# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2254 ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_global _audit_creation_method Xtal3.6 _audit_creation_date 00-04-16 _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 ; An investigation of 1,4,7-tri(4-alkynyl)-1,4,7-triacyclononanes - ligand synthesis and metal co-ordination chemistry ; _publ_section_title_footnote ; ? ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Skelton, Brian W.' . ; Crystallography Centre, 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_dbspot # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C48 H60 B1 N3' _chemical_formula_moiety ? _chemical_formula_weight 689.84 _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 11.7630(10) _cell_length_b 26.994(3) _cell_length_c 12.9070(10) _cell_angle_alpha 90.00000 _cell_angle_beta 90.296(2) _cell_angle_gamma 90.00000 _cell_volume 4098.3(7) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.118 _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 26 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu .064 _exptl_crystal_description prism _exptl_crystal_size_max .38 _exptl_crystal_size_mid .35 _exptl_crystal_size_min .12 _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 .762 _exptl_absorpt_correction_T_max .928 _diffrn_reflns_number 40295 _reflns_number_total 10355 _reflns_Friedel_coverage 0 _reflns_number_gt 7171 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.12 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .032 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _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 .048 _refine_ls_wR_factor_ref .058 _refine_ls_goodness_of_fit_ref .997 _refine_ls_number_reflns 7171 _refine_ls_number_parameters 712 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment mixed _refine_ls_shift/su_max .081 _refine_diff_density_min -.283 _refine_diff_density_max .314 _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 ? 0 192 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 240 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' B ? 0 4 0 .001 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 12 .004 .003 '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 N1 .60730(12) .32215(5) .68212(11) .0254(7) Uani ? ? 1.00000 ? ? C11 .52032(16) .32323(7) .76735(14) .0282(9) Uani ? ? 1.00000 ? ? C12 .50709(16) .37379(7) .81726(13) .0278(9) Uani ? ? 1.00000 ? ? C13 .46003(18) .41328(7) .74311(15) .0345(10) Uani ? ? 1.00000 ? ? C14 .44520(17) .46102(7) .79628(16) .0379(10) Uani ? ? 1.00000 ? ? C15 .43498(19) .49796(8) .84475(18) .0454(12) Uani ? ? 1.00000 ? ? C16 .4218(3) .54322(10) .9073(3) .0652(18) Uani ? ? 1.00000 ? ? C2 .59032(19) .27801(7) .61242(15) .0349(10) Uani ? ? 1.00000 ? ? C3 .5140(2) .29348(8) .52282(16) .0403(11) Uani ? ? 1.00000 ? ? N4 .54874(14) .34207(6) .48218(11) .0339(8) Uani ? ? 1.00000 ? ? C41 .4598(2) .36225(10) .41354(19) .0481(13) Uani ? ? 1.00000 ? ? C42 .4807(2) .41493(12) .3783(3) .075(2) Uani ? ? 1.00000 ? ? C43 .4737(3) .45186(15) .4508(3) .051(2) Uani ? ? .657(5) ? ? C44 .3644(4) .45636(14) .5037(3) .050(2) Uani ? ? .657(5) ? ? C45 .2645(3) .45924(9) .5405(2) .0599(16) Uani ? ? 1.00000 ? ? C46 .1664(3) .46688(13) .6048(3) .071(2) Uani ? ? 1.00000 ? ? C5 .66180(18) .34062(8) .43258(14) .0359(10) Uani ? ? 1.00000 ? ? C6 .74048(17) .38239(7) .46744(14) .0328(9) Uani ? ? 1.00000 ? ? N7 .74936(13) .38768(5) .58112(11) .0281(7) Uani ? ? 1.00000 ? ? C71 .80655(19) .43422(8) .60893(16) .0377(11) Uani ? ? 1.00000 ? ? C72 .7996(2) .44666(8) .72343(18) .0417(12) Uani ? ? 1.00000 ? ? C73 .8531(3) .49736(12) .7467(3) .070(2) Uani ? ? 1.00000 ? ? C74 .8510(3) .50809(11) .8586(3) .0699(18) Uani ? ? 1.00000 ? ? C75 .8485(3) .51393(11) .9492(3) .0721(19) Uani ? ? 1.00000 ? ? C76 .8484(3) .51994(17) 1.0627(3) .087(2) Uani ? ? 1.00000 ? ? C8 .80267(16) .34463(7) .63216(14) .0297(9) Uani ? ? 1.00000 ? ? C9 .72714(15) .32627(7) .72036(14) .0295(9) Uani ? ? 1.00000 ? ? B .10089(16) .25403(7) .57726(14) .0221(8) Uani ? ? 1.00000 ? ? C111 -.01430(14) .22057(6) .55362(12) .0229(8) Uani ? ? 1.00000 ? ? C112 -.09935(14) .23374(6) .48174(13) .0242(8) Uani ? ? 1.00000 ? ? C113 -.19722(15) .20534(7) .46605(13) .0278(8) Uani ? ? 1.00000 ? ? C114 -.21431(15) .16218(7) .52301(13) .0293(9) Uani ? ? 1.00000 ? ? C115 -.13192(15) .14772(7) .59420(13) .0281(9) Uani ? ? 1.00000 ? ? C116 -.03466(15) .17634(6) .60835(13) .0253(8) Uani ? ? 1.00000 ? ? C121 .20797(14) .21573(6) .59868(12) .0231(8) Uani ? ? 1.00000 ? ? C122 .22487(15) .17370(6) .53588(13) .0266(8) Uani ? ? 1.00000 ? ? C123 .31272(16) .14001(7) .55227(15) .0312(9) Uani ? ? 1.00000 ? ? C124 .38823(16) .14693(7) .63419(15) .0340(10) Uani ? ? 1.00000 ? ? C125 .37436(16) .18762(7) .69828(15) .0331(9) Uani ? ? 1.00000 ? ? C126 .28616(15) .22115(7) .68044(13) .0272(8) Uani ? ? 1.00000 ? ? C131 .12557(13) .29042(6) .47706(12) .0228(7) Uani ? ? 1.00000 ? ? C132 .20091(14) .27860(6) .39715(13) .0253(8) Uani ? ? 1.00000 ? ? C133 .21489(15) .30840(7) .30961(13) .0276(8) Uani ? ? 1.00000 ? ? C134 .15519(15) .35227(7) .29962(13) .0271(8) Uani ? ? 1.00000 ? ? C135 .08110(15) .36599(7) .37802(14) .0289(9) Uani ? ? 1.00000 ? ? C136 .06691(15) .33544(6) .46380(13) .0261(8) Uani ? ? 1.00000 ? ? C141 .08077(14) .28874(6) .68035(12) .0226(7) Uani ? ? 1.00000 ? ? C142 .14497(15) .33203(6) .69721(13) .0270(8) Uani ? ? 1.00000 ? ? C143 .12815(16) .36311(7) .78177(14) .0305(9) Uani ? ? 1.00000 ? ? C144 .04479(15) .35216(7) .85418(13) .0284(9) Uani ? ? 1.00000 ? ? C145 -.01780(15) .30921(7) .84245(13) .0267(8) Uani ? ? 1.00000 ? ? C146 .00042(14) .27806(6) .75746(12) .0246(8) Uani ? ? 1.00000 ? ? C43' .3835(5) .4471(2) .3700(4) .037(3) Uani ? ? .343(5) ? ? C44' .3067(5) .4536(2) .4602(5) .033(3) Uani ? ? .343(5) ? ? H1 .5961(17) .3498(8) .6400(16) .031(5) Uiso ? ? 1.00000 ? ? H11a .5429(17) .2968(8) .8181(16) .036(5) Uiso ? ? 1.00000 ? ? H11b .4480(18) .3130(8) .7359(16) .033(5) Uiso ? ? 1.00000 ? ? H12a .5813(17) .3850(7) .8467(15) .030(5) Uiso ? ? 1.00000 ? ? H12b .4550(18) .3696(8) .8761(17) .037(6) Uiso ? ? 1.00000 ? ? H13a .387(2) .4010(9) .7136(19) .053(7) Uiso ? ? 1.00000 ? ? H13b .5116(18) .4177(8) .6839(17) .038(6) Uiso ? ? 1.00000 ? ? H16a .384(3) .5683(14) .871(3) .097(12) Uiso ? ? 1.00000 ? ? H16b .495(3) .5559(14) .926(3) .109(13) Uiso ? ? 1.00000 ? ? H16c .379(3) .5356(11) .971(3) .081(10) Uiso ? ? 1.00000 ? ? H2a .5548(18) .2510(8) .6530(16) .036(6) Uiso ? ? 1.00000 ? ? H2b .6668(18) .2667(8) .5889(16) .034(5) Uiso ? ? 1.00000 ? ? H3a .434(2) .2960(8) .5440(17) .043(6) Uiso ? ? 1.00000 ? ? H3b .518(2) .2670(9) .4692(18) .047(6) Uiso ? ? 1.00000 ? ? H41a .387(2) .3609(9) .4517(19) .051(7) Uiso ? ? 1.00000 ? ? H41b .451(2) .3386(10) .353(2) .062(8) Uiso ? ? 1.00000 ? ? H42a .42772 .42331 .32581 .09200 Uiso ? ? .657(5) ? ? H42b .55622 .41680 .34979 .09200 Uiso ? ? .657(5) ? ? H43a .49052 .48303 .41806 .05400 Uiso ? ? .657(5) ? ? H43b .53280 .44614 .50198 .05400 Uiso ? ? .657(5) ? ? H46a .122(3) .4374(15) .615(3) .113(13) Uiso ? ? 1.00000 ? ? H46b .188(4) .4770(17) .682(4) .154(19) Uiso ? ? 1.00000 ? ? H46c .122(3) .4931(14) .583(3) .101(12) Uiso ? ? 1.00000 ? ? H5a .6566(19) .3422(8) .3545(18) .045(6) Uiso ? ? 1.00000 ? ? H5b .6981(18) .3075(8) .4487(16) .038(6) Uiso ? ? 1.00000 ? ? H6a .7121(16) .4150(7) .4407(15) .029(5) Uiso ? ? 1.00000 ? ? H6b .8169(18) .3775(7) .4360(15) .031(5) Uiso ? ? 1.00000 ? ? H71a .7708(18) .4610(8) .5679(16) .035(5) Uiso ? ? 1.00000 ? ? H71b .890(2) .4338(9) .5868(18) .050(7) Uiso ? ? 1.00000 ? ? H72a .839(2) .4203(9) .7658(19) .051(7) Uiso ? ? 1.00000 ? ? H72b .719(2) .4474(8) .7431(17) .042(6) Uiso ? ? 1.00000 ? ? H73a .817(3) .5231(15) .706(3) .121(15) Uiso ? ? 1.00000 ? ? H73b .934(3) .4985(11) .725(2) .080(10) Uiso ? ? 1.00000 ? ? H76a .843(4) .4867(17) 1.102(3) .135(17) Uiso ? ? 1.00000 ? ? H76b .782(3) .5382(15) 1.081(3) .113(14) Uiso ? ? 1.00000 ? ? H76c .918(3) .5371(13) 1.084(3) .092(10) Uiso ? ? 1.00000 ? ? H8a .8789(17) .3537(7) .6627(15) .030(5) Uiso ? ? 1.00000 ? ? H8b .8127(16) .3184(7) .5809(15) .024(5) Uiso ? ? 1.00000 ? ? H9a .7498(18) .2938(8) .7441(16) .035(5) Uiso ? ? 1.00000 ? ? H9b .7271(17) .3507(7) .7797(16) .030(5) Uiso ? ? 1.00000 ? ? H112 -.0896(15) .2637(7) .4397(14) .024(5) Uiso ? ? 1.00000 ? ? H113 -.2535(18) .2158(8) .4165(16) .036(6) Uiso ? ? 1.00000 ? ? H114 -.2841(18) .1425(8) .5118(16) .032(5) Uiso ? ? 1.00000 ? ? H115 -.1440(17) .1171(8) .6342(15) .031(5) Uiso ? ? 1.00000 ? ? H116 .0226(17) .1654(7) .6588(16) .032(5) Uiso ? ? 1.00000 ? ? H122 .1698(17) .1669(7) .4788(15) .028(5) Uiso ? ? 1.00000 ? ? H123 .3209(17) .1114(8) .5053(16) .036(6) Uiso ? ? 1.00000 ? ? H124 .4497(18) .1233(8) .6457(16) .037(6) Uiso ? ? 1.00000 ? ? H125 .427(2) .1935(9) .7576(18) .050(7) Uiso ? ? 1.00000 ? ? H126 .2764(16) .2503(7) .7281(15) .026(5) Uiso ? ? 1.00000 ? ? H132 .2466(17) .2477(8) .4039(15) .029(5) Uiso ? ? 1.00000 ? ? H133 .2691(19) .2978(8) .2564(18) .043(6) Uiso ? ? 1.00000 ? ? H134 .1652(17) .3725(7) .2387(16) .030(5) Uiso ? ? 1.00000 ? ? H135 .0381(17) .3975(8) .3729(15) .031(5) Uiso ? ? 1.00000 ? ? H136 .0151(17) .3467(8) .5177(16) .033(5) Uiso ? ? 1.00000 ? ? H142 .2023(16) .3418(7) .6457(15) .027(5) Uiso ? ? 1.00000 ? ? H143 .1768(18) .3927(8) .7894(16) .039(6) Uiso ? ? 1.00000 ? ? H144 .0314(18) .3746(8) .9139(17) .038(6) Uiso ? ? 1.00000 ? ? H145 -.0781(18) .3005(8) .8928(17) .037(6) Uiso ? ? 1.00000 ? ? H146 -.0466(16) .2479(7) .7498(14) .025(5) Uiso ? ? 1.00000 ? ? H42'a .51786 .41413 .31322 .09200 Uiso ? ? .343(5) ? ? H42'b .53158 .43009 .42808 .09200 Uiso ? ? .343(5) ? ? H43'a .33799 .43446 .31430 .06100 Uiso ? ? .343(5) ? ? H43'b .41097 .47928 .34981 .06100 Uiso ? ? .343(5) ? ? 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 N1 .0305(8) .0229(7) .0229(7) .0000(6) .0050(6) .0009(6) C11 .0305(9) .0286(9) .0255(8) -.0029(7) .0059(7) .0016(7) C12 .0302(9) .0289(9) .0245(8) .0011(7) .0069(7) .0003(7) C13 .0362(10) .0332(10) .0340(10) .0071(8) .0022(8) -.0010(8) C14 .0370(10) .0335(10) .0434(11) .0045(8) .0080(9) .0054(8) C15 .0477(13) .0341(11) .0546(13) .0023(9) .0152(10) .0030(9) C16 .082(2) .0366(13) .078(2) -.0005(14) .0231(17) -.0113(13) C2 .0486(12) .0250(9) .0313(9) -.0036(8) .0081(8) -.0048(7) C3 .0512(13) .0386(11) .0312(10) -.0113(9) .0010(9) -.0096(8) N4 .0388(9) .0389(9) .0241(7) -.0011(7) .0040(6) -.0023(6) C41 .0402(12) .0638(15) .0403(12) .0071(11) .0050(10) .0047(11) C42 .0494(15) .087(2) .090(2) .0226(14) .0245(15) .0455(18) C43 .045(2) .061(2) .047(2) .0146(17) .0105(15) .0190(17) C44 .042(2) .057(2) .050(2) .0140(17) .0051(18) .0263(17) C45 .0774(18) .0452(13) .0573(15) .0101(12) .0227(14) .0223(12) C46 .0553(17) .0675(19) .092(2) .0183(15) .0285(16) .0401(18) C5 .0435(11) .0425(11) .0219(8) .0075(9) .0071(8) -.0011(8) C6 .0337(10) .0397(10) .0249(8) .0056(8) .0084(7) .0080(8) N7 .0296(8) .0281(7) .0265(7) .0027(6) .0049(6) .0055(6) C71 .0387(11) .0337(10) .0406(11) -.0061(8) .0059(9) .0061(8) C72 .0408(12) .0379(11) .0466(12) -.0114(9) .0057(10) -.0039(9) C73 .083(2) .0603(18) .0669(18) -.0390(16) .0150(16) -.0176(15) C74 .0692(18) .0600(16) .081(2) -.0316(14) .0173(15) -.0320(15) C75 .0672(18) .0643(17) .085(2) -.0294(14) .0231(15) -.0414(16) C76 .080(2) .099(3) .081(2) -.039(2) .0253(19) -.056(2) C8 .0297(9) .0318(9) .0278(9) .0062(7) .0053(7) .0065(7) C9 .0281(9) .0331(9) .0273(9) .0019(7) .0043(7) .0057(7) B .0222(8) .0243(8) .0198(8) -.0008(7) .0029(6) -.0008(7) C111 .0226(8) .0269(8) .0192(7) .0004(6) .0045(6) -.0038(6) C112 .0251(8) .0262(8) .0213(7) .0012(6) .0032(6) -.0034(6) C113 .0256(9) .0338(9) .0238(8) .0020(7) -.0002(7) -.0054(7) C114 .0268(9) .0342(9) .0270(8) -.0056(7) .0048(7) -.0072(7) C115 .0324(9) .0286(9) .0235(8) -.0038(7) .0076(7) -.0003(7) C116 .0270(8) .0285(8) .0204(7) .0002(7) .0023(6) -.0008(6) C121 .0238(8) .0252(8) .0203(7) -.0010(6) .0045(6) .0033(6) C122 .0278(9) .0291(8) .0230(8) .0011(7) .0021(7) .0002(7) C123 .0330(10) .0282(9) .0324(9) .0032(7) .0079(7) .0014(7) C124 .0296(9) .0360(10) .0364(10) .0074(8) .0029(8) .0085(8) C125 .0284(9) .0418(10) .0290(9) .0011(8) -.0020(7) .0052(8) C126 .0273(9) .0305(9) .0240(8) -.0009(7) .0022(7) .0010(7) C131 .0222(8) .0269(8) .0193(7) -.0034(6) .0003(6) .0001(6) C132 .0262(8) .0262(8) .0235(8) -.0004(7) .0025(6) -.0005(6) C133 .0278(9) .0333(9) .0216(8) -.0025(7) .0048(6) -.0015(7) C134 .0281(9) .0312(9) .0222(8) -.0049(7) .0004(7) .0043(7) C135 .0285(9) .0294(9) .0289(9) .0010(7) .0009(7) .0043(7) C136 .0260(8) .0281(8) .0242(8) .0014(7) .0039(7) .0006(7) C141 .0237(8) .0247(8) .0194(7) .0028(6) -.0002(6) .0005(6) C142 .0283(9) .0307(9) .0221(8) -.0019(7) .0029(7) -.0010(7) C143 .0354(10) .0290(9) .0272(9) -.0033(7) .0004(7) -.0018(7) C144 .0333(9) .0306(9) .0211(8) .0057(7) -.0003(7) -.0028(7) C145 .0278(9) .0326(9) .0197(7) .0050(7) .0018(6) .0040(7) C146 .0263(8) .0263(8) .0211(8) .0003(7) .0009(6) .0020(6) C43' .035(3) .041(3) .034(3) .005(2) -.006(2) .008(2) C44' .026(3) .027(3) .047(4) .002(2) -.005(3) .009(2) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published N1 C11 . . 1.506(2) ? N1 C2 . . 1.506(2) ? N1 C9 . . 1.495(2) ? N1 H1 . . .93(2) ? C11 C12 . . 1.517(3) ? C11 H11a . . 1.00(2) ? C11 H11b . . .98(2) ? C12 C13 . . 1.534(3) ? C12 H12a . . 1.00(2) ? C12 H12b . . .98(2) ? C13 C14 . . 1.471(3) ? C13 H13a . . .99(2) ? C13 H13b . . .98(2) ? C14 C15 . . 1.184(3) ? C15 C16 . . 1.473(4) ? C16 H16a . . .93(4) ? C16 H16b . . .95(4) ? C16 H16c . . .99(3) ? C2 C3 . . 1.519(3) ? C2 H2a . . .99(2) ? C2 H2b . . 1.00(2) ? C3 N4 . . 1.471(3) ? C3 H3a . . .98(2) ? C3 H3b . . 1.00(2) ? N4 C41 . . 1.472(3) ? N4 C5 . . 1.480(3) ? C41 C42 . . 1.513(4) ? C41 H41a . . .99(2) ? C41 H41b . . 1.02(3) ? C42 C43 . . 1.370(5) ? C42 C43' . . 1.440(7) ? C42 H42a . . .946(3) ? C42 H42b . . .964(3) ? C42 H42'a . . .949(3) ? C42 H42'b . . .966(3) ? C43 C43' . . 1.490(7) ? C43 C44 . . 1.465(6) ? C43 C44' . . 1.970(7) ? C43 H42'b . . .947(4) ? C43 H43a . . .963(4) ? C43 H43b . . .968(4) ? C43' C44 . . 1.760(7) ? C43' C44' . . 1.488(9) ? C43' H42a . . 1.006(6) ? C43' H43'a . . .957(6) ? C43' H43'b . . .962(6) ? C44 C44' . . .882(8) ? C44 C45 . . 1.271(5) ? C44' C45 . . 1.161(7) ? C45 C46 . . 1.440(4) ? C46 H46a . . .96(4) ? C46 H46b . . 1.06(5) ? C46 H46c . . .92(4) ? C5 C6 . . 1.525(3) ? C5 H5a . . 1.01(2) ? C5 H5b . . 1.01(2) ? C6 N7 . . 1.477(2) ? C6 H6a . . 1.00(2) ? C6 H6b . . 1.00(2) ? N7 C71 . . 1.469(3) ? N7 C8 . . 1.474(2) ? C71 C72 . . 1.518(3) ? C71 H71a . . .99(2) ? C71 H71b . . 1.02(2) ? C72 C73 . . 1.535(4) ? C72 H72a . . 1.01(2) ? C72 H72b . . .98(2) ? C73 C74 . . 1.473(5) ? C73 H73a . . .97(4) ? C73 H73b . . 1.00(3) ? C74 C75 . . 1.180(5) ? C75 C76 . . 1.474(5) ? C76 H76a . . 1.04(5) ? C76 H76b . . .96(4) ? C76 H76c . . .98(3) ? C8 C9 . . 1.530(3) ? C8 H8a . . 1.01(2) ? C8 H8b . . .98(2) ? C9 H9a . . .97(2) ? C9 H9b . . 1.01(2) ? B C111 . . 1.655(2) ? B C121 . . 1.652(2) ? B C131 . . 1.651(2) ? B C141 . . 1.645(2) ? C111 C112 . . 1.406(2) ? C111 C116 . . 1.409(2) ? C112 C113 . . 1.397(2) ? C112 H112 . . .98(2) ? C113 C114 . . 1.393(3) ? C113 H113 . . .96(2) ? C114 C115 . . 1.388(2) ? C114 H114 . . .99(2) ? C115 C116 . . 1.392(2) ? C115 H115 . . .98(2) ? C116 H116 . . .98(2) ? C121 C122 . . 1.409(2) ? C121 C126 . . 1.404(2) ? C122 C123 . . 1.392(3) ? C122 H122 . . 1.00(2) ? C123 C124 . . 1.390(3) ? C123 H123 . . .99(2) ? C124 C125 . . 1.385(3) ? C124 H124 . . .98(2) ? C125 C126 . . 1.395(3) ? C125 H125 . . .99(2) ? C126 H126 . . 1.01(2) ? C131 C132 . . 1.400(2) ? C131 C136 . . 1.407(2) ? C132 C133 . . 1.397(2) ? C132 H132 . . 1.00(2) ? C133 C134 . . 1.382(3) ? C133 H133 . . .98(2) ? C134 C135 . . 1.389(2) ? C134 H134 . . .96(2) ? C135 C136 . . 1.391(2) ? C135 H135 . . .99(2) ? C136 H136 . . .98(2) ? C141 C142 . . 1.408(2) ? C141 C146 . . 1.406(2) ? C142 C143 . . 1.391(2) ? C142 H142 . . .99(2) ? C143 C144 . . 1.390(3) ? C143 H143 . . .99(2) ? C144 C145 . . 1.381(3) ? C144 H144 . . .99(2) ? C145 C146 . . 1.400(2) ? C145 H145 . . .99(2) ? C146 H146 . . .99(2) ? H42b H42'a . . .65528(4) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published C11 N1 C2 . . . 111.30(14) ? C11 N1 C9 . . . 113.59(13) ? C11 N1 H1 . . . 108.4(12) ? C2 N1 C9 . . . 112.21(14) ? C2 N1 H1 . . . 105.5(13) ? C9 N1 H1 . . . 105.2(12) ? N1 C11 C12 . . . 113.51(14) ? N1 C11 H11a . . . 106.6(12) ? N1 C11 H11b . . . 106.5(12) ? C12 C11 H11a . . . 113.0(12) ? C12 C11 H11b . . . 109.7(12) ? H11a C11 H11b . . . 107.2(17) ? C11 C12 C13 . . . 113.43(15) ? C11 C12 H12a . . . 110.0(11) ? C11 C12 H12b . . . 106.9(12) ? C13 C12 H12a . . . 109.9(11) ? C13 C12 H12b . . . 109.6(12) ? H12a C12 H12b . . . 106.7(17) ? C12 C13 C14 . . . 111.16(16) ? C12 C13 H13a . . . 108.3(14) ? C12 C13 H13b . . . 110.3(12) ? C14 C13 H13a . . . 111.6(14) ? C14 C13 H13b . . . 109.3(12) ? H13a C13 H13b . . . 106.0(19) ? C13 C14 C15 . . . 175.8(2) ? C14 C15 C16 . . . 178.6(3) ? C15 C16 H16a . . . 112(2) ? C15 C16 H16b . . . 110(2) ? C15 C16 H16c . . . 109.7(18) ? H16a C16 H16b . . . 107(3) ? H16a C16 H16c . . . 108(3) ? H16b C16 H16c . . . 110(3) ? N1 C2 C3 . . . 108.27(15) ? N1 C2 H2a . . . 108.7(12) ? N1 C2 H2b . . . 107.8(12) ? C3 C2 H2a . . . 110.8(12) ? C3 C2 H2b . . . 112.5(12) ? H2a C2 H2b . . . 108.6(17) ? C2 C3 N4 . . . 110.65(17) ? C2 C3 H3a . . . 111.7(13) ? C2 C3 H3b . . . 107.4(13) ? N4 C3 H3a . . . 107.7(13) ? N4 C3 H3b . . . 112.2(14) ? H3a C3 H3b . . . 107.2(19) ? C3 N4 C41 . . . 110.31(17) ? C3 N4 C5 . . . 112.49(16) ? C41 N4 C5 . . . 112.76(15) ? N4 C41 C42 . . . 114.4(2) ? N4 C41 H41a . . . 107.4(14) ? N4 C41 H41b . . . 107.4(15) ? C42 C41 H41a . . . 109.1(14) ? C42 C41 H41b . . . 112.0(15) ? H41a C41 H41b . . . 106(2) ? C41 C42 C43 . . . 117.9(3) ? C41 C42 C43' . . . 117.4(3) ? C41 C42 H42a . . . 109.4(3) ? C41 C42 H42b . . . 108.4(3) ? C41 C42 H42'a . . . 108.7(3) ? C41 C42 H42'b . . . 107.4(3) ? C43 C42 C43' . . . 64.0(3) ? C43 C42 H42a . . . 105.9(3) ? C43 C42 H42b . . . 106.3(3) ? C43 C42 H42'a . . . 130.6(3) ? C43 C42 H42'b . . . 43.7(2) ? C43' C42 H42a . . . 44.1(3) ? C43' C42 H42b . . . 132.2(4) ? C43' C42 H42'a . . . 108.4(4) ? C43' C42 H42'b . . . 106.4(4) ? H42a C42 H42b . . . 108.6(3) ? H42a C42 H42'a . . . 71.1(2) ? H42a C42 H42'b . . . 141.1(4) ? H42b C42 H42'a . . . 40.04(12) ? H42b C42 H42'b . . . 70.3(2) ? H42'a C42 H42'b . . . 108.2(3) ? C42 C43 C43' . . . 60.3(3) ? C42 C43 C44 . . . 115.8(3) ? C42 C43 C44' . . . 97.0(3) ? C42 C43 H42'b . . . 44.8(2) ? C42 C43 H43a . . . 108.8(3) ? C42 C43 H43b . . . 107.7(3) ? C43' C43 C44 . . . 73.1(3) ? C43' C43 C44' . . . 48.5(3) ? C43' C43 H42'b . . . 103.9(4) ? C43' C43 H43a . . . 85.1(3) ? C43' C43 H43b . . . 165.9(4) ? C44 C43 C44' . . . 24.6(3) ? C44 C43 H42'b . . . 146.1(4) ? C44 C43 H43a . . . 108.4(3) ? C44 C43 H43b . . . 108.9(3) ? C44' C43 H42'b . . . 138.8(4) ? C44' C43 H43a . . . 102.3(3) ? C44' C43 H43b . . . 132.4(4) ? H42'b C43 H43a . . . 104.9(3) ? H42'b C43 H43b . . . 66.3(2) ? H43a C43 H43b . . . 106.9(4) ? C42 C43' C43 . . . 55.7(3) ? C42 C43' C44 . . . 96.7(4) ? C42 C43' C44' . . . 119.8(5) ? C42 C43' H42a . . . 40.9(3) ? C42 C43' H43'a . . . 106.3(5) ? C42 C43' H43'b . . . 107.3(5) ? C43 C43' C44 . . . 52.8(3) ? C43 C43' C44' . . . 82.8(4) ? C43 C43' H42a . . . 94.8(4) ? C43 C43' H43'a . . . 161.8(6) ? C43 C43' H43'b . . . 82.7(4) ? C44 C43' C44' . . . 30.0(3) ? C44 C43' H42a . . . 135.7(5) ? C44 C43' H43'a . . . 135.5(5) ? C44 C43' H43'b . . . 100.5(4) ? C44' C43' H42a . . . 146.7(6) ? C44' C43' H43'a . . . 106.8(5) ? C44' C43' H43'b . . . 108.2(5) ? H42a C43' H43'a . . . 68.6(4) ? H42a C43' H43'b . . . 104.4(5) ? H43'a C43' H43'b . . . 107.9(6) ? C43 C44 C43' . . . 54.1(3) ? C43 C44 C44' . . . 111.8(6) ? C43 C44 C45 . . . 173.9(4) ? C43' C44 C44' . . . 57.6(5) ? C43' C44 C45 . . . 119.8(4) ? C44' C44 C45 . . . 62.2(5) ? C43 C44' C43' . . . 48.6(3) ? C43 C44' C44 . . . 43.7(4) ? C43 C44' C45 . . . 119.2(5) ? C43' C44' C44 . . . 92.3(6) ? C43' C44' C45 . . . 167.9(6) ? C44 C44' C45 . . . 75.6(6) ? C44 C45 C44' . . . 42.2(4) ? C44 C45 C46 . . . 165.6(3) ? C44' C45 C46 . . . 151.7(4) ? C45 C46 H46a . . . 114(2) ? C45 C46 H46b . . . 113(3) ? C45 C46 H46c . . . 113(2) ? H46a C46 H46b . . . 102(3) ? H46a C46 H46c . . . 111(3) ? H46b C46 H46c . . . 103(3) ? N4 C5 C6 . . . 113.47(16) ? N4 C5 H5a . . . 112.4(13) ? N4 C5 H5b . . . 108.3(12) ? C6 C5 H5a . . . 107.3(13) ? C6 C5 H5b . . . 109.7(12) ? H5a C5 H5b . . . 105.4(18) ? C5 C6 N7 . . . 113.83(15) ? C5 C6 H6a . . . 110.3(11) ? C5 C6 H6b . . . 109.2(12) ? N7 C6 H6a . . . 106.2(11) ? N7 C6 H6b . . . 111.0(12) ? H6a C6 H6b . . . 106.0(16) ? C6 N7 C71 . . . 110.81(15) ? C6 N7 C8 . . . 113.29(14) ? C71 N7 C8 . . . 111.83(14) ? N7 C71 C72 . . . 113.60(17) ? N7 C71 H71a . . . 107.5(12) ? N7 C71 H71b . . . 111.2(13) ? C72 C71 H71a . . . 109.6(12) ? C72 C71 H71b . . . 109.3(13) ? H71a C71 H71b . . . 105.3(18) ? C71 C72 C73 . . . 111.3(2) ? C71 C72 H72a . . . 110.2(14) ? C71 C72 H72b . . . 108.2(13) ? C73 C72 H72a . . . 109.8(14) ? C73 C72 H72b . . . 109.1(13) ? H72a C72 H72b . . . 108(2) ? C72 C73 C74 . . . 111.0(3) ? C72 C73 H73a . . . 111(2) ? C72 C73 H73b . . . 111.2(18) ? C74 C73 H73a . . . 113(2) ? C74 C73 H73b . . . 107.0(18) ? H73a C73 H73b . . . 104(3) ? C73 C74 C75 . . . 176.3(3) ? C74 C75 C76 . . . 178.1(3) ? C75 C76 H76a . . . 113(2) ? C75 C76 H76b . . . 108(2) ? C75 C76 H76c . . . 109(2) ? H76a C76 H76b . . . 105(3) ? H76a C76 H76c . . . 109(3) ? H76b C76 H76c . . . 112(3) ? N7 C8 C9 . . . 109.90(15) ? N7 C8 H8a . . . 111.0(11) ? N7 C8 H8b . . . 108.8(11) ? C9 C8 H8a . . . 107.8(11) ? C9 C8 H8b . . . 110.0(11) ? H8a C8 H8b . . . 109.3(16) ? N1 C9 C8 . . . 109.18(14) ? N1 C9 H9a . . . 107.2(13) ? N1 C9 H9b . . . 107.2(11) ? C8 C9 H9a . . . 111.6(13) ? C8 C9 H9b . . . 110.8(11) ? H9a C9 H9b . . . 110.7(17) ? C111 B C121 . . . 108.19(13) ? C111 B C131 . . . 109.10(13) ? C111 B C141 . . . 109.80(13) ? C121 B C131 . . . 111.50(13) ? C121 B C141 . . . 109.50(13) ? C131 B C141 . . . 108.74(13) ? B C111 C112 . . . 124.22(14) ? B C111 C116 . . . 120.74(14) ? C112 C111 C116 . . . 115.02(15) ? C111 C112 C113 . . . 122.67(15) ? C111 C112 H112 . . . 119.2(11) ? C113 C112 H112 . . . 118.1(11) ? C112 C113 C114 . . . 120.24(16) ? C112 C113 H113 . . . 120.0(13) ? C114 C113 H113 . . . 119.7(13) ? C113 C114 C115 . . . 118.84(16) ? C113 C114 H114 . . . 119.6(12) ? C115 C114 H114 . . . 121.5(12) ? C114 C115 C116 . . . 120.10(16) ? C114 C115 H115 . . . 118.7(11) ? C116 C115 H115 . . . 121.2(11) ? C111 C116 C115 . . . 123.12(15) ? C111 C116 H116 . . . 118.1(12) ? C115 C116 H116 . . . 118.7(12) ? B C121 C122 . . . 121.16(14) ? B C121 C126 . . . 123.82(14) ? C122 C121 C126 . . . 115.00(15) ? C121 C122 C123 . . . 123.06(16) ? C121 C122 H122 . . . 118.8(11) ? C123 C122 H122 . . . 118.1(11) ? C122 C123 C124 . . . 119.92(17) ? C122 C123 H123 . . . 119.5(12) ? C124 C123 H123 . . . 120.5(12) ? C123 C124 C125 . . . 118.95(18) ? C123 C124 H124 . . . 119.9(12) ? C125 C124 H124 . . . 121.2(12) ? C124 C125 C126 . . . 120.38(17) ? C124 C125 H125 . . . 120.7(14) ? C126 C125 H125 . . . 118.9(14) ? C121 C126 C125 . . . 122.70(16) ? C121 C126 H126 . . . 117.7(11) ? C125 C126 H126 . . . 119.6(11) ? B C131 C132 . . . 123.78(14) ? B C131 C136 . . . 121.38(14) ? C132 C131 C136 . . . 114.77(15) ? C131 C132 C133 . . . 122.83(16) ? C131 C132 H132 . . . 118.0(11) ? C133 C132 H132 . . . 119.2(11) ? C132 C133 C134 . . . 120.44(16) ? C132 C133 H133 . . . 118.6(13) ? C134 C133 H133 . . . 121.0(13) ? C133 C134 C135 . . . 118.73(16) ? C133 C134 H134 . . . 119.7(12) ? C135 C134 H134 . . . 121.5(12) ? C134 C135 C136 . . . 120.00(17) ? C134 C135 H135 . . . 120.1(12) ? C136 C135 H135 . . . 119.9(12) ? C131 C136 C135 . . . 123.21(16) ? C131 C136 H136 . . . 119.3(12) ? C135 C136 H136 . . . 117.5(12) ? B C141 C142 . . . 121.23(14) ? B C141 C146 . . . 123.75(14) ? C142 C141 C146 . . . 115.02(15) ? C141 C142 C143 . . . 122.91(16) ? C141 C142 H142 . . . 119.1(11) ? C143 C142 H142 . . . 118.0(11) ? C142 C143 C144 . . . 120.20(17) ? C142 C143 H143 . . . 118.8(12) ? C144 C143 H143 . . . 121.0(12) ? C143 C144 C145 . . . 118.83(16) ? C143 C144 H144 . . . 120.5(12) ? C145 C144 H144 . . . 120.7(12) ? C144 C145 C146 . . . 120.43(16) ? C144 C145 H145 . . . 120.6(12) ? C146 C145 H145 . . . 118.9(12) ? C141 C146 C145 . . . 122.54(15) ? C141 C146 H146 . . . 118.4(11) ? C145 C146 H146 . . . 119.0(11) ? C42 H42a C43' . . . 95.0(4) ? C42 H42b H42'a . . . 68.7(2) ? C42 H42'a H42b . . . 71.22(18) ? C42 H42'b C43 . . . 91.5(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 N1 C12 2.529(2) . . ? N1 C3 2.451(3) . . ? N1 N4 2.721(2) . . ? N1 N7 2.765(2) . . ? N1 C8 2.466(2) . . ? N1 H11a 2.03(2) . . ? N1 H11b 2.02(2) . . ? N1 H2a 2.05(2) . . ? N1 H2b 2.05(2) . . ? N1 H9a 2.01(2) . . ? N1 H9b 2.04(2) . . ? C11 C13 2.551(3) . . ? C11 C2 2.487(3) . . ? C11 C9 2.512(3) . . ? C11 H1 2.01(2) . . ? C11 H12a 2.08(2) . . ? C11 H12b 2.03(2) . . ? C11 H2a 2.48(2) . . ? C11 H9b 2.55(2) . . ? C12 C14 2.479(3) . . ? C12 H1 2.60(2) . . ? C12 H11a 2.12(2) . . ? C12 H11b 2.07(2) . . ? C12 H13a 2.07(2) . . ? C12 H13b 2.09(2) . . ? C13 C15 2.653(3) . . ? C13 H1 2.70(2) . . ? C13 H12a 2.09(2) . . ? C13 H12b 2.08(2) . . ? C14 C16 2.656(4) . . ? C14 H12a 2.68(2) . . ? C14 H12b 2.68(2) . . ? C14 H13a 2.06(2) . . ? C14 H13b 2.02(2) . . ? C15 H16a 2.02(4) . . ? C15 H16b 2.00(4) . . ? C15 H16c 2.03(3) . . ? C2 N4 2.459(2) . . ? C2 C5 2.995(3) . . ? C2 C9 2.491(3) . . ? C2 H1 1.97(2) . . ? C2 H11b 2.50(2) . . ? C2 H3a 2.09(2) . . ? C2 H3b 2.05(2) . . ? C2 H5b 2.60(2) . . ? C2 H9a 2.56(2) . . ? C3 C41 2.415(3) . . ? C3 C5 2.453(3) . . ? C3 H1 2.35(2) . . ? C3 H2a 2.09(2) . . ? C3 H2b 2.11(2) . . ? C3 H41a 2.52(2) . . ? C3 H41b 2.61(3) . . ? C3 H5b 2.40(2) . . ? N4 C42 2.509(4) . . ? N4 C6 2.512(3) . . ? N4 N7 2.947(2) . . ? N4 H1 2.12(2) . . ? N4 H3a 2.00(2) . . ? N4 H3b 2.07(2) . . ? N4 H41a 2.00(2) . . ? N4 H41b 2.02(3) . . ? N4 H42b 2.6455(16) . . ? N4 H42'b 2.4844(17) . . ? N4 H5a 2.08(2) . . ? N4 H5b 2.04(2) . . ? C41 C43 2.472(5) . . ? C41 C43' 2.523(6) . . ? C41 C5 2.458(3) . . ? C41 H3a 2.48(2) . . ? C41 H42a 2.034(3) . . ? C41 H42b 2.035(3) . . ? C41 H42'a 2.028(3) . . ? C41 H42'b 2.025(3) . . ? C41 H43b 2.675(3) . . ? C41 H5a 2.50(2) . . ? C42 C44 2.402(5) . . ? C42 C44' 2.534(7) . . ? C42 H41a 2.06(2) . . ? C42 H41b 2.12(3) . . ? C42 H43a 1.912(3) . . ? C42 H43b 1.903(3) . . ? C42 H43'a 1.941(3) . . ? C42 H43'b 1.955(3) . . ? C43 C43 2.956(6) . '3 666' ? C43 C45 2.732(5) . . ? C43 H41a 2.66(2) . . ? C43 H42a 1.866(4) . . ? C43 H42b 1.884(4) . . ? C43 H42'a 2.114(4) . . ? C43 H43a 2.474(4) . '3 666' ? C43 H43'a 2.418(4) . . ? C43 H43'b 1.668(4) . . ? C43' C45 2.635(6) . . ? C43' H41a 2.56(2) . . ? C43' H42b 2.207(6) . . ? C43' H42'a 1.960(6) . . ? C43' H42'b 1.948(6) . . ? C43' H43a 1.703(6) . . ? C43' H43b 2.441(6) . . ? C43' H73a 2.67(4) . '3 666' ? C44 C46 2.690(5) . . ? C44 H41a 2.68(2) . . ? C44 H42a 2.577(4) . . ? C44 H42'b 2.312(4) . . ? C44 H43a 2.567(4) . '3 666' ? C44 H43a 1.990(4) . . ? C44 H43b 2.001(4) . . ? C44 H43'a 2.533(4) . . ? C44 H43'b 2.154(4) . . ? C44' C46 2.523(8) . . ? C44' H41a 2.68(2) . . ? C44' H42a 2.394(7) . . ? C44' H43a 2.370(6) . . ? C44' H43'a 1.989(7) . . ? C44' H43'b 2.008(7) . . ? C44' H71a 2.50(2) . '3 666' ? C44' H73a 2.66(4) . '3 666' ? C45 H46a 2.03(4) . . ? C45 H46b 2.10(5) . . ? C45 H46c 1.99(4) . . ? C45 H71a 2.60(2) . '3 666' ? C5 N7 2.516(2) . . ? C5 H3b 2.65(2) . . ? C5 H41b 2.68(3) . . ? C5 H42b 2.627(2) . . ? C5 H6a 2.09(2) . . ? C5 H6b 2.08(2) . . ? C5 H8b 2.672(19) . . ? C6 C71 2.425(3) . . ? C6 C8 2.465(3) . . ? C6 H5a 2.06(2) . . ? C6 H5b 2.10(2) . . ? C6 H71a 2.51(2) . . ? C6 H8b 2.42(2) . . ? N7 C72 2.499(3) . . ? N7 C9 2.460(2) . . ? N7 H1 2.21(2) . . ? N7 H6a 2.00(2) . . ? N7 H6b 2.06(2) . . ? N7 H71a 2.00(2) . . ? N7 H71b 2.07(2) . . ? N7 H72b 2.66(2) . . ? N7 H8a 2.06(2) . . ? N7 H8b 2.01(2) . . ? C71 C73 2.521(4) . . ? C71 C8 2.437(3) . . ? C71 H6a 2.49(2) . . ? C71 H72a 2.09(2) . . ? C71 H72b 2.05(2) . . ? C71 H8a 2.43(2) . . ? C72 C74 2.479(4) . . ? C72 C8 2.996(3) . . ? C72 H71a 2.07(2) . . ? C72 H71b 2.09(2) . . ? C72 H73a 2.09(4) . . ? C72 H73b 2.11(3) . . ? C73 C75 2.652(5) . . ? C73 H71a 2.68(2) . . ? C73 H72a 2.10(3) . . ? C73 H72b 2.07(2) . . ? C74 C76 2.654(5) . . ? C74 H72a 2.66(2) . . ? C74 H72b 2.70(2) . . ? C74 H73a 2.05(4) . . ? C74 H73b 2.01(3) . . ? C75 H76a 2.11(4) . . ? C75 H76b 1.99(4) . . ? C75 H76c 2.02(3) . . ? C8 H1 2.44(2) . . ? C8 H2b 2.70(2) . . ? C8 H6b 2.69(2) . . ? C8 H71b 2.68(2) . . ? C8 H9a 2.09(2) . . ? C8 H9b 2.11(2) . . ? C9 H1 1.96(2) . . ? C9 H11a 2.64(2) . . ? C9 H2b 2.44(2) . . ? C9 H8a 2.07(2) . . ? C9 H8b 2.078(19) . . ? B C112 2.709(2) . . ? B C116 2.666(3) . . ? B C122 2.669(3) . . ? B C126 2.698(3) . . ? B C132 2.694(2) . . ? B C136 2.670(2) . . ? B C142 2.663(3) . . ? B C146 2.694(2) . . ? B H112 2.863(18) . . ? B H116 2.77(2) . . ? B H122 2.80(2) . . ? B H126 2.832(19) . . ? B H132 2.83(2) . . ? B H136 2.80(2) . . ? B H142 2.79(2) . . ? B H146 2.835(19) . . ? C111 C113 2.460(2) . . ? C111 C114 2.858(2) . . ? C111 C115 2.462(2) . . ? C111 C121 2.679(2) . . ? C111 C131 2.694(2) . . ? C111 C141 2.701(2) . . ? C111 H112 2.071(19) . . ? C111 H116 2.06(2) . . ? C111 H146 2.666(19) . . ? C112 C114 2.419(2) . . ? C112 C115 2.766(2) . . ? C112 C116 2.374(2) . . ? C112 H113 2.05(2) . . ? C113 C115 2.394(2) . . ? C113 C116 2.758(2) . . ? C113 H112 2.052(19) . . ? C113 H114 2.07(2) . . ? C114 C116 2.409(2) . . ? C114 H113 2.05(2) . . ? C114 H115 2.05(2) . . ? C115 H114 2.08(2) . . ? C115 H116 2.05(2) . . ? C116 H115 2.08(2) . . ? C116 H146 2.66(2) . . ? C121 C123 2.462(2) . . ? C121 C124 2.854(3) . . ? C121 C125 2.456(2) . . ? C121 C131 2.730(2) . . ? C121 C141 2.693(2) . . ? C121 H116 2.69(2) . . ? C121 H122 2.08(2) . . ? C121 H126 2.072(19) . . ? C121 H132 2.70(2) . . ? C122 C124 2.408(3) . . ? C122 C125 2.755(3) . . ? C122 C126 2.372(2) . . ? C122 H123 2.07(2) . . ? C122 H132 2.64(2) . . ? C123 C125 2.391(3) . . ? C123 C126 2.764(3) . . ? C123 H122 2.06(2) . . ? C123 H124 2.06(2) . . ? C124 C126 2.412(3) . . ? C124 H123 2.07(2) . . ? C124 H125 2.08(2) . . ? C125 H124 2.07(2) . . ? C125 H126 2.08(2) . . ? C126 H125 2.07(2) . . ? C131 C133 2.456(2) . . ? C131 C134 2.857(2) . . ? C131 C135 2.462(2) . . ? C131 C141 2.679(2) . . ? C131 H112 2.672(18) . . ? C131 H132 2.06(2) . . ? C131 H136 2.07(2) . . ? C132 C134 2.413(2) . . ? C132 C135 2.758(2) . . ? C132 C136 2.365(2) . . ? C132 H133 2.06(2) . . ? C133 C135 2.385(3) . . ? C133 C136 2.750(2) . . ? C133 H132 2.07(2) . . ? C133 H134 2.04(2) . . ? C134 C136 2.408(2) . . ? C134 H133 2.07(2) . . ? C134 H135 2.07(2) . . ? C135 H134 2.06(2) . . ? C135 H136 2.03(2) . . ? C136 H112 2.688(19) . . ? C136 H135 2.07(2) . . ? C141 C143 2.459(2) . . ? C141 C144 2.855(2) . . ? C141 C145 2.460(2) . . ? C141 H126 2.596(19) . . ? C141 H142 2.07(2) . . ? C141 H146 2.068(19) . . ? C142 C144 2.411(2) . . ? C142 C145 2.756(2) . . ? C142 C146 2.373(2) . . ? C142 H143 2.06(2) . . ? C143 C145 2.386(3) . . ? C143 C146 2.761(3) . . ? C143 H142 2.05(2) . . ? C143 H144 2.08(2) . . ? C144 C146 2.414(2) . . ? C144 H143 2.08(2) . . ? C144 H145 2.07(2) . . ? C145 H3b 2.66(2) . '4 455' ? C145 H144 2.07(2) . . ? C145 H146 2.07(2) . . ? C146 H145 2.07(2) . . ? H1 H11b 2.36(3) . . ? H1 H13b 2.16(3) . . ? H1 H9b 2.37(3) . . ? H11a H11b 1.60(3) . . ? H11a H12b 2.35(3) . . ? H11b H12b 2.37(3) . . ? H11b H2a 2.35(3) . . ? H12a H12b 1.59(3) . . ? H12a H9b 2.14(3) . . ? H12b H13a 2.39(3) . . ? H13a H13b 1.58(3) . . ? H16a H16b 1.51(5) . . ? H16a H16c 1.56(5) . . ? H16b H16c 1.58(5) . . ? H2a H2b 1.62(3) . . ? H2a H3a 2.33(3) . . ? H2b H3b 2.33(3) . . ? H2b H5b 2.15(3) . . ? H2b H8b 2.21(3) . . ? H2b H9a 2.34(3) . . ? H3a H3b 1.59(3) . . ? H3a H41a 2.19(3) . . ? H3b H5b 2.40(3) . . ? H3b H145 2.36(3) . '4 554' ? H41a H41b 1.60(4) . . ? H41a H42a 2.39(2) . . ? H41b H42a 2.33(3) . . ? H41b H42'a 2.24(3) . . ? H42a H42b 1.55133(13) . . ? H42a H42'a 1.10176(9) . . ? H42a H42'b 1.80327(10) . . ? H42a H43a 2.13380(15) . . ? H42a H43'a 1.10685(9) . . ? H42a H43'b 1.55502(16) . . ? H42b H42'b 1.11213(7) . . ? H42b H43a 2.13940(17) . . ? H42b H43b 2.13712(14) . . ? H42b H5a 2.34(2) . . ? H42b H6a 2.17(2) . . ? H42'a H42'b 1.55145(11) . . ? H42'a H43a 2.32340(18) . . ? H42'a H43'a 2.18594(17) . . ? H42'a H43'b 2.21427(17) . . ? H42'b H43a 1.51380(15) . . ? H42'b H43b 1.04765(7) . . ? H42'b H43'b 2.18671(12) . . ? H42'b H6a 2.17(2) . . ? H43a H43a 2.31480(16) . '3 666' ? H43a H43b 1.55134(9) . . ? H43a H43b 2.19066(19) . '3 666' ? H43a H43'b 1.28582(7) . . ? H43'a H43'b 1.55137(11) . . ? H43'a H73a 2.17(4) . '3 666' ? H46a H46b 1.58(6) . . ? H46a H46c 1.56(6) . . ? H46b H46c 1.55(6) . . ? H5a H5b 1.61(3) . . ? H5a H6a 2.35(3) . . ? H5a H6b 2.36(3) . . ? H5b H6b 2.36(3) . . ? H5b H8b 2.19(3) . . ? H6a H6b 1.60(3) . . ? H6a H71a 2.17(3) . . ? H71a H71b 1.60(3) . . ? H71a H72b 2.37(3) . . ? H71b H8a 2.38(3) . . ? H72a H72b 1.61(3) . . ? H72a H8a 2.29(3) . . ? H72a H9b 2.30(3) . . ? H72b H73a 2.40(5) . . ? H73a H73b 1.55(5) . . ? H76a H76b 1.59(6) . . ? H76a H76c 1.64(6) . . ? H76b H76c 1.61(5) . . ? H8a H8b 1.62(3) . . ? H8a H9b 2.35(3) . . ? H8b H9a 2.33(3) . . ? H9a H9b 1.63(3) . . ? H9a H132 2.35(3) . 4 ? H112 H113 2.34(3) . . ? H113 H114 2.36(3) . . ? H114 H115 2.38(3) . . ? H115 H116 2.37(3) . . ? H122 H123 2.35(3) . . ? H123 H124 2.38(3) . . ? H124 H125 2.40(3) . . ? H125 H126 2.37(3) . . ? H132 H133 2.35(3) . . ? H133 H134 2.37(3) . . ? H134 H135 2.39(3) . . ? H135 H136 2.34(3) . . ? H142 H143 2.33(3) . . ? H144 H145 2.39(3) . . ? H145 H146 2.36(3) . . ? _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 1496 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 36 _reflns_limit_l_min -17 _reflns_limit_l_max 17 _reflns_number_observed ? _reflns_d_resolution_high .73 _reflns_d_resolution_low 11.617 _diffrn_reflns_av_sigmaI/netI .087 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150 _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 .078 _refine_ls_wR_factor_all .086 _refine_ls_goodness_of_fit_all 1.213 _refine_ls_shift/su_mean .007 #========================================================================== # 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_dbmol # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C45 H51 Mo1 N3 O4' _chemical_formula_moiety ? _chemical_formula_weight 793.86 _chemical_melting_point ? _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M I_b_a_2 _symmetry_space_group_name_Hall i_2_-2c loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,+z -x,+y,1/2+z +x,-y,1/2+z 1/2+x,1/2+y,1/2+z 1/2-x,1/2-y,1/2+z 1/2-x,1/2+y,+z 1/2+x,1/2-y,+z _cell_length_a 25.283(5) _cell_length_b 14.986(3) _cell_length_c 21.337(4) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 8084(3) _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 1.304 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 7736 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu .37 _exptl_crystal_description prism _exptl_crystal_size_max .45 _exptl_crystal_size_mid .3 _exptl_crystal_size_min .15 _exptl_crystal_size_rad ? _exptl_crystal_colour ? _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 .824 _exptl_absorpt_correction_T_max .901 _diffrn_reflns_number 46794 _reflns_number_total 5249 _reflns_Friedel_coverage .968 _reflns_number_gt 5249 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.17 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .048 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _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 .037 _refine_ls_wR_factor_ref .045 _refine_ls_goodness_of_fit_ref 1.548 _refine_ls_number_reflns 4249 _refine_ls_number_parameters 497 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .05 _refine_diff_density_min -.705 _refine_diff_density_max 1.099 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack xabs refined' _refine_ls_abs_structure_Flack -.02(5) # 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 ? 0 360 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 408 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Mo ? 0 8 -1.825 .688 '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 32 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Mo .747549(13) -.020570(19) .00000 .02169(14) Uani ? ? 1.00000 ? ? N1 .79254(19) -.1351(3) -.0526(2) .027(2) Uani ? ? 1.00000 ? ? C11 .8366(2) -.1061(4) -.0936(3) .030(3) Uani ? ? 1.00000 ? ? C12 .8849(2) -.0705(4) -.0586(3) .038(3) Uani ? ? 1.00000 ? ? C13 .9283(2) -.0418(5) -.1049(4) .051(4) Uani ? ? 1.00000 ? ? C14 .9161(2) .0407(5) -.1394(3) .045(4) Uani ? ? 1.00000 ? ? C15 .9068(3) .1084(5) -.1670(3) .047(4) Uani ? ? 1.00000 ? ? C151 .8955(3) .1876(5) -.2024(4) .041(4) Uani ? ? 1.00000 ? ? C152 .8443(4) .2118(6) -.2181(4) .044(4) Uani ? ? 1.00000 ? ? C153 .8351(4) .2854(6) -.2559(4) .050(5) Uani ? ? 1.00000 ? ? C154 .8765(4) .3356(7) -.2773(4) .057(6) Uani ? ? 1.00000 ? ? C155 .9272(3) .3153(6) -.2608(4) .056(5) Uani ? ? 1.00000 ? ? C156 .9370(3) .2415(5) -.2240(4) .049(4) Uani ? ? 1.00000 ? ? C2 .8113(2) -.2056(3) -.0079(3) .030(3) Uani ? ? 1.00000 ? ? C3 .8134(2) -.1704(4) .0586(3) .032(3) Uani ? ? 1.00000 ? ? N4 .76193(18) -.1279(3) .0781(2) .027(2) Uani ? ? 1.00000 ? ? C41 .7710(2) -.0905(4) .1425(2) .031(3) Uani ? ? 1.00000 ? ? C42 .7229(2) -.0466(4) .1715(3) .036(3) Uani ? ? 1.00000 ? ? C43 .7368(3) -.0088(5) .2372(2) .040(4) Uani ? ? 1.00000 ? ? C44 .7753(3) .0646(4) .2339(3) .038(3) Uani ? ? 1.00000 ? ? C45 .8056(3) .1250(4) .2308(3) .040(3) Uani ? ? 1.00000 ? ? C451 .8419(3) .1985(6) .2306(4) .038(4) Uani ? ? 1.00000 ? ? C452 .8344(4) .2707(5) .2706(4) .041(4) Uani ? ? 1.00000 ? ? C453 .8706(4) .3399(6) .2742(4) .044(4) Uani ? ? 1.00000 ? ? C454 .9145(3) .3398(6) .2366(4) .058(5) Uani ? ? 1.00000 ? ? C455 .9215(4) .2732(8) .1933(5) .091(7) Uani ? ? 1.00000 ? ? C456 .8857(4) .2039(7) .1903(5) .080(7) Uani ? ? 1.00000 ? ? C5 .7190(3) -.1967(4) .0795(3) .030(3) Uani ? ? 1.00000 ? ? C6 .6700(2) -.1642(4) .0465(3) .030(3) Uani ? ? 1.00000 ? ? N7 .68099(17) -.1283(3) -.0184(2) .026(2) Uani ? ? 1.00000 ? ? C71 .6303(2) -.0913(4) -.0424(3) .033(3) Uani ? ? 1.00000 ? ? C72 .6309(2) -.0544(4) -.1088(3) .035(3) Uani ? ? 1.00000 ? ? C73 .5768(2) -.0184(5) -.1263(3) .041(3) Uani ? ? 1.00000 ? ? C74 .5620(2) .0612(4) -.0906(3) .042(3) Uani ? ? 1.00000 ? ? C75 .5491(2) .1250(5) -.0611(3) .044(4) Uani ? ? 1.00000 ? ? C751 .5305(3) .2004(5) -.0238(4) .047(4) Uani ? ? 1.00000 ? ? C752 .5518(3) .2192(5) .0359(4) .049(4) Uani ? ? 1.00000 ? ? C753 .5313(3) .2878(5) .0709(4) .061(5) Uani ? ? 1.00000 ? ? C754 .4910(4) .3395(6) .0482(5) .074(6) Uani ? ? 1.00000 ? ? C755 .4698(3) .3238(5) -.0100(5) .064(5) Uani ? ? 1.00000 ? ? C756 .4895(3) .2544(5) -.0464(4) .056(4) Uani ? ? 1.00000 ? ? C8 .7012(3) -.2009(4) -.0600(3) .030(3) Uani ? ? 1.00000 ? ? C9 .7505(2) -.1724(4) -.0949(2) .027(2) Uani ? ? 1.00000 ? ? C01 .6993(2) .0612(3) .0395(2) .027(3) Uani ? ? 1.00000 ? ? O01 .66872(16) .1107(2) .06264(18) .036(2) Uani ? ? 1.00000 ? ? C02 .7438(2) .0573(3) -.0724(2) .028(2) Uani ? ? 1.00000 ? ? O02 .74312(17) .1059(2) -.11507(17) .037(2) Uani ? ? 1.00000 ? ? C03 .8034(2) .0577(3) .0281(2) .028(3) Uani ? ? 1.00000 ? ? O03 .83631(17) .1074(3) .0458(2) .044(2) Uani ? ? 1.00000 ? ? O10 .50000 .00000 .1857(3) .058(4) Uani ? ? 1.00000 ? ? C10 .50000 .00000 .1293(5) .043(5) Uani ? ? 1.00000 ? ? C101 .5479(3) -.0272(6) .0928(4) .065(5) Uani ? ? 1.00000 ? ? O20 .9999(6) -.0814(11) .1837(12) .131(14) Uani ? ? .50000 ? ? C20 .9693(7) -.0212(11) .1932(9) .069(10) Uani ? ? .50000 ? ? C201 .9149(6) -.0299(10) .1769(9) .064(10) Uani ? ? .50000 ? ? C202 .9854(9) .0556(13) .2328(10) .078(13) Uani ? ? .50000 ? ? H11a .84719 -.15460 -.11912 .03800 Uiso ? ? 1.00000 ? ? H11b .82406 -.05873 -.12002 .03800 Uiso ? ? 1.00000 ? ? H12a .87566 -.02159 -.03360 .04900 Uiso ? ? 1.00000 ? ? H12b .89874 -.11750 -.03257 .04900 Uiso ? ? 1.00000 ? ? H13a .96119 -.03329 -.08340 .06300 Uiso ? ? 1.00000 ? ? H13b .93402 -.08891 -.13559 .06300 Uiso ? ? 1.00000 ? ? H152 .81567 .17800 -.20264 .05900 Uiso ? ? 1.00000 ? ? H153 .79896 .30130 -.26734 .06900 Uiso ? ? 1.00000 ? ? H154 .87062 .38843 -.30441 .07600 Uiso ? ? 1.00000 ? ? H155 .95663 .35015 -.27663 .07400 Uiso ? ? 1.00000 ? ? H156 .97278 .22721 -.21215 .06400 Uiso ? ? 1.00000 ? ? H2a .78797 -.25564 -.00992 .03900 Uiso ? ? 1.00000 ? ? H2b .84605 -.22575 -.02041 .03900 Uiso ? ? 1.00000 ? ? H3a .82149 -.21779 .08664 .04300 Uiso ? ? 1.00000 ? ? H3b .84091 -.12645 .06133 .04300 Uiso ? ? 1.00000 ? ? H41a .78264 -.13746 .16900 .04200 Uiso ? ? 1.00000 ? ? H41b .79887 -.04694 .13944 .04200 Uiso ? ? 1.00000 ? ? H42a .71076 .00178 .14515 .04800 Uiso ? ? 1.00000 ? ? H42b .69456 -.08872 .17477 .04800 Uiso ? ? 1.00000 ? ? H43a .70389 .01415 .25598 .05700 Uiso ? ? 1.00000 ? ? H43b .74884 -.05566 .26270 .05700 Uiso ? ? 1.00000 ? ? H452 .80346 .27291 .29485 .05000 Uiso ? ? 1.00000 ? ? H453 .86576 .38733 .30205 .05500 Uiso ? ? 1.00000 ? ? H454 .94091 .38624 .24098 .07500 Uiso ? ? 1.00000 ? ? H455 .95188 .27565 .16442 .10900 Uiso ? ? 1.00000 ? ? H456 .89295 .15413 .16197 .09800 Uiso ? ? 1.00000 ? ? H5a .73028 -.24957 .05796 .03700 Uiso ? ? 1.00000 ? ? H5b .70974 -.21045 .12072 .03700 Uiso ? ? 1.00000 ? ? H6a .64532 -.21234 .04222 .04200 Uiso ? ? 1.00000 ? ? H6b .65417 -.11817 .07054 .04200 Uiso ? ? 1.00000 ? ? H71a .60445 -.13811 -.04088 .04400 Uiso ? ? 1.00000 ? ? H71b .61936 -.04456 -.01525 .04400 Uiso ? ? 1.00000 ? ? H72a .65663 -.00853 -.11204 .04600 Uiso ? ? 1.00000 ? ? H72b .64026 -.10146 -.13754 .04600 Uiso ? ? 1.00000 ? ? H73a .57678 -.00286 -.17021 .04800 Uiso ? ? 1.00000 ? ? H73b .55084 -.06283 -.11954 .04800 Uiso ? ? 1.00000 ? ? H752 .58038 .18387 .05097 .06300 Uiso ? ? 1.00000 ? ? H753 .54533 .29944 .11129 .07600 Uiso ? ? 1.00000 ? ? H754 .47827 .38737 .07428 .09600 Uiso ? ? 1.00000 ? ? H755 .44162 .35977 -.02522 .08200 Uiso ? ? 1.00000 ? ? H756 .47546 .24391 -.08828 .07300 Uiso ? ? 1.00000 ? ? H8a .70905 -.25236 -.03480 .04000 Uiso ? ? 1.00000 ? ? H8b .67406 -.21786 -.08939 .04000 Uiso ? ? 1.00000 ? ? H9a .74059 -.12880 -.12535 .03800 Uiso ? ? 1.00000 ? ? H9b .76443 -.22342 -.11687 .03800 Uiso ? ? 1.00000 ? ? H101a .55675 .01342 .05780 .10300 Uiso ? ? 1.00000 ? ? H101b .54742 -.08579 .07535 .10300 Uiso ? ? 1.00000 ? ? H101c .57864 -.02065 .11716 .10300 Uiso ? ? 1.00000 ? ? H201a .90269 -.08815 .18315 .10000 Uiso ? ? .50000 ? ? H201b .89420 .01178 .19926 .10000 Uiso ? ? .50000 ? ? H201c .90928 -.01520 .13237 .10000 Uiso ? ? .50000 ? ? H202a .96193 .10367 .23057 .11200 Uiso ? ? .50000 ? ? H202b 1.02108 .07921 .22173 .11200 Uiso ? ? .50000 ? ? H202c .98826 .03318 .27520 .11200 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 Mo .03116(16) .01419(14) .01972(13) -.00049(15) -.0000(3) .0006(3) N1 .036(2) .020(2) .025(2) .0023(19) -.003(2) -.0010(18) C11 .035(3) .025(3) .030(3) .000(2) .004(2) -.003(2) C12 .036(3) .033(3) .044(3) .003(2) -.004(2) -.003(3) C13 .032(3) .041(4) .079(5) .000(3) .006(3) .003(3) C14 .034(3) .047(4) .055(4) -.009(3) .003(3) .003(3) C15 .043(3) .054(4) .045(4) -.008(3) .002(3) -.001(3) C151 .045(4) .039(4) .039(4) -.001(3) .002(3) -.002(3) C152 .046(4) .035(4) .051(5) -.008(3) .002(3) -.017(3) C153 .051(4) .046(5) .055(5) .004(4) -.013(4) -.014(4) C154 .083(7) .053(6) .035(4) .006(5) .002(4) -.002(4) C155 .059(5) .064(5) .045(4) -.003(4) .009(3) .012(4) C156 .049(4) .050(4) .048(4) -.002(3) .005(3) .002(3) C2 .041(2) .019(2) .030(4) .0046(17) -.001(3) -.002(2) C3 .045(3) .022(3) .029(3) .006(2) -.005(2) .003(2) N4 .044(3) .018(2) .020(2) -.0027(19) -.0032(18) .0017(17) C41 .046(3) .027(3) .022(2) .002(2) -.003(2) .002(2) C42 .046(3) .038(3) .023(3) -.001(2) .000(2) .000(2) C43 .069(4) .029(3) .021(4) .001(3) .001(2) .001(3) C44 .053(3) .036(3) .026(3) .006(3) -.002(2) -.005(3) C45 .051(3) .041(3) .029(3) .011(3) -.002(2) -.007(3) C451 .042(4) .039(4) .034(4) .002(3) -.003(3) -.006(3) C452 .052(4) .038(4) .032(3) .001(3) .013(3) .005(3) C453 .061(5) .037(4) .034(4) .002(4) .007(4) -.001(3) C454 .053(4) .063(5) .057(5) -.015(4) .001(3) -.012(4) C455 .060(5) .114(9) .099(8) -.029(5) .039(5) -.050(7) C456 .067(6) .086(7) .086(7) -.021(5) .024(5) -.056(6) C5 .047(4) .017(3) .026(3) -.004(3) .002(3) .002(2) C6 .043(3) .021(3) .027(3) -.012(2) .006(2) .002(2) N7 .037(2) .019(2) .024(2) -.0016(17) .0028(16) -.0002(15) C71 .034(3) .035(3) .031(3) -.010(2) .004(2) -.002(2) C72 .039(3) .036(3) .031(3) -.005(2) -.002(2) .003(2) C73 .032(3) .055(4) .035(3) -.006(3) -.007(2) .006(3) C74 .035(3) .043(4) .047(4) -.002(3) -.003(3) .012(3) C75 .032(3) .051(4) .050(4) -.004(3) -.002(3) .019(3) C751 .037(4) .036(3) .067(4) -.005(3) .007(3) .021(3) C752 .046(4) .046(4) .056(5) .004(3) .012(3) .016(3) C753 .064(5) .057(5) .061(5) .010(4) .022(4) .010(4) C754 .084(6) .053(5) .085(6) .022(4) .041(5) .020(5) C755 .050(4) .055(4) .086(8) .018(3) .012(4) .033(5) C756 .050(4) .044(4) .074(5) .000(4) .001(3) .022(4) C8 .041(3) .022(3) .026(3) -.006(3) .001(2) -.008(2) C9 .038(3) .019(2) .024(2) .000(2) .003(2) -.0061(19) C01 .035(3) .020(2) .025(2) -.001(2) -.000(2) .005(2) O01 .047(2) .0216(19) .038(2) .0068(16) .0079(18) .0012(16) C02 .041(3) .018(2) .026(2) -.003(2) .000(2) -.0055(18) O02 .064(3) .0222(18) .0251(17) -.0047(18) -.0048(18) .0069(14) C03 .031(3) .022(2) .031(3) .005(2) -.002(2) .004(2) O03 .049(2) .024(2) .059(3) -.0072(18) -.012(2) -.006(2) O10 .066(4) .063(4) .046(4) .021(4) .00000 .00000 C10 .048(5) .036(5) .046(5) -.005(4) .00000 .00000 C101 .068(5) .063(5) .065(5) .006(4) .027(4) -.001(4) O20 .056(8) .116(13) .22(2) .010(9) -.014(11) -.047(15) C20 .077(10) .051(9) .079(11) .020(8) -.035(9) -.016(9) C201 .061(9) .050(9) .083(12) .011(7) -.006(8) .000(8) C202 .096(15) .068(11) .070(12) -.013(11) -.016(10) -.015(10) # 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 Mo N1 . . 2.344(5) ? Mo N4 . . 2.344(4) ? Mo N7 . . 2.364(4) ? Mo C01 . . 1.924(5) ? Mo C02 . . 1.938(5) ? Mo C03 . . 1.930(5) ? N1 C11 . . 1.482(7) ? N1 C2 . . 1.500(7) ? N1 C9 . . 1.504(7) ? C11 C12 . . 1.528(8) ? C11 H11a . . .946(5) ? C11 H11b . . .961(5) ? C12 C13 . . 1.539(9) ? C12 H12a . . .935(6) ? C12 H12b . . .964(6) ? C13 C14 . . 1.473(10) ? C13 H13a . . .957(7) ? C13 H13b . . .974(8) ? C14 C15 . . 1.196(10) ? C15 C151 . . 1.435(11) ? C151 C152 . . 1.385(12) ? C151 C156 . . 1.403(11) ? C152 C153 . . 1.386(13) ? C152 H152 . . .943(9) ? C153 C154 . . 1.367(14) ? C153 H153 . . .976(10) ? C154 C155 . . 1.363(14) ? C154 H154 . . .991(10) ? C155 C156 . . 1.380(11) ? C155 H155 . . .970(8) ? C156 H156 . . .964(8) ? C2 C3 . . 1.515(9) ? C2 H2a . . .954(5) ? C2 H2b . . .967(5) ? C3 N4 . . 1.508(8) ? C3 H3a . . .951(6) ? C3 H3b . . .959(6) ? N4 C41 . . 1.502(7) ? N4 C5 . . 1.497(8) ? C41 C42 . . 1.513(8) ? C41 H41a . . .949(5) ? C41 H41b . . .964(6) ? C42 C43 . . 1.551(8) ? C42 H42a . . .969(6) ? C42 H42b . . .958(6) ? C43 C44 . . 1.471(9) ? C43 H43a . . .987(6) ? C43 H43b . . .939(6) ? C44 C45 . . 1.187(9) ? C45 C451 . . 1.434(11) ? C451 C452 . . 1.390(11) ? C451 C456 . . 1.405(14) ? C452 C453 . . 1.385(12) ? C452 H452 . . .940(9) ? C453 C454 . . 1.368(12) ? C453 H453 . . .935(8) ? C454 C455 . . 1.372(14) ? C454 H454 . . .969(8) ? C455 C456 . . 1.378(15) ? C455 H455 . . .986(10) ? C456 H456 . . .977(11) ? C5 C6 . . 1.506(8) ? C5 H5a . . .959(6) ? C5 H5b . . .934(6) ? C6 N7 . . 1.512(7) ? C6 H6a . . .959(6) ? C6 H6b . . .948(5) ? N7 C71 . . 1.488(7) ? N7 C8 . . 1.495(7) ? C71 C72 . . 1.521(8) ? C71 H71a . . .958(6) ? C71 H71b . . .950(6) ? C72 C73 . . 1.516(8) ? C72 H72a . . .949(6) ? C72 H72b . . .965(6) ? C73 C74 . . 1.464(9) ? C73 H73a . . .965(6) ? C73 H73b . . .947(6) ? C74 C75 . . 1.189(10) ? C75 C751 . . 1.461(10) ? C751 C752 . . 1.412(11) ? C751 C756 . . 1.401(10) ? C752 C753 . . 1.371(11) ? C752 H752 . . .953(7) ? C753 C754 . . 1.368(12) ? C753 H753 . . .949(8) ? C754 C755 . . 1.372(14) ? C754 H754 . . .964(9) ? C755 C756 . . 1.389(12) ? C755 H755 . . .951(8) ? C756 H756 . . .974(9) ? C8 C9 . . 1.512(8) ? C8 H8a . . .961(6) ? C8 H8b . . .964(6) ? C9 H9a . . .954(5) ? C9 H9b . . .964(5) ? C01 O01 . . 1.180(6) ? C02 O02 . . 1.167(6) ? C03 O03 . . 1.180(7) ? O10 C10 . . 1.203(12) ? C10 C101 . . 1.497(10) ? C10 C101 . '2 655' 1.497(10) ? C101 H101a . . .989(9) ? C101 H101b . . .954(8) ? C101 H101c . . .939(9) ? O20 C20 . . 1.21(2) ? O20 C20 . '2 755' 1.74(2) ? O20 C202 . '2 755' 1.18(3) ? O20 H202a . '2 755' 1.43(2) ? O20 H202b . '2 755' .97(2) ? C20 C201 . . 1.42(2) ? C20 C202 . . 1.49(3) ? C20 C20 . '2 755' 1.68(2) ? C20 C202 . '2 755' 1.51(3) ? C20 H202b . '2 755' 1.090(17) ? C201 H201a . . .935(15) ? C201 H201b . . .945(16) ? C201 H201c . . .985(19) ? C202 H202a . . .93(2) ? C202 H202b . . 1.00(2) ? C202 H202c . . .97(2) ? C202 C202 . '2 755' 1.82(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 N1 Mo N4 . . . 76.26(15) ? N1 Mo N7 . . . 76.49(15) ? N1 Mo C01 . . . 169.6(2) ? N1 Mo C02 . . . 94.74(18) ? N1 Mo C03 . . . 103.8(2) ? N4 Mo N7 . . . 76.11(15) ? N4 Mo C01 . . . 102.97(19) ? N4 Mo C02 . . . 170.75(19) ? N4 Mo C03 . . . 94.7(2) ? N7 Mo C01 . . . 93.18(18) ? N7 Mo C02 . . . 104.12(18) ? N7 Mo C03 . . . 170.57(19) ? C01 Mo C02 . . . 86.3(2) ? C01 Mo C03 . . . 86.6(2) ? C02 Mo C03 . . . 85.3(2) ? Mo N1 C11 . . . 115.7(3) ? Mo N1 C2 . . . 111.4(3) ? Mo N1 C9 . . . 102.5(3) ? C11 N1 C2 . . . 110.1(4) ? C11 N1 C9 . . . 106.6(4) ? C2 N1 C9 . . . 110.1(4) ? N1 C11 C12 . . . 114.4(5) ? N1 C11 H11a . . . 109.2(5) ? N1 C11 H11b . . . 108.3(5) ? C12 C11 H11a . . . 108.9(5) ? C12 C11 H11b . . . 106.9(5) ? H11a C11 H11b . . . 108.9(5) ? C11 C12 C13 . . . 110.8(5) ? C11 C12 H12a . . . 110.7(5) ? C11 C12 H12b . . . 108.4(5) ? C13 C12 H12a . . . 109.0(5) ? C13 C12 H12b . . . 108.3(5) ? H12a C12 H12b . . . 109.6(6) ? C12 C13 C14 . . . 113.9(5) ? C12 C13 H13a . . . 110.5(7) ? C12 C13 H13b . . . 109.6(6) ? C14 C13 H13a . . . 108.1(6) ? C14 C13 H13b . . . 107.7(7) ? H13a C13 H13b . . . 106.9(6) ? C13 C14 C15 . . . 179.0(7) ? C14 C15 C151 . . . 177.8(8) ? C15 C151 C152 . . . 122.0(7) ? C15 C151 C156 . . . 120.0(7) ? C152 C151 C156 . . . 117.9(7) ? C151 C152 C153 . . . 120.4(8) ? C151 C152 H152 . . . 119.4(8) ? C153 C152 H152 . . . 120.2(9) ? C152 C153 C154 . . . 120.3(9) ? C152 C153 H153 . . . 119.8(9) ? C154 C153 H153 . . . 119.9(9) ? C153 C154 C155 . . . 120.7(9) ? C153 C154 H154 . . . 121.3(10) ? C155 C154 H154 . . . 118.0(10) ? C154 C155 C156 . . . 119.7(8) ? C154 C155 H155 . . . 120.8(9) ? C156 C155 H155 . . . 119.4(8) ? C151 C156 C155 . . . 121.0(7) ? C151 C156 H156 . . . 119.2(7) ? C155 C156 H156 . . . 119.8(7) ? N1 C2 C3 . . . 111.1(4) ? N1 C2 H2a . . . 109.3(5) ? N1 C2 H2b . . . 109.4(5) ? C3 C2 H2a . . . 109.8(6) ? C3 C2 H2b . . . 109.5(5) ? H2a C2 H2b . . . 107.7(5) ? C2 C3 N4 . . . 112.0(5) ? C2 C3 H3a . . . 109.7(5) ? C2 C3 H3b . . . 108.8(5) ? N4 C3 H3a . . . 109.1(5) ? N4 C3 H3b . . . 108.6(5) ? H3a C3 H3b . . . 108.6(6) ? Mo N4 C3 . . . 103.2(3) ? Mo N4 C41 . . . 114.7(3) ? Mo N4 C5 . . . 112.0(3) ? C3 N4 C41 . . . 106.2(4) ? C3 N4 C5 . . . 109.9(4) ? C41 N4 C5 . . . 110.4(4) ? N4 C41 C42 . . . 114.5(5) ? N4 C41 H41a . . . 108.4(5) ? N4 C41 H41b . . . 107.6(5) ? C42 C41 H41a . . . 109.1(5) ? C42 C41 H41b . . . 108.7(5) ? H41a C41 H41b . . . 108.4(5) ? C41 C42 C43 . . . 110.3(5) ? C41 C42 H42a . . . 110.1(5) ? C41 C42 H42b . . . 110.2(5) ? C43 C42 H42a . . . 108.8(5) ? C43 C42 H42b . . . 110.2(5) ? H42a C42 H42b . . . 107.3(6) ? C42 C43 C44 . . . 112.4(5) ? C42 C43 H43a . . . 107.7(5) ? C42 C43 H43b . . . 108.9(6) ? C44 C43 H43a . . . 108.5(6) ? C44 C43 H43b . . . 111.9(6) ? H43a C43 H43b . . . 107.3(5) ? C43 C44 C45 . . . 178.7(6) ? C44 C45 C451 . . . 176.9(7) ? C45 C451 C452 . . . 120.6(7) ? C45 C451 C456 . . . 123.4(8) ? C452 C451 C456 . . . 116.0(8) ? C451 C452 C453 . . . 121.8(8) ? C451 C452 H452 . . . 118.6(8) ? C453 C452 H452 . . . 119.6(8) ? C452 C453 C454 . . . 120.1(8) ? C452 C453 H453 . . . 121.2(9) ? C454 C453 H453 . . . 118.7(9) ? C453 C454 C455 . . . 120.0(8) ? C453 C454 H454 . . . 120.1(8) ? C455 C454 H454 . . . 119.9(8) ? C454 C455 C456 . . . 119.7(9) ? C454 C455 H455 . . . 119.7(10) ? C456 C455 H455 . . . 120.7(11) ? C451 C456 C455 . . . 122.1(10) ? C451 C456 H456 . . . 118.8(10) ? C455 C456 H456 . . . 118.8(10) ? N4 C5 C6 . . . 111.4(4) ? N4 C5 H5a . . . 110.2(5) ? N4 C5 H5b . . . 110.7(5) ? C6 C5 H5a . . . 106.8(5) ? C6 C5 H5b . . . 107.7(6) ? H5a C5 H5b . . . 110.1(6) ? C5 C6 N7 . . . 113.1(5) ? C5 C6 H6a . . . 109.7(5) ? C5 C6 H6b . . . 109.3(5) ? N7 C6 H6a . . . 107.5(5) ? N7 C6 H6b . . . 108.3(5) ? H6a C6 H6b . . . 108.9(6) ? Mo N7 C6 . . . 102.8(3) ? Mo N7 C71 . . . 114.6(3) ? Mo N7 C8 . . . 110.6(3) ? C6 N7 C71 . . . 106.8(4) ? C6 N7 C8 . . . 110.4(4) ? C71 N7 C8 . . . 111.2(4) ? N7 C71 C72 . . . 116.5(4) ? N7 C71 H71a . . . 107.7(5) ? N7 C71 H71b . . . 108.4(5) ? C72 C71 H71a . . . 107.7(5) ? C72 C71 H71b . . . 107.6(5) ? H71a C71 H71b . . . 108.8(5) ? C71 C72 C73 . . . 110.5(5) ? C71 C72 H72a . . . 109.8(5) ? C71 C72 H72b . . . 109.2(5) ? C73 C72 H72a . . . 110.0(5) ? C73 C72 H72b . . . 109.0(5) ? H72a C72 H72b . . . 108.3(5) ? C72 C73 C74 . . . 113.1(5) ? C72 C73 H73a . . . 109.1(5) ? C72 C73 H73b . . . 109.7(6) ? C74 C73 H73a . . . 108.0(6) ? C74 C73 H73b . . . 108.4(5) ? H73a C73 H73b . . . 108.5(6) ? C73 C74 C75 . . . 178.8(7) ? C74 C75 C751 . . . 176.5(7) ? C75 C751 C752 . . . 121.5(6) ? C75 C751 C756 . . . 119.9(7) ? C752 C751 C756 . . . 118.5(7) ? C751 C752 C753 . . . 119.8(7) ? C751 C752 H752 . . . 118.9(7) ? C753 C752 H752 . . . 121.3(8) ? C752 C753 C754 . . . 120.9(8) ? C752 C753 H753 . . . 119.4(8) ? C754 C753 H753 . . . 119.7(8) ? C753 C754 C755 . . . 120.9(8) ? C753 C754 H754 . . . 117.8(9) ? C755 C754 H754 . . . 121.3(9) ? C754 C755 C756 . . . 119.7(7) ? C754 C755 H755 . . . 120.3(9) ? C756 C755 H755 . . . 120.1(10) ? C751 C756 C755 . . . 120.3(8) ? C751 C756 H756 . . . 119.4(7) ? C755 C756 H756 . . . 120.3(7) ? N7 C8 C9 . . . 111.6(5) ? N7 C8 H8a . . . 108.8(5) ? N7 C8 H8b . . . 109.6(5) ? C9 C8 H8a . . . 109.4(6) ? C9 C8 H8b . . . 109.9(5) ? H8a C8 H8b . . . 107.4(6) ? N1 C9 C8 . . . 113.0(4) ? N1 C9 H9a . . . 109.8(5) ? N1 C9 H9b . . . 109.1(5) ? C8 C9 H9a . . . 108.2(5) ? C8 C9 H9b . . . 108.5(5) ? H9a C9 H9b . . . 108.0(5) ? Mo C01 O01 . . . 178.4(5) ? Mo C02 O02 . . . 177.5(4) ? Mo C03 O03 . . . 177.9(5) ? O10 C10 C101 . . . 121.3(5) ? O10 C10 C101 . . '2 655' 121.3(5) ? C101 C10 C101 . . '2 655' 117.3(8) ? C10 C101 H101a . . . 114.0(7) ? C10 C101 H101b . . . 116.3(7) ? C10 C101 H101c . . . 110.7(8) ? H101a C101 H101b . . . 106.0(8) ? H101a C101 H101c . . . 99.6(8) ? H101b C101 H101c . . . 108.9(8) ? C20 O20 C20 . . '2 755' 66.8(13) ? C20 O20 C202 . . '2 755' 78.9(18) ? C20 O20 H202a . . '2 755' 119(2) ? C20 O20 H202b . . '2 755' 58.9(13) ? C20 O20 C202 '2 755' . '2 755' 57.6(14) ? C20 O20 H202a '2 755' . '2 755' 79.7(10) ? C20 O20 H202b '2 755' . '2 755' 96.8(15) ? C202 O20 H202a '2 755' . '2 755' 40.6(12) ? C202 O20 H202b '2 755' . '2 755' 54.3(16) ? H202a O20 H202b '2 755' . '2 755' 78.0(15) ? O20 C20 C201 . . . 120.6(16) ? O20 C20 C202 . . . 119.9(18) ? O20 C20 O20 . . '2 755' 110.8(15) ? O20 C20 C20 . . '2 755' 71.8(13) ? O20 C20 C202 . . '2 755' 49.7(15) ? O20 C20 H202b . . '2 755' 49.7(13) ? C201 C20 C202 . . . 118.5(16) ? C201 C20 O20 . . '2 755' 119.2(13) ? C201 C20 C20 . . '2 755' 158.2(15) ? C201 C20 C202 . . '2 755' 146.6(16) ? C201 C20 H202b . . '2 755' 106.2(14) ? C202 C20 O20 . . '2 755' 42.0(12) ? C202 C20 C20 . . '2 755' 56.8(12) ? C202 C20 C202 . . '2 755' 74.8(14) ? C202 C20 H202b . . '2 755' 103.8(15) ? O20 C20 C20 '2 755' . '2 755' 41.3(8) ? O20 C20 C202 '2 755' . '2 755' 91.6(13) ? O20 C20 H202b '2 755' . '2 755' 132.2(15) ? C20 C20 C202 '2 755' . '2 755' 55.2(11) ? C20 C20 H202b '2 755' . '2 755' 95.4(13) ? C202 C20 H202b '2 755' . '2 755' 41.1(10) ? C20 C201 H201a . . . 111.7(15) ? C20 C201 H201b . . . 110.5(16) ? C20 C201 H201c . . . 110.7(16) ? H201a C201 H201b . . . 111.2(17) ? H201a C201 H201c . . . 107.4(17) ? H201b C201 H201c . . . 105.0(15) ? C20 C202 H202a . . . 113.1(19) ? C20 C202 H202b . . . 112.9(18) ? C20 C202 H202c . . . 106.4(17) ? C20 C202 O20 . . '2 755' 80.4(16) ? C20 C202 C20 . . '2 755' 68.0(13) ? C20 C202 C202 . . '2 755' 53.3(11) ? H202a C202 H202b . . . 106.9(19) ? H202a C202 H202c . . . 111(2) ? H202a C202 O20 . . '2 755' 84.4(17) ? H202a C202 C20 . . '2 755' 136(2) ? H202a C202 C202 . . '2 755' 164(2) ? H202b C202 H202c . . . 106(2) ? H202b C202 O20 . . '2 755' 52.2(13) ? H202b C202 C20 . . '2 755' 45.9(11) ? H202b C202 C202 . . '2 755' 87.7(15) ? H202c C202 O20 . . '2 755' 157(2) ? H202c C202 C20 . . '2 755' 110.3(18) ? H202c C202 C202 . . '2 755' 69.6(13) ? O20 C202 C20 '2 755' . '2 755' 51.4(13) ? O20 C202 C202 '2 755' . '2 755' 99.9(16) ? C20 C202 C202 '2 755' . '2 755' 51.9(11) ? C202 H202a O20 . . '2 755' 55.0(15) ? C202 H202b O20 . . '2 755' 73.5(16) ? C202 H202b C20 . . '2 755' 93.0(15) ? O20 H202b C20 '2 755' . '2 755' 71.4(14) ? 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 Mo C11 3.272(5) . . ? Mo C12 3.765(6) . . ? Mo C2 3.212(5) . . ? Mo C3 3.063(6) . . ? Mo C41 3.270(5) . . ? Mo C42 3.733(5) . . ? Mo C5 3.219(6) . . ? Mo C6 3.076(6) . . ? Mo C71 3.276(6) . . ? Mo C72 3.787(6) . . ? Mo C8 3.212(6) . . ? Mo C9 3.047(5) . . ? Mo O01 3.103(4) . . ? Mo O02 3.104(4) . . ? Mo O03 3.110(4) . . ? Mo H11b 3.2599(5) . . ? Mo H12a 3.3175(7) . . ? Mo H3b 3.1308(5) . . ? Mo H41b 3.2698(5) . . ? Mo H42a 3.2510(6) . . ? Mo H6b 3.1589(5) . . ? Mo H71b 3.2771(7) . . ? Mo H72a 3.3214(5) . . ? Mo H9a 3.1329(5) . . ? N1 C12 2.530(7) . . ? N1 C3 2.487(7) . . ? N1 N4 2.895(6) . . ? N1 N7 2.915(6) . . ? N1 C8 2.516(8) . . ? N1 H11a 2.003(5) . . ? N1 H11b 2.004(4) . . ? N1 H2a 2.027(4) . . ? N1 H2b 2.037(5) . . ? N1 H9a 2.036(5) . . ? N1 H9b 2.035(4) . . ? C11 C13 2.524(8) . . ? C11 C2 2.445(8) . . ? C11 C9 2.394(8) . . ? C11 H12a 2.055(5) . . ? C11 H12b 2.048(5) . . ? C11 H13b 2.634(5) . . ? C11 H2b 2.390(5) . . ? C11 H9a 2.543(5) . . ? C11 H9b 2.581(5) . . ? C12 C14 2.524(9) . . ? C12 C2 2.956(8) . . ? C12 H11a 2.041(6) . . ? C12 H11b 2.028(6) . . ? C12 H13a 2.077(6) . . ? C12 H13b 2.078(6) . . ? C12 H2b 2.654(6) . . ? C13 C15 2.668(10) . . ? C13 H11a 2.676(6) . . ? C13 H11b 2.668(6) . . ? C13 H12a 2.044(8) . . ? C13 H12b 2.056(8) . . ? C14 C151 2.630(11) . . ? C14 H12a 2.648(7) . . ? C14 H13a 1.990(7) . . ? C14 H13b 1.997(7) . . ? C15 C152 2.467(11) . . ? C15 C156 2.458(10) . . ? C15 H152 2.641(7) . . ? C15 H156 2.624(7) . . ? C151 C153 2.405(12) . . ? C151 C154 2.777(13) . . ? C151 C155 2.421(12) . . ? C151 H152 2.023(8) . . ? C151 H156 2.053(8) . . ? C152 C154 2.387(13) . . ? C152 C155 2.762(12) . . ? C152 C156 2.388(12) . . ? C152 H153 2.053(9) . . ? C153 C155 2.373(13) . . ? C153 C156 2.744(12) . . ? C153 H152 2.030(9) . . ? C153 H154 2.064(9) . . ? C154 C156 2.372(13) . . ? C154 H153 2.038(11) . . ? C154 H155 2.038(11) . . ? C155 H154 2.027(8) . . ? C155 H156 2.038(8) . . ? C156 H155 2.039(8) . . ? C2 N4 2.505(7) . . ? C2 C5 2.989(9) . . ? C2 C8 2.998(8) . . ? C2 C9 2.462(8) . . ? C2 H11a 2.653(7) . . ? C2 H12b 2.629(5) . . ? C2 H3a 2.042(7) . . ? C2 H3b 2.038(6) . . ? C2 H5a 2.569(6) . . ? C2 H9b 2.623(7) . . ? C3 C41 2.406(8) . . ? C3 C5 2.460(9) . . ? C3 H2a 2.046(6) . . ? C3 H2b 2.052(6) . . ? C3 H41a 2.530(6) . . ? C3 H41b 2.556(6) . . ? C3 H5a 2.414(6) . . ? N4 C42 2.536(7) . . ? N4 C6 2.480(7) . . ? N4 N7 2.902(6) . . ? N4 H3a 2.028(5) . . ? N4 H3b 2.029(5) . . ? N4 H41a 2.015(4) . . ? N4 H41b 2.015(4) . . ? N4 H5a 2.037(4) . . ? N4 H5b 2.025(4) . . ? C41 C43 2.514(8) . . ? C41 C5 2.463(8) . . ? C41 H3a 2.586(5) . . ? C41 H3b 2.533(5) . . ? C41 H42a 2.058(6) . . ? C41 H42b 2.051(6) . . ? C41 H43b 2.676(5) . . ? C41 H5b 2.417(6) . . ? C42 C44 2.511(8) . . ? C42 C5 2.987(8) . . ? C42 H41a 2.033(6) . . ? C42 H41b 2.038(6) . . ? C42 H43a 2.076(6) . . ? C42 H43b 2.057(5) . . ? C43 C45 2.658(9) . . ? C43 H41a 2.678(6) . . ? C43 H41b 2.671(6) . . ? C43 H42a 2.077(5) . . ? C43 H42b 2.085(6) . . ? C44 C451 2.620(11) . . ? C44 H41b 2.685(6) . . ? C44 H42a 2.672(6) . . ? C44 H43a 2.014(6) . . ? C44 H43b 2.019(6) . . ? C45 C452 2.454(10) . . ? C45 C456 2.500(12) . . ? C45 H452 2.605(6) . . ? C45 H456 2.687(6) . . ? C451 C453 2.425(12) . . ? C451 C454 2.805(12) . . ? C451 C455 2.436(13) . . ? C451 H452 2.017(8) . . ? C451 H456 2.062(8) . . ? C452 C454 2.386(12) . . ? C452 C455 2.750(14) . . ? C452 C456 2.370(14) . . ? C452 H453 2.033(8) . . ? C453 C455 2.373(14) . . ? C453 C456 2.739(14) . . ? C453 H452 2.021(9) . . ? C453 H454 2.035(9) . . ? C454 C456 2.378(14) . . ? C454 H453 1.993(8) . . ? C454 H455 2.048(8) . . ? C455 H454 2.036(11) . . ? C455 H456 2.037(11) . . ? C456 H455 2.063(11) . . ? C456 H202a 2.590(11) . . ? C5 N7 2.517(7) . . ? C5 H3a 2.614(7) . . ? C5 H41a 2.650(6) . . ? C5 H42b 2.672(6) . . ? C5 H6a 2.040(6) . . ? C5 H6b 2.028(6) . . ? C5 H8a 2.589(6) . . ? C6 C71 2.408(8) . . ? C6 C8 2.468(8) . . ? C6 H5a 2.005(6) . . ? C6 H5b 1.999(6) . . ? C6 H71a 2.525(6) . . ? C6 H71b 2.567(5) . . ? C6 H8a 2.394(6) . . ? N7 C72 2.559(7) . . ? N7 C9 2.488(7) . . ? N7 H6a 2.018(4) . . ? N7 H6b 2.021(4) . . ? N7 H71a 1.999(4) . . ? N7 H71b 2.001(4) . . ? N7 H8a 2.021(4) . . ? N7 H8b 2.032(4) . . ? C71 C73 2.496(8) . . ? C71 C8 2.461(8) . . ? C71 H6a 2.587(6) . . ? C71 H6b 2.516(6) . . ? C71 H72a 2.048(6) . . ? C71 H72b 2.052(6) . . ? C71 H73b 2.632(6) . . ? C71 H8b 2.414(6) . . ? C72 C74 2.487(9) . . ? C72 H71a 2.029(6) . . ? C72 H71b 2.022(6) . . ? C72 H73a 2.046(6) . . ? C72 H73b 2.040(6) . . ? C73 C75 2.653(10) . . ? C73 H71a 2.652(7) . . ? C73 H71b 2.632(6) . . ? C73 H72a 2.046(6) . . ? C73 H72b 2.044(6) . . ? C74 C751 2.649(10) . . ? C74 H71b 2.683(6) . . ? C74 H72a 2.651(6) . . ? C74 H73a 1.987(7) . . ? C74 H73b 1.979(7) . . ? C75 C752 2.507(10) . . ? C75 C756 2.477(10) . . ? C75 H752 2.669(7) . . ? C75 H756 2.642(6) . . ? C751 C753 2.407(11) . . ? C751 C754 2.775(12) . . ? C751 C755 2.419(10) . . ? C751 H752 2.050(7) . . ? C751 H756 2.061(7) . . ? C752 C754 2.382(12) . . ? C752 C755 2.776(11) . . ? C752 C756 2.418(11) . . ? C752 H753 2.015(8) . . ? C753 C755 2.383(12) . . ? C753 C756 2.762(12) . . ? C753 H752 2.036(8) . . ? C753 H754 2.007(8) . . ? C754 C756 2.388(13) . . ? C754 H753 2.015(10) . . ? C754 H755 2.026(10) . . ? C755 H754 2.046(10) . . ? C755 H756 2.060(10) . . ? C756 H755 2.040(7) . . ? C8 H2a 2.574(6) . . ? C8 H6a 2.605(6) . . ? C8 H71a 2.653(6) . . ? C8 H9a 2.025(6) . . ? C8 H9b 2.035(6) . . ? C9 H11a 2.514(6) . . ? C9 H11b 2.579(6) . . ? C9 H2a 2.397(5) . . ? C9 H8a 2.044(5) . . ? C9 H8b 2.052(6) . . ? C01 C02 2.640(7) . . ? C01 C03 2.644(7) . . ? C01 H42a 2.442(5) . . ? O01 H3a 2.632(4) . '7 655' ? O01 H42a 2.626(4) . . ? O01 H752 2.500(4) . . ? C02 C03 2.620(7) . . ? C02 H72a 2.559(5) . . ? O02 H9b 2.565(4) . '7 655' ? C03 H12a 2.547(5) . . ? O10 C101 2.359(11) . '2 655' ? O10 C101 2.359(11) . . ? O10 H155 2.625(2) . '6 655' ? O10 H155 2.625(2) . '5 445' ? O10 H454 2.555(3) . '8 455' ? O10 H454 2.555(3) . '7 645' ? O10 H101c 2.487(4) . . ? O10 H101c 2.487(4) . '2 655' ? C10 H101a 2.104(7) . '2 655' ? C10 H101a 2.104(7) . . ? C10 H101b 2.101(5) . '2 655' ? C10 H101b 2.101(5) . . ? C10 H101c 2.0288(13) . . ? C10 H101c 2.0288(13) . '2 655' ? C101 C101 2.558(12) . '2 655' ? O20 O20 2.44(2) . '2 755' ? O20 C201 2.29(2) . . ? O20 C201 2.73(2) . '2 755' ? O20 C202 2.33(3) . . ? O20 H753 2.62(2) . '7 645' ? O20 H754 2.44(2) . '7 645' ? O20 H201a 2.459(14) . . ? O20 H202b 2.595(18) . . ? O20 H202c 2.10(2) . '2 755' ? O20 H202c 2.62(2) . . ? C20 H201a 1.971(17) . . ? C20 H201b 1.965(17) . . ? C20 H201c 1.998(18) . . ? C20 H202a 2.278(17) . '2 755' ? C20 H202a 2.042(16) . . ? C20 H202b 2.086(17) . . ? C20 H202c 2.061(18) . '2 755' ? C20 H202c 1.989(18) . . ? C201 C202 2.81(3) . '2 755' ? C201 C202 2.50(3) . . ? C201 H202a 2.595(16) . . ? C201 H202b 2.020(17) . '2 755' ? C202 H201b 2.50(2) . . ? C202 H202b 2.04(2) . '2 755' ? C202 H202c 1.74(2) . '2 755' ? H11a H11b 1.5513(3) . . ? H11a H12b 2.3277(3) . . ? H11a H2b 2.3609(4) . . ? H11a H9b 2.3333(4) . . ? H11b H12a 2.3263(3) . . ? H11b H9a 2.3599(4) . . ? H12a H12b 1.5514(3) . . ? H12b H13a 2.2939(3) . . ? H12b H2b 2.1151(3) . . ? H13a H13a 2.2015(4) . '2 755' ? H13a H13b 1.55135(18) . . ? H152 H153 2.3449(3) . . ? H153 H154 2.3692(3) . . ? H154 H155 2.3258(4) . . ? H155 H156 2.3354(3) . . ? H2a H2b 1.5515(3) . . ? H2a H3a 2.2989(4) . . ? H2a H5a 2.0575(3) . . ? H2a H8a 2.0653(4) . . ? H2b H3a 2.3700(4) . . ? H2b H3b 2.2963(3) . . ? H3a H3b 1.5513(2) . . ? H3a H41a 2.3457(3) . . ? H3b H41b 2.3081(3) . . ? H41a H41b 1.5512(2) . . ? H41a H42b 2.3469(4) . . ? H41a H5b 2.3780(3) . . ? H41b H42a 2.3474(4) . . ? H42a H42b 1.5513(2) . . ? H42a H43a 2.3784(4) . . ? H42b H43a 2.3312(3) . . ? H42b H43b 2.3767(3) . . ? H42b H5b 2.1921(3) . . ? H43a H43b 1.5513(2) . . ? H452 H453 2.3334(3) . . ? H452 H9b 2.2521(3) . 4 ? H453 H454 2.3040(3) . . ? H453 H73a 2.3363(3) . '6 655' ? H454 H455 2.3435(3) . . ? H455 H456 2.3535(3) . . ? H456 H201b 2.2770(4) . . ? H456 H202a 2.3991(3) . . ? H5a H5b 1.5513(2) . . ? H5a H6a 2.2446(4) . . ? H5a H8a 2.0511(4) . . ? H5b H6a 2.3365(3) . . ? H5b H6b 2.2434(3) . . ? H6a H6b 1.5514(3) . . ? H6a H71a 2.3343(3) . . ? H6a H8a 2.3784(3) . . ? H6b H71b 2.3113(3) . . ? H71a H71b 1.5513(3) . . ? H71a H72b 2.3184(4) . . ? H71a H8b 2.3658(3) . . ? H71b H72a 2.3334(4) . . ? H71b H101a 2.3854(3) . . ? H72a H72b 1.5514(3) . . ? H72a H73a 2.3714(4) . . ? H72b H73a 2.2902(3) . . ? H72b H73b 2.3651(4) . . ? H72b H8b 2.1974(3) . . ? H73a H73b 1.55135(18) . . ? H752 H753 2.3327(3) . . ? H753 H754 2.2879(3) . . ? H754 H755 2.3531(4) . . ? H755 H756 2.3573(3) . . ? H8a H8b 1.5513(2) . . ? H8a H9b 2.2836(3) . . ? H8b H9a 2.2802(3) . . ? H8b H9b 2.3603(4) . . ? H9a H9b 1.5514(3) . . ? H101a H101b 1.5512(3) . . ? H101a H101c 1.4735(2) . . ? H101b H101c 1.54008(18) . . ? H201a H201b 1.5514(3) . . ? H201a H201c 1.5482(2) . . ? H201a H202b 2.1000(4) . '2 755' ? H201b H201c 1.5316(3) . . ? H201b H202a 2.2967(3) . . ? H202a H202b 1.5513(3) . . ? H202a H202c 1.57031(19) . . ? H202b H202c 1.57035(19) . . ? H202b H202c 2.0480(3) . '2 755' ? H202c H202c 1.15818(18) . '2 755' ? _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 3328 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 34 _reflns_limit_k_min 0 _reflns_limit_k_max 20 _reflns_limit_l_min 0 _reflns_limit_l_max 29 _reflns_number_observed ? _reflns_d_resolution_high .729 _reflns_d_resolution_low 10.646 _diffrn_reflns_av_sigmaI/netI .05 _diffrn_reflns_theta_min 1.91 _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 .051 _refine_ls_wR_factor_all .049 _refine_ls_goodness_of_fit_all 1.485 _refine_ls_shift/su_mean .004 #========================================================================== # 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_dbrhpf # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C47 H57 F6 N3 P1 Rh1' _chemical_formula_moiety ? _chemical_formula_weight 911.86 _chemical_melting_point ? _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P_21_21_21 _symmetry_space_group_name_Hall p_2ac_2ab loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z _cell_length_a 11.4850(10) _cell_length_b 12.312(2) _cell_length_c 30.350(4) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 4291.6(10) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 6389 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu .498 _exptl_crystal_description plate _exptl_crystal_size_max .25 _exptl_crystal_size_mid .15 _exptl_crystal_size_min .04 _exptl_crystal_size_rad ? _exptl_crystal_colour ? _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 .823 _exptl_absorpt_correction_T_max .928 _diffrn_reflns_number 50587 _reflns_number_total 6089 _reflns_Friedel_coverage .828 _reflns_number_gt 5265 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.29 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .051 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 41 _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 .038 _refine_ls_wR_factor_ref .041 _refine_ls_goodness_of_fit_ref 1.417 _refine_ls_number_reflns 5200 _refine_ls_number_parameters 549 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .076 _refine_diff_density_min -.542 _refine_diff_density_max .815 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack xabs refined' _refine_ls_abs_structure_Flack -.02(3) # 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 ? 0 188 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 228 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' F ? 0 24 .014 .01 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 12 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 4 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' Rh ? 0 4 -1.287 .919 '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 Rh 1.01365(2) .75592(2) .139627(10) .01899(13) Uani ? ? 1.00000 ? ? N1 .8854(3) .8220(3) .09133(12) .021(2) Uani ? ? 1.00000 ? ? C11 .7656(4) .8461(4) .10890(15) .024(2) Uani ? ? 1.00000 ? ? C12 .6850(4) .9116(4) .07875(18) .030(3) Uani ? ? 1.00000 ? ? C13 .5695(4) .9349(4) .10206(17) .034(3) Uani ? ? 1.00000 ? ? C14 .4981(4) 1.0094(3) .07613(16) .030(2) Uani ? ? 1.00000 ? ? C15 .4426(4) 1.0712(4) .05422(17) .030(2) Uani ? ? 1.00000 ? ? C151 .3763(4) 1.1435(4) .02642(17) .028(2) Uani ? ? 1.00000 ? ? C152 .2877(4) 1.1030(4) -.00038(16) .030(3) Uani ? ? 1.00000 ? ? C153 .2271(5) 1.1711(4) -.02857(17) .033(3) Uani ? ? 1.00000 ? ? C154 .2538(5) 1.2801(4) -.03018(18) .037(3) Uani ? ? 1.00000 ? ? C155 .3398(5) 1.3217(4) -.00336(19) .038(3) Uani ? ? 1.00000 ? ? C156 .4014(4) 1.2543(5) .02481(16) .033(2) Uani ? ? 1.00000 ? ? C2 .8771(3) .7460(5) .05196(14) .026(2) Uani ? ? 1.00000 ? ? C3 .9303(4) .6348(4) .05907(16) .025(2) Uani ? ? 1.00000 ? ? N4 1.0500(3) .6380(3) .07755(12) .0217(19) Uani ? ? 1.00000 ? ? C41 1.0868(4) .5278(4) .09132(15) .025(2) Uani ? ? 1.00000 ? ? C42 1.0903(5) .4392(4) .05584(16) .031(3) Uani ? ? 1.00000 ? ? C43 1.1223(5) .3290(4) .07733(17) .033(3) Uani ? ? 1.00000 ? ? C44 1.0283(5) .2881(4) .10537(17) .033(3) Uani ? ? 1.00000 ? ? C45 .9466(4) .2585(4) .12640(15) .031(2) Uani ? ? 1.00000 ? ? C451 .8421(4) .2269(4) .14919(15) .029(2) Uani ? ? 1.00000 ? ? C452 .8361(4) .1299(4) .17287(16) .030(3) Uani ? ? 1.00000 ? ? C453 .7338(5) .1011(4) .19425(19) .037(3) Uani ? ? 1.00000 ? ? C454 .6372(5) .1685(5) .1919(2) .041(3) Uani ? ? 1.00000 ? ? C455 .6419(4) .2632(5) .16844(18) .040(3) Uani ? ? 1.00000 ? ? C456 .7435(5) .2931(4) .14722(17) .035(3) Uani ? ? 1.00000 ? ? C5 1.1371(4) .6875(4) .04741(16) .028(3) Uani ? ? 1.00000 ? ? C6 1.2094(4) .7727(4) .07106(15) .027(2) Uani ? ? 1.00000 ? ? N7 1.1368(3) .8551(3) .09468(13) .022(2) Uani ? ? 1.00000 ? ? C71 1.2169(4) .9351(4) .11510(17) .029(2) Uani ? ? 1.00000 ? ? C72 1.1545(4) 1.0185(4) .14364(18) .031(2) Uani ? ? 1.00000 ? ? C73 1.2403(5) 1.0945(4) .1670(2) .039(3) Uani ? ? 1.00000 ? ? C74 1.3239(5) 1.0376(4) .1957(2) .037(3) Uani ? ? 1.00000 ? ? C75 1.3936(5) .9912(4) .21726(18) .035(3) Uani ? ? 1.00000 ? ? C751 1.4860(5) .9427(4) .24319(16) .034(3) Uani ? ? 1.00000 ? ? C752 1.5241(5) .9939(4) .28174(17) .036(3) Uani ? ? 1.00000 ? ? C753 1.6165(5) .9522(5) .30559(18) .040(3) Uani ? ? 1.00000 ? ? C754 1.6716(5) .8586(5) .2912(2) .041(3) Uani ? ? 1.00000 ? ? C755 1.6345(5) .8061(5) .2534(2) .044(3) Uani ? ? 1.00000 ? ? C756 1.5411(5) .8475(4) .22929(17) .036(3) Uani ? ? 1.00000 ? ? C8 1.0626(4) .9157(4) .06256(16) .026(2) Uani ? ? 1.00000 ? ? C9 .9380(4) .9271(4) .07734(16) .025(2) Uani ? ? 1.00000 ? ? C01 .9070(5) .7787(4) .19563(17) .031(3) Uani ? ? 1.00000 ? ? C02 .8875(4) .6755(5) .17613(17) .031(3) Uani ? ? 1.00000 ? ? C03 .9300(5) .5707(5) .19665(18) .036(3) Uani ? ? 1.00000 ? ? C04 1.0615(5) .5727(4) .20604(18) .036(3) Uani ? ? 1.00000 ? ? C05 1.1257(4) .6581(4) .17954(17) .028(3) Uani ? ? 1.00000 ? ? C06 1.1419(4) .7645(5) .19214(15) .032(3) Uani ? ? 1.00000 ? ? C07 1.0964(6) .8163(4) .23336(17) .039(3) Uani ? ? 1.00000 ? ? C08 .9686(5) .7899(4) .24010(17) .041(3) Uani ? ? 1.00000 ? ? P .51447(12) .58543(9) .07766(4) .0290(6) Uani ? ? 1.00000 ? ? F1 .4850(6) .6987(4) .05356(16) .060(3) Uani ? ? .846(8) ? ? F2 .5421(5) .4738(4) .10174(17) .048(3) Uani ? ? .846(8) ? ? F3 .4996(7) .5200(3) .03324(12) .088(4) Uani ? ? .846(8) ? ? F4 .6458(4) .6008(4) .0656(3) .089(4) Uani ? ? .846(8) ? ? F5 .5306(7) .6507(4) .12155(14) .083(4) Uani ? ? .846(8) ? ? F6 .3823(4) .5707(5) .0901(2) .085(4) Uani ? ? .846(8) ? ? F1' .543(3) .690(2) .0524(10) .049(8) Uiso ? ? .154(8) ? ? F2' .490(3) .471(3) .0945(11) .053(9) Uiso ? ? .154(8) ? ? F3' .407(2) .582(2) .0476(8) .048(7) Uiso ? ? .154(8) ? ? F4' .599(3) .554(3) .0407(10) .071(9) Uiso ? ? .154(8) ? ? F5' .616(3) .606(2) .1114(10) .061(8) Uiso ? ? .154(8) ? ? F6' .436(3) .633(2) .1140(9) .057(8) Uiso ? ? .154(8) ? ? H11a .77479 .88606 .13588 .03100 Uiso ? ? 1.00000 ? ? H11b .72870 .77884 .11547 .03100 Uiso ? ? 1.00000 ? ? H12a .66782 .87177 .05266 .04000 Uiso ? ? 1.00000 ? ? H12b .71986 .97907 .07083 .04000 Uiso ? ? 1.00000 ? ? H13a .58797 .96796 .13027 .04300 Uiso ? ? 1.00000 ? ? H13b .53073 .86877 .10737 .04300 Uiso ? ? 1.00000 ? ? H152 .26789 1.02719 .00067 .03700 Uiso ? ? 1.00000 ? ? H153 .16738 1.14218 -.04779 .04200 Uiso ? ? 1.00000 ? ? H154 .21189 1.32693 -.05020 .04600 Uiso ? ? 1.00000 ? ? H155 .35826 1.39778 -.00452 .04700 Uiso ? ? 1.00000 ? ? H156 .45958 1.28408 .04423 .04300 Uiso ? ? 1.00000 ? ? H2a .91682 .78059 .02778 .03300 Uiso ? ? 1.00000 ? ? H2b .79728 .73873 .04445 .03300 Uiso ? ? 1.00000 ? ? H3a .88088 .59532 .07847 .03300 Uiso ? ? 1.00000 ? ? H3b .93181 .59799 .03114 .03300 Uiso ? ? 1.00000 ? ? H41a 1.03416 .50390 .11358 .03000 Uiso ? ? 1.00000 ? ? H41b 1.16283 .53319 .10354 .03000 Uiso ? ? 1.00000 ? ? H42a 1.14686 .45779 .03379 .03700 Uiso ? ? 1.00000 ? ? H42b 1.01595 .43370 .04172 .03700 Uiso ? ? 1.00000 ? ? H43a 1.19120 .33780 .09411 .04400 Uiso ? ? 1.00000 ? ? H43b 1.13694 .27672 .05441 .04400 Uiso ? ? 1.00000 ? ? H452 .90254 .08345 .17500 .03700 Uiso ? ? 1.00000 ? ? H453 .73145 .03546 .21100 .04700 Uiso ? ? 1.00000 ? ? H454 .56556 .14606 .20630 .05200 Uiso ? ? 1.00000 ? ? H455 .57465 .31053 .16674 .04900 Uiso ? ? 1.00000 ? ? H456 .74819 .36005 .13049 .04700 Uiso ? ? 1.00000 ? ? H5a 1.09739 .72299 .02366 .03600 Uiso ? ? 1.00000 ? ? H5b 1.18752 .63420 .03599 .03600 Uiso ? ? 1.00000 ? ? H6a 1.25858 .73722 .09187 .03700 Uiso ? ? 1.00000 ? ? H6b 1.25707 .81005 .05017 .03700 Uiso ? ? 1.00000 ? ? H71a 1.25673 .97289 .09208 .03800 Uiso ? ? 1.00000 ? ? H71b 1.27221 .89810 .13280 .03800 Uiso ? ? 1.00000 ? ? H72a 1.10950 .98097 .16506 .03900 Uiso ? ? 1.00000 ? ? H72b 1.10373 1.06011 .12535 .03900 Uiso ? ? 1.00000 ? ? H73a 1.19596 1.14462 .18479 .04900 Uiso ? ? 1.00000 ? ? H73b 1.28153 1.13527 .14543 .04900 Uiso ? ? 1.00000 ? ? H752 1.48611 1.05895 .29172 .04300 Uiso ? ? 1.00000 ? ? H753 1.64217 .99016 .33188 .05300 Uiso ? ? 1.00000 ? ? H754 1.73614 .82915 .30785 .05500 Uiso ? ? 1.00000 ? ? H755 1.67219 .74150 .24362 .05300 Uiso ? ? 1.00000 ? ? H756 1.51526 .81014 .20311 .04800 Uiso ? ? 1.00000 ? ? H8a 1.06521 .87868 .03463 .03400 Uiso ? ? 1.00000 ? ? H8b 1.09601 .98703 .05797 .03400 Uiso ? ? 1.00000 ? ? H9a .93367 .97755 .10106 .03200 Uiso ? ? 1.00000 ? ? H9b .89181 .95638 .05322 .03200 Uiso ? ? 1.00000 ? ? H01 .84899 .84188 .18971 .04000 Uiso ? ? 1.00000 ? ? H02 .81158 .65779 .15899 .04000 Uiso ? ? 1.00000 ? ? H03a .91452 .51012 .17669 .04700 Uiso ? ? 1.00000 ? ? H03b .88815 .55564 .22330 .04700 Uiso ? ? 1.00000 ? ? H04a 1.09547 .50365 .20067 .04200 Uiso ? ? 1.00000 ? ? H04b 1.07285 .58995 .23692 .04200 Uiso ? ? 1.00000 ? ? H05 1.17747 .64126 .15838 .03800 Uiso ? ? 1.00000 ? ? H06 1.18496 .81176 .17267 .04000 Uiso ? ? 1.00000 ? ? H07a 1.10437 .89334 .23258 .04900 Uiso ? ? 1.00000 ? ? H07b 1.13903 .78969 .25852 .04900 Uiso ? ? 1.00000 ? ? H08a .96151 .72277 .25630 .04900 Uiso ? ? 1.00000 ? ? H08b .93208 .84571 .25759 .04900 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 Rh .01827(13) .01942(13) .01928(13) .00169(14) -.00022(13) .00155(14) N1 .0181(18) .022(2) .023(2) .0021(15) .0015(15) .0026(16) C11 .017(2) .028(2) .026(2) .0023(17) -.002(2) .005(2) C12 .018(2) .037(3) .037(3) .007(2) -.000(2) .009(2) C13 .026(3) .043(3) .034(3) .009(2) -.003(2) .006(2) C14 .019(2) .032(2) .039(3) .003(2) .002(2) .004(2) C15 .019(2) .035(3) .035(3) .000(2) .003(2) .003(2) C151 .016(2) .032(3) .038(3) .0034(19) .008(2) .006(2) C152 .025(2) .026(2) .038(3) .0022(19) .004(2) .001(2) C153 .029(3) .038(3) .033(3) .007(2) .001(2) -.001(2) C154 .038(3) .040(3) .034(3) .011(2) .002(2) .010(2) C155 .042(3) .026(3) .044(3) -.003(2) .009(3) .006(2) C156 .027(2) .032(2) .039(3) -.004(3) .0040(19) .001(3) C2 .022(2) .031(2) .023(2) -.000(3) -.0035(16) .000(2) C3 .023(2) .030(3) .023(2) -.0004(19) -.001(2) -.003(2) N4 .020(2) .0223(18) .023(2) .0009(14) .0033(16) -.0004(16) C41 .026(2) .025(2) .022(2) .0032(18) .000(2) -.0030(18) C42 .040(3) .026(2) .026(2) .002(2) .005(2) -.004(2) C43 .037(3) .026(2) .037(3) .005(2) .010(2) -.005(2) C44 .037(3) .026(2) .035(3) .006(2) .003(2) -.0022(19) C45 .035(2) .028(2) .030(2) .002(2) .0003(18) -.002(2) C451 .032(2) .032(3) .022(2) .0007(19) .0018(18) -.0047(18) C452 .032(3) .028(2) .030(3) .002(2) .002(2) -.003(2) C453 .039(3) .033(3) .039(3) -.003(2) .005(2) .001(2) C454 .035(3) .042(3) .045(3) -.005(2) .009(3) -.005(3) C455 .033(3) .044(3) .043(3) .011(3) .006(2) -.002(3) C456 .039(3) .031(2) .034(3) .006(2) .001(2) -.000(2) C5 .027(3) .033(3) .023(2) .006(2) .008(2) .001(2) C6 .019(2) .032(3) .032(2) .0027(18) .0078(19) .005(2) N7 .0187(19) .022(2) .026(2) .0005(15) -.0020(16) .0021(15) C71 .021(2) .024(2) .042(3) -.0022(18) -.002(2) .003(2) C72 .024(2) .022(2) .047(3) -.0016(17) -.005(2) -.002(2) C73 .034(3) .025(3) .059(4) -.000(2) -.008(3) -.003(2) C74 .033(3) .031(3) .047(3) -.008(2) .000(3) -.009(2) C75 .032(3) .032(3) .042(3) -.007(2) .000(2) -.003(2) C751 .029(3) .034(2) .038(3) -.007(2) .000(2) .003(2) C752 .033(3) .034(3) .039(3) .000(2) .003(2) -.001(2) C753 .040(3) .047(3) .034(3) -.011(3) -.001(3) .003(2) C754 .035(3) .044(3) .046(3) -.002(2) .002(3) .014(3) C755 .042(3) .032(3) .057(4) .006(2) .013(3) .005(3) C756 .040(3) .032(3) .037(3) -.003(2) .004(2) .003(2) C8 .025(2) .023(2) .030(3) -.0003(18) .002(2) .007(2) C9 .023(2) .023(2) .028(2) .0025(18) .002(2) .005(2) C01 .034(3) .031(3) .027(3) .010(2) .005(2) .003(2) C02 .023(3) .041(3) .030(3) -.001(2) .002(2) .010(2) C03 .046(3) .034(3) .030(3) -.007(2) -.002(2) .009(2) C04 .047(3) .024(3) .037(3) .004(2) -.008(2) .006(2) C05 .025(2) .035(3) .025(3) .006(2) -.003(2) -.005(2) C06 .032(2) .042(3) .021(2) .000(3) -.0071(18) .006(2) C07 .063(4) .027(3) .026(3) -.001(2) -.013(3) -.001(2) C08 .060(4) .037(3) .026(2) .014(3) .007(3) -.001(2) P .0284(6) .0303(6) .0283(6) -.0007(5) .0015(6) .0036(5) F1 .073(4) .047(2) .059(3) .017(3) .014(3) .028(2) F2 .050(3) .036(2) .057(3) .016(2) .007(3) .0145(19) F3 .179(7) .055(3) .029(2) -.055(4) -.007(3) -.0009(17) F4 .032(3) .072(4) .163(7) -.011(2) .026(3) .003(4) F5 .171(7) .047(3) .031(2) -.009(4) -.007(3) -.0064(18) F6 .026(2) .088(4) .141(6) .013(2) .021(3) .055(4) # 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 Rh N1 . . 2.232(4) ? Rh N4 . . 2.415(4) ? Rh N7 . . 2.313(4) ? Rh C01 . . 2.114(5) ? Rh C02 . . 2.075(5) ? Rh C05 . . 2.139(5) ? Rh C06 . . 2.173(5) ? N1 C11 . . 1.505(6) ? N1 C2 . . 1.521(6) ? N1 C9 . . 1.489(6) ? C11 C12 . . 1.531(7) ? C11 H11a . . .961(5) ? C11 H11b . . .952(4) ? C12 C13 . . 1.531(7) ? C12 H12a . . .952(5) ? C12 H12b . . .953(5) ? C13 C14 . . 1.460(7) ? C13 H13a . . .971(5) ? C13 H13b . . .942(5) ? C14 C15 . . 1.195(7) ? C15 C151 . . 1.444(7) ? C151 C152 . . 1.395(7) ? C151 C156 . . 1.395(7) ? C152 C153 . . 1.385(7) ? C152 H152 . . .961(5) ? C153 C154 . . 1.378(7) ? C153 H153 . . .968(5) ? C154 C155 . . 1.379(8) ? C154 H154 . . .966(5) ? C155 C156 . . 1.386(7) ? C155 H155 . . .962(5) ? C156 H156 . . .963(5) ? C2 C3 . . 1.515(7) ? C2 H2a . . .963(4) ? C2 H2b . . .948(4) ? C3 N4 . . 1.486(6) ? C3 H3a . . .952(5) ? C3 H3b . . .962(5) ? N4 C41 . . 1.482(6) ? N4 C5 . . 1.485(6) ? C41 C42 . . 1.533(7) ? C41 H41a . . .953(5) ? C41 H41b . . .951(5) ? C42 C43 . . 1.550(7) ? C42 H42a . . .961(5) ? C42 H42b . . .957(5) ? C43 C44 . . 1.464(7) ? C43 H43a . . .947(5) ? C43 H43b . . .963(5) ? C44 C45 . . 1.192(7) ? C45 C451 . . 1.439(7) ? C451 C452 . . 1.395(7) ? C451 C456 . . 1.396(7) ? C452 C453 . . 1.389(7) ? C452 H452 . . .956(5) ? C453 C454 . . 1.388(8) ? C453 H453 . . .955(5) ? C454 C455 . . 1.367(8) ? C454 H454 . . .972(6) ? C455 C456 . . 1.382(7) ? C455 H455 . . .969(5) ? C456 H456 . . .970(5) ? C5 C6 . . 1.519(7) ? C5 H5a . . .958(5) ? C5 H5b . . .941(5) ? C6 N7 . . 1.495(6) ? C6 H6a . . .954(5) ? C6 H6b . . .956(5) ? N7 C71 . . 1.484(6) ? N7 C8 . . 1.495(6) ? C71 C72 . . 1.523(7) ? C71 H71a . . .956(5) ? C71 H71b . . .948(5) ? C72 C73 . . 1.533(7) ? C72 H72a . . .950(5) ? C72 H72b . . .954(5) ? C73 C74 . . 1.473(8) ? C73 H73a . . .965(6) ? C73 H73b . . .951(6) ? C74 C75 . . 1.181(8) ? C75 C751 . . 1.450(7) ? C751 C752 . . 1.399(7) ? C751 C756 . . 1.397(7) ? C752 C753 . . 1.383(8) ? C752 H752 . . .961(5) ? C753 C754 . . 1.386(8) ? C753 H753 . . .970(6) ? C754 C755 . . 1.383(9) ? C754 H754 . . .968(6) ? C755 C756 . . 1.396(8) ? C755 H755 . . .953(6) ? C756 H756 . . .965(5) ? C8 C9 . . 1.506(6) ? C8 H8a . . .963(5) ? C8 H8b . . .968(5) ? C9 H9a . . .952(5) ? C9 H9b . . .973(5) ? C01 C02 . . 1.420(7) ? C01 C08 . . 1.530(7) ? C01 H01 . . 1.040(5) ? C02 C03 . . 1.513(8) ? C02 H02 . . 1.039(5) ? C03 C04 . . 1.537(8) ? C03 H03a . . .977(5) ? C03 H03b . . .959(5) ? C04 C05 . . 1.515(7) ? C04 H04a . . .950(5) ? C04 H04b . . .970(6) ? C05 C06 . . 1.377(8) ? C05 H05 . . .899(5) ? C06 C07 . . 1.499(7) ? C06 H06 . . .965(5) ? C07 C08 . . 1.517(9) ? C07 H07a . . .953(5) ? C07 H07b . . .965(6) ? C08 H08a . . .965(5) ? C08 H08b . . .965(5) ? P F1 . . 1.611(5) ? P F2 . . 1.588(5) ? P F3 . . 1.580(4) ? P F4 . . 1.564(5) ? P F5 . . 1.567(4) ? P F6 . . 1.575(5) ? P F1' . . 1.54(3) ? P F2' . . 1.52(3) ? P F3' . . 1.54(2) ? P F4' . . 1.53(3) ? P F5' . . 1.57(3) ? P F6' . . 1.54(3) ? F1 F1' . . .68(3) ? F2 F2' . . .64(3) ? F3 F3' . . 1.38(2) ? F3 F4' . . 1.24(3) ? F4 F4' . . 1.09(3) ? F4 F5' . . 1.44(3) ? F5 F5' . . 1.16(3) ? F5 F6' . . 1.13(3) ? F6 F3' . . 1.33(3) ? F6 F6' . . 1.22(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 N1 Rh N4 . . . 79.69(13) ? N1 Rh N7 . . . 79.85(13) ? N1 Rh C01 . . . 95.59(17) ? N1 Rh C02 . . . 93.67(17) ? N1 Rh C05 . . . 167.04(17) ? N1 Rh C06 . . . 155.71(18) ? N4 Rh N7 . . . 75.60(13) ? N4 Rh C01 . . . 143.85(16) ? N4 Rh C02 . . . 104.50(17) ? N4 Rh C05 . . . 89.95(16) ? N4 Rh C06 . . . 118.95(16) ? N7 Rh C01 . . . 139.32(16) ? N7 Rh C02 . . . 173.43(17) ? N7 Rh C05 . . . 105.26(16) ? N7 Rh C06 . . . 89.56(16) ? C01 Rh C02 . . . 39.6(2) ? C01 Rh C05 . . . 88.2(2) ? C01 Rh C06 . . . 78.26(19) ? C02 Rh C05 . . . 81.3(2) ? C02 Rh C06 . . . 96.0(2) ? C05 Rh C06 . . . 37.2(2) ? Rh N1 C11 . . . 116.3(3) ? Rh N1 C2 . . . 109.5(3) ? Rh N1 C9 . . . 103.7(3) ? C11 N1 C2 . . . 110.0(3) ? C11 N1 C9 . . . 107.5(3) ? C2 N1 C9 . . . 109.6(3) ? N1 C11 C12 . . . 116.4(4) ? N1 C11 H11a . . . 107.6(4) ? N1 C11 H11b . . . 108.0(4) ? C12 C11 H11a . . . 107.9(4) ? C12 C11 H11b . . . 108.3(4) ? H11a C11 H11b . . . 108.4(4) ? C11 C12 C13 . . . 110.3(4) ? C11 C12 H12a . . . 110.6(4) ? C11 C12 H12b . . . 110.8(4) ? C13 C12 H12a . . . 107.6(4) ? C13 C12 H12b . . . 108.5(4) ? H12a C12 H12b . . . 109.0(5) ? C12 C13 C14 . . . 110.8(4) ? C12 C13 H13a . . . 107.2(4) ? C12 C13 H13b . . . 109.1(5) ? C14 C13 H13a . . . 109.5(5) ? C14 C13 H13b . . . 111.7(5) ? H13a C13 H13b . . . 108.4(5) ? C13 C14 C15 . . . 178.0(5) ? C14 C15 C151 . . . 178.0(5) ? C15 C151 C152 . . . 120.4(4) ? C15 C151 C156 . . . 120.9(4) ? C152 C151 C156 . . . 118.7(4) ? C151 C152 C153 . . . 120.7(4) ? C151 C152 H152 . . . 120.0(5) ? C153 C152 H152 . . . 119.3(5) ? C152 C153 C154 . . . 120.0(5) ? C152 C153 H153 . . . 120.4(5) ? C154 C153 H153 . . . 119.6(5) ? C153 C154 C155 . . . 120.0(5) ? C153 C154 H154 . . . 119.6(5) ? C155 C154 H154 . . . 120.5(5) ? C154 C155 C156 . . . 120.6(5) ? C154 C155 H155 . . . 119.9(5) ? C156 C155 H155 . . . 119.6(5) ? C151 C156 C155 . . . 120.1(4) ? C151 C156 H156 . . . 119.6(5) ? C155 C156 H156 . . . 120.2(5) ? N1 C2 C3 . . . 114.8(4) ? N1 C2 H2a . . . 107.3(4) ? N1 C2 H2b . . . 107.9(4) ? C3 C2 H2a . . . 108.4(4) ? C3 C2 H2b . . . 109.8(5) ? H2a C2 H2b . . . 108.5(4) ? C2 C3 N4 . . . 113.8(4) ? C2 C3 H3a . . . 108.0(4) ? C2 C3 H3b . . . 108.0(4) ? N4 C3 H3a . . . 109.4(4) ? N4 C3 H3b . . . 109.2(4) ? H3a C3 H3b . . . 108.3(5) ? Rh N4 C3 . . . 98.6(3) ? Rh N4 C41 . . . 112.3(3) ? Rh N4 C5 . . . 110.5(3) ? C3 N4 C41 . . . 110.2(3) ? C3 N4 C5 . . . 113.7(4) ? C41 N4 C5 . . . 111.0(3) ? N4 C41 C42 . . . 117.4(4) ? N4 C41 H41a . . . 107.6(4) ? N4 C41 H41b . . . 107.9(4) ? C42 C41 H41a . . . 107.2(4) ? C42 C41 H41b . . . 107.4(4) ? H41a C41 H41b . . . 109.1(4) ? C41 C42 C43 . . . 109.5(4) ? C41 C42 H42a . . . 109.8(4) ? C41 C42 H42b . . . 110.0(4) ? C43 C42 H42a . . . 109.9(4) ? C43 C42 H42b . . . 109.7(4) ? H42a C42 H42b . . . 108.0(5) ? C42 C43 C44 . . . 111.8(4) ? C42 C43 H43a . . . 109.0(4) ? C42 C43 H43b . . . 108.9(5) ? C44 C43 H43a . . . 110.0(5) ? C44 C43 H43b . . . 108.6(4) ? H43a C43 H43b . . . 108.6(5) ? C43 C44 C45 . . . 175.6(5) ? C44 C45 C451 . . . 175.4(5) ? C45 C451 C452 . . . 121.3(4) ? C45 C451 C456 . . . 119.9(4) ? C452 C451 C456 . . . 118.8(4) ? C451 C452 C453 . . . 120.1(5) ? C451 C452 H452 . . . 120.5(5) ? C453 C452 H452 . . . 119.4(5) ? C452 C453 C454 . . . 119.9(5) ? C452 C453 H453 . . . 119.3(5) ? C454 C453 H453 . . . 120.8(5) ? C453 C454 C455 . . . 120.4(5) ? C453 C454 H454 . . . 118.9(5) ? C455 C454 H454 . . . 120.7(5) ? C454 C455 C456 . . . 120.2(5) ? C454 C455 H455 . . . 120.6(5) ? C456 C455 H455 . . . 119.2(6) ? C451 C456 C455 . . . 120.6(5) ? C451 C456 H456 . . . 118.3(5) ? C455 C456 H456 . . . 121.1(5) ? N4 C5 C6 . . . 111.1(4) ? N4 C5 H5a . . . 109.3(4) ? N4 C5 H5b . . . 110.8(4) ? C6 C5 H5a . . . 107.5(4) ? C6 C5 H5b . . . 108.6(4) ? H5a C5 H5b . . . 109.5(5) ? C5 C6 N7 . . . 113.0(4) ? C5 C6 H6a . . . 108.7(4) ? C5 C6 H6b . . . 109.4(4) ? N7 C6 H6a . . . 108.9(4) ? N7 C6 H6b . . . 108.2(4) ? H6a C6 H6b . . . 108.7(4) ? Rh N7 C6 . . . 105.4(3) ? Rh N7 C71 . . . 118.9(3) ? Rh N7 C8 . . . 107.4(3) ? C6 N7 C71 . . . 107.7(3) ? C6 N7 C8 . . . 110.1(4) ? C71 N7 C8 . . . 107.1(3) ? N7 C71 C72 . . . 113.2(4) ? N7 C71 H71a . . . 108.3(4) ? N7 C71 H71b . . . 109.4(4) ? C72 C71 H71a . . . 108.2(4) ? C72 C71 H71b . . . 108.5(5) ? H71a C71 H71b . . . 109.1(4) ? C71 C72 C73 . . . 111.8(4) ? C71 C72 H72a . . . 108.5(4) ? C71 C72 H72b . . . 108.6(5) ? C73 C72 H72a . . . 109.3(5) ? C73 C72 H72b . . . 109.6(4) ? H72a C72 H72b . . . 109.1(4) ? C72 C73 C74 . . . 113.7(4) ? C72 C73 H73a . . . 108.0(5) ? C72 C73 H73b . . . 108.8(5) ? C74 C73 H73a . . . 108.5(5) ? C74 C73 H73b . . . 109.5(5) ? H73a C73 H73b . . . 108.1(5) ? C73 C74 C75 . . . 177.3(6) ? C74 C75 C751 . . . 174.8(6) ? C75 C751 C752 . . . 119.8(4) ? C75 C751 C756 . . . 120.9(5) ? C752 C751 C756 . . . 119.3(5) ? C751 C752 C753 . . . 120.7(5) ? C751 C752 H752 . . . 119.8(5) ? C753 C752 H752 . . . 119.5(5) ? C752 C753 C754 . . . 119.6(5) ? C752 C753 H753 . . . 119.0(5) ? C754 C753 H753 . . . 121.4(6) ? C753 C754 C755 . . . 120.6(5) ? C753 C754 H754 . . . 119.8(6) ? C755 C754 H754 . . . 119.6(6) ? C754 C755 C756 . . . 120.1(5) ? C754 C755 H755 . . . 120.6(6) ? C756 C755 H755 . . . 119.4(6) ? C751 C756 C755 . . . 119.7(5) ? C751 C756 H756 . . . 120.6(5) ? C755 C756 H756 . . . 119.6(5) ? N7 C8 C9 . . . 113.2(4) ? N7 C8 H8a . . . 108.6(4) ? N7 C8 H8b . . . 108.8(4) ? C9 C8 H8a . . . 109.6(4) ? C9 C8 H8b . . . 109.6(4) ? H8a C8 H8b . . . 106.9(5) ? N1 C9 C8 . . . 112.9(4) ? N1 C9 H9a . . . 109.2(4) ? N1 C9 H9b . . . 108.3(4) ? C8 C9 H9a . . . 109.6(4) ? C8 C9 H9b . . . 109.2(4) ? H9a C9 H9b . . . 107.4(4) ? Rh C01 C02 . . . 68.7(3) ? Rh C01 C08 . . . 117.0(4) ? Rh C01 H01 . . . 109.4(4) ? C02 C01 C08 . . . 121.4(4) ? C02 C01 H01 . . . 119.7(5) ? C08 C01 H01 . . . 112.4(4) ? Rh C02 C01 . . . 71.7(3) ? Rh C02 C03 . . . 113.7(3) ? Rh C02 H02 . . . 114.8(4) ? C01 C02 C03 . . . 122.7(5) ? C01 C02 H02 . . . 121.9(5) ? C03 C02 H02 . . . 107.3(5) ? C02 C03 C04 . . . 112.3(4) ? C02 C03 H03a . . . 109.7(5) ? C02 C03 H03b . . . 110.5(5) ? C04 C03 H03a . . . 107.8(5) ? C04 C03 H03b . . . 109.8(5) ? H03a C03 H03b . . . 106.5(5) ? C03 C04 C05 . . . 113.0(4) ? C03 C04 H04a . . . 110.9(5) ? C03 C04 H04b . . . 108.4(5) ? C05 C04 H04a . . . 109.3(5) ? C05 C04 H04b . . . 107.2(5) ? H04a C04 H04b . . . 107.8(5) ? Rh C05 C04 . . . 113.5(3) ? Rh C05 C06 . . . 72.7(3) ? Rh C05 H05 . . . 97.1(4) ? C04 C05 C06 . . . 125.3(5) ? C04 C05 H05 . . . 122.8(5) ? C06 C05 H05 . . . 109.1(5) ? Rh C06 C05 . . . 70.0(3) ? Rh C06 C07 . . . 113.3(4) ? Rh C06 H06 . . . 85.8(3) ? C05 C06 C07 . . . 126.1(5) ? C05 C06 H06 . . . 118.2(5) ? C07 C06 H06 . . . 115.7(5) ? C06 C07 C08 . . . 111.0(4) ? C06 C07 H07a . . . 111.7(5) ? C06 C07 H07b . . . 109.8(5) ? C08 C07 H07a . . . 108.1(5) ? C08 C07 H07b . . . 108.1(5) ? H07a C07 H07b . . . 108.0(5) ? C01 C08 C07 . . . 110.3(4) ? C01 C08 H08a . . . 109.5(5) ? C01 C08 H08b . . . 110.4(5) ? C07 C08 H08a . . . 109.5(5) ? C07 C08 H08b . . . 110.0(5) ? H08a C08 H08b . . . 107.1(5) ? F1 P F2 . . . 179.3(3) ? F1 P F3 . . . 91.8(2) ? F1 P F4 . . . 89.5(3) ? F1 P F5 . . . 88.1(2) ? F1 P F6 . . . 90.4(3) ? F1 P F1' . . . 24.8(11) ? F1 P F2' . . . 156.0(13) ? F1 P F3' . . . 65.5(9) ? F1 P F4' . . . 91.2(12) ? F1 P F5' . . . 108.2(11) ? F1 P F6' . . . 82.6(11) ? F2 P F3 . . . 88.4(2) ? F2 P F4 . . . 91.2(3) ? F2 P F5 . . . 91.7(3) ? F2 P F6 . . . 89.0(3) ? F2 P F1' . . . 155.8(11) ? F2 P F2' . . . 23.5(12) ? F2 P F3' . . . 114.2(9) ? F2 P F4' . . . 89.4(12) ? F2 P F5' . . . 72.0(11) ? F2 P F6' . . . 96.8(11) ? F3 P F4 . . . 88.0(4) ? F3 P F5 . . . 179.4(4) ? F3 P F6 . . . 92.4(4) ? F3 P F1' . . . 91.4(11) ? F3 P F2' . . . 78.2(12) ? F3 P F3' . . . 52.7(9) ? F3 P F4' . . . 46.8(12) ? F3 P F5' . . . 136.0(11) ? F3 P F6' . . . 137.9(11) ? F4 P F5 . . . 91.3(4) ? F4 P F6 . . . 179.6(4) ? F4 P F1' . . . 64.6(11) ? F4 P F2' . . . 111.6(12) ? F4 P F3' . . . 129.9(9) ? F4 P F4' . . . 41.3(12) ? F4 P F5' . . . 54.6(11) ? F4 P F6' . . . 133.3(11) ? F5 P F6 . . . 88.2(4) ? F5 P F1' . . . 88.3(11) ? F5 P F2' . . . 102.1(12) ? F5 P F3' . . . 127.8(9) ? F5 P F4' . . . 132.6(12) ? F5 P F5' . . . 43.5(11) ? F5 P F6' . . . 42.7(12) ? F6 P F1' . . . 115.2(11) ? F6 P F2' . . . 68.6(12) ? F6 P F3' . . . 50.4(9) ? F6 P F4' . . . 139.2(12) ? F6 P F5' . . . 125.1(11) ? F6 P F6' . . . 46.2(11) ? F1' P F2' . . . 169.2(16) ? F1' P F3' . . . 84.3(14) ? F1' P F4' . . . 73.2(16) ? F1' P F5' . . . 91.8(15) ? F1' P F6' . . . 99.5(15) ? F2' P F3' . . . 91.5(15) ? F2' P F4' . . . 97.3(17) ? F2' P F5' . . . 93.7(16) ? F2' P F6' . . . 90.3(16) ? F3' P F4' . . . 94.0(15) ? F3' P F5' . . . 170.7(14) ? F3' P F6' . . . 87.9(14) ? F4' P F5' . . . 92.9(16) ? F4' P F6' . . . 172.2(16) ? F5' P F6' . . . 84.5(15) ? P F1 F1' . . . 71(2) ? P F2 F2' . . . 72(3) ? P F3 F3' . . . 62.1(10) ? P F3 F4' . . . 64.6(14) ? F3' F3 F4' . . . 117.9(18) ? P F4 F4' . . . 67.8(17) ? P F4 F5' . . . 62.9(12) ? F4' F4 F5' . . . 125(2) ? P F5 F5' . . . 68.4(15) ? P F5 F6' . . . 67.4(15) ? F5' F5 F6' . . . 131(2) ? P F6 F3' . . . 63.3(10) ? P F6 F6' . . . 65.4(14) ? F3' F6 F6' . . . 113.7(17) ? P F1' F1 . . . 84(3) ? P F2' F2 . . . 84(3) ? P F3' F3 . . . 65.2(10) ? P F3' F6 . . . 66.2(11) ? F3 F3' F6 . . . 114.2(17) ? P F4' F3 . . . 68.6(16) ? P F4' F4 . . . 70.9(17) ? F3 F4' F4 . . . 139(3) ? P F5' F4 . . . 62.6(12) ? P F5' F5 . . . 68.2(15) ? F4 F5' F5 . . . 119(2) ? P F6' F5 . . . 69.9(16) ? P F6' F6 . . . 68.3(14) ? F5 F6' F6 . . . 136(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 Rh C11 3.197(4) . . ? Rh C2 3.091(4) . . ? Rh C3 3.019(5) . . ? Rh C41 3.278(5) . . ? Rh C5 3.249(5) . . ? Rh C6 3.070(4) . . ? Rh C71 3.297(5) . . ? Rh C72 3.617(4) . . ? Rh C8 3.108(5) . . ? Rh C9 2.961(5) . . ? Rh C03 3.020(6) . . ? Rh C04 3.074(5) . . ? Rh C07 3.090(5) . . ? Rh C08 3.121(5) . . ? Rh H11a 3.1790(4) . . ? Rh H11b 3.3656(4) . . ? Rh H3a 3.1113(4) . . ? Rh H41a 3.2107(6) . . ? Rh H41b 3.4140(5) . . ? Rh H6a 3.1728(4) . . ? Rh H71b 3.4533(4) . . ? Rh H72a 3.0797(5) . . ? Rh H9a 3.1080(5) . . ? Rh H01 2.6470(3) . . ? Rh H02 2.6816(3) . . ? Rh H03a 3.4235(5) . . ? Rh H05 2.4201(3) . . ? Rh H06 2.3129(3) . . ? Rh H07a 3.4506(4) . . ? N1 C12 2.581(6) . . ? N1 C3 2.557(6) . . ? N1 N4 2.981(5) . . ? N1 N7 2.918(5) . . ? N1 C8 2.497(6) . . ? N1 H11a 2.016(4) . . ? N1 H11b 2.015(4) . . ? N1 H2a 2.028(4) . . ? N1 H2b 2.025(4) . . ? N1 H9a 2.015(4) . . ? N1 H9b 2.020(4) . . ? C11 C13 2.512(7) . . ? C11 C2 2.479(6) . . ? C11 C9 2.415(6) . . ? C11 F4 3.570(7) . . ? C11 F5 3.636(8) . . ? C11 F1' 3.63(3) . . ? C11 F5' 3.42(3) . . ? C11 H12a 2.067(4) . . ? C11 H12b 2.071(5) . . ? C11 H13a 2.614(4) . . ? C11 H2b 2.389(5) . . ? C11 H9a 2.530(4) . . ? C11 H9b 2.608(4) . . ? C11 H01 2.634(5) . . ? C12 C14 2.462(7) . . ? C12 C9 2.913(6) . . ? C12 F1 3.568(7) . . ? C12 F1' 3.28(3) . . ? C12 H11a 2.042(5) . . ? C12 H11b 2.041(5) . . ? C12 H13a 2.042(5) . . ? C12 H13b 2.042(5) . . ? C12 H2b 2.698(5) . . ? C12 H9b 2.559(5) . . ? C13 C15 2.655(7) . . ? C13 F1 3.400(7) . . ? C13 F5 3.576(7) . . ? C13 F1' 3.39(3) . . ? C13 H11a 2.641(5) . . ? C13 H11b 2.683(5) . . ? C13 H12a 2.032(5) . . ? C13 H12b 2.044(5) . . ? C14 C151 2.638(7) . . ? C14 H12a 2.679(5) . . ? C14 H12b 2.579(5) . . ? C14 H13a 2.006(5) . . ? C14 H13b 2.009(4) . . ? C15 C152 2.463(7) . . ? C15 C156 2.470(7) . . ? C15 H152 2.639(5) . . ? C15 H156 2.646(5) . . ? C151 C153 2.415(7) . . ? C151 C154 2.786(7) . . ? C151 C155 2.409(7) . . ? C151 H152 2.052(5) . . ? C151 H156 2.050(5) . . ? C152 C154 2.393(7) . . ? C152 C155 2.760(7) . . ? C152 C156 2.400(7) . . ? C152 F4 3.586(8) . '3 465' ? C152 F4' 3.15(3) . '3 465' ? C152 H153 2.052(5) . . ? C153 C155 2.387(7) . . ? C153 C156 2.771(7) . . ? C153 F2 3.554(7) . '3 465' ? C153 F3 3.519(8) . '3 465' ? C153 F4 3.652(8) . '3 465' ? C153 F4' 3.16(3) . '3 465' ? C153 H152 2.036(5) . . ? C153 H154 2.036(5) . . ? C154 C156 2.401(7) . . ? C154 H153 2.038(5) . . ? C154 H155 2.036(5) . . ? C155 F3 3.250(8) . '1 565' ? C155 F3' 3.64(2) . '1 565' ? C155 H154 2.045(6) . . ? C155 H156 2.048(6) . . ? C156 F3 3.470(7) . '1 565' ? C156 F2' 3.56(3) . '1 565' ? C156 H155 2.040(6) . . ? C2 N4 2.514(6) . . ? C2 C9 2.460(7) . . ? C2 F1 3.501(7) . '3 565' ? C2 F4 3.228(7) . . ? C2 H11b 2.604(4) . . ? C2 H3a 2.023(5) . . ? C2 H3b 2.029(5) . . ? C2 H5a 2.687(4) . . ? C2 H9b 2.596(6) . . ? C3 C41 2.434(7) . . ? C3 C5 2.487(7) . . ? C3 F4 3.300(6) . . ? C3 H2a 2.036(5) . . ? C3 H2b 2.041(5) . . ? C3 H41a 2.600(5) . . ? C3 H5a 2.453(5) . . ? N4 C42 2.576(6) . . ? N4 C6 2.478(6) . . ? N4 N7 2.899(5) . . ? N4 H3a 2.013(3) . . ? N4 H3b 2.017(4) . . ? N4 H41a 1.989(4) . . ? N4 H41b 1.992(4) . . ? N4 H5a 2.016(4) . . ? N4 H5b 2.021(4) . . ? C41 C43 2.517(7) . . ? C41 C5 2.445(7) . . ? C41 F6 3.435(6) . '1 655' ? C41 H3a 2.537(5) . . ? C41 H3b 2.693(5) . . ? C41 H42a 2.066(5) . . ? C41 H42b 2.066(5) . . ? C41 H43a 2.630(5) . . ? C41 H5b 2.424(5) . . ? C41 H05 2.680(5) . . ? C42 C44 2.495(7) . . ? C42 H41a 2.030(5) . . ? C42 H41b 2.032(5) . . ? C42 H43a 2.062(5) . . ? C42 H43b 2.072(5) . . ? C43 C45 2.654(7) . . ? C43 H41a 2.621(5) . . ? C43 H41b 2.677(5) . . ? C43 H42a 2.083(5) . . ? C43 H42b 2.079(5) . . ? C44 C451 2.629(7) . . ? C44 H41a 2.669(5) . . ? C44 H42b 2.639(5) . . ? C44 H43a 1.998(5) . . ? C44 H43b 1.992(5) . . ? C45 C452 2.471(7) . . ? C45 C456 2.454(7) . . ? C45 H452 2.661(5) . . ? C45 H456 2.602(5) . . ? C451 C453 2.412(7) . . ? C451 C454 2.780(7) . . ? C451 C455 2.413(7) . . ? C451 H452 2.053(5) . . ? C451 H456 2.042(5) . . ? C452 C454 2.404(8) . . ? C452 C455 2.772(7) . . ? C452 C456 2.402(7) . . ? C452 H453 2.034(5) . . ? C453 C455 2.390(8) . . ? C453 C456 2.764(7) . . ? C453 H452 2.036(6) . . ? C453 H454 2.043(5) . . ? C454 C456 2.383(8) . . ? C454 H453 2.048(6) . . ? C454 H455 2.038(6) . . ? C455 F2 3.484(8) . . ? C455 H454 2.042(6) . . ? C455 H456 2.058(6) . . ? C456 F2 3.494(7) . . ? C456 H455 2.039(5) . . ? C5 N7 2.513(6) . . ? C5 C8 2.974(7) . . ? C5 F6 3.418(7) . '1 655' ? C5 F1' 3.55(3) . '3 565' ? C5 F3' 3.36(2) . '1 655' ? C5 H3b 2.649(5) . . ? C5 H41b 2.568(5) . . ? C5 H6a 2.036(5) . . ? C5 H6b 2.046(5) . . ? C5 H8a 2.525(5) . . ? C6 C71 2.406(7) . . ? C6 C8 2.451(6) . . ? C6 F1 3.337(8) . '1 655' ? C6 F6 3.236(7) . '1 655' ? C6 F3' 3.34(2) . '1 655' ? C6 F6' 3.38(3) . '1 655' ? C6 H5a 2.025(5) . . ? C6 H5b 2.026(5) . . ? C6 H71a 2.603(5) . . ? C6 H71b 2.533(5) . . ? C6 H8a 2.380(4) . . ? N7 C72 2.510(6) . . ? N7 C9 2.505(6) . . ? N7 H6a 2.017(4) . . ? N7 H6b 2.010(4) . . ? N7 H71a 2.002(4) . . ? N7 H71b 2.009(4) . . ? N7 H72a 2.658(4) . . ? N7 H8a 2.021(4) . . ? N7 H8b 2.025(4) . . ? N7 H06 2.488(4) . . ? C71 C73 2.532(7) . . ? C71 C8 2.396(7) . . ? C71 H6a 2.581(5) . . ? C71 H6b 2.543(5) . . ? C71 H72a 2.035(5) . . ? C71 H72b 2.039(5) . . ? C71 H8b 2.312(5) . . ? C71 H06 2.344(5) . . ? C72 C74 2.517(8) . . ? C72 C8 2.961(7) . . ? C72 H71a 2.036(5) . . ? C72 H71b 2.033(4) . . ? C72 H73a 2.048(5) . . ? C72 H73b 2.049(4) . . ? C73 C75 2.654(8) . . ? C73 H71b 2.657(5) . . ? C73 H72a 2.053(5) . . ? C73 H72b 2.059(6) . . ? C74 C751 2.628(8) . . ? C74 H71b 2.636(6) . . ? C74 H73a 2.001(5) . . ? C74 H73b 2.003(6) . . ? C75 C752 2.465(8) . . ? C75 C756 2.476(7) . . ? C75 H752 2.633(6) . . ? C75 H756 2.665(5) . . ? C751 C753 2.418(8) . . ? C751 C754 2.782(8) . . ? C751 C755 2.415(8) . . ? C751 H752 2.054(5) . . ? C751 H756 2.063(5) . . ? C752 C754 2.393(8) . . ? C752 C755 2.773(8) . . ? C752 C756 2.412(7) . . ? C752 F2 3.626(7) . '4 755' ? C752 F5 3.569(7) . '4 755' ? C752 F6' 3.63(3) . '4 755' ? C752 H753 2.039(5) . . ? C753 C755 2.405(8) . . ? C753 C756 2.788(8) . . ? C753 F2 3.361(8) . '4 755' ? C753 F6 3.485(9) . '4 755' ? C753 F2' 3.28(3) . '4 755' ? C753 F6' 3.36(3) . '4 755' ? C753 H752 2.036(6) . . ? C753 H754 2.047(6) . . ? C754 C756 2.407(8) . . ? C754 H753 2.064(6) . . ? C754 H755 2.041(6) . . ? C755 H754 2.042(6) . . ? C755 H756 2.052(6) . . ? C756 H755 2.040(5) . . ? C8 F3 3.099(6) . '3 565' ? C8 F4' 3.18(3) . '3 565' ? C8 H2a 2.586(5) . . ? C8 H5a 2.681(5) . . ? C8 H6b 2.612(5) . . ? C8 H71a 2.503(5) . . ? C8 H72b 2.648(5) . . ? C8 H9a 2.034(5) . . ? C8 H9b 2.044(5) . . ? C9 F3 3.491(6) . '3 565' ? C9 H11a 2.632(5) . . ? C9 H12b 2.593(4) . . ? C9 H2a 2.361(5) . . ? C9 H8a 2.042(5) . . ? C9 H8b 2.045(4) . . ? C01 C03 2.575(7) . . ? C01 C05 2.959(7) . . ? C01 C06 2.706(7) . . ? C01 C07 2.501(8) . . ? C01 H02 2.158(5) . . ? C01 H08a 2.063(5) . . ? C01 H08b 2.073(5) . . ? C02 C04 2.533(8) . . ? C02 C05 2.746(7) . . ? C02 C08 2.573(8) . . ? C02 H01 2.136(6) . . ? C02 H03a 2.060(6) . . ? C02 H03b 2.056(5) . . ? C02 H08a 2.642(5) . . ? C03 C05 2.546(7) . . ? C03 H02 2.075(6) . . ? C03 H04a 2.076(6) . . ? C03 H04b 2.060(6) . . ? C03 H08a 2.629(5) . . ? C04 C06 2.570(8) . . ? C04 H03a 2.058(5) . . ? C04 H03b 2.069(6) . . ? C04 H05 2.140(5) . . ? C04 H08a 2.657(5) . . ? C05 C07 2.565(7) . . ? C05 H04a 2.036(5) . . ? C05 H04b 2.026(5) . . ? C05 H06 2.022(5) . . ? C06 C08 2.486(7) . . ? C06 H04b 2.663(5) . . ? C06 H05 1.876(5) . . ? C06 H07a 2.052(5) . . ? C06 H07b 2.039(5) . . ? C07 H06 2.105(6) . . ? C07 H08a 2.052(6) . . ? C07 H08b 2.057(6) . . ? C08 H01 2.153(6) . . ? C08 H07a 2.027(6) . . ? C08 H07b 2.036(6) . . ? P H11b 3.6112(13) . . ? P H13b 3.6079(13) . . ? P H153 3.4292(13) . '3 565' ? P H6a 3.5093(13) . '1 455' ? P H753 3.4856(13) . '4 745' ? P H8a 3.4857(13) . '3 465' ? F1 F2 3.199(7) . . ? F1 F3 2.291(6) . . ? F1 F4 2.235(8) . . ? F1 F5 2.210(7) . . ? F1 F6 2.260(8) . . ? F1 F2' 3.06(3) . . ? F1 F3' 1.70(2) . . ? F1 F4' 2.25(3) . . ? F1 F5' 2.58(3) . . ? F1 F6' 2.08(3) . . ? F1 H12a 2.991(6) . . ? F1 H13b 2.707(5) . . ? F1 H2a 2.602(5) . '3 465' ? F1 H5a 2.844(5) . '3 465' ? F1 H6a 2.888(6) . '1 455' ? F1 H6b 2.957(6) . '1 455' ? F1 H8a 2.987(5) . '3 465' ? F2 F3 2.210(7) . . ? F2 F4 2.252(8) . . ? F2 F5 2.263(6) . . ? F2 F6 2.217(7) . . ? F2 F1' 3.05(3) . . ? F2 F3' 2.63(2) . . ? F2 F4' 2.20(3) . . ? F2 F5' 1.86(3) . . ? F2 F6' 2.34(3) . . ? F2 H153 2.606(5) . '3 565' ? F2 H156 3.066(5) . '1 545' ? F2 H455 2.841(5) . . ? F2 H456 2.886(5) . . ? F2 H753 2.929(5) . '4 745' ? F3 F4 2.185(8) . . ? F3 F5 3.147(6) . . ? F3 F6 2.277(8) . . ? F3 F1' 2.23(3) . . ? F3 F2' 1.96(3) . . ? F3 F5' 2.92(3) . . ? F3 F6' 2.91(3) . . ? F3 H152 3.300(7) . '3 565' ? F3 H153 2.810(6) . '3 565' ? F3 H155 2.492(6) . '1 545' ? F3 H156 2.959(4) . '1 545' ? F3 H2a 3.219(4) . '3 465' ? F3 H8a 2.523(4) . '3 465' ? F3 H8b 2.983(4) . '3 465' ? F3 H9b 2.916(5) . '3 465' ? F4 F5 2.240(9) . . ? F4 F6 3.139(6) . . ? F4 F1' 1.66(3) . . ? F4 F2' 2.55(3) . . ? F4 F3' 2.81(2) . . ? F4 F6' 2.85(3) . . ? F4 H11b 2.829(6) . . ? F4 H12a 3.368(6) . . ? F4 H152 2.914(6) . '3 565' ? F4 H153 3.050(6) . '3 565' ? F4 H2b 2.514(5) . . ? F4 H3a 2.729(5) . . ? F4 H8a 3.189(8) . '3 465' ? F5 F6 2.187(9) . . ? F5 F1' 2.16(3) . . ? F5 F2' 2.40(3) . . ? F5 F3' 2.79(2) . . ? F5 F4' 2.84(3) . . ? F5 H11b 2.774(7) . . ? F5 H13b 2.719(5) . . ? F5 H752 2.871(4) . '4 745' ? F5 H753 3.137(6) . '4 745' ? F5 H756 3.164(4) . '1 455' ? F6 F1' 2.63(3) . . ? F6 F2' 1.74(3) . . ? F6 F4' 2.91(3) . . ? F6 F5' 2.79(3) . . ? F6 H41b 2.595(4) . '1 455' ? F6 H5b 2.884(5) . '1 455' ? F6 H6a 2.495(5) . '1 455' ? F6 H753 2.582(7) . '4 745' ? F6 H05 3.253(6) . '1 455' ? F1' F2' 3.04(4) . . ? F1' F3' 2.06(4) . . ? F1' F4' 1.83(4) . . ? F1' F5' 2.23(4) . . ? F1' F6' 2.35(4) . . ? F1' H11b 3.06(3) . . ? F1' H12a 2.66(3) . . ? F1' H13b 2.77(3) . . ? F1' H2a 2.86(3) . '3 465' ? F1' H2b 2.99(3) . . ? F1' H5a 2.62(3) . '3 465' ? F1' H8a 2.78(3) . '3 465' ? F2' F3' 2.19(4) . . ? F2' F4' 2.29(5) . . ? F2' F5' 2.25(4) . . ? F2' F6' 2.17(4) . . ? F2' H153 2.85(3) . '3 565' ? F2' H156 2.79(3) . '1 545' ? F2' H455 3.11(3) . . ? F2' H753 2.71(3) . '4 745' ? F3' F4' 2.25(4) . . ? F3' F5' 3.10(4) . . ? F3' F6' 2.14(4) . . ? F3' H155 2.82(2) . '1 545' ? F3' H2a 2.85(2) . '3 465' ? F3' H41b 3.33(2) . '1 455' ? F3' H5b 2.62(2) . '1 455' ? F3' H6a 2.89(2) . '1 455' ? F3' H6b 3.29(2) . '1 455' ? F3' H8a 3.13(2) . '3 465' ? F3' H9b 3.10(2) . '3 465' ? F4' F5' 2.25(4) . . ? F4' F6' 3.07(4) . . ? F4' H152 2.52(3) . '3 565' ? F4' H153 2.55(3) . '3 565' ? F4' H2b 3.22(3) . . ? F4' H8a 2.46(3) . '3 465' ? F4' H8b 3.04(3) . '3 465' ? F5' F6' 2.09(4) . . ? F5' H11b 2.50(3) . . ? F5' H2b 3.34(3) . . ? F5' H3a 3.21(3) . . ? F5' H752 3.22(3) . '4 745' ? F5' H02 2.75(3) . . ? F6' H13b 3.10(3) . . ? F6' H6a 2.50(3) . '1 455' ? F6' H752 3.13(3) . '4 745' ? F6' H753 2.57(3) . '4 745' ? F6' H05 3.26(3) . '1 455' ? H11a H11b 1.55131(19) . . ? H11a H12b 2.3679(2) . . ? H11a H13a 2.37686(18) . . ? H11a H9a 2.39067(16) . . ? H11a H01 1.92125(19) . . ? H11b H12a 2.3306(2) . . ? H11b H2b 2.3474(3) . . ? H11b H02 2.2072(2) . . ? H12a H12b 1.55131(19) . . ? H12a H13b 2.28854(18) . . ? H12a H2b 2.2262(2) . . ? H12b H13a 2.3596(2) . . ? H12b H9b 2.06487(17) . . ? H13a H13b 1.55133(16) . . ? H152 H153 2.3452(2) . . ? H153 H154 2.3325(4) . . ? H154 H155 2.34711(16) . . ? H155 H156 2.34582(19) . . ? H155 H9b 2.3574(3) . '3 475' ? H2a H2b 1.55129(11) . . ? H2a H3b 2.2571(4) . . ? H2a H5a 2.19531(17) . . ? H2a H8a 2.09910(17) . . ? H2a H9b 2.3158(3) . . ? H2b H3a 2.2595(2) . . ? H2b H3b 2.3565(2) . . ? H3a H3b 1.55134(18) . . ? H3a H41a 2.34552(16) . . ? H3b H42b 2.2646(3) . . ? H41a H41b 1.55136(12) . . ? H41a H42b 2.3553(3) . . ? H41a H03a 2.3585(2) . . ? H41b H42a 2.3188(3) . . ? H41b H05 2.1375(2) . . ? H42a H42b 1.55126(13) . . ? H42a H43b 2.3183(3) . . ? H42a H5b 2.2226(3) . . ? H43a H43b 1.55102(14) . . ? H452 H453 2.32465(16) . . ? H453 H454 2.34618(19) . . ? H454 H455 2.3565(3) . . ? H455 H456 2.35682(16) . . ? H5a H5b 1.55132(14) . . ? H5a H6b 2.27147(16) . . ? H5a H8a 1.9803(3) . . ? H5b H6a 2.2696(2) . . ? H5b H6b 2.3475(3) . . ? H6a H6b 1.55115(16) . . ? H6a H71b 2.3433(3) . . ? H6b H71a 2.3743(3) . . ? H71a H71b 1.55140(16) . . ? H71a H72b 2.29358(15) . . ? H71a H8b 2.12350(15) . . ? H71b H72a 2.34345(16) . . ? H71b H06 1.89694(15) . . ? H72a H72b 1.55122(16) . . ? H72a H73a 2.3247(3) . . ? H72a H06 2.2682(3) . . ? H72a H07a 2.3166(3) . . ? H72b H73a 2.3365(2) . . ? H72b H73b 2.32328(17) . . ? H72b H8b 2.2359(3) . . ? H72b H9a 2.32195(16) . . ? H73a H73b 1.55116(13) . . ? H752 H753 2.32711(16) . . ? H753 H754 2.3720(3) . . ? H754 H755 2.3461(2) . . ? H755 H756 2.33971(16) . . ? H8a H8b 1.5513(2) . . ? H8a H9b 2.28025(17) . . ? H8b H9a 2.28039(17) . . ? H8b H9b 2.3798(2) . . ? H9a H9b 1.55152(18) . . ? H01 H08b 2.2709(2) . . ? H02 H03a 2.2342(2) . . ? H03a H03b 1.55144(17) . . ? H03a H04a 2.20340(17) . . ? H03b H04b 2.20208(18) . . ? H04a H04b 1.55141(16) . . ? H04a H05 2.3248(2) . . ? H04a H08b 2.3423(3) . '4 745' ? H04b H08a 2.1576(2) . . ? H05 H06 2.1453(3) . . ? H06 H07a 2.2741(2) . . ? H07a H07b 1.55139(18) . . ? H07a H08b 2.19898(16) . . ? H07b H08a 2.20004(17) . . ? H08a H08b 1.5514(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 1896 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 16 _reflns_limit_l_min 0 _reflns_limit_l_max 41 _reflns_number_observed ? _reflns_d_resolution_high .726 _reflns_d_resolution_low 11.383 _diffrn_reflns_av_sigmaI/netI .054 _diffrn_reflns_theta_min 1.78 _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 .05 _refine_ls_wR_factor_all .044 _refine_ls_goodness_of_fit_all 1.418 _refine_ls_shift/su_mean .006 #========================================================================== # 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_dbcu # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C39 H45 Cl2 Cu1 N3' _chemical_formula_moiety ? _chemical_formula_weight 690.26 _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 16.974(2) _cell_length_b 12.331(2) _cell_length_c 17.456(2) _cell_angle_alpha 90.00000 _cell_angle_beta 101.945(2) _cell_angle_gamma 90.00000 _cell_volume 3574.5(8) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.283 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 7802 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu .791 _exptl_crystal_description prism _exptl_crystal_size_max .5 _exptl_crystal_size_mid .45 _exptl_crystal_size_min .3 _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 .664 _exptl_absorpt_correction_T_max .802 _diffrn_reflns_number 34673 _reflns_number_total 8951 _reflns_Friedel_coverage 0 _reflns_number_gt 7508 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.17 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .022 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _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 .028 _refine_ls_wR_factor_ref .039 _refine_ls_goodness_of_fit_ref 1.15 _refine_ls_number_reflns 7508 _refine_ls_number_parameters 586 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max .086 _refine_diff_density_min -.199 _refine_diff_density_max .437 _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 ? 0 156 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 180 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 12 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cu ? 0 4 .263 1.266 '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' 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 Cu .154427(10) .386002(13) .160424(10) .01896(8) Uani ? ? 1.00000 ? ? Cl1 .10265(2) .54964(3) .11337(2) .02825(16) Uani ? ? 1.00000 ? ? Cl2 .17279(2) .44294(3) .28719(2) .02776(16) Uani ? ? 1.00000 ? ? N1 .15116(7) .33140(10) .04494(7) .0232(5) Uani ? ? 1.00000 ? ? C11 .18410(10) .41347(15) -.00222(10) .0292(7) Uani ? ? 1.00000 ? ? C12 .26755(11) .45452(17) .03840(11) .0369(8) Uani ? ? 1.00000 ? ? C13 .28253(17) .5665(3) .00826(17) .0660(15) Uani ? ? 1.00000 ? ? C14 .36219(16) .6110(2) .04310(15) .0643(14) Uani ? ? 1.00000 ? ? C15 .42721(16) .6479(3) .06824(14) .0648(14) Uani ? ? 1.00000 ? ? C151 .50585(15) .6970(3) .09010(13) .0603(13) Uani ? ? 1.00000 ? ? C152 .57472(18) .6331(3) .10793(16) .0667(16) Uani ? ? 1.00000 ? ? C153 .65049(18) .6822(3) .12333(17) .0757(18) Uani ? ? 1.00000 ? ? C154 .65690(18) .7933(3) .11941(15) .0754(18) Uani ? ? 1.00000 ? ? C155 .5894(2) .8563(3) .10303(17) .0767(18) Uani ? ? 1.00000 ? ? C156 .5129(2) .8086(3) .08960(17) .0728(17) Uani ? ? 1.00000 ? ? C2 .19551(10) .22672(14) .04674(10) .0289(7) Uani ? ? 1.00000 ? ? C3 .25307(10) .21101(14) .12440(10) .0281(7) Uani ? ? 1.00000 ? ? N4 .21322(7) .23842(10) .19052(7) .0231(5) Uani ? ? 1.00000 ? ? C41 .27579(10) .23772(13) .26507(9) .0274(7) Uani ? ? 1.00000 ? ? C42 .34335(10) .31993(14) .26771(10) .0277(7) Uani ? ? 1.00000 ? ? C43 .38341(12) .34039(15) .35337(11) .0348(8) Uani ? ? 1.00000 ? ? C44 .45958(11) .40040(13) .36475(10) .0309(7) Uani ? ? 1.00000 ? ? C45 .52335(11) .44541(13) .37577(10) .0310(7) Uani ? ? 1.00000 ? ? C451 .60195(10) .49545(13) .38952(10) .0303(7) Uani ? ? 1.00000 ? ? C452 .63727(11) .53434(14) .46396(11) .0326(8) Uani ? ? 1.00000 ? ? C453 .71426(12) .57880(17) .47823(12) .0403(9) Uani ? ? 1.00000 ? ? C454 .75581(12) .58672(18) .41800(14) .0447(10) Uani ? ? 1.00000 ? ? C455 .72092(13) .55013(18) .34391(14) .0458(10) Uani ? ? 1.00000 ? ? C456 .64479(12) .50432(16) .32938(12) .0392(9) Uani ? ? 1.00000 ? ? C5 .14981(10) .15573(13) .19702(10) .0287(7) Uani ? ? 1.00000 ? ? C6 .07031(10) .20540(13) .20694(10) .0277(7) Uani ? ? 1.00000 ? ? N7 .04164(7) .28906(10) .14722(7) .0234(5) Uani ? ? 1.00000 ? ? C71 -.02105(9) .36025(13) .16723(10) .0264(7) Uani ? ? 1.00000 ? ? C72 -.10036(10) .30668(15) .17457(11) .0311(7) Uani ? ? 1.00000 ? ? C73 -.15855(10) .39506(15) .19098(11) .0310(7) Uani ? ? 1.00000 ? ? C74 -.23889(10) .35251(15) .19259(10) .0314(7) Uani ? ? 1.00000 ? ? C75 -.30274(10) .31208(15) .19286(10) .0319(8) Uani ? ? 1.00000 ? ? C751 -.37696(10) .25634(15) .19479(11) .0318(7) Uani ? ? 1.00000 ? ? C752 -.43469(12) .2406(2) .12688(13) .0466(10) Uani ? ? 1.00000 ? ? C753 -.50379(13) .1805(2) .12953(16) .0569(13) Uani ? ? 1.00000 ? ? C754 -.51526(13) .13725(17) .19930(16) .0496(11) Uani ? ? 1.00000 ? ? C755 -.45946(12) .15517(17) .26704(15) .0450(10) Uani ? ? 1.00000 ? ? C756 -.39024(11) .21403(16) .26535(12) .0386(9) Uani ? ? 1.00000 ? ? C8 .02201(9) .24815(14) .06569(9) .0271(7) Uani ? ? 1.00000 ? ? C9 .06334(9) .31551(14) .01175(9) .0263(7) Uani ? ? 1.00000 ? ? H11a .1476(11) .4735(16) -.0084(11) .023(4) Uiso ? ? 1.00000 ? ? H11b .1869(13) .3834(17) -.0546(13) .033(5) Uiso ? ? 1.00000 ? ? H12a .3106(15) .403(2) .0306(14) .044(6) Uiso ? ? 1.00000 ? ? H12b .2709(14) .467(2) .0957(14) .043(6) Uiso ? ? 1.00000 ? ? H13a .241(2) .618(2) .0160(18) .069(10) Uiso ? ? 1.00000 ? ? H13b .276(2) .561(3) -.050(2) .088(10) Uiso ? ? 1.00000 ? ? H152 .5700(16) .556(2) .1086(15) .050(7) Uiso ? ? 1.00000 ? ? H153 .696(2) .633(3) .139(2) .105(14) Uiso ? ? 1.00000 ? ? H154 .709(2) .828(3) .1298(19) .083(10) Uiso ? ? 1.00000 ? ? H155 .589(2) .934(3) .096(2) .083(10) Uiso ? ? 1.00000 ? ? H156 .470(2) .851(3) .075(2) .076(10) Uiso ? ? 1.00000 ? ? H2a .2257(13) .2240(18) .0043(13) .037(5) Uiso ? ? 1.00000 ? ? H2b .1571(12) .1678(17) .0369(11) .028(5) Uiso ? ? 1.00000 ? ? H3a .2979(12) .2601(16) .1272(11) .027(5) Uiso ? ? 1.00000 ? ? H3b .2709(13) .1377(18) .1313(12) .032(5) Uiso ? ? 1.00000 ? ? H41a .2996(12) .1657(17) .2727(11) .029(5) Uiso ? ? 1.00000 ? ? H41b .2461(12) .2547(17) .3074(12) .032(5) Uiso ? ? 1.00000 ? ? H42a .3234(13) .3892(18) .2464(13) .038(6) Uiso ? ? 1.00000 ? ? H42b .3823(12) .2935(17) .2403(12) .030(5) Uiso ? ? 1.00000 ? ? H43a .3899(14) .273(2) .3774(14) .043(6) Uiso ? ? 1.00000 ? ? H43b .3468(15) .379(2) .3801(15) .049(7) Uiso ? ? 1.00000 ? ? H452 .6094(12) .5298(17) .5052(12) .031(5) Uiso ? ? 1.00000 ? ? H453 .7395(18) .605(2) .5279(18) .068(9) Uiso ? ? 1.00000 ? ? H454 .8099(17) .618(2) .4302(15) .057(7) Uiso ? ? 1.00000 ? ? H455 .7494(15) .556(2) .3043(14) .049(7) Uiso ? ? 1.00000 ? ? H456 .6205(14) .480(2) .2802(14) .044(6) Uiso ? ? 1.00000 ? ? H5a .1701(12) .1082(16) .2401(12) .029(5) Uiso ? ? 1.00000 ? ? H5b .1421(12) .1102(15) .1506(11) .026(5) Uiso ? ? 1.00000 ? ? H6a .0774(12) .2418(17) .2580(12) .031(5) Uiso ? ? 1.00000 ? ? H6b .0325(11) .1467(16) .2050(11) .023(4) Uiso ? ? 1.00000 ? ? H71a -.0331(12) .4154(17) .1269(12) .027(5) Uiso ? ? 1.00000 ? ? H71b .0018(12) .3959(16) .2176(12) .028(5) Uiso ? ? 1.00000 ? ? H72a -.0905(13) .2531(18) .2181(13) .038(6) Uiso ? ? 1.00000 ? ? H72b -.1232(14) .271(2) .1281(14) .042(6) Uiso ? ? 1.00000 ? ? H73a -.1639(14) .452(2) .1511(14) .045(6) Uiso ? ? 1.00000 ? ? H73b -.1345(12) .4327(18) .2406(12) .033(5) Uiso ? ? 1.00000 ? ? H752 -.4301(15) .275(2) .0803(14) .049(6) Uiso ? ? 1.00000 ? ? H753 -.5422(17) .172(2) .0826(17) .065(8) Uiso ? ? 1.00000 ? ? H754 -.5630(17) .097(2) .1968(16) .058(7) Uiso ? ? 1.00000 ? ? H755 -.4675(17) .124(2) .3128(17) .061(8) Uiso ? ? 1.00000 ? ? H756 -.3499(16) .226(2) .3138(15) .055(7) Uiso ? ? 1.00000 ? ? H8a -.0379(12) .2505(17) .0445(12) .031(5) Uiso ? ? 1.00000 ? ? H8b .0376(11) .1712(16) .0647(11) .023(4) Uiso ? ? 1.00000 ? ? H9a .0577(12) .2790(17) -.0381(12) .029(5) Uiso ? ? 1.00000 ? ? H9b .0386(12) .3886(16) .0056(11) .027(5) 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 Cu .01710(9) .01541(9) .02263(9) -.00044(6) .00013(6) -.00081(6) Cl1 .02759(18) .01935(16) .03416(19) .00121(13) -.00209(14) .00069(13) Cl2 .02874(18) .02452(17) .02841(18) .00243(13) .00215(14) -.00531(13) N1 .0203(6) .0249(6) .0232(6) -.0017(5) .0016(5) -.0008(5) C11 .0262(7) .0355(8) .0251(7) -.0057(7) .0037(6) .0021(6) C12 .0272(8) .0463(11) .0356(9) -.0102(7) .0030(7) .0050(8) C13 .0515(14) .079(2) .0571(14) -.0358(14) -.0134(11) .0289(14) C14 .0585(14) .0780(18) .0498(13) -.0368(13) -.0044(11) .0200(12) C15 .0586(14) .0855(19) .0456(12) -.0380(14) .0003(10) .0102(12) C151 .0535(13) .090(2) .0354(10) -.0405(14) .0044(9) -.0029(11) C152 .0583(16) .093(2) .0511(13) -.0313(15) .0165(11) -.0204(14) C153 .0515(15) .122(3) .0576(15) -.0297(18) .0196(12) -.0354(17) C154 .0594(16) .126(3) .0434(12) -.0559(19) .0168(11) -.0272(15) C155 .075(2) .099(2) .0508(14) -.0528(19) -.0014(13) -.0014(15) C156 .0595(16) .096(2) .0551(15) -.0388(17) -.0062(12) .0061(15) C2 .0271(7) .0295(8) .0294(8) .0025(6) .0040(6) -.0068(6) C3 .0261(7) .0247(7) .0318(8) .0053(6) .0016(6) -.0050(6) N4 .0225(6) .0180(6) .0256(6) .0013(5) -.0020(5) -.0012(5) C41 .0278(7) .0216(7) .0279(7) .0037(6) -.0052(6) .0008(6) C42 .0236(7) .0276(8) .0293(7) .0043(6) -.0008(6) -.0025(6) C43 .0404(10) .0287(8) .0311(8) -.0081(7) -.0027(7) -.0010(7) C44 .0355(9) .0247(7) .0281(8) .0016(6) -.0032(6) -.0012(6) C45 .0334(8) .0243(7) .0314(8) .0040(6) -.0022(6) -.0013(6) C451 .0292(8) .0228(7) .0372(8) .0056(6) .0029(6) .0018(6) C452 .0304(8) .0313(8) .0347(9) .0006(7) .0038(7) .0012(7) C453 .0331(9) .0417(10) .0428(10) -.0016(8) .0001(8) -.0022(8) C454 .0289(9) .0447(11) .0608(13) .0007(8) .0095(8) .0003(9) C455 .0418(10) .0479(12) .0528(12) .0051(9) .0212(9) .0007(9) C456 .0419(10) .0370(9) .0385(10) .0054(8) .0080(8) -.0041(8) C5 .0315(8) .0185(7) .0331(8) -.0019(6) .0001(6) .0018(6) C6 .0296(8) .0223(7) .0305(8) -.0056(6) .0050(6) .0023(6) N7 .0210(6) .0224(6) .0256(6) -.0027(5) .0019(5) -.0009(5) C71 .0193(7) .0263(7) .0333(8) -.0036(6) .0046(6) -.0004(6) C72 .0218(7) .0333(8) .0390(9) -.0067(6) .0079(6) -.0006(7) C73 .0216(7) .0363(9) .0356(9) -.0039(6) .0071(6) .0036(7) C74 .0244(7) .0393(9) .0311(8) -.0007(6) .0069(6) .0035(7) C75 .0256(8) .0383(9) .0333(8) -.0010(7) .0096(6) .0023(7) C751 .0222(7) .0343(8) .0411(9) -.0006(6) .0118(6) .0001(7) C752 .0307(9) .0679(14) .0421(10) -.0109(9) .0099(8) -.0013(10) C753 .0294(10) .0742(16) .0658(15) -.0158(10) .0068(10) -.0137(13) C754 .0326(10) .0360(10) .0873(17) -.0080(8) .0286(11) -.0043(10) C755 .0386(10) .0345(10) .0692(14) .0013(8) .0282(10) .0118(9) C756 .0319(9) .0389(10) .0479(11) .0016(7) .0149(8) .0103(8) C8 .0232(7) .0275(8) .0281(7) -.0066(6) -.0004(6) -.0035(6) C9 .0213(7) .0310(8) .0241(7) -.0051(6) -.0013(5) -.0028(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 Cu Cl1 . . 2.2847(5) ? Cu Cl2 . . 2.2805(5) ? Cu N1 . . 2.1152(13) ? Cu N4 . . 2.0896(13) ? Cu N7 . . 2.2281(13) ? N1 C11 . . 1.485(2) ? N1 C2 . . 1.491(2) ? N1 C9 . . 1.4962(19) ? C11 C12 . . 1.533(2) ? C11 H11a . . .96(2) ? C11 H11b . . 1.00(2) ? C12 C13 . . 1.518(4) ? C12 H12a . . 1.00(3) ? C12 H12b . . 1.00(2) ? C13 C14 . . 1.469(4) ? C13 H13a . . .98(3) ? C13 H13b . . 1.00(4) ? C14 C15 . . 1.190(4) ? C15 C151 . . 1.443(4) ? C151 C152 . . 1.390(4) ? C151 C156 . . 1.381(5) ? C152 C153 . . 1.396(4) ? C152 H152 . . .95(3) ? C153 C154 . . 1.378(6) ? C153 H153 . . .97(4) ? C154 C155 . . 1.365(5) ? C154 H154 . . .96(3) ? C155 C156 . . 1.400(5) ? C155 H155 . . .97(4) ? C156 H156 . . .89(3) ? C2 C3 . . 1.510(2) ? C2 H2a . . .98(2) ? C2 H2b . . .97(2) ? C3 N4 . . 1.492(2) ? C3 H3a . . .97(2) ? C3 H3b . . .95(2) ? N4 C41 . . 1.4999(19) ? N4 C5 . . 1.504(2) ? C41 C42 . . 1.524(2) ? C41 H41a . . .97(2) ? C41 H41b . . 1.00(2) ? C42 C43 . . 1.530(2) ? C42 H42a . . .96(2) ? C42 H42b . . .95(2) ? C43 C44 . . 1.467(3) ? C43 H43a . . .93(2) ? C43 H43b . . .98(3) ? C44 C45 . . 1.196(2) ? C45 C451 . . 1.444(2) ? C451 C452 . . 1.398(2) ? C451 C456 . . 1.400(3) ? C452 C453 . . 1.391(3) ? C452 H452 . . .94(2) ? C453 C454 . . 1.385(3) ? C453 H453 . . .94(3) ? C454 C455 . . 1.382(3) ? C454 H454 . . .98(3) ? C455 C456 . . 1.385(3) ? C455 H455 . . .92(3) ? C456 H456 . . .92(2) ? C5 C6 . . 1.524(2) ? C5 H5a . . .96(2) ? C5 H5b . . .97(2) ? C6 N7 . . 1.476(2) ? C6 H6a . . .98(2) ? C6 H6b . . .96(2) ? N7 C71 . . 1.476(2) ? N7 C8 . . 1.482(2) ? C71 C72 . . 1.529(2) ? C71 H71a . . .97(2) ? C71 H71b . . .99(2) ? C72 C73 . . 1.537(3) ? C72 H72a . . 1.00(2) ? C72 H72b . . .93(2) ? C73 C74 . . 1.467(2) ? C73 H73a . . .98(2) ? C73 H73b . . .99(2) ? C74 C75 . . 1.194(2) ? C75 C751 . . 1.442(2) ? C751 C752 . . 1.386(3) ? C751 C756 . . 1.398(3) ? C752 C753 . . 1.396(3) ? C752 H752 . . .94(3) ? C753 C754 . . 1.380(4) ? C753 H753 . . .94(3) ? C754 C755 . . 1.371(3) ? C754 H754 . . .94(3) ? C755 C756 . . 1.387(3) ? C755 H755 . . .92(3) ? C756 H756 . . .98(2) ? C8 C9 . . 1.530(2) ? C8 H8a . . 1.01(2) ? C8 H8b . . .99(2) ? C9 H9a . . .97(2) ? C9 H9b . . .99(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 Cu Cl2 . . . 92.413(16) ? Cl1 Cu N1 . . . 90.36(4) ? Cl1 Cu N4 . . . 171.00(4) ? Cl1 Cu N7 . . . 100.27(3) ? Cl2 Cu N1 . . . 173.77(4) ? Cl2 Cu N4 . . . 93.55(4) ? Cl2 Cu N7 . . . 101.97(4) ? N1 Cu N4 . . . 83.07(5) ? N1 Cu N7 . . . 83.00(5) ? N4 Cu N7 . . . 85.08(5) ? Cu N1 C11 . . . 111.89(10) ? Cu N1 C2 . . . 109.99(9) ? Cu N1 C9 . . . 103.78(10) ? C11 N1 C2 . . . 110.81(13) ? C11 N1 C9 . . . 109.51(11) ? C2 N1 C9 . . . 110.67(12) ? N1 C11 C12 . . . 112.74(13) ? N1 C11 H11a . . . 106.3(12) ? N1 C11 H11b . . . 110.5(12) ? C12 C11 H11a . . . 108.2(11) ? C12 C11 H11b . . . 109.4(12) ? H11a C11 H11b . . . 109.7(16) ? C11 C12 C13 . . . 110.19(16) ? C11 C12 H12a . . . 111.0(13) ? C11 C12 H12b . . . 111.7(13) ? C13 C12 H12a . . . 110.6(15) ? C13 C12 H12b . . . 102.9(14) ? H12a C12 H12b . . . 110.1(18) ? C12 C13 C14 . . . 113.7(2) ? C12 C13 H13a . . . 111(2) ? C12 C13 H13b . . . 108(2) ? C14 C13 H13a . . . 109.5(18) ? C14 C13 H13b . . . 110(2) ? H13a C13 H13b . . . 104(3) ? C13 C14 C15 . . . 177.2(3) ? C14 C15 C151 . . . 173.7(3) ? C15 C151 C152 . . . 120.7(3) ? C15 C151 C156 . . . 119.5(3) ? C152 C151 C156 . . . 119.7(3) ? C151 C152 C153 . . . 119.7(3) ? C151 C152 H152 . . . 119.9(16) ? C153 C152 H152 . . . 120.4(16) ? C152 C153 C154 . . . 120.0(3) ? C152 C153 H153 . . . 115(2) ? C154 C153 H153 . . . 125(2) ? C153 C154 C155 . . . 120.3(3) ? C153 C154 H154 . . . 121(2) ? C155 C154 H154 . . . 119(2) ? C154 C155 C156 . . . 120.3(4) ? C154 C155 H155 . . . 125(2) ? C156 C155 H155 . . . 114(2) ? C151 C156 C155 . . . 119.8(3) ? C151 C156 H156 . . . 121(2) ? C155 C156 H156 . . . 118(2) ? N1 C2 C3 . . . 111.09(13) ? N1 C2 H2a . . . 110.6(13) ? N1 C2 H2b . . . 109.1(12) ? C3 C2 H2a . . . 109.3(12) ? C3 C2 H2b . . . 110.5(11) ? H2a C2 H2b . . . 106.1(18) ? C2 C3 N4 . . . 110.65(13) ? C2 C3 H3a . . . 108.8(11) ? C2 C3 H3b . . . 111.4(12) ? N4 C3 H3a . . . 107.3(12) ? N4 C3 H3b . . . 107.5(14) ? H3a C3 H3b . . . 111.1(18) ? Cu N4 C3 . . . 105.79(9) ? Cu N4 C41 . . . 116.02(9) ? Cu N4 C5 . . . 107.31(9) ? C3 N4 C41 . . . 108.47(12) ? C3 N4 C5 . . . 110.54(12) ? C41 N4 C5 . . . 108.66(12) ? N4 C41 C42 . . . 114.56(13) ? N4 C41 H41a . . . 108.9(11) ? N4 C41 H41b . . . 105.4(11) ? C42 C41 H41a . . . 108.3(12) ? C42 C41 H41b . . . 109.3(12) ? H41a C41 H41b . . . 110.4(17) ? C41 C42 C43 . . . 108.58(15) ? C41 C42 H42a . . . 112.0(13) ? C41 C42 H42b . . . 110.7(12) ? C43 C42 H42a . . . 106.3(13) ? C43 C42 H42b . . . 109.5(11) ? H42a C42 H42b . . . 110(2) ? C42 C43 C44 . . . 114.62(16) ? C42 C43 H43a . . . 106.2(14) ? C42 C43 H43b . . . 110.5(14) ? C44 C43 H43a . . . 111.9(14) ? C44 C43 H43b . . . 108.5(14) ? H43a C43 H43b . . . 105(2) ? C43 C44 C45 . . . 177.09(18) ? C44 C45 C451 . . . 177.64(18) ? C45 C451 C452 . . . 120.30(17) ? C45 C451 C456 . . . 120.95(16) ? C452 C451 C456 . . . 118.74(16) ? C451 C452 C453 . . . 120.50(19) ? C451 C452 H452 . . . 120.3(12) ? C453 C452 H452 . . . 119.2(12) ? C452 C453 C454 . . . 119.92(19) ? C452 C453 H453 . . . 122(2) ? C454 C453 H453 . . . 118(2) ? C453 C454 C455 . . . 120.0(2) ? C453 C454 H454 . . . 117.7(17) ? C455 C454 H454 . . . 122.3(17) ? C454 C455 C456 . . . 120.5(2) ? C454 C455 H455 . . . 119.1(14) ? C456 C455 H455 . . . 120.4(14) ? C451 C456 C455 . . . 120.30(18) ? C451 C456 H456 . . . 118.1(16) ? C455 C456 H456 . . . 121.6(16) ? N4 C5 C6 . . . 113.61(13) ? N4 C5 H5a . . . 109.1(12) ? N4 C5 H5b . . . 107.7(12) ? C6 C5 H5a . . . 109.9(13) ? C6 C5 H5b . . . 110.9(11) ? H5a C5 H5b . . . 105.4(16) ? C5 C6 N7 . . . 111.77(14) ? C5 C6 H6a . . . 110.0(12) ? C5 C6 H6b . . . 107.1(12) ? N7 C6 H6a . . . 106.4(12) ? N7 C6 H6b . . . 112.4(10) ? H6a C6 H6b . . . 109.2(17) ? Cu N7 C6 . . . 98.71(9) ? Cu N7 C71 . . . 107.61(9) ? Cu N7 C8 . . . 107.44(10) ? C6 N7 C71 . . . 113.40(13) ? C6 N7 C8 . . . 114.60(12) ? C71 N7 C8 . . . 113.57(11) ? N7 C71 C72 . . . 116.96(14) ? N7 C71 H71a . . . 107.5(13) ? N7 C71 H71b . . . 107.8(12) ? C72 C71 H71a . . . 107.9(12) ? C72 C71 H71b . . . 107.9(13) ? H71a C71 H71b . . . 108.5(17) ? C71 C72 C73 . . . 108.68(14) ? C71 C72 H72a . . . 109.8(13) ? C71 C72 H72b . . . 110.2(16) ? C73 C72 H72a . . . 110.0(14) ? C73 C72 H72b . . . 109.2(14) ? H72a C72 H72b . . . 109(2) ? C72 C73 C74 . . . 112.69(15) ? C72 C73 H73a . . . 110.3(15) ? C72 C73 H73b . . . 109.3(12) ? C74 C73 H73a . . . 108.8(13) ? C74 C73 H73b . . . 111.4(13) ? H73a C73 H73b . . . 104.0(18) ? C73 C74 C75 . . . 176.2(2) ? C74 C75 C751 . . . 176.0(2) ? C75 C751 C752 . . . 120.88(18) ? C75 C751 C756 . . . 119.96(15) ? C752 C751 C756 . . . 119.12(17) ? C751 C752 C753 . . . 119.7(2) ? C751 C752 H752 . . . 120.4(15) ? C753 C752 H752 . . . 119.6(15) ? C752 C753 C754 . . . 120.5(2) ? C752 C753 H753 . . . 118(2) ? C754 C753 H753 . . . 122(2) ? C753 C754 C755 . . . 120.0(2) ? C753 C754 H754 . . . 116.0(16) ? C755 C754 H754 . . . 123.9(16) ? C754 C755 C756 . . . 120.2(2) ? C754 C755 H755 . . . 118.7(17) ? C756 C755 H755 . . . 121.0(17) ? C751 C756 C755 . . . 120.39(18) ? C751 C756 H756 . . . 119.6(17) ? C755 C756 H756 . . . 120.0(17) ? N7 C8 C9 . . . 111.45(13) ? N7 C8 H8a . . . 110.6(12) ? N7 C8 H8b . . . 109.7(11) ? C9 C8 H8a . . . 108.3(12) ? C9 C8 H8b . . . 110.6(12) ? H8a C8 H8b . . . 106.0(16) ? N1 C9 C8 . . . 112.32(12) ? N1 C9 H9a . . . 108.3(12) ? N1 C9 H9b . . . 106.7(11) ? C8 C9 H9a . . . 109.2(13) ? C8 C9 H9b . . . 108.8(13) ? H9a C9 H9b . . . 111.5(16) ? 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 Cu C11 3.0035(18) . . ? Cu C12 3.260(2) . . ? Cu C2 2.9757(18) . . ? Cu C3 2.8793(18) . . ? Cu C41 3.0604(15) . . ? Cu C42 3.4595(15) . . ? Cu C5 2.9151(17) . . ? Cu C6 2.8527(17) . . ? Cu C71 3.0222(17) . . ? Cu C8 3.0229(15) . . ? Cu C9 2.8671(15) . . ? Cu H11a 3.12(2) . . ? Cu H12b 2.67(3) . . ? Cu H3a 3.04(2) . . ? Cu H41b 3.16(2) . . ? Cu H42a 2.95(2) . . ? Cu H6a 2.95(2) . . ? Cu H71a 3.14(2) . . ? Cu H71b 2.97(2) . . ? Cu H9b 2.994(18) . . ? Cl1 N1 3.1232(14) . . ? Cl1 N7 3.4641(14) . . ? Cl1 H11a 2.58(2) . . ? Cl1 H41a 2.718(19) . 2 ? Cl1 H43a 2.75(2) . 2 ? Cl1 H9b 2.80(2) . . ? Cl2 N4 3.1871(14) . . ? Cl2 N7 3.5034(13) . . ? Cl2 H41b 2.62(2) . . ? Cl2 H754 2.72(3) . '2 455' ? N1 C12 2.513(2) . . ? N1 C3 2.475(2) . . ? N1 N4 2.7882(17) . . ? N1 C5 3.430(2) . . ? N1 N7 2.879(2) . . ? N1 C8 2.514(2) . . ? N1 H11a 1.98(2) . . ? N1 H11b 2.06(2) . . ? N1 H12a 2.91(3) . . ? N1 H12b 2.64(2) . . ? N1 H2a 2.06(2) . . ? N1 H2b 2.03(2) . . ? N1 H3a 2.750(19) . . ? N1 H3b 3.29(2) . . ? N1 H5b 3.31(2) . . ? N1 H8a 3.36(2) . . ? N1 H8b 2.83(2) . . ? N1 H9a 2.020(18) . . ? N1 H9b 2.02(2) . . ? C11 C13 2.502(4) . . ? C11 C2 2.450(3) . . ? C11 C9 2.435(2) . . ? C11 H12a 2.11(2) . . ? C11 H12b 2.12(2) . . ? C11 H13a 2.69(3) . . ? C11 H13b 2.64(4) . . ? C11 H2a 2.44(2) . . ? C11 H9a 2.68(2) . . ? C11 H9b 2.52(2) . . ? C12 C14 2.501(3) . . ? C12 H11a 2.044(18) . . ? C12 H11b 2.09(2) . . ? C12 H13a 2.08(3) . . ? C12 H13b 2.06(4) . . ? C13 C15 2.659(4) . . ? C13 H11a 2.52(2) . . ? C13 H12a 2.09(2) . . ? C13 H12b 2.00(2) . . ? C14 C151 2.630(4) . . ? C14 H12b 2.64(2) . . ? C14 H13a 2.02(3) . . ? C14 H13b 2.04(3) . . ? C15 C152 2.463(4) . . ? C15 C156 2.440(5) . . ? C15 H152 2.63(3) . . ? C15 H156 2.60(3) . . ? C151 C153 2.410(4) . . ? C151 C154 2.776(4) . . ? C151 C155 2.405(5) . . ? C151 H152 2.04(3) . . ? C151 H156 2.00(3) . . ? C152 C154 2.403(5) . . ? C152 C155 2.766(6) . . ? C152 C156 2.397(5) . . ? C152 H153 2.01(4) . . ? C153 C155 2.380(6) . . ? C153 C156 2.768(5) . . ? C153 H152 2.05(3) . . ? C153 H154 2.04(3) . . ? C154 C156 2.399(4) . . ? C154 H153 2.09(4) . . ? C154 H155 2.08(4) . . ? C155 H154 2.01(3) . . ? C155 H156 1.98(3) . . ? C156 H155 2.00(4) . . ? C2 N4 2.469(2) . . ? C2 N7 3.519(2) . . ? C2 C9 2.457(2) . . ? C2 H11b 2.60(2) . . ? C2 H3a 2.038(18) . . ? C2 H3b 2.06(2) . . ? C2 H5b 2.62(2) . . ? C2 H9a 2.578(18) . . ? C3 C41 2.428(2) . . ? C3 C42 2.970(2) . . ? C3 C5 2.462(3) . . ? C3 H2a 2.06(2) . . ? C3 H2b 2.059(18) . . ? C3 H41a 2.61(2) . . ? C3 H5b 2.38(2) . . ? N4 C42 2.544(2) . . ? N4 C6 2.534(2) . . ? N4 N7 2.9209(18) . . ? N4 C8 3.5169(19) . . ? N4 H2a 3.31(2) . . ? N4 H2b 2.79(2) . . ? N4 H3a 2.00(2) . . ? N4 H3b 2.00(2) . . ? N4 H41a 2.035(19) . . ? N4 H41b 2.01(2) . . ? N4 H42a 2.67(2) . . ? N4 H42b 2.90(2) . . ? N4 H5a 2.03(2) . . ? N4 H5b 2.023(19) . . ? N4 H6a 2.80(2) . . ? N4 H6b 3.33(2) . . ? C41 C43 2.480(2) . . ? C41 C5 2.440(2) . . ? C41 H3a 2.53(2) . . ? C41 H3b 2.63(2) . . ? C41 H42a 2.09(2) . . ? C41 H42b 2.06(2) . . ? C41 H43a 2.49(2) . . ? C41 H5a 2.37(2) . . ? C42 C44 2.523(2) . . ? C42 H3a 2.525(19) . . ? C42 H41a 2.05(2) . . ? C42 H41b 2.08(2) . . ? C42 H43a 2.00(2) . . ? C42 H43b 2.08(3) . . ? C43 C45 2.662(3) . . ? C43 H41b 2.53(2) . . ? C43 H42a 2.03(2) . . ? C43 H42b 2.05(2) . . ? C44 C451 2.640(2) . . ? C44 H42b 2.65(2) . . ? C44 H43a 2.01(2) . . ? C44 H43b 2.00(3) . . ? C45 C452 2.466(2) . . ? C45 C456 2.474(3) . . ? C45 H452 2.64(2) . . ? C45 H456 2.61(3) . . ? C451 C453 2.422(2) . . ? C451 C454 2.792(3) . . ? C451 C455 2.415(3) . . ? C451 H452 2.04(2) . . ? C451 H456 2.01(3) . . ? C452 C454 2.404(3) . . ? C452 C455 2.771(3) . . ? C452 C456 2.408(3) . . ? C452 H453 2.05(3) . . ? C453 C455 2.397(3) . . ? C453 C456 2.778(3) . . ? C453 H452 2.03(2) . . ? C453 H454 2.03(3) . . ? C454 C456 2.402(3) . . ? C454 H453 2.01(3) . . ? C454 H455 2.00(3) . . ? C455 H454 2.07(2) . . ? C455 H456 2.03(2) . . ? C456 H455 2.02(3) . . ? C5 N7 2.484(2) . . ? C5 H3b 2.56(2) . . ? C5 H41a 2.615(19) . . ? C5 H41b 2.56(2) . . ? C5 H6a 2.08(2) . . ? C5 H6b 2.03(2) . . ? C5 H8b 2.679(17) . . ? C6 C71 2.467(2) . . ? C6 C8 2.489(2) . . ? C6 H5a 2.06(2) . . ? C6 H5b 2.08(2) . . ? C6 H71b 2.65(2) . . ? C6 H8b 2.466(19) . . ? N7 C72 2.561(2) . . ? N7 C9 2.489(2) . . ? N7 H2b 3.37(2) . . ? N7 H5a 3.30(2) . . ? N7 H5b 2.78(2) . . ? N7 H6a 1.99(2) . . ? N7 H6b 2.05(2) . . ? N7 H71a 1.99(2) . . ? N7 H71b 2.01(2) . . ? N7 H72a 2.81(2) . . ? N7 H72b 2.76(2) . . ? N7 H8a 2.065(19) . . ? N7 H8b 2.04(2) . . ? N7 H9a 3.30(2) . . ? N7 H9b 2.75(2) . . ? C71 C73 2.491(2) . . ? C71 C8 2.474(2) . . ? C71 H6a 2.52(2) . . ? C71 H72a 2.09(2) . . ? C71 H72b 2.05(2) . . ? C71 H73a 2.64(2) . . ? C71 H73b 2.68(2) . . ? C71 H8a 2.50(2) . . ? C72 C74 2.501(3) . . ? C72 H71a 2.05(2) . . ? C72 H71b 2.06(2) . . ? C72 H73a 2.09(2) . . ? C72 H73b 2.09(2) . . ? C73 C75 2.659(2) . . ? C73 H71a 2.61(2) . . ? C73 H71b 2.66(2) . . ? C73 H72a 2.10(2) . . ? C73 H72b 2.04(2) . . ? C74 C751 2.634(2) . . ? C74 H13b 2.66(3) . '3 565' ? C74 H72b 2.66(3) . . ? C74 H73a 2.01(3) . . ? C74 H73b 2.05(2) . . ? C75 C752 2.460(3) . . ? C75 C756 2.459(3) . . ? C75 H752 2.64(2) . . ? C75 H756 2.63(3) . . ? C751 C753 2.407(3) . . ? C751 C754 2.784(3) . . ? C751 C755 2.416(3) . . ? C751 H752 2.03(2) . . ? C751 H756 2.07(3) . . ? C752 C754 2.410(4) . . ? C752 C755 2.774(4) . . ? C752 C756 2.401(3) . . ? C752 H753 2.02(3) . . ? C753 C755 2.383(4) . . ? C753 C756 2.760(3) . . ? C753 H752 2.03(3) . . ? C753 H754 1.98(3) . . ? C754 C756 2.391(3) . . ? C754 H753 2.04(3) . . ? C754 H755 1.99(3) . . ? C755 H754 2.05(3) . . ? C755 H756 2.06(3) . . ? C756 H755 2.02(3) . . ? C8 H2b 2.64(2) . . ? C8 H71a 2.59(2) . . ? C8 H9a 2.06(2) . . ? C8 H9b 2.07(2) . . ? C9 H11a 2.48(2) . . ? C9 H2b 2.40(2) . . ? C9 H8a 2.08(2) . . ? C9 H8b 2.09(2) . . ? H11a H11b 1.60(3) . . ? H11a H13a 2.36(4) . . ? H11a H9b 2.18(3) . . ? H11b H12a 2.32(3) . . ? H11b H2a 2.25(3) . . ? H12a H12b 1.64(4) . . ? H12b H13a 2.31(4) . . ? H13a H13b 1.56(5) . . ? H13b H73a 2.32(4) . '3 565' ? H152 H153 2.29(5) . . ? H154 H155 2.39(5) . . ? H155 H156 2.22(5) . . ? H2a H2b 1.56(3) . . ? H2a H3a 2.28(3) . . ? H2b H3b 2.30(3) . . ? H2b H5b 2.17(3) . . ? H2b H8b 2.18(3) . . ? H2b H9a 2.35(3) . . ? H3a H3b 1.58(3) . . ? H3a H42b 2.22(3) . . ? H3b H5b 2.31(3) . . ? H41a H41b 1.62(3) . . ? H41a H42b 2.26(3) . . ? H41a H5a 2.27(3) . . ? H41b H5a 2.38(3) . . ? H42a H42b 1.56(3) . . ? H42a H43b 2.29(3) . . ? H42b H43a 2.39(3) . . ? H43a H43b 1.51(3) . . ? H43b H452 2.28(3) . '3 666' ? H43b H453 2.40(4) . '3 666' ? H452 H453 2.35(4) . . ? H453 H454 2.28(5) . . ? H454 H455 2.35(3) . . ? H455 H456 2.34(3) . . ? H5a H5b 1.54(3) . . ? H5a H6a 2.34(3) . . ? H5a H6b 2.34(3) . . ? H5b H6b 2.30(3) . . ? H5b H8b 2.20(2) . . ? H6a H6b 1.59(3) . . ? H6a H71b 2.32(3) . . ? H71a H71b 1.59(3) . . ? H71a H72b 2.35(3) . . ? H71a H73a 2.39(3) . . ? H71b H72a 2.36(3) . . ? H72a H72b 1.57(3) . . ? H72a H73b 2.40(3) . . ? H72b H8a 2.27(3) . . ? H73a H73b 1.56(3) . . ? H752 H753 2.30(4) . . ? H753 H754 2.29(4) . . ? H754 H755 2.34(4) . . ? H755 H756 2.35(4) . . ? H8a H8b 1.59(3) . . ? H8a H9b 2.33(3) . . ? H8b H9a 2.31(3) . . ? H9a H9b 1.62(3) . . ? _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 1452 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 23 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min -23 _reflns_limit_l_max 22 _reflns_number_observed ? _reflns_d_resolution_high .729 _reflns_d_resolution_low 10.814 _diffrn_reflns_av_sigmaI/netI .036 _diffrn_reflns_theta_min 1.88 _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 .039 _refine_ls_wR_factor_all .057 _refine_ls_goodness_of_fit_all 1.518 _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