0143(14) -0.0015(13) N1B 0.0236(12) 0.0189(11) 0.0233(11) -0.0018(9) 0.0118(10) -0.0006(9) C2B 0.0244(14) 0.0206(13) 0.0216(13) -0.0009(10) 0.0102(12) -0.0019(11) C3B 0.0286(15) 0.0196(13) 0.0276(14) 0.0019(11) 0.0132(12) 0.0005(11) C4B 0.0267(15) 0.0254(14) 0.0290(15) 0.0026(11) 0.0119(13) -0.0026(11) C5B 0.0293(16) 0.0310(16) 0.0319(15) -0.0009(12) 0.0189(13) -0.0013(12) C6B 0.0258(14) 0.0255(14) 0.0245(13) -0.0019(11) 0.0125(12) 0.0000(11) C41B 0.0396(18) 0.0290(17) 0.0439(19) 0.0086(14) 0.0242(16) -0.0037(14) C61B 0.0395(19) 0.0256(16) 0.0420(19) -0.0043(13) 0.0265(16) -0.0003(13) B1 0.036(3) 0.095(6) 0.037(3) 0.000 0.020(3) 0.000 _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 Cu1 N1A 2.055(2) 2_656 ? Cu1 N1A 2.055(2) . ? Cu1 N1B 2.056(2) . ? Cu1 N1B 2.056(2) 2_656 ? N1A C6A 1.352(4) . ? N1A C2A 1.358(4) . ? C2A C3A 1.387(4) . ? C2A C2A 1.492(6) 2_656 ? C3A C4A 1.394(4) . ? C3A H3AA 0.9500 . ? C4A C5A 1.386(4) . ? C4A C41A 1.503(4) . ? C5A C6A 1.394(4) . ? C5A H5AA 0.9500 . ? C6A C61A 1.493(4) . ? C41A H41A 0.9800 . ? C41A H41B 0.9800 . ? C41A H41C 0.9800 . ? C61A H61A 0.9800 . ? C61A H61B 0.9800 . ? C61A H61C 0.9800 . ? N1B C6B 1.347(4) . ? N1B C2B 1.358(4) . ? C2B C3B 1.385(4) . ? C2B C2B 1.492(6) 2_656 ? C3B C4B 1.383(4) . ? C3B H3BA 0.9500 . ? C4B C5B 1.392(4) . ? C4B C41B 1.509(4) . ? C5B C6B 1.400(4) . ? C5B H5BA 0.9500 . ? C6B C61B 1.496(4) . ? C41B H41D 0.9800 . ? C41B H41E 0.9800 . ? C41B H41F 0.9800 . ? C61B H61D 0.9800 . ? C61B H61E 0.9800 . ? C61B H61F 0.9800 . ? B1 F2' 1.291(8) . ? B1 F2' 1.291(8) 2_656 ? B1 F2 1.303(7) . ? B1 F2 1.303(7) 2_656 ? B1 F1A 1.318(8) 2_656 ? B1 F1A 1.318(8) . ? B1 F1" 1.341(7) 2_656 ? B1 F1" 1.341(7) . ? B1 F2A 1.394(8) . ? B1 F2A 1.394(8) 2_656 ? B1 F2" 1.396(7) . ? B1 F2" 1.396(7) 2_656 ? 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 N1A Cu1 N1A 80.60(13) 2_656 . ? N1A Cu1 N1B 117.63(9) 2_656 . ? N1A Cu1 N1B 134.37(9) . . ? N1A Cu1 N1B 134.37(9) 2_656 2_656 ? N1A Cu1 N1B 117.63(9) . 2_656 ? N1B Cu1 N1B 80.63(13) . 2_656 ? C6A N1A C2A 117.9(2) . . ? C6A N1A Cu1 127.70(19) . . ? C2A N1A Cu1 114.21(18) . . ? N1A C2A C3A 122.7(3) . . ? N1A C2A C2A 115.42(16) . 2_656 ? C3A C2A C2A 121.87(17) . 2_656 ? C2A C3A C4A 119.5(3) . . ? C2A C3A H3AA 120.2 . . ? C4A C3A H3AA 120.2 . . ? C5A C4A C3A 117.6(3) . . ? C5A C4A C41A 122.0(3) . . ? C3A C4A C41A 120.4(3) . . ? C4A C5A C6A 120.5(3) . . ? C4A C5A H5AA 119.7 . . ? C6A C5A H5AA 119.7 . . ? N1A C6A C5A 121.7(3) . . ? N1A C6A C61A 117.4(3) . . ? C5A C6A C61A 120.9(3) . . ? C4A C41A H41A 109.5 . . ? C4A C41A H41B 109.5 . . ? H41A C41A H41B 109.5 . . ? C4A C41A H41C 109.5 . . ? H41A C41A H41C 109.5 . . ? H41B C41A H41C 109.5 . . ? C6A C61A H61A 109.5 . . ? C6A C61A H61B 109.5 . . ? H61A C61A H61B 109.5 . . ? C6A C61A H61C 109.5 . . ? H61A C61A H61C 109.5 . . ? H61B C61A H61C 109.5 . . ? C6B N1B C2B 118.1(2) . . ? C6B N1B Cu1 127.37(19) . . ? C2B N1B Cu1 114.06(18) . . ? N1B C2B C3B 122.6(3) . . ? N1B C2B C2B 115.31(16) . 2_656 ? C3B C2B C2B 122.12(17) . 2_656 ? C4B C3B C2B 119.9(3) . . ? C4B C3B H3BA 120.1 . . ? C2B C3B H3BA 120.1 . . ? C3B C4B C5B 117.8(3) . . ? C3B C4B C41B 120.7(3) . . ? C5B C4B C41B 121.6(3) . . ? C4B C5B C6B 120.1(3) . . ? C4B C5B H5BA 120.0 . . ? C6B C5B H5BA 120.0 . . ? N1B C6B C5B 121.7(3) . . ? N1B C6B C61B 117.7(3) . . ? C5B C6B C61B 120.6(3) . . ? C4B C41B H41D 109.5 . . ? C4B C41B H41E 109.5 . . ? H41D C41B H41E 109.5 . . ? C4B C41B H41F 109.5 . . ? H41D C41B H41F 109.5 . . ? H41E C41B H41F 109.5 . . ? C6B C61B H61D 109.5 . . ? C6B C61B H61E 109.5 . . ? H61D C61B H61E 109.5 . . ? C6B C61B H61F 109.5 . . ? H61D C61B H61F 109.5 . . ? H61E C61B H61F 109.5 . . ? F2' B1 F2' 119.2(9) . 2_656 ? F2' B1 F2 175.5(7) . . ? F2' B1 F2 60.5(6) 2_656 . ? F2' B1 F2 60.5(6) . 2_656 ? F2' B1 F2 175.5(7) 2_656 2_656 ? F2 B1 F2 120.1(8) . 2_656 ? F2' B1 F1A 137.4(9) . 2_656 ? F2' B1 F1A 78.9(8) 2_656 2_656 ? F2 B1 F1A 46.9(9) . 2_656 ? F2 B1 F1A 98.4(8) 2_656 2_656 ? F2' B1 F1A 78.9(8) . . ? F2' B1 F1A 137.4(9) 2_656 . ? F2 B1 F1A 98.4(8) . . ? F2 B1 F1A 46.9(9) 2_656 . ? F1A B1 F1A 115.0(9) 2_656 . ? F2' B1 F1" 47.5(7) . 2_656 ? F2' B1 F1" 96.6(7) 2_656 2_656 ? F2 B1 F1" 128.2(6) . 2_656 ? F2 B1 F1" 86.3(5) 2_656 2_656 ? F1A B1 F1" 174.6(9) 2_656 2_656 ? F1A B1 F1" 66.4(6) . 2_656 ? F2' B1 F1" 96.6(7) . . ? F2' B1 F1" 47.5(7) 2_656 . ? F2 B1 F1" 86.3(5) . . ? F2 B1 F1" 128.2(6) 2_656 . ? F1A B1 F1" 66.4(6) 2_656 . ? F1A B1 F1" 174.6(9) . . ? F1" B1 F1" 112.7(8) 2_656 . ? F2' B1 F2A 33.5(9) . . ? F2' B1 F2A 102.2(7) 2_656 . ? F2 B1 F2A 150.3(8) . . ? F2 B1 F2A 75.3(7) 2_656 . ? F1A B1 F2A 109.2(3) 2_656 . ? F1A B1 F2A 109.4(3) . . ? F1" B1 F2A 74.5(8) 2_656 . ? F1" B1 F2A 65.5(8) . . ? F2' B1 F2A 102.2(7) . 2_656 ? F2' B1 F2A 33.5(9) 2_656 2_656 ? F2 B1 F2A 75.3(7) . 2_656 ? F2 B1 F2A 150.3(8) 2_656 2_656 ? F1A B1 F2A 109.4(3) 2_656 2_656 ? F1A B1 F2A 109.2(3) . 2_656 ? F1" B1 F2A 65.5(8) 2_656 2_656 ? F1" B1 F2A 74.5(8) . 2_656 ? F2A B1 F2A 104.0(8) . 2_656 ? F2' B1 F2" 152.1(7) . . ? F2' B1 F2" 73.8(6) 2_656 . ? F2 B1 F2" 24.0(6) . . ? F2 B1 F2" 108.5(6) 2_656 . ? F1A B1 F2" 66.2(8) 2_656 . ? F1A B1 F2" 76.1(8) . . ? F1" B1 F2" 109.8(3) 2_656 . ? F1" B1 F2" 108.9(3) . . ? F2A B1 F2" 174.3(8) . . ? F2A B1 F2" 75.0(6) 2_656 . ? F2' B1 F2" 73.8(6) . 2_656 ? F2' B1 F2" 152.1(7) 2_656 2_656 ? F2 B1 F2" 108.5(6) . 2_656 ? F2 B1 F2" 24.0(6) 2_656 2_656 ? F1A B1 F2" 76.1(8) 2_656 2_656 ? F1A B1 F2" 66.2(8) . 2_656 ? F1" B1 F2" 108.9(3) 2_656 2_656 ? F1" B1 F2" 109.8(3) . 2_656 ? F2A B1 F2" 75.0(6) . 2_656 ? F2A B1 F2" 174.3(8) 2_656 2_656 ? F2" B1 F2" 106.5(7) . 2_656 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.076 _refine_diff_density_min -0.707 _refine_diff_density_rms 0.095