# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global #============================================================================== #=============================================================================== # 1. submission details _publ_contact_author_name 'Manfred Scheer' _publ_contact_author_address # address of author for correspondence ; Institute of Inorganic Chemistry University of Regensburg Regensburg 93040 GERMANY ; _publ_contact_author_email MANFRED.SCHEER@CHEMIE.UNI-REGENSBURG.DE _publ_contact_author_fax ? _publ_contact_author_phone ? _publ_requested_journal 'Chemical Communications' _journal_coden_Cambridge 182 # publication choise fi, ci or ei for inorganic # fm, cm or em for metal-organic # fo, co or eo for organic _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter # include date of submission ; date of submission ? please consider this cif submission for publication as a regular structural paper in acta crystallographica c. ; #=============================================================================== # 2. processing summary (journal office only) _journal_coden_astm ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? #=============================================================================== # 3. title and author list _publ_section_title ; Cu(I) mediated oligomerisation of a phosphaalkyne ; _publ_section_title_footnote ; ; # the loop structure below should contain the names and adresses of all # authors, in the required order of publication. repeat as necessary. loop_ _publ_author_name 'Manfred Scheer' J.Nixon 'Ulf Vogel' #=============================================================================== # 4. text _publ_section_synopsis ; ? ; _publ_section_abstract ; ? ; # insert blank lines between paragraphs _publ_section_comment ; ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; the data were collected at 103k using an oxford diffraction cryojet cooler. the structure was solved by direct methods (sir-97) and refined by full-matrix anisotropic least squares (shelxl97). the h-atoms were calculated geometrically and a riding model was used during refinement process. ; # insert blank lines between references _publ_section_references ; altomare, a., burla, m.c., camalli, m., cascarano, g.l., giacovazzo, c. guagliardi, a., moliterni, a.g.g., polidori, g. & spagna, r. (1999) j. appl. cryst. 32, 115-119. cosier, j. & glazer, a.m. (1986). j. appl. cryst. 19, 105-107. flack, h.d. (1983). acta cryst. a39, 876-881. l. j. farrugia, j. appl. cryst (1997), 30, 565. sheldrick, g.m. shelxl97. program for crystal structure refinement. university of g\\"ottingen, germany, 1997. sheldrick, g.m. shelxs97. program for crystal structure solution. university of g\\"ottingen, germany, 1997. sluis, p. v.d., spek, a.l. (1990). acta cryst. a46, 194-201. spek, a.l. (2003). j. appl. cryst. 36, 7-13. wilson, a.j.c. (1992) ed. international tables for crystallography, volume c, kluwer academic publishers, dordrecht, the netherlands. ; _publ_section_acknowledgements ; ; _publ_section_figure_captions ; view of the title compound with the atom numbering scheme. displacement ellipsoids for non-h atoms are drawn at the 50% probability level. ; #=============================================================================== data_476 _database_code_depnum_ccdc_archive 'CCDC 656701' # 0. audit details _audit_creation_date 'apr 13 10:10:07 2007' _audit_creation_method 'platon option' _audit_update_record ; ; #=============================================================================== # 5. chemical data _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H40 Cu3 I3 N P5' # ex: 'c12 h16 n2 o6, h2 o' and '(cd 2+)3, (c6 n6 cr 3-)2, 2(h2 o)' _chemical_formula_structural ? _chemical_formula_sum 'C22 H40 Cu3 I3 N P5' _chemical_formula_iupac ? _chemical_formula_weight 1044.75 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source p p 0.2955 0.4335 'international tables vol c tables 4.2.6.8 and 6.1.1.4' n n 0.0311 0.0180 'international tables vol c tables 4.2.6.8 and 6.1.1.4' i i -0.3257 6.8362 'international tables vol c tables 4.2.6.8 and 6.1.1.4' cu cu -1.9646 0.5888 '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' c c 0.0181 0.0091 'international tables vol c tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. crystal data _symmetry_cell_setting triclinic _symmetry_space_group_name_hall '-p 1' _symmetry_space_group_name_h-m 'p -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 11.693(2) _cell_length_b 12.8918(16) _cell_length_c 13.172(3) _cell_angle_alpha 89.985(13) _cell_angle_beta 64.793(18) _cell_angle_gamma 77.478(12) _cell_volume 1744.2(6) _cell_formula_units_z 2 _cell_measurement_temperature 103(1) _cell_measurement_reflns_used 3361 _cell_measurement_theta_min 3.5255 _cell_measurement_theta_max 51.2205 _cell_special_details ; ; _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.085 _exptl_crystal_size_mid 0.053 _exptl_crystal_size_min 0.024 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.989 _exptl_crystal_density_method 'not measured' _exptl_crystal_f_000 1000 _exptl_absorpt_coefficient_mu 25.236 _exptl_crystal_density_meas_temp ? # permitted for _exptl_absorpt_correction_type : # analytical 'analytical from crystal shape' # example: de meulenaer&tompa: abst # cylinder 'cylindrical' # gaussian 'gaussian from crystal shape' # example: platon/absg # integration 'integration from crystal shape' # multi-scan 'symmetry-related measurements' # example: sadabs, mulabs # none 'no absorption corr. applied' # numerical 'numerical from crystal shape' # psi-scan 'psi-scan corrections' # example: platon/absp # refdelf 'refined from delta-f' # example: shelxa, difabs, delabs # sphere 'spherical' # example: platon/abss _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; crysalis red, oxford diffraction ltd., version 1.171.30.3 (release 12-05-2006 crysalis171 .net) (compiled may 12 2006,14:43:55) empirical absorption correction using spherical harmonics, implemented in scale3 abspack scaling algorithm. ; _exptl_absorpt_correction_t_min 0.449 _exptl_absorpt_correction_t_max 1.450 #=============================================================================== # 7. experimental data _exptl_special_details ; ; _diffrn_ambient_temperature 103(1) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_probe X-ray _diffrn_radiation_type cuk\a _diffrn_radiation_source 'enhance (cu) x-ray source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'oxford diffraction gemini ultra' _diffrn_measurement_method omega-scan _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -78.00 -23.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 0.1529 -75.0000 120.0000 0.0000 0.0000 55 #__ type_ start__ end____ width___ exp.time_ 2 omega -37.00 18.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 0.1529 87.0000 44.0000 0.0000 0.0000 55 #__ type_ start__ end____ width___ exp.time_ 3 omega 23.00 78.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 0.1529 75.0000 120.0000 0.0000 0.0000 55 #__ type_ start__ end____ width___ exp.time_ 4 omega -23.00 28.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 0.1529 -45.0000 120.0000 0.0000 0.0000 51 #__ type_ start__ end____ width___ exp.time_ 5 omega 24.00 75.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 0.1529 45.0000 240.0000 0.0000 0.0000 51 #__ type_ start__ end____ width___ exp.time_ 6 omega -113.00 -63.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -60.8272 117.0000 178.0000 0.0000 0.0000 50 #__ type_ start__ end____ width___ exp.time_ 7 omega -106.00 -54.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -60.8272 105.0000 92.0000 0.0000 0.0000 52 #__ type_ start__ end____ width___ exp.time_ 8 phi 60.00 120.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames -40.0000 -60.8272 0.0000 - 0.0000 0.0000 60 #__ type_ start__ end____ width___ exp.time_ 9 omega -139.00 -84.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -60.8272 -75.0000 240.0000 0.0000 0.0000 55 #__ type_ start__ end____ width___ exp.time_ 10 omega -82.00 -29.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -60.8272 -66.0000 345.0000 0.0000 0.0000 53 #__ type_ start__ end____ width___ exp.time_ 11 omega -54.00 -2.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -60.8272 105.0000 92.0000 0.0000 0.0000 52 #__ type_ start__ end____ width___ exp.time_ 12 omega -135.00 -83.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -60.8272 -60.0000 289.0000 0.0000 0.0000 52 #__ type_ start__ end____ width___ exp.time_ 13 omega -137.00 -83.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -60.8272 -69.0000 259.0000 0.0000 0.0000 54 #__ type_ start__ end____ width___ exp.time_ 14 omega -83.00 -28.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -60.8272 -72.0000 149.0000 0.0000 0.0000 55 #__ type_ start__ end____ width___ exp.time_ 15 omega -83.00 -29.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -60.8272 -69.0000 259.0000 0.0000 0.0000 54 #__ type_ start__ end____ width___ exp.time_ 16 omega -131.00 -83.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -60.8272 -66.0000 345.0000 0.0000 0.0000 48 #__ type_ start__ end____ width___ exp.time_ 17 omega -140.00 -84.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -60.8272 -78.0000 45.0000 0.0000 0.0000 56 #__ type_ start__ end____ width___ exp.time_ 18 omega 29.00 84.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 62.4840 75.0000 23.0000 0.0000 0.0000 55 #__ type_ start__ end____ width___ exp.time_ 19 omega 31.00 84.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 62.4840 66.0000 209.0000 0.0000 0.0000 53 #__ type_ start__ end____ width___ exp.time_ 20 omega 31.00 84.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 62.4840 75.0000 240.0000 0.0000 0.0000 53 #__ type_ start__ end____ width___ exp.time_ 21 omega 98.00 126.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 62.4840 45.0000 120.0000 0.0000 0.0000 28 #__ type_ start__ end____ width___ exp.time_ 22 omega 46.00 93.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 62.4840 -75.0000 240.0000 0.0000 0.0000 47 #__ type_ start__ end____ width___ exp.time_ 23 omega 47.00 77.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 62.4840 45.0000 0.0000 0.0000 0.0000 30 #__ type_ start__ end____ width___ exp.time_ 24 omega 35.00 85.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 62.4840 45.0000 120.0000 0.0000 0.0000 50 ; _diffrn_detector_area_resol_mean 10.5431 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 11103 _diffrn_reflns_av_r_equivalents 0.0487 _diffrn_reflns_av_sigmai/neti 0.1286 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 51.27 _diffrn_reflns_theta_full 51.27 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measured_fraction_theta_full 0.987 _diffrn_reflns_reduction_process ; ; # number of unique reflections _reflns_number_total 3742 # number of observed reflections (> n sig(i)) _reflns_number_gt 2138 _reflns_threshold_expression i>2\s(i) _computing_data_collection ; crysalis ccd, oxford diffraction ltd., version 1.171.30.3 (release 12-05-2006 crysalis171 .net) ; _computing_cell_refinement ; crysalis red, oxford diffraction ltd., version 1.171.30.3 (release 12-05-2006 crysalis171 .net) ; _computing_data_reduction ; crysalis red, oxford diffraction ltd., version 1.171.30.3 (release 12-05-2006 crysalis171 .net) ; _computing_structure_solution 'sir-97 (altomare, 1993)' _computing_structure_refinement 'shelxl-97 (sheldrick, 1997)' _computing_molecular_graphics 'platon (spek, 1990)' _computing_publication_material 'platon (spek, 2003)' #=============================================================================== # 8. refinement data _refine_special_details ; refinement on f^2^ for all reflections except those flagged by the user for potential systematic errors. weighted r-factors wr and all goodnesses 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 observed criterion of f^2^ > 2sigma(f^2^) is used only for calculating -r-factor-obs etc. and is not relevant to the choice of reflections for refinement. r-factors based on f^2^ are statistically about twice as large as those based on f, and r-factors based on all data will be even larger. ; _refine_ls_structure_factor_coef fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(fo^2^)+(0.0297p)^2^] where p=(fo^2^+2fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # permitted for _refine_ls_hydrogen_treatment : # refall - refined all h parameters # refxyz - refined h coordinates only # refu - refined h u only # noref - no refinement of h parameters # constr - h parameters constrained # mixed - some constrained, some independent # undef - h-atom parameters not defined _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_abs_structure_details ? _refine_ls_abs_structure_flack . _refine_ls_number_reflns 3742 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_r_factor_all 0.0749 _refine_ls_r_factor_gt 0.0368 _refine_ls_wr_factor_ref 0.0655 _refine_ls_wr_factor_gt 0.0628 _refine_ls_goodness_of_fit_ref 0.811 _refine_ls_restrained_s_all 0.811 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.886 _refine_diff_density_min -0.452 _refine_diff_density_rms 0.119 #=============================================================================== # 9. atomic coordinates and displacement parameters loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_u_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags i1 i uani 0.52286(6) 0.60044(5) 0.10849(6) 1.000 0.0400(3) . . i2 i uani 0.40529(6) 0.40074(5) 0.59822(6) 1.000 0.0371(3) . . i3 i uani 0.20318(6) 0.63250(6) 0.43801(6) 1.000 0.0424(3) . . cu1 cu uani 0.44372(13) 0.53088(11) 0.31152(12) 1.000 0.0396(6) . . cu2 cu uani 0.64393(14) 0.41109(12) -0.02385(12) 1.000 0.0454(7) . . cu3 cu uani 0.34219(13) 0.60111(11) 0.54559(12) 1.000 0.0432(6) . . p1 p uani 0.5195(3) 0.3517(2) 0.2747(2) 1.000 0.0351(11) . . p2 p uani 0.6673(3) 0.2970(2) 0.0971(2) 1.000 0.0392(11) . . p3 p uani 0.6890(3) 0.2882(2) 0.3075(2) 1.000 0.0385(11) . . p4 p uani 0.8291(3) 0.1257(2) 0.1341(2) 1.000 0.0491(12) . . p5 p uani 0.5776(3) 0.1127(2) 0.2413(3) 1.000 0.0503(12) . . n1 n uani 0.8031(9) 0.4332(8) -0.1504(8) 1.000 0.051(4) . . c1 c uani 0.8932(13) 0.4458(9) -0.2189(10) 1.000 0.042(6) . . c1l c uani 1.0156(9) 0.4503(8) -0.3189(9) 1.000 0.065(5) . . c2 c uani 0.7983(9) 0.2749(8) 0.1490(7) 1.000 0.036(4) . . c3 c uani 0.7012(9) 0.1394(8) 0.2885(8) 1.000 0.037(4) . . c4 c uani 0.6824(9) 0.1509(7) 0.0932(9) 1.000 0.036(4) . . c5 c uani 0.4483(9) 0.2338(7) 0.3093(8) 1.000 0.043(4) . . c11 c uani 0.9131(10) 0.3269(9) 0.1029(9) 1.000 0.037(5) . . c31 c uani 0.7322(11) 0.0673(9) 0.3692(10) 1.000 0.045(5) . . c41 c uani 0.7023(11) 0.0828(9) -0.0079(10) 1.000 0.049(5) . . c51 c uani 0.3124(10) 0.2470(10) 0.3093(10) 1.000 0.048(5) . . c111 c uani 0.8689(9) 0.4467(8) 0.1164(7) 1.000 0.043(5) . . c112 c uani 0.9961(9) 0.2832(8) -0.0225(8) 1.000 0.055(5) . . c113 c uani 0.9992(10) 0.2902(8) 0.1656(8) 1.000 0.058(5) . . c311 c uani 0.6192(10) 0.0959(7) 0.4869(9) 1.000 0.058(5) . . c312 c uani 0.8569(10) 0.0872(8) 0.3736(9) 1.000 0.061(5) . . c313 c uani 0.7583(10) -0.0517(8) 0.3300(8) 1.000 0.062(5) . . c411 c uani 0.7343(10) -0.0376(8) 0.0046(9) 1.000 0.062(6) . . c412 c uani 0.8132(10) 0.1098(8) -0.1129(8) 1.000 0.064(5) . . c413 c uani 0.5791(10) 0.1099(7) -0.0264(8) 1.000 0.050(5) . . c511 c uani 0.2809(9) 0.1381(8) 0.3061(8) 1.000 0.057(5) . . c512 c uani 0.3124(10) 0.3007(8) 0.2054(8) 1.000 0.047(5) . . c513 c uani 0.2068(9) 0.3154(8) 0.4153(8) 1.000 0.052(5) . . h1l1 h uiso 1.08320 0.38570 -0.32900 1.000 0.0980 calc r h1l2 h uiso 1.04430 0.51340 -0.30710 1.000 0.0980 calc r h1l3 h uiso 0.99980 0.45480 -0.38630 1.000 0.0980 calc r h5a h uiso 0.42780 0.23050 0.39100 1.000 0.0510 calc r h11a h uiso 0.81640 0.46850 0.07520 1.000 0.0640 calc r h11b h uiso 0.94500 0.47750 0.08630 1.000 0.0640 calc r h11c h uiso 0.81640 0.47210 0.19660 1.000 0.0640 calc r h11d h uiso 0.94580 0.30690 -0.06530 1.000 0.0820 calc r h11e h uiso 1.01990 0.20500 -0.02920 1.000 0.0820 calc r h11f h uiso 1.07530 0.31010 -0.05270 1.000 0.0820 calc r h11g h uiso 1.07330 0.32350 0.13720 1.000 0.0870 calc r h11h h uiso 1.03120 0.21230 0.15250 1.000 0.0870 calc r h11i h uiso 0.94740 0.31160 0.24670 1.000 0.0870 calc r h31a h uiso 0.60550 0.17110 0.51190 1.000 0.0870 calc r h31b h uiso 0.63940 0.05050 0.53960 1.000 0.0870 calc r h31c h uiso 0.54000 0.08460 0.48470 1.000 0.0870 calc r h31d h uiso 0.93050 0.06780 0.29870 1.000 0.0920 calc r h31e h uiso 0.87630 0.04340 0.42780 1.000 0.0920 calc r h31f h uiso 0.84250 0.16280 0.39730 1.000 0.0920 calc r h31g h uiso 0.83220 -0.06950 0.25510 1.000 0.0920 calc r h31h h uiso 0.68080 -0.06550 0.32640 1.000 0.0920 calc r h31i h uiso 0.77830 -0.09590 0.38360 1.000 0.0920 calc r h41a h uiso 0.66210 -0.05420 0.07020 1.000 0.0940 calc r h41b h uiso 0.81400 -0.05640 0.01520 1.000 0.0940 calc r h41c h uiso 0.74700 -0.07860 -0.06350 1.000 0.0940 calc r h41d h uiso 0.79160 0.18630 -0.12040 1.000 0.0950 calc r h41e h uiso 0.82400 0.06880 -0.18040 1.000 0.0950 calc r h41f h uiso 0.89440 0.09140 -0.10470 1.000 0.0950 calc r h41g h uiso 0.55830 0.18610 -0.03580 1.000 0.0750 calc r h41h h uiso 0.50650 0.09370 0.03900 1.000 0.0750 calc r h41i h uiso 0.59340 0.06750 -0.09430 1.000 0.0750 calc r h51a h uiso 0.28130 0.10270 0.37180 1.000 0.0850 calc r h51b h uiso 0.34650 0.09370 0.23690 1.000 0.0850 calc r h51c h uiso 0.19470 0.14820 0.30740 1.000 0.0850 calc r h51d h uiso 0.33250 0.37050 0.20650 1.000 0.0710 calc r h51e h uiso 0.22630 0.31030 0.20660 1.000 0.0710 calc r h51f h uiso 0.37820 0.25560 0.13680 1.000 0.0710 calc r h51g h uiso 0.20650 0.28150 0.48200 1.000 0.0770 calc r h51h h uiso 0.12190 0.32260 0.41480 1.000 0.0770 calc r h51i h uiso 0.22390 0.38630 0.41750 1.000 0.0770 calc 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 i1 0.0371(5) 0.0478(5) 0.0365(5) 0.0074(4) -0.0176(4) -0.0095(4) i2 0.0266(5) 0.0492(5) 0.0363(5) 0.0033(4) -0.0135(4) -0.0109(4) i3 0.0281(5) 0.0580(6) 0.0394(5) -0.0015(4) -0.0163(4) -0.0038(4) cu1 0.0316(10) 0.0479(11) 0.0385(11) 0.0035(9) -0.0157(9) -0.0069(9) cu2 0.0370(11) 0.0596(12) 0.0384(11) 0.0040(9) -0.0161(9) -0.0102(9) cu3 0.0342(10) 0.0561(12) 0.0421(11) 0.0037(9) -0.0199(9) -0.0094(9) p1 0.0277(19) 0.043(2) 0.035(2) 0.0034(17) -0.0147(16) -0.0070(16) p2 0.0321(19) 0.042(2) 0.043(2) -0.0006(17) -0.0179(17) -0.0049(17) p3 0.0280(19) 0.051(2) 0.035(2) 0.0039(17) -0.0141(17) -0.0056(17) p4 0.042(2) 0.051(2) 0.051(2) 0.0006(19) -0.022(2) -0.0009(18) p5 0.046(2) 0.048(2) 0.058(2) 0.0009(19) -0.025(2) -0.0083(18) n1 0.035(7) 0.070(8) 0.049(8) -0.002(7) -0.012(6) -0.028(7) c1 0.061(11) 0.040(8) 0.045(10) -0.001(8) -0.040(9) -0.014(9) c1l 0.035(8) 0.084(10) 0.059(9) 0.003(8) 0.000(8) -0.026(8) c2 0.031(7) 0.062(9) 0.017(7) 0.005(6) -0.012(6) -0.013(7) c3 0.040(7) 0.042(8) 0.024(7) 0.006(6) -0.016(6) 0.004(6) c4 0.017(7) 0.020(7) 0.058(8) -0.021(6) -0.008(6) 0.003(5) c5 0.039(8) 0.048(8) 0.035(7) 0.000(6) -0.008(6) -0.017(7) c11 0.030(8) 0.036(9) 0.039(9) -0.007(7) -0.011(7) -0.003(7) c31 0.040(8) 0.046(9) 0.051(9) 0.004(8) -0.024(8) -0.004(7) c41 0.045(9) 0.041(9) 0.058(10) -0.004(8) -0.021(8) -0.005(7) c51 0.023(8) 0.052(9) 0.057(10) 0.000(8) -0.002(7) -0.016(7) c111 0.036(7) 0.072(10) 0.024(7) 0.006(7) -0.015(6) -0.018(7) c112 0.036(8) 0.068(9) 0.051(9) -0.006(7) -0.008(7) -0.016(7) c113 0.044(8) 0.088(10) 0.049(8) -0.009(8) -0.023(7) -0.024(7) c311 0.064(9) 0.040(8) 0.063(9) 0.020(7) -0.024(8) -0.004(7) c312 0.062(9) 0.054(9) 0.085(10) 0.024(7) -0.057(8) 0.005(7) c313 0.070(9) 0.041(9) 0.063(9) -0.012(7) -0.035(8) 0.021(7) c411 0.078(10) 0.037(9) 0.090(10) -0.009(7) -0.061(9) 0.003(7) c412 0.054(9) 0.088(10) 0.045(9) -0.009(8) -0.019(8) -0.014(8) c413 0.054(9) 0.044(8) 0.061(9) -0.006(7) -0.038(7) -0.004(7) c511 0.048(8) 0.076(10) 0.059(9) 0.022(8) -0.030(7) -0.026(8) c512 0.060(9) 0.055(8) 0.043(8) 0.007(7) -0.035(7) -0.019(7) c513 0.044(8) 0.067(9) 0.049(9) 0.015(7) -0.023(8) -0.018(7) #=============================================================================== # 10. molecular geometry _geom_special_details ; bond distances, angles etc. have been calculated using the rounded fractional coordinates. all su's are estimated from the variances of the (full) variance-covariance matrix. the cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag i1 cu1 2.6577(17) . . yes i1 cu2 2.7209(17) . . yes i1 cu2 2.655(2) . 2_665 yes i2 cu3 2.7029(17) . . yes i2 cu1 2.7877(19) . 2_666 yes i2 cu3 2.7409(19) . 2_666 yes i3 cu1 2.6105(18) . . yes i3 cu3 2.5476(19) . . yes cu1 p1 2.259(3) . . yes cu2 p2 2.230(3) . . yes cu2 n1 1.978(11) . . yes cu3 p3 2.256(3) . 2_666 yes p1 p2 2.233(4) . . yes p1 p3 2.193(5) . . yes p1 c5 1.854(10) . . yes p2 c2 1.897(12) . . yes p2 c4 1.852(9) . . yes p3 c2 1.912(9) . . yes p3 c3 1.901(10) . . yes p4 c2 1.873(10) . . yes p4 c3 1.923(10) . . yes p4 c4 1.971(12) . . yes p5 c3 1.891(12) . . yes p5 c4 1.943(11) . . yes p5 c5 1.830(10) . . yes n1 c1 1.102(17) . . yes c1 c1l 1.489(18) . . no c2 c11 1.522(16) . . no c3 c31 1.519(16) . . no c4 c41 1.499(16) . . no c5 c51 1.561(18) . . no c11 c111 1.503(15) . . no c11 c112 1.545(14) . . no c11 c113 1.556(17) . . no c31 c311 1.526(16) . . no c31 c312 1.559(19) . . no c31 c313 1.542(15) . . no c41 c411 1.542(15) . . no c41 c412 1.544(16) . . no c41 c413 1.529(19) . . no c51 c511 1.532(17) . . no c51 c512 1.534(16) . . no c51 c513 1.520(16) . . no c1l h1l1 0.9800 . . no c1l h1l2 0.9800 . . no c1l h1l3 0.9800 . . no c5 h5a 1.0000 . . no c111 h11a 0.9800 . . no c111 h11b 0.9800 . . no c111 h11c 0.9800 . . no c112 h11d 0.9800 . . no c112 h11e 0.9800 . . no c112 h11f 0.9800 . . no c113 h11g 0.9800 . . no c113 h11h 0.9800 . . no c113 h11i 0.9800 . . no c311 h31a 0.9800 . . no c311 h31b 0.9800 . . no c311 h31c 0.9800 . . no c312 h31d 0.9800 . . no c312 h31e 0.9800 . . no c312 h31f 0.9800 . . no c313 h31g 0.9800 . . no c313 h31h 0.9800 . . no c313 h31i 0.9800 . . no c411 h41a 0.9800 . . no c411 h41b 0.9800 . . no c411 h41c 0.9800 . . no c412 h41d 0.9800 . . no c412 h41e 0.9800 . . no c412 h41f 0.9800 . . no c413 h41g 0.9800 . . no c413 h41h 0.9800 . . no c413 h41i 0.9800 . . no c511 h51a 0.9800 . . no c511 h51b 0.9800 . . no c511 h51c 0.9800 . . no c512 h51d 0.9800 . . no c512 h51e 0.9800 . . no c512 h51f 0.9800 . . no c513 h51g 0.9800 . . no c513 h51h 0.9800 . . no c513 h51i 0.9800 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag cu1 i1 cu2 100.12(5) . . . yes cu1 i1 cu2 110.03(6) . . 2_665 yes cu2 i1 cu2 79.56(6) . . 2_665 yes cu1 i2 cu3 89.21(5) 2_666 . . yes cu3 i2 cu3 86.50(5) . . 2_666 yes cu1 i2 cu3 62.18(5) 2_666 . 2_666 yes cu1 i3 cu3 67.21(5) . . . yes i1 cu1 i3 109.43(6) . . . yes i1 cu1 p1 103.92(8) . . . yes i1 cu1 i2 103.88(6) . . 2_666 yes i3 cu1 p1 125.90(11) . . . yes i2 cu1 i3 106.25(6) 2_666 . . yes i2 cu1 p1 105.48(11) 2_666 . . yes i1 cu2 p2 102.97(9) . . . yes i1 cu2 n1 106.9(3) . . . yes i1 cu2 i1 100.44(6) . . 2_665 yes p2 cu2 n1 118.1(3) . . . yes i1 cu2 p2 119.67(12) 2_665 . . yes i1 cu2 n1 106.5(3) 2_665 . . yes i2 cu3 i3 117.47(6) . . . yes i2 cu3 i2 93.50(5) . . 2_666 yes i2 cu3 p3 106.01(9) . . 2_666 yes i2 cu3 i3 109.48(6) 2_666 . . yes i3 cu3 p3 124.16(11) . . 2_666 yes i2 cu3 p3 100.57(11) 2_666 . 2_666 yes cu1 p1 p2 114.05(13) . . . yes cu1 p1 p3 114.33(16) . . . yes cu1 p1 c5 136.2(4) . . . yes p2 p1 p3 81.48(16) . . . yes p2 p1 c5 99.9(3) . . . yes p3 p1 c5 96.8(4) . . . yes cu2 p2 p1 112.55(15) . . . yes cu2 p2 c2 126.9(3) . . . yes cu2 p2 c4 130.5(4) . . . yes p1 p2 c2 88.5(3) . . . yes p1 p2 c4 101.3(4) . . . yes c2 p2 c4 87.5(5) . . . yes p1 p3 c2 89.2(4) . . . yes p1 p3 c3 99.8(4) . . . yes cu3 p3 p1 103.91(14) 2_666 . . yes c2 p3 c3 86.3(4) . . . yes cu3 p3 c2 133.4(4) 2_666 . . yes cu3 p3 c3 133.0(3) 2_666 . . yes c2 p4 c3 86.8(4) . . . yes c2 p4 c4 84.8(4) . . . yes c3 p4 c4 86.8(5) . . . yes c3 p5 c4 88.5(5) . . . yes c3 p5 c5 99.4(5) . . . yes c4 p5 c5 103.9(4) . . . yes cu2 n1 c1 178.1(12) . . . yes n1 c1 c1l 172.8(13) . . . yes p2 c2 p3 98.7(5) . . . yes p2 c2 p4 94.5(5) . . . yes p2 c2 c11 123.3(7) . . . yes p3 c2 p4 93.6(4) . . . yes p3 c2 c11 120.6(7) . . . yes p4 c2 c11 119.4(8) . . . yes p3 c3 p4 92.4(5) . . . yes p3 c3 p5 111.5(6) . . . yes p3 c3 c31 119.3(8) . . . yes p4 c3 p5 90.6(5) . . . yes p4 c3 c31 118.8(8) . . . yes p5 c3 c31 118.1(8) . . . yes p2 c4 p4 92.8(5) . . . yes p2 c4 p5 110.6(5) . . . yes p2 c4 c41 123.5(8) . . . yes p4 c4 p5 87.7(5) . . . yes p4 c4 c41 116.0(8) . . . yes p5 c4 c41 117.7(8) . . . yes p1 c5 p5 108.9(6) . . . yes p1 c5 c51 115.6(7) . . . yes p5 c5 c51 120.9(8) . . . yes c2 c11 c111 111.6(10) . . . no c2 c11 c112 107.6(9) . . . no c2 c11 c113 108.6(9) . . . no c111 c11 c112 111.2(8) . . . no c111 c11 c113 110.5(9) . . . no c112 c11 c113 107.2(9) . . . no c3 c31 c311 109.2(10) . . . no c3 c31 c312 108.4(9) . . . no c3 c31 c313 111.7(9) . . . no c311 c31 c312 108.9(10) . . . no c311 c31 c313 110.2(9) . . . no c312 c31 c313 108.4(10) . . . no c4 c41 c411 112.5(9) . . . no c4 c41 c412 108.6(10) . . . no c4 c41 c413 109.6(9) . . . no c411 c41 c412 110.2(9) . . . no c411 c41 c413 108.5(10) . . . no c412 c41 c413 107.4(9) . . . no c5 c51 c511 110.7(9) . . . no c5 c51 c512 109.7(10) . . . no c5 c51 c513 110.2(9) . . . no c511 c51 c512 108.7(9) . . . no c511 c51 c513 108.4(9) . . . no c512 c51 c513 109.2(10) . . . no c1 c1l h1l1 109.00 . . . no c1 c1l h1l2 109.00 . . . no c1 c1l h1l3 109.00 . . . no h1l1 c1l h1l2 109.00 . . . no h1l1 c1l h1l3 110.00 . . . no h1l2 c1l h1l3 109.00 . . . no p1 c5 h5a 103.00 . . . no p5 c5 h5a 103.00 . . . no c51 c5 h5a 103.00 . . . no c11 c111 h11a 109.00 . . . no c11 c111 h11b 109.00 . . . no c11 c111 h11c 109.00 . . . no h11a c111 h11b 110.00 . . . no h11a c111 h11c 109.00 . . . no h11b c111 h11c 110.00 . . . no c11 c112 h11d 109.00 . . . no c11 c112 h11e 110.00 . . . no c11 c112 h11f 109.00 . . . no h11d c112 h11e 109.00 . . . no h11d c112 h11f 109.00 . . . no h11e c112 h11f 109.00 . . . no c11 c113 h11g 110.00 . . . no c11 c113 h11h 110.00 . . . no c11 c113 h11i 110.00 . . . no h11g c113 h11h 109.00 . . . no h11g c113 h11i 109.00 . . . no h11h c113 h11i 109.00 . . . no c31 c311 h31a 109.00 . . . no c31 c311 h31b 110.00 . . . no c31 c311 h31c 109.00 . . . no h31a c311 h31b 110.00 . . . no h31a c311 h31c 109.00 . . . no h31b c311 h31c 109.00 . . . no c31 c312 h31d 110.00 . . . no c31 c312 h31e 110.00 . . . no c31 c312 h31f 110.00 . . . no h31d c312 h31e 109.00 . . . no h31d c312 h31f 110.00 . . . no h31e c312 h31f 109.00 . . . no c31 c313 h31g 110.00 . . . no c31 c313 h31h 109.00 . . . no c31 c313 h31i 110.00 . . . no h31g c313 h31h 109.00 . . . no h31g c313 h31i 109.00 . . . no h31h c313 h31i 109.00 . . . no c41 c411 h41a 109.00 . . . no c41 c411 h41b 109.00 . . . no c41 c411 h41c 109.00 . . . no h41a c411 h41b 109.00 . . . no h41a c411 h41c 109.00 . . . no h41b c411 h41c 110.00 . . . no c41 c412 h41d 109.00 . . . no c41 c412 h41e 109.00 . . . no c41 c412 h41f 110.00 . . . no h41d c412 h41e 109.00 . . . no h41d c412 h41f 109.00 . . . no h41e c412 h41f 109.00 . . . no c41 c413 h41g 109.00 . . . no c41 c413 h41h 110.00 . . . no c41 c413 h41i 110.00 . . . no h41g c413 h41h 109.00 . . . no h41g c413 h41i 109.00 . . . no h41h c413 h41i 110.00 . . . no c51 c511 h51a 110.00 . . . no c51 c511 h51b 110.00 . . . no c51 c511 h51c 109.00 . . . no h51a c511 h51b 109.00 . . . no h51a c511 h51c 110.00 . . . no h51b c511 h51c 109.00 . . . no c51 c512 h51d 109.00 . . . no c51 c512 h51e 109.00 . . . no c51 c512 h51f 109.00 . . . no h51d c512 h51e 109.00 . . . no h51d c512 h51f 110.00 . . . no h51e c512 h51f 109.00 . . . no c51 c513 h51g 110.00 . . . no c51 c513 h51h 109.00 . . . no c51 c513 h51i 109.00 . . . no h51g c513 h51h 109.00 . . . no h51g c513 h51i 109.00 . . . no h51h c513 h51i 109.00 . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag cu2 i1 cu1 i3 -135.30(6) . . . . no cu2 i1 cu1 i3 -52.82(7) 2_665 . . . no cu2 i1 cu1 p1 1.42(12) . . . . no cu2 i1 cu1 p1 83.90(12) 2_665 . . . no cu2 i1 cu1 i2 111.56(6) . . . 2_666 no cu2 i1 cu1 i2 -165.95(5) 2_665 . . 2_666 no cu2 i1 cu2 n1 -111.3(3) 2_665 2_665 . . no cu2 i1 cu2 i1 0.00(6) 2_665 . . 2_665 no cu1 i1 cu2 i1 97.06(6) 2_665 2_665 . . no cu2 i1 cu2 i1 0.00(6) 2_665 2_665 . . no cu1 i1 cu2 p2 -151.37(10) 2_665 2_665 . . no cu2 i1 cu2 p2 111.57(11) 2_665 2_665 . . no cu1 i1 cu2 n1 -14.2(3) 2_665 2_665 . . no cu2 i1 cu2 n1 111.0(3) 2_665 . . . no cu1 i1 cu2 i1 108.72(6) . . . 2_665 no cu2 i1 cu2 p2 -123.98(12) 2_665 . . . no cu1 i1 cu2 n1 -140.3(3) . . . . no cu1 i1 cu2 p2 -15.27(12) . . . . no cu3 i2 cu3 i3 114.10(7) 2_666 . . . no cu1 i2 cu3 i2 62.18(5) 2_666 . . 2_666 no cu3 i2 cu1 i3 114.92(6) 2_666 2_666 . . no cu3 i2 cu1 p1 -107.13(9) . 2_666 . . no cu1 i2 cu3 i3 176.28(7) 2_666 . . . no cu3 i2 cu1 p1 -20.67(9) 2_666 2_666 . . no cu3 i2 cu3 i2 0.00(6) 2_666 . . 2_666 no cu3 i2 cu1 i1 143.87(7) . 2_666 . . no cu3 i2 cu1 i1 -129.67(6) 2_666 2_666 . . no cu3 i2 cu1 i3 28.47(5) . 2_666 . . no cu3 i2 cu3 p3 -102.05(11) 2_666 . . 2_666 no cu1 i2 cu3 p3 -162.03(10) . 2_666 . 2_666 no cu3 i2 cu3 i2 0.00(5) 2_666 2_666 . . no cu1 i2 cu3 p3 -39.87(11) 2_666 . . 2_666 no cu1 i2 cu3 i2 90.96(6) . 2_666 . . no cu3 i2 cu3 i3 -120.78(6) 2_666 2_666 . . no cu1 i2 cu3 i3 -29.83(5) . 2_666 . . no cu1 i3 cu3 i2 30.63(5) . . . 2_666 no cu1 i3 cu3 p3 149.00(13) . . . 2_666 no cu3 i3 cu1 p1 94.17(12) . . . . no cu3 i3 cu1 i2 -29.47(5) . . . 2_666 no cu3 i3 cu1 i1 -141.06(7) . . . . no cu1 i3 cu3 i2 -74.25(7) . . . . no i2 cu1 p1 p2 -95.23(18) 2_666 . . . no i2 cu1 p1 p3 -3.87(15) 2_666 . . . no i3 cu1 p1 c5 3.4(5) . . . . no i3 cu1 p1 p3 -127.85(14) . . . . no i1 cu1 p1 p2 13.8(2) . . . . no i1 cu1 p1 p3 105.10(13) . . . . no i2 cu1 p1 c5 127.4(5) 2_666 . . . no i3 cu1 p1 p2 140.80(16) . . . . no i1 cu1 p1 c5 -123.7(5) . . . . no i1 cu2 p2 c2 -80.8(4) . . . . no i1 cu2 p2 p1 25.2(2) . . . . no i1 cu2 p2 c2 169.1(4) 2_665 . . . no i1 cu2 p2 c4 44.3(5) 2_665 . . . no i1 cu2 p2 c4 154.5(5) . . . . no n1 cu2 p2 p1 142.6(4) . . . . no n1 cu2 p2 c2 36.7(5) . . . . no n1 cu2 p2 c4 -88.1(6) . . . . no i1 cu2 p2 p1 -84.96(18) 2_665 . . . no i2 cu3 p3 p1 47.33(14) . . 2_666 2_666 no i2 cu3 p3 c2 -55.1(5) . . 2_666 2_666 no i2 cu3 p3 c3 165.4(5) . . 2_666 2_666 no i3 cu3 p3 p1 -171.90(11) . . 2_666 2_666 no i3 cu3 p3 c2 85.7(5) . . 2_666 2_666 no i3 cu3 p3 c3 -53.9(6) . . 2_666 2_666 no cu1 p1 p2 cu2 -27.2(3) . . . . no cu1 p1 p2 c2 102.6(4) . . . . no cu1 p1 p2 c4 -170.3(4) . . . . no p3 p1 p2 cu2 -140.09(17) . . . . no p3 p1 p2 c2 -10.4(3) . . . . no p3 p1 p2 c4 76.8(4) . . . . no c5 p1 p2 cu2 124.4(4) . . . . no c5 p1 p2 c2 -105.9(5) . . . . no c5 p1 p2 c4 -18.7(5) . . . . no cu1 p1 p3 c2 -102.4(3) . . . . no cu1 p1 p3 c3 171.6(3) . . . . no cu1 p1 p3 cu3 32.50(17) . . . 2_666 no p2 p1 p3 c2 10.3(3) . . . . no p2 p1 p3 c3 -75.8(3) . . . . no p2 p1 p3 cu3 145.11(14) . . . 2_666 no c5 p1 p3 c2 109.3(4) . . . . no c5 p1 p3 c3 23.2(4) . . . . no c5 p1 p3 cu3 -115.9(3) . . . 2_666 no cu1 p1 c5 p5 177.8(2) . . . . no cu1 p1 c5 c51 37.7(10) . . . . no p2 p1 c5 p5 36.6(5) . . . . no p2 p1 c5 c51 -103.4(7) . . . . no p3 p1 c5 p5 -45.9(5) . . . . no p3 p1 c5 c51 174.1(7) . . . . no cu2 p2 c2 p3 129.3(3) . . . . no cu2 p2 c2 p4 -136.4(3) . . . . no cu2 p2 c2 c11 -6.5(10) . . . . no p1 p2 c2 p3 11.9(4) . . . . no p1 p2 c2 p4 106.3(3) . . . . no p1 p2 c2 c11 -123.8(8) . . . . no c4 p2 c2 p3 -89.5(5) . . . . no c4 p2 c2 p4 4.9(4) . . . . no c4 p2 c2 c11 134.8(9) . . . . no cu2 p2 c4 p4 134.2(3) . . . . no cu2 p2 c4 p5 -137.3(4) . . . . no cu2 p2 c4 c41 10.3(13) . . . . no p1 p2 c4 p4 -92.6(4) . . . . no p1 p2 c4 p5 -4.1(6) . . . . no p1 p2 c4 c41 143.5(10) . . . . no c2 p2 c4 p4 -4.7(4) . . . . no c2 p2 c4 p5 83.9(6) . . . . no c2 p2 c4 c41 -128.6(10) . . . . no p1 p3 c2 p2 -12.1(4) . . . . no p1 p3 c2 p4 -107.3(4) . . . . no p1 p3 c2 c11 125.2(8) . . . . no c3 p3 c2 p2 87.8(5) . . . . no c3 p3 c2 p4 -7.4(5) . . . . no c3 p3 c2 c11 -134.9(9) . . . . no cu3 p3 c2 p2 -120.7(4) 2_666 . . . no cu3 p3 c2 p4 144.2(3) 2_666 . . . no cu3 p3 c2 c11 16.6(11) 2_666 . . . no p1 p3 c3 p4 95.8(4) . . . . no p1 p3 c3 p5 4.2(5) . . . . no p1 p3 c3 c31 -139.0(9) . . . . no c2 p3 c3 p4 7.2(5) . . . . no c2 p3 c3 p5 -84.4(6) . . . . no c2 p3 c3 c31 132.4(10) . . . . no cu3 p3 c3 p4 -144.6(3) 2_666 . . . no cu3 p3 c3 p5 123.8(4) 2_666 . . . no cu3 p3 c3 c31 -19.4(12) 2_666 . . . no c3 p4 c2 p2 -91.7(5) . . . . no c3 p4 c2 p3 7.3(5) . . . . no c3 p4 c2 c11 135.7(8) . . . . no c4 p4 c2 p2 -4.7(4) . . . . no c4 p4 c2 p3 94.4(5) . . . . no c4 p4 c2 c11 -137.3(8) . . . . no c2 p4 c3 p3 -7.3(5) . . . . no c2 p4 c3 p5 104.2(5) . . . . no c2 p4 c3 c31 -133.0(9) . . . . no c4 p4 c3 p3 -92.3(5) . . . . no c4 p4 c3 p5 19.2(4) . . . . no c4 p4 c3 c31 142.1(9) . . . . no c2 p4 c4 p2 4.8(4) . . . . no c2 p4 c4 p5 -105.8(4) . . . . no c2 p4 c4 c41 134.4(8) . . . . no c3 p4 c4 p2 91.8(5) . . . . no c3 p4 c4 p5 -18.7(4) . . . . no c3 p4 c4 c41 -138.6(8) . . . . no c4 p5 c3 p3 73.3(5) . . . . no c4 p5 c3 p4 -19.5(4) . . . . no c4 p5 c3 c31 -143.0(8) . . . . no c5 p5 c3 p3 -30.6(6) . . . . no c5 p5 c3 p4 -123.4(4) . . . . no c5 p5 c3 c31 113.2(8) . . . . no c3 p5 c4 p2 -73.1(6) . . . . no c3 p5 c4 p4 19.0(4) . . . . no c3 p5 c4 c41 137.4(9) . . . . no c5 p5 c4 p2 26.2(7) . . . . no c5 p5 c4 p4 118.3(5) . . . . no c5 p5 c4 c41 -123.4(9) . . . . no c3 p5 c5 p1 49.9(6) . . . . no c3 p5 c5 c51 -172.6(8) . . . . no c4 p5 c5 p1 -40.9(7) . . . . no c4 p5 c5 c51 96.7(9) . . . . no p2 c2 c11 c111 57.9(11) . . . . no p2 c2 c11 c112 -64.4(11) . . . . no p2 c2 c11 c113 180.0(7) . . . . no p3 c2 c11 c111 -68.8(11) . . . . no p3 c2 c11 c112 168.9(7) . . . . no p3 c2 c11 c113 53.3(11) . . . . no p4 c2 c11 c111 176.5(7) . . . . no p4 c2 c11 c112 54.2(11) . . . . no p4 c2 c11 c113 -61.4(10) . . . . no p3 c3 c31 c311 66.4(12) . . . . no p3 c3 c31 c312 -52.1(11) . . . . no p3 c3 c31 c313 -171.4(8) . . . . no p4 c3 c31 c311 177.7(8) . . . . no p4 c3 c31 c312 59.3(11) . . . . no p4 c3 c31 c313 -60.1(13) . . . . no p5 c3 c31 c311 -74.5(11) . . . . no p5 c3 c31 c312 167.1(7) . . . . no p5 c3 c31 c313 47.7(12) . . . . no p2 c4 c41 c411 170.5(9) . . . . no p2 c4 c41 c412 48.3(14) . . . . no p2 c4 c41 c413 -68.7(12) . . . . no p4 c4 c41 c411 57.7(12) . . . . no p4 c4 c41 c412 -64.5(10) . . . . no p4 c4 c41 c413 178.5(7) . . . . no p5 c4 c41 c411 -44.2(14) . . . . no p5 c4 c41 c412 -166.3(8) . . . . no p5 c4 c41 c413 76.7(10) . . . . no p1 c5 c51 c511 164.3(7) . . . . no p1 c5 c51 c512 44.3(11) . . . . no p1 c5 c51 c513 -75.9(10) . . . . no p5 c5 c51 c511 29.4(12) . . . . no p5 c5 c51 c512 -90.6(10) . . . . no p5 c5 c51 c513 149.2(8) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag i1 p1 3.880(3) . . no i1 p2 3.886(3) . . no i1 i1 4.1312(14) . 2_665 no i2 i2 3.9653(13) . 2_666 no i2 p3 3.856(3) . . no i2 cu1 4.0195(18) . . no i2 p1 3.890(3) . . no i2 p3 3.970(3) . 2_666 no i3 c1l 3.840(12) . 2_665 no i3 c1 3.726(14) . 2_665 no i1 h11a 3.3200 . . no i1 h41g 3.0100 . 2_665 no i2 h31a 3.2000 . . no i2 h11c 2.9800 . 2_666 no i3 h51i 3.1300 . . no i3 h1l3 3.1500 . 2_665 no i3 h31f 3.2200 . 2_666 no i3 h51h 3.3600 . 2_566 no cu1 i2 4.0195(18) . . no cu1 c512 4.114(11) . . no cu1 c513 4.168(11) . . no cu2 c112 4.098(12) . . no cu2 c412 3.882(10) . . no cu2 c111 3.900(11) . . no cu2 c413 4.117(10) . . no cu3 c312 4.066(10) . 2_666 no cu3 c311 4.030(9) . 2_666 no cu3 c113 4.125(11) . 2_666 no cu3 c111 4.194(9) . 2_666 no cu1 h51i 3.3200 . . no cu1 h51d 3.2500 . . no cu2 h51d 3.6800 . 2_665 no cu2 h11d 3.3000 . . no cu2 h41g 3.2900 . . no cu2 h11a 3.0300 . . no cu2 h41d 2.9900 . . no cu3 h1l2 3.6200 . 1_456 no cu3 h11c 3.3500 . 2_666 no cu3 h11i 3.2700 . 2_666 no cu3 h31a 3.1600 . 2_666 no cu3 h31f 3.2000 . 2_666 no p1 i1 3.880(3) . . no p1 cu2 3.712(3) . . no p1 cu3 4.264(3) . . no p1 cu3 3.504(4) . 2_666 no p2 i1 3.886(3) . . no p2 cu1 3.768(3) . . no p3 i2 3.856(3) . . no p1 h51i 3.0800 . . no p1 h51d 2.6600 . . no p2 h11a 3.0400 . . no p2 h41d 2.8100 . . no p2 h41g 3.0700 . . no p2 h11d 3.0700 . . no p3 h11c 3.1100 . . no p3 h11i 2.8600 . . no p3 h31a 2.9800 . . no p3 h31f 2.7900 . . no p4 h11e 2.7500 . . no p4 h11h 2.9200 . . no p4 h31d 2.9100 . . no p4 h31g 2.9800 . . no p4 h41b 2.9000 . . no p4 h41f 2.9100 . . no p5 h31c 3.0800 . . no p5 h31h 2.8200 . . no p5 h41a 2.8100 . . no p5 h41h 3.1300 . . no p5 h51a 3.1800 . . no p5 h51b 2.7900 . . no n1 h11d 2.6700 . . no c1 i3 3.726(14) . 2_665 no c1 c512 3.567(17) . 2_665 no c1l i3 3.840(12) . 2_665 no c1l c513 3.454(14) . 1_654 no c1 h11d 2.8700 . . no c1 h51d 3.0900 . 2_665 no c1l h51g 3.0800 . 1_654 no c111 cu2 3.900(11) . . no c111 cu3 4.194(9) . 2_666 no c112 cu2 4.098(12) . . no c113 cu3 4.125(11) . 2_666 no c111 h11b 2.9600 . 2_765 no c113 h51e 2.9900 . 1_655 no c113 h1l2 2.9600 . 2_765 no c311 cu3 4.030(9) . 2_666 no c312 cu3 4.066(10) . 2_666 no c412 cu2 3.882(10) . . no c413 cu2 4.117(10) . . no c411 h11h 3.0600 . 2_755 no c512 c1 3.567(17) . 2_665 no c512 cu1 4.114(11) . . no c413 h41h 3.0300 . 2_655 no c413 h51f 2.7300 . . no c513 cu1 4.168(11) . . no c513 c1l 3.454(14) . 1_456 no c513 h1l1 3.0900 . 1_456 no c513 h1l3 2.9400 . 1_456 no h1l1 c513 3.0900 . 1_654 no h1l1 h51g 2.4900 . 1_654 no h1l2 cu3 3.6200 . 1_654 no h1l2 c113 2.9600 . 2_765 no h1l2 h11i 2.4300 . 2_765 no h1l3 c513 2.9400 . 1_654 no h1l3 i3 3.1500 . 2_665 no h5a h51g 2.2800 . . no h11a i1 3.3200 . . no h11a cu2 3.0300 . . no h11a p2 3.0400 . . no h11a h11d 2.5100 . . no h11b h11f 2.5600 . . no h11b h11g 2.4900 . . no h11b c111 2.9600 . 2_765 no h11b h11b 2.2300 . 2_765 no h11c p3 3.1100 . . no h11c h11i 2.5600 . . no h11c i2 2.9800 . 2_666 no h11c cu3 3.3500 . 2_666 no h11d cu2 3.3000 . . no h11d p2 3.0700 . . no h11d n1 2.6700 . . no h11d c1 2.8700 . . no h11d h11a 2.5100 . . no h11e p4 2.7500 . . no h11e h11h 2.4600 . . no h11e h41b 2.4800 . 2_755 no h11f h11b 2.5600 . . no h11f h11g 2.5000 . . no h11g h11b 2.4900 . . no h11g h11f 2.5000 . . no h11g h51e 2.3100 . 1_655 no h11h p4 2.9200 . . no h11h h11e 2.4600 . . no h11h c411 3.0600 . 2_755 no h11h h41c 2.5600 . 2_755 no h11i p3 2.8600 . . no h11i h11c 2.5600 . . no h11i cu3 3.2700 . 2_666 no h11i h1l2 2.4300 . 2_765 no h31a i2 3.2000 . . no h31a p3 2.9800 . . no h31a h31f 2.5100 . . no h31a cu3 3.1600 . 2_666 no h31b h31e 2.5000 . . no h31b h31i 2.5000 . . no h31b h51a 2.5000 . 2_656 no h31c p5 3.0800 . . no h31c h31h 2.5500 . . no h31c h31c 2.5200 . 2_656 no h31d p4 2.9100 . . no h31d h31g 2.5000 . . no h31e h31b 2.5000 . . no h31e h31i 2.5200 . . no h31f p3 2.7900 . . no h31f h31a 2.5100 . . no h31f i3 3.2200 . 2_666 no h31f cu3 3.2000 . 2_666 no h31g p4 2.9800 . . no h31g h31d 2.5000 . . no h31h p5 2.8200 . . no h31h h31c 2.5500 . . no h31i h31b 2.5000 . . no h31i h31e 2.5200 . . no h41a p5 2.8100 . . no h41a h41h 2.5000 . . no h41b p4 2.9000 . . no h41b h41f 2.5500 . . no h41b h11e 2.4800 . 2_755 no h41c h41e 2.5200 . . no h41c h41i 2.4700 . . no h41c h11h 2.5600 . 2_755 no h41d cu2 2.9900 . . no h41d p2 2.8100 . . no h41d h41g 2.4700 . . no h41e h41c 2.5200 . . no h41e h41i 2.4400 . . no h41f p4 2.9100 . . no h41f h41b 2.5500 . . no h41g cu2 3.2900 . . no h41g p2 3.0700 . . no h41g h41d 2.4700 . . no h41g h51f 2.3500 . . no h41g i1 3.0100 . 2_665 no h41h p5 3.1300 . . no h41h h41a 2.5000 . . no h41h h51b 2.4800 . . no h41h h51f 2.2900 . . no h41h c413 3.0300 . 2_655 no h41h h41i 2.5600 . 2_655 no h41i h41c 2.4700 . . no h41i h41e 2.4400 . . no h41i h41h 2.5600 . 2_655 no h41i h51b 2.5700 . 2_655 no h51a p5 3.1800 . . no h51a h51g 2.5000 . . no h51a h31b 2.5000 . 2_656 no h51b p5 2.7900 . . no h51b h41h 2.4800 . . no h51b h51f 2.4800 . . no h51b h41i 2.5700 . 2_655 no h51c h51e 2.4900 . . no h51c h51h 2.4300 . . no h51d cu1 3.2500 . . no h51d p1 2.6600 . . no h51d h51i 2.5000 . . no h51d cu2 3.6800 . 2_665 no h51d c1 3.0900 . 2_665 no h51e c113 2.9900 . 1_455 no h51e h11g 2.3100 . 1_455 no h51e h51c 2.4900 . . no h51e h51h 2.4700 . . no h51f c413 2.7300 . . no h51f h41g 2.3500 . . no h51f h41h 2.2900 . . no h51f h51b 2.4800 . . no h51g c1l 3.0800 . 1_456 no h51g h1l1 2.4900 . 1_456 no h51g h5a 2.2800 . . no h51g h51a 2.5000 . . no h51h h51c 2.4300 . . no h51h h51e 2.4700 . . no h51h i3 3.3600 . 2_566 no h51i i3 3.1300 . . no h51i cu1 3.3200 . . no h51i p1 3.0800 . . no h51i h51d 2.5000 . . no loop_ _geom_hbond_atom_site_label_d _geom_hbond_atom_site_label_h _geom_hbond_atom_site_label_a _geom_hbond_distance_dh _geom_hbond_distance_ha _geom_hbond_distance_da _geom_hbond_angle_dha _geom_hbond_site_symmetry_a _geom_hbond_publ_flag # #d h a d - h h...a d...a d - h...a symm(a) # c111 h11c i2 0.9800 2.9800 3.909(9) 158.00 2_666 yes c112 h11e p4 0.9800 2.7500 3.237(11) 111.00 . yes c313 h31h p5 0.9800 2.8200 3.237(12) 107.00 . yes c411 h41a p5 0.9800 2.8100 3.230(11) 107.00 . yes c413 h41g i1 0.9800 3.0100 3.962(9) 166.00 2_665 yes c511 h51b p5 0.9800 2.7900 3.140(12) 102.00 . yes # loop mechanism for extra tables(s) #loop_ #_publ_manuscript_incl_extra_item #'_geom_extra_tablea_col_1' #'_geom_extra_tablea_col_2' #'_geom_extra_tablea_col_3' #'_geom_extra_table_head_a' #'_geom_table_footnote_a' #'_geom_extra_tableb_col_1' #'_geom_extra_tableb_col_2' #'_geom_extra_tableb_col_3' #'_geom_extra_table_head_b' #'_geom_table_footnote_b' # #loop_ #_geom_extra_tablea_col_1 #_geom_extra_tablea_col_2 #_geom_extra_tablea_col_3 # ? ? ? # #loop_ #_geom_extra_tableb_col_1 #_geom_extra_tableb_col_2 #_geom_extra_tableb_col_3 # ? ? ? # #_geom_table_footnote_a #; # ? #; # #_geom_table_footnote_b #; # ? #; # #_geom_table_footnote_a #; # ? #; # #_geom_table_footnote_b #; # ? #; #===end # Attachment 'compound3.cif' # CIF-file generated for u512_neu R = 0.04 #============================================================================== #=============================================================================== data_u512_neu _database_code_depnum_ccdc_archive 'CCDC 656702' # 0. AUDIT DETAILS _audit_creation_date 'Apr 13 16:08:54 2007' _audit_creation_method 'PLATON
option' _audit_update_record ; ; #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H78 Cu4 I4 N2 P8' # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_structural ? _chemical_formula_sum 'C22 H39 Cu2 I2 N P4' _chemical_formula_iupac ? _chemical_formula_weight 1644.64 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 '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' C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,1/2-y,1/2+z _cell_length_a 15.505(3) _cell_length_b 11.6415(18) _cell_length_c 18.001(3) _cell_angle_alpha 90 _cell_angle_beta 111.426(18) _cell_angle_gamma 90 _cell_volume 3024.7(10) _cell_formula_units_Z 2 _cell_measurement_temperature 104(1) _cell_measurement_reflns_used 6773 _cell_measurement_theta_min 2.6216 _cell_measurement_theta_max 51.2281 _cell_special_details ; ; _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.806 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 19.841 _exptl_crystal_density_meas_temp ? # Permitted for _exptl_absorpt_correction_type : # analytical 'analytical from crystal shape' # Example: de Meulenaer&Tompa: ABST # cylinder 'cylindrical' # gaussian 'Gaussian from crystal shape' # Example: PLATON/ABSG # integration 'integration from crystal shape' # multi-scan 'symmetry-related measurements' # Example: SADABS, MULABS # none 'no absorption corr. applied' # numerical 'numerical from crystal shape' # psi-scan 'psi-scan corrections' # Example: PLATON/ABSP # refdelf 'refined from delta-F' # Example: SHELXA, DIFABS, DELABS # sphere 'spherical' # Example: PLATON/ABSS _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.30.3 (release 12-05-2006 CrysAlis171 .NET) (compiled May 12 2006,14:43:55) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.49020 _exptl_absorpt_correction_T_max 1.39953 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ; _diffrn_ambient_temperature 104(1) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini Ultra' _diffrn_measurement_method omega-scan _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -28.00 23.00 1.0000 34.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 0.1529 45.0000 120.0000 0.0000 0.0000 51 #__ type_ start__ end____ width___ exp.time_ 2 omega -28.00 23.00 1.0000 34.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 0.1529 45.0000 0.0000 0.0000 0.0000 51 #__ type_ start__ end____ width___ exp.time_ 3 omega 23.00 78.00 1.0000 34.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 0.1529 75.0000 120.0000 0.0000 0.0000 55 #__ type_ start__ end____ width___ exp.time_ 4 omega 25.00 77.00 1.0000 34.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 0.1529 35.0000 -149.0000 0.0000 0.0000 52 #__ type_ start__ end____ width___ exp.time_ 5 omega -83.00 -28.00 1.0000 34.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -60.8272 -72.0000 257.0000 0.0000 0.0000 55 #__ type_ start__ end____ width___ exp.time_ 6 omega -89.00 -38.00 1.0000 34.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -60.8272 45.0000 240.0000 0.0000 0.0000 51 #__ type_ start__ end____ width___ exp.time_ 7 omega -108.00 -56.00 1.0000 34.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -60.8272 108.0000 217.0000 0.0000 0.0000 52 #__ type_ start__ end____ width___ exp.time_ 8 omega -139.00 -84.00 1.0000 34.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -60.8272 -75.0000 240.0000 0.0000 0.0000 55 #__ type_ start__ end____ width___ exp.time_ 9 omega -83.00 -30.00 1.0000 34.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -60.8272 -65.0000 60.0000 0.0000 0.0000 53 #__ type_ start__ end____ width___ exp.time_ 10 omega -70.00 -29.00 1.0000 34.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -60.8272 -69.0000 159.0000 0.0000 0.0000 41 #__ type_ start__ end____ width___ exp.time_ 11 omega 86.00 137.00 1.0000 34.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 62.4840 45.0000 0.0000 0.0000 0.0000 51 #__ type_ start__ end____ width___ exp.time_ 12 omega 39.00 90.00 1.0000 34.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 62.4840 -45.0000 240.0000 0.0000 0.0000 51 #__ type_ start__ end____ width___ exp.time_ 13 omega 35.00 63.00 1.0000 34.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 62.4840 35.0000 30.0000 0.0000 0.0000 28 #__ type_ start__ end____ width___ exp.time_ 14 omega 41.00 84.00 1.0000 34.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 62.4840 67.0000 183.0000 0.0000 0.0000 43 #__ type_ start__ end____ width___ exp.time_ 15 omega -12.00 38.00 1.0000 34.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 62.4840 -35.0000 149.0000 0.0000 0.0000 50 #__ type_ start__ end____ width___ exp.time_ 16 omega 86.00 137.00 1.0000 34.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 62.4840 45.0000 240.0000 0.0000 0.0000 51 #__ type_ start__ end____ width___ exp.time_ 17 omega 43.00 90.00 1.0000 34.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 62.4840 -35.0000 149.0000 0.0000 0.0000 47 #__ type_ start__ end____ width___ exp.time_ 18 omega 85.00 136.00 1.0000 34.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 62.4840 55.0000 110.0000 0.0000 0.0000 51 ; _diffrn_detector_area_resol_mean 10.5431 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 13212 _diffrn_reflns_av_R_equivalents 0.0466 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 51.53 _diffrn_reflns_theta_full 51.53 _diffrn_measured_fraction_theta_max 0.981 _diffrn_measured_fraction_theta_full 0.981 _diffrn_reflns_reduction_process ; ; # number of unique reflections _reflns_number_total 3267 # number of observed reflections (> n sig(I)) _reflns_number_gt 2433 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.30.3 (release 12-05-2006 CrysAlis171 .NET) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.30.3 (release 12-05-2006 CrysAlis171 .NET) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.30.3 (release 12-05-2006 CrysAlis171 .NET) ; _computing_structure_solution 'SIR-97 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating -R-factor-obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0713P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # Permitted for _refine_ls_hydrogen_treatment : # refall - refined all H parameters # refxyz - refined H coordinates only # refU - refined H U only # noref - no refinement of H parameters # constr - H parameters constrained # mixed - some constrained, some independent # undef - H-atom parameters not defined _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack . _refine_ls_number_reflns 3267 _refine_ls_number_parameters 293 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0536 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.1000 _refine_ls_wR_factor_gt 0.0963 _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_restrained_S_all 0.937 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.941 _refine_diff_density_min -0.657 _refine_diff_density_rms 0.120 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags I1 I Uani 0.88461(4) 0.71574(5) 0.03083(4) 1.000 0.0478(2) . . I2 I Uani 0.96547(3) 1.06967(5) 0.08734(3) 1.000 0.0430(2) . . Cu1 Cu Uani 1.00529(8) 0.84611(11) 0.13498(8) 1.000 0.0494(5) . . Cu2 Cu Uani 0.89483(8) 0.91280(10) -0.03188(8) 1.000 0.0483(5) . . P1 P Uani 1.15336(15) 0.84045(19) 0.14572(15) 1.000 0.0462(9) . . P2 P Uani 0.77742(14) 1.00649(19) -0.12515(14) 1.000 0.0424(8) . . P3 P Uani 0.59568(17) 0.9568(2) -0.19219(17) 1.000 0.0613(10) . . P4 P Uani 1.35965(15) 0.8160(2) 0.19037(15) 1.000 0.0482(9) . . N1 N Uani 0.9976(5) 0.8496(6) 0.2444(5) 1.000 0.048(3) . . C1 C Uani 1.2464(5) 0.7527(7) 0.1827(5) 1.000 0.042(3) . . C2 C Uani 0.6728(5) 1.0685(7) -0.1154(5) 1.000 0.047(3) . . C3 C Uani 0.6978(6) 0.9641(8) -0.2269(6) 1.000 0.061(4) . . C4 C Uani 0.6222(6) 1.0603(8) -0.2624(6) 1.000 0.054(3) . . C5 C Uani 1.2372(6) 0.6273(8) 0.2027(6) 1.000 0.051(4) . . C6 C Uani 1.2214(7) 0.5586(8) 0.1265(6) 1.000 0.077(5) . . C7 C Uani 1.3264(6) 0.5823(8) 0.2676(6) 1.000 0.066(4) . . C8 C Uani 1.1582(6) 0.6091(8) 0.2323(6) 1.000 0.070(4) . . C9 C Uani 0.6585(6) 1.0839(8) -0.0374(6) 1.000 0.051(4) . . C10 C Uani 0.6877(6) 0.9769(9) 0.0149(6) 1.000 0.065(4) . . C11 C Uani 0.5541(5) 1.1088(9) -0.0543(6) 1.000 0.069(4) . . C12 C Uani 0.7155(6) 1.1904(9) 0.0059(6) 1.000 0.063(4) . . C13 C Uani 0.7334(6) 0.8714(8) -0.2696(6) 1.000 0.056(4) . . C14 C Uani 0.7737(7) 0.7713(8) -0.2111(6) 1.000 0.066(4) . . C15 C Uani 0.8135(6) 0.9228(8) -0.2912(6) 1.000 0.071(4) . . C16 C Uani 0.6625(6) 0.8145(8) -0.3443(6) 1.000 0.075(4) . . C17 C Uani 0.5529(6) 1.0808(8) -0.3486(6) 1.000 0.060(4) . . C18 C Uani 0.4934(7) 1.1822(10) -0.3506(6) 1.000 0.093(5) . . C19 C Uani 0.4841(6) 0.9799(9) -0.3821(6) 1.000 0.079(4) . . C20 C Uani 0.6078(8) 1.1056(9) -0.4009(6) 1.000 0.082(5) . . C100 C Uani 1.0109(6) 0.8664(8) 0.3078(7) 1.000 0.046(3) . . C101 C Uani 1.0288(6) 0.8897(8) 0.3905(6) 1.000 0.067(4) . . H6A H Uiso 1.22650 0.47630 0.13900 1.000 0.1150 calc R H6B H Uiso 1.26810 0.58000 0.10420 1.000 0.1150 calc R H6C H Uiso 1.15940 0.57520 0.08750 1.000 0.1150 calc R H7A H Uiso 1.31890 0.50080 0.27750 1.000 0.0980 calc R H7B H Uiso 1.33850 0.62600 0.31690 1.000 0.0980 calc R H7C H Uiso 1.37860 0.59160 0.24960 1.000 0.0980 calc R H8A H Uiso 1.15690 0.52860 0.24760 1.000 0.1050 calc R H8B H Uiso 1.09930 0.62870 0.18970 1.000 0.1050 calc R H8C H Uiso 1.16730 0.65850 0.27870 1.000 0.1050 calc R H10A H Uiso 0.67350 0.98750 0.06330 1.000 0.0980 calc R H10B H Uiso 0.75440 0.96460 0.02980 1.000 0.0980 calc R H10C H Uiso 0.65390 0.91000 -0.01460 1.000 0.0980 calc R H10D H Uiso 0.97780 0.85960 0.40470 1.000 0.1010 calc R H10E H Uiso 1.03390 0.97290 0.39960 1.000 0.1010 calc R H10F H Uiso 1.08690 0.85260 0.42360 1.000 0.1010 calc R H11A H Uiso 0.54500 1.11900 -0.00360 1.000 0.1040 calc R H11B H Uiso 0.51650 1.04410 -0.08350 1.000 0.1040 calc R H11C H Uiso 0.53540 1.17890 -0.08630 1.000 0.1040 calc R H12A H Uiso 0.70810 1.20110 0.05720 1.000 0.0940 calc R H12B H Uiso 0.69310 1.25890 -0.02730 1.000 0.0940 calc R H12C H Uiso 0.78110 1.17830 0.01490 1.000 0.0940 calc R H14A H Uiso 0.78890 0.70730 -0.23950 1.000 0.0990 calc R H14B H Uiso 0.72790 0.74600 -0.18880 1.000 0.0990 calc R H14C H Uiso 0.82990 0.79700 -0.16780 1.000 0.0990 calc R H15A H Uiso 0.83910 0.86330 -0.31570 1.000 0.1080 calc R H15B H Uiso 0.86210 0.95120 -0.24260 1.000 0.1080 calc R H15C H Uiso 0.78980 0.98640 -0.32880 1.000 0.1080 calc R H16A H Uiso 0.69330 0.75430 -0.36360 1.000 0.1120 calc R H16B H Uiso 0.63690 0.87250 -0.38610 1.000 0.1120 calc R H16C H Uiso 0.61240 0.78050 -0.33070 1.000 0.1120 calc R H18A H Uiso 0.45850 1.16800 -0.31580 1.000 0.1390 calc R H18B H Uiso 0.45020 1.19480 -0.40530 1.000 0.1390 calc R H18C H Uiso 0.53250 1.25030 -0.33190 1.000 0.1390 calc R H19A H Uiso 0.50860 0.92760 -0.41220 1.000 0.1180 calc R H19B H Uiso 0.42410 1.01030 -0.41730 1.000 0.1180 calc R H19C H Uiso 0.47600 0.93820 -0.33770 1.000 0.1180 calc R H20A H Uiso 0.63430 1.03400 -0.41160 1.000 0.1240 calc R H20B H Uiso 0.65780 1.15970 -0.37360 1.000 0.1240 calc R H20C H Uiso 0.56690 1.13930 -0.45130 1.000 0.1240 calc 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 I1 0.0545(4) 0.0368(4) 0.0556(4) 0.0023(3) 0.0242(3) -0.0044(3) I2 0.0410(3) 0.0359(4) 0.0566(4) -0.0008(3) 0.0233(3) 0.0010(3) Cu1 0.0465(7) 0.0457(8) 0.0617(9) 0.0026(7) 0.0267(7) -0.0016(6) Cu2 0.0466(7) 0.0397(8) 0.0625(10) 0.0045(7) 0.0245(7) 0.0003(6) P1 0.0426(13) 0.0378(14) 0.0638(17) 0.0041(13) 0.0260(12) -0.0004(11) P2 0.0429(13) 0.0380(14) 0.0516(16) 0.0016(12) 0.0237(12) 0.0000(11) P3 0.0503(15) 0.0568(17) 0.075(2) 0.0016(15) 0.0208(14) -0.0053(13) P4 0.0420(13) 0.0491(15) 0.0550(17) 0.0013(13) 0.0195(12) -0.0001(12) N1 0.051(5) 0.046(5) 0.055(6) 0.009(5) 0.028(5) 0.006(4) C1 0.039(5) 0.038(5) 0.049(6) 0.004(5) 0.017(4) 0.003(4) C2 0.035(5) 0.050(6) 0.055(6) 0.001(5) 0.015(5) 0.002(4) C3 0.055(6) 0.046(6) 0.080(8) -0.021(6) 0.024(6) -0.006(5) C4 0.046(5) 0.049(6) 0.055(7) -0.001(5) 0.006(5) -0.001(5) C5 0.054(6) 0.044(6) 0.058(7) 0.006(6) 0.025(5) 0.011(5) C6 0.107(9) 0.044(7) 0.072(8) 0.002(6) 0.025(7) -0.006(6) C7 0.058(6) 0.054(7) 0.081(8) 0.015(6) 0.020(6) -0.001(5) C8 0.059(6) 0.057(7) 0.101(9) 0.016(6) 0.036(6) 0.004(5) C9 0.047(6) 0.054(6) 0.062(7) 0.016(6) 0.031(5) 0.015(5) C10 0.061(6) 0.080(8) 0.069(7) 0.016(6) 0.040(6) 0.018(6) C11 0.047(6) 0.085(8) 0.086(8) 0.014(7) 0.036(6) 0.013(6) C12 0.059(6) 0.079(8) 0.050(7) -0.006(6) 0.019(5) 0.014(6) C13 0.059(6) 0.055(7) 0.057(7) -0.010(6) 0.025(5) -0.008(5) C14 0.074(7) 0.046(6) 0.085(8) -0.006(6) 0.037(6) 0.002(5) C15 0.074(7) 0.075(8) 0.078(8) -0.016(6) 0.043(6) -0.011(6) C16 0.065(7) 0.056(7) 0.090(9) -0.027(6) 0.013(6) 0.003(6) C17 0.060(6) 0.054(7) 0.065(7) -0.005(6) 0.021(6) -0.011(6) C18 0.088(8) 0.071(8) 0.075(9) -0.008(7) -0.022(6) 0.013(7) C19 0.059(7) 0.070(8) 0.092(8) 0.001(7) 0.008(6) 0.001(6) C20 0.102(8) 0.083(9) 0.055(7) 0.006(6) 0.020(7) -0.023(7) C100 0.041(5) 0.050(6) 0.052(7) -0.001(6) 0.023(6) -0.007(5) C101 0.085(7) 0.041(6) 0.082(9) -0.018(6) 0.038(7) -0.012(5) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Cu1 2.5993(16) . . yes I1 Cu2 2.5871(14) . . yes I2 Cu1 2.7392(15) . . yes I2 Cu2 2.7245(15) . . yes I2 Cu2 2.7037(15) . 3_775 yes Cu1 P1 2.233(3) . . yes Cu1 N1 2.017(8) . . yes Cu2 P2 2.256(3) . . yes P1 C1 1.693(9) . . yes P1 P2 2.180(3) . 3_775 yes P2 C2 1.842(9) . . yes P2 C3 1.863(10) . . yes P3 C2 1.956(9) . . yes P3 C3 1.905(10) . . yes P3 C4 1.897(10) . . yes P4 C1 1.862(9) . . yes P4 C2 1.840(9) . 3_775 yes P4 C4 1.889(10) . 3_775 yes N1 C100 1.101(14) . . yes C1 C5 1.523(12) . . no C2 C9 1.510(13) . . no C3 C4 1.578(14) . . no C3 C13 1.540(14) . . no C4 C17 1.550(14) . . no C5 C6 1.528(14) . . no C5 C7 1.540(14) . . no C5 C8 1.519(14) . . no C9 C10 1.527(14) . . no C9 C11 1.561(13) . . no C9 C12 1.556(14) . . no C13 C14 1.542(14) . . no C13 C15 1.551(14) . . no C13 C16 1.541(14) . . no C17 C18 1.491(15) . . no C17 C19 1.553(14) . . no C17 C20 1.510(16) . . no C100 C101 1.437(15) . . no C6 H6A 0.9800 . . no C6 H6B 0.9800 . . no C6 H6C 0.9800 . . no C7 H7A 0.9800 . . no C7 H7B 0.9800 . . no C7 H7C 0.9800 . . no C8 H8A 0.9800 . . no C8 H8B 0.9800 . . no C8 H8C 0.9800 . . no C10 H10A 0.9800 . . no C10 H10B 0.9800 . . no C10 H10C 0.9800 . . no C11 H11A 0.9800 . . no C11 H11B 0.9800 . . no C11 H11C 0.9800 . . no C12 H12A 0.9800 . . no C12 H12B 0.9800 . . no C12 H12C 0.9800 . . no C14 H14A 0.9800 . . no C14 H14B 0.9800 . . no C14 H14C 0.9800 . . no C15 H15A 0.9800 . . no C15 H15B 0.9800 . . no C15 H15C 0.9800 . . no C16 H16A 0.9800 . . no C16 H16B 0.9800 . . no C16 H16C 0.9800 . . no C18 H18A 0.9800 . . no C18 H18B 0.9800 . . no C18 H18C 0.9800 . . no C19 H19A 0.9800 . . no C19 H19B 0.9800 . . no C19 H19C 0.9800 . . no C20 H20A 0.9800 . . no C20 H20B 0.9800 . . no C20 H20C 0.9800 . . no C101 H10D 0.9800 . . no C101 H10E 0.9800 . . no C101 H10F 0.9800 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cu1 I1 Cu2 69.77(5) . . . yes Cu1 I2 Cu2 65.77(4) . . . yes Cu1 I2 Cu2 93.90(4) . . 3_775 yes Cu2 I2 Cu2 84.58(5) . . 3_775 yes I1 Cu1 I2 107.96(5) . . . yes I1 Cu1 P1 119.44(8) . . . yes I1 Cu1 N1 115.6(2) . . . yes I2 Cu1 P1 99.33(8) . . . yes I2 Cu1 N1 101.5(2) . . . yes P1 Cu1 N1 110.0(3) . . . yes I1 Cu2 I2 108.77(5) . . . yes I1 Cu2 P2 126.30(8) . . . yes I1 Cu2 I2 114.40(5) . . 3_775 yes I2 Cu2 P2 104.19(8) . . . yes I2 Cu2 I2 95.42(5) . . 3_775 yes I2 Cu2 P2 103.08(8) 3_775 . . yes Cu1 P1 C1 138.9(3) . . . yes Cu1 P1 P2 121.02(13) . . 3_775 yes P2 P1 C1 99.1(3) 3_775 . . yes Cu2 P2 C2 128.2(3) . . . yes Cu2 P2 C3 132.0(3) . . . yes Cu2 P2 P1 102.01(12) . . 3_775 yes C2 P2 C3 84.7(4) . . . yes P1 P2 C2 101.6(3) 3_775 . . yes P1 P2 C3 103.9(3) 3_775 . . yes C2 P3 C3 80.5(4) . . . yes C2 P3 C4 79.8(4) . . . yes C3 P3 C4 49.0(4) . . . yes C1 P4 C2 103.7(4) . . 3_775 yes C1 P4 C4 104.6(4) . . 3_775 yes C2 P4 C4 83.0(4) 3_775 . 3_775 yes Cu1 N1 C100 163.9(8) . . . yes P1 C1 P4 115.8(5) . . . yes P1 C1 C5 122.1(7) . . . yes P4 C1 C5 121.9(6) . . . yes P2 C2 P3 90.3(4) . . . yes P2 C2 C9 124.7(6) . . . yes P2 C2 P4 103.4(4) . . 3_775 yes P3 C2 C9 118.5(6) . . . yes P3 C2 P4 92.0(4) . . 3_775 yes P4 C2 C9 120.1(6) 3_775 . . yes P2 C3 P3 91.2(5) . . . yes P2 C3 C4 109.7(6) . . . yes P2 C3 C13 116.5(7) . . . yes P3 C3 C4 65.2(5) . . . yes P3 C3 C13 128.7(7) . . . yes C4 C3 C13 130.1(8) . . . no P3 C4 C3 65.7(5) . . . yes P3 C4 C17 121.7(7) . . . yes P3 C4 P4 92.4(5) . . 3_775 yes C3 C4 C17 131.0(8) . . . no P4 C4 C3 111.2(7) 3_775 . . yes P4 C4 C17 116.4(7) 3_775 . . yes C1 C5 C6 106.7(8) . . . no C1 C5 C7 111.7(8) . . . no C1 C5 C8 112.0(8) . . . no C6 C5 C7 107.9(8) . . . no C6 C5 C8 110.9(8) . . . no C7 C5 C8 107.6(8) . . . no C2 C9 C10 111.4(8) . . . no C2 C9 C11 109.6(8) . . . no C2 C9 C12 108.1(8) . . . no C10 C9 C11 108.9(8) . . . no C10 C9 C12 110.8(8) . . . no C11 C9 C12 108.0(8) . . . no C3 C13 C14 108.6(8) . . . no C3 C13 C15 108.7(8) . . . no C3 C13 C16 117.7(8) . . . no C14 C13 C15 107.5(8) . . . no C14 C13 C16 104.7(8) . . . no C15 C13 C16 109.2(8) . . . no C4 C17 C18 110.1(8) . . . no C4 C17 C19 113.5(8) . . . no C4 C17 C20 108.1(8) . . . no C18 C17 C19 105.0(8) . . . no C18 C17 C20 108.6(8) . . . no C19 C17 C20 111.5(8) . . . no N1 C100 C101 179.3(13) . . . yes C5 C6 H6A 109.00 . . . no C5 C6 H6B 110.00 . . . no C5 C6 H6C 109.00 . . . no H6A C6 H6B 109.00 . . . no H6A C6 H6C 109.00 . . . no H6B C6 H6C 110.00 . . . no C5 C7 H7A 110.00 . . . no C5 C7 H7B 109.00 . . . no C5 C7 H7C 109.00 . . . no H7A C7 H7B 110.00 . . . no H7A C7 H7C 109.00 . . . no H7B C7 H7C 109.00 . . . no C5 C8 H8A 110.00 . . . no C5 C8 H8B 109.00 . . . no C5 C8 H8C 109.00 . . . no H8A C8 H8B 109.00 . . . no H8A C8 H8C 109.00 . . . no H8B C8 H8C 109.00 . . . no C9 C10 H10A 109.00 . . . no C9 C10 H10B 109.00 . . . no C9 C10 H10C 110.00 . . . no H10A C10 H10B 109.00 . . . no H10A C10 H10C 109.00 . . . no H10B C10 H10C 110.00 . . . no C9 C11 H11A 109.00 . . . no C9 C11 H11B 109.00 . . . no C9 C11 H11C 109.00 . . . no H11A C11 H11B 109.00 . . . no H11A C11 H11C 110.00 . . . no H11B C11 H11C 110.00 . . . no C9 C12 H12A 109.00 . . . no C9 C12 H12B 109.00 . . . no C9 C12 H12C 109.00 . . . no H12A C12 H12B 109.00 . . . no H12A C12 H12C 110.00 . . . no H12B C12 H12C 109.00 . . . no C13 C14 H14A 109.00 . . . no C13 C14 H14B 109.00 . . . no C13 C14 H14C 109.00 . . . no H14A C14 H14B 109.00 . . . no H14A C14 H14C 109.00 . . . no H14B C14 H14C 109.00 . . . no C13 C15 H15A 109.00 . . . no C13 C15 H15B 109.00 . . . no C13 C15 H15C 109.00 . . . no H15A C15 H15B 110.00 . . . no H15A C15 H15C 110.00 . . . no H15B C15 H15C 109.00 . . . no C13 C16 H16A 109.00 . . . no C13 C16 H16B 109.00 . . . no C13 C16 H16C 109.00 . . . no H16A C16 H16B 109.00 . . . no H16A C16 H16C 109.00 . . . no H16B C16 H16C 110.00 . . . no C17 C18 H18A 109.00 . . . no C17 C18 H18B 109.00 . . . no C17 C18 H18C 109.00 . . . no H18A C18 H18B 109.00 . . . no H18A C18 H18C 109.00 . . . no H18B C18 H18C 110.00 . . . no C17 C19 H19A 110.00 . . . no C17 C19 H19B 109.00 . . . no C17 C19 H19C 109.00 . . . no H19A C19 H19B 110.00 . . . no H19A C19 H19C 110.00 . . . no H19B C19 H19C 109.00 . . . no C17 C20 H20A 109.00 . . . no C17 C20 H20B 109.00 . . . no C17 C20 H20C 109.00 . . . no H20A C20 H20B 109.00 . . . no H20A C20 H20C 110.00 . . . no H20B C20 H20C 109.00 . . . no C100 C101 H10D 109.00 . . . no C100 C101 H10E 109.00 . . . no C100 C101 H10F 109.00 . . . no H10D C101 H10E 109.00 . . . no H10D C101 H10F 109.00 . . . no H10E C101 H10F 109.00 . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cu2 I1 Cu1 I2 21.62(5) . . . . no Cu2 I1 Cu1 P1 -90.63(10) . . . . no Cu2 I1 Cu1 N1 134.5(3) . . . . no Cu1 I1 Cu2 I2 83.44(6) . . . 3_775 no Cu1 I1 Cu2 I2 -21.85(5) . . . . no Cu1 I1 Cu2 P2 -146.66(11) . . . . no Cu2 I2 Cu1 I1 -103.37(6) 3_775 . . . no Cu2 I2 Cu1 N1 -143.1(3) . . . . no Cu2 I2 Cu1 P1 104.13(9) . . . . no Cu2 I2 Cu1 P1 21.86(8) 3_775 . . . no Cu2 I2 Cu1 I1 -21.11(5) . . . . no Cu1 I2 Cu2 I1 21.31(5) . . . . no Cu2 I2 Cu2 I1 118.07(6) 3_775 . . . no Cu1 I2 Cu2 P2 158.27(9) . . . . no Cu2 I2 Cu2 P2 -104.97(8) 3_775 . . . no Cu2 I2 Cu1 N1 134.6(2) 3_775 . . . no Cu2 I2 Cu2 I2 0.00(7) 3_775 . . 3_775 no Cu2 I2 Cu2 P2 105.95(8) 3_775 3_775 . . no Cu1 I2 Cu2 I2 -65.18(5) 3_775 3_775 . . no Cu1 I2 Cu2 I1 -178.63(6) 3_775 3_775 . . no Cu2 I2 Cu2 I1 -113.45(6) 3_775 3_775 . . no Cu1 I2 Cu2 I2 -96.75(5) . . . 3_775 no Cu1 I2 Cu2 P2 40.77(8) 3_775 3_775 . . no Cu2 I2 Cu2 I2 -0.02(8) 3_775 3_775 . . no I2 Cu1 P1 C1 168.7(5) . . . . no I1 Cu1 P1 P2 119.78(13) . . . 3_775 no N1 Cu1 P1 P2 -103.0(3) . . . 3_775 no N1 Cu1 P1 C1 62.7(5) . . . . no I2 Cu1 P1 P2 2.93(16) . . . 3_775 no I1 Cu1 P1 C1 -74.5(5) . . . . no I1 Cu2 P2 C3 -57.1(5) . . . . no I1 Cu2 P2 C2 66.1(4) . . . . no I2 Cu2 P2 P1 -44.30(12) 3_775 . . 3_775 no I1 Cu2 P2 P1 -178.47(9) . . . 3_775 no I2 Cu2 P2 C2 -60.6(4) . . . . no I2 Cu2 P2 C3 176.2(4) . . . . no I2 Cu2 P2 P1 54.84(12) . . . 3_775 no I2 Cu2 P2 C2 -159.7(3) 3_775 . . . no I2 Cu2 P2 C3 77.1(4) 3_775 . . . no Cu1 P1 C1 P4 -167.6(2) . . . . no Cu1 P1 C1 C5 16.7(10) . . . . no P2 P1 C1 P4 0.1(5) 3_775 . . . no P2 P1 C1 C5 -175.6(7) 3_775 . . . no Cu1 P1 P2 Cu2 -32.06(17) . . 3_775 3_775 no Cu1 P1 P2 C2 -165.6(3) . . 3_775 3_775 no Cu1 P1 P2 C3 107.1(3) . . 3_775 3_775 no C1 P1 P2 Cu2 157.4(3) . . 3_775 3_775 no C1 P1 P2 C2 23.9(4) . . 3_775 3_775 no C1 P1 P2 C3 -63.5(4) . . 3_775 3_775 no Cu2 P2 C2 P3 -114.1(3) . . . . no Cu2 P2 C2 C9 11.6(9) . . . . no Cu2 P2 C2 P4 153.8(2) . . . 3_775 no C3 P2 C2 P3 27.2(4) . . . . no C3 P2 C2 C9 152.9(8) . . . . no C3 P2 C2 P4 -64.9(4) . . . 3_775 no P1 P2 C2 P3 130.4(2) 3_775 . . . no P1 P2 C2 C9 -104.0(7) 3_775 . . . no P1 P2 C2 P4 38.3(4) 3_775 . . 3_775 no Cu2 P2 C3 P3 110.6(4) . . . . no Cu2 P2 C3 C4 174.7(5) . . . . no Cu2 P2 C3 C13 -24.6(9) . . . . no C2 P2 C3 P3 -28.0(4) . . . . no C2 P2 C3 C4 36.0(7) . . . . no C2 P2 C3 C13 -163.2(8) . . . . no P1 P2 C3 P3 -128.7(3) 3_775 . . . no P1 P2 C3 C4 -64.7(7) 3_775 . . . no P1 P2 C3 C13 96.1(7) 3_775 . . . no C3 P3 C2 P2 -26.9(4) . . . . no C3 P3 C2 C9 -157.4(7) . . . . no C3 P3 C2 P4 76.5(4) . . . 3_775 no C4 P3 C2 P2 -76.7(4) . . . . no C4 P3 C2 C9 152.8(7) . . . . no C4 P3 C2 P4 26.7(4) . . . 3_775 no C2 P3 C3 P2 26.5(4) . . . . no C2 P3 C3 C4 -84.7(5) . . . . no C2 P3 C3 C13 152.7(9) . . . . no C4 P3 C3 P2 111.2(6) . . . . no C4 P3 C3 C13 -122.6(11) . . . . no C2 P3 C4 C3 86.2(5) . . . . no C2 P3 C4 C17 -149.2(8) . . . . no C2 P3 C4 P4 -26.0(4) . . . 3_775 no C3 P3 C4 C17 124.5(10) . . . . no C3 P3 C4 P4 -112.2(6) . . . 3_775 no C2 P4 C1 P1 -24.2(6) 3_775 . . . no C2 P4 C1 C5 151.5(7) 3_775 . . . no C4 P4 C1 P1 62.1(6) 3_775 . . . no C4 P4 C1 C5 -122.3(7) 3_775 . . . no C1 P4 C2 P2 39.3(5) . . 3_775 3_775 no C1 P4 C2 P3 130.0(4) . . 3_775 3_775 no C1 P4 C2 C9 -105.2(7) . . 3_775 3_775 no C1 P4 C4 P3 -129.9(4) . . 3_775 3_775 no C1 P4 C4 C3 -65.0(7) . . 3_775 3_775 no C1 P4 C4 C17 102.7(7) . . 3_775 3_775 no P1 C1 C5 C6 88.3(9) . . . . no P1 C1 C5 C7 -154.0(7) . . . . no P1 C1 C5 C8 -33.2(11) . . . . no P4 C1 C5 C6 -87.1(9) . . . . no P4 C1 C5 C7 30.6(11) . . . . no P4 C1 C5 C8 151.4(7) . . . . no P2 C2 C9 C10 -45.0(11) . . . . no P2 C2 C9 C11 -165.6(6) . . . . no P2 C2 C9 C12 77.0(9) . . . . no P3 C2 C9 C10 67.5(9) . . . . no P3 C2 C9 C11 -53.2(9) . . . . no P3 C2 C9 C12 -170.6(6) . . . . no P4 C2 C9 C10 178.6(6) 3_775 . . . no P4 C2 C9 C11 57.9(9) 3_775 . . . no P4 C2 C9 C12 -59.5(9) 3_775 . . . no P2 C3 C4 P3 -81.9(5) . . . . no P2 C3 C4 C17 166.3(8) . . . . no P2 C3 C4 P4 0.9(8) . . . 3_775 no P3 C3 C4 C17 -111.8(10) . . . . no P3 C3 C4 P4 82.8(5) . . . 3_775 no C13 C3 C4 P3 120.8(10) . . . . no C13 C3 C4 C17 9.0(17) . . . . no C13 C3 C4 P4 -156.5(8) . . . 3_775 no P2 C3 C13 C14 47.6(10) . . . . no P2 C3 C13 C15 -69.1(9) . . . . no P2 C3 C13 C16 166.2(7) . . . . no P3 C3 C13 C14 -67.9(11) . . . . no P3 C3 C13 C15 175.5(7) . . . . no P3 C3 C13 C16 50.7(12) . . . . no C4 C3 C13 C14 -156.3(10) . . . . no C4 C3 C13 C15 87.0(12) . . . . no C4 C3 C13 C16 -37.7(14) . . . . no P3 C4 C17 C18 94.0(9) . . . . no P3 C4 C17 C19 -23.3(11) . . . . no P3 C4 C17 C20 -147.5(7) . . . . no C3 C4 C17 C18 178.1(10) . . . . no C3 C4 C17 C19 60.8(13) . . . . no C3 C4 C17 C20 -63.5(13) . . . . no P4 C4 C17 C18 -17.1(11) 3_775 . . . no P4 C4 C17 C19 -134.4(7) 3_775 . . . no P4 C4 C17 C20 101.3(8) 3_775 . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag I2 P1 3.805(3) . . no I2 P2 3.940(3) . . no I2 C101 3.745(9) . 2_755 no I2 C12 3.872(10) . . no I2 I2 4.0156(11) . 3_775 no I2 N1 3.712(8) . . no I2 P2 3.894(3) . 3_775 no I2 Cu1 4.3021(17) . 3_775 no I1 H10D 3.2300 . 4_564 no I1 H10E 3.1600 . 2_745 no I1 H15A 3.2300 . 4_565 no I2 H10B 3.2900 . . no I2 H12C 2.9600 . . no I2 H14C 3.3500 . 3_775 no I2 H15B 3.0900 . 3_775 no Cu1 C8 3.643(10) . . no Cu1 C15 4.155(10) . 3_775 no Cu1 I2 4.3021(17) . 3_775 no Cu2 C14 3.496(10) . . no Cu2 P1 4.200(3) . . no Cu2 C10 3.682(10) . . no Cu1 H8C 3.6100 . . no Cu1 H15B 3.2600 . 3_775 no Cu1 H8B 2.9100 . . no Cu2 H10B 2.8500 . . no Cu2 H14B 3.6200 . . no Cu2 H14C 2.6500 . . no Cu2 H15B 3.6700 . . no P1 I2 3.805(3) . . no P1 Cu2 4.200(3) . . no P1 N1 3.483(9) . . no P1 Cu2 3.448(3) . 3_775 no P2 Cu1 3.842(3) . 3_775 no P2 I2 3.894(3) . 3_775 no P2 I2 3.940(3) . . no P3 C18 3.674(12) . 2_644 no P1 H8C 3.1400 . . no P1 H15B 3.0500 . 3_775 no P1 H8B 2.8100 . . no P2 H10B 2.9800 . . no P2 H14C 2.7700 . . no P2 H15B 2.9400 . . no P3 H10C 3.0400 . . no P3 H14B 3.1800 . . no P3 H19C 2.6100 . . no P3 H11B 2.8500 . . no P3 H7C 3.1900 . 4_464 no P4 H7C 2.8000 . . no P4 H11C 2.9000 . 3_775 no P4 H12B 2.8800 . 3_775 no P4 H18A 2.9000 . 3_775 no P4 H18C 2.6000 . 3_775 no N1 I2 3.712(8) . . no N1 P1 3.483(9) . . no C8 Cu1 3.643(10) . . no C10 Cu2 3.682(10) . . no C12 I2 3.872(10) . . no C14 Cu2 3.496(10) . . no C15 Cu1 4.155(10) . 3_775 no C16 C17 3.523(13) . . no C16 C19 3.232(14) . . no C16 C20 3.551(14) . . no C17 C16 3.523(13) . . no C18 P3 3.674(12) . 2_654 no C19 C16 3.232(14) . . no C20 C16 3.551(14) . . no C101 I2 3.745(9) . 2_745 no C7 H18C 2.8400 . 3_775 no C13 H20A 3.1000 . . no C16 H19A 2.6100 . . no C16 H20A 2.7900 . . no C17 H16B 2.9500 . . no C19 H16C 2.9800 . . no C19 H16B 2.7000 . . no C20 H15C 2.9800 . . no C20 H12A 2.9800 . 4_574 no C20 H16B 2.7500 . . no C100 H8A 3.0700 . 2_755 no H6A H7A 2.4000 . . no H6B H7C 2.5500 . . no H6B H12B 2.5300 . 3_775 no H6C H8B 2.4300 . . no H7A H6A 2.4000 . . no H7A H8A 2.3900 . . no H7B H8C 2.5200 . . no H7B H18C 2.4000 . 3_775 no H7C P4 2.8000 . . no H7C H6B 2.5500 . . no H7C H18C 2.4500 . 3_775 no H7C P3 3.1900 . 4_665 no H7C H19C 2.5700 . 4_665 no H8A H7A 2.3900 . . no H8A C100 3.0700 . 2_745 no H8B Cu1 2.9100 . . no H8B P1 2.8100 . . no H8B H6C 2.4300 . . no H8C Cu1 3.6100 . . no H8C P1 3.1400 . . no H8C H7B 2.5200 . . no H10A H11A 2.4500 . . no H10A H12A 2.5500 . . no H10B I2 3.2900 . . no H10B Cu2 2.8500 . . no H10B P2 2.9800 . . no H10B H12C 2.5500 . . no H10C P3 3.0400 . . no H10C H11B 2.5700 . . no H10D I1 3.2300 . 4_565 no H10E I1 3.1600 . 2_755 no H11A H10A 2.4500 . . no H11A H12A 2.5500 . . no H11B P3 2.8500 . . no H11B H10C 2.5700 . . no H11C H12B 2.4700 . . no H11C H16C 2.5300 . 2_654 no H11C P4 2.9000 . 3_775 no H12A H10A 2.5500 . . no H12A H11A 2.5500 . . no H12A C20 2.9800 . 4_575 no H12A H20B 2.3400 . 4_575 no H12B H11C 2.4700 . . no H12B P4 2.8800 . 3_775 no H12B H6B 2.5300 . 3_775 no H12C I2 2.9600 . . no H12C H10B 2.5500 . . no H14A H15A 2.5600 . . no H14A H16A 2.2500 . . no H14B Cu2 3.6200 . . no H14B P3 3.1800 . . no H14B H16C 2.5600 . . no H14C Cu2 2.6500 . . no H14C P2 2.7700 . . no H14C H15B 2.4000 . . no H14C I2 3.3500 . 3_775 no H15A H14A 2.5600 . . no H15A H16A 2.4600 . . no H15A I1 3.2300 . 4_564 no H15B Cu2 3.6700 . . no H15B P2 2.9400 . . no H15B H14C 2.4000 . . no H15B I2 3.0900 . 3_775 no H15B Cu1 3.2600 . 3_775 no H15B P1 3.0500 . 3_775 no H15C C20 2.9800 . . no H15C H16B 2.5800 . . no H15C H20A 2.3900 . . no H16A H14A 2.2500 . . no H16A H15A 2.4600 . . no H16B C17 2.9500 . . no H16B C19 2.7000 . . no H16B C20 2.7500 . . no H16B H15C 2.5800 . . no H16B H19A 1.9800 . . no H16B H20A 1.9300 . . no H16C C19 2.9800 . . no H16C H14B 2.5600 . . no H16C H19A 2.4400 . . no H16C H11C 2.5300 . 2_644 no H18A H19B 2.5100 . . no H18A P4 2.9000 . 3_775 no H18B H19B 2.1800 . . no H18B H20C 2.3400 . . no H18C H20B 2.5500 . . no H18C P4 2.6000 . 3_775 no H18C C7 2.8400 . 3_775 no H18C H7B 2.4000 . 3_775 no H18C H7C 2.4500 . 3_775 no H19A C16 2.6100 . . no H19A H16B 1.9800 . . no H19A H16C 2.4400 . . no H19A H20A 2.3100 . . no H19A H20C 2.4300 . 3_674 no H19B H18A 2.5100 . . no H19B H18B 2.1800 . . no H19C P3 2.6100 . . no H19C H7C 2.5700 . 4_464 no H20A C13 3.1000 . . no H20A C16 2.7900 . . no H20A H15C 2.3900 . . no H20A H16B 1.9300 . . no H20A H19A 2.3100 . . no H20B H18C 2.5500 . . no H20B H12A 2.3400 . 4_574 no H20C H18B 2.3400 . . no H20C H19A 2.4300 . 3_674 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C7 H7C P4 0.9800 2.8000 3.182(10) 104.00 . yes C11 H11B P3 0.9800 2.8500 3.298(10) 109.00 . yes C12 H12C I2 0.9800 2.9600 3.872(10) 156.00 . yes C18 H18C P4 0.9800 2.6000 2.951(11) 101.00 3_775 yes C19 H19C P3 0.9800 2.6100 3.230(10) 121.00 . yes # Loop Mechanism for Extra Tables(s) #loop_ #_publ_manuscript_incl_extra_item #'_geom_extra_tableA_col_1' #'_geom_extra_tableA_col_2' #'_geom_extra_tableA_col_3' #'_geom_extra_table_head_A' #'_geom_table_footnote_A' #'_geom_extra_tableB_col_1' #'_geom_extra_tableB_col_2' #'_geom_extra_tableB_col_3' #'_geom_extra_table_head_B' #'_geom_table_footnote_B' # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 # ? ? ? # #loop_ #_geom_extra_tableB_col_1 #_geom_extra_tableB_col_2 #_geom_extra_tableB_col_3 # ? ? ? # #_geom_table_footnote_A #; # ? #; # #_geom_table_footnote_B #; # ? #; # #_geom_table_footnote_A #; # ? #; # #_geom_table_footnote_B #; # ? #; #===END # Attachment 'compound6.cif' data_u512_2 _database_code_depnum_ccdc_archive 'CCDC 656703' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H37 P5, 0.5(C7 H8)' _chemical_formula_structural '(P5 H C4)(C4 H9)4 * 0.5(C7 H8)' _chemical_formula_sum 'C23.50 H41 P5' _chemical_formula_weight 478.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' P P 0.2955 0.4335 '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/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 23.7888(3) _cell_length_b 11.2636(2) _cell_length_c 10.38680(10) _cell_angle_alpha 90.00 _cell_angle_beta 108.2020(10) _cell_angle_gamma 90.00 _cell_volume 2643.85(6) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 16404 _cell_measurement_theta_min 1.9472 _cell_measurement_theta_max 65.3244 _exptl_crystal_description block _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.202 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1028 _exptl_absorpt_coefficient_mu 3.259 _exptl_absorpt_correction_T_min 0.208 _exptl_absorpt_correction_T_max 0.613 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Gemini R-Ultra' _diffrn_measurement_method 'combined phi- and omega-scans' _diffrn_detector_area_resol_mean 10.5431 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25696 _diffrn_reflns_av_R_equivalents 0.1366 _diffrn_reflns_av_sigmaI/netI 0.0440 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.91 _diffrn_reflns_theta_max 65.50 _reflns_number_total 2385 _reflns_number_gt 2156 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Siemens-XP _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1503P)^2^+10.0028P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2385 _refine_ls_number_parameters 158 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0850 _refine_ls_R_factor_gt 0.0810 _refine_ls_wR_factor_ref 0.2363 _refine_ls_wR_factor_gt 0.2302 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _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 P1 P 0.82551(4) 0.37921(8) 0.16827(9) 0.0276(4) Uani 1 1 d . . . P3 P 0.80058(6) 0.5000 0.37558(13) 0.0306(4) Uani 1 2 d S . . P4 P 0.91659(6) 0.5000 0.42535(14) 0.0346(5) Uani 1 2 d S . . P5 P 0.94957(7) 0.5000 0.25403(16) 0.0497(6) Uani 1 2 d S . . H1 H 0.9586 0.6095 0.2447 0.050 Uiso 0.50 1 d PR . . C1 C 0.85654(16) 0.3850(3) 0.3599(4) 0.0287(9) Uani 1 1 d . . . C2 C 0.7731(2) 0.5000 0.1860(5) 0.0236(10) Uani 1 2 d S . . C3 C 0.8729(2) 0.5000 0.1280(5) 0.0266(11) Uani 1 2 d S . . C4 C 0.86377(18) 0.2653(4) 0.4348(4) 0.0356(9) Uani 1 1 d . . . C5 C 0.8054(2) 0.1972(4) 0.3913(5) 0.0459(11) Uani 1 1 d . . . H5A H 0.7925 0.1859 0.2928 0.069 Uiso 1 1 calc R . . H5B H 0.7753 0.2423 0.4169 0.069 Uiso 1 1 calc R . . H5C H 0.8109 0.1196 0.4362 0.069 Uiso 1 1 calc R . . C6 C 0.8809(2) 0.2853(5) 0.5882(4) 0.0492(12) Uani 1 1 d . . . H6A H 0.8885 0.2086 0.6350 0.074 Uiso 1 1 calc R . . H6B H 0.8485 0.3258 0.6098 0.074 Uiso 1 1 calc R . . H6C H 0.9167 0.3343 0.6180 0.074 Uiso 1 1 calc R . . C7 C 0.9122(2) 0.1934(5) 0.4013(6) 0.0589(14) Uani 1 1 d . . . H7A H 0.9003 0.1778 0.3037 0.088 Uiso 1 1 calc R . . H7B H 0.9181 0.1179 0.4506 0.088 Uiso 1 1 calc R . . H7C H 0.9493 0.2386 0.4283 0.088 Uiso 1 1 calc R . . C8 C 0.7058(2) 0.5000 0.1169(6) 0.0299(12) Uani 1 2 d S . . C9 C 0.6888(3) 0.5000 -0.0368(6) 0.0473(16) Uani 1 2 d S . . H9A H 0.7056 0.5714 -0.0597 0.050 Uiso 1 1 d R . . H9B H 0.6457 0.5000 -0.0697 0.050 Uiso 1 2 d SR . . C10 C 0.68004(19) 0.6110(4) 0.1615(5) 0.0480(12) Uani 1 1 d . . . H10A H 0.6378 0.6169 0.1108 0.072 Uiso 1 1 calc R . . H10B H 0.7007 0.6814 0.1437 0.072 Uiso 1 1 calc R . . H10C H 0.6851 0.6060 0.2587 0.072 Uiso 1 1 calc R . . C11 C 0.8788(2) 0.5000 -0.0176(5) 0.0328(12) Uani 1 2 d S . . C12 C 0.9122(2) 0.3885(5) -0.0373(5) 0.0469(12) Uani 1 1 d . . . H12A H 0.9528 0.3913 0.0245 0.070 Uiso 1 1 calc R . . H12B H 0.9128 0.3852 -0.1311 0.070 Uiso 1 1 calc R . . H12C H 0.8922 0.3179 -0.0178 0.070 Uiso 1 1 calc R . . C13 C 0.8176(3) 0.5000 -0.1249(6) 0.0437(15) Uani 1 2 d S . . H13A H 0.8220 0.5000 -0.2135 0.052 Uiso 1 2 d SR . . H13B H 0.7962 0.4305 -0.1142 0.052 Uiso 1 1 d R . . C1S C 0.4954(5) 0.5000 -0.0764(16) 0.048(3) Uani 0.50 2 d SP . . C2S C 0.4979(4) 0.3943(10) 0.1258(13) 0.061(3) Uani 0.50 1 d P . . H2SA H 0.4924 0.3195 0.1648 0.074 Uiso 0.50 1 d PR . . C3S C 0.4970(4) 0.5000 -0.2070(10) 0.074(2) Uani 1 2 d S . . H3SA H 0.4933 0.5799 -0.2407 0.111 Uiso 0.25 1 d PR . . H3SB H 0.5339 0.4671 -0.2094 0.111 Uiso 0.25 1 d PR . . H3SC H 0.4649 0.4529 -0.2626 0.111 Uiso 0.25 1 d PR . . H3SD H 0.4908 0.5000 -0.3029 0.089 Uiso 0.50 2 d SPR . . C4S C 0.5000 0.3953(6) 0.0000 0.0519(18) Uani 1 2 d S . . H4SA H 0.5050 0.3212 -0.0408 0.062 Uiso 0.50 1 d PR . . 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 P1 0.0290(6) 0.0282(6) 0.0295(6) 0.0001(4) 0.0147(4) 0.0013(3) P3 0.0361(8) 0.0317(8) 0.0263(7) 0.000 0.0131(6) 0.000 P4 0.0307(8) 0.0420(9) 0.0320(8) 0.000 0.0110(6) 0.000 P5 0.0294(9) 0.0875(14) 0.0344(9) 0.000 0.0129(7) 0.000 C1 0.0216(18) 0.033(2) 0.0328(19) 0.0054(15) 0.0107(15) 0.0005(14) C2 0.020(2) 0.027(3) 0.026(2) 0.000 0.0091(19) 0.000 C3 0.024(2) 0.036(3) 0.024(2) 0.000 0.013(2) 0.000 C4 0.038(2) 0.030(2) 0.040(2) 0.0085(17) 0.0147(17) 0.0043(17) C5 0.059(3) 0.037(2) 0.045(2) 0.0065(19) 0.021(2) -0.008(2) C6 0.059(3) 0.050(3) 0.037(2) 0.013(2) 0.013(2) -0.001(2) C7 0.060(3) 0.054(3) 0.068(3) 0.024(3) 0.028(3) 0.027(3) C8 0.023(3) 0.029(3) 0.038(3) 0.000 0.010(2) 0.000 C9 0.028(3) 0.071(5) 0.039(3) 0.000 0.004(3) 0.000 C10 0.024(2) 0.055(3) 0.063(3) -0.012(2) 0.0091(19) 0.0073(19) C11 0.033(3) 0.046(3) 0.025(3) 0.000 0.017(2) 0.000 C12 0.050(3) 0.058(3) 0.042(2) -0.009(2) 0.028(2) 0.005(2) C13 0.046(4) 0.063(4) 0.023(3) 0.000 0.011(2) 0.000 C1S 0.022(6) 0.051(8) 0.074(9) 0.000 0.018(6) 0.000 C2S 0.039(5) 0.051(6) 0.085(9) 0.026(6) 0.008(5) -0.001(4) C3S 0.057(5) 0.091(7) 0.077(6) 0.000 0.024(4) 0.000 C4S 0.040(4) 0.032(3) 0.083(6) 0.000 0.018(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 P1 C2 1.893(3) . ? P1 C3 1.895(3) . ? P1 C1 1.896(4) . ? P3 C2 1.871(5) . ? P3 C1 1.901(4) . ? P3 C1 1.901(4) 6_565 ? P3 P4 2.644(2) . ? P4 C1 1.891(4) . ? P4 C1 1.891(4) 6_565 ? P4 P5 2.157(2) . ? P5 C3 1.884(5) . ? P5 H1 1.2609 . ? C1 C4 1.539(5) . ? C2 C8 1.536(7) . ? C2 P1 1.893(3) 6_565 ? C3 C11 1.562(7) . ? C3 P1 1.895(3) 6_565 ? C4 C5 1.527(6) . ? C4 C6 1.533(6) . ? C4 C7 1.535(6) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.519(8) . ? C8 C10 1.527(5) 6_565 ? C8 C10 1.527(5) . ? C9 H9A 0.9600 . ? C9 H9B 0.9751 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C13 1.533(8) . ? C11 C12 1.533(5) 6_565 ? C11 C12 1.533(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9586 . ? C13 H13B 0.9587 . ? C1S C2S 1.326(12) 2_655 ? C1S C2S 1.326(12) 5_665 ? C1S C3S 1.369(17) . ? C1S C4S 1.406(10) . ? C1S C4S 1.406(10) 5_665 ? C1S C1S 1.53(3) 5_665 ? C2S C4S 1.324(13) . ? C2S C1S 1.326(12) 5_665 ? C2S C3S 1.442(14) 5_665 ? C2S H2SA 0.9601 . ? C3S C2S 1.442(14) 2_655 ? C3S C2S 1.442(14) 5_665 ? C3S H3SA 0.9600 . ? C3S H3SB 0.9600 . ? C3S H3SC 0.9601 . ? C3S H3SD 0.9600 . ? C4S C2S 1.324(13) 2_655 ? C4S C1S 1.406(10) 5_665 ? C4S H4SA 0.9600 . ? 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 C2 P1 C3 87.74(16) . . ? C2 P1 C1 85.74(19) . . ? C3 P1 C1 98.26(19) . . ? C2 P3 C1 86.21(16) . . ? C2 P3 C1 86.21(16) . 6_565 ? C1 P3 C1 85.9(2) . 6_565 ? C2 P3 P4 101.90(16) . . ? C1 P3 P4 45.62(12) . . ? C1 P3 P4 45.62(12) 6_565 . ? C1 P4 C1 86.5(2) . 6_565 ? C1 P4 P5 97.59(13) . . ? C1 P4 P5 97.59(13) 6_565 . ? C1 P4 P3 45.93(12) . . ? C1 P4 P3 45.93(12) 6_565 . ? P5 P4 P3 117.71(8) . . ? C3 P5 P4 92.88(16) . . ? C3 P5 H1 95.6 . . ? P4 P5 H1 100.2 . . ? C4 C1 P4 117.8(3) . . ? C4 C1 P1 116.5(3) . . ? P4 C1 P1 113.80(19) . . ? C4 C1 P3 121.6(3) . . ? P4 C1 P3 88.45(17) . . ? P1 C1 P3 93.42(17) . . ? C8 C2 P3 117.5(4) . . ? C8 C2 P1 125.2(2) . . ? P3 C2 P1 94.47(19) . . ? C8 C2 P1 125.2(2) . 6_565 ? P3 C2 P1 94.47(19) . 6_565 ? P1 C2 P1 91.9(2) . 6_565 ? C11 C3 P5 108.2(3) . . ? C11 C3 P1 117.0(2) . . ? P5 C3 P1 111.1(2) . . ? C11 C3 P1 117.0(2) . 6_565 ? P5 C3 P1 111.1(2) . 6_565 ? P1 C3 P1 91.8(2) . 6_565 ? C5 C4 C6 107.7(3) . . ? C5 C4 C7 110.2(4) . . ? C6 C4 C7 109.8(4) . . ? C5 C4 C1 110.0(3) . . ? C6 C4 C1 110.4(4) . . ? C7 C4 C1 108.7(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C10 108.6(3) . 6_565 ? C9 C8 C10 108.6(3) . . ? C10 C8 C10 110.0(5) 6_565 . ? C9 C8 C2 112.8(4) . . ? C10 C8 C2 108.5(3) 6_565 . ? C10 C8 C2 108.5(3) . . ? C8 C9 H9A 105.4 . . ? C8 C9 H9B 105.9 . . ? H9A C9 H9B 112.7 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C13 C11 C12 108.5(3) . 6_565 ? C13 C11 C12 108.5(3) . . ? C12 C11 C12 110.0(5) 6_565 . ? C13 C11 C3 110.6(4) . . ? C12 C11 C3 109.7(3) 6_565 . ? C12 C11 C3 109.7(3) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.4 . . ? C2S C1S C2S 127.8(17) 2_655 5_665 ? C2S C1S C3S 64.7(9) 2_655 . ? C2S C1S C3S 64.7(9) 5_665 . ? C2S C1S C4S 57.9(6) 2_655 . ? C2S C1S C4S 166.9(13) 5_665 . ? C3S C1S C4S 122.5(5) . . ? C2S C1S C4S 166.9(13) 2_655 5_665 ? C2S C1S C4S 57.9(6) 5_665 5_665 ? C3S C1S C4S 122.5(5) . 5_665 ? C4S C1S C4S 114.0(11) . 5_665 ? C2S C1S C1S 113.9(9) 2_655 5_665 ? C2S C1S C1S 113.9(9) 5_665 5_665 ? C3S C1S C1S 170.8(14) . 5_665 ? C4S C1S C1S 57.0(5) . 5_665 ? C4S C1S C1S 57.0(5) 5_665 5_665 ? C4S C2S C1S 64.1(9) . 5_665 ? C4S C2S C3S 123.2(9) . 5_665 ? C1S C2S C3S 59.1(8) 5_665 5_665 ? C4S C2S H2SA 118.4 . . ? C1S C2S H2SA 177.4 5_665 . ? C3S C2S H2SA 118.4 5_665 . ? C1S C3S C2S 56.2(6) . 2_655 ? C1S C3S C2S 56.2(6) . 5_665 ? C2S C3S C2S 111.3(11) 2_655 5_665 ? C1S C3S H3SA 109.5 . . ? C2S C3S H3SA 165.7 2_655 . ? C2S C3S H3SA 54.5 5_665 . ? C1S C3S H3SB 109.4 . . ? C2S C3S H3SB 77.6 2_655 . ? C2S C3S H3SB 115.0 5_665 . ? H3SA C3S H3SB 109.5 . . ? C1S C3S H3SC 109.5 . . ? C2S C3S H3SC 78.6 2_655 . ? C2S C3S H3SC 135.6 5_665 . ? H3SA C3S H3SC 109.5 . . ? H3SB C3S H3SC 109.5 . . ? C1S C3S H3SD 170.2 . . ? C2S C3S H3SD 124.3 2_655 . ? C2S C3S H3SD 124.3 5_665 . ? H3SA C3S H3SD 69.8 . . ? H3SB C3S H3SD 79.5 . . ? H3SC C3S H3SD 62.7 . . ? C2S C4S C2S 179.0(11) . 2_655 ? C2S C4S C1S 123.0(8) . . ? C2S C4S C1S 58.0(7) 2_655 . ? C2S C4S C1S 58.0(7) . 5_665 ? C2S C4S C1S 123.0(8) 2_655 5_665 ? C1S C4S C1S 66.0(11) . 5_665 ? C2S C4S H4SA 118.4 . . ? C2S C4S H4SA 60.6 2_655 . ? C1S C4S H4SA 118.6 . . ? C1S C4S H4SA 168.4 5_665 . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 65.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.973 _refine_diff_density_min -0.560 _refine_diff_density_rms 0.122