# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 loop_ _publ_author_name _publ_author_address _publ_author_footnote 'J. Nierengarten' ; Laboratoire de Chimie de Coordination du CNRS (UPR 8241), 205 route de Narbonne, 31077 Toulouse Cedex 4, France ; ; ? # Footnote for author 1 ; 'Gianluca Accorsi' ; Laboratoire de Chimie de Coordination du CNRS (UPR 8241), 205 route de Narbonne, 31077 Toulouse Cedex 4, France ; ; ? # Footnote 2 ; 'Nicola Armaroli' ; Laboratoire de Chimie de Coordination du CNRS (UPR 8241), 205 route de Narbonne, 31077 Toulouse Cedex 4, France ; ; ? # Footnote 2 ; 'Beatrice Delavaux-Nicot' ; Laboratoire de Chimie de Coordination du CNRS (UPR 8241), 205 route de Narbonne, 31077 Toulouse Cedex 4, France ; ; ? # Footnote 2 ; ; P.Destruel ; ; Laboratoire de Physico-Chimie Bioinorganique, ULP-CNRS (UMR 7177), Institut de Chimie, ECPM, 25 rue Becquerel, 67087 Strasbourg Cedex 2, France ; ; ? # Footnote 2 ; 'Carine Duhayon' ; Istituto per la Sintesi Organica e la Fotoreattivit\`a, Molecular Photoscience Group, Consiglio Nazionale delle Ricerche, Via Gobetti 101, 40129 Bologna, Italy ; ; ? # Footnote 2 ; 'Michel Holler' ; Istituto per la Sintesi Organica e la Fotoreattivit\`a, Molecular Photoscience Group, Consiglio Nazionale delle Ricerche, Via Gobetti 101, 40129 Bologna, Italy ; ; ? # Footnote 2 ; 'Omar Moudam' ; Laboratoire Plasma et Conversion d'Energie (LAPLACE), UPS-CNRS (UMR 5213), 118 route de Narbonne, 31062 Toulouse Cedex 9 France ; ; ? # Footnote 2 ; 'Jose Navarro' ; Laboratoire Plasma et Conversion d'Energie (LAPLACE), UPS-CNRS (UMR 5213), 118 route de Narbonne, 31062 Toulouse Cedex 9 France ; ; ? # Footnote for author 1 ; 'I. Seguy' ; Laboratoire Plasma et Conversion d'Energie (LAPLACE), UPS-CNRS (UMR 5213), 118 route de Narbonne, 31062 Toulouse Cedex 9 France ; ; ? # Footnote 2 ; _publ_contact_author_name 'J. Nierengarten' _publ_contact_author_address ; Groupe de Chimie des Fullerenes et des Systemes Conjugues Laboratoire de Chimie de Coordination du CNRS 205 205 route de Narbonne Toulouse Cedex 4 31077 FRANCE ; _publ_contact_author_email JFNIERENGARTEN@LCC-TOULOUSE.FR _publ_section_title ; Electrophosphorescent homo- and heteroleptic copper(I) complexes prepared from various bis-phosphine ligands ; _journal_coden_ASTM ? _journal_coeditor_code ? _journal_coeditor_name ? _journal_coeditor_notes ? _journal_date_accepted ? _journal_date_from_coeditor ? _journal_date_printers_final ? _journal_date_printers_first ? _journal_date_proofs_in ? _journal_date_proofs_out ? # PROCESSING SUMMARY (IUCr Office Use Only): _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_volume ? _journal_year ? _publ_contact_author_fax ' 33 (0) 5 61 55 30 03' _publ_contact_author_phone '33 (0) 5 61 33 31 51' # Check this file using the IUCr facility at: # http://checkcif.iucr.org/ # The content below is held in the file 'script/refcif.dat'. This is a text # file which you may edit to reflect local conditions. # Items which need looking at are represented by a '?'. # Items for which there are choices are prefixed with 'choose from'. _publ_contact_letter ; ; _publ_requested_category EO # choose from: FI FM FO CI CM CO AD _publ_requested_coeditor_name ? data_1 _database_code_depnum_ccdc_archive 'CCDC 645318' _audit_creation_date 07-04-16 _audit_creation_method CRYSTALS_ver_12.84 _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 14.6080(14) _cell_length_b 19.213(2) _cell_length_c 21.0316(17) _cell_angle_alpha 80.126(11) _cell_angle_beta 80.686(11) _cell_angle_gamma 89.676(12) _cell_volume 5737.2(10) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? 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' 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' 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' 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' 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' 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' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C61.75 H51.50 B1 Cl1.50 Cu1 F4 O1 P4 # Dc = 1.32 Fooo = 2342.00 Mu = 6.15 M = 2274.02 # Found Formula = C61.75 H51.50 B1 Cl1.50 Cu1 F4 O1 P4 # Dc = 1.32 FOOO = 2342.00 Mu = 6.15 M = 2274.02 _chemical_formula_sum 'C61.75 H51.50 B1 Cl1.50 Cu1 F4 O1 P4' _chemical_formula_moiety '(C61 H50 Cu O P4), 0.75(C H2 Cl2), (B F4)' _chemical_compound_source ? _chemical_formula_weight 1137.01 _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 3 _cell_measurement_theta_max 24 _cell_measurement_temperature 180 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_max 0.37 _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 2342 _exptl_absorpt_coefficient_mu 0.615 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 0.94 _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'IPDS (Stoe & Cie, 1996)' _computing_cell_refinement 'IPDS (Stoe & Cie, 1996)' _computing_data_reduction 'XRED (Stoe & Cie 1996)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _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 180 _diffrn_reflns_number 57446 _reflns_number_total 20986 _diffrn_reflns_av_R_equivalents 0.085 # Number of reflections with Friedels Law is 20986 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 22609 _diffrn_reflns_theta_min 2.041 _diffrn_reflns_theta_max 26.022 _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 25.241 _diffrn_measured_fraction_theta_full 0.940 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _reflns_limit_h_min -17 _reflns_limit_h_max 18 _reflns_limit_k_min -23 _reflns_limit_k_max 23 _reflns_limit_l_min 0 _reflns_limit_l_max 24 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.15 _refine_diff_density_max 1.44 _refine_ls_number_reflns 6820 _refine_ls_number_restraints 0 _refine_ls_number_parameters 651 #_refine_ls_R_factor_ref 0.0714 _refine_ls_wR_factor_ref 0.0789 _refine_ls_goodness_of_fit_ref 1.1740 #_reflns_number_all 20908 _refine_ls_R_factor_all 0.1980 _refine_ls_wR_factor_all 0.2368 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 6820 _refine_ls_R_factor_gt 0.0714 _refine_ls_wR_factor_gt 0.0789 _refine_ls_shift/su_max 0.000311 # 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 F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed # WARNING. The IUCr will not accept Unit Weights _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Quasi-Unit weights W = 1.0 or 1./2F ; _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_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 Fih. ; ? ; _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: ; 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. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # End of 'script/refcif.dat' # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. & Spagna, R. (1999). J. App. Cryst. 32, 115-119. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Stoe & Cie (1996). IPDS Software. Stoe & Cie (1996). XRED V1.08. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Cu1 Cu 0.20673(10) 0.87970(7) 0.24563(7) 0.0301 1.0000 Uani . . . . . . Cu2 Cu 0.69081(10) 0.37958(7) 0.24280(7) 0.0293 1.0000 Uani . . . . . . P1 P 0.1766(2) 0.93098(17) 0.33658(16) 0.0303 1.0000 Uani . . . . . . P2 P 0.2543(2) 0.96373(16) 0.15415(16) 0.0300 1.0000 Uani . . . . . . P3 P 0.1100(2) 0.79572(17) 0.22035(17) 0.0321 1.0000 Uani . . . . . . P4 P 0.2984(2) 0.77525(17) 0.23604(17) 0.0327 1.0000 Uani . . . . . . P101 P 0.6896(2) 0.46560(16) 0.15267(16) 0.0295 1.0000 Uani . . . . . . P102 P 0.6752(2) 0.42666(16) 0.33568(16) 0.0300 1.0000 Uani . . . . . . P103 P 0.8006(2) 0.29534(16) 0.21723(16) 0.0297 1.0000 Uani . . . . . . P104 P 0.6041(2) 0.27716(16) 0.23195(17) 0.0317 1.0000 Uani . . . . . . O1 O 0.3450(5) 0.9974(4) 0.2663(4) 0.034(2) 1.0000 Uiso . . . . . . O101 O 0.5407(5) 0.4954(4) 0.2629(4) 0.033(2) 1.0000 Uiso . . . . . . C1 C 0.1962(8) 1.0258(6) 0.3162(6) 0.028(3) 1.0000 Uiso . . . . . . C2 C 0.1316(9) 1.0757(6) 0.3309(6) 0.042(3) 1.0000 Uiso . . . . . . C3 C 0.1500(10) 1.1486(7) 0.3085(7) 0.050(4) 1.0000 Uiso . . . . . . C4 C 0.2350(9) 1.1688(7) 0.2714(7) 0.049(4) 1.0000 Uiso . . . . . . C5 C 0.3028(9) 1.1213(6) 0.2566(7) 0.040(3) 1.0000 Uiso . . . . . . C6 C 0.2807(8) 1.0499(6) 0.2786(6) 0.035(3) 1.0000 Uiso . . . . . . C7 C 0.4041(8) 1.0095(6) 0.2049(6) 0.037(3) 1.0000 Uiso . . . . . . C8 C 0.4962(8) 1.0268(6) 0.2067(7) 0.040(3) 1.0000 Uiso . . . . . . C9 C 0.5579(9) 1.0358(7) 0.1484(7) 0.044(3) 1.0000 Uiso . . . . . . C10 C 0.5272(9) 1.0281(7) 0.0917(7) 0.045(3) 1.0000 Uiso . . . . . . C11 C 0.4346(9) 1.0104(6) 0.0914(7) 0.044(3) 1.0000 Uiso . . . . . . C12 C 0.3709(8) 0.9988(6) 0.1492(6) 0.029(3) 1.0000 Uiso . . . . . . C13 C 0.2457(8) 0.9034(6) 0.4000(6) 0.032(3) 1.0000 Uiso . . . . . . C14 C 0.2689(9) 0.8326(7) 0.4139(7) 0.045(3) 1.0000 Uiso . . . . . . C15 C 0.3184(9) 0.8080(7) 0.4640(7) 0.050(4) 1.0000 Uiso . . . . . . C16 C 0.3481(9) 0.8556(7) 0.4991(7) 0.050(4) 1.0000 Uiso . . . . . . C17 C 0.3262(8) 0.9250(7) 0.4860(6) 0.043(3) 1.0000 Uiso . . . . . . C18 C 0.2761(8) 0.9499(6) 0.4369(6) 0.037(3) 1.0000 Uiso . . . . . . C19 C 0.0588(8) 0.9226(6) 0.3814(6) 0.032(3) 1.0000 Uiso . . . . . . C20 C -0.0156(8) 0.9276(6) 0.3478(7) 0.037(3) 1.0000 Uiso . . . . . . C21 C -0.1074(10) 0.9217(7) 0.3789(7) 0.051(4) 1.0000 Uiso . . . . . . C22 C -0.1246(12) 0.9094(8) 0.4462(9) 0.073(5) 1.0000 Uiso . . . . . . C23 C -0.0523(13) 0.9025(10) 0.4821(11) 0.092(6) 1.0000 Uiso . . . . . . C24 C 0.0402(11) 0.9090(8) 0.4484(8) 0.067(5) 1.0000 Uiso . . . . . . C25 C 0.1809(8) 1.0393(6) 0.1458(6) 0.032(3) 1.0000 Uiso . . . . . . C26 C 0.2142(10) 1.1079(7) 0.1210(7) 0.047(4) 1.0000 Uiso . . . . . . C27 C 0.1546(10) 1.1627(8) 0.1100(8) 0.060(4) 1.0000 Uiso . . . . . . C28 C 0.0601(9) 1.1516(7) 0.1255(7) 0.049(4) 1.0000 Uiso . . . . . . C29 C 0.0254(10) 1.0836(7) 0.1500(7) 0.049(4) 1.0000 Uiso . . . . . . C30 C 0.0845(8) 1.0291(7) 0.1613(6) 0.039(3) 1.0000 Uiso . . . . . . C31 C 0.2569(8) 0.9346(6) 0.0750(6) 0.030(3) 1.0000 Uiso . . . . . . C32 C 0.3148(8) 0.8789(6) 0.0603(6) 0.036(3) 1.0000 Uiso . . . . . . C33 C 0.3116(9) 0.8509(7) 0.0033(6) 0.042(3) 1.0000 Uiso . . . . . . C34 C 0.2550(9) 0.8789(7) -0.0384(7) 0.046(4) 1.0000 Uiso . . . . . . C35 C 0.2005(9) 0.9359(7) -0.0274(7) 0.049(4) 1.0000 Uiso . . . . . . C36 C 0.2012(8) 0.9634(6) 0.0305(6) 0.040(3) 1.0000 Uiso . . . . . . C37 C 0.2129(8) 0.7480(6) 0.1886(6) 0.034(3) 1.0000 Uiso . . . . . . C38 C 0.0366(8) 0.8104(6) 0.1574(6) 0.035(3) 1.0000 Uiso . . . . . . C39 C 0.0671(9) 0.8064(7) 0.0929(7) 0.046(4) 1.0000 Uiso . . . . . . C40 C 0.0092(10) 0.8253(8) 0.0454(8) 0.062(4) 1.0000 Uiso . . . . . . C41 C -0.0763(11) 0.8490(8) 0.0634(8) 0.063(4) 1.0000 Uiso . . . . . . C42 C -0.1085(11) 0.8531(8) 0.1283(8) 0.066(4) 1.0000 Uiso . . . . . . C43 C -0.0514(10) 0.8336(7) 0.1740(8) 0.052(4) 1.0000 Uiso . . . . . . C44 C 0.0462(8) 0.7303(6) 0.2849(6) 0.031(3) 1.0000 Uiso . . . . . . C45 C 0.0311(9) 0.7422(8) 0.3472(7) 0.053(4) 1.0000 Uiso . . . . . . C46 C -0.0132(11) 0.6885(9) 0.3978(9) 0.075(5) 1.0000 Uiso . . . . . . C47 C -0.0391(11) 0.6251(9) 0.3824(9) 0.067(4) 1.0000 Uiso . . . . . . C48 C -0.0244(10) 0.6144(8) 0.3207(8) 0.061(4) 1.0000 Uiso . . . . . . C49 C 0.0184(9) 0.6668(7) 0.2707(7) 0.045(3) 1.0000 Uiso . . . . . . C50 C 0.3094(8) 0.6997(6) 0.2979(6) 0.034(3) 1.0000 Uiso . . . . . . C51 C 0.2544(9) 0.6393(7) 0.3110(7) 0.050(4) 1.0000 Uiso . . . . . . C52 C 0.2726(10) 0.5822(8) 0.3590(7) 0.053(4) 1.0000 Uiso . . . . . . C53 C 0.3438(9) 0.5862(7) 0.3918(7) 0.051(4) 1.0000 Uiso . . . . . . C54 C 0.3975(10) 0.6448(7) 0.3814(7) 0.052(4) 1.0000 Uiso . . . . . . C55 C 0.3825(9) 0.7024(7) 0.3343(7) 0.048(4) 1.0000 Uiso . . . . . . C56 C 0.4102(8) 0.7756(6) 0.1834(6) 0.038(3) 1.0000 Uiso . . . . . . C57 C 0.4786(9) 0.8264(7) 0.1864(7) 0.046(4) 1.0000 Uiso . . . . . . C58 C 0.5655(10) 0.8286(8) 0.1449(8) 0.060(4) 1.0000 Uiso . . . . . . C59 C 0.5806(11) 0.7832(8) 0.1025(8) 0.067(4) 1.0000 Uiso . . . . . . C60 C 0.5171(10) 0.7330(8) 0.0983(8) 0.062(4) 1.0000 Uiso . . . . . . C61 C 0.4316(9) 0.7287(7) 0.1400(6) 0.043(3) 1.0000 Uiso . . . . . . C101 C 0.5759(8) 0.5025(6) 0.1464(6) 0.030(3) 1.0000 Uiso . . . . . . C102 C 0.5428(9) 0.5191(6) 0.0862(7) 0.042(3) 1.0000 Uiso . . . . . . C103 C 0.4520(9) 0.5380(6) 0.0838(7) 0.043(3) 1.0000 Uiso . . . . . . C104 C 0.3919(10) 0.5414(7) 0.1390(7) 0.051(4) 1.0000 Uiso . . . . . . C105 C 0.4214(9) 0.5273(7) 0.1998(7) 0.048(4) 1.0000 Uiso . . . . . . C106 C 0.5136(8) 0.5097(6) 0.2012(6) 0.033(3) 1.0000 Uiso . . . . . . C107 C 0.5967(8) 0.5469(6) 0.2796(6) 0.031(3) 1.0000 Uiso . . . . . . C108 C 0.5848(9) 0.6183(6) 0.2587(6) 0.041(3) 1.0000 Uiso . . . . . . C109 C 0.6423(9) 0.6659(7) 0.2765(7) 0.051(4) 1.0000 Uiso . . . . . . C110 C 0.7065(9) 0.6434(7) 0.3160(7) 0.048(4) 1.0000 Uiso . . . . . . C111 C 0.7159(9) 0.5720(7) 0.3371(7) 0.044(3) 1.0000 Uiso . . . . . . C112 C 0.6603(8) 0.5220(6) 0.3181(6) 0.033(3) 1.0000 Uiso . . . . . . C113 C 0.7249(8) 0.4381(6) 0.0731(6) 0.032(3) 1.0000 Uiso . . . . . . C114 C 0.6774(9) 0.3835(6) 0.0563(6) 0.039(3) 1.0000 Uiso . . . . . . C115 C 0.7050(9) 0.3585(7) -0.0019(6) 0.041(3) 1.0000 Uiso . . . . . . C116 C 0.7803(9) 0.3866(7) -0.0429(7) 0.052(4) 1.0000 Uiso . . . . . . C117 C 0.8302(9) 0.4422(7) -0.0299(7) 0.048(4) 1.0000 Uiso . . . . . . C118 C 0.8020(8) 0.4674(6) 0.0288(6) 0.040(3) 1.0000 Uiso . . . . . . C119 C 0.7664(8) 0.5408(6) 0.1468(6) 0.032(3) 1.0000 Uiso . . . . . . C120 C 0.7432(9) 0.6090(6) 0.1248(6) 0.040(3) 1.0000 Uiso . . . . . . C121 C 0.8071(9) 0.6650(7) 0.1176(7) 0.050(4) 1.0000 Uiso . . . . . . C122 C 0.8937(9) 0.6505(7) 0.1319(7) 0.050(4) 1.0000 Uiso . . . . . . C123 C 0.9202(9) 0.5838(7) 0.1537(7) 0.047(3) 1.0000 Uiso . . . . . . C124 C 0.8547(8) 0.5284(6) 0.1619(6) 0.036(3) 1.0000 Uiso . . . . . . C125 C 0.7740(8) 0.4184(6) 0.3789(6) 0.032(3) 1.0000 Uiso . . . . . . C126 C 0.8621(8) 0.4297(6) 0.3443(7) 0.040(3) 1.0000 Uiso . . . . . . C127 C 0.9404(10) 0.4207(7) 0.3736(7) 0.049(4) 1.0000 Uiso . . . . . . C128 C 0.9300(10) 0.4012(7) 0.4400(8) 0.057(4) 1.0000 Uiso . . . . . . C129 C 0.8436(11) 0.3879(9) 0.4767(9) 0.074(5) 1.0000 Uiso . . . . . . C130 C 0.7641(10) 0.3973(7) 0.4460(7) 0.055(4) 1.0000 Uiso . . . . . . C131 C 0.5768(7) 0.3945(6) 0.3990(6) 0.026(3) 1.0000 Uiso . . . . . . C132 C 0.5610(8) 0.3230(6) 0.4153(6) 0.039(3) 1.0000 Uiso . . . . . . C133 C 0.4893(9) 0.2950(7) 0.4656(7) 0.047(4) 1.0000 Uiso . . . . . . C134 C 0.4329(9) 0.3395(7) 0.4971(7) 0.043(3) 1.0000 Uiso . . . . . . C135 C 0.4463(9) 0.4108(7) 0.4798(7) 0.047(4) 1.0000 Uiso . . . . . . C136 C 0.5191(8) 0.4391(7) 0.4316(6) 0.037(3) 1.0000 Uiso . . . . . . C137 C 0.7137(8) 0.2480(7) 0.1863(7) 0.038(3) 1.0000 Uiso . . . . . . C138 C 0.8391(8) 0.2294(6) 0.2797(6) 0.031(3) 1.0000 Uiso . . . . . . C139 C 0.8676(8) 0.1636(7) 0.2658(7) 0.043(3) 1.0000 Uiso . . . . . . C140 C 0.8914(9) 0.1125(7) 0.3139(7) 0.049(4) 1.0000 Uiso . . . . . . C141 C 0.8872(9) 0.1240(7) 0.3761(7) 0.044(3) 1.0000 Uiso . . . . . . C142 C 0.8611(9) 0.1891(7) 0.3903(7) 0.052(4) 1.0000 Uiso . . . . . . C143 C 0.8355(8) 0.2408(7) 0.3429(6) 0.040(3) 1.0000 Uiso . . . . . . C144 C 0.9019(8) 0.3106(6) 0.1531(6) 0.032(3) 1.0000 Uiso . . . . . . C145 C 0.9834(10) 0.3359(7) 0.1711(8) 0.054(4) 1.0000 Uiso . . . . . . C146 C 1.0602(11) 0.3559(8) 0.1228(8) 0.064(4) 1.0000 Uiso . . . . . . C147 C 1.0577(11) 0.3481(8) 0.0598(8) 0.065(4) 1.0000 Uiso . . . . . . C148 C 0.9816(10) 0.3247(7) 0.0414(8) 0.057(4) 1.0000 Uiso . . . . . . C149 C 0.9013(9) 0.3053(7) 0.0891(7) 0.044(3) 1.0000 Uiso . . . . . . C150 C 0.5619(8) 0.2023(6) 0.2950(6) 0.034(3) 1.0000 Uiso . . . . . . C151 C 0.4723(9) 0.2038(7) 0.3289(7) 0.051(4) 1.0000 Uiso . . . . . . C152 C 0.4345(11) 0.1474(8) 0.3768(8) 0.061(4) 1.0000 Uiso . . . . . . C153 C 0.4872(9) 0.0907(7) 0.3905(7) 0.051(4) 1.0000 Uiso . . . . . . C154 C 0.5755(10) 0.0874(7) 0.3594(7) 0.053(4) 1.0000 Uiso . . . . . . C155 C 0.6134(9) 0.1429(6) 0.3115(6) 0.037(3) 1.0000 Uiso . . . . . . C156 C 0.5174(8) 0.2781(6) 0.1788(6) 0.035(3) 1.0000 Uiso . . . . . . C157 C 0.5162(9) 0.2281(7) 0.1376(6) 0.043(3) 1.0000 Uiso . . . . . . C158 C 0.4498(10) 0.2326(8) 0.0959(7) 0.057(4) 1.0000 Uiso . . . . . . C159 C 0.3856(10) 0.2843(8) 0.0968(8) 0.060(4) 1.0000 Uiso . . . . . . C160 C 0.3836(11) 0.3331(8) 0.1392(8) 0.061(4) 1.0000 Uiso . . . . . . C161 C 0.4517(9) 0.3299(7) 0.1785(7) 0.047(4) 1.0000 Uiso . . . . . . C200 C 0.5563(14) 0.8911(10) 0.3679(10) 0.100(6) 1.0000 Uiso . . . . . . C300 C 0.252(2) 0.3673(14) 0.3884(14) 0.053(8) 0.5000 Uiso . . . . . . Cl1 Cl 0.5882(5) 0.8087(4) 0.3525(3) 0.132(2) 1.0000 Uiso . . . . . . Cl2 Cl 0.6013(4) 0.9013(3) 0.4437(3) 0.0954(15) 1.0000 Uiso . . . . . . Cl3 Cl 0.2241(10) 0.2836(7) 0.4001(7) 0.138(5) 0.5000 Uiso . . . . . . Cl4 Cl 0.1992(5) 0.4038(4) 0.4594(4) 0.061(2) 0.5000 Uiso . . . . . . B1 B 0.7705(11) 0.9943(8) 0.2246(8) 0.045(4) 1.0000 Uiso . . . . . . B2 B 0.1452(13) 0.4898(9) 0.2245(9) 0.057(5) 1.0000 Uiso . . . . . . F1 F 0.7237(7) 0.9458(5) 0.1984(5) 0.088(3) 1.0000 Uiso . . . . . . F2 F 0.7260(7) 0.9956(5) 0.2872(5) 0.086(3) 1.0000 Uiso . . . . . . F3 F 0.8601(6) 0.9728(4) 0.2273(4) 0.070(2) 1.0000 Uiso . . . . . . F4 F 0.7701(5) 1.0604(4) 0.1877(4) 0.062(2) 1.0000 Uiso . . . . . . F5 F 0.1591(7) 0.4823(6) 0.2883(6) 0.099(3) 1.0000 Uiso . . . . . . F6 F 0.2028(7) 0.4487(5) 0.1896(5) 0.093(3) 1.0000 Uiso . . . . . . F7 F 0.0539(6) 0.4719(4) 0.2241(4) 0.071(2) 1.0000 Uiso . . . . . . F8 F 0.1630(6) 0.5607(5) 0.1965(5) 0.074(3) 1.0000 Uiso . . . . . . H21 H 0.0746 1.0613 0.3561 0.0501 1.0000 Uiso R . . . . . H31 H 0.1054 1.1819 0.3185 0.0611 1.0000 Uiso R . . . . . H41 H 0.2475 1.2167 0.2552 0.0601 1.0000 Uiso R . . . . . H51 H 0.3608 1.1357 0.2329 0.0480 1.0000 Uiso R . . . . . H81 H 0.5152 1.0319 0.2460 0.0479 1.0000 Uiso R . . . . . H91 H 0.6201 1.0470 0.1478 0.0539 1.0000 Uiso R . . . . . H101 H 0.5688 1.0348 0.0527 0.0542 1.0000 Uiso R . . . . . H111 H 0.4153 1.0065 0.0522 0.0530 1.0000 Uiso R . . . . . H141 H 0.2504 0.8011 0.3892 0.0540 1.0000 Uiso R . . . . . H151 H 0.3312 0.7602 0.4740 0.0611 1.0000 Uiso R . . . . . H161 H 0.3833 0.8402 0.5319 0.0601 1.0000 Uiso R . . . . . H171 H 0.3454 0.9565 0.5106 0.0520 1.0000 Uiso R . . . . . H181 H 0.2625 0.9977 0.4282 0.0451 1.0000 Uiso R . . . . . H201 H -0.0034 0.9354 0.3023 0.0450 1.0000 Uiso R . . . . . H211 H -0.1559 0.9260 0.3545 0.0611 1.0000 Uiso R . . . . . H221 H -0.1857 0.9058 0.4678 0.0872 1.0000 Uiso R . . . . . H231 H -0.0640 0.8939 0.5274 0.1092 1.0000 Uiso R . . . . . H241 H 0.0890 0.9038 0.4721 0.0801 1.0000 Uiso R . . . . . H261 H 0.2778 1.1168 0.1116 0.0559 1.0000 Uiso R . . . . . H271 H 0.1789 1.2080 0.0914 0.0720 1.0000 Uiso R . . . . . H281 H 0.0198 1.1893 0.1194 0.0592 1.0000 Uiso R . . . . . H291 H -0.0381 1.0750 0.1586 0.0589 1.0000 Uiso R . . . . . H301 H 0.0598 0.9845 0.1797 0.0480 1.0000 Uiso R . . . . . H321 H 0.3554 0.8606 0.0884 0.0439 1.0000 Uiso R . . . . . H331 H 0.3489 0.8131 -0.0053 0.0510 1.0000 Uiso R . . . . . H341 H 0.2523 0.8594 -0.0758 0.0552 1.0000 Uiso R . . . . . H351 H 0.1639 0.9561 -0.0578 0.0590 1.0000 Uiso R . . . . . H361 H 0.1636 1.0011 0.0387 0.0481 1.0000 Uiso R . . . . . H371 H 0.2322 0.7643 0.1420 0.0422 1.0000 Uiso R . . . . . H372 H 0.2029 0.6969 0.1971 0.0422 1.0000 Uiso R . . . . . H391 H 0.1264 0.7906 0.0804 0.0559 1.0000 Uiso R . . . . . H401 H 0.0302 0.8215 0.0019 0.0750 1.0000 Uiso R . . . . . H411 H -0.1142 0.8625 0.0320 0.0760 1.0000 Uiso R . . . . . H421 H -0.1680 0.8686 0.1409 0.0790 1.0000 Uiso R . . . . . H431 H -0.0734 0.8361 0.2175 0.0629 1.0000 Uiso R . . . . . H451 H 0.0492 0.7850 0.3569 0.0639 1.0000 Uiso R . . . . . H461 H -0.0245 0.6961 0.4410 0.0891 1.0000 Uiso R . . . . . H471 H -0.0675 0.5895 0.4155 0.0792 1.0000 Uiso R . . . . . H481 H -0.0426 0.5716 0.3110 0.0722 1.0000 Uiso R . . . . . H491 H 0.0284 0.6593 0.2278 0.0541 1.0000 Uiso R . . . . . H511 H 0.2055 0.6361 0.2882 0.0599 1.0000 Uiso R . . . . . H521 H 0.2347 0.5419 0.3681 0.0641 1.0000 Uiso R . . . . . H531 H 0.3562 0.5474 0.4222 0.0621 1.0000 Uiso R . . . . . H541 H 0.4451 0.6475 0.4056 0.0641 1.0000 Uiso R . . . . . H551 H 0.4204 0.7426 0.3267 0.0590 1.0000 Uiso R . . . . . H571 H 0.4664 0.8584 0.2154 0.0560 1.0000 Uiso R . . . . . H581 H 0.6114 0.8610 0.1474 0.0720 1.0000 Uiso R . . . . . H591 H 0.6371 0.7864 0.0743 0.0801 1.0000 Uiso R . . . . . H601 H 0.5300 0.7023 0.0683 0.0740 1.0000 Uiso R . . . . . H611 H 0.3885 0.6939 0.1385 0.0519 1.0000 Uiso R . . . . . H1021 H 0.5831 0.5171 0.0476 0.0509 1.0000 Uiso R . . . . . H1031 H 0.4324 0.5488 0.0433 0.0521 1.0000 Uiso R . . . . . H1041 H 0.3304 0.5531 0.1367 0.0611 1.0000 Uiso R . . . . . H1051 H 0.3807 0.5296 0.2385 0.0579 1.0000 Uiso R . . . . . H1081 H 0.5389 0.6334 0.2336 0.0501 1.0000 Uiso R . . . . . H1091 H 0.6378 0.7140 0.2611 0.0621 1.0000 Uiso R . . . . . H1101 H 0.7441 0.6761 0.3285 0.0571 1.0000 Uiso R . . . . . H1111 H 0.7594 0.5569 0.3639 0.0531 1.0000 Uiso R . . . . . H1141 H 0.6254 0.3634 0.0850 0.0479 1.0000 Uiso R . . . . . H1151 H 0.6706 0.3226 -0.0121 0.0491 1.0000 Uiso R . . . . . H1161 H 0.7999 0.3684 -0.0810 0.0632 1.0000 Uiso R . . . . . H1171 H 0.8816 0.4625 -0.0593 0.0580 1.0000 Uiso R . . . . . H1181 H 0.8353 0.5044 0.0383 0.0481 1.0000 Uiso R . . . . . H1201 H 0.6843 0.6181 0.1145 0.0490 1.0000 Uiso R . . . . . H1211 H 0.7904 0.7112 0.1032 0.0609 1.0000 Uiso R . . . . . H1221 H 0.9363 0.6876 0.1264 0.0601 1.0000 Uiso R . . . . . H1231 H 0.9796 0.5748 0.1629 0.0560 1.0000 Uiso R . . . . . H1241 H 0.8705 0.4829 0.1778 0.0439 1.0000 Uiso R . . . . . H1261 H 0.8693 0.4440 0.2991 0.0480 1.0000 Uiso R . . . . . H1271 H 0.9995 0.4276 0.3483 0.0590 1.0000 Uiso R . . . . . H1281 H 0.9822 0.3970 0.4604 0.0683 1.0000 Uiso R . . . . . H1291 H 0.8374 0.3726 0.5216 0.0891 1.0000 Uiso R . . . . . H1301 H 0.7051 0.3891 0.4706 0.0661 1.0000 Uiso R . . . . . H1321 H 0.5983 0.2928 0.3928 0.0471 1.0000 Uiso R . . . . . H1331 H 0.4805 0.2461 0.4774 0.0571 1.0000 Uiso R . . . . . H1341 H 0.3852 0.3213 0.5307 0.0520 1.0000 Uiso R . . . . . H1351 H 0.4067 0.4409 0.5005 0.0571 1.0000 Uiso R . . . . . H1361 H 0.5294 0.4880 0.4211 0.0460 1.0000 Uiso R . . . . . H1371 H 0.7206 0.1972 0.1958 0.0460 1.0000 Uiso R . . . . . H1372 H 0.7168 0.2635 0.1396 0.0460 1.0000 Uiso R . . . . . H1391 H 0.8704 0.1543 0.2234 0.0522 1.0000 Uiso R . . . . . H1401 H 0.9107 0.0689 0.3037 0.0590 1.0000 Uiso R . . . . . H1411 H 0.9017 0.0881 0.4086 0.0542 1.0000 Uiso R . . . . . H1421 H 0.8607 0.1985 0.4324 0.0622 1.0000 Uiso R . . . . . H1431 H 0.8158 0.2839 0.3538 0.0490 1.0000 Uiso R . . . . . H1451 H 0.9854 0.3388 0.2147 0.0649 1.0000 Uiso R . . . . . H1461 H 1.1132 0.3744 0.1338 0.0770 1.0000 Uiso R . . . . . H1471 H 1.1110 0.3592 0.0285 0.0770 1.0000 Uiso R . . . . . H1481 H 0.9808 0.3210 -0.0020 0.0680 1.0000 Uiso R . . . . . H1491 H 0.8481 0.2888 0.0767 0.0540 1.0000 Uiso R . . . . . H1511 H 0.4369 0.2431 0.3193 0.0608 1.0000 Uiso R . . . . . H1521 H 0.3741 0.1493 0.3987 0.0741 1.0000 Uiso R . . . . . H1531 H 0.4621 0.0530 0.4224 0.0611 1.0000 Uiso R . . . . . H1541 H 0.6110 0.0479 0.3700 0.0639 1.0000 Uiso R . . . . . H1551 H 0.6741 0.1401 0.2905 0.0449 1.0000 Uiso R . . . . . H1571 H 0.5592 0.1923 0.1379 0.0518 1.0000 Uiso R . . . . . H1581 H 0.4500 0.2003 0.0676 0.0681 1.0000 Uiso R . . . . . H1591 H 0.3421 0.2873 0.0686 0.0721 1.0000 Uiso R . . . . . H1601 H 0.3379 0.3670 0.1410 0.0742 1.0000 Uiso R . . . . . H1611 H 0.4530 0.3632 0.2053 0.0570 1.0000 Uiso R . . . . . H2001 H 0.5860 0.9263 0.3323 0.1162 1.0000 Uiso R . . . . . H2002 H 0.4892 0.8950 0.3716 0.1154 1.0000 Uiso R . . . . . H3001 H 0.3191 0.3747 0.3794 0.0628 0.5000 Uiso R . . . . . H3002 H 0.2273 0.3908 0.3509 0.0631 0.5000 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 0.0409(10) 0.0264(8) 0.0239(10) -0.0062(7) -0.0056(7) -0.0029(7) Cu2 0.0384(9) 0.0258(8) 0.0243(10) -0.0047(7) -0.0063(7) 0.0020(7) P1 0.036(2) 0.0319(18) 0.024(2) -0.0061(15) -0.0057(15) -0.0002(15) P2 0.040(2) 0.0279(17) 0.0224(19) -0.0043(14) -0.0067(15) -0.0027(14) P3 0.039(2) 0.0306(18) 0.028(2) -0.0074(15) -0.0066(16) -0.0014(15) P4 0.040(2) 0.0316(18) 0.029(2) -0.0067(15) -0.0092(15) 0.0040(15) P101 0.0379(19) 0.0282(17) 0.024(2) -0.0072(14) -0.0080(15) 0.0016(14) P102 0.039(2) 0.0281(18) 0.023(2) -0.0058(15) -0.0052(15) 0.0019(14) P103 0.0359(19) 0.0291(17) 0.025(2) -0.0052(14) -0.0057(15) 0.0025(14) P104 0.038(2) 0.0291(18) 0.030(2) -0.0070(15) -0.0080(15) -0.0016(14) _refine_ls_extinction_method None 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 . 2.279(4) yes Cu1 . P2 . 2.304(3) yes Cu1 . P3 . 2.333(3) yes Cu1 . P4 . 2.425(4) yes Cu2 . P101 . 2.294(3) yes Cu2 . P102 . 2.268(4) yes Cu2 . P103 . 2.339(4) yes Cu2 . P104 . 2.409(3) yes P1 . C1 . 1.811(11) yes P1 . C13 . 1.808(12) yes P1 . C19 . 1.817(12) yes P2 . C12 . 1.816(11) yes P2 . C25 . 1.801(12) yes P2 . C31 . 1.839(13) yes P3 . C37 . 1.849(12) yes P3 . C38 . 1.819(12) yes P3 . C44 . 1.819(12) yes P4 . C37 . 1.850(12) yes P4 . C50 . 1.801(12) yes P4 . C56 . 1.818(13) yes P101 . C101 . 1.818(11) yes P101 . C113 . 1.834(13) yes P101 . C119 . 1.810(12) yes P102 . C112 . 1.824(12) yes P102 . C125 . 1.820(12) yes P102 . C131 . 1.824(11) yes P103 . C137 . 1.829(12) yes P103 . C138 . 1.819(12) yes P103 . C144 . 1.822(12) yes P104 . C137 . 1.865(13) yes P104 . C150 . 1.816(12) yes P104 . C156 . 1.818(12) yes O1 . C6 . 1.403(14) yes O1 . C7 . 1.416(14) yes O101 . C106 . 1.400(14) yes O101 . C107 . 1.412(13) yes C1 . C2 . 1.380(16) yes C1 . C6 . 1.389(16) yes C2 . C3 . 1.412(17) yes C2 . H21 . 0.927 no C3 . C4 . 1.375(18) yes C3 . H31 . 0.935 no C4 . C5 . 1.378(17) yes C4 . H41 . 0.932 no C5 . C6 . 1.392(16) yes C5 . H51 . 0.928 no C7 . C8 . 1.396(16) yes C7 . C12 . 1.384(16) yes C8 . C9 . 1.385(17) yes C8 . H81 . 0.933 no C9 . C10 . 1.370(17) yes C9 . H91 . 0.933 no C10 . C11 . 1.397(17) yes C10 . H101 . 0.928 no C11 . C12 . 1.392(17) yes C11 . H111 . 0.930 no C13 . C14 . 1.394(16) yes C13 . C18 . 1.397(16) yes C14 . C15 . 1.389(18) yes C14 . H141 . 0.929 no C15 . C16 . 1.381(18) yes C15 . H151 . 0.932 no C16 . C17 . 1.362(17) yes C16 . H161 . 0.933 no C17 . C18 . 1.379(17) yes C17 . H171 . 0.932 no C18 . H181 . 0.933 no C19 . C20 . 1.383(16) yes C19 . C24 . 1.370(19) yes C20 . C21 . 1.389(18) yes C20 . H201 . 0.932 no C21 . C22 . 1.38(2) yes C21 . H211 . 0.935 no C22 . C23 . 1.39(2) yes C22 . H221 . 0.930 no C23 . C24 . 1.41(2) yes C23 . H231 . 0.926 no C24 . H241 . 0.930 no C25 . C26 . 1.392(16) yes C25 . C30 . 1.400(16) yes C26 . C27 . 1.375(18) yes C26 . H261 . 0.928 no C27 . C28 . 1.376(18) yes C27 . H271 . 0.937 no C28 . C29 . 1.385(18) yes C28 . H281 . 0.935 no C29 . C30 . 1.368(17) yes C29 . H291 . 0.926 no C30 . H301 . 0.927 no C31 . C32 . 1.406(16) yes C31 . C36 . 1.382(16) yes C32 . C33 . 1.404(17) yes C32 . H321 . 0.929 no C33 . C34 . 1.345(17) yes C33 . H331 . 0.930 no C34 . C35 . 1.380(18) yes C34 . H341 . 0.933 no C35 . C36 . 1.409(18) yes C35 . H351 . 0.933 no C36 . H361 . 0.930 no C37 . H371 . 0.971 no C37 . H372 . 0.974 no C38 . C39 . 1.374(17) yes C38 . C43 . 1.369(18) yes C39 . C40 . 1.410(19) yes C39 . H391 . 0.928 no C40 . C41 . 1.345(19) yes C40 . H401 . 0.932 no C41 . C42 . 1.39(2) yes C41 . H411 . 0.932 no C42 . C43 . 1.38(2) yes C42 . H421 . 0.929 no C43 . H431 . 0.928 no C44 . C45 . 1.351(18) yes C44 . C49 . 1.382(17) yes C45 . C46 . 1.42(2) yes C45 . H451 . 0.930 no C46 . C47 . 1.38(2) yes C46 . H461 . 0.932 no C47 . C48 . 1.33(2) yes C47 . H471 . 0.933 no C48 . C49 . 1.394(19) yes C48 . H481 . 0.932 no C49 . H491 . 0.926 no C50 . C51 . 1.378(17) yes C50 . C55 . 1.416(17) yes C51 . C52 . 1.414(18) yes C51 . H511 . 0.929 no C52 . C53 . 1.347(18) yes C52 . H521 . 0.928 no C53 . C54 . 1.341(18) yes C53 . H531 . 0.932 no C54 . C55 . 1.395(18) yes C54 . H541 . 0.932 no C55 . H551 . 0.929 no C56 . C57 . 1.416(17) yes C56 . C61 . 1.390(17) yes C57 . C58 . 1.416(19) yes C57 . H571 . 0.933 no C58 . C59 . 1.34(2) yes C58 . H581 . 0.931 no C59 . C60 . 1.365(19) yes C59 . H591 . 0.931 no C60 . C61 . 1.399(19) yes C60 . H601 . 0.934 no C61 . H611 . 0.929 no C101 . C102 . 1.413(17) yes C101 . C106 . 1.373(16) yes C102 . C103 . 1.380(17) yes C102 . H1021 . 0.928 no C103 . C104 . 1.349(18) yes C103 . H1031 . 0.932 no C104 . C105 . 1.398(18) yes C104 . H1041 . 0.931 no C105 . C106 . 1.392(17) yes C105 . H1051 . 0.934 no C107 . C108 . 1.385(16) yes C107 . C112 . 1.361(16) yes C108 . C109 . 1.382(17) yes C108 . H1081 . 0.934 no C109 . C110 . 1.372(18) yes C109 . H1091 . 0.931 no C110 . C111 . 1.381(17) yes C110 . H1101 . 0.933 no C111 . C112 . 1.409(17) yes C111 . H1111 . 0.930 no C113 . C114 . 1.386(16) yes C113 . C118 . 1.393(17) yes C114 . C115 . 1.391(17) yes C114 . H1141 . 0.930 no C115 . C116 . 1.336(18) yes C115 . H1151 . 0.928 no C116 . C117 . 1.387(18) yes C116 . H1161 . 0.930 no C117 . C118 . 1.402(18) yes C117 . H1171 . 0.932 no C118 . H1181 . 0.930 no C119 . C120 . 1.372(16) yes C119 . C124 . 1.388(16) yes C120 . C121 . 1.401(17) yes C120 . H1201 . 0.929 no C121 . C122 . 1.362(18) yes C121 . H1211 . 0.933 no C122 . C123 . 1.363(17) yes C122 . H1221 . 0.928 no C123 . C124 . 1.404(17) yes C123 . H1231 . 0.928 no C124 . H1241 . 0.924 no C125 . C126 . 1.371(16) yes C125 . C130 . 1.383(18) yes C126 . C127 . 1.381(17) yes C126 . H1261 . 0.931 no C127 . C128 . 1.366(19) yes C127 . H1271 . 0.935 no C128 . C129 . 1.37(2) yes C128 . H1281 . 0.929 no C129 . C130 . 1.41(2) yes C129 . H1291 . 0.929 no C130 . H1301 . 0.930 no C131 . C132 . 1.369(15) yes C131 . C136 . 1.387(16) yes C132 . C133 . 1.399(18) yes C132 . H1321 . 0.929 no C133 . C134 . 1.363(18) yes C133 . H1331 . 0.934 no C134 . C135 . 1.363(17) yes C134 . H1341 . 0.930 no C135 . C136 . 1.387(18) yes C135 . H1351 . 0.929 no C136 . H1361 . 0.934 no C137 . H1371 . 0.971 no C137 . H1372 . 0.969 no C138 . C139 . 1.394(17) yes C138 . C143 . 1.377(17) yes C139 . C140 . 1.370(18) yes C139 . H1391 . 0.933 no C140 . C141 . 1.356(18) yes C140 . H1401 . 0.931 no C141 . C142 . 1.372(18) yes C141 . H1411 . 0.933 no C142 . C143 . 1.377(17) yes C142 . H1421 . 0.934 no C143 . H1431 . 0.928 no C144 . C145 . 1.419(17) yes C144 . C149 . 1.368(17) yes C145 . C146 . 1.39(2) yes C145 . H1451 . 0.933 no C146 . C147 . 1.37(2) yes C146 . H1461 . 0.932 no C147 . C148 . 1.340(19) yes C147 . H1471 . 0.935 no C148 . C149 . 1.421(19) yes C148 . H1481 . 0.928 no C149 . H1491 . 0.932 no C150 . C151 . 1.388(17) yes C150 . C155 . 1.388(16) yes C151 . C152 . 1.396(19) yes C151 . H1511 . 0.925 no C152 . C153 . 1.347(18) yes C152 . H1521 . 0.931 no C153 . C154 . 1.356(18) yes C153 . H1531 . 0.931 no C154 . C155 . 1.385(18) yes C154 . H1541 . 0.933 no C155 . H1551 . 0.930 no C156 . C157 . 1.401(17) yes C156 . C161 . 1.379(17) yes C157 . C158 . 1.403(18) yes C157 . H1571 . 0.930 no C158 . C159 . 1.362(19) yes C158 . H1581 . 0.930 no C159 . C160 . 1.40(2) yes C159 . H1591 . 0.933 no C160 . C161 . 1.387(19) yes C160 . H1601 . 0.932 no C161 . H1611 . 0.926 no C200 . Cl1 . 1.72(2) yes C200 . Cl2 . 1.86(2) yes C200 . H2001 . 0.966 no C200 . H2002 . 0.974 no C300 . Cl3 . 1.63(3) yes C300 . Cl4 . 1.82(3) yes C300 . H3001 . 0.972 no C300 . H3002 . 0.961 no B1 . F1 . 1.395(18) yes B1 . F2 . 1.375(18) yes B1 . F3 . 1.377(17) yes B1 . F4 . 1.370(17) yes B2 . F5 . 1.37(2) yes B2 . F6 . 1.37(2) yes B2 . F7 . 1.380(18) yes B2 . F8 . 1.396(19) 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 . 110.51(13) yes P1 . Cu1 . P3 . 124.44(13) yes P2 . Cu1 . P3 . 109.77(13) yes P1 . Cu1 . P4 . 125.43(13) yes P2 . Cu1 . P4 . 108.26(13) yes P3 . Cu1 . P4 . 73.28(12) yes P101 . Cu2 . P102 . 111.20(12) yes P101 . Cu2 . P103 . 109.44(13) yes P102 . Cu2 . P103 . 124.03(13) yes P101 . Cu2 . P104 . 109.51(12) yes P102 . Cu2 . P104 . 123.63(13) yes P103 . Cu2 . P104 . 73.86(12) yes Cu1 . P1 . C1 . 111.1(4) yes Cu1 . P1 . C13 . 116.9(4) yes C1 . P1 . C13 . 104.0(5) yes Cu1 . P1 . C19 . 117.3(4) yes C1 . P1 . C19 . 103.0(5) yes C13 . P1 . C19 . 102.9(6) yes Cu1 . P2 . C12 . 113.9(4) yes Cu1 . P2 . C25 . 114.5(4) yes C12 . P2 . C25 . 105.9(5) yes Cu1 . P2 . C31 . 115.9(4) yes C12 . P2 . C31 . 103.6(5) yes C25 . P2 . C31 . 101.6(5) yes Cu1 . P3 . C37 . 90.0(4) yes Cu1 . P3 . C38 . 126.2(4) yes C37 . P3 . C38 . 107.4(6) yes Cu1 . P3 . C44 . 120.4(4) yes C37 . P3 . C44 . 103.8(6) yes C38 . P3 . C44 . 104.5(5) yes Cu1 . P4 . C37 . 87.2(4) yes Cu1 . P4 . C50 . 128.7(4) yes C37 . P4 . C50 . 105.5(6) yes Cu1 . P4 . C56 . 124.0(4) yes C37 . P4 . C56 . 105.3(6) yes C50 . P4 . C56 . 100.7(6) yes Cu2 . P101 . C101 . 113.7(4) yes Cu2 . P101 . C113 . 115.9(4) yes C101 . P101 . C113 . 103.1(5) yes Cu2 . P101 . C119 . 115.2(4) yes C101 . P101 . C119 . 105.3(5) yes C113 . P101 . C119 . 102.1(6) yes Cu2 . P102 . C112 . 111.0(4) yes Cu2 . P102 . C125 . 116.2(4) yes C112 . P102 . C125 . 103.0(5) yes Cu2 . P102 . C131 . 116.7(4) yes C112 . P102 . C131 . 104.5(5) yes C125 . P102 . C131 . 104.0(5) yes Cu2 . P103 . C137 . 90.0(4) yes Cu2 . P103 . C138 . 122.3(4) yes C137 . P103 . C138 . 104.0(6) yes Cu2 . P103 . C144 . 125.6(4) yes C137 . P103 . C144 . 107.0(6) yes C138 . P103 . C144 . 103.4(5) yes Cu2 . P104 . C137 . 87.0(4) yes Cu2 . P104 . C150 . 127.8(4) yes C137 . P104 . C150 . 105.7(6) yes Cu2 . P104 . C156 . 124.7(4) yes C137 . P104 . C156 . 106.2(6) yes C150 . P104 . C156 . 100.4(5) yes C6 . O1 . C7 . 116.6(9) yes C106 . O101 . C107 . 117.3(9) yes P1 . C1 . C2 . 125.2(9) yes P1 . C1 . C6 . 117.1(9) yes C2 . C1 . C6 . 117.4(11) yes C1 . C2 . C3 . 121.6(12) yes C1 . C2 . H21 . 119.6 no C3 . C2 . H21 . 118.8 no C2 . C3 . C4 . 117.9(13) yes C2 . C3 . H31 . 120.8 no C4 . C3 . H31 . 121.4 no C3 . C4 . C5 . 122.9(13) yes C3 . C4 . H41 . 118.8 no C5 . C4 . H41 . 118.3 no C4 . C5 . C6 . 117.1(12) yes C4 . C5 . H51 . 122.1 no C6 . C5 . H51 . 120.8 no O1 . C6 . C5 . 121.5(11) yes O1 . C6 . C1 . 115.4(10) yes C5 . C6 . C1 . 123.0(11) yes O1 . C7 . C8 . 115.3(10) yes O1 . C7 . C12 . 120.0(10) yes C8 . C7 . C12 . 124.5(11) yes C7 . C8 . C9 . 117.6(12) yes C7 . C8 . H81 . 120.9 no C9 . C8 . H81 . 121.6 no C8 . C9 . C10 . 119.8(12) yes C8 . C9 . H91 . 120.0 no C10 . C9 . H91 . 120.2 no C9 . C10 . C11 . 121.3(13) yes C9 . C10 . H101 . 119.3 no C11 . C10 . H101 . 119.4 no C10 . C11 . C12 . 120.8(12) yes C10 . C11 . H111 . 119.6 no C12 . C11 . H111 . 119.6 no P2 . C12 . C11 . 122.9(9) yes P2 . C12 . C7 . 121.0(9) yes C11 . C12 . C7 . 115.9(11) yes P1 . C13 . C14 . 119.1(9) yes P1 . C13 . C18 . 122.9(9) yes C14 . C13 . C18 . 118.0(11) yes C13 . C14 . C15 . 121.5(13) yes C13 . C14 . H141 . 119.1 no C15 . C14 . H141 . 119.4 no C14 . C15 . C16 . 118.9(13) yes C14 . C15 . H151 . 120.6 no C16 . C15 . H151 . 120.4 no C15 . C16 . C17 . 120.3(13) yes C15 . C16 . H161 . 120.0 no C17 . C16 . H161 . 119.7 no C16 . C17 . C18 . 121.3(13) yes C16 . C17 . H171 . 119.6 no C18 . C17 . H171 . 119.0 no C13 . C18 . C17 . 120.0(12) yes C13 . C18 . H181 . 119.8 no C17 . C18 . H181 . 120.2 no P1 . C19 . C20 . 119.9(10) yes P1 . C19 . C24 . 122.2(10) yes C20 . C19 . C24 . 117.8(12) yes C19 . C20 . C21 . 123.0(13) yes C19 . C20 . H201 . 118.2 no C21 . C20 . H201 . 118.7 no C20 . C21 . C22 . 118.2(14) yes C20 . C21 . H211 . 120.6 no C22 . C21 . H211 . 121.2 no C21 . C22 . C23 . 120.9(17) yes C21 . C22 . H221 . 119.3 no C23 . C22 . H221 . 119.8 no C22 . C23 . C24 . 119.0(20) yes C22 . C23 . H231 . 120.8 no C24 . C23 . H231 . 120.2 no C23 . C24 . C19 . 121.0(16) yes C23 . C24 . H241 . 119.4 no C19 . C24 . H241 . 119.5 no P2 . C25 . C26 . 123.6(9) yes P2 . C25 . C30 . 119.2(9) yes C26 . C25 . C30 . 117.1(11) yes C25 . C26 . C27 . 121.2(13) yes C25 . C26 . H261 . 119.3 no C27 . C26 . H261 . 119.5 no C26 . C27 . C28 . 120.8(14) yes C26 . C27 . H271 . 119.4 no C28 . C27 . H271 . 119.9 no C27 . C28 . C29 . 119.0(13) yes C27 . C28 . H281 . 120.5 no C29 . C28 . H281 . 120.5 no C28 . C29 . C30 . 120.3(13) yes C28 . C29 . H291 . 119.9 no C30 . C29 . H291 . 119.7 no C25 . C30 . C29 . 121.5(12) yes C25 . C30 . H301 . 119.6 no C29 . C30 . H301 . 118.9 no P2 . C31 . C32 . 118.9(9) yes P2 . C31 . C36 . 122.5(9) yes C32 . C31 . C36 . 118.5(12) yes C31 . C32 . C33 . 120.1(12) yes C31 . C32 . H321 . 119.9 no C33 . C32 . H321 . 120.0 no C32 . C33 . C34 . 119.9(13) yes C32 . C33 . H331 . 119.5 no C34 . C33 . H331 . 120.7 no C33 . C34 . C35 . 121.7(14) yes C33 . C34 . H341 . 119.4 no C35 . C34 . H341 . 118.9 no C34 . C35 . C36 . 119.0(13) yes C34 . C35 . H351 . 120.7 no C36 . C35 . H351 . 120.3 no C35 . C36 . C31 . 120.6(12) yes C35 . C36 . H361 . 119.5 no C31 . C36 . H361 . 120.0 no P4 . C37 . P3 . 100.4(6) yes P4 . C37 . H371 . 111.0 no P3 . C37 . H371 . 110.9 no P4 . C37 . H372 . 111.6 no P3 . C37 . H372 . 112.7 no H371 . C37 . H372 . 109.8 no P3 . C38 . C39 . 123.8(10) yes P3 . C38 . C43 . 118.0(11) yes C39 . C38 . C43 . 117.9(13) yes C38 . C39 . C40 . 120.9(13) yes C38 . C39 . H391 . 119.7 no C40 . C39 . H391 . 119.5 no C39 . C40 . C41 . 119.6(16) yes C39 . C40 . H401 . 120.1 no C41 . C40 . H401 . 120.3 no C40 . C41 . C42 . 120.5(16) yes C40 . C41 . H411 . 119.8 no C42 . C41 . H411 . 119.7 no C41 . C42 . C43 . 119.1(16) yes C41 . C42 . H421 . 120.7 no C43 . C42 . H421 . 120.3 no C42 . C43 . C38 . 122.2(16) yes C42 . C43 . H431 . 118.8 no C38 . C43 . H431 . 119.0 no P3 . C44 . C45 . 119.8(10) yes P3 . C44 . C49 . 119.8(10) yes C45 . C44 . C49 . 120.2(12) yes C44 . C45 . C46 . 119.2(14) yes C44 . C45 . H451 . 120.4 no C46 . C45 . H451 . 120.3 no C45 . C46 . C47 . 119.4(17) yes C45 . C46 . H461 . 120.1 no C47 . C46 . H461 . 120.5 no C46 . C47 . C48 . 120.6(17) yes C46 . C47 . H471 . 119.8 no C48 . C47 . H471 . 119.6 no C47 . C48 . C49 . 120.4(15) yes C47 . C48 . H481 . 119.7 no C49 . C48 . H481 . 119.9 no C48 . C49 . C44 . 120.1(14) yes C48 . C49 . H491 . 120.1 no C44 . C49 . H491 . 119.8 no P4 . C50 . C51 . 125.1(10) yes P4 . C50 . C55 . 116.8(9) yes C51 . C50 . C55 . 118.0(12) yes C50 . C51 . C52 . 119.8(13) yes C50 . C51 . H511 . 120.1 no C52 . C51 . H511 . 120.2 no C51 . C52 . C53 . 120.5(14) yes C51 . C52 . H521 . 119.4 no C53 . C52 . H521 . 120.1 no C52 . C53 . C54 . 121.3(14) yes C52 . C53 . H531 . 119.3 no C54 . C53 . H531 . 119.4 no C53 . C54 . C55 . 120.3(14) yes C53 . C54 . H541 . 120.4 no C55 . C54 . H541 . 119.3 no C50 . C55 . C54 . 120.1(13) yes C50 . C55 . H551 . 119.9 no C54 . C55 . H551 . 120.0 no P4 . C56 . C57 . 118.6(10) yes P4 . C56 . C61 . 123.0(10) yes C57 . C56 . C61 . 118.4(12) yes C56 . C57 . C58 . 119.5(14) yes C56 . C57 . H571 . 120.3 no C58 . C57 . H571 . 120.1 no C57 . C58 . C59 . 119.1(15) yes C57 . C58 . H581 . 120.1 no C59 . C58 . H581 . 120.8 no C58 . C59 . C60 . 123.4(16) yes C58 . C59 . H591 . 118.3 no C60 . C59 . H591 . 118.3 no C59 . C60 . C61 . 118.5(15) yes C59 . C60 . H601 . 121.0 no C61 . C60 . H601 . 120.4 no C60 . C61 . C56 . 121.0(13) yes C60 . C61 . H611 . 119.3 no C56 . C61 . H611 . 119.7 no P101 . C101 . C102 . 122.5(9) yes P101 . C101 . C106 . 121.3(9) yes C102 . C101 . C106 . 115.9(11) yes C101 . C102 . C103 . 121.3(12) yes C101 . C102 . H1021 . 119.1 no C103 . C102 . H1021 . 119.7 no C102 . C103 . C104 . 121.0(13) yes C102 . C103 . H1031 . 119.1 no C104 . C103 . H1031 . 119.9 no C103 . C104 . C105 . 120.3(13) yes C103 . C104 . H1041 . 120.0 no C105 . C104 . H1041 . 119.7 no C104 . C105 . C106 . 117.9(13) yes C104 . C105 . H1051 . 121.4 no C106 . C105 . H1051 . 120.7 no O101 . C106 . C105 . 116.4(11) yes O101 . C106 . C101 . 119.9(10) yes C105 . C106 . C101 . 123.6(11) yes O101 . C107 . C108 . 120.9(10) yes O101 . C107 . C112 . 116.1(10) yes C108 . C107 . C112 . 123.0(11) yes C107 . C108 . C109 . 118.0(12) yes C107 . C108 . H1081 . 120.6 no C109 . C108 . H1081 . 121.4 no C108 . C109 . C110 . 121.0(13) yes C108 . C109 . H1091 . 119.5 no C110 . C109 . H1091 . 119.5 no C109 . C110 . C111 . 119.8(13) yes C109 . C110 . H1101 . 120.4 no C111 . C110 . H1101 . 119.9 no C110 . C111 . C112 . 120.5(12) yes C110 . C111 . H1111 . 119.6 no C112 . C111 . H1111 . 119.9 no P102 . C112 . C111 . 124.2(9) yes P102 . C112 . C107 . 118.0(9) yes C111 . C112 . C107 . 117.6(11) yes P101 . C113 . C114 . 120.2(9) yes P101 . C113 . C118 . 122.7(9) yes C114 . C113 . C118 . 117.0(12) yes C113 . C114 . C115 . 122.0(12) yes C113 . C114 . H1141 . 118.5 no C115 . C114 . H1141 . 119.6 no C114 . C115 . C116 . 119.7(13) yes C114 . C115 . H1151 . 119.6 no C116 . C115 . H1151 . 120.7 no C115 . C116 . C117 . 121.5(15) yes C115 . C116 . H1161 . 119.4 no C117 . C116 . H1161 . 119.2 no C116 . C117 . C118 . 118.6(13) yes C116 . C117 . H1171 . 121.0 no C118 . C117 . H1171 . 120.4 no C117 . C118 . C113 . 121.2(12) yes C117 . C118 . H1181 . 119.4 no C113 . C118 . H1181 . 119.4 no P101 . C119 . C120 . 123.1(9) yes P101 . C119 . C124 . 118.3(9) yes C120 . C119 . C124 . 118.6(11) yes C119 . C120 . C121 . 120.9(12) yes C119 . C120 . H1201 . 119.5 no C121 . C120 . H1201 . 119.7 no C120 . C121 . C122 . 118.9(13) yes C120 . C121 . H1211 . 120.2 no C122 . C121 . H1211 . 120.9 no C121 . C122 . C123 . 122.6(13) yes C121 . C122 . H1221 . 118.8 no C123 . C122 . H1221 . 118.7 no C122 . C123 . C124 . 117.9(12) yes C122 . C123 . H1231 . 121.5 no C124 . C123 . H1231 . 120.6 no C123 . C124 . C119 . 121.3(11) yes C123 . C124 . H1241 . 119.6 no C119 . C124 . H1241 . 119.2 no P102 . C125 . C126 . 119.6(10) yes P102 . C125 . C130 . 122.2(10) yes C126 . C125 . C130 . 118.1(12) yes C125 . C126 . C127 . 122.6(13) yes C125 . C126 . H1261 . 118.5 no C127 . C126 . H1261 . 118.9 no C126 . C127 . C128 . 119.0(14) yes C126 . C127 . H1271 . 120.3 no C128 . C127 . H1271 . 120.7 no C127 . C128 . C129 . 120.6(15) yes C127 . C128 . H1281 . 119.6 no C129 . C128 . H1281 . 119.8 no C128 . C129 . C130 . 119.7(17) yes C128 . C129 . H1291 . 120.1 no C130 . C129 . H1291 . 120.2 no C129 . C130 . C125 . 119.9(14) yes C129 . C130 . H1301 . 120.3 no C125 . C130 . H1301 . 119.8 no P102 . C131 . C132 . 117.9(9) yes P102 . C131 . C136 . 122.8(9) yes C132 . C131 . C136 . 119.2(11) yes C131 . C132 . C133 . 120.5(12) yes C131 . C132 . H1321 . 119.7 no C133 . C132 . H1321 . 119.8 no C132 . C133 . C134 . 119.7(13) yes C132 . C133 . H1331 . 119.9 no C134 . C133 . H1331 . 120.4 no C133 . C134 . C135 . 120.2(13) yes C133 . C134 . H1341 . 120.2 no C135 . C134 . H1341 . 119.7 no C134 . C135 . C136 . 120.8(13) yes C134 . C135 . H1351 . 119.9 no C136 . C135 . H1351 . 119.3 no C131 . C136 . C135 . 119.6(12) yes C131 . C136 . H1361 . 120.0 no C135 . C136 . H1361 . 120.4 no P104 . C137 . P103 . 101.2(6) yes P104 . C137 . H1371 . 112.2 no P103 . C137 . H1371 . 111.9 no P104 . C137 . H1372 . 110.5 no P103 . C137 . H1372 . 110.7 no H1371 . C137 . H1372 . 110.1 no P103 . C138 . C139 . 120.5(10) yes P103 . C138 . C143 . 121.6(9) yes C139 . C138 . C143 . 117.8(12) yes C138 . C139 . C140 . 120.5(14) yes C138 . C139 . H1391 . 119.6 no C140 . C139 . H1391 . 119.9 no C139 . C140 . C141 . 121.4(14) yes C139 . C140 . H1401 . 119.4 no C141 . C140 . H1401 . 119.2 no C140 . C141 . C142 . 118.9(14) yes C140 . C141 . H1411 . 120.2 no C142 . C141 . H1411 . 120.9 no C141 . C142 . C143 . 120.7(14) yes C141 . C142 . H1421 . 119.8 no C143 . C142 . H1421 . 119.5 no C138 . C143 . C142 . 120.8(13) yes C138 . C143 . H1431 . 119.7 no C142 . C143 . H1431 . 119.5 no P103 . C144 . C145 . 116.0(10) yes P103 . C144 . C149 . 124.3(9) yes C145 . C144 . C149 . 119.4(12) yes C144 . C145 . C146 . 118.9(15) yes C144 . C145 . H1451 . 120.4 no C146 . C145 . H1451 . 120.6 no C145 . C146 . C147 . 120.0(16) yes C145 . C146 . H1461 . 119.7 no C147 . C146 . H1461 . 120.3 no C146 . C147 . C148 . 122.3(16) yes C146 . C147 . H1471 . 119.0 no C148 . C147 . H1471 . 118.7 no C147 . C148 . C149 . 119.2(15) yes C147 . C148 . H1481 . 120.9 no C149 . C148 . H1481 . 120.0 no C148 . C149 . C144 . 120.2(13) yes C148 . C149 . H1491 . 119.7 no C144 . C149 . H1491 . 120.1 no P104 . C150 . C151 . 118.4(10) yes P104 . C150 . C155 . 124.2(9) yes C151 . C150 . C155 . 117.4(12) yes C150 . C151 . C152 . 121.5(13) yes C150 . C151 . H1511 . 119.1 no C152 . C151 . H1511 . 119.4 no C151 . C152 . C153 . 118.7(15) yes C151 . C152 . H1521 . 120.2 no C153 . C152 . H1521 . 121.2 no C152 . C153 . C154 . 121.8(14) yes C152 . C153 . H1531 . 118.8 no C154 . C153 . H1531 . 119.3 no C153 . C154 . C155 . 119.9(14) yes C153 . C154 . H1541 . 120.5 no C155 . C154 . H1541 . 119.7 no C150 . C155 . C154 . 120.7(12) yes C150 . C155 . H1551 . 120.2 no C154 . C155 . H1551 . 119.1 no P104 . C156 . C157 . 121.8(9) yes P104 . C156 . C161 . 119.1(10) yes C157 . C156 . C161 . 119.1(12) yes C156 . C157 . C158 . 119.6(12) yes C156 . C157 . H1571 . 120.1 no C158 . C157 . H1571 . 120.3 no C157 . C158 . C159 . 119.9(15) yes C157 . C158 . H1581 . 119.7 no C159 . C158 . H1581 . 120.4 no C158 . C159 . C160 . 121.4(15) yes C158 . C159 . H1591 . 119.5 no C160 . C159 . H1591 . 119.2 no C159 . C160 . C161 . 118.3(15) yes C159 . C160 . H1601 . 121.0 no C161 . C160 . H1601 . 120.7 no C160 . C161 . C156 . 121.7(14) yes C160 . C161 . H1611 . 119.2 no C156 . C161 . H1611 . 119.1 no Cl1 . C200 . Cl2 . 106.1(11) yes Cl1 . C200 . H2001 . 109.0 no Cl2 . C200 . H2001 . 109.0 no Cl1 . C200 . H2002 . 109.6 no Cl2 . C200 . H2002 . 113.7 no H2001 . C200 . H2002 . 109.4 no Cl3 . C300 . Cl4 . 108.7(16) yes Cl3 . C300 . H3001 . 111.2 no Cl4 . C300 . H3001 . 112.1 no Cl3 . C300 . H3002 . 108.4 no Cl4 . C300 . H3002 . 108.4 no H3001 . C300 . H3002 . 107.9 no F1 . B1 . F2 . 108.3(12) yes F1 . B1 . F3 . 109.3(12) yes F2 . B1 . F3 . 108.6(12) yes F1 . B1 . F4 . 110.4(13) yes F2 . B1 . F4 . 109.4(13) yes F3 . B1 . F4 . 110.6(12) yes F5 . B2 . F6 . 112.2(14) yes F5 . B2 . F7 . 108.5(14) yes F6 . B2 . F7 . 109.8(14) yes F5 . B2 . F8 . 107.2(14) yes F6 . B2 . F8 . 109.1(14) yes F7 . B2 . F8 . 110.1(13) yes # Attachment 'CIFOmar1402061.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 645319' _audit_creation_date 07-04-16 _audit_creation_method CRYSTALS_ver_12.84 _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 13.5721(9) _cell_length_b 12.5841(8) _cell_length_c 14.9692(12) _cell_angle_alpha 90 _cell_angle_beta 100.516(6) _cell_angle_gamma 90 _cell_volume 2513.7(3) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 2/n 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y,-z+1/2 x+1/2,-y,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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' 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' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 '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' 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' _cell_formula_units_Z 2 # Given Formula = C60 H48 B1 Cu1 F4 P4 # Dc = 1.38 Fooo = 1076.00 Mu = 6.17 M = 521.64 # Found Formula = C60 H48 B1 Cu1 F4 P4 # Dc = 1.38 FOOO = 1076.00 Mu = 6.17 M = 521.64 _chemical_formula_sum 'C60 H48 B1 Cu1 F4 P4' _chemical_formula_moiety 'C60 H48 Cu P4, B F4' _chemical_compound_source ? _chemical_formula_weight 1043.29 _cell_measurement_reflns_used 5032 _cell_measurement_theta_min 3 _cell_measurement_theta_max 24 _cell_measurement_temperature 180 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_max 0.50 _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1076 _exptl_absorpt_coefficient_mu 0.617 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.77 _exptl_absorpt_correction_T_max 0.94 _diffrn_measurement_device_type 'Oxford Diffraction XCALIBUR' _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 'Xcalibur, (Oxford Diffraction, 2002)' _computing_cell_refinement 'CrysAlis RED, (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis RED, (Oxford Diffraction, 2002)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 180 _diffrn_reflns_number 11658 _reflns_number_total 5719 _diffrn_reflns_av_R_equivalents 0.038 # Number of reflections with Friedels Law is 5719 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 6717 _diffrn_reflns_theta_min 2.758 _diffrn_reflns_theta_max 28.997 _diffrn_measured_fraction_theta_max 0.849 _diffrn_reflns_theta_full 25.228 _diffrn_measured_fraction_theta_full 0.892 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 7 _reflns_limit_h_min -18 _reflns_limit_h_max 18 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.77 _refine_diff_density_max 1.17 _refine_ls_number_reflns 3534 _refine_ls_number_restraints 0 _refine_ls_number_parameters 308 #_refine_ls_R_factor_ref 0.0509 _refine_ls_wR_factor_ref 0.0579 _refine_ls_goodness_of_fit_ref 1.1501 #_reflns_number_all 5706 _refine_ls_R_factor_all 0.0798 _refine_ls_wR_factor_all 0.0630 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>2.5\s(I) _reflns_number_gt 3534 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_gt 0.0579 _refine_ls_shift/su_max 0.000393 # 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 F _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, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 9.40 4.57 7.26 4.11 ; _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_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 Fih. ; ? ; _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: ; 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. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # End of 'script/refcif.dat' # 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. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Oxford Diffraction, (2002). CrysAlis RED. Oxford Diffraction, (2002). Xcalibur User Manual. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Cu1 Cu 0.7500 0.37042(4) 0.7500 0.0173 1.0000 Uani S T . . . . P1 P 0.69915(7) 0.28229(6) 0.61410(5) 0.0186 1.0000 Uani . . . . . . P2 P 0.86423(6) 0.45042(6) 0.67657(5) 0.0169 1.0000 Uani . . . . . . C1 C 0.7283(2) 0.3767(2) 0.52945(19) 0.0180 1.0000 Uani . . . . . . C2 C 0.7978(3) 0.4574(2) 0.5591(2) 0.0191 1.0000 Uani . . . . . . C3 C 0.8203(3) 0.5325(3) 0.4969(2) 0.0229 1.0000 Uani . . . . . . C4 C 0.7745(3) 0.5274(3) 0.4062(2) 0.0307 1.0000 Uani . . . . . . C5 C 0.7082(3) 0.4458(3) 0.3765(2) 0.0308 1.0000 Uani . . . . . . C6 C 0.6847(3) 0.3717(3) 0.4375(2) 0.0276 1.0000 Uani . . . . . . C7 C 0.5703(3) 0.2430(3) 0.5697(2) 0.0238 1.0000 Uani . . . . . . C8 C 0.5388(3) 0.1395(3) 0.5778(3) 0.0352 1.0000 Uani . . . . . . C9 C 0.4371(4) 0.1130(4) 0.5522(3) 0.0504 1.0000 Uani . . . . . . C10 C 0.3690(4) 0.1892(5) 0.5178(3) 0.0577 1.0000 Uani . . . . . . C11 C 0.3986(3) 0.2918(5) 0.5089(3) 0.0498 1.0000 Uani . . . . . . C12 C 0.4995(3) 0.3194(4) 0.5356(2) 0.0344 1.0000 Uani . . . . . . C13 C 0.7752(3) 0.1654(2) 0.6014(2) 0.0211 1.0000 Uani . . . . . . C14 C 0.7735(3) 0.1142(3) 0.5186(2) 0.0322 1.0000 Uani . . . . . . C15 C 0.8389(4) 0.0307(3) 0.5128(3) 0.0439 1.0000 Uani . . . . . . C16 C 0.9064(4) -0.0015(3) 0.5877(3) 0.0439 1.0000 Uani . . . . . . C17 C 0.9090(3) 0.0483(3) 0.6702(3) 0.0379 1.0000 Uani . . . . . . C18 C 0.8438(3) 0.1311(3) 0.6769(2) 0.0279 1.0000 Uani . . . . . . C19 C 0.9250(2) 0.5788(3) 0.7025(2) 0.0211 1.0000 Uani . . . . . . C20 C 0.8899(3) 0.6460(3) 0.7631(3) 0.0328 1.0000 Uani . . . . . . C21 C 0.9343(4) 0.7450(3) 0.7830(3) 0.0438 1.0000 Uani . . . . . . C22 C 1.0142(4) 0.7760(3) 0.7448(3) 0.0408 1.0000 Uani . . . . . . C23 C 1.0516(3) 0.7087(3) 0.6853(3) 0.0350 1.0000 Uani . . . . . . C24 C 1.0064(3) 0.6095(3) 0.6646(2) 0.0273 1.0000 Uani . . . . . . C25 C 0.9686(2) 0.3626(2) 0.6643(2) 0.0172 1.0000 Uani . . . . . . C26 C 0.9789(3) 0.3145(3) 0.5832(2) 0.0242 1.0000 Uani . . . . . . C27 C 1.0542(3) 0.2414(3) 0.5805(3) 0.0305 1.0000 Uani . . . . . . C28 C 1.1208(3) 0.2148(3) 0.6595(3) 0.0325 1.0000 Uani . . . . . . C29 C 1.1115(3) 0.2636(3) 0.7403(3) 0.0319 1.0000 Uani . . . . . . C30 C 1.0367(3) 0.3375(3) 0.7433(2) 0.0260 1.0000 Uani . . . . . . B1 B 0.7500 1.0545(8) 0.2500 0.058(2) 1.0000 Uiso S . . . . . F1 F 0.8013(4) 0.9952(4) 0.1988(3) 0.1049(14) 1.0000 Uiso . . . . . . F2 F 0.8507(5) 1.0601(5) 0.3175(4) 0.0629(16) 0.5000 Uiso . . . . . . F3 F 0.7475(5) 1.1508(5) 0.2071(4) 0.0609(15) 0.5000 Uiso . . . . . . H31 H 0.8656 0.5859 0.5160 0.0282 1.0000 Uiso R . . . . . H41 H 0.7886 0.5783 0.3651 0.0372 1.0000 Uiso R . . . . . H51 H 0.6800 0.4418 0.3155 0.0369 1.0000 Uiso R . . . . . H61 H 0.6398 0.3168 0.4169 0.0335 1.0000 Uiso R . . . . . H81 H 0.5854 0.0874 0.6006 0.0438 1.0000 Uiso R . . . . . H91 H 0.4164 0.0433 0.5589 0.0628 1.0000 Uiso R . . . . . H101 H 0.3021 0.1715 0.5006 0.0699 1.0000 Uiso R . . . . . H111 H 0.3513 0.3437 0.4846 0.0598 1.0000 Uiso R . . . . . H121 H 0.5192 0.3904 0.5310 0.0428 1.0000 Uiso R . . . . . H141 H 0.7280 0.1362 0.4667 0.0379 1.0000 Uiso R . . . . . H151 H 0.8373 -0.0035 0.4570 0.0498 1.0000 Uiso R . . . . . H161 H 0.9507 -0.0578 0.5831 0.0538 1.0000 Uiso R . . . . . H171 H 0.9553 0.0275 0.7206 0.0438 1.0000 Uiso R . . . . . H181 H 0.8452 0.1641 0.7329 0.0333 1.0000 Uiso R . . . . . H201 H 0.8371 0.6254 0.7903 0.0409 1.0000 Uiso R . . . . . H211 H 0.9098 0.7903 0.8230 0.0532 1.0000 Uiso R . . . . . H221 H 1.0443 0.8418 0.7584 0.0460 1.0000 Uiso R . . . . . H231 H 1.1065 0.7292 0.6594 0.0418 1.0000 Uiso R . . . . . H241 H 1.0307 0.5641 0.6241 0.0329 1.0000 Uiso R . . . . . H261 H 0.9346 0.3315 0.5296 0.0298 1.0000 Uiso R . . . . . H271 H 1.0599 0.2106 0.5253 0.0369 1.0000 Uiso R . . . . . H281 H 1.1703 0.1631 0.6575 0.0401 1.0000 Uiso R . . . . . H291 H 1.1555 0.2469 0.7932 0.0380 1.0000 Uiso R . . . . . H301 H 1.0319 0.3706 0.7979 0.0313 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 0.0158(3) 0.0181(3) 0.0189(3) 0.0000 0.0057(2) 0.0000 P1 0.0196(4) 0.0170(4) 0.0194(3) -0.0013(3) 0.0047(3) -0.0024(3) P2 0.0144(4) 0.0191(4) 0.0179(3) 0.0009(3) 0.0046(3) -0.0001(3) C1 0.0181(16) 0.0167(13) 0.0206(12) 0.0011(11) 0.0071(12) 0.0015(12) C2 0.0176(16) 0.0213(14) 0.0185(12) 0.0008(11) 0.0039(12) 0.0020(12) C3 0.0196(17) 0.0213(15) 0.0280(15) 0.0041(12) 0.0048(13) -0.0026(12) C4 0.038(2) 0.0304(17) 0.0242(15) 0.0100(13) 0.0063(15) -0.0018(16) C5 0.031(2) 0.042(2) 0.0179(14) 0.0038(14) 0.0020(14) 0.0024(16) C6 0.0275(19) 0.0314(17) 0.0235(14) -0.0022(14) 0.0036(13) -0.0012(15) C7 0.0188(17) 0.0305(16) 0.0236(14) -0.0055(12) 0.0077(13) -0.0041(13) C8 0.031(2) 0.036(2) 0.0409(19) -0.0100(16) 0.0145(17) -0.0119(17) C9 0.036(3) 0.062(3) 0.058(3) -0.021(2) 0.020(2) -0.027(2) C10 0.020(2) 0.103(4) 0.052(3) -0.027(3) 0.013(2) -0.020(3) C11 0.020(2) 0.090(4) 0.039(2) -0.012(2) 0.0048(18) 0.007(2) C12 0.025(2) 0.051(2) 0.0279(17) -0.0058(16) 0.0065(15) 0.0035(17) C13 0.0195(17) 0.0185(14) 0.0275(15) -0.0022(12) 0.0103(13) -0.0044(12) C14 0.032(2) 0.037(2) 0.0280(16) -0.0076(15) 0.0052(15) 0.0001(16) C15 0.053(3) 0.040(2) 0.040(2) -0.0180(18) 0.0116(19) 0.007(2) C16 0.053(3) 0.031(2) 0.049(2) -0.0092(17) 0.012(2) 0.0117(19) C17 0.042(3) 0.0322(19) 0.0381(19) 0.0005(16) 0.0049(18) 0.0119(17) C18 0.035(2) 0.0219(15) 0.0280(15) -0.0017(13) 0.0095(14) -0.0005(15) C19 0.0151(16) 0.0222(14) 0.0246(14) 0.0003(11) 0.0000(13) -0.0019(12) C20 0.033(2) 0.0313(18) 0.0355(18) -0.0045(14) 0.0104(16) -0.0014(16) C21 0.055(3) 0.0302(19) 0.048(2) -0.0116(17) 0.012(2) -0.0025(19) C22 0.049(3) 0.0199(16) 0.047(2) -0.0013(15) -0.008(2) -0.0039(16) C23 0.034(2) 0.0269(17) 0.043(2) 0.0038(15) 0.0042(17) -0.0116(16) C24 0.0260(19) 0.0233(16) 0.0320(16) 0.0005(13) 0.0038(14) -0.0035(13) C25 0.0124(14) 0.0167(13) 0.0235(13) 0.0025(11) 0.0058(12) -0.0013(11) C26 0.0232(18) 0.0252(16) 0.0254(15) -0.0005(12) 0.0076(14) -0.0026(13) C27 0.0228(19) 0.0298(17) 0.0408(19) -0.0028(15) 0.0112(16) 0.0007(15) C28 0.0198(19) 0.0246(17) 0.054(2) 0.0038(16) 0.0104(17) 0.0005(14) C29 0.0198(18) 0.0368(19) 0.0382(18) 0.0106(15) 0.0025(15) 0.0031(15) C30 0.0225(18) 0.0313(17) 0.0245(15) 0.0037(13) 0.0048(14) -0.0004(14) _refine_ls_extinction_method None 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 3_656 2.3092(8) yes Cu1 . P2 3_656 2.2907(9) yes Cu1 . P1 . 2.3092(8) yes Cu1 . P2 . 2.2907(9) yes P1 . C1 . 1.832(3) yes P1 . C7 . 1.822(4) yes P1 . C13 . 1.826(3) yes P2 . C2 . 1.825(3) yes P2 . C19 . 1.824(3) yes P2 . C25 . 1.832(3) yes C1 . C2 . 1.403(4) yes C1 . C6 . 1.398(4) yes C2 . C3 . 1.399(4) yes C3 . C4 . 1.388(5) yes C3 . H31 . 0.919 no C4 . C5 . 1.385(5) yes C4 . H41 . 0.932 no C5 . C6 . 1.382(5) yes C5 . H51 . 0.924 no C6 . H61 . 0.935 no C7 . C8 . 1.384(5) yes C7 . C12 . 1.389(5) yes C8 . C9 . 1.404(6) yes C8 . H81 . 0.931 no C9 . C10 . 1.365(8) yes C9 . H91 . 0.931 no C10 . C11 . 1.366(8) yes C10 . H101 . 0.926 no C11 . C12 . 1.398(6) yes C11 . H111 . 0.942 no C12 . H121 . 0.939 no C13 . C14 . 1.394(5) yes C13 . C18 . 1.395(5) yes C14 . C15 . 1.388(6) yes C14 . H141 . 0.941 no C15 . C16 . 1.374(6) yes C15 . H151 . 0.936 no C16 . C17 . 1.380(6) yes C16 . H161 . 0.940 no C17 . C18 . 1.382(5) yes C17 . H171 . 0.927 no C18 . H181 . 0.933 no C19 . C20 . 1.386(5) yes C19 . C24 . 1.385(5) yes C20 . C21 . 1.392(6) yes C20 . H201 . 0.925 no C21 . C22 . 1.372(7) yes C21 . H211 . 0.931 no C22 . C23 . 1.390(6) yes C22 . H221 . 0.930 no C23 . C24 . 1.400(5) yes C23 . H231 . 0.938 no C24 . H241 . 0.935 no C25 . C26 . 1.386(5) yes C25 . C30 . 1.398(4) yes C26 . C27 . 1.381(5) yes C26 . H261 . 0.936 no C27 . C28 . 1.392(5) yes C27 . H271 . 0.929 no C28 . C29 . 1.382(6) yes C28 . H281 . 0.939 no C29 . C30 . 1.384(5) yes C29 . H291 . 0.925 no C30 . H301 . 0.930 no B1 . F2 3_655 1.546(7) yes B1 . F3 3_655 1.369(10) yes B1 . F1 3_655 1.351(7) yes B1 . F1 . 1.351(7) yes B1 . F2 . 1.546(7) yes B1 . F3 . 1.369(10) 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 3_656 Cu1 . P2 3_656 84.72(3) yes P1 3_656 Cu1 . P1 . 122.59(5) yes P2 3_656 Cu1 . P1 . 120.94(3) yes P1 3_656 Cu1 . P2 . 120.94(3) yes P2 3_656 Cu1 . P2 . 127.85(5) yes P1 . Cu1 . P2 . 84.72(3) yes Cu1 . P1 . C1 . 103.32(10) yes Cu1 . P1 . C7 . 124.34(11) yes C1 . P1 . C7 . 103.76(15) yes Cu1 . P1 . C13 . 113.24(11) yes C1 . P1 . C13 . 104.61(15) yes C7 . P1 . C13 . 105.49(16) yes Cu1 . P2 . C2 . 103.00(12) yes Cu1 . P2 . C19 . 127.37(12) yes C2 . P2 . C19 . 106.64(14) yes Cu1 . P2 . C25 . 112.72(10) yes C2 . P2 . C25 . 100.81(14) yes C19 . P2 . C25 . 103.18(15) yes P1 . C1 . C2 . 117.9(2) yes P1 . C1 . C6 . 123.1(3) yes C2 . C1 . C6 . 119.0(3) yes P2 . C2 . C1 . 117.1(2) yes P2 . C2 . C3 . 123.0(2) yes C1 . C2 . C3 . 119.6(3) yes C2 . C3 . C4 . 120.4(3) yes C2 . C3 . H31 . 120.1 no C4 . C3 . H31 . 119.5 no C3 . C4 . C5 . 119.9(3) yes C3 . C4 . H41 . 120.3 no C5 . C4 . H41 . 119.8 no C4 . C5 . C6 . 120.2(3) yes C4 . C5 . H51 . 119.0 no C6 . C5 . H51 . 120.8 no C1 . C6 . C5 . 120.9(3) yes C1 . C6 . H61 . 119.4 no C5 . C6 . H61 . 119.7 no P1 . C7 . C8 . 121.0(3) yes P1 . C7 . C12 . 120.0(3) yes C8 . C7 . C12 . 118.7(4) yes C7 . C8 . C9 . 120.3(4) yes C7 . C8 . H81 . 119.7 no C9 . C8 . H81 . 120.0 no C8 . C9 . C10 . 120.0(5) yes C8 . C9 . H91 . 119.7 no C10 . C9 . H91 . 120.4 no C9 . C10 . C11 . 120.7(4) yes C9 . C10 . H101 . 119.9 no C11 . C10 . H101 . 119.4 no C10 . C11 . C12 . 119.8(5) yes C10 . C11 . H111 . 120.1 no C12 . C11 . H111 . 120.1 no C11 . C12 . C7 . 120.6(4) yes C11 . C12 . H121 . 119.5 no C7 . C12 . H121 . 119.9 no P1 . C13 . C14 . 123.2(3) yes P1 . C13 . C18 . 118.1(2) yes C14 . C13 . C18 . 118.5(3) yes C13 . C14 . C15 . 119.9(4) yes C13 . C14 . H141 . 120.0 no C15 . C14 . H141 . 120.1 no C14 . C15 . C16 . 120.7(4) yes C14 . C15 . H151 . 119.5 no C16 . C15 . H151 . 119.7 no C15 . C16 . C17 . 120.1(4) yes C15 . C16 . H161 . 120.2 no C17 . C16 . H161 . 119.7 no C16 . C17 . C18 . 119.7(4) yes C16 . C17 . H171 . 120.2 no C18 . C17 . H171 . 120.1 no C13 . C18 . C17 . 121.1(3) yes C13 . C18 . H181 . 119.4 no C17 . C18 . H181 . 119.5 no P2 . C19 . C20 . 118.9(3) yes P2 . C19 . C24 . 121.6(3) yes C20 . C19 . C24 . 119.5(3) yes C19 . C20 . C21 . 120.0(4) yes C19 . C20 . H201 . 120.3 no C21 . C20 . H201 . 119.7 no C20 . C21 . C22 . 120.6(4) yes C20 . C21 . H211 . 119.6 no C22 . C21 . H211 . 119.8 no C21 . C22 . C23 . 120.2(4) yes C21 . C22 . H221 . 120.7 no C23 . C22 . H221 . 119.1 no C22 . C23 . C24 . 119.2(4) yes C22 . C23 . H231 . 120.5 no C24 . C23 . H231 . 120.2 no C23 . C24 . C19 . 120.5(4) yes C23 . C24 . H241 . 119.7 no C19 . C24 . H241 . 119.8 no P2 . C25 . C26 . 123.7(2) yes P2 . C25 . C30 . 117.1(3) yes C26 . C25 . C30 . 119.0(3) yes C25 . C26 . C27 . 120.7(3) yes C25 . C26 . H261 . 120.0 no C27 . C26 . H261 . 119.3 no C26 . C27 . C28 . 120.3(4) yes C26 . C27 . H271 . 119.1 no C28 . C27 . H271 . 120.6 no C27 . C28 . C29 . 119.2(4) yes C27 . C28 . H281 . 119.8 no C29 . C28 . H281 . 121.1 no C28 . C29 . C30 . 120.8(3) yes C28 . C29 . H291 . 120.0 no C30 . C29 . H291 . 119.2 no C25 . C30 . C29 . 120.0(3) yes C25 . C30 . H301 . 120.0 no C29 . C30 . H301 . 120.0 no F2 3_655 B1 . F3 3_655 102.1(5) yes F2 3_655 B1 . F1 3_655 84.8(3) yes F3 3_655 B1 . F1 3_655 101.2(4) yes F2 3_655 B1 . F1 . 98.1(4) yes F3 3_655 B1 . F1 . 141.7(5) yes F1 3_655 B1 . F1 . 112.9(8) yes F2 3_655 B1 . F2 . 174.8(9) yes F3 3_655 B1 . F2 . 73.2(4) yes F1 3_655 B1 . F2 . 98.1(4) yes F1 . B1 . F2 . 84.8(3) yes F2 3_655 B1 . F3 . 73.2(4) yes F3 3_655 B1 . F3 . 55.5(6) yes F1 3_655 B1 . F3 . 141.7(5) yes F1 . B1 . F3 . 101.2(4) yes F2 . B1 . F3 . 102.1(5) yes