# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2278 data_global _audit_creation_method Xtal3.6 _audit_creation_date 00-07-24 _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 Nedlands Western Australia 6907 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 _publ_contact_letter ; ? #<< contact letter ; _publ_requested_journal J.Chem.Soc.,(Dalton) _publ_requested_category ? _publ_section_title ; Palladium carbene complexes derived form imidazolium-linked ortho-cyclophanes ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Baker, Murray V.' . ; Department of Chemistry, University of Western Australia, Nedlands, WA 6907 Australia. ; 'Skelton, Brian W.' . ; Department of Chemistry, University of Western Australia, Nedlands, WA 6907 Australia. ; 'White, Allan H.' . ; Department of Chemistry, University of Western Australia, Nedlands, WA 6907 Australia. ; 'Williams, Charlotte C.' . ; Department of Chemistry, University of Western Australia, Nedlands, WA 6907 Australia. ; _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _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. ; _publ_section_figure_captions ; ? #<< figure captions ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_mbpd # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C26 H26.25 Br1.75 N6 O.25 Pd1' _chemical_formula_moiety ? _chemical_formula_weight 673.04 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p_1_21/n_1 _symmetry_space_group_name_Hall -p_2yn loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 14.592(2) _cell_length_b 8.6343(9) _cell_length_c 22.013(2) _cell_angle_alpha 90.00000 _cell_angle_beta 104.547(2) _cell_angle_gamma 90.00000 _cell_volume 2684.5(5) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.665 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 2833 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26.4 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 3.32 _exptl_crystal_description plate _exptl_crystal_size_max .30 _exptl_crystal_size_mid .30 _exptl_crystal_size_min .08 _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 .636 _exptl_absorpt_correction_T_max .894 _diffrn_reflns_number 29981 _reflns_number_total 6700 _reflns_Friedel_coverage ? _reflns_number_gt 3285 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.19 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .091 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .043 _refine_ls_wR_factor_ref .037 _refine_ls_goodness_of_fit_ref .914 _refine_ls_number_reflns 3285 _refine_ls_number_parameters 318 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .043 _refine_diff_density_min -.638 _refine_diff_density_max .834 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 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 ? 0 104 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 105 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Br ? 0 7 -.374 2.456 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 24 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 1 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' Pd ? 0 4 -1.177 1.007 '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 Pd .44685(3) .75185(6) .27533(2) .0357(2) Uani ? ? 1.00000 ? ? Br1 .51992(5) .99730(9) .32142(3) .0529(5) Uani ? ? .868(3) ? ? O1 .51992(5) .99730(9) .32142(3) .0529(5) Uani ? ? .132(3) ? ? Br2 .41354(5) .65217(9) .37319(3) .0526(5) Uani ? ? .873(3) ? ? O2 .41354(5) .65217(9) .37319(3) .0526(5) Uani ? ? .127(3) ? ? C11 .2484(4) .8171(7) .0955(3) .040(3) Uani ? ? 1.00000 ? ? C12 .2092(4) .6858(7) .1162(3) .038(3) Uani ? ? 1.00000 ? ? C13 .1454(4) .5966(7) .0717(3) .049(4) Uani ? ? 1.00000 ? ? C14 .1205(4) .6372(8) .0086(3) .053(4) Uani ? ? 1.00000 ? ? C15 .1589(4) .7668(9) -.0111(3) .053(4) Uani ? ? 1.00000 ? ? C16 .2223(4) .8566(7) .0321(3) .047(4) Uani ? ? 1.00000 ? ? C1 .3176(4) .9224(7) .1390(3) .047(4) Uani ? ? 1.00000 ? ? N21 .4171(3) .8797(5) .1450(2) .040(3) Uani ? ? 1.00000 ? ? C22 .4740(4) .8083(6) .1953(3) .035(3) Uani ? ? 1.00000 ? ? N23 .5562(3) .7835(5) .1793(2) .040(3) Uani ? ? 1.00000 ? ? C24 .5503(5) .8413(8) .1200(3) .051(4) Uani ? ? 1.00000 ? ? C25 .4646(5) .9007(8) .0982(3) .050(4) Uani ? ? 1.00000 ? ? C2 .6373(4) .7026(7) .2189(3) .049(4) Uani ? ? 1.00000 ? ? C31 .6083(4) .4070(8) .2150(3) .046(4) Uani ? ? 1.00000 ? ? C32 .6491(4) .5402(8) .1953(3) .047(4) Uani ? ? 1.00000 ? ? C33 .7031(5) .5212(9) .1521(3) .065(5) Uani ? ? 1.00000 ? ? C34 .7137(5) .3795(11) .1265(4) .079(6) Uani ? ? 1.00000 ? ? C35 .6724(5) .2532(10) .1442(4) .077(5) Uani ? ? 1.00000 ? ? C36 .6214(5) .2647(9) .1889(3) .062(4) Uani ? ? 1.00000 ? ? C3 .5502(4) .4113(7) .2631(3) .045(3) Uani ? ? 1.00000 ? ? N41 .4484(3) .4269(6) .2338(2) .040(3) Uani ? ? 1.00000 ? ? C42 .3984(4) .5562(7) .2333(2) .036(3) Uani ? ? 1.00000 ? ? N43 .3098(3) .5229(6) .1995(2) .038(3) Uani ? ? 1.00000 ? ? C44 .3054(5) .3705(8) .1794(3) .049(4) Uani ? ? 1.00000 ? ? C45 .3923(5) .3114(7) .2006(3) .049(4) Uani ? ? 1.00000 ? ? C4 .2310(4) .6322(8) .1834(3) .048(4) Uani ? ? 1.00000 ? ? N101 .7132(5) .3913(9) .3957(3) .091(5) Uani ? ? 1.00000 ? ? C101 .6565(6) .3556(9) .4199(3) .064(5) Uani ? ? 1.00000 ? ? C102 .5813(6) .3119(9) .4475(4) .085(6) Uani ? ? 1.00000 ? ? N201 .3846(9) .2284(10) .0249(4) .158(8) Uani ? ? 1.00000 ? ? C201 .3946(7) .3518(11) .0363(4) .089(6) Uani ? ? 1.00000 ? ? C202 .4071(7) .5102(11) .0520(4) .104(7) Uani ? ? 1.00000 ? ? H1a .30759 1.02686 .12312 .05400 Uiso ? ? 1.00000 ? ? H1b .30515 .92116 .17968 .05400 Uiso ? ? 1.00000 ? ? H13 .11701 .50497 .08550 .06000 Uiso ? ? 1.00000 ? ? H14 .07694 .57428 -.02132 .06100 Uiso ? ? 1.00000 ? ? H15 .13976 .79580 -.05484 .06400 Uiso ? ? 1.00000 ? ? H16 .25071 .94756 .01812 .05500 Uiso ? ? 1.00000 ? ? H2a .69411 .76101 .21964 .05100 Uiso ? ? 1.00000 ? ? H2b .63022 .69776 .26068 .05100 Uiso ? ? 1.00000 ? ? H24 .59918 .83603 .09735 .06400 Uiso ? ? 1.00000 ? ? H25 .43957 .94811 .05756 .05900 Uiso ? ? 1.00000 ? ? H3a .56111 .31896 .28775 .05000 Uiso ? ? 1.00000 ? ? H3b .57032 .49796 .29078 .05000 Uiso ? ? 1.00000 ? ? H33 .73314 .61082 .13891 .07800 Uiso ? ? 1.00000 ? ? H34 .74901 .36574 .09680 .09800 Uiso ? ? 1.00000 ? ? H35 .67930 .14879 .12641 .08800 Uiso ? ? 1.00000 ? ? H36 .59215 .17183 .20313 .07300 Uiso ? ? 1.00000 ? ? H4a .24737 .72285 .21034 .05600 Uiso ? ? 1.00000 ? ? H4b .17608 .58730 .19151 .05600 Uiso ? ? 1.00000 ? ? H44 .25080 .31816 .15387 .05700 Uiso ? ? 1.00000 ? ? H45 .41165 .20568 .19484 .05900 Uiso ? ? 1.00000 ? ? H102a .60382 .28092 .49059 .11100 Uiso ? ? 1.00000 ? ? H102b .54315 .22903 .42538 .11100 Uiso ? ? 1.00000 ? ? H102c .53948 .39871 .44754 .11100 Uiso ? ? 1.00000 ? ? H202a .34719 .56420 .04156 .13700 Uiso ? ? 1.00000 ? ? H202b .43366 .52690 .09731 .13700 Uiso ? ? 1.00000 ? ? H202c .44914 .56393 .03164 .13700 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 Pd .0333(2) .0433(3) .0287(2) .0000(3) .00409(15) -.0053(3) Br1 .0554(5) .0484(5) .0533(5) -.0037(4) .0108(4) -.0130(4) O1 .0554(5) .0484(5) .0533(5) -.0037(4) .0108(4) -.0130(4) Br2 .0537(5) .0684(6) .0363(4) .0108(4) .0123(3) .0066(4) O2 .0537(5) .0684(6) .0363(4) .0108(4) .0123(3) .0066(4) C11 .036(3) .043(4) .040(4) .013(3) .005(3) -.006(3) C12 .025(3) .050(4) .037(3) .007(3) .004(3) -.002(3) C13 .040(4) .056(5) .048(4) -.001(3) .007(3) -.003(3) C14 .048(4) .059(5) .045(4) -.000(4) .001(3) -.011(4) C15 .050(4) .067(5) .033(3) .015(4) -.003(3) -.001(4) C16 .047(4) .044(4) .046(4) .007(3) .004(3) .007(3) C1 .050(4) .039(4) .048(4) .007(3) .006(3) -.004(3) N21 .036(3) .043(3) .040(3) .003(2) .005(2) .003(2) C22 .036(3) .030(3) .036(3) -.005(3) .003(3) -.011(3) N23 .039(3) .040(4) .043(3) -.000(2) .012(2) -.001(2) C24 .061(5) .049(4) .050(4) -.007(4) .027(3) .005(3) C25 .053(4) .056(5) .043(4) -.008(4) .012(3) .012(3) C2 .033(3) .059(5) .053(4) -.009(3) .009(3) -.004(3) C31 .032(3) .052(4) .047(4) .005(3) -.004(3) -.005(3) C32 .028(3) .054(5) .054(4) .004(3) .005(3) -.007(3) C33 .051(4) .071(6) .081(5) .008(4) .030(4) -.003(4) C34 .069(6) .092(7) .087(6) .022(5) .039(5) -.013(5) C35 .064(5) .080(6) .087(6) .016(5) .017(4) -.029(6) C36 .051(4) .053(5) .075(5) .003(4) .004(3) -.008(4) C3 .048(4) .042(4) .036(3) .006(3) -.003(3) .003(3) N41 .041(3) .040(3) .038(3) -.006(3) .006(2) -.001(2) C42 .039(4) .046(4) .022(3) -.008(3) .007(3) -.004(3) N43 .033(3) .045(3) .035(3) -.003(3) .008(2) .004(2) C44 .052(4) .047(5) .047(4) -.017(4) .009(3) -.001(3) C45 .054(4) .036(4) .054(4) -.013(3) .008(3) .000(3) C4 .036(4) .068(5) .041(4) -.004(3) .013(3) -.004(3) N101 .071(5) .121(7) .079(5) -.007(5) .016(4) -.018(5) C101 .067(5) .068(6) .048(5) .001(5) -.000(4) -.015(4) C102 .110(7) .070(6) .082(6) -.024(5) .038(5) -.007(4) N201 .285(14) .084(7) .084(6) .001(8) .008(7) -.002(5) C201 .139(9) .065(7) .059(5) -.003(7) .017(5) -.005(5) C202 .135(9) .084(7) .111(7) -.000(6) .061(6) -.009(6) # 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 Pd Br1 . . 2.4728(9) ? Pd O1 . . 2.4728(9) ? Pd Br2 . . 2.4786(9) ? Pd O2 . . 2.4786(9) ? Pd C22 . . 1.962(6) ? Pd C42 . . 1.970(6) ? C11 C12 . . 1.397(9) ? C11 C16 . . 1.393(8) ? C11 C1 . . 1.509(8) ? C12 C13 . . 1.400(8) ? C12 C4 . . 1.505(8) ? C13 C14 . . 1.391(9) ? C13 H13 . . .976(7) ? C14 C15 . . 1.369(10) ? C14 H14 . . .960(6) ? C15 C16 . . 1.386(8) ? C15 H15 . . .965(6) ? C16 H16 . . .974(6) ? C1 N21 . . 1.472(8) ? C1 H1a . . .965(6) ? C1 H1b . . .958(6) ? N21 C22 . . 1.353(7) ? N21 C25 . . 1.391(9) ? C22 N23 . . 1.350(8) ? N23 C24 . . 1.381(8) ? N23 C2 . . 1.459(7) ? C24 C25 . . 1.325(9) ? C24 H24 . . .969(8) ? C25 H25 . . .968(6) ? C2 C32 . . 1.520(9) ? C2 H2a . . .966(6) ? C2 H2b . . .952(7) ? C31 C32 . . 1.413(9) ? C31 C36 . . 1.390(10) ? C31 C3 . . 1.514(9) ? C32 C33 . . 1.389(11) ? C33 C34 . . 1.371(12) ? C33 H33 . . .969(8) ? C34 C35 . . 1.350(13) ? C34 H34 . . .936(9) ? C35 C36 . . 1.378(12) ? C35 H35 . . .998(9) ? C36 H36 . . .995(8) ? C3 N41 . . 1.469(7) ? C3 H3a . . .955(6) ? C3 H3b . . .963(6) ? N41 C42 . . 1.333(8) ? N41 C45 . . 1.378(8) ? C42 N43 . . 1.351(7) ? N43 C44 . . 1.384(8) ? N43 C4 . . 1.461(8) ? C44 C45 . . 1.337(9) ? C44 H44 . . .965(6) ? C45 H45 . . .973(6) ? C4 H4a . . .975(6) ? C4 H4b . . .947(6) ? N101 C101 . . 1.133(12) ? C101 C102 . . 1.432(13) ? C102 H102a . . .960(8) ? C102 H102b . . .961(8) ? C102 H102c . . .967(8) ? N201 C201 . . 1.096(12) ? C201 C202 . . 1.411(13) ? C202 H202a . . .967(10) ? C202 H202b . . .986(9) ? C202 H202c . . .964(11) ? 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 Br1 Pd O1 . . . .00(10) ? Br1 Pd Br2 . . . 95.71(3) ? Br1 Pd O2 . . . 95.71(3) ? Br1 Pd C22 . . . 89.54(16) ? Br1 Pd C42 . . . 174.02(18) ? O1 Pd Br2 . . . 95.71(3) ? O1 Pd O2 . . . 95.71(3) ? O1 Pd C22 . . . 89.54(16) ? O1 Pd C42 . . . 174.02(18) ? Br2 Pd O2 . . . .00000 ? Br2 Pd C22 . . . 174.07(16) ? Br2 Pd C42 . . . 89.13(16) ? O2 Pd C22 . . . 174.07(16) ? O2 Pd C42 . . . 89.13(16) ? C22 Pd C42 . . . 85.5(2) ? C12 C11 C16 . . . 119.6(5) ? C12 C11 C1 . . . 123.1(5) ? C16 C11 C1 . . . 117.3(5) ? C11 C12 C13 . . . 118.2(5) ? C11 C12 C4 . . . 124.6(5) ? C13 C12 C4 . . . 117.3(5) ? C12 C13 C14 . . . 121.5(6) ? C12 C13 H13 . . . 119.2(6) ? C14 C13 H13 . . . 119.4(6) ? C13 C14 C15 . . . 119.8(5) ? C13 C14 H14 . . . 120.3(7) ? C15 C14 H14 . . . 119.9(6) ? C14 C15 C16 . . . 119.7(5) ? C14 C15 H15 . . . 119.3(6) ? C16 C15 H15 . . . 121.0(7) ? C11 C16 C15 . . . 121.2(6) ? C11 C16 H16 . . . 118.9(5) ? C15 C16 H16 . . . 119.9(6) ? C11 C1 N21 . . . 113.2(5) ? C11 C1 H1a . . . 108.5(5) ? C11 C1 H1b . . . 109.4(6) ? N21 C1 H1a . . . 108.8(6) ? N21 C1 H1b . . . 109.1(5) ? H1a C1 H1b . . . 107.6(6) ? C1 N21 C22 . . . 125.2(5) ? C1 N21 C25 . . . 124.3(4) ? C22 N21 C25 . . . 110.4(5) ? Pd C22 N21 . . . 128.8(5) ? Pd C22 N23 . . . 126.0(4) ? N21 C22 N23 . . . 105.2(5) ? C22 N23 C24 . . . 109.9(5) ? C22 N23 C2 . . . 124.2(5) ? C24 N23 C2 . . . 125.9(5) ? N23 C24 C25 . . . 108.2(6) ? N23 C24 H24 . . . 126.2(6) ? C25 C24 H24 . . . 125.6(6) ? N21 C25 C24 . . . 106.4(5) ? N21 C25 H25 . . . 126.7(6) ? C24 C25 H25 . . . 126.9(7) ? N23 C2 C32 . . . 112.4(4) ? N23 C2 H2a . . . 108.9(5) ? N23 C2 H2b . . . 109.2(6) ? C32 C2 H2a . . . 108.5(6) ? C32 C2 H2b . . . 109.8(6) ? H2a C2 H2b . . . 107.9(5) ? C32 C31 C36 . . . 118.7(6) ? C32 C31 C3 . . . 123.2(6) ? C36 C31 C3 . . . 118.1(6) ? C2 C32 C31 . . . 123.6(6) ? C2 C32 C33 . . . 118.4(6) ? C31 C32 C33 . . . 118.0(6) ? C32 C33 C34 . . . 121.9(7) ? C32 C33 H33 . . . 119.2(7) ? C34 C33 H33 . . . 118.9(8) ? C33 C34 C35 . . . 119.8(8) ? C33 C34 H34 . . . 122.6(9) ? C35 C34 H34 . . . 117.6(9) ? C34 C35 C36 . . . 120.5(8) ? C34 C35 H35 . . . 121.3(9) ? C36 C35 H35 . . . 118.1(8) ? C31 C36 C35 . . . 121.0(7) ? C31 C36 H36 . . . 117.8(7) ? C35 C36 H36 . . . 121.2(8) ? C31 C3 N41 . . . 112.1(4) ? C31 C3 H3a . . . 109.5(6) ? C31 C3 H3b . . . 109.0(6) ? N41 C3 H3a . . . 109.4(5) ? N41 C3 H3b . . . 108.8(5) ? H3a C3 H3b . . . 107.9(5) ? C3 N41 C42 . . . 124.8(5) ? C3 N41 C45 . . . 124.6(5) ? C42 N41 C45 . . . 110.5(5) ? Pd C42 N41 . . . 125.7(4) ? Pd C42 N43 . . . 128.5(4) ? N41 C42 N43 . . . 105.8(5) ? C42 N43 C44 . . . 109.9(5) ? C42 N43 C4 . . . 125.6(5) ? C44 N43 C4 . . . 124.5(4) ? N43 C44 C45 . . . 106.7(5) ? N43 C44 H44 . . . 126.6(6) ? C45 C44 H44 . . . 126.6(7) ? N41 C45 C44 . . . 107.1(5) ? N41 C45 H45 . . . 126.4(6) ? C44 C45 H45 . . . 126.5(6) ? C12 C4 N43 . . . 113.4(5) ? C12 C4 H4a . . . 108.0(6) ? C12 C4 H4b . . . 109.3(5) ? N43 C4 H4a . . . 108.3(4) ? N43 C4 H4b . . . 110.0(6) ? H4a C4 H4b . . . 107.6(6) ? N101 C101 C102 . . . 177.0(7) ? C101 C102 H102a . . . 112.6(8) ? C101 C102 H102b . . . 112.9(8) ? C101 C102 H102c . . . 110.3(7) ? H102a C102 H102b . . . 107.7(8) ? H102a C102 H102c . . . 105.9(8) ? H102b C102 H102c . . . 107.0(8) ? N201 C201 C202 . . . 179.0(11) ? C201 C202 H202a . . . 110.8(9) ? C201 C202 H202b . . . 112.5(8) ? C201 C202 H202c . . . 114.3(10) ? H202a C202 H202b . . . 105.8(10) ? H202a C202 H202c . . . 107.5(9) ? H202b C202 H202c . . . 105.4(9) ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- 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 ? ? ? ? ? ? _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 1334 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 19 _reflns_limit_k_min 0 _reflns_limit_k_max 11 _reflns_limit_l_min -29 _reflns_limit_l_max 28 _reflns_number_observed ? _reflns_d_resolution_high .729 _reflns_d_resolution_low 13.392 _diffrn_reflns_av_sigmaI/netI .224 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _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 .127 _refine_ls_wR_factor_all .051 _refine_ls_goodness_of_fit_all .862 _refine_ls_shift/su_mean .002 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end #===END ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_cwcl # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C24 H26 Cl2 N4 Ni1 O1 S1' _chemical_formula_moiety ? _chemical_formula_weight 548.16 _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 12.7600(10) _cell_length_b 8.7243(8) _cell_length_c 22.027(2) _cell_angle_alpha 90.00000 _cell_angle_beta 102.8290(10) _cell_angle_gamma 90.00000 _cell_volume 2390.9(4) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8073 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu 1.148 _exptl_crystal_description prism _exptl_crystal_size_max .12 _exptl_crystal_size_mid .11 _exptl_crystal_size_min .07 _exptl_crystal_size_rad ? _exptl_crystal_colour green _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 .798 _exptl_absorpt_correction_T_max .928 _diffrn_reflns_number 28196 _reflns_number_total 6081 _reflns_Friedel_coverage 0 _reflns_number_gt 4783 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.27 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .039 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? #<< do not append units _diffrn_standards_decay_% 0 #<< do not append % _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .031 _refine_ls_wR_factor_ref .036 _refine_ls_goodness_of_fit_ref 1.147 _refine_ls_number_reflns 4783 _refine_ls_number_parameters 402 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max .046 _refine_diff_density_min -.324 _refine_diff_density_max .444 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 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 96 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 104 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 8 .132 .159 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 16 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ni ? 0 4 .285 1.113 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 4 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' S ? 0 4 .11 .124 '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 Ni .20967(2) .87654(3) .001825(11) .01678(12) Uani ? ? 1.00000 ? ? Cl1 .25698(4) 1.09984(6) -.03331(2) .0235(2) Uani ? ? 1.00000 ? ? Cl2 .08843(4) .82064(6) -.08438(2) .0240(2) Uani ? ? 1.00000 ? ? C1 .46752(17) .7760(2) .05725(10) .0229(10) Uani ? ? 1.00000 ? ? C11 .48397(16) .6100(2) .07732(9) .0215(9) Uani ? ? 1.00000 ? ? C12 .41094(15) .4930(2) .05259(9) .0216(9) Uani ? ? 1.00000 ? ? C13 .43166(17) .3442(3) .07467(10) .0258(10) Uani ? ? 1.00000 ? ? C14 .52236(18) .3101(3) .12081(10) .0303(11) Uani ? ? 1.00000 ? ? C15 .59380(18) .4243(3) .14492(11) .0310(11) Uani ? ? 1.00000 ? ? C16 .57516(17) .5732(3) .12300(10) .0259(10) Uani ? ? 1.00000 ? ? C2 .17914(15) 1.0482(2) .13105(9) .0196(9) Uani ? ? 1.00000 ? ? N21 .40843(12) .86094(18) .09663(7) .0185(7) Uani ? ? 1.00000 ? ? C22 .30507(15) .9091(2) .07796(9) .0180(8) Uani ? ? 1.00000 ? ? N23 .28452(12) .98422(18) .12767(7) .0181(7) Uani ? ? 1.00000 ? ? C24 .37367(16) .9823(2) .17712(9) .0212(9) Uani ? ? 1.00000 ? ? C25 .45089(16) .9041(2) .15793(9) .0212(9) Uani ? ? 1.00000 ? ? C3 .02142(16) .7898(2) .07830(9) .0208(9) Uani ? ? 1.00000 ? ? C31 .05041(15) .8321(2) .14660(9) .0201(9) Uani ? ? 1.00000 ? ? C32 .12347(15) .9494(2) .17067(9) .0194(9) Uani ? ? 1.00000 ? ? C33 .14737(16) .9766(2) .23494(9) .0209(9) Uani ? ? 1.00000 ? ? C34 .10149(17) .8897(2) .27482(10) .0235(10) Uani ? ? 1.00000 ? ? C35 .02820(17) .7759(3) .25081(10) .0262(10) Uani ? ? 1.00000 ? ? C36 .00320(17) .7491(3) .18739(10) .0247(10) Uani ? ? 1.00000 ? ? C4 .30969(15) .5207(3) .00276(9) .0211(9) Uani ? ? 1.00000 ? ? N41 .09118(12) .6681(2) .06291(7) .0190(7) Uani ? ? 1.00000 ? ? C42 .17318(15) .6918(2) .03421(8) .0179(8) Uani ? ? 1.00000 ? ? N43 .21602(13) .55189(19) .02969(7) .0193(7) Uani ? ? 1.00000 ? ? C44 .15906(16) .4400(2) .05391(9) .0225(9) Uani ? ? 1.00000 ? ? C45 .08125(17) .5124(2) .07451(9) .0231(9) Uani ? ? 1.00000 ? ? O1 .31639(13) .29506(17) .24950(8) .0348(8) Uani ? ? 1.00000 ? ? S .23993(4) .42778(6) .23628(2) .0257(2) Uani ? ? 1.00000 ? ? C01 .3109(2) .5808(3) .20927(13) .0380(13) Uani ? ? 1.00000 ? ? C02 .2355(2) .5056(3) .31061(12) .0372(13) Uani ? ? 1.00000 ? ? H1a .4275(17) .789(2) .0154(10) .022(6) Uiso ? ? 1.00000 ? ? H1b .5324(18) .826(3) .0597(10) .024(6) Uiso ? ? 1.00000 ? ? H13 .3893(18) .269(3) .0585(11) .029(6) Uiso ? ? 1.00000 ? ? H14 .5322(18) .207(3) .1352(11) .032(6) Uiso ? ? 1.00000 ? ? H15 .656(2) .403(3) .1756(12) .040(7) Uiso ? ? 1.00000 ? ? H16 .6205(17) .648(2) .1374(10) .020(6) Uiso ? ? 1.00000 ? ? H2a .1370(16) 1.057(2) .0886(9) .014(5) Uiso ? ? 1.00000 ? ? H2b .1915(18) 1.151(3) .1492(11) .031(6) Uiso ? ? 1.00000 ? ? H24 .3740(16) 1.031(3) .2133(9) .021(5) Uiso ? ? 1.00000 ? ? H25 .5189(19) .880(2) .1762(10) .025(6) Uiso ? ? 1.00000 ? ? H3a .0249(17) .871(2) .0517(10) .019(5) Uiso ? ? 1.00000 ? ? H3b -.0458(17) .754(2) .0671(9) .019(5) Uiso ? ? 1.00000 ? ? H33 .1928(15) 1.055(2) .2510(8) .007(4) Uiso ? ? 1.00000 ? ? H34 .1212(17) .909(2) .3167(10) .024(6) Uiso ? ? 1.00000 ? ? H35 -.0058(18) .720(3) .2761(10) .031(6) Uiso ? ? 1.00000 ? ? H36 -.0472(17) .678(3) .1697(10) .022(6) Uiso ? ? 1.00000 ? ? H4a .2945(16) .429(3) -.0238(10) .021(5) Uiso ? ? 1.00000 ? ? H4b .3164(17) .609(3) -.0233(10) .027(6) Uiso ? ? 1.00000 ? ? H44 .1786(16) .340(3) .0524(9) .019(5) Uiso ? ? 1.00000 ? ? H45 .0282(17) .475(3) .0940(10) .027(6) Uiso ? ? 1.00000 ? ? H01a .327(2) .551(4) .1697(15) .069(10) Uiso ? ? 1.00000 ? ? H01b .378(2) .603(3) .2383(12) .043(7) Uiso ? ? 1.00000 ? ? H01c .264(2) .667(3) .2047(13) .055(9) Uiso ? ? 1.00000 ? ? H02a .201(2) .433(4) .3336(14) .068(10) Uiso ? ? 1.00000 ? ? H02b .197(3) .596(4) .3032(15) .066(10) Uiso ? ? 1.00000 ? ? H02c .307(2) .531(3) .3349(11) .038(7) 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 Ni .01861(13) .01563(13) .01546(12) -.00210(9) .00240(9) .00069(10) Cl1 .0265(2) .0205(2) .0223(2) -.00573(19) .0028(2) .00195(19) Cl2 .0264(3) .0240(3) .0188(2) -.0048(2) -.00068(19) .0014(2) C1 .0221(10) .0209(11) .0286(11) -.0029(8) .0120(9) -.0028(9) C11 .0220(10) .0207(10) .0240(10) -.0004(8) .0099(8) -.0038(8) C12 .0224(10) .0239(11) .0190(9) .0009(8) .0057(8) -.0034(8) C13 .0260(11) .0231(11) .0271(11) -.0024(9) .0031(9) -.0028(9) C14 .0326(12) .0237(12) .0319(12) .0050(9) .0012(10) .0033(10) C15 .0260(11) .0329(13) .0310(12) .0049(9) -.0003(9) -.0015(10) C16 .0213(10) .0262(11) .0294(11) -.0018(9) .0045(9) -.0085(9) C2 .0190(9) .0182(10) .0214(10) .0019(8) .0041(8) .0006(8) N21 .0186(8) .0168(8) .0206(8) -.0021(6) .0051(6) -.0013(6) C22 .0198(9) .0140(9) .0206(9) -.0024(7) .0052(7) .0023(7) N23 .0177(8) .0184(8) .0183(8) -.0004(6) .0044(6) .0008(7) C24 .0215(10) .0218(10) .0184(9) -.0046(8) .0003(8) -.0028(8) C25 .0177(10) .0227(11) .0215(10) -.0039(8) .0004(8) -.0014(8) C3 .0181(10) .0218(11) .0215(10) -.0013(8) .0020(8) .0021(8) C31 .0175(9) .0204(10) .0221(10) .0041(7) .0036(8) .0013(8) C32 .0166(9) .0170(10) .0248(10) .0050(7) .0054(8) .0029(8) C33 .0210(10) .0172(10) .0245(10) .0024(8) .0052(8) -.0004(8) C34 .0261(10) .0253(11) .0202(10) .0039(8) .0074(8) -.0010(8) C35 .0255(11) .0268(11) .0289(11) -.0006(9) .0115(9) .0038(9) C36 .0212(10) .0239(11) .0292(11) -.0025(8) .0063(9) .0008(9) C4 .0236(10) .0208(10) .0193(10) -.0007(8) .0054(8) -.0022(8) N41 .0188(8) .0188(8) .0181(8) -.0039(6) .0012(6) .0003(6) C42 .0185(9) .0182(10) .0153(9) -.0027(7) .0004(7) -.0013(7) N43 .0209(8) .0176(8) .0183(8) -.0020(6) .0023(6) .0007(7) C44 .0268(11) .0162(10) .0227(10) -.0042(8) .0014(8) .0030(8) C45 .0252(10) .0203(11) .0228(10) -.0070(8) .0031(8) .0033(8) O1 .0408(9) .0213(8) .0418(9) .0021(7) .0078(8) -.0052(7) S .0247(3) .0277(3) .0225(2) -.0028(2) .0009(2) .0007(2) C01 .0427(15) .0356(15) .0343(13) -.0082(12) .0058(12) .0081(11) C02 .0387(14) .0445(17) .0299(12) .0080(12) .0107(11) -.0024(11) # 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 Ni Cl1 . . 2.2285(6) ? Ni Cl2 . . 2.2208(5) ? Ni C22 . . 1.8623(17) ? Ni C42 . . 1.863(2) ? C1 C11 . . 1.516(3) ? C1 N21 . . 1.470(3) ? C1 H1a . . .96(2) ? C1 H1b . . .93(2) ? C11 C12 . . 1.408(3) ? C11 C16 . . 1.396(3) ? C12 C13 . . 1.390(3) ? C12 C4 . . 1.517(2) ? C13 C14 . . 1.392(3) ? C13 H13 . . .87(2) ? C14 C15 . . 1.375(3) ? C14 H14 . . .95(2) ? C15 C16 . . 1.388(3) ? C15 H15 . . .94(2) ? C16 H16 . . .88(2) ? C2 N23 . . 1.473(3) ? C2 C32 . . 1.511(3) ? C2 H2a . . .972(18) ? C2 H2b . . .98(2) ? N21 C22 . . 1.358(2) ? N21 C25 . . 1.391(2) ? C22 N23 . . 1.351(3) ? N23 C24 . . 1.389(2) ? C24 C25 . . 1.341(3) ? C24 H24 . . .90(2) ? C25 H25 . . .90(2) ? C3 C31 . . 1.513(3) ? C3 N41 . . 1.473(3) ? C3 H3a . . .92(2) ? C3 H3b . . .89(2) ? C31 C32 . . 1.407(3) ? C31 C36 . . 1.391(3) ? C32 C33 . . 1.401(3) ? C33 C34 . . 1.385(3) ? C33 H33 . . .915(19) ? C34 C35 . . 1.385(3) ? C34 H34 . . .92(2) ? C35 C36 . . 1.382(3) ? C35 H35 . . .92(2) ? C36 H36 . . .92(2) ? C4 N43 . . 1.473(3) ? C4 H4a . . .98(2) ? C4 H4b . . .97(2) ? N41 C42 . . 1.353(3) ? N41 C45 . . 1.393(3) ? C42 N43 . . 1.350(3) ? N43 C44 . . 1.392(3) ? C44 C45 . . 1.338(3) ? C44 H44 . . .91(2) ? C45 H45 . . .94(2) ? O1 S . . 1.5004(16) ? S C01 . . 1.787(3) ? S C02 . . 1.785(3) ? C01 H01a . . .98(3) ? C01 H01b . . .97(3) ? C01 H01c . . .96(3) ? C02 H02a . . .98(3) ? C02 H02b . . .92(3) ? C02 H02c . . .98(2) ? 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 Cl1 Ni Cl2 . . . 94.94(2) ? Cl1 Ni C22 . . . 90.35(6) ? Cl1 Ni C42 . . . 177.82(5) ? Cl2 Ni C22 . . . 174.48(7) ? Cl2 Ni C42 . . . 87.22(5) ? C22 Ni C42 . . . 87.49(8) ? C11 C1 N21 . . . 111.45(18) ? C11 C1 H1a . . . 113.8(13) ? C11 C1 H1b . . . 111.7(14) ? N21 C1 H1a . . . 106.0(14) ? N21 C1 H1b . . . 107.2(15) ? H1a C1 H1b . . . 106(2) ? C1 C11 C12 . . . 122.91(16) ? C1 C11 C16 . . . 117.97(17) ? C12 C11 C16 . . . 119.11(18) ? C11 C12 C13 . . . 118.90(17) ? C11 C12 C4 . . . 123.27(18) ? C13 C12 C4 . . . 117.84(17) ? C12 C13 C14 . . . 121.2(2) ? C12 C13 H13 . . . 120.4(15) ? C14 C13 H13 . . . 118.4(15) ? C13 C14 C15 . . . 119.9(2) ? C13 C14 H14 . . . 118.1(13) ? C15 C14 H14 . . . 122.0(13) ? C14 C15 C16 . . . 119.8(2) ? C14 C15 H15 . . . 121.2(15) ? C16 C15 H15 . . . 119.0(15) ? C11 C16 C15 . . . 121.1(2) ? C11 C16 H16 . . . 117.8(13) ? C15 C16 H16 . . . 121.1(13) ? N23 C2 C32 . . . 111.36(16) ? N23 C2 H2a . . . 107.2(13) ? N23 C2 H2b . . . 107.6(14) ? C32 C2 H2a . . . 111.5(12) ? C32 C2 H2b . . . 109.9(15) ? H2a C2 H2b . . . 109.2(17) ? C1 N21 C22 . . . 124.62(15) ? C1 N21 C25 . . . 124.70(16) ? C22 N21 C25 . . . 110.68(17) ? Ni C22 N21 . . . 128.49(15) ? Ni C22 N23 . . . 126.73(14) ? N21 C22 N23 . . . 104.76(15) ? C2 N23 C22 . . . 124.66(14) ? C2 N23 C24 . . . 124.23(16) ? C22 N23 C24 . . . 110.92(16) ? N23 C24 C25 . . . 106.85(17) ? N23 C24 H24 . . . 122.0(13) ? C25 C24 H24 . . . 131.1(13) ? N21 C25 C24 . . . 106.77(16) ? N21 C25 H25 . . . 120.1(15) ? C24 C25 H25 . . . 133.1(15) ? C31 C3 N41 . . . 112.20(15) ? C31 C3 H3a . . . 114.2(13) ? C31 C3 H3b . . . 111.5(14) ? N41 C3 H3a . . . 106.7(14) ? N41 C3 H3b . . . 106.3(14) ? H3a C3 H3b . . . 105.4(18) ? C3 C31 C32 . . . 123.19(19) ? C3 C31 C36 . . . 118.04(17) ? C32 C31 C36 . . . 118.76(18) ? C2 C32 C31 . . . 123.68(18) ? C2 C32 C33 . . . 117.55(17) ? C31 C32 C33 . . . 118.77(19) ? C32 C33 C34 . . . 121.40(18) ? C32 C33 H33 . . . 119.6(12) ? C34 C33 H33 . . . 119.0(12) ? C33 C34 C35 . . . 119.6(2) ? C33 C34 H34 . . . 118.6(14) ? C35 C34 H34 . . . 121.7(14) ? C34 C35 C36 . . . 119.5(2) ? C34 C35 H35 . . . 121.2(13) ? C36 C35 H35 . . . 119.3(13) ? C31 C36 C35 . . . 121.9(2) ? C31 C36 H36 . . . 116.2(14) ? C35 C36 H36 . . . 121.9(15) ? C12 C4 N43 . . . 112.01(16) ? C12 C4 H4a . . . 109.0(12) ? C12 C4 H4b . . . 112.3(12) ? N43 C4 H4a . . . 108.6(13) ? N43 C4 H4b . . . 106.0(14) ? H4a C4 H4b . . . 108.9(19) ? C3 N41 C42 . . . 124.54(17) ? C3 N41 C45 . . . 125.22(18) ? C42 N41 C45 . . . 110.23(17) ? Ni C42 N41 . . . 126.57(15) ? Ni C42 N43 . . . 127.90(16) ? N41 C42 N43 . . . 105.32(17) ? C4 N43 C42 . . . 125.10(17) ? C4 N43 C44 . . . 124.34(17) ? C42 N43 C44 . . . 110.56(17) ? N43 C44 C45 . . . 106.81(18) ? N43 C44 H44 . . . 119.1(15) ? C45 C44 H44 . . . 134.0(15) ? N41 C45 C44 . . . 107.0(2) ? N41 C45 H45 . . . 122.1(14) ? C44 C45 H45 . . . 130.9(14) ? O1 S C01 . . . 106.58(12) ? O1 S C02 . . . 105.51(11) ? C01 S C02 . . . 98.21(14) ? S C01 H01a . . . 109(2) ? S C01 H01b . . . 111.5(16) ? S C01 H01c . . . 105.8(19) ? H01a C01 H01b . . . 108(2) ? H01a C01 H01c . . . 112(3) ? H01b C01 H01c . . . 111(2) ? S C02 H02a . . . 109.7(19) ? S C02 H02b . . . 107(2) ? S C02 H02c . . . 111.8(16) ? H02a C02 H02b . . . 111(3) ? H02a C02 H02c . . . 110(2) ? H02b C02 H02c . . . 108(2) ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- 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 Ni C1 3.362(2) . . ? Ni C2 3.315(2) . . ? Ni N21 2.9086(14) . . ? Ni N23 2.8814(15) . . ? Ni C3 3.313(2) . . ? Ni C4 3.355(2) . . ? Ni N41 2.8823(17) . . ? Ni N43 2.8954(17) . . ? Ni H1a 2.83(2) . . ? Ni H2a 2.79(2) . . ? Ni H3a 2.81(2) . . ? Ni H4b 2.82(2) . . ? Cl1 C22 2.913(2) . . ? Cl1 H13 2.76(2) . '1 565' ? Cl2 C42 2.8288(18) . . ? C1 C12 2.569(3) . . ? C1 C16 2.496(3) . . ? C1 C22 2.504(3) . . ? C1 C25 2.534(3) . . ? C1 H16 2.58(2) . . ? C11 C13 2.410(3) . . ? C11 C14 2.792(3) . . ? C11 C15 2.424(3) . . ? C11 N21 2.467(3) . . ? C11 C4 2.574(3) . . ? C11 H1a 2.09(2) . . ? C11 H1b 2.05(2) . . ? C11 H16 1.97(2) . . ? C12 C14 2.424(3) . . ? C12 C15 2.798(3) . . ? C12 C16 2.417(3) . . ? C12 N43 2.479(2) . . ? C12 H13 1.98(2) . . ? C12 H4a 2.06(2) . . ? C12 H4b 2.09(2) . . ? C13 C15 2.396(3) . . ? C13 C16 2.759(3) . . ? C13 C4 2.491(3) . . ? C13 H14 2.02(2) . . ? C13 H4a 2.58(2) . . ? C14 C16 2.390(3) . . ? C14 H13 1.96(2) . . ? C14 H15 2.03(2) . . ? C15 H14 2.05(2) . . ? C15 H16 1.99(2) . . ? C16 H1b 2.60(2) . . ? C16 H15 2.02(2) . . ? C2 C22 2.502(3) . . ? C2 C24 2.530(3) . . ? C2 C31 2.573(3) . . ? C2 C33 2.491(3) . . ? C2 H33 2.609(19) . . ? N21 N23 2.146(2) . . ? N21 C24 2.193(3) . . ? N21 H1a 1.96(2) . . ? N21 H1b 1.96(3) . . ? N21 H25 2.00(2) . . ? C22 C24 2.257(3) . . ? C22 C25 2.261(2) . . ? C22 C42 2.576(3) . . ? C22 H1a 2.53(2) . . ? C22 H2a 2.56(2) . . ? N23 C25 2.193(2) . . ? N23 C32 2.465(3) . . ? N23 H2a 1.991(19) . . ? N23 H2b 2.00(2) . . ? N23 H24 2.018(19) . . ? C24 H25 2.06(2) . . ? C25 H1b 2.69(2) . . ? C25 H24 2.05(2) . . ? C3 C32 2.569(3) . . ? C3 C36 2.490(3) . . ? C3 C42 2.502(3) . . ? C3 C45 2.545(3) . . ? C3 H36 2.56(2) . . ? C31 C33 2.416(3) . . ? C31 C34 2.799(3) . . ? C31 C35 2.424(3) . . ? C31 N41 2.478(3) . . ? C31 H3a 2.07(2) . . ? C31 H3b 2.02(2) . . ? C31 H36 1.97(2) . . ? C32 C34 2.429(3) . . ? C32 C35 2.800(3) . . ? C32 C36 2.408(3) . . ? C32 H2a 2.08(2) . . ? C32 H2b 2.06(2) . . ? C32 H33 2.016(18) . . ? C33 C35 2.394(3) . . ? C33 C36 2.750(3) . . ? C33 H2b 2.58(2) . . ? C33 H34 1.99(2) . . ? C34 C36 2.390(3) . . ? C34 H33 2.00(2) . . ? C34 H35 2.02(2) . . ? C35 S 3.738(2) . 2 ? C35 H34 2.02(2) . . ? C35 H36 2.02(2) . . ? C36 H3b 2.58(2) . . ? C36 H35 2.00(2) . . ? C4 C42 2.506(3) . . ? C4 C44 2.534(3) . . ? C4 H13 2.61(2) . . ? C4 H44 2.70(2) . . ? N41 N43 2.149(2) . . ? N41 C44 2.196(3) . . ? N41 H3a 1.95(2) . . ? N41 H3b 1.92(2) . . ? N41 H45 2.05(2) . . ? C42 C44 2.254(3) . . ? C42 C45 2.253(3) . . ? C42 H3a 2.55(2) . . ? C42 H4b 2.55(2) . . ? N43 C45 2.192(3) . . ? N43 H4a 2.02(2) . . ? N43 H4b 1.98(2) . . ? N43 H44 2.00(2) . . ? C44 S 3.921(2) . . ? C44 H4a 2.69(2) . . ? C44 H45 2.08(2) . . ? C45 S 3.760(2) . . ? C45 H3b 2.65(2) . . ? C45 H44 2.08(2) . . ? O1 C01 2.641(3) . . ? O1 C02 2.621(3) . . ? O1 H24 2.60(2) . '1 545' ? O1 H25 2.47(2) . '2 645' ? O1 H33 2.63(2) . '1 545' ? S H2b 3.06(2) . '1 545' ? S H25 3.28(2) . '2 645' ? S H33 3.34(2) . '1 545' ? S H35 3.45(2) . '2 545' ? S H45 3.68(2) . . ? S H01a 2.30(3) . . ? S H01b 2.32(3) . . ? S H01c 2.25(3) . . ? S H02a 2.31(3) . . ? S H02b 2.23(3) . . ? S H02c 2.33(2) . . ? C01 C02 2.700(4) . . ? H1a H1b 1.51(3) . . ? H1a H4b 2.16(3) . . ? H13 H14 2.26(3) . . ? H13 H4a 2.39(3) . . ? H14 H15 2.37(3) . . ? H15 H16 2.30(3) . . ? H2a H2b 1.59(3) . . ? H2a H3a 2.20(3) . . ? H2b H33 2.39(3) . . ? H3a H3b 1.45(3) . . ? H3b H36 2.36(3) . . ? H33 H34 2.27(3) . . ? H34 H35 2.34(3) . . ? H35 H36 2.32(3) . . ? H4a H4b 1.59(3) . . ? H01a H01b 1.57(4) . . ? H01a H01c 1.60(5) . . ? H01b H01c 1.59(4) . . ? H02a H02b 1.57(5) . . ? H02a H02c 1.60(4) . . ? H02b H02c 1.53(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 1136 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 17 _reflns_limit_k_min 0 _reflns_limit_k_max 11 _reflns_limit_l_min -29 _reflns_limit_l_max 28 _reflns_number_observed ? _reflns_d_resolution_high .727 _reflns_d_resolution_low 10.716 _diffrn_reflns_av_sigmaI/netI .057 _diffrn_reflns_theta_min 1.9 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 153 _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 .048 _refine_ls_wR_factor_all .039 _refine_ls_goodness_of_fit_all 1.089 _refine_ls_shift/su_mean .001 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end #===END ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_cwi # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C22.5 H22 I2 N4 O.5 Pd1' _chemical_formula_moiety ? _chemical_formula_weight 716.68 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/n_1 _symmetry_space_group_name_Hall -p_2yn loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 10.3800(10) _cell_length_b 8.9810(10) _cell_length_c 25.693(3) _cell_angle_alpha 90.00000 _cell_angle_beta 95.946(2) _cell_angle_gamma 90.00000 _cell_volume 2382.3(4) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.998 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu 3.39 _exptl_crystal_description plate _exptl_crystal_size_max .4 _exptl_crystal_size_mid .38 _exptl_crystal_size_min .08 _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 .502 _exptl_absorpt_correction_T_max .802 _diffrn_reflns_number 26807 _reflns_number_total 5935 _reflns_Friedel_coverage 0 _reflns_number_gt 5744 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.01 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .042 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 34 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? #<< do not append units _diffrn_standards_decay_% 0 #<< do not append % _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .031 _refine_ls_wR_factor_ref .044 _refine_ls_goodness_of_fit_ref 1.259 _refine_ls_number_reflns 5744 _refine_ls_number_parameters 278 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .043 _refine_diff_density_min -1.056 _refine_diff_density_max 1.496 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef 1001(142) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 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 90 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 88 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' I ? 0 8 -.726 1.812 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 16 .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' Pd ? 0 4 -1.177 1.007 '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 Pd .65622(2) .18054(3) .138078(10) .01698(13) Uani ? ? 1.00000 ? ? I1 .69474(3) -.07205(3) .089636(10) .02767(13) Uani ? ? 1.00000 ? ? I2 .89926(2) .27507(3) .144223(9) .02384(13) Uani ? ? 1.00000 ? ? C1 .3942(4) .2441(5) .05068(15) .0254(17) Uani ? ? 1.00000 ? ? C11 .3496(4) .4034(5) .04204(14) .0254(17) Uani ? ? 1.00000 ? ? C12 .4292(4) .5265(4) .05758(14) .0226(16) Uani ? ? 1.00000 ? ? C13 .3843(4) .6700(5) .04446(15) .0279(18) Uani ? ? 1.00000 ? ? C14 .2624(4) .6930(6) .01729(18) .034(2) Uani ? ? 1.00000 ? ? C15 .1838(4) .5726(6) .00333(16) .034(2) Uani ? ? 1.00000 ? ? C16 .2277(4) .4294(5) .01561(16) .031(2) Uani ? ? 1.00000 ? ? C2 .4733(4) .0237(4) .22697(15) .0275(18) Uani ? ? 1.00000 ? ? N21 .3731(3) .1845(4) .10213(12) .0219(14) Uani ? ? 1.00000 ? ? C22 .4686(4) .1384(4) .13820(14) .0212(15) Uani ? ? 1.00000 ? ? N23 .4079(3) .0854(4) .17825(13) .0238(14) Uani ? ? 1.00000 ? ? C24 .2737(4) .0992(5) .16699(17) .032(2) Uani ? ? 1.00000 ? ? C25 .2523(4) .1608(6) .11971(18) .035(2) Uani ? ? 1.00000 ? ? C3 .6289(4) .2998(5) .26435(14) .0256(17) Uani ? ? 1.00000 ? ? C31 .5139(4) .2422(4) .29033(14) .0236(16) Uani ? ? 1.00000 ? ? C32 .4451(4) .1119(4) .27442(14) .0235(16) Uani ? ? 1.00000 ? ? C33 .3480(4) .0618(5) .30347(16) .0272(18) Uani ? ? 1.00000 ? ? C34 .3172(4) .1369(6) .34760(17) .033(2) Uani ? ? 1.00000 ? ? C35 .3833(4) .2660(5) .36316(17) .032(2) Uani ? ? 1.00000 ? ? C36 .4813(4) .3177(5) .33464(16) .0285(18) Uani ? ? 1.00000 ? ? C4 .5650(3) .5109(4) .08510(14) .0211(15) Uani ? ? 1.00000 ? ? N41 .5945(3) .4023(4) .22012(12) .0209(14) Uani ? ? 1.00000 ? ? C42 .6060(3) .3712(4) .16934(13) .0181(14) Uani ? ? 1.00000 ? ? N43 .5663(3) .4940(3) .14250(12) .0196(13) Uani ? ? 1.00000 ? ? C44 .5330(4) .6051(4) .17634(15) .0256(17) Uani ? ? 1.00000 ? ? C45 .5505(4) .5472(4) .22508(15) .0252(17) Uani ? ? 1.00000 ? ? O0 1.0071(8) .0862(12) .0312(3) .060(5) Uani ? ? .50000 ? ? C0 1.00000 .00000 .00000 .098(9) Uani ? ? 1.00000 ? ? H1a .34939 .18319 .02416 .03100 Uiso ? ? 1.00000 ? ? H1b .48497 .23973 .04677 .03100 Uiso ? ? 1.00000 ? ? H13 .43799 .75465 .05457 .03500 Uiso ? ? 1.00000 ? ? H14 .23316 .79206 .00779 .04200 Uiso ? ? 1.00000 ? ? H15 .09864 .58712 -.01460 .04200 Uiso ? ? 1.00000 ? ? H16 .17215 .34589 .00556 .03900 Uiso ? ? 1.00000 ? ? H2a .56440 .02365 .22516 .03300 Uiso ? ? 1.00000 ? ? H2b .44495 -.07636 .23112 .03300 Uiso ? ? 1.00000 ? ? H24 .20977 .07003 .18959 .03800 Uiso ? ? 1.00000 ? ? H25 .16959 .18399 .10119 .04100 Uiso ? ? 1.00000 ? ? H3a .68561 .35090 .28998 .03200 Uiso ? ? 1.00000 ? ? H3b .67395 .21680 .25173 .03200 Uiso ? ? 1.00000 ? ? H33 .30022 -.02584 .29197 .03400 Uiso ? ? 1.00000 ? ? H34 .25132 .09826 .36718 .04000 Uiso ? ? 1.00000 ? ? H35 .36136 .32013 .39332 .03900 Uiso ? ? 1.00000 ? ? H36 .52700 .40652 .34533 .03600 Uiso ? ? 1.00000 ? ? H4a .60499 .42501 .07139 .02500 Uiso ? ? 1.00000 ? ? H4b .61441 .59655 .07783 .02500 Uiso ? ? 1.00000 ? ? H44 .50338 .70288 .16694 .03100 Uiso ? ? 1.00000 ? ? H45 .53570 .59703 .25702 .03000 Uiso ? ? 1.00000 ? ? H0a 1.01260 -.09510 .01591 .07800 Uiso ? ? .50000 ? ? H0b 1.06609 .01771 -.02221 .07800 Uiso ? ? .50000 ? ? H0c .91750 .00621 -.01968 .07800 Uiso ? ? .50000 ? ? 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 Pd .01656(13) .01882(14) .01596(13) -.00005(9) .00360(9) -.00113(9) I1 .03112(15) .02311(13) .02844(14) .00173(9) .00149(10) -.00812(9) I2 .01750(12) .02835(14) .02565(13) -.00218(8) .00214(9) .00399(9) C1 .0262(18) .030(2) .0192(17) -.0050(15) -.0002(14) -.0025(14) C11 .0263(18) .034(2) .0168(16) .0026(15) .0047(14) -.0002(14) C12 .0228(17) .0288(18) .0169(15) .0025(14) .0056(13) .0021(14) C13 .031(2) .033(2) .0200(17) .0034(16) .0074(15) .0049(15) C14 .027(2) .045(2) .031(2) .0115(17) .0099(16) .0107(18) C15 .025(2) .056(3) .0232(18) .0054(18) .0041(15) .0093(18) C16 .026(2) .048(3) .0205(18) -.0018(17) .0022(15) .0003(16) C2 .037(2) .0220(17) .0244(18) -.0010(15) .0080(16) .0015(14) N21 .0194(14) .0282(16) .0185(14) -.0049(12) .0040(11) -.0017(12) C22 .0237(17) .0214(16) .0190(16) -.0033(13) .0051(13) -.0061(13) N23 .0244(15) .0246(15) .0231(15) -.0065(12) .0058(12) -.0030(12) C24 .0209(18) .045(2) .031(2) -.0107(17) .0080(15) -.0029(18) C25 .0193(18) .048(3) .038(2) -.0106(17) .0057(16) -.004(2) C3 .0244(18) .036(2) .0163(16) .0003(15) .0003(13) -.0006(14) C31 .0230(17) .0298(19) .0183(16) .0050(14) .0030(13) .0038(14) C32 .0245(17) .0276(18) .0187(16) .0054(14) .0043(13) .0038(14) C33 .0255(18) .030(2) .0272(19) -.0009(15) .0075(15) .0050(15) C34 .029(2) .044(2) .029(2) -.0007(18) .0130(16) .0071(18) C35 .035(2) .037(2) .026(2) .0053(17) .0134(16) -.0008(16) C36 .031(2) .033(2) .0224(18) .0000(16) .0047(15) -.0009(15) C4 .0147(15) .0253(17) .0233(17) -.0001(12) .0027(12) .0024(13) N41 .0201(14) .0241(15) .0192(14) -.0017(11) .0047(11) -.0021(11) C42 .0158(14) .0214(16) .0178(15) -.0012(12) .0044(12) -.0015(12) N43 .0207(14) .0193(14) .0190(14) .0004(11) .0031(11) -.0031(11) C44 .032(2) .0194(17) .0261(18) -.0003(14) .0073(15) -.0068(14) C45 .0287(19) .0256(18) .0216(17) -.0005(14) .0047(14) -.0065(14) O0 .045(4) .089(7) .048(5) -.010(4) .008(4) -.014(5) C0 .111(10) .125(11) .064(7) .088(9) .040(7) .032(7) # 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 Pd I1 . . 2.6378(4) ? Pd I2 . . 2.6510(4) ? Pd C22 . . 1.984(4) ? Pd C42 . . 1.984(4) ? C1 C11 . . 1.512(6) ? C1 N21 . . 1.464(5) ? C1 H1a . . .956(4) ? C1 H1b . . .959(4) ? C11 C12 . . 1.413(6) ? C11 C16 . . 1.393(6) ? C12 C13 . . 1.400(6) ? C12 C4 . . 1.516(5) ? C13 C14 . . 1.395(6) ? C13 H13 . . .962(4) ? C14 C15 . . 1.380(7) ? C14 H14 . . .964(5) ? C15 C16 . . 1.390(7) ? C15 H15 . . .962(4) ? C16 H16 . . .965(5) ? C2 N23 . . 1.469(5) ? C2 C32 . . 1.508(6) ? C2 H2a . . .952(4) ? C2 H2b . . .955(4) ? N21 C22 . . 1.350(5) ? N21 C25 . . 1.392(5) ? C22 N23 . . 1.348(5) ? N23 C24 . . 1.398(5) ? C24 C25 . . 1.332(6) ? C24 H24 . . .962(4) ? C25 H25 . . .960(4) ? C3 C31 . . 1.518(6) ? C3 N41 . . 1.477(5) ? C3 H3a . . .954(4) ? C3 H3b . . .954(4) ? C31 C32 . . 1.409(5) ? C31 C36 . . 1.397(6) ? C32 C33 . . 1.390(6) ? C33 C34 . . 1.385(6) ? C33 H33 . . .961(4) ? C34 C35 . . 1.384(7) ? C34 H34 . . .955(5) ? C35 C36 . . 1.394(6) ? C35 H35 . . .962(4) ? C36 H36 . . .954(4) ? C4 N43 . . 1.481(5) ? C4 H4a . . .960(4) ? C4 H4b . . .954(4) ? N41 C42 . . 1.352(5) ? N41 C45 . . 1.390(5) ? C42 N43 . . 1.343(5) ? N43 C44 . . 1.390(5) ? C44 C45 . . 1.351(5) ? C44 H44 . . .953(4) ? C45 H45 . . .961(4) ? O0 C0 . . 1.112(10) ? O0 H0a . '3 755' 1.210(9) ? O0 H0b . '3 755' 1.210(10) ? O0 H0c . '3 755' 1.199(10) ? C0 H0a . . .95005(9) ? C0 H0b . . .95008(7) ? C0 H0c . . .94995(7) ? C0 H0a . '3 755' .95005(9) ? C0 H0b . '3 755' .95008(7) ? C0 H0c . '3 755' .94995(7) ? 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 I1 Pd I2 . . . 96.528(12) ? I1 Pd C22 . . . 91.91(11) ? I1 Pd C42 . . . 172.91(9) ? I2 Pd C22 . . . 171.54(11) ? I2 Pd C42 . . . 89.30(10) ? C22 Pd C42 . . . 82.24(14) ? C11 C1 N21 . . . 114.0(3) ? C11 C1 H1a . . . 108.6(3) ? C11 C1 H1b . . . 108.2(4) ? N21 C1 H1a . . . 109.1(4) ? N21 C1 H1b . . . 108.7(3) ? H1a C1 H1b . . . 108.2(4) ? C1 C11 C12 . . . 122.5(3) ? C1 C11 C16 . . . 118.6(4) ? C12 C11 C16 . . . 118.8(4) ? C11 C12 C13 . . . 118.8(3) ? C11 C12 C4 . . . 123.2(3) ? C13 C12 C4 . . . 117.9(3) ? C12 C13 C14 . . . 121.2(4) ? C12 C13 H13 . . . 119.6(4) ? C14 C13 H13 . . . 119.2(4) ? C13 C14 C15 . . . 119.7(4) ? C13 C14 H14 . . . 120.6(4) ? C15 C14 H14 . . . 119.7(4) ? C14 C15 C16 . . . 119.6(4) ? C14 C15 H15 . . . 120.5(5) ? C16 C15 H15 . . . 119.9(5) ? C11 C16 C15 . . . 121.8(4) ? C11 C16 H16 . . . 119.2(4) ? C15 C16 H16 . . . 119.0(4) ? N23 C2 C32 . . . 112.3(3) ? N23 C2 H2a . . . 109.4(4) ? N23 C2 H2b . . . 109.2(3) ? C32 C2 H2a . . . 108.5(3) ? C32 C2 H2b . . . 108.5(4) ? H2a C2 H2b . . . 108.9(4) ? C1 N21 C22 . . . 124.3(3) ? C1 N21 C25 . . . 125.0(3) ? C22 N21 C25 . . . 110.6(3) ? Pd C22 N21 . . . 126.3(3) ? Pd C22 N23 . . . 127.2(3) ? N21 C22 N23 . . . 105.3(3) ? C2 N23 C22 . . . 124.9(3) ? C2 N23 C24 . . . 124.9(3) ? C22 N23 C24 . . . 110.2(3) ? N23 C24 C25 . . . 107.1(4) ? N23 C24 H24 . . . 125.8(4) ? C25 C24 H24 . . . 127.1(4) ? N21 C25 C24 . . . 106.8(4) ? N21 C25 H25 . . . 126.5(5) ? C24 C25 H25 . . . 126.8(5) ? C31 C3 N41 . . . 114.3(3) ? C31 C3 H3a . . . 108.5(3) ? C31 C3 H3b . . . 108.5(4) ? N41 C3 H3a . . . 108.3(4) ? N41 C3 H3b . . . 108.3(3) ? H3a C3 H3b . . . 108.8(4) ? C3 C31 C32 . . . 123.6(3) ? C3 C31 C36 . . . 117.5(3) ? C32 C31 C36 . . . 118.8(4) ? C2 C32 C31 . . . 122.4(4) ? C2 C32 C33 . . . 118.4(4) ? C31 C32 C33 . . . 119.2(4) ? C32 C33 C34 . . . 121.6(4) ? C32 C33 H33 . . . 118.7(4) ? C34 C33 H33 . . . 119.7(4) ? C33 C34 C35 . . . 119.7(4) ? C33 C34 H34 . . . 119.5(5) ? C35 C34 H34 . . . 120.8(5) ? C34 C35 C36 . . . 119.6(4) ? C34 C35 H35 . . . 120.3(5) ? C36 C35 H35 . . . 120.1(4) ? C31 C36 C35 . . . 121.2(4) ? C31 C36 H36 . . . 119.0(4) ? C35 C36 H36 . . . 119.8(4) ? C12 C4 N43 . . . 112.7(3) ? C12 C4 H4a . . . 108.6(3) ? C12 C4 H4b . . . 109.1(3) ? N43 C4 H4a . . . 108.9(3) ? N43 C4 H4b . . . 109.2(3) ? H4a C4 H4b . . . 108.3(4) ? C3 N41 C42 . . . 125.1(3) ? C3 N41 C45 . . . 124.7(3) ? C42 N41 C45 . . . 110.2(3) ? Pd C42 N41 . . . 128.5(3) ? Pd C42 N43 . . . 125.5(3) ? N41 C42 N43 . . . 105.8(3) ? C4 N43 C42 . . . 124.5(3) ? C4 N43 C44 . . . 124.9(3) ? C42 N43 C44 . . . 110.6(3) ? N43 C44 C45 . . . 106.6(3) ? N43 C44 H44 . . . 126.7(4) ? C45 C44 H44 . . . 126.8(4) ? N41 C45 C44 . . . 106.8(3) ? N41 C45 H45 . . . 126.7(4) ? C44 C45 H45 . . . 126.5(4) ? C0 O0 H0a . . '3 755' 48.1(4) ? C0 O0 H0b . . '3 755' 48.1(4) ? C0 O0 H0c . . '3 755' 48.4(4) ? H0a O0 H0b '3 755' . '3 755' 79.7(5) ? H0a O0 H0c '3 755' . '3 755' 81.1(6) ? H0b O0 H0c '3 755' . '3 755' 80.3(7) ? O0 C0 H0a . . . 108.6(5) ? O0 C0 H0b . . . 108.6(5) ? O0 C0 H0c . . . 109.4(4) ? O0 C0 O0 . . '3 755' 180.0000 ? O0 C0 H0a . . '3 755' 71.4(5) ? O0 C0 H0b . . '3 755' 71.4(5) ? O0 C0 H0c . . '3 755' 70.6(4) ? H0a C0 H0b . . . 109.460(3) ? H0a C0 H0c . . . 110.985(3) ? H0a C0 O0 . . '3 755' 71.4(5) ? H0a C0 H0a . . '3 755' 180.0000 ? H0a C0 H0b . . '3 755' 70.540(3) ? H0a C0 H0c . . '3 755' 69.015(3) ? H0b C0 H0c . . . 109.734(8) ? H0b C0 O0 . . '3 755' 71.4(5) ? H0b C0 H0a . . '3 755' 70.540(3) ? H0b C0 H0b . . '3 755' 180.0000 ? H0b C0 H0c . . '3 755' 70.266(8) ? H0c C0 O0 . . '3 755' 70.6(5) ? H0c C0 H0a . . '3 755' 69.015(2) ? H0c C0 H0b . . '3 755' 70.266(8) ? H0c C0 H0c . . '3 755' 180.0000 ? O0 C0 H0a '3 755' . '3 755' 108.6(5) ? O0 C0 H0b '3 755' . '3 755' 108.6(5) ? O0 C0 H0c '3 755' . '3 755' 109.4(5) ? H0a C0 H0b '3 755' . '3 755' 109.460(3) ? H0a C0 H0c '3 755' . '3 755' 110.985(3) ? H0b C0 H0c '3 755' . '3 755' 109.734(8) ? C0 H0a O0 . . '3 755' 60.5(5) ? C0 H0b O0 . . '3 755' 60.5(4) ? C0 H0c O0 . . '3 755' 61.0(4) ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- 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 Pd C1 3.392(4) . . ? Pd C2 3.421(4) . . ? Pd N21 2.989(3) . . ? Pd N23 2.999(3) . . ? Pd C3 3.456(4) . . ? Pd C4 3.359(4) . . ? Pd N41 3.016(3) . . ? Pd N43 2.972(3) . . ? Pd H1b 2.8429(3) . . ? Pd H2a 2.8882(3) . . ? Pd H3b 2.9249(4) . . ? Pd H4a 2.8018(3) . . ? C1 C12 2.566(6) . . ? C1 C16 2.498(6) . . ? C1 C22 2.489(5) . . ? C1 C25 2.533(6) . . ? C1 H16 2.634(4) . . ? C11 C13 2.422(6) . . ? C11 C14 2.805(6) . . ? C11 C15 2.431(6) . . ? C11 N21 2.496(5) . . ? C11 C4 2.577(5) . . ? C11 H1a 2.030(4) . . ? C11 H1b 2.028(4) . . ? C11 H16 2.045(4) . . ? C11 H4a 2.687(4) . . ? C12 C14 2.436(6) . . ? C12 C15 2.806(5) . . ? C12 C16 2.415(5) . . ? C12 N43 2.495(4) . . ? C12 H1b 2.661(4) . . ? C12 H13 2.053(4) . . ? C12 H4a 2.037(4) . . ? C12 H4b 2.038(4) . . ? C13 C15 2.400(6) . . ? C13 C16 2.759(6) . . ? C13 C4 2.499(5) . . ? C13 H14 2.060(4) . . ? C13 H4b 2.540(4) . . ? C14 C16 2.394(7) . . ? C14 H13 2.045(4) . . ? C14 H15 2.044(4) . . ? C15 H14 2.037(5) . . ? C15 H16 2.041(5) . . ? C16 H1a 2.544(5) . . ? C16 H15 2.047(4) . . ? C2 C22 2.498(5) . . ? C2 C24 2.542(6) . . ? C2 C31 2.556(6) . . ? C2 C33 2.490(6) . . ? C2 H33 2.614(4) . . ? N21 N23 2.145(4) . . ? N21 C24 2.187(6) . . ? N21 H1a 1.993(3) . . ? N21 H1b 1.990(3) . . ? N21 H25 2.110(3) . . ? C22 C24 2.252(6) . . ? C22 C25 2.255(5) . . ? C22 C42 2.610(5) . . ? C22 H1b 2.541(4) . . ? C22 H2a 2.566(3) . . ? N23 C25 2.197(5) . . ? N23 C32 2.473(5) . . ? N23 H2a 1.999(3) . . ? N23 H2b 1.999(3) . . ? N23 H24 2.111(3) . . ? C24 H25 2.056(4) . . ? C25 H24 2.061(5) . . ? C3 C32 2.581(6) . . ? C3 C36 2.492(6) . . ? C3 C42 2.511(5) . . ? C3 C45 2.539(6) . . ? C3 H36 2.612(4) . . ? C31 C33 2.413(6) . . ? C31 C34 2.802(6) . . ? C31 C35 2.431(6) . . ? C31 N41 2.517(5) . . ? C31 H2a 2.667(4) . . ? C31 H3a 2.033(4) . . ? C31 H3b 2.034(4) . . ? C31 H36 2.038(4) . . ? C32 C34 2.422(6) . . ? C32 C35 2.798(6) . . ? C32 C36 2.415(6) . . ? C32 H2a 2.022(4) . . ? C32 H2b 2.024(4) . . ? C32 H3b 2.675(4) . . ? C32 H33 2.034(4) . . ? C33 C35 2.394(6) . . ? C33 C36 2.758(6) . . ? C33 H2b 2.529(4) . . ? C33 H34 2.033(4) . . ? C34 C36 2.401(6) . . ? C34 H33 2.039(5) . . ? C34 H35 2.046(5) . . ? C35 H34 2.046(5) . . ? C35 H36 2.042(5) . . ? C36 H3a 2.532(4) . . ? C36 H35 2.052(4) . . ? C4 C42 2.500(5) . . ? C4 C44 2.546(5) . . ? C4 H13 2.633(4) . . ? N41 N43 2.150(4) . . ? N41 C44 2.200(5) . . ? N41 H3a 1.994(3) . . ? N41 H3b 1.994(3) . . ? N41 H45 2.110(3) . . ? C42 C44 2.247(5) . . ? C42 C45 2.248(5) . . ? C42 H3b 2.567(3) . . ? C42 H4a 2.561(3) . . ? N43 C45 2.197(5) . . ? N43 H4a 2.009(3) . . ? N43 H4b 2.008(3) . . ? N43 H44 2.104(3) . . ? C44 H45 2.071(4) . . ? C45 H44 2.067(4) . . ? O0 O0 2.224(14) . '3 755' ? O0 H25 2.494(9) . '1 655' ? O0 H0a 1.677(11) . . ? O0 H0b 1.677(9) . . ? O0 H0c 1.685(9) . . ? H1a H1b 1.55128(12) . . ? H1a H16 2.35925(17) . . ? H1b H4a 2.13490(16) . . ? H13 H14 2.35553(18) . . ? H13 H4b 2.34520(16) . . ? H14 H15 2.34561(18) . . ? H15 H16 2.3372(2) . . ? H2a H2b 1.55141(11) . . ? H2a H3b 2.14648(17) . . ? H2b H33 2.32242(17) . . ? H3a H3b 1.55122(13) . . ? H3a H36 2.33828(17) . . ? H33 H34 2.3318(2) . . ? H34 H35 2.3595(2) . . ? H35 H36 2.34897(16) . . ? H4a H4b 1.55146(17) . . ? H0a H0a 1.90011(18) . '3 755' ? H0a H0b 1.55134(11) . . ? H0a H0b 1.09720(8) . '3 755' ? H0a H0c 1.56571(10) . . ? H0a H0c 1.07637(8) . '3 755' ? H0b H0b 1.90016(14) . '3 755' ? H0b H0c 1.09342(12) . '3 755' ? H0b H0c 1.55388(15) . . ? H0c H0c 1.89990(15) . '3 755' ? _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 1364 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 14 _reflns_limit_k_min 0 _reflns_limit_k_max 12 _reflns_limit_l_min -34 _reflns_limit_l_max 33 _reflns_number_observed ? _reflns_d_resolution_high .733 _reflns_d_resolution_low 9.917 _diffrn_reflns_av_sigmaI/netI .01 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 153 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression 'Eq22 p292 "Cryst. Comp." Munksgaard 1970' _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .032 _refine_ls_wR_factor_all .045 _refine_ls_goodness_of_fit_all 1.248 _refine_ls_shift/su_mean .002 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end #===END ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_ccw325 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C50 H58 I2 N14 O12 Pd1' _chemical_formula_moiety ? _chemical_formula_weight 1407.33 _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 11.672(2) _cell_length_b 15.279(2) _cell_length_c 16.558(2) _cell_angle_alpha 90.00000 _cell_angle_beta 102.283(2) _cell_angle_gamma 90.00000 _cell_volume 2885.3(7) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.62 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 1.462 _exptl_crystal_description prism _exptl_crystal_size_max .38 _exptl_crystal_size_mid .28 _exptl_crystal_size_min .22 _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 .759 _exptl_absorpt_correction_T_max .862 _diffrn_reflns_number 33318 _reflns_number_total 7270 _reflns_Friedel_coverage 0 _reflns_number_gt 6555 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.1 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .018 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? #<< do not append units _diffrn_standards_decay_% 0 #<< do not append % _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .023 _refine_ls_wR_factor_ref .032 _refine_ls_goodness_of_fit_ref 1.04 _refine_ls_number_reflns 6555 _refine_ls_number_parameters 462 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment mixed _refine_ls_shift/su_max .03 _refine_diff_density_min -.659 _refine_diff_density_max .858 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 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 ? 0 100 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 116 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' I ? 0 4 -.726 1.812 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 28 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 24 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' Pd ? 0 2 -1.177 1.007 '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 Pd 1.00000 .00000 .00000 .01340(8) Uani ? ? 1.00000 ? ? I 1.266381(11) .154919(9) .434942(8) .03023(7) Uani ? ? 1.00000 ? ? C1 1.07658(16) .00031(12) .22009(11) .0203(7) Uani ? ? 1.00000 ? ? C11 .98093(15) -.02934(12) .26355(11) .0198(7) Uani ? ? 1.00000 ? ? C12 .88579(15) -.08106(11) .22515(11) .0194(7) Uani ? ? 1.00000 ? ? C13 .80344(17) -.10793(13) .27007(12) .0238(8) Uani ? ? 1.00000 ? ? C14 .81268(17) -.08344(14) .35187(12) .0267(8) Uani ? ? 1.00000 ? ? C15 .90622(18) -.03166(14) .38957(12) .0271(9) Uani ? ? 1.00000 ? ? C16 .98989(18) -.00523(13) .34630(12) .0244(8) Uani ? ? 1.00000 ? ? C2 .95798(15) .22293(12) -.00073(11) .0197(7) Uani ? ? 1.00000 ? ? N21 1.04789(13) .08282(10) .17467(9) .0181(6) Uani ? ? 1.00000 ? ? C22 1.02099(14) .09299(11) .09123(10) .0166(7) Uani ? ? 1.00000 ? ? N23 .99570(13) .17936(10) .07967(9) .0177(6) Uani ? ? 1.00000 ? ? C24 1.00818(17) .22271(12) .15478(11) .0224(8) Uani ? ? 1.00000 ? ? C25 1.04136(17) .16209(12) .21427(11) .0227(8) Uani ? ? 1.00000 ? ? C3 .74038(16) .11760(12) -.07792(11) .0200(7) Uani ? ? 1.00000 ? ? C31 .73430(16) .21111(12) -.04943(11) .0205(7) Uani ? ? 1.00000 ? ? C32 .83482(15) .25978(12) -.01359(10) .0194(7) Uani ? ? 1.00000 ? ? C33 .82151(18) .34673(12) .00829(12) .0253(8) Uani ? ? 1.00000 ? ? C34 .7118(2) .38571(14) -.00279(14) .0309(9) Uani ? ? 1.00000 ? ? C35 .6129(2) .33798(14) -.03748(14) .0316(10) Uani ? ? 1.00000 ? ? C36 .62462(17) .25144(13) -.06080(13) .0262(8) Uani ? ? 1.00000 ? ? C4 .86627(17) -.10937(12) .13575(11) .0207(7) Uani ? ? 1.00000 ? ? N41 .74302(12) .05417(10) -.01083(9) .0177(6) Uani ? ? 1.00000 ? ? C42 .83270(15) -.00053(11) .02051(10) .0163(7) Uani ? ? 1.00000 ? ? N43 .79549(12) -.04500(10) .08045(9) .0179(6) Uani ? ? 1.00000 ? ? C44 .68386(16) -.01833(13) .08707(12) .0237(8) Uani ? ? 1.00000 ? ? C45 .65093(15) .04379(13) .02938(12) .0235(8) Uani ? ? 1.00000 ? ? C10 .7485(3) .1648(2) .2584(2) .0527(15) Uani ? ? 1.00000 ? ? N10 .79733(19) .25464(14) .25796(13) .0400(10) Uani ? ? 1.00000 ? ? O11 .88619(17) .27127(13) .30796(11) .0476(9) Uani ? ? 1.00000 ? ? O12 .7494(3) .3078(2) .2089(2) .104(2) Uani ? ? 1.00000 ? ? C20 .4655(3) -.0525(2) .36156(18) .0472(14) Uani ? ? 1.00000 ? ? N20 .51882(17) -.04499(15) .28797(13) .0400(10) Uani ? ? 1.00000 ? ? O21 .51411(17) -.10757(14) .24154(12) .0526(10) Uani ? ? 1.00000 ? ? O22 .56966(17) .02298(15) .27932(14) .0567(11) Uani ? ? 1.00000 ? ? C30 .3473(5) .2043(2) .1689(4) .113(3) Uani ? ? 1.00000 ? ? N30 .37306(18) .11270(14) .15366(13) .0406(10) Uani ? ? 1.00000 ? ? O31 .4462(2) .09776(19) .11402(15) .0725(15) Uani ? ? 1.00000 ? ? O32 .31845(16) .05660(13) .18229(13) .0504(10) Uani ? ? 1.00000 ? ? H1a 1.0936(18) -.0418(14) .1800(13) .015(5) Uiso ? ? 1.00000 ? ? H1b 1.148(2) .0112(16) .2594(16) .030(6) Uiso ? ? 1.00000 ? ? H13 .740(3) -.1443(18) .2424(18) .041(7) Uiso ? ? 1.00000 ? ? H14 .755(2) -.1024(17) .3840(16) .035(7) Uiso ? ? 1.00000 ? ? H15 .914(2) -.0144(18) .4435(18) .041(7) Uiso ? ? 1.00000 ? ? H16 1.056(2) .0283(16) .3734(15) .028(6) Uiso ? ? 1.00000 ? ? H2a .964(2) .1802(15) -.0402(14) .022(5) Uiso ? ? 1.00000 ? ? H2b 1.015(2) .2734(16) -.0039(14) .024(6) Uiso ? ? 1.00000 ? ? H24 .997(2) .2831(17) .1588(15) .028(6) Uiso ? ? 1.00000 ? ? H25 1.062(2) .1666(16) .2701(16) .029(6) Uiso ? ? 1.00000 ? ? H3a .8075(19) .1085(14) -.1011(13) .017(5) Uiso ? ? 1.00000 ? ? H3b .672(2) .1049(14) -.1190(14) .019(5) Uiso ? ? 1.00000 ? ? H33 .889(2) .3809(18) .0314(16) .033(6) Uiso ? ? 1.00000 ? ? H34 .706(2) .4425(18) .0116(16) .033(6) Uiso ? ? 1.00000 ? ? H35 .542(2) .3632(18) -.0468(16) .036(7) Uiso ? ? 1.00000 ? ? H36 .562(2) .2209(17) -.0823(15) .028(6) Uiso ? ? 1.00000 ? ? H4a .828(2) -.1633(16) .1268(15) .025(6) Uiso ? ? 1.00000 ? ? H4b .935(2) -.1151(17) .1160(15) .033(6) Uiso ? ? 1.00000 ? ? H44 .645(2) -.0410(17) .1272(15) .031(6) Uiso ? ? 1.00000 ? ? H45 .580(2) .0752(16) .0104(15) .028(6) Uiso ? ? 1.00000 ? ? H10a .699(5) .158(3) .296(4) .13(2) Uiso ? ? 1.00000 ? ? H10b .693(6) .180(4) .206(4) .15(2) Uiso ? ? 1.00000 ? ? H10c .795(4) .128(3) .240(3) .102(16) Uiso ? ? 1.00000 ? ? H20a .425(3) .002(2) .366(2) .058(9) Uiso ? ? 1.00000 ? ? H20b .535(3) -.065(3) .412(2) .082(12) Uiso ? ? 1.00000 ? ? H20c .416(3) -.096(2) .352(2) .052(9) Uiso ? ? 1.00000 ? ? H30a .29476 .20784 .20537 .18300 Uiso ? ? 1.00000 ? ? H30b .30962 .23143 .11705 .18300 Uiso ? ? 1.00000 ? ? H30c .42246 .23298 .19157 .18300 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 Pd .01398(8) .01357(8) .01351(8) .00021(6) .00489(6) -.00051(6) I .02763(8) .02929(8) .03218(8) .00221(5) .00278(5) .00427(5) C1 .0203(8) .0207(8) .0210(8) .0025(6) .0065(7) .0038(6) C11 .0206(8) .0210(8) .0189(8) .0043(7) .0065(6) .0031(6) C12 .0216(8) .0182(8) .0190(8) .0038(6) .0060(6) .0026(6) C13 .0232(8) .0266(9) .0222(8) .0003(7) .0067(7) .0046(7) C14 .0253(9) .0342(10) .0228(9) .0049(8) .0099(7) .0058(7) C15 .0302(10) .0344(10) .0176(8) .0057(8) .0074(7) .0007(7) C16 .0251(9) .0276(9) .0198(8) .0022(7) .0033(7) -.0002(7) C2 .0209(8) .0202(8) .0188(8) .0018(7) .0061(6) .0026(6) N21 .0184(7) .0189(7) .0174(6) -.0005(5) .0047(5) -.0007(5) C22 .0138(7) .0185(8) .0179(7) -.0006(6) .0047(6) -.0007(6) N23 .0189(7) .0171(7) .0172(6) -.0007(5) .0041(5) -.0011(5) C24 .0273(9) .0190(8) .0206(8) -.0019(7) .0045(7) -.0054(7) C25 .0260(9) .0232(9) .0180(8) -.0011(7) .0028(7) -.0056(6) C3 .0220(8) .0193(8) .0188(7) .0002(7) .0049(7) -.0000(6) C31 .0226(8) .0196(8) .0201(8) .0023(6) .0067(6) .0008(6) C32 .0212(8) .0198(8) .0181(7) .0019(6) .0065(6) .0017(6) C33 .0279(10) .0201(9) .0276(9) -.0007(7) .0054(8) -.0017(7) C34 .0349(11) .0204(9) .0394(11) .0060(8) .0120(9) -.0026(8) C35 .0266(10) .0291(10) .0404(12) .0087(8) .0099(9) .0005(8) C36 .0203(8) .0263(9) .0318(10) .0012(7) .0049(7) .0003(8) C4 .0250(8) .0185(8) .0197(8) .0012(7) .0072(7) .0018(6) N41 .0155(6) .0196(7) .0182(6) -.0001(5) .0043(5) -.0005(5) C42 .0172(7) .0167(7) .0157(7) -.0020(6) .0052(6) -.0024(6) N43 .0151(6) .0210(7) .0179(6) -.0015(5) .0044(5) -.0003(5) C44 .0167(8) .0313(10) .0249(9) -.0021(7) .0084(7) .0004(7) C45 .0156(8) .0309(10) .0247(8) .0006(7) .0060(7) .0007(7) C10 .0488(16) .0489(16) .0616(19) -.0117(13) .0147(15) -.0139(14) N10 .0440(11) .0392(11) .0413(11) .0092(9) .0194(9) -.0002(9) O11 .0516(10) .0559(11) .0407(9) -.0154(9) .0222(8) -.0218(8) O12 .089(2) .084(2) .129(3) .0316(17) .0019(19) .048(2) C20 .0455(14) .0548(17) .0444(14) -.0080(13) .0168(12) -.0111(12) N20 .0304(9) .0495(12) .0378(10) .0050(9) .0023(8) -.0016(9) O21 .0432(10) .0656(13) .0466(10) .0103(9) .0041(8) -.0179(9) O22 .0430(10) .0611(13) .0647(13) -.0075(9) .0083(9) .0124(10) C30 .126(4) .0347(17) .205(6) .010(2) .093(4) -.004(3) N30 .0353(10) .0438(11) .0443(11) .0069(9) .0123(9) -.0045(9) O31 .0621(14) .101(2) .0653(14) .0199(13) .0380(12) -.0003(13) O32 .0381(9) .0447(10) .0686(13) -.0082(8) .0121(9) -.0047(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 Pd C22 . . 2.0501(17) ? Pd C42 . . 2.0520(18) ? Pd C22 . '3 755' 2.0501(17) ? Pd C42 . '3 755' 2.0520(18) ? C1 C11 . . 1.520(3) ? C1 N21 . . 1.470(2) ? C1 H1a . . .98(2) ? C1 H1b . . .96(2) ? C11 C12 . . 1.401(2) ? C11 C16 . . 1.401(3) ? C12 C13 . . 1.396(3) ? C12 C4 . . 1.512(2) ? C13 C14 . . 1.387(3) ? C13 H13 . . .96(3) ? C14 C15 . . 1.385(3) ? C14 H14 . . .98(3) ? C15 C16 . . 1.388(3) ? C15 H15 . . .92(3) ? C16 H16 . . .96(2) ? C2 N23 . . 1.470(2) ? C2 C32 . . 1.516(3) ? C2 H2a . . .94(2) ? C2 H2b . . 1.02(2) ? N21 C22 . . 1.359(2) ? N21 C25 . . 1.387(2) ? C22 N23 . . 1.357(2) ? N23 C24 . . 1.389(2) ? C24 C25 . . 1.348(3) ? C24 H24 . . .94(3) ? C25 H25 . . .91(3) ? C3 C31 . . 1.511(3) ? C3 N41 . . 1.470(2) ? C3 H3a . . .95(2) ? C3 H3b . . .95(2) ? C31 C32 . . 1.409(2) ? C31 C36 . . 1.397(3) ? C32 C33 . . 1.394(3) ? C33 C34 . . 1.389(3) ? C33 H33 . . .95(3) ? C34 C35 . . 1.382(3) ? C34 H34 . . .91(3) ? C35 C36 . . 1.392(3) ? C35 H35 . . .89(3) ? C36 H36 . . .88(2) ? C4 N43 . . 1.472(2) ? C4 H4a . . .93(2) ? C4 H4b . . .93(3) ? N41 C42 . . 1.354(2) ? N41 C45 . . 1.389(3) ? C42 N43 . . 1.349(2) ? N43 C44 . . 1.392(2) ? C44 C45 . . 1.343(3) ? C44 H44 . . .95(3) ? C45 H45 . . .95(2) ? C10 N10 . . 1.488(4) ? C10 H10a . . .94(7) ? C10 H10b . . .99(6) ? C10 H10c . . .88(5) ? N10 O11 . . 1.208(3) ? N10 O12 . . 1.199(4) ? C20 N20 . . 1.486(4) ? C20 H20a . . .96(3) ? C20 H20b . . 1.06(4) ? C20 H20c . . .87(3) ? N20 O21 . . 1.221(3) ? N20 O22 . . 1.219(3) ? C30 N30 . . 1.465(5) ? C30 H30a . . .950(7) ? C30 H30b . . .970(6) ? C30 H30c . . .981(5) ? N30 O31 . . 1.204(4) ? N30 O32 . . 1.222(3) ? 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 C22 Pd C42 . . . 81.35(7) ? C22 Pd C22 . . '3 755' 180.0000 ? C22 Pd C42 . . '3 755' 98.65(7) ? C42 Pd C22 . . '3 755' 98.65(6) ? C42 Pd C42 . . '3 755' 180.0000 ? C22 Pd C42 '3 755' . '3 755' 81.35(6) ? C11 C1 N21 . . . 112.80(15) ? C11 C1 H1a . . . 113.7(13) ? C11 C1 H1b . . . 110.6(17) ? N21 C1 H1a . . . 105.9(13) ? N21 C1 H1b . . . 105.6(15) ? H1a C1 H1b . . . 108(2) ? C1 C11 C12 . . . 122.98(16) ? C1 C11 C16 . . . 118.36(16) ? C12 C11 C16 . . . 118.64(18) ? C11 C12 C13 . . . 119.55(16) ? C11 C12 C4 . . . 123.06(17) ? C13 C12 C4 . . . 117.39(15) ? C12 C13 C14 . . . 121.43(17) ? C12 C13 H13 . . . 117(2) ? C14 C13 H13 . . . 121(2) ? C13 C14 C15 . . . 119.0(2) ? C13 C14 H14 . . . 122.0(15) ? C15 C14 H14 . . . 119.0(15) ? C14 C15 C16 . . . 120.48(18) ? C14 C15 H15 . . . 120.3(18) ? C16 C15 H15 . . . 119.2(18) ? C11 C16 C15 . . . 120.91(17) ? C11 C16 H16 . . . 118.9(16) ? C15 C16 H16 . . . 120.2(16) ? N23 C2 C32 . . . 112.81(16) ? N23 C2 H2a . . . 105.2(14) ? N23 C2 H2b . . . 108.4(12) ? C32 C2 H2a . . . 112.0(13) ? C32 C2 H2b . . . 108.4(13) ? H2a C2 H2b . . . 110(2) ? C1 N21 C22 . . . 126.62(15) ? C1 N21 C25 . . . 122.45(15) ? C22 N21 C25 . . . 110.90(14) ? Pd C22 N21 . . . 129.45(12) ? Pd C22 N23 . . . 125.57(12) ? N21 C22 N23 . . . 104.53(14) ? C2 N23 C22 . . . 125.63(14) ? C2 N23 C24 . . . 123.31(15) ? C22 N23 C24 . . . 111.05(14) ? N23 C24 C25 . . . 106.61(16) ? N23 C24 H24 . . . 123.0(15) ? C25 C24 H24 . . . 130.4(14) ? N21 C25 C24 . . . 106.90(16) ? N21 C25 H25 . . . 121.3(15) ? C24 C25 H25 . . . 131.7(15) ? C31 C3 N41 . . . 112.48(15) ? C31 C3 H3a . . . 111.2(13) ? C31 C3 H3b . . . 109.1(14) ? N41 C3 H3a . . . 108.7(13) ? N41 C3 H3b . . . 106.6(14) ? H3a C3 H3b . . . 109(2) ? C3 C31 C32 . . . 122.71(16) ? C3 C31 C36 . . . 118.53(16) ? C32 C31 C36 . . . 118.75(17) ? C2 C32 C31 . . . 122.88(16) ? C2 C32 C33 . . . 118.17(16) ? C31 C32 C33 . . . 118.91(17) ? C32 C33 C34 . . . 121.66(18) ? C32 C33 H33 . . . 120.0(16) ? C34 C33 H33 . . . 118.3(16) ? C33 C34 C35 . . . 119.6(2) ? C33 C34 H34 . . . 119.8(16) ? C35 C34 H34 . . . 120.6(16) ? C34 C35 C36 . . . 119.6(2) ? C34 C35 H35 . . . 120.1(17) ? C36 C35 H35 . . . 120.3(17) ? C31 C36 C35 . . . 121.52(18) ? C31 C36 H36 . . . 118.7(17) ? C35 C36 H36 . . . 119.7(17) ? C12 C4 N43 . . . 111.45(15) ? C12 C4 H4a . . . 112.1(16) ? C12 C4 H4b . . . 114.0(15) ? N43 C4 H4a . . . 108.0(14) ? N43 C4 H4b . . . 104.9(15) ? H4a C4 H4b . . . 106(2) ? C3 N41 C42 . . . 125.95(16) ? C3 N41 C45 . . . 122.95(15) ? C42 N41 C45 . . . 111.10(15) ? Pd C42 N41 . . . 128.29(13) ? Pd C42 N43 . . . 126.20(11) ? N41 C42 N43 . . . 104.44(15) ? C4 N43 C42 . . . 124.64(15) ? C4 N43 C44 . . . 123.90(16) ? C42 N43 C44 . . . 111.34(14) ? N43 C44 C45 . . . 106.38(17) ? N43 C44 H44 . . . 123.0(15) ? C45 C44 H44 . . . 130.6(15) ? N41 C45 C44 . . . 106.74(16) ? N41 C45 H45 . . . 119.5(16) ? C44 C45 H45 . . . 133.6(16) ? N10 C10 H10a . . . 113(3) ? N10 C10 H10b . . . 87(3) ? N10 C10 H10c . . . 109(3) ? H10a C10 H10b . . . 102(5) ? H10a C10 H10c . . . 132(5) ? H10b C10 H10c . . . 101(5) ? C10 N10 O11 . . . 117.7(2) ? C10 N10 O12 . . . 120.3(2) ? O11 N10 O12 . . . 122.0(2) ? N20 C20 H20a . . . 107(2) ? N20 C20 H20b . . . 107(2) ? N20 C20 H20c . . . 106(2) ? H20a C20 H20b . . . 114(3) ? H20a C20 H20c . . . 111(3) ? H20b C20 H20c . . . 112(3) ? C20 N20 O21 . . . 119.0(2) ? C20 N20 O22 . . . 117.5(2) ? O21 N20 O22 . . . 123.4(2) ? N30 C30 H30a . . . 110.3(4) ? N30 C30 H30b . . . 109.1(5) ? N30 C30 H30c . . . 107.0(4) ? H30a C30 H30b . . . 107.8(5) ? H30a C30 H30c . . . 112.1(6) ? H30b C30 H30c . . . 110.4(5) ? C30 N30 O31 . . . 118.0(3) ? C30 N30 O32 . . . 117.4(3) ? O31 N30 O32 . . . 124.5(3) ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- 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 Pd C1 3.5628(19) . '3 755' ? Pd C1 3.5628(19) . . ? Pd C2 3.4410(19) . '3 755' ? Pd C2 3.4410(19) . . ? Pd N21 3.0969(15) . '3 755' ? Pd N21 3.0969(15) . . ? Pd N23 3.0465(15) . . ? Pd N23 3.0465(15) . '3 755' ? Pd C3 3.5231(18) . . ? Pd C3 3.5231(18) . '3 755' ? Pd C4 3.431(2) . . ? Pd C4 3.431(2) . '3 755' ? Pd N41 3.0798(15) . . ? Pd N41 3.0798(15) . '3 755' ? Pd N43 3.0492(16) . . ? Pd N43 3.0492(16) . '3 755' ? Pd H1a 3.02(2) . . ? Pd H1a 3.02(2) . '3 755' ? Pd H2a 2.84(2) . '3 755' ? Pd H2a 2.84(2) . . ? Pd H3a 3.00(2) . . ? Pd H3a 3.00(2) . '3 755' ? Pd H4b 2.82(3) . '3 755' ? Pd H4b 2.82(3) . . ? I H14 3.17(3) . '3 756' ? I H16 3.12(2) . . ? I H25 3.23(2) . . ? I H35 3.18(3) . '4 655' ? I H4a 3.08(2) . '2 755' ? C1 C12 2.567(3) . . ? C1 C16 2.510(3) . . ? C1 C22 2.528(2) . . ? C1 C25 2.504(3) . . ? C1 H16 2.63(3) . . ? C1 H25 2.69(2) . . ? C11 C13 2.417(3) . . ? C11 C14 2.811(3) . . ? C11 C15 2.427(3) . . ? C11 N21 2.491(2) . . ? C11 C4 2.561(2) . . ? C11 H1a 2.11(2) . . ? C11 H1b 2.06(3) . . ? C11 H16 2.04(2) . . ? C12 C14 2.428(3) . . ? C12 C15 2.786(3) . . ? C12 C16 2.410(2) . . ? C12 N43 2.466(2) . . ? C12 H13 2.02(3) . . ? C12 H4a 2.05(2) . . ? C12 H4b 2.08(3) . . ? C13 C15 2.388(3) . . ? C13 C16 2.761(3) . . ? C13 C4 2.486(3) . . ? C13 H14 2.08(3) . . ? C13 H4a 2.59(3) . . ? C14 C16 2.407(3) . . ? C14 H13 2.05(3) . . ? C14 H15 2.01(3) . . ? C15 H14 2.05(3) . . ? C15 H16 2.05(3) . . ? C16 H1b 2.58(3) . . ? C16 H15 2.00(3) . . ? C2 C22 2.515(2) . . ? C2 C24 2.516(2) . . ? C2 C31 2.570(2) . . ? C2 C33 2.498(3) . . ? C2 H33 2.64(3) . . ? N21 N23 2.148(2) . . ? N21 C24 2.197(2) . . ? N21 H1a 1.97(2) . . ? N21 H1b 1.96(2) . . ? N21 H25 2.01(3) . . ? C22 C24 2.264(3) . . ? C22 C25 2.262(3) . . ? C22 C42 2.674(2) . . ? C22 H1a 2.57(2) . . ? C22 H2a 2.52(2) . . ? N23 C25 2.194(2) . . ? N23 C32 2.487(2) . . ? N23 H2a 1.94(2) . . ? N23 H2b 2.04(2) . . ? N23 H24 2.05(3) . . ? C24 H25 2.07(3) . . ? C25 H1b 2.65(2) . . ? C25 H24 2.08(3) . . ? C3 C32 2.563(2) . . ? C3 C36 2.500(3) . . ? C3 C42 2.516(2) . . ? C3 C45 2.512(3) . . ? C3 H36 2.60(3) . . ? C3 H45 2.69(3) . . ? C31 C33 2.414(3) . . ? C31 C34 2.805(3) . . ? C31 C35 2.434(3) . . ? C31 N41 2.478(2) . . ? C31 H2a 2.70(2) . . ? C31 H3a 2.06(2) . . ? C31 H3b 2.03(2) . . ? C31 H36 1.97(2) . . ? C32 C34 2.430(3) . . ? C32 C35 2.803(3) . . ? C32 C36 2.415(3) . . ? C32 H2a 2.06(2) . . ? C32 H2b 2.08(2) . . ? C32 H33 2.04(3) . . ? C33 C35 2.395(3) . . ? C33 C36 2.755(3) . . ? C33 H2b 2.56(2) . . ? C33 H34 2.00(3) . . ? C34 C36 2.398(3) . . ? C34 H33 2.02(3) . . ? C34 H35 1.99(3) . . ? C35 H34 2.00(3) . . ? C35 H36 1.98(3) . . ? C36 H3b 2.54(2) . . ? C36 H35 2.00(3) . . ? C4 C42 2.498(2) . . ? C4 C44 2.527(3) . . ? C4 H13 2.58(3) . . ? N41 N43 2.136(2) . . ? N41 C44 2.193(3) . . ? N41 H3a 1.99(2) . . ? N41 H3b 1.97(2) . . ? N41 H45 2.03(3) . . ? C42 C44 2.263(3) . . ? C42 C45 2.261(3) . . ? C42 H3a 2.58(2) . . ? C42 H4b 2.49(2) . . ? N43 C45 2.190(2) . . ? N43 H4a 1.97(2) . . ? N43 H4b 1.94(3) . . ? N43 H44 2.07(3) . . ? C44 H45 2.11(2) . . ? C45 H3b 2.69(2) . . ? C45 H44 2.09(3) . . ? C10 O11 2.312(4) . . ? C10 O12 2.335(5) . . ? N10 H10a 2.05(6) . . ? N10 H10b 1.75(6) . . ? N10 H10c 1.96(5) . . ? O11 O12 2.106(4) . . ? O11 H2a 2.59(2) . 4 ? O11 H3a 2.66(2) . 4 ? O11 H10c 2.59(5) . . ? O12 H10b 2.05(6) . . ? O12 H20c 2.46(3) . '2 655' ? C20 O21 2.336(4) . . ? C20 O22 2.317(4) . . ? N20 H20a 2.00(4) . . ? N20 H20b 2.05(4) . . ? N20 H20c 1.92(4) . . ? O21 O22 2.149(3) . . ? O21 H13 2.70(3) . . ? O21 H3b 2.64(2) . '3 655' ? O21 H20c 2.35(4) . . ? O22 H10a 2.53(6) . . ? O22 H20a 2.46(4) . . ? O22 H20b 2.69(4) . . ? C30 O31 2.292(6) . . ? C30 O32 2.300(4) . . ? N30 H30a 2.004(2) . . ? N30 H30b 2.004(2) . . ? N30 H30c 1.987(2) . . ? O31 O32 2.148(3) . . ? O31 H45 2.58(3) . . ? O31 H30b 2.598(3) . . ? O31 H30c 2.479(3) . . ? O32 H1b 2.67(3) . '1 455' ? O32 H3b 2.69(2) . '3 655' ? O32 H30a 2.368(2) . . ? H1a H1b 1.56(3) . . ? H1a H3a 2.17(3) . '3 755' ? H1a H4b 2.23(3) . . ? H1b H16 2.37(4) . . ? H13 H4a 2.37(4) . . ? H14 H15 2.33(4) . . ? H15 H16 2.32(4) . . ? H2a H2b 1.61(3) . . ? H2a H3a 2.19(3) . . ? H2a H4b 2.14(4) . '3 755' ? H2b H33 2.36(4) . . ? H3a H3b 1.55(3) . . ? H3b H36 2.34(4) . . ? H33 H34 2.29(4) . . ? H34 H35 2.29(4) . . ? H35 H36 2.28(4) . . ? H4a H4b 1.49(4) . . ? H10a H10b 1.51(9) . . ? H10a H10c 1.66(9) . . ? H10b H10c 1.45(8) . . ? H20a H20b 1.69(5) . . ? H20a H20c 1.52(5) . . ? H20b H20c 1.60(5) . . ? H30a H30b 1.55130(17) . . ? H30a H30c 1.6020(2) . . ? H30b H30c 1.60196(17) . . ? _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 1408 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 15 _reflns_limit_k_min 0 _reflns_limit_k_max 20 _reflns_limit_l_min -22 _reflns_limit_l_max 21 _reflns_number_observed ? _reflns_d_resolution_high .731 _reflns_d_resolution_low 11.379 _diffrn_reflns_av_sigmaI/netI .017 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _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 .027 _refine_ls_wR_factor_all .033 _refine_ls_goodness_of_fit_all 1.022 _refine_ls_shift/su_mean .001 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end #===END ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_ccw167 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C19 H24 Br2 N4 O1 Pd1' _chemical_formula_moiety ? _chemical_formula_weight 590.66 _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 11.207(3) _cell_length_b 13.300(3) _cell_length_c 15.434(3) _cell_angle_alpha 90.00000 _cell_angle_beta 106.661(3) _cell_angle_gamma 90.00000 _cell_volume 2203.9(9) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.78 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 5847 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26.4 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 4.48 _exptl_crystal_description block _exptl_crystal_size_max .40 _exptl_crystal_size_mid .30 _exptl_crystal_size_min .20 _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 .407 _exptl_absorpt_correction_T_max .802 _diffrn_reflns_number 25643 _reflns_number_total 5589 _reflns_Friedel_coverage ? _reflns_number_gt 3828 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.08 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .044 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .039 _refine_ls_wR_factor_ref .047 _refine_ls_goodness_of_fit_ref 1.402 _refine_ls_number_reflns 3828 _refine_ls_number_parameters 245 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .04 _refine_diff_density_min -1.085 _refine_diff_density_max .936 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef 94(192) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 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 76 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 96 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Br ? 0 8 -.374 2.456 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 16 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 4 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' Pd ? 0 4 -1.177 1.007 '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 Pd .31153(3) .83637(3) .25624(2) .03093(18) Uani ? ? 1.00000 ? ? Br1 .20176(6) .68642(4) .17891(4) .0581(3) Uani ? ? 1.00000 ? ? Br2 .21881(6) .94888(5) .12727(4) .0590(3) Uani ? ? 1.00000 ? ? C1 .2120(5) .7469(5) .4305(4) .061(4) Uani ? ? 1.00000 ? ? C2 .5870(5) .7085(4) .3280(3) .042(3) Uani ? ? 1.00000 ? ? N21 .3361(4) .7207(3) .4258(3) .048(2) Uani ? ? 1.00000 ? ? C22 .3874(4) .7486(4) .3614(3) .037(2) Uani ? ? 1.00000 ? ? N23 .4975(4) .7016(3) .3798(3) .040(2) Uani ? ? 1.00000 ? ? C24 .5159(6) .6429(5) .4559(4) .061(3) Uani ? ? 1.00000 ? ? C25 .4147(6) .6555(5) .4856(4) .068(4) Uani ? ? 1.00000 ? ? C3 .6073(4) .9350(4) .2984(3) .039(2) Uani ? ? 1.00000 ? ? C31 .7097(4) .8743(4) .3637(3) .035(2) Uani ? ? 1.00000 ? ? C32 .7002(4) .7701(4) .3762(3) .035(2) Uani ? ? 1.00000 ? ? C33 .8010(5) .7210(4) .4345(4) .043(3) Uani ? ? 1.00000 ? ? C34 .9088(5) .7701(4) .4811(3) .044(3) Uani ? ? 1.00000 ? ? C35 .9157(5) .8727(4) .4679(4) .047(3) Uani ? ? 1.00000 ? ? C36 .8180(5) .9223(4) .4095(4) .043(3) Uani ? ? 1.00000 ? ? C4 .2204(6) 1.0274(5) .3663(5) .074(4) Uani ? ? 1.00000 ? ? N41 .5192(4) .9816(3) .3396(3) .035(2) Uani ? ? 1.00000 ? ? C42 .3993(5) .9541(3) .3253(3) .035(2) Uani ? ? 1.00000 ? ? N43 .3487(4) 1.0238(3) .3670(3) .045(2) Uani ? ? 1.00000 ? ? C44 .4370(6) 1.0949(4) .4068(4) .051(3) Uani ? ? 1.00000 ? ? C45 .5419(5) 1.0688(4) .3898(4) .050(3) Uani ? ? 1.00000 ? ? O0 .7215(6) .8317(5) .1485(4) .121(5) Uani ? ? 1.00000 ? ? C0 .8247(8) .8652(7) .1726(5) .081(5) Uani ? ? 1.00000 ? ? C01 .9275(8) .8102(7) .2318(6) .111(6) Uani ? ? 1.00000 ? ? C02 .8546(11) .9691(9) .1485(7) .142(8) Uani ? ? 1.00000 ? ? H1a .17896 .69503 .45964 .09400 Uiso ? ? 1.00000 ? ? H1b .15697 .75722 .37142 .09400 Uiso ? ? 1.00000 ? ? H1c .21491 .80799 .46464 .09400 Uiso ? ? 1.00000 ? ? H2a .54809 .73981 .26951 .05300 Uiso ? ? 1.00000 ? ? H2b .61390 .64308 .31577 .05300 Uiso ? ? 1.00000 ? ? H24 .58734 .60152 .48449 .07600 Uiso ? ? 1.00000 ? ? H25 .39897 .62324 .53823 .08200 Uiso ? ? 1.00000 ? ? H3a .56246 .89181 .24988 .04900 Uiso ? ? 1.00000 ? ? H3b .64610 .98676 .27202 .04900 Uiso ? ? 1.00000 ? ? H33 .79564 .64959 .44244 .05600 Uiso ? ? 1.00000 ? ? H34 .97597 .73456 .52180 .05500 Uiso ? ? 1.00000 ? ? H35 .99019 .90791 .50162 .06000 Uiso ? ? 1.00000 ? ? H36 .82560 .99453 .40052 .05700 Uiso ? ? 1.00000 ? ? H4a .16430 1.00985 .30666 .11100 Uiso ? ? 1.00000 ? ? H4b .20077 .98383 .40889 .11100 Uiso ? ? 1.00000 ? ? H4c .19587 1.09486 .37758 .11100 Uiso ? ? 1.00000 ? ? H44 .42435 1.15308 .44165 .06600 Uiso ? ? 1.00000 ? ? H45 .62051 1.10539 .40810 .06200 Uiso ? ? 1.00000 ? ? H01a .96436 .84629 .28561 .16100 Uiso ? ? 1.00000 ? ? H01b .99089 .79766 .20166 .16100 Uiso ? ? 1.00000 ? ? H01c .89808 .74687 .24633 .16100 Uiso ? ? 1.00000 ? ? H02a .78093 .99297 .10107 .18300 Uiso ? ? 1.00000 ? ? H02b .91952 .96306 .11794 .18300 Uiso ? ? 1.00000 ? ? H02c .87358 1.01332 .19603 .18300 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 Pd .0272(2) .0332(2) .0296(2) .00306(16) .00384(14) -.00170(16) Br1 .0536(4) .0515(4) .0597(4) -.0011(3) .0010(3) -.0113(3) Br2 .0704(4) .0510(4) .0500(4) .0105(3) .0082(3) .0107(3) C1 .051(4) .077(5) .059(4) -.001(3) .021(3) .001(3) C2 .040(3) .031(3) .049(3) .002(2) -.000(3) -.005(2) N21 .042(3) .057(3) .038(2) -.008(2) .001(2) .007(2) C22 .034(3) .038(3) .035(3) -.007(2) .001(2) -.003(2) N23 .031(2) .036(2) .046(3) -.0034(19) -.002(2) .008(2) C24 .044(3) .059(4) .065(4) -.009(3) -.007(3) .024(3) C25 .061(4) .076(5) .051(4) -.021(4) -.009(3) .027(3) C3 .036(3) .038(3) .042(3) -.001(2) .010(2) .002(2) C31 .031(3) .036(3) .036(3) .004(2) .007(2) -.004(2) C32 .027(3) .036(3) .039(3) .002(2) .006(2) -.005(2) C33 .041(3) .033(3) .051(3) .001(2) .007(3) -.000(2) C34 .034(3) .049(3) .042(3) .003(2) -.001(2) .000(2) C35 .033(3) .048(3) .053(3) -.006(2) .002(3) -.009(3) C36 .040(3) .031(3) .055(3) -.002(2) .008(3) -.003(2) C4 .061(4) .073(5) .098(5) .005(4) .038(4) -.021(4) N41 .032(2) .032(2) .038(2) -.0009(18) .0045(18) -.0027(18) C42 .040(3) .034(3) .030(2) .005(2) .008(2) .001(2) N43 .047(3) .042(3) .047(3) .006(2) .015(2) -.007(2) C44 .064(4) .040(3) .050(3) -.000(3) .015(3) -.013(3) C45 .052(4) .035(3) .052(3) -.006(3) .000(3) -.008(3) O0 .070(4) .206(8) .073(4) -.005(4) -.002(3) -.018(4) C0 .063(5) .126(7) .053(4) .014(5) .015(4) -.019(4) C01 .070(5) .180(10) .083(6) .044(6) .022(5) .006(6) C02 .167(10) .144(10) .111(8) .027(8) .033(7) -.015(7) # 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 Pd Br1 . . 2.4645(8) ? Pd Br2 . . 2.4688(7) ? Pd C22 . . 1.982(5) ? Pd C42 . . 1.989(4) ? C1 N21 . . 1.455(8) ? C1 H1a . . .955(7) ? C1 H1b . . .953(5) ? C1 H1c . . .964(7) ? C2 N23 . . 1.454(8) ? C2 C32 . . 1.514(6) ? C2 H2a . . .976(5) ? C2 H2b . . .957(5) ? N21 C22 . . 1.335(7) ? N21 C25 . . 1.384(7) ? C22 N23 . . 1.339(6) ? N23 C24 . . 1.376(8) ? C24 C25 . . 1.350(10) ? C24 H24 . . .967(6) ? C25 H25 . . .978(7) ? C3 C31 . . 1.524(6) ? C3 N41 . . 1.457(7) ? C3 H3a . . .963(5) ? C3 H3b . . .965(5) ? C31 C32 . . 1.407(7) ? C31 C36 . . 1.374(7) ? C32 C33 . . 1.389(6) ? C33 C34 . . 1.381(7) ? C33 H33 . . .961(5) ? C34 C35 . . 1.385(8) ? C34 H34 . . .956(5) ? C35 C36 . . 1.372(7) ? C35 H35 . . .968(5) ? C36 H36 . . .977(5) ? C4 N43 . . 1.435(9) ? C4 H4a . . .983(6) ? C4 H4b . . .948(8) ? C4 H4c . . .968(7) ? N41 C42 . . 1.348(6) ? N41 C45 . . 1.377(7) ? C42 N43 . . 1.343(7) ? N43 C44 . . 1.379(7) ? C44 C45 . . 1.323(9) ? C44 H44 . . .976(6) ? C45 H45 . . .975(5) ? O0 C0 . . 1.194(10) ? C0 C01 . . 1.447(11) ? C0 C02 . . 1.494(16) ? C01 H01a . . .945(8) ? C01 H01b . . .969(10) ? C01 H01c . . .954(10) ? C02 H02a . . .985(10) ? C02 H02b . . .977(13) ? C02 H02c . . .916(11) ? 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 Br1 Pd Br2 . . . 93.65(3) ? Br1 Pd C22 . . . 87.54(14) ? Br1 Pd C42 . . . 176.70(14) ? Br2 Pd C22 . . . 178.78(14) ? Br2 Pd C42 . . . 89.08(13) ? C22 Pd C42 . . . 89.71(18) ? N21 C1 H1a . . . 110.9(5) ? N21 C1 H1b . . . 110.6(6) ? N21 C1 H1c . . . 110.3(5) ? H1a C1 H1b . . . 108.8(6) ? H1a C1 H1c . . . 107.9(7) ? H1b C1 H1c . . . 108.2(6) ? N23 C2 C32 . . . 112.1(4) ? N23 C2 H2a . . . 109.8(4) ? N23 C2 H2b . . . 110.9(5) ? C32 C2 H2a . . . 108.2(5) ? C32 C2 H2b . . . 108.8(4) ? H2a C2 H2b . . . 106.8(5) ? C1 N21 C22 . . . 126.3(4) ? C1 N21 C25 . . . 123.5(5) ? C22 N21 C25 . . . 110.0(5) ? Pd C22 N21 . . . 126.7(4) ? Pd C22 N23 . . . 127.0(4) ? N21 C22 N23 . . . 106.3(4) ? C2 N23 C22 . . . 126.4(4) ? C2 N23 C24 . . . 123.1(4) ? C22 N23 C24 . . . 110.4(5) ? N23 C24 C25 . . . 106.5(5) ? N23 C24 H24 . . . 127.9(7) ? C25 C24 H24 . . . 125.6(7) ? N21 C25 C24 . . . 106.7(6) ? N21 C25 H25 . . . 126.6(7) ? C24 C25 H25 . . . 126.6(6) ? C31 C3 N41 . . . 114.4(4) ? C31 C3 H3a . . . 108.9(4) ? C31 C3 H3b . . . 108.2(4) ? N41 C3 H3a . . . 109.0(4) ? N41 C3 H3b . . . 109.0(4) ? H3a C3 H3b . . . 107.1(5) ? C3 C31 C32 . . . 122.7(4) ? C3 C31 C36 . . . 118.7(4) ? C32 C31 C36 . . . 118.5(4) ? C2 C32 C31 . . . 123.5(4) ? C2 C32 C33 . . . 118.3(4) ? C31 C32 C33 . . . 118.2(4) ? C32 C33 C34 . . . 122.8(5) ? C32 C33 H33 . . . 118.6(5) ? C34 C33 H33 . . . 118.6(5) ? C33 C34 C35 . . . 117.8(4) ? C33 C34 H34 . . . 121.0(5) ? C35 C34 H34 . . . 121.2(5) ? C34 C35 C36 . . . 120.2(4) ? C34 C35 H35 . . . 118.2(5) ? C36 C35 H35 . . . 121.5(5) ? C31 C36 C35 . . . 122.4(5) ? C31 C36 H36 . . . 118.9(4) ? C35 C36 H36 . . . 118.7(5) ? N43 C4 H4a . . . 111.7(7) ? N43 C4 H4b . . . 114.0(6) ? N43 C4 H4c . . . 111.4(6) ? H4a C4 H4b . . . 106.8(6) ? H4a C4 H4c . . . 104.5(6) ? H4b C4 H4c . . . 107.9(8) ? C3 N41 C42 . . . 125.6(4) ? C3 N41 C45 . . . 124.3(4) ? C42 N41 C45 . . . 109.6(4) ? Pd C42 N41 . . . 128.1(4) ? Pd C42 N43 . . . 126.1(4) ? N41 C42 N43 . . . 105.8(4) ? C4 N43 C42 . . . 125.4(5) ? C4 N43 C44 . . . 124.7(5) ? C42 N43 C44 . . . 109.8(5) ? N43 C44 C45 . . . 107.3(5) ? N43 C44 H44 . . . 126.2(6) ? C45 C44 H44 . . . 126.5(6) ? N41 C45 C44 . . . 107.5(5) ? N41 C45 H45 . . . 126.1(6) ? C44 C45 H45 . . . 126.3(6) ? O0 C0 C01 . . . 122.2(9) ? O0 C0 C02 . . . 122.3(8) ? C01 C0 C02 . . . 115.5(8) ? C0 C01 H01a . . . 111.5(9) ? C0 C01 H01b . . . 110.2(8) ? C0 C01 H01c . . . 109.2(8) ? H01a C01 H01b . . . 108.2(8) ? H01a C01 H01c . . . 109.6(9) ? H01b C01 H01c . . . 108.1(9) ? C0 C02 H02a . . . 106.4(10) ? C0 C02 H02b . . . 107.2(10) ? C0 C02 H02c . . . 114.3(10) ? H02a C02 H02b . . . 104.4(10) ? H02a C02 H02c . . . 110.0(12) ? H02b C02 H02c . . . 113.9(12) ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- 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 Pd C1 3.408(7) . . ? Pd C2 3.419(5) . . ? Pd N21 2.979(5) . . ? Pd N23 2.985(4) . . ? Pd C3 3.448(5) . . ? Pd C4 3.374(8) . . ? Pd N41 3.014(4) . . ? Pd N43 2.983(4) . . ? Pd H1b 3.0057(6) . . ? Pd H2a 2.8997(7) . . ? Pd H3a 2.9359(8) . . ? Pd H4a 3.0640(6) . . ? Br1 Br2 3.5978(11) . . ? Br1 C22 3.096(4) . . ? Br1 H1b 3.2897(9) . . ? Br1 H3b 3.1292(8) . '2 645' ? Br1 H34 3.1415(7) . '4 464' ? Br1 H36 2.8097(8) . '2 645' ? Br1 H45 2.9096(9) . '2 645' ? Br1 H01b 2.8936(9) . '1 455' ? Br1 H02c 3.2670(8) . '2 645' ? Br2 C42 3.145(4) . . ? Br2 H1a 3.1455(8) . '4 564' ? Br2 H2b 3.1644(8) . '2 655' ? Br2 H25 2.9114(9) . '4 564' ? Br2 H33 2.8652(8) . '2 655' ? Br2 H4a 3.1091(9) . . ? C1 C22 2.490(9) . . ? C1 C25 2.501(9) . . ? C2 C22 2.493(8) . . ? C2 C24 2.489(9) . . ? C2 C31 2.574(7) . . ? C2 C33 2.494(7) . . ? C2 H3a 2.699(5) . . ? C2 H33 2.614(5) . . ? N21 N23 2.140(7) . . ? N21 C24 2.194(8) . . ? N21 H1a 2.005(5) . . ? N21 H1b 2.001(4) . . ? N21 H1c 2.005(5) . . ? N21 H25 2.119(4) . . ? C22 C24 2.230(7) . . ? C22 C25 2.228(8) . . ? C22 C42 2.801(7) . . ? C22 H1b 2.633(5) . . ? C22 H2a 2.595(6) . . ? N23 C25 2.185(9) . . ? N23 C32 2.463(7) . . ? N23 H2a 2.007(5) . . ? N23 H2b 2.006(5) . . ? N23 H24 2.113(4) . . ? C24 H2b 2.692(7) . . ? C24 H25 2.087(7) . . ? C25 H1a 2.610(7) . . ? C25 H24 2.068(7) . . ? C3 C32 2.573(7) . . ? C3 C36 2.495(6) . . ? C3 C42 2.495(8) . . ? C3 C45 2.506(8) . . ? C3 H2a 2.685(5) . . ? C3 H36 2.624(4) . . ? C31 C33 2.400(7) . . ? C31 C34 2.805(6) . . ? C31 C35 2.406(6) . . ? C31 N41 2.505(6) . . ? C31 H2a 2.662(4) . . ? C31 H3a 2.050(4) . . ? C31 H3b 2.042(5) . . ? C31 H36 2.036(5) . . ? C32 C34 2.433(6) . . ? C32 C35 2.782(7) . . ? C32 C36 2.391(7) . . ? C32 H2a 2.042(4) . . ? C32 H2b 2.035(5) . . ? C32 H3a 2.660(4) . . ? C32 H33 2.033(5) . . ? C33 C35 2.369(7) . . ? C33 C36 2.720(7) . . ? C33 H2b 2.574(5) . . ? C33 H34 2.044(5) . . ? C34 C36 2.390(7) . . ? C34 H33 2.025(5) . . ? C34 H35 2.031(5) . . ? C35 H34 2.050(5) . . ? C35 H36 2.031(5) . . ? C36 H3b 2.570(5) . . ? C36 H35 2.052(5) . . ? C4 C42 2.469(9) . . ? C4 C44 2.493(9) . . ? N41 N43 2.147(6) . . ? N41 C44 2.178(8) . . ? N41 H3a 1.991(4) . . ? N41 H3b 1.992(5) . . ? N41 H45 2.105(4) . . ? C42 C44 2.227(7) . . ? C42 C45 2.227(7) . . ? C42 H3a 2.571(5) . . ? C42 H4a 2.670(5) . . ? N43 C45 2.176(7) . . ? N43 H4a 2.017(4) . . ? N43 H4b 2.016(5) . . ? N43 H4c 2.003(5) . . ? N43 H44 2.108(4) . . ? C44 H4c 2.609(6) . . ? C44 H45 2.056(7) . . ? C45 H3b 2.660(6) . . ? C45 H44 2.059(6) . . ? O0 C01 2.315(10) . . ? O0 C02 2.359(14) . . ? O0 H24 2.698(5) . '4 564' ? O0 H01c 2.399(6) . . ? O0 H02a 2.420(7) . . ? C0 H01a 1.998(7) . . ? C0 H01b 2.000(9) . . ? C0 H01c 1.978(9) . . ? C0 H02a 2.009(9) . . ? C0 H02b 2.012(9) . . ? C0 H02c 2.049(10) . . ? C01 C02 2.487(15) . . ? C01 H02b 2.672(9) . . ? C02 H01a 2.677(11) . . ? H1a H1b 1.5513(2) . . ? H1a H1c 1.5516(3) . . ? H1b H1c 1.5530(2) . . ? H2a H2b 1.5514(3) . . ? H2a H3a 2.0573(4) . . ? H2b H33 2.3864(4) . . ? H3a H3b 1.5513(3) . . ? H3b H36 2.3881(4) . . ? H33 H34 2.3329(4) . . ? H34 H35 2.3380(5) . . ? H35 H36 2.3482(3) . . ? H4a H4b 1.5513(3) . . ? H4a H4c 1.5426(2) . . ? H4b H4c 1.5498(3) . . ? H01a H01b 1.5513(2) . . ? H01a H01c 1.5523(3) . . ? H01b H01c 1.5571(2) . . ? H02a H02b 1.5513(4) . . ? H02a H02c 1.5578(2) . . ? H02b H02c 1.5876(2) . . ? _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 1160 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 15 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min -21 _reflns_limit_l_max 20 _reflns_number_observed ? _reflns_d_resolution_high .731 _reflns_d_resolution_low 10.714 _diffrn_reflns_av_sigmaI/netI .097 _diffrn_reflns_theta_min 1.9 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression 'Eq22 p292 "Cryst. Comp." Munksgaard 1970' _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .07 _refine_ls_wR_factor_all .051 _refine_ls_goodness_of_fit_all 1.228 _refine_ls_shift/su_mean .002 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end #===END