######################################## # # # CIF generated by the Xtal System # # # ######################################## data_global _audit_creation_method Xtal3.6 _audit_creation_date 04-09-02 _audit_update_record ? #============================================================================== # (Publishing Staff Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Skelton, B. W.' _publ_contact_author_address ; Department of Chemistry University of Western Australia 35 Stirling Highway Crawley Western Australia 6009 Australia ; _publ_contact_author_email bws@crystal.uwa.edu.au _publ_contact_author_fax (+61)_08_9380_1118 _publ_contact_author_phone (+61)_08-9380_3481 loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Skelton, Brian W.' . ; Department of Chemistry, University of Western Australia, 35 Stirling Highway, Crawley, WA 6009, Australia. ; _publ_section_references ; Sheldrick, G M. (1996). SADABS. Pogram for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_vjh285 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C25 H26 Br2 N4 O1' _chemical_formula_moiety 'C22 H20 N4, 2Br, C3 H6 O' _chemical_formula_weight 558.32 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _cell_length_a 9.9690(10) _cell_length_b 10.2860(10) _cell_length_c 11.9850(10) _cell_angle_alpha 80.957(3) _cell_angle_beta 86.821(3) _cell_angle_gamma 75.278(3) _cell_volume 1173.7(2) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.58 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 4372 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 33.5 _cell_measurement_temperature 150(2) _exptl_absorpt_coefficient_mu 3.479 _exptl_crystal_description prism _exptl_crystal_size_max .32 _exptl_crystal_size_mid .22 _exptl_crystal_size_min .15 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .70 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 20859 _reflns_number_total 10267 _reflns_Friedel_coverage 0 _reflns_number_gt 6546 _reflns_threshold_expression 'I > 2.00 sig(I)' _diffrn_reflns_theta_max 35. _diffrn_reflns_theta_full 35.0 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .038 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt .045 _refine_ls_wR_factor_ref .114 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_number_reflns 10267 _refine_ls_number_parameters 289 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/(sig^2(F^2) + 6F^2) ; _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .024 _refine_diff_density_min -.978 _refine_diff_density_max 1.712 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 50 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 52 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Br ? 0 4 -.374 2.456 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 8 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 2 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Br1 .63884(3) .14394(3) .11309(3) .02461(17) Uani ? ? 1.00000 ? ? Br2 .67970(3) .17628(3) .50950(3) .02597(18) Uani ? ? 1.00000 ? ? C1 .2490(3) .4780(3) .5728(2) .0202(15) Uani ? ? 1.00000 ? ? C11 .3061(3) .4271(3) .6912(2) .0195(14) Uani ? ? 1.00000 ? ? C12 .3451(3) .2914(3) .7460(2) .0201(15) Uani ? ? 1.00000 ? ? C13 .3810(3) .2664(3) .8595(3) .0269(18) Uani ? ? 1.00000 ? ? C14 .3774(4) .3716(3) .9207(3) .030(2) Uani ? ? 1.00000 ? ? C15 .3379(3) .5048(3) .8674(3) .029(2) Uani ? ? 1.00000 ? ? C16 .3049(3) .5310(3) .7536(3) .0229(16) Uani ? ? 1.00000 ? ? C2 .3479(3) .1422(3) .3101(2) .0224(16) Uani ? ? 1.00000 ? ? N21 .3163(2) .4069(2) .4792(2) .0186(12) Uani ? ? 1.00000 ? ? C22 .2903(3) .2941(3) .4548(2) .0182(14) Uani ? ? 1.00000 ? ? N23 .3454(2) .2683(2) .3548(2) .0190(13) Uani ? ? 1.00000 ? ? C24 .4112(3) .3683(3) .3128(2) .0213(15) Uani ? ? 1.00000 ? ? C25 .3916(3) .4555(3) .3899(2) .0220(15) Uani ? ? 1.00000 ? ? C3 .0268(3) .2410(3) .3849(2) .0205(15) Uani ? ? 1.00000 ? ? C31 .0835(3) .1789(3) .2798(2) .0184(14) Uani ? ? 1.00000 ? ? C32 .2238(3) .1468(3) .2425(2) .0206(15) Uani ? ? 1.00000 ? ? C33 .2528(3) .1059(3) .1363(3) .0255(18) Uani ? ? 1.00000 ? ? C34 .1507(3) .0964(4) .0668(3) .030(2) Uani ? ? 1.00000 ? ? C35 .0142(3) .1280(3) .1037(3) .0270(18) Uani ? ? 1.00000 ? ? C36 -.0179(3) .1686(3) .2089(3) .0232(16) Uani ? ? 1.00000 ? ? C4 .3620(3) .1668(3) .6898(2) .0204(15) Uani ? ? 1.00000 ? ? N41 .0966(2) .1834(2) .4939(2) .0194(13) Uani ? ? 1.00000 ? ? C42 .2104(3) .2134(3) .5248(2) .0195(14) Uani ? ? 1.00000 ? ? N43 .2379(2) .1608(2) .6317(2) .0195(13) Uani ? ? 1.00000 ? ? C44 .1383(3) .0936(3) .6719(2) .0217(15) Uani ? ? 1.00000 ? ? C45 .0490(3) .1093(3) .5858(2) .0222(16) Uani ? ? 1.00000 ? ? C01 .1756(4) .7150(4) .2057(3) .039(2) Uani ? ? 1.00000 ? ? C02 .0941(3) .6098(4) .2343(3) .033(2) Uani ? ? 1.00000 ? ? O02 .0657(3) .5699(3) .3314(2) .0348(16) Uani ? ? 1.00000 ? ? C03 .0488(5) .5553(5) .1379(4) .051(3) Uani ? ? 1.00000 ? ? H13 .40812 .17560 .89665 .03100 Uiso ? ? 1.00000 ? ? H14 .40082 .35147 .99882 .03400 Uiso ? ? 1.00000 ? ? H15 .33215 .57852 .90933 .03400 Uiso ? ? 1.00000 ? ? H16 .28040 .62345 .71663 .02600 Uiso ? ? 1.00000 ? ? H2a .42914 .12036 .26328 .02500 Uiso ? ? 1.00000 ? ? H2b .35454 .07004 .37241 .02500 Uiso ? ? 1.00000 ? ? H24 .46084 .37558 .24204 .02400 Uiso ? ? 1.00000 ? ? H25 .42317 .53734 .38265 .02500 Uiso ? ? 1.00000 ? ? H33 .34774 .08410 .11133 .02900 Uiso ? ? 1.00000 ? ? H34 .17480 .06787 -.00547 .03400 Uiso ? ? 1.00000 ? ? H35 -.05767 .12326 .05645 .03100 Uiso ? ? 1.00000 ? ? H36 -.11266 .19130 .23266 .02600 Uiso ? ? 1.00000 ? ? H4a .43610 .16464 .63474 .02400 Uiso ? ? 1.00000 ? ? H4b .38695 .08815 .74513 .02400 Uiso ? ? 1.00000 ? ? H44 .13130 .04540 .74566 .02400 Uiso ? ? 1.00000 ? ? H45 -.03200 .07502 .58900 .02500 Uiso ? ? 1.00000 ? ? H1a .25375 .57063 .55444 .02300 Uiso ? ? 1.00000 ? ? H1b .15439 .47481 .57578 .02300 Uiso ? ? 1.00000 ? ? H3a -.06685 .23536 .39410 .02300 Uiso ? ? 1.00000 ? ? H3b .02890 .33451 .36976 .02300 Uiso ? ? 1.00000 ? ? H01a .20855 .73518 .27358 .05700 Uiso ? ? 1.00000 ? ? H01b .12044 .79735 .16658 .05700 Uiso ? ? 1.00000 ? ? H01c .25416 .68346 .15930 .05700 Uiso ? ? 1.00000 ? ? H03a .00924 .62741 .08051 .07400 Uiso ? ? 1.00000 ? ? H03b -.01898 .50542 .16391 .07400 Uiso ? ? 1.00000 ? ? H03c .12607 .49543 .10687 .07400 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br1 .02078(12) .02418(13) .02695(14) -.00454(10) .00258(10) -.00078(10) Br2 .02016(12) .02283(13) .03202(15) -.00471(10) .00237(10) .00266(11) C1 .0174(10) .0188(11) .0229(12) -.0029(8) .0014(9) -.0021(9) C11 .0151(10) .0176(10) .0244(12) -.0035(8) .0021(9) -.0011(9) C12 .0196(11) .0174(10) .0226(12) -.0050(9) .0019(9) -.0011(9) C13 .0291(14) .0230(13) .0270(14) -.0055(11) -.0026(11) .0005(10) C14 .0345(16) .0301(15) .0235(14) -.0051(12) -.0030(11) -.0024(11) C15 .0315(15) .0275(14) .0281(14) -.0093(12) .0021(12) -.0063(11) C16 .0212(12) .0197(11) .0265(13) -.0043(9) .0031(10) -.0023(10) C2 .0199(11) .0206(11) .0244(12) -.0017(9) .0044(9) -.0033(9) N21 .0158(9) .0161(9) .0227(10) -.0043(7) .0015(8) .0008(8) C22 .0167(10) .0162(10) .0203(11) -.0041(8) .0036(8) -.0005(8) N23 .0156(9) .0192(10) .0212(10) -.0048(7) .0021(7) -.0003(8) C24 .0170(11) .0228(12) .0226(12) -.0068(9) .0025(9) .0030(9) C25 .0190(11) .0241(12) .0219(12) -.0080(9) -.0009(9) .0037(9) C3 .0183(11) .0190(11) .0230(12) -.0028(9) .0026(9) -.0032(9) C31 .0182(10) .0146(10) .0212(11) -.0034(8) .0026(9) -.0011(8) C32 .0191(11) .0182(11) .0241(12) -.0051(9) .0039(9) -.0030(9) C33 .0253(13) .0281(14) .0245(13) -.0088(11) .0072(10) -.0075(11) C34 .0305(15) .0351(16) .0264(14) -.0105(12) .0060(11) -.0109(12) C35 .0273(14) .0308(14) .0255(14) -.0104(11) .0015(11) -.0077(11) C36 .0222(12) .0198(11) .0274(13) -.0056(9) .0015(10) -.0029(10) C4 .0183(11) .0175(11) .0237(12) -.0042(9) .0017(9) .0009(9) N41 .0190(10) .0174(9) .0214(10) -.0046(8) .0049(8) -.0029(8) C42 .0194(11) .0166(10) .0222(12) -.0054(9) .0036(9) -.0016(9) N43 .0184(9) .0166(9) .0222(10) -.0037(7) .0034(8) -.0015(8) C44 .0224(12) .0192(11) .0223(12) -.0063(9) .0060(9) -.0001(9) C45 .0225(12) .0225(12) .0225(12) -.0091(10) .0066(9) -.0024(9) C01 .042(2) .0376(18) .0361(18) -.0118(15) .0051(15) .0026(14) C02 .0265(14) .0304(15) .0345(17) -.0011(12) .0012(12) .0033(12) O02 .0295(11) .0348(12) .0350(13) -.0060(10) .0023(9) .0057(10) C03 .059(3) .056(3) .041(2) -.022(2) -.003(2) -.001(2) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published C1 C11 . . 1.522(4) ? C1 N21 . . 1.473(4) ? C1 H1a . . .956 ? C1 H1b . . .951 ? C11 C12 . . 1.412(4) ? C11 C16 . . 1.394(4) ? C12 C13 . . 1.393(4) ? C12 C4 . . 1.508(4) ? C13 C14 . . 1.392(5) ? C13 H13 . . .948 ? C14 C15 . . 1.385(4) ? C14 H14 . . .955 ? C15 C16 . . 1.389(4) ? C15 H15 . . .963 ? C16 H16 . . .960 ? C2 N23 . . 1.474(4) ? C2 C32 . . 1.502(4) ? C2 H2a . . .958 ? C2 H2b . . .959 ? N21 C22 . . 1.330(4) ? N21 C25 . . 1.376(4) ? C22 N23 . . 1.328(4) ? C22 C42 . . 1.438(4) ? N23 C24 . . 1.373(4) ? C24 C25 . . 1.359(4) ? C24 H24 . . .960 ? C25 H25 . . .961 ? C3 C31 . . 1.518(4) ? C3 N41 . . 1.480(4) ? C3 H3a . . .949 ? C3 H3b . . .956 ? C31 C32 . . 1.417(4) ? C31 C36 . . 1.391(4) ? C32 C33 . . 1.395(4) ? C33 C34 . . 1.382(5) ? C33 H33 . . .958 ? C34 C35 . . 1.381(5) ? C34 H34 . . .957 ? C35 C36 . . 1.385(5) ? C35 H35 . . .953 ? C36 H36 . . .952 ? C4 N43 . . 1.471(4) ? C4 H4a . . .961 ? C4 H4b . . .951 ? N41 C42 . . 1.334(4) ? N41 C45 . . 1.371(4) ? C42 N43 . . 1.325(3) ? N43 C44 . . 1.373(4) ? C44 C45 . . 1.364(4) ? C44 H44 . . .952 ? C45 H45 . . .957 ? C01 C02 . . 1.499(6) ? C01 H01a . . .964 ? C01 H01b . . .952 ? C01 H01c . . .952 ? C02 O02 . . 1.215(4) ? C02 C03 . . 1.499(7) ? C03 H03a . . .948 ? C03 H03b . . .958 ? C03 H03c . . .954 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published C11 C1 N21 . . . 118.6(2) ? C11 C1 H1a . . . 107.0 ? C11 C1 H1b . . . 107.3 ? N21 C1 H1a . . . 107.3 ? N21 C1 H1b . . . 107.3 ? H1a C1 H1b . . . 108.9 ? C1 C11 C12 . . . 127.8(3) ? C1 C11 C16 . . . 113.6(2) ? C12 C11 C16 . . . 118.3(3) ? C11 C12 C13 . . . 119.1(3) ? C11 C12 C4 . . . 125.3(3) ? C13 C12 C4 . . . 115.4(2) ? C12 C13 C14 . . . 121.8(3) ? C12 C13 H13 . . . 119.6 ? C14 C13 H13 . . . 118.6 ? C13 C14 C15 . . . 119.2(3) ? C13 C14 H14 . . . 119.9 ? C15 C14 H14 . . . 120.8 ? C14 C15 C16 . . . 119.6(3) ? C14 C15 H15 . . . 120.0 ? C16 C15 H15 . . . 120.4 ? C11 C16 C15 . . . 122.0(3) ? C11 C16 H16 . . . 118.9 ? C15 C16 H16 . . . 119.1 ? N23 C2 C32 . . . 115.3(2) ? N23 C2 H2a . . . 108.7 ? N23 C2 H2b . . . 108.4 ? C32 C2 H2a . . . 108.3 ? C32 C2 H2b . . . 107.9 ? H2a C2 H2b . . . 108.1 ? C1 N21 C22 . . . 124.0(2) ? C1 N21 C25 . . . 127.5(2) ? C22 N21 C25 . . . 107.2(2) ? N21 C22 N23 . . . 110.2(2) ? N21 C22 C42 . . . 125.2(2) ? N23 C22 C42 . . . 124.6(3) ? C2 N23 C22 . . . 123.0(2) ? C2 N23 C24 . . . 128.6(2) ? C22 N23 C24 . . . 107.9(3) ? N23 C24 C25 . . . 107.0(2) ? N23 C24 H24 . . . 126.4 ? C25 C24 H24 . . . 126.6 ? N21 C25 C24 . . . 107.7(3) ? N21 C25 H25 . . . 126.1 ? C24 C25 H25 . . . 126.1 ? C31 C3 N41 . . . 119.1(2) ? C31 C3 H3a . . . 106.9 ? C31 C3 H3b . . . 106.8 ? N41 C3 H3a . . . 107.7 ? N41 C3 H3b . . . 107.1 ? H3a C3 H3b . . . 109.0 ? C3 C31 C32 . . . 126.8(3) ? C3 C31 C36 . . . 114.2(2) ? C32 C31 C36 . . . 118.5(3) ? C2 C32 C31 . . . 126.1(3) ? C2 C32 C33 . . . 115.7(2) ? C31 C32 C33 . . . 118.0(3) ? C32 C33 C34 . . . 122.7(3) ? C32 C33 H33 . . . 117.9 ? C34 C33 H33 . . . 119.4 ? C33 C34 C35 . . . 118.9(3) ? C33 C34 H34 . . . 120.2 ? C35 C34 H34 . . . 120.9 ? C34 C35 C36 . . . 119.8(3) ? C34 C35 H35 . . . 120.0 ? C36 C35 H35 . . . 120.2 ? C31 C36 C35 . . . 122.1(3) ? C31 C36 H36 . . . 119.2 ? C35 C36 H36 . . . 118.7 ? C12 C4 N43 . . . 114.7(2) ? C12 C4 H4a . . . 108.4 ? C12 C4 H4b . . . 108.9 ? N43 C4 H4a . . . 107.8 ? N43 C4 H4b . . . 108.4 ? H4a C4 H4b . . . 108.4 ? C3 N41 C42 . . . 123.8(2) ? C3 N41 C45 . . . 127.9(3) ? C42 N41 C45 . . . 107.6(2) ? C22 C42 N41 . . . 125.8(2) ? C22 C42 N43 . . . 124.3(3) ? N41 C42 N43 . . . 109.9(2) ? C4 N43 C42 . . . 123.8(2) ? C4 N43 C44 . . . 128.0(2) ? C42 N43 C44 . . . 108.0(2) ? N43 C44 C45 . . . 107.0(2) ? N43 C44 H44 . . . 127.3 ? C45 C44 H44 . . . 125.7 ? N41 C45 C44 . . . 107.4(3) ? N41 C45 H45 . . . 126.3 ? C44 C45 H45 . . . 126.3 ? C02 C01 H01a . . . 110.4 ? C02 C01 H01b . . . 111.3 ? C02 C01 H01c . . . 110.8 ? H01a C01 H01b . . . 108.1 ? H01a C01 H01c . . . 108.0 ? H01b C01 H01c . . . 108.3 ? C01 C02 O02 . . . 121.7(4) ? C01 C02 C03 . . . 117.3(3) ? O02 C02 C03 . . . 121.0(4) ? C02 C03 H03a . . . 110.4 ? C02 C03 H03b . . . 109.9 ? C02 C03 H03c . . . 110.1 ? H03a C03 H03b . . . 108.9 ? H03a C03 H03c . . . 109.1 ? H03b C03 H03c . . . 108.4 ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 564 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 16 _reflns_limit_k_min -15 _reflns_limit_k_max 16 _reflns_limit_l_min -19 _reflns_limit_l_max 19 _reflns_number_observed ? _reflns_d_resolution_high .618 _reflns_d_resolution_low 11.807 _diffrn_reflns_av_sigmaI/netI .124 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .093 _refine_ls_wR_factor_all .114 _refine_ls_goodness_of_fit_all 1.038 _refine_ls_shift/su_mean .001 #===END ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_global _audit_creation_method Xtal3.6 _audit_creation_date 04-12-03 _audit_update_record ? #============================================================================== # (Publishing Staff Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Skelton, B. W.' _publ_contact_author_address ; Department of Chemistry University of Western Australia 35 Stirling Highway Crawley Western Australia 6009 Australia ; _publ_contact_author_email bws@crystal.uwa.edu.au _publ_contact_author_fax (+61)_08_6488_1118 _publ_contact_author_phone (+61)_08_6488_7107 _publ_contact_letter ; ? #<< contact letter ; _publ_requested_journal ? _publ_requested_category ? _publ_section_title ; ? #<< paper title text ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Skelton, Brian W.' . ; Department of Chemistry, University of Western Australia, 35 Stirling Highway, Crawley, WA 6009, Australia. ; _publ_section_references ; Sheldrick, G M. (1996). SADABS. Program for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_vjh297 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C10 H16 I2 N4' _chemical_formula_moiety 'C10 H16 N4, 2I' _chemical_formula_weight 446.1 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 9.2022(5) _cell_length_b 15.0505(8) _cell_length_c 11.0279(6) _cell_angle_alpha 90.00000 _cell_angle_beta 104.6030(10) _cell_angle_gamma 90.00000 _cell_volume 1478.00(14) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 2.005 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8846 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 37.5 _cell_measurement_temperature 150(2) _exptl_absorpt_coefficient_mu 4.239 _exptl_crystal_description block _exptl_crystal_size_max .38 _exptl_crystal_size_mid .18 _exptl_crystal_size_min .18 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .629 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 29258 _reflns_number_total 7750 _reflns_Friedel_coverage 0 _reflns_number_gt 6948 _reflns_threshold_expression 'Fsqd > .00 sig(Fsqd)' _diffrn_reflns_theta_max 37.5 _diffrn_reflns_theta_full 37.5 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .026 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt .025 _refine_ls_wR_factor_gt .056 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_number_reflns 7750 _refine_ls_number_parameters 145 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/(sig^2(F^2) + 7*F^2) ; _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .003 _refine_diff_density_min -1.338 _refine_diff_density_max 1.346 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 40 .002 .002 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' H ? 0 64 0 0 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' I ? 0 8 -.726 1.812 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' N ? 0 16 .004 .003 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group I1 .104593(16) .285193(10) .433373(13) .01949(5) Uani ? ? 1.00000 ? ? I2 .638013(18) .403853(11) .804615(15) .02444(6) Uani ? ? 1.00000 ? ? N11 .1595(2) .49483(12) .78565(17) .0176(6) Uani ? ? 1.00000 ? ? C11 .2015(3) .41110(14) .7361(2) .0240(8) Uani ? ? 1.00000 ? ? C12 .2272(2) .57412(13) .78628(17) .0150(6) Uani ? ? 1.00000 ? ? N13 .1596(2) .63216(12) .84638(17) .0173(6) Uani ? ? 1.00000 ? ? C13 .1955(3) .72609(15) .8692(2) .0233(8) Uani ? ? 1.00000 ? ? C14 .0454(3) .58974(16) .8826(2) .0220(8) Uani ? ? 1.00000 ? ? C15 .0451(2) .50369(16) .8444(2) .0212(8) Uani ? ? 1.00000 ? ? N21 .4805(2) .62911(13) .7789(2) .0210(7) Uani ? ? 1.00000 ? ? C21 .5449(3) .6419(2) .9127(3) .0333(11) Uani ? ? 1.00000 ? ? C22 .3456(2) .59454(13) .72495(19) .0161(6) Uani ? ? 1.00000 ? ? N23 .3357(2) .58568(12) .60085(17) .0182(6) Uani ? ? 1.00000 ? ? C23 .2080(3) .55164(17) .5053(2) .0237(8) Uani ? ? 1.00000 ? ? C24 .4682(3) .61486(16) .5785(2) .0244(9) Uani ? ? 1.00000 ? ? C25 .5575(3) .64213(17) .6885(3) .0265(9) Uani ? ? 1.00000 ? ? H11a .18039 .36238 .78528 .03600 Uiso ? ? 1.00000 ? ? H11b .30668 .41093 .74114 .03600 Uiso ? ? 1.00000 ? ? H11c .14723 .40319 .65193 .03600 Uiso ? ? 1.00000 ? ? H13a .25838 .73332 .95136 .03600 Uiso ? ? 1.00000 ? ? H13b .10509 .75879 .86202 .03600 Uiso ? ? 1.00000 ? ? H13c .24526 .74794 .80911 .03600 Uiso ? ? 1.00000 ? ? H14 -.01822 .61473 .92951 .02700 Uiso ? ? 1.00000 ? ? H15 -.02267 .45794 .85458 .02700 Uiso ? ? 1.00000 ? ? H21a .48542 .61050 .95896 .05000 Uiso ? ? 1.00000 ? ? H21b .54418 .70334 .93281 .05000 Uiso ? ? 1.00000 ? ? H21c .64523 .62030 .93617 .05000 Uiso ? ? 1.00000 ? ? H23a .11738 .57174 .52174 .03600 Uiso ? ? 1.00000 ? ? H23b .20961 .48796 .50696 .03600 Uiso ? ? 1.00000 ? ? H23c .21359 .57168 .42455 .03600 Uiso ? ? 1.00000 ? ? H24 .49222 .61598 .49892 .03100 Uiso ? ? 1.00000 ? ? H25 .65665 .66600 .70186 .03400 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 I1 .02037(6) .01909(6) .02063(6) .00104(4) .00822(4) -.00147(4) I2 .02496(7) .02820(7) .02243(6) .00563(5) .01021(5) .00240(5) N11 .0200(7) .0150(6) .0190(7) -.0045(5) .0074(6) .0005(5) C11 .0340(11) .0141(7) .0268(10) -.0048(7) .0131(9) -.0008(7) C12 .0170(7) .0148(7) .0140(6) -.0029(5) .0055(5) .0003(5) N13 .0183(7) .0169(7) .0185(7) -.0008(5) .0079(5) -.0009(5) C13 .0294(10) .0162(8) .0258(9) -.0014(7) .0096(8) -.0028(7) C14 .0211(8) .0261(9) .0222(9) -.0017(7) .0117(7) .0014(7) C15 .0197(8) .0250(9) .0210(8) -.0064(7) .0092(7) .0022(7) N21 .0167(7) .0209(8) .0276(8) -.0058(6) .0096(6) -.0022(6) C21 .0234(10) .0442(15) .0323(12) -.0108(10) .0067(9) -.0108(11) C22 .0177(7) .0143(7) .0184(7) -.0025(6) .0082(6) .0013(6) N23 .0215(7) .0185(7) .0173(7) .0018(6) .0098(6) .0036(5) C23 .0270(10) .0258(10) .0182(8) .0026(8) .0059(7) -.0001(7) C24 .0268(10) .0218(9) .0314(11) .0024(8) .0199(9) .0058(8) C25 .0238(9) .0250(10) .0363(12) -.0046(8) .0178(9) .0016(9) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published N11 C11 . . 1.464(3) ? N11 C12 . . 1.345(3) ? N11 C15 . . 1.375(3) ? C11 H11a . . .961 ? C11 H11b . . .955 ? C11 H11c . . .944 ? C12 N13 . . 1.341(3) ? C12 C22 . . 1.453(3) ? N13 C13 . . 1.459(3) ? N13 C14 . . 1.372(3) ? C13 H13a . . .951 ? C13 H13b . . .952 ? C13 H13c . . .954 ? C14 C15 . . 1.361(3) ? C14 H14 . . .952 ? C15 H15 . . .954 ? N21 C21 . . 1.458(3) ? N21 C22 . . 1.339(3) ? N21 C25 . . 1.374(4) ? C21 H21a . . .961 ? C21 H21b . . .951 ? C21 H21c . . .951 ? C22 N23 . . 1.355(3) ? N23 C23 . . 1.459(3) ? N23 C24 . . 1.375(3) ? C23 H23a . . .947 ? C23 H23b . . .959 ? C23 H23c . . .954 ? C24 C25 . . 1.347(3) ? C24 H24 . . .958 ? C25 H25 . . .957 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published C11 N11 C12 . . . 126.9(2) ? C11 N11 C15 . . . 124.4(2) ? C12 N11 C15 . . . 108.67(19) ? N11 C11 H11a . . . 109.6 ? N11 C11 H11b . . . 109.8 ? N11 C11 H11c . . . 110.6 ? H11a C11 H11b . . . 108.1 ? H11a C11 H11c . . . 109.1 ? H11b C11 H11c . . . 109.5 ? N11 C12 N13 . . . 108.0(2) ? N11 C12 C22 . . . 125.86(19) ? N13 C12 C22 . . . 126.04(18) ? C12 N13 C13 . . . 127.1(2) ? C12 N13 C14 . . . 108.99(18) ? C13 N13 C14 . . . 123.9(2) ? N13 C13 H13a . . . 109.4 ? N13 C13 H13b . . . 109.3 ? N13 C13 H13c . . . 110.0 ? H13a C13 H13b . . . 109.2 ? H13a C13 H13c . . . 109.8 ? H13b C13 H13c . . . 109.1 ? N13 C14 C15 . . . 107.2(2) ? N13 C14 H14 . . . 126.6 ? C15 C14 H14 . . . 126.2 ? N11 C15 C14 . . . 107.2(2) ? N11 C15 H15 . . . 125.9 ? C14 C15 H15 . . . 126.9 ? C21 N21 C22 . . . 126.5(2) ? C21 N21 C25 . . . 124.3(2) ? C22 N21 C25 . . . 108.8(2) ? N21 C21 H21a . . . 109.4 ? N21 C21 H21b . . . 109.8 ? N21 C21 H21c . . . 110.4 ? H21a C21 H21b . . . 108.4 ? H21a C21 H21c . . . 109.3 ? H21b C21 H21c . . . 109.4 ? C12 C22 N21 . . . 126.6(2) ? C12 C22 N23 . . . 125.58(17) ? N21 C22 N23 . . . 107.8(2) ? C22 N23 C23 . . . 126.9(2) ? C22 N23 C24 . . . 108.21(18) ? C23 N23 C24 . . . 124.9(2) ? N23 C23 H23a . . . 109.7 ? N23 C23 H23b . . . 109.4 ? N23 C23 H23c . . . 109.9 ? H23a C23 H23b . . . 109.0 ? H23a C23 H23c . . . 109.6 ? H23b C23 H23c . . . 109.2 ? N23 C24 C25 . . . 107.7(2) ? N23 C24 H24 . . . 126.2 ? C25 C24 H24 . . . 126.2 ? N21 C25 C24 . . . 107.5(2) ? N21 C25 H25 . . . 126.0 ? C24 C25 H25 . . . 126.5 ? _exptl_crystal_F_000 840 _reflns_limit_h_min 0 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 25 _reflns_limit_l_min -18 _reflns_limit_l_max 18 _reflns_number_observed ? _reflns_d_resolution_high .584 _reflns_d_resolution_low 8.69 _diffrn_reflns_av_sigmaI/netI .024 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .029 _refine_ls_wR_factor_ref .062 _refine_ls_goodness_of_fit_all 1.046 _refine_ls_shift/su_mean .0003 #===END data_global _audit_creation_date 06-09-07 _audit_update_record ? #============================================================================== # (Publishing Staff Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Skelton, B. W.' _publ_contact_author_address ; Department of Chemistry University of Western Australia 35 Stirling Highway Crawley Western Australia 6009 Australia ; _publ_contact_author_email bws@crystal.uwa.edu.au _publ_contact_author_fax (+61)_08_6488_1118 _publ_contact_author_phone (+61)_08_6488_7107 loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Skelton, Brian W.' . ; Chemistry, University of Western Australia, 35 Stirling Highway, Crawley, WA 6009, Australia. ; _publ_section_references ; Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; data_vjh543 _audit_creation_date 2006-09-09T15:33:18-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C65.80 H58.60 B Br Cl3.60 N4 P Pd' _chemical_formula_moiety 'C40 H35 Br N4 P Pd, C24 H20 B, 1.80(C H2 Cl2)' _chemical_formula_weight 1261.08 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M F_d_d_2 _symmetry_space_group_name_Hall f_2_-2d loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/4, y+1/4, z+1/4' 'x+3/4, -y+3/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/4, y+3/4, z+3/4' 'x+3/4, -y+5/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+3/4, y+1/4, z+3/4' 'x+5/4, -y+3/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+3/4, y+3/4, z+1/4' 'x+5/4, -y+5/4, z+1/4' _cell_length_a 38.434(2) _cell_length_b 48.007(3) _cell_length_c 12.7080(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 23448(2) _cell_formula_units_Z 16 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6624 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 32.35 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_density_diffrn 1.429 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10298 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.237 _exptl_crystal_description prism _exptl_crystal_size_max .48 _exptl_crystal_size_mid .42 _exptl_crystal_size_min .36 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .91 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_unetI/netI 0.0337 _diffrn_reflns_number 22236 _diffrn_reflns_limit_h_min -60 _diffrn_reflns_limit_h_max 60 _diffrn_reflns_limit_k_min -74 _diffrn_reflns_limit_k_max 74 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 33.9 _diffrn_reflns_theta_full 33.9 _diffrn_measured_fraction_theta_full 0.970 _diffrn_measured_fraction_theta_max 0.970 _reflns_number_total 22236 _reflns_number_gt 19090 _reflns_threshold_expression I>2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_molecular_graphics xtal _computing_publication_material 'WinGX' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0444P)^2^+46.6711P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 22236 _refine_ls_number_parameters 704 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0905 _refine_ls_wR_factor_gt 0.084 _refine_ls_goodness_of_fit_ref 1.05 _refine_ls_restrained_S_all 1.05 _refine_ls_shift/su_max 0.045 _refine_ls_shift/su_mean 0.001 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.012(4) _refine_diff_density_max 0.772 _refine_diff_density_min -0.6 _refine_diff_density_rms 0.09 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Pd Pd 0.504357(4) 0.126213(3) 0.500010(13) 0.01707(3) Uani 1 1 d . . . Br Br 0.563477(5) 0.145762(5) 0.49045(2) 0.02669(5) Uani 1 1 d . . . C11 C 0.43247(5) 0.13900(4) 0.2451(2) 0.0208(4) Uani 1 1 d . . . C12 C 0.44931(5) 0.16485(5) 0.2410(2) 0.0216(4) Uani 1 1 d . . . C13 C 0.43387(7) 0.18658(5) 0.18476(19) 0.0256(5) Uani 1 1 d . . . H13 H 0.4453 0.2041 0.1817 0.031 Uiso 1 1 calc R . . C14 C 0.40240(7) 0.18320(6) 0.1335(2) 0.0306(5) Uani 1 1 d . . . H14 H 0.3925 0.1982 0.0949 0.037 Uiso 1 1 calc R . . C15 C 0.38550(7) 0.15777(6) 0.1389(2) 0.0300(5) Uani 1 1 d . . . H15 H 0.3636 0.1553 0.1053 0.036 Uiso 1 1 calc R . . C16 C 0.40062(6) 0.13584(5) 0.1935(2) 0.0257(5) Uani 1 1 d . . . H16 H 0.3891 0.1184 0.1959 0.031 Uiso 1 1 calc R . . C1 C 0.44769(6) 0.11366(5) 0.29961(18) 0.0219(4) Uani 1 1 d . . . H1A H 0.4417 0.0968 0.2583 0.026 Uiso 1 1 calc R . . H1B H 0.4734 0.1154 0.3003 0.026 Uiso 1 1 calc R . . N21 N 0.43540(5) 0.10987(4) 0.40817(16) 0.0196(4) Uani 1 1 d . . . C22 C 0.45473(5) 0.11404(4) 0.4949(2) 0.0184(3) Uani 1 1 d . . . N23 N 0.43394(5) 0.10880(4) 0.57717(16) 0.0199(4) Uani 1 1 d . . . C24 C 0.40137(6) 0.10028(5) 0.5419(2) 0.0245(5) Uani 1 1 d . . . H24 H 0.3822 0.095 0.5845 0.029 Uiso 1 1 calc R . . C25 C 0.40221(6) 0.10094(5) 0.4370(2) 0.0245(5) Uani 1 1 d . . . H25 H 0.3837 0.0962 0.3907 0.029 Uiso 1 1 calc R . . C2 C 0.44329(6) 0.11337(5) 0.68809(18) 0.0203(4) Uani 1 1 d . . . H2A H 0.4688 0.1156 0.6939 0.024 Uiso 1 1 calc R . . H2B H 0.4365 0.0968 0.7299 0.024 Uiso 1 1 calc R . . C31 C 0.44027(6) 0.16575(5) 0.73188(18) 0.0211(4) Uani 1 1 d . . . C32 C 0.42567(6) 0.13891(4) 0.73290(18) 0.0201(4) Uani 1 1 d . . . C33 C 0.39305(6) 0.13502(5) 0.77910(19) 0.0242(4) Uani 1 1 d . . . H33 H 0.3831 0.1169 0.7802 0.029 Uiso 1 1 calc R . . C34 C 0.37495(7) 0.15712(6) 0.8234(2) 0.0308(5) Uani 1 1 d . . . H34 H 0.3527 0.1541 0.8542 0.037 Uiso 1 1 calc R . . C35 C 0.38938(8) 0.18354(6) 0.8226(2) 0.0325(6) Uani 1 1 d . . . H35 H 0.3772 0.1988 0.8528 0.039 Uiso 1 1 calc R . . C36 C 0.42175(7) 0.18764(5) 0.7774(2) 0.0288(5) Uani 1 1 d . . . H36 H 0.4316 0.2058 0.7775 0.035 Uiso 1 1 calc R . . C3 C 0.47553(6) 0.17229(5) 0.68417(19) 0.0221(4) Uani 1 1 d . . . H3A H 0.4865 0.1876 0.7246 0.027 Uiso 1 1 calc R . . H3B H 0.4907 0.1557 0.6902 0.027 Uiso 1 1 calc R . . N41 N 0.47316(5) 0.18054(4) 0.57256(16) 0.0192(3) Uani 1 1 d . . . C42 C 0.48417(5) 0.16502(4) 0.4903(2) 0.0191(4) Uani 1 1 d . . . N43 N 0.47769(5) 0.18013(4) 0.40456(15) 0.0195(3) Uani 1 1 d . . . C44 C 0.46268(6) 0.20545(5) 0.43142(19) 0.0207(4) Uani 1 1 d . . . H44 H 0.4559 0.2198 0.3844 0.025 Uiso 1 1 calc R . . C45 C 0.45966(6) 0.20569(5) 0.5363(2) 0.0224(4) Uani 1 1 d . . . H45 H 0.4501 0.2202 0.5781 0.027 Uiso 1 1 calc R . . C4 C 0.48351(6) 0.17084(5) 0.29578(19) 0.0221(4) Uani 1 1 d . . . H4A H 0.498 0.1538 0.2961 0.027 Uiso 1 1 calc R . . H4B H 0.4963 0.1854 0.2566 0.027 Uiso 1 1 calc R . . P1 P 0.525130(14) 0.080826(12) 0.52292(4) 0.01830(10) Uani 1 1 d . . . C111 C 0.49306(6) 0.05643(5) 0.57649(19) 0.0219(4) Uani 1 1 d . . . C112 C 0.49407(7) 0.04677(6) 0.6787(2) 0.0304(5) Uani 1 1 d . . . H112 H 0.5127 0.0519 0.7237 0.036 Uiso 1 1 calc R . . C113 C 0.46781(8) 0.02947(6) 0.7161(3) 0.0397(7) Uani 1 1 d . . . H113 H 0.4687 0.0229 0.7866 0.048 Uiso 1 1 calc R . . C114 C 0.44057(8) 0.02175(6) 0.6521(3) 0.0412(7) Uani 1 1 d . . . H114 H 0.4227 0.01 0.6782 0.049 Uiso 1 1 calc R . . C115 C 0.43942(7) 0.03138(6) 0.5488(3) 0.0368(6) Uani 1 1 d . . . H115 H 0.4207 0.0262 0.5041 0.044 Uiso 1 1 calc R . . C116 C 0.46552(6) 0.04847(5) 0.5115(2) 0.0293(5) Uani 1 1 d . . . H116 H 0.4647 0.0549 0.4408 0.035 Uiso 1 1 calc R . . C121 C 0.53773(6) 0.06354(6) 0.4020(2) 0.0273(5) Uani 1 1 d . . . C122 C 0.54115(7) 0.07853(8) 0.3095(2) 0.0366(6) Uani 1 1 d . . . H122 H 0.5384 0.0982 0.3096 0.044 Uiso 1 1 calc R . . C123 C 0.54867(9) 0.06439(10) 0.2154(3) 0.0565(10) Uani 1 1 d . . . H123 H 0.5499 0.0744 0.151 0.068 Uiso 1 1 calc R . . C124 C 0.55436(11) 0.03546(11) 0.2169(3) 0.0663(12) Uani 1 1 d . . . H124 H 0.5602 0.026 0.1536 0.08 Uiso 1 1 calc R . . C125 C 0.55156(11) 0.02086(9) 0.3087(3) 0.0617(11) Uani 1 1 d . . . H125 H 0.5558 0.0014 0.3093 0.074 Uiso 1 1 calc R . . C126 C 0.54252(9) 0.03437(7) 0.4007(3) 0.0406(7) Uani 1 1 d . . . H126 H 0.5395 0.024 0.4636 0.049 Uiso 1 1 calc R . . C131 C 0.56219(6) 0.07924(5) 0.61134(18) 0.0211(4) Uani 1 1 d . . . C132 C 0.59122(6) 0.06256(6) 0.5927(2) 0.0284(5) Uani 1 1 d . . . H132 H 0.5915 0.0504 0.5338 0.034 Uiso 1 1 calc R . . C133 C 0.61975(7) 0.06365(6) 0.6598(2) 0.0358(6) Uani 1 1 d . . . H133 H 0.6396 0.0525 0.6454 0.043 Uiso 1 1 calc R . . C134 C 0.61947(7) 0.08079(6) 0.7470(3) 0.0352(5) Uani 1 1 d . . . H134 H 0.6389 0.0813 0.7933 0.042 Uiso 1 1 calc R . . C135 C 0.59044(7) 0.09739(6) 0.7668(2) 0.0330(6) Uani 1 1 d . . . H135 H 0.5901 0.1093 0.8265 0.04 Uiso 1 1 calc R . . C136 C 0.56211(6) 0.09659(5) 0.6997(2) 0.0271(5) Uani 1 1 d . . . H136 H 0.5424 0.1079 0.7139 0.033 Uiso 1 1 calc R . . B2 B 0.55506(6) 0.19048(5) 0.01576(19) 0.0174(4) Uani 1 1 d . . . C211 C 0.58901(6) 0.18073(4) 0.08582(17) 0.0181(4) Uani 1 1 d . . . C212 C 0.62312(6) 0.19038(5) 0.06999(19) 0.0211(4) Uani 1 1 d . . . H212 H 0.6276 0.2024 0.0123 0.025 Uiso 1 1 calc R . . C213 C 0.65070(6) 0.18290(5) 0.1361(2) 0.0254(5) Uani 1 1 d . . . H213 H 0.6733 0.1902 0.1235 0.031 Uiso 1 1 calc R . . C214 C 0.64523(6) 0.16488(5) 0.22003(19) 0.0270(5) Uani 1 1 d . . . H214 H 0.664 0.1595 0.2643 0.032 Uiso 1 1 calc R . . C215 C 0.61174(6) 0.15491(5) 0.2380(2) 0.0262(4) Uani 1 1 d . . . H215 H 0.6074 0.1427 0.2954 0.031 Uiso 1 1 calc R . . C216 C 0.58458(6) 0.16279(5) 0.17217(19) 0.0232(4) Uani 1 1 d . . . H216 H 0.562 0.1557 0.1862 0.028 Uiso 1 1 calc R . . C221 C 0.53371(6) 0.21473(4) 0.08191(18) 0.0188(4) Uani 1 1 d . . . C222 C 0.54149(6) 0.22227(5) 0.18564(18) 0.0207(4) Uani 1 1 d . . . H222 H 0.5613 0.2142 0.2183 0.025 Uiso 1 1 calc R . . C223 C 0.52134(6) 0.24110(4) 0.2433(2) 0.0226(4) Uani 1 1 d . . . H223 H 0.5275 0.2455 0.3138 0.027 Uiso 1 1 calc R . . C224 C 0.49238(6) 0.25340(5) 0.1980(2) 0.0245(5) Uani 1 1 d . . . H224 H 0.4781 0.2657 0.2376 0.029 Uiso 1 1 calc R . . C225 C 0.48457(6) 0.24746(5) 0.0935(2) 0.0241(4) Uani 1 1 d . . . H225 H 0.4652 0.2562 0.0606 0.029 Uiso 1 1 calc R . . C226 C 0.50501(6) 0.22876(5) 0.03705(19) 0.0210(4) Uani 1 1 d . . . H226 H 0.4994 0.2253 -0.0346 0.025 Uiso 1 1 calc R . . C231 C 0.53008(5) 0.16303(4) -0.0043(2) 0.0197(4) Uani 1 1 d . . . C232 C 0.49357(6) 0.16331(5) -0.0068(2) 0.0238(4) Uani 1 1 d . . . H232 H 0.482 0.1805 0.0058 0.029 Uiso 1 1 calc R . . C233 C 0.47336(6) 0.13972(5) -0.0269(2) 0.0291(5) Uani 1 1 d . . . H233 H 0.4487 0.1411 -0.0271 0.035 Uiso 1 1 calc R . . C234 C 0.48937(7) 0.11427(6) -0.0464(2) 0.0304(5) Uani 1 1 d . . . H234 H 0.4759 0.0981 -0.0608 0.037 Uiso 1 1 calc R . . C235 C 0.52540(7) 0.11282(5) -0.0444(2) 0.0311(5) Uani 1 1 d . . . H235 H 0.5368 0.0955 -0.0566 0.037 Uiso 1 1 calc R . . C236 C 0.54496(6) 0.13671(5) -0.0246(2) 0.0271(5) Uani 1 1 d . . . H236 H 0.5696 0.1352 -0.0249 0.033 Uiso 1 1 calc R . . C241 C 0.56821(5) 0.20337(5) -0.09712(17) 0.0185(4) Uani 1 1 d . . . C242 C 0.58328(6) 0.23020(5) -0.10185(18) 0.0213(4) Uani 1 1 d . . . H242 H 0.584 0.2411 -0.0396 0.026 Uiso 1 1 calc R . . C243 C 0.59708(6) 0.24124(5) -0.1940(2) 0.0258(5) Uani 1 1 d . . . H243 H 0.6072 0.2593 -0.1935 0.031 Uiso 1 1 calc R . . C244 C 0.59609(6) 0.22603(6) -0.28648(19) 0.0274(5) Uani 1 1 d . . . H244 H 0.6054 0.2335 -0.3496 0.033 Uiso 1 1 calc R . . C245 C 0.58131(7) 0.19977(6) -0.28582(19) 0.0277(5) Uani 1 1 d . . . H245 H 0.5805 0.1891 -0.3488 0.033 Uiso 1 1 calc R . . C246 C 0.56755(6) 0.18884(5) -0.19294(19) 0.0229(4) Uani 1 1 d . . . H246 H 0.5573 0.1708 -0.1946 0.027 Uiso 1 1 calc R . . Cl11 Cl 0.64906(3) 0.202525(19) 0.47374(8) 0.0625(3) Uani 1 1 d . . . Cl12 Cl 0.60074(2) 0.246872(15) 0.42104(6) 0.03991(16) Uani 1 1 d . . . C01 C 0.61260(10) 0.21187(6) 0.3987(3) 0.0479(8) Uani 1 1 d . . . H01A H 0.5928 0.1996 0.4171 0.057 Uiso 1 1 calc R . . H01B H 0.6179 0.2092 0.3231 0.057 Uiso 1 1 calc R . . Cl21 Cl 0.60282(6) 0.00700(3) 0.90054(15) 0.0988(8) Uani 0.801(3) 1 d P . . Cl22 Cl 0.53295(5) 0.02844(4) 0.93792(11) 0.0860(6) Uani 0.801(3) 1 d P . . C02 C 0.57390(15) 0.03370(10) 0.8894(4) 0.0576(13) Uani 0.801(3) 1 d P . . H02A H 0.5718 0.0385 0.8139 0.069 Uiso 0.801(3) 1 calc PR . . H02B H 0.5839 0.0501 0.9255 0.069 Uiso 0.801(3) 1 calc 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 Pd 0.01316(6) 0.01613(6) 0.02193(7) 0.00066(6) 0.00048(6) -0.00126(5) Br 0.01547(9) 0.02658(10) 0.03802(13) 0.00135(10) 0.00265(9) -0.00458(7) C11 0.0205(9) 0.0232(9) 0.0188(9) -0.0029(9) -0.0012(8) -0.0026(7) C12 0.0211(9) 0.0234(9) 0.0203(9) -0.0014(9) 0.0020(9) -0.0036(7) C13 0.0321(12) 0.0235(11) 0.0213(11) 0.0000(9) 0.0017(9) -0.0027(9) C14 0.0346(13) 0.0299(13) 0.0271(12) -0.0002(10) -0.0035(10) 0.0045(10) C15 0.0259(11) 0.0344(13) 0.0298(12) -0.0016(10) -0.0083(10) 0.0010(10) C16 0.0229(11) 0.0277(12) 0.0265(12) -0.0046(9) -0.0019(9) -0.0037(9) C1 0.0214(10) 0.0211(10) 0.0232(11) -0.0037(8) -0.0003(8) -0.0028(8) N21 0.0147(8) 0.0193(9) 0.0249(9) -0.0009(7) 0.0014(6) -0.0028(6) C22 0.0163(8) 0.0152(8) 0.0236(9) 0.0007(8) 0.0005(8) 0.0022(6) N23 0.0178(8) 0.0175(9) 0.0244(9) -0.0006(7) 0.0033(7) -0.0013(6) C24 0.0150(9) 0.0241(11) 0.0344(12) -0.0023(9) 0.0031(8) -0.0036(8) C25 0.0163(10) 0.0250(11) 0.0323(12) -0.0039(9) 0.0007(8) -0.0059(8) C2 0.0199(10) 0.0188(10) 0.0222(10) 0.0031(8) 0.0023(8) 0.0003(7) C31 0.0222(9) 0.0219(9) 0.0191(10) 0.0008(8) -0.0023(8) -0.0019(7) C32 0.0211(9) 0.0187(9) 0.0204(10) 0.0009(8) -0.0010(8) -0.0002(7) C33 0.0248(11) 0.0226(10) 0.0253(11) 0.0002(8) 0.0035(8) -0.0008(8) C34 0.0292(12) 0.0291(12) 0.0341(14) -0.0029(10) 0.0096(10) 0.0004(10) C35 0.0378(14) 0.0259(12) 0.0339(14) -0.0045(10) 0.0090(11) 0.0029(10) C36 0.0366(13) 0.0212(11) 0.0285(12) -0.0028(9) 0.0046(10) -0.0044(9) C3 0.0238(10) 0.0200(10) 0.0225(10) 0.0000(8) -0.0046(8) -0.0040(8) N41 0.0186(8) 0.0166(8) 0.0225(9) 0.0012(7) -0.0010(7) -0.0037(6) C42 0.0138(7) 0.0187(8) 0.0250(10) 0.0001(9) 0.0002(8) -0.0043(6) N43 0.0181(8) 0.0175(8) 0.0230(9) 0.0010(7) -0.0013(7) -0.0031(6) C44 0.0197(10) 0.0159(9) 0.0266(11) 0.0019(8) -0.0038(8) -0.0027(7) C45 0.0233(10) 0.0157(9) 0.0283(11) -0.0023(8) -0.0030(8) -0.0022(8) C4 0.0201(10) 0.0223(10) 0.0241(11) -0.0018(8) 0.0012(8) -0.0058(8) P1 0.0161(2) 0.0179(2) 0.0209(3) -0.00120(19) 0.00068(18) 0.00094(18) C111 0.0186(9) 0.0166(9) 0.0305(12) 0.0003(8) 0.0024(8) 0.0025(7) C112 0.0285(12) 0.0298(12) 0.0329(13) 0.0048(10) 0.0034(10) -0.0019(10) C113 0.0375(15) 0.0356(14) 0.0459(17) 0.0117(12) 0.0136(12) -0.0031(11) C114 0.0333(14) 0.0256(13) 0.065(2) 0.0046(13) 0.0163(14) -0.0027(10) C115 0.0236(11) 0.0247(12) 0.0620(19) -0.0024(12) -0.0001(12) -0.0048(9) C116 0.0259(10) 0.0211(10) 0.0407(15) 0.0007(10) -0.0053(10) -0.0022(8) C121 0.0225(11) 0.0349(13) 0.0245(12) -0.0079(10) -0.0002(9) 0.0010(9) C122 0.0251(12) 0.0592(19) 0.0254(13) -0.0019(12) 0.0016(10) -0.0038(12) C123 0.0393(17) 0.104(3) 0.0262(15) -0.0048(17) 0.0035(12) -0.0147(19) C124 0.057(2) 0.091(3) 0.051(2) -0.043(2) 0.0049(18) 0.000(2) C125 0.067(3) 0.063(2) 0.056(2) -0.037(2) 0.0008(19) 0.012(2) C126 0.0433(16) 0.0365(15) 0.0421(17) -0.0139(13) 0.0013(13) 0.0072(12) C131 0.0189(9) 0.0226(10) 0.0218(10) 0.0018(8) 0.0011(8) 0.0016(7) C132 0.0219(11) 0.0335(13) 0.0298(12) -0.0049(10) -0.0011(9) 0.0056(9) C133 0.0269(12) 0.0421(15) 0.0384(15) -0.0063(12) -0.0066(11) 0.0115(11) C134 0.0253(11) 0.0440(14) 0.0363(13) -0.0016(13) -0.0109(12) -0.0001(10) C135 0.0307(12) 0.0378(13) 0.0304(14) -0.0092(11) -0.0032(10) -0.0016(10) C136 0.0243(11) 0.0273(11) 0.0296(12) -0.0053(9) 0.0002(9) 0.0026(9) B2 0.0168(9) 0.0170(9) 0.0186(11) -0.0007(8) 0.0018(8) 0.0026(7) C211 0.0184(9) 0.0176(9) 0.0183(9) -0.0032(7) 0.0005(7) 0.0034(7) C212 0.0211(10) 0.0189(10) 0.0233(10) 0.0003(8) 0.0000(8) 0.0016(7) C213 0.0196(10) 0.0258(11) 0.0309(12) -0.0047(9) -0.0033(9) 0.0036(8) C214 0.0252(11) 0.0321(12) 0.0238(11) -0.0033(9) -0.0052(8) 0.0110(9) C215 0.0277(10) 0.0313(11) 0.0195(10) 0.0024(9) 0.0019(9) 0.0106(8) C216 0.0234(10) 0.0224(10) 0.0237(11) 0.0015(8) 0.0003(8) 0.0050(8) C221 0.0179(9) 0.0158(9) 0.0228(10) 0.0003(8) 0.0025(7) 0.0005(7) C222 0.0193(9) 0.0207(10) 0.0220(10) -0.0002(8) 0.0003(8) 0.0020(7) C223 0.0243(9) 0.0202(9) 0.0235(10) -0.0026(9) 0.0056(9) -0.0010(7) C224 0.0209(10) 0.0187(10) 0.0338(13) -0.0036(9) 0.0080(9) 0.0003(8) C225 0.0170(9) 0.0209(10) 0.0343(13) 0.0005(9) 0.0021(9) 0.0026(8) C226 0.0186(9) 0.0203(10) 0.0243(10) 0.0005(8) -0.0002(8) 0.0023(7) C231 0.0206(9) 0.0183(8) 0.0202(9) 0.0014(8) -0.0013(9) -0.0004(7) C232 0.0190(8) 0.0246(9) 0.0278(11) 0.0004(10) 0.0008(9) 0.0003(7) C233 0.0221(10) 0.0328(12) 0.0324(13) -0.0035(10) 0.0003(9) -0.0038(9) C234 0.0309(12) 0.0259(12) 0.0345(13) -0.0034(10) 0.0002(10) -0.0103(10) C235 0.0312(12) 0.0219(11) 0.0403(14) -0.0037(10) 0.0010(11) -0.0003(9) C236 0.0225(10) 0.0213(10) 0.0375(14) -0.0041(9) -0.0005(9) -0.0015(8) C241 0.0162(9) 0.0214(10) 0.0180(9) 0.0000(7) -0.0007(7) 0.0039(7) C242 0.0225(10) 0.0210(10) 0.0203(10) -0.0017(8) -0.0006(8) 0.0003(8) C243 0.0224(10) 0.0252(11) 0.0298(12) 0.0065(9) 0.0009(9) 0.0010(8) C244 0.0223(10) 0.0394(13) 0.0206(10) 0.0070(9) 0.0046(8) 0.0074(9) C245 0.0279(11) 0.0359(13) 0.0193(10) -0.0021(9) 0.0006(8) 0.0101(10) C246 0.0229(10) 0.0234(11) 0.0224(11) -0.0033(8) -0.0024(8) 0.0046(8) Cl11 0.0832(7) 0.0442(4) 0.0600(6) -0.0113(4) -0.0283(5) 0.0276(4) Cl12 0.0533(4) 0.0299(3) 0.0365(3) 0.0027(3) -0.0008(3) 0.0076(3) C01 0.061(2) 0.0290(14) 0.054(2) -0.0061(14) -0.0158(16) 0.0047(14) Cl21 0.1602(19) 0.0512(8) 0.0849(12) -0.0154(7) -0.0613(12) 0.0277(9) Cl22 0.1255(15) 0.0875(11) 0.0449(7) 0.0003(7) -0.0113(8) -0.0406(10) C02 0.079(4) 0.048(3) 0.046(3) -0.004(2) -0.021(2) -0.005(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Pd C22 1.9960(19) . ? Pd C42 2.022(2) . ? Pd P1 2.3387(6) . ? Pd Br 2.4614(3) . ? C11 C16 1.397(3) . ? C11 C12 1.401(3) . ? C11 C1 1.517(3) . ? C12 C13 1.397(3) . ? C12 C4 1.515(3) . ? C13 C14 1.383(4) . ? C13 H13 0.95 . ? C14 C15 1.385(4) . ? C14 H14 0.95 . ? C15 C16 1.388(4) . ? C15 H15 0.95 . ? C16 H16 0.95 . ? C1 N21 1.470(3) . ? C1 H1A 0.99 . ? C1 H1B 0.99 . ? N21 C22 1.345(3) . ? N21 C25 1.395(3) . ? C22 N23 1.339(3) . ? N23 C24 1.391(3) . ? N23 C2 1.471(3) . ? C24 C25 1.334(3) . ? C24 H24 0.95 . ? C25 H25 0.95 . ? C2 C32 1.512(3) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C31 C36 1.395(3) . ? C31 C32 1.405(3) . ? C31 C3 1.517(3) . ? C32 C33 1.397(3) . ? C33 C34 1.388(4) . ? C33 H33 0.95 . ? C34 C35 1.385(4) . ? C34 H34 0.95 . ? C35 C36 1.384(4) . ? C35 H35 0.95 . ? C36 H36 0.95 . ? C3 N41 1.475(3) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? N41 C42 1.352(3) . ? N41 C45 1.393(3) . ? C42 N43 1.333(3) . ? N43 C44 1.388(3) . ? N43 C4 1.470(3) . ? C44 C45 1.338(3) . ? C44 H44 0.95 . ? C45 H45 0.95 . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? P1 C121 1.812(3) . ? P1 C131 1.816(2) . ? P1 C111 1.831(2) . ? C111 C112 1.380(4) . ? C111 C116 1.396(3) . ? C112 C113 1.391(4) . ? C112 H112 0.95 . ? C113 C114 1.376(5) . ? C113 H113 0.95 . ? C114 C115 1.393(5) . ? C114 H114 0.95 . ? C115 C116 1.380(4) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C121 C122 1.385(4) . ? C121 C126 1.413(4) . ? C122 C123 1.404(5) . ? C122 H122 0.95 . ? C123 C124 1.406(7) . ? C123 H123 0.95 . ? C124 C125 1.366(7) . ? C124 H124 0.95 . ? C125 C126 1.381(4) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C131 C132 1.394(3) . ? C131 C136 1.398(3) . ? C132 C133 1.390(4) . ? C132 H132 0.95 . ? C133 C134 1.381(4) . ? C133 H133 0.95 . ? C134 C135 1.394(4) . ? C134 H134 0.95 . ? C135 C136 1.383(4) . ? C135 H135 0.95 . ? C136 H136 0.95 . ? B2 C241 1.642(3) . ? B2 C211 1.647(3) . ? B2 C231 1.650(3) . ? B2 C221 1.654(3) . ? C211 C212 1.405(3) . ? C211 C216 1.405(3) . ? C212 C213 1.399(3) . ? C212 H212 0.95 . ? C213 C214 1.389(4) . ? C213 H213 0.95 . ? C214 C215 1.392(4) . ? C214 H214 0.95 . ? C215 C216 1.390(3) . ? C215 H215 0.95 . ? C216 H216 0.95 . ? C221 C222 1.399(3) . ? C221 C226 1.412(3) . ? C222 C223 1.398(3) . ? C222 H222 0.95 . ? C223 C224 1.386(3) . ? C223 H223 0.95 . ? C224 C225 1.390(4) . ? C224 H224 0.95 . ? C225 C226 1.393(3) . ? C225 H225 0.95 . ? C226 H226 0.95 . ? C231 C232 1.404(3) . ? C231 C236 1.411(3) . ? C232 C233 1.396(3) . ? C232 H232 0.95 . ? C233 C234 1.390(4) . ? C233 H233 0.95 . ? C234 C235 1.387(4) . ? C234 H234 0.95 . ? C235 C236 1.394(3) . ? C235 H235 0.95 . ? C236 H236 0.95 . ? C241 C246 1.404(3) . ? C241 C242 1.413(3) . ? C242 C243 1.391(3) . ? C242 H242 0.95 . ? C243 C244 1.384(4) . ? C243 H243 0.95 . ? C244 C245 1.383(4) . ? C244 H244 0.95 . ? C245 C246 1.396(4) . ? C245 H245 0.95 . ? C246 H246 0.95 . ? Cl11 C01 1.754(4) . ? Cl12 C01 1.764(3) . ? C01 H01A 0.99 . ? C01 H01B 0.99 . ? Cl21 C02 1.702(5) . ? Cl22 C02 1.709(6) . ? C02 H02A 0.99 . ? C02 H02B 0.99 . ? 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 C22 Pd C42 84.33(8) . . ? C22 Pd P1 93.29(6) . . ? C42 Pd P1 175.59(7) . . ? C22 Pd Br 172.85(6) . . ? C42 Pd Br 89.99(5) . . ? P1 Pd Br 92.651(16) . . ? C16 C11 C12 118.9(2) . . ? C16 C11 C1 117.7(2) . . ? C12 C11 C1 123.3(2) . . ? C13 C12 C11 119.0(2) . . ? C13 C12 C4 117.5(2) . . ? C11 C12 C4 123.5(2) . . ? C14 C13 C12 121.7(2) . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C13 C14 C15 119.3(2) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C14 C15 C16 119.8(2) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C15 C16 C11 121.3(2) . . ? C15 C16 H16 119.4 . . ? C11 C16 H16 119.4 . . ? N21 C1 C11 113.86(19) . . ? N21 C1 H1A 108.8 . . ? C11 C1 H1A 108.8 . . ? N21 C1 H1B 108.8 . . ? C11 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? C22 N21 C25 109.6(2) . . ? C22 N21 C1 125.01(18) . . ? C25 N21 C1 125.4(2) . . ? N23 C22 N21 106.40(17) . . ? N23 C22 Pd 126.86(18) . . ? N21 C22 Pd 126.74(17) . . ? C22 N23 C24 109.9(2) . . ? C22 N23 C2 125.03(19) . . ? C24 N23 C2 124.9(2) . . ? C25 C24 N23 107.1(2) . . ? C25 C24 H24 126.5 . . ? N23 C24 H24 126.5 . . ? C24 C25 N21 107.0(2) . . ? C24 C25 H25 126.5 . . ? N21 C25 H25 126.5 . . ? N23 C2 C32 111.86(18) . . ? N23 C2 H2A 109.2 . . ? C32 C2 H2A 109.2 . . ? N23 C2 H2B 109.2 . . ? C32 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? C36 C31 C32 118.9(2) . . ? C36 C31 C3 117.8(2) . . ? C32 C31 C3 123.4(2) . . ? C33 C32 C31 119.0(2) . . ? C33 C32 C2 116.86(19) . . ? C31 C32 C2 124.1(2) . . ? C34 C33 C32 121.2(2) . . ? C34 C33 H33 119.4 . . ? C32 C33 H33 119.4 . . ? C35 C34 C33 119.8(2) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C36 C35 C34 119.6(2) . . ? C36 C35 H35 120.2 . . ? C34 C35 H35 120.2 . . ? C35 C36 C31 121.6(2) . . ? C35 C36 H36 119.2 . . ? C31 C36 H36 119.2 . . ? N41 C3 C31 112.62(19) . . ? N41 C3 H3A 109.1 . . ? C31 C3 H3A 109.1 . . ? N41 C3 H3B 109.1 . . ? C31 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? C42 N41 C45 109.8(2) . . ? C42 N41 C3 125.2(2) . . ? C45 N41 C3 125.0(2) . . ? N43 C42 N41 105.88(18) . . ? N43 C42 Pd 128.56(18) . . ? N41 C42 Pd 125.52(18) . . ? C42 N43 C44 110.69(19) . . ? C42 N43 C4 125.1(2) . . ? C44 N43 C4 124.1(2) . . ? C45 C44 N43 106.8(2) . . ? C45 C44 H44 126.6 . . ? N43 C44 H44 126.6 . . ? C44 C45 N41 106.8(2) . . ? C44 C45 H45 126.6 . . ? N41 C45 H45 126.6 . . ? N43 C4 C12 110.97(19) . . ? N43 C4 H4A 109.4 . . ? C12 C4 H4A 109.4 . . ? N43 C4 H4B 109.4 . . ? C12 C4 H4B 109.4 . . ? H4A C4 H4B 108 . . ? C121 P1 C131 107.22(11) . . ? C121 P1 C111 101.67(11) . . ? C131 P1 C111 105.74(11) . . ? C121 P1 Pd 114.34(9) . . ? C131 P1 Pd 112.57(8) . . ? C111 P1 Pd 114.35(7) . . ? C112 C111 C116 119.1(2) . . ? C112 C111 P1 123.09(19) . . ? C116 C111 P1 117.72(19) . . ? C111 C112 C113 120.1(3) . . ? C111 C112 H112 119.9 . . ? C113 C112 H112 119.9 . . ? C114 C113 C112 120.7(3) . . ? C114 C113 H113 119.6 . . ? C112 C113 H113 119.6 . . ? C113 C114 C115 119.5(3) . . ? C113 C114 H114 120.3 . . ? C115 C114 H114 120.3 . . ? C116 C115 C114 119.9(3) . . ? C116 C115 H115 120.1 . . ? C114 C115 H115 120.1 . . ? C115 C116 C111 120.7(3) . . ? C115 C116 H116 119.7 . . ? C111 C116 H116 119.7 . . ? C122 C121 C126 119.5(3) . . ? C122 C121 P1 120.5(2) . . ? C126 C121 P1 119.9(2) . . ? C121 C122 C123 119.4(3) . . ? C121 C122 H122 120.3 . . ? C123 C122 H122 120.3 . . ? C122 C123 C124 119.9(3) . . ? C122 C123 H123 120 . . ? C124 C123 H123 120 . . ? C125 C124 C123 120.4(3) . . ? C125 C124 H124 119.8 . . ? C123 C124 H124 119.8 . . ? C124 C125 C126 120.1(4) . . ? C124 C125 H125 119.9 . . ? C126 C125 H125 119.9 . . ? C125 C126 C121 120.6(4) . . ? C125 C126 H126 119.7 . . ? C121 C126 H126 119.7 . . ? C132 C131 C136 118.7(2) . . ? C132 C131 P1 123.14(19) . . ? C136 C131 P1 118.07(17) . . ? C133 C132 C131 120.4(2) . . ? C133 C132 H132 119.8 . . ? C131 C132 H132 119.8 . . ? C134 C133 C132 120.6(2) . . ? C134 C133 H133 119.7 . . ? C132 C133 H133 119.7 . . ? C133 C134 C135 119.4(2) . . ? C133 C134 H134 120.3 . . ? C135 C134 H134 120.3 . . ? C136 C135 C134 120.3(3) . . ? C136 C135 H135 119.9 . . ? C134 C135 H135 119.9 . . ? C135 C136 C131 120.6(2) . . ? C135 C136 H136 119.7 . . ? C131 C136 H136 119.7 . . ? C241 B2 C211 109.59(17) . . ? C241 B2 C231 110.20(18) . . ? C211 B2 C231 108.50(17) . . ? C241 B2 C221 109.35(17) . . ? C211 B2 C221 108.55(17) . . ? C231 B2 C221 110.62(17) . . ? C212 C211 C216 115.3(2) . . ? C212 C211 B2 124.61(19) . . ? C216 C211 B2 120.01(19) . . ? C213 C212 C211 122.4(2) . . ? C213 C212 H212 118.8 . . ? C211 C212 H212 118.8 . . ? C214 C213 C212 120.4(2) . . ? C214 C213 H213 119.8 . . ? C212 C213 H213 119.8 . . ? C213 C214 C215 118.7(2) . . ? C213 C214 H214 120.7 . . ? C215 C214 H214 120.7 . . ? C216 C215 C214 120.1(2) . . ? C216 C215 H215 119.9 . . ? C214 C215 H215 119.9 . . ? C215 C216 C211 123.1(2) . . ? C215 C216 H216 118.5 . . ? C211 C216 H216 118.5 . . ? C222 C221 C226 115.1(2) . . ? C222 C221 B2 123.71(19) . . ? C226 C221 B2 121.2(2) . . ? C223 C222 C221 122.9(2) . . ? C223 C222 H222 118.6 . . ? C221 C222 H222 118.6 . . ? C224 C223 C222 120.2(2) . . ? C224 C223 H223 119.9 . . ? C222 C223 H223 119.9 . . ? C223 C224 C225 118.9(2) . . ? C223 C224 H224 120.6 . . ? C225 C224 H224 120.6 . . ? C224 C225 C226 120.2(2) . . ? C224 C225 H225 119.9 . . ? C226 C225 H225 119.9 . . ? C225 C226 C221 122.7(2) . . ? C225 C226 H226 118.7 . . ? C221 C226 H226 118.7 . . ? C232 C231 C236 114.18(19) . . ? C232 C231 B2 125.27(18) . . ? C236 C231 B2 120.51(18) . . ? C233 C232 C231 123.5(2) . . ? C233 C232 H232 118.2 . . ? C231 C232 H232 118.2 . . ? C234 C233 C232 119.9(2) . . ? C234 C233 H233 120 . . ? C232 C233 H233 120 . . ? C235 C234 C233 118.9(2) . . ? C235 C234 H234 120.6 . . ? C233 C234 H234 120.6 . . ? C234 C235 C236 120.0(2) . . ? C234 C235 H235 120 . . ? C236 C235 H235 120 . . ? C235 C236 C231 123.5(2) . . ? C235 C236 H236 118.3 . . ? C231 C236 H236 118.3 . . ? C246 C241 C242 115.1(2) . . ? C246 C241 B2 124.4(2) . . ? C242 C241 B2 120.46(19) . . ? C243 C242 C241 122.6(2) . . ? C243 C242 H242 118.7 . . ? C241 C242 H242 118.7 . . ? C244 C243 C242 120.2(2) . . ? C244 C243 H243 119.9 . . ? C242 C243 H243 119.9 . . ? C245 C244 C243 119.1(2) . . ? C245 C244 H244 120.4 . . ? C243 C244 H244 120.4 . . ? C244 C245 C246 120.2(2) . . ? C244 C245 H245 119.9 . . ? C246 C245 H245 119.9 . . ? C245 C246 C241 122.7(2) . . ? C245 C246 H246 118.7 . . ? C241 C246 H246 118.7 . . ? Cl11 C01 Cl12 111.26(18) . . ? Cl11 C01 H01A 109.4 . . ? Cl12 C01 H01A 109.4 . . ? Cl11 C01 H01B 109.4 . . ? Cl12 C01 H01B 109.4 . . ? H01A C01 H01B 108 . . ? Cl21 C02 Cl22 117.4(3) . . ? Cl21 C02 H02A 107.9 . . ? Cl22 C02 H02A 108 . . ? Cl21 C02 H02B 107.9 . . ? Cl22 C02 H02B 108 . . ? H02A C02 H02B 107.2 . . ? #===END