# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2099 ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_global _audit_creation_method Xtal3.6 _audit_creation_date 00-01-20 _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 'Somers. N.' _publ_contact_author_address ; Department of Chemistry University of Western Australia Nedlands Western Australia 6907 Australia ; _publ_contact_author_email neil@crystal.uwa.edu.au _publ_contact_author_fax (+61)_08_9380_1005 _publ_contact_author_phone (+61)_08-9380_2413 _publ_contact_letter ; ? #<< contact letter ; _publ_requested_journal ? _publ_requested_category FO _publ_section_title ; ? #<< paper title text ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Somers, Neil' . ; Department of Chemistry, University of Western Australia, Nedlands, WA 6907 Australia. ; 'Skelton, Brian W.' . ; Crystallography Centre, University of Western Australia, Nedlands, WA 6907 Australia. ; 'White, Allan H.' . ; 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 ; #<< references text 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_cpm48 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C28 H35 B1 Cu1 N6 P1' _chemical_formula_moiety ? _chemical_formula_weight 560.96 _chemical_melting_point ? _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P_b_c_a _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 -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 14.479(2) _cell_length_b 18.019(3) _cell_length_c 21.808(4) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 5689.6(16) _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 1.31 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu .852 _exptl_crystal_description plate _exptl_crystal_size_max .7 _exptl_crystal_size_mid .4 _exptl_crystal_size_min .07 _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 .644 _exptl_absorpt_correction_T_max .837 _diffrn_reflns_number 66048 _reflns_number_total 7365 _reflns_Friedel_coverage 0 _reflns_number_gt 5820 _reflns_threshold_expression 'F > 4.0sig(F )' _diffrn_reflns_theta_max 29.26 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .059 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? #<< do not append units _diffrn_standards_decay_% 0 #<< do not append % _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .036 _refine_ls_wR_factor_ref .046 _refine_ls_goodness_of_fit_ref 1.584 _refine_ls_number_reflns 5820 _refine_ls_number_parameters 334 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .004 _refine_diff_density_min -.376 _refine_diff_density_max .498 _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 ? 0 224 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 280 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 48 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 8 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' B ? 0 8 0 .001 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cu ? 0 8 .263 1.266 '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 .900550(16) .073050(11) .322989(9) .02345(12) Uani ? ? 1.00000 ? ? P .81040(3) .02288(2) .25552(2) .0226(2) Uani ? ? 1.00000 ? ? C111 .75601(13) -.06369(9) .28058(8) .0238(9) Uani ? ? 1.00000 ? ? C112 .69898(14) -.10572(10) .24294(9) .0309(10) Uani ? ? 1.00000 ? ? C113 .66099(15) -.17167(11) .26429(10) .0371(11) Uani ? ? 1.00000 ? ? C114 .67938(14) -.19623(11) .32304(9) .0353(11) Uani ? ? 1.00000 ? ? C115 .73477(15) -.15453(11) .36083(9) .0350(11) Uani ? ? 1.00000 ? ? C116 .77298(14) -.08813(10) .33999(9) .0296(10) Uani ? ? 1.00000 ? ? C121 .86933(13) -.00388(9) .18428(8) .0249(9) Uani ? ? 1.00000 ? ? C122 .96060(14) -.02756(11) .18852(9) .0332(11) Uani ? ? 1.00000 ? ? C123 1.00993(16) -.04674(12) .13656(10) .0416(12) Uani ? ? 1.00000 ? ? C124 .96937(17) -.04152(13) .07944(10) .0441(13) Uani ? ? 1.00000 ? ? C125 .88002(18) -.01757(15) .07437(10) .0494(14) Uani ? ? 1.00000 ? ? C126 .82969(15) .00094(12) .12636(9) .0382(11) Uani ? ? 1.00000 ? ? C131 .71063(15) .07579(11) .22867(10) .0357(11) Uani ? ? 1.00000 ? ? N11 .92227(11) .16835(8) .43060(7) .0259(8) Uani ? ? 1.00000 ? ? N12 .85437(11) .12850(8) .40139(7) .0268(8) Uani ? ? 1.00000 ? ? C13 .77437(14) .14797(11) .42786(9) .0320(10) Uani ? ? 1.00000 ? ? C14 .79019(15) .20030(11) .47354(9) .0355(11) Uani ? ? 1.00000 ? ? C15 .88407(15) .21256(10) .47427(8) .0314(10) Uani ? ? 1.00000 ? ? C16 .68509(15) .11586(14) .40606(11) .0478(14) Uani ? ? 1.00000 ? ? C17 .93972(18) .26453(12) .51268(10) .0467(13) Uani ? ? 1.00000 ? ? N21 1.03943(10) .18729(8) .34612(6) .0233(7) Uani ? ? 1.00000 ? ? N22 .98848(10) .15857(8) .29858(6) .0233(7) Uani ? ? 1.00000 ? ? C23 1.01510(13) .19470(9) .24807(8) .0233(8) Uani ? ? 1.00000 ? ? C24 1.08258(13) .24700(10) .26265(8) .0276(9) Uani ? ? 1.00000 ? ? C25 1.09665(13) .24098(10) .32514(8) .0268(9) Uani ? ? 1.00000 ? ? C26 .97335(14) .17705(10) .18705(8) .0291(10) Uani ? ? 1.00000 ? ? C27 1.16188(16) .28227(12) .36552(10) .0416(12) Uani ? ? 1.00000 ? ? N31 1.04772(11) .07339(8) .41408(6) .0237(7) Uani ? ? 1.00000 ? ? N32 1.00379(11) .02344(8) .37619(6) .0245(8) Uani ? ? 1.00000 ? ? C33 1.03663(13) -.04336(10) .39128(8) .0258(9) Uani ? ? 1.00000 ? ? C34 1.10018(14) -.03727(10) .43909(9) .0299(10) Uani ? ? 1.00000 ? ? C35 1.10558(13) .03708(10) .45257(8) .0263(9) Uani ? ? 1.00000 ? ? C36 1.00505(15) -.11252(10) .35960(9) .0326(10) Uani ? ? 1.00000 ? ? C37 1.16414(16) .07490(12) .49916(9) .0384(11) Uani ? ? 1.00000 ? ? B 1.02456(15) .15720(11) .41179(9) .0259(10) Uani ? ? 1.00000 ? ? H112 .68624 -.08831 .20208 .03800 Uiso ? ? 1.00000 ? ? H113 .62191 -.20079 .23718 .04500 Uiso ? ? 1.00000 ? ? H114 .65294 -.24179 .33850 .04400 Uiso ? ? 1.00000 ? ? H115 .74770 -.17172 .40167 .04400 Uiso ? ? 1.00000 ? ? H116 .81080 -.05854 .36672 .03700 Uiso ? ? 1.00000 ? ? H122 .99069 -.03000 .22837 .04300 Uiso ? ? 1.00000 ? ? H123 1.07244 -.06533 .13971 .05300 Uiso ? ? 1.00000 ? ? H124 1.00505 -.05406 .04324 .05500 Uiso ? ? 1.00000 ? ? H125 .85150 -.01415 .03478 .06300 Uiso ? ? 1.00000 ? ? H126 .76678 .01825 .12232 .04800 Uiso ? ? 1.00000 ? ? H131a .72988 .12342 .21418 .05200 Uiso ? ? 1.00000 ? ? H131b .66778 .08281 .26146 .05200 Uiso ? ? 1.00000 ? ? H131c .68055 .05017 .19618 .05200 Uiso ? ? 1.00000 ? ? H16a .69294 .06411 .39740 .07100 Uiso ? ? 1.00000 ? ? H16b .63911 .12133 .43677 .07100 Uiso ? ? 1.00000 ? ? H16c .66398 .13968 .36925 .07100 Uiso ? ? 1.00000 ? ? H14 .74364 .22365 .49867 .04500 Uiso ? ? 1.00000 ? ? H17a .90188 .28766 .54252 .06800 Uiso ? ? 1.00000 ? ? H17b .98823 .23793 .53328 .06800 Uiso ? ? 1.00000 ? ? H17c .96750 .30169 .48749 .06800 Uiso ? ? 1.00000 ? ? H26a .99158 .21279 .15715 .04400 Uiso ? ? 1.00000 ? ? H26b .90761 .17642 .18953 .04400 Uiso ? ? 1.00000 ? ? H26c .99431 .12928 .17436 .04400 Uiso ? ? 1.00000 ? ? H24 1.11271 .28019 .23478 .03300 Uiso ? ? 1.00000 ? ? H27a 1.20458 .24821 .38398 .06200 Uiso ? ? 1.00000 ? ? H27b 1.19629 .31738 .34198 .06200 Uiso ? ? 1.00000 ? ? H27c 1.13075 .30834 .39776 .06200 Uiso ? ? 1.00000 ? ? H36a 1.05769 -.14279 .34995 .04800 Uiso ? ? 1.00000 ? ? H36b .96530 -.14001 .38591 .04800 Uiso ? ? 1.00000 ? ? H36c .97325 -.10150 .32250 .04800 Uiso ? ? 1.00000 ? ? H34 1.13441 -.07653 .45854 .03700 Uiso ? ? 1.00000 ? ? H37a 1.20990 .10546 .47969 .05700 Uiso ? ? 1.00000 ? ? H37b 1.12754 .10594 .52519 .05700 Uiso ? ? 1.00000 ? ? H37c 1.19492 .03901 .52382 .05700 Uiso ? ? 1.00000 ? ? H 1.06447 .18428 .44075 .03200 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 .02631(13) .02229(12) .02175(12) -.00230(8) -.00152(9) -.00007(8) P .0224(2) .0214(2) .0240(2) -.00059(18) -.00226(18) .00177(17) C111 .0216(9) .0245(8) .0252(8) -.0011(7) .0002(7) .0011(7) C112 .0321(11) .0324(10) .0284(9) -.0062(8) -.0049(8) .0029(8) C113 .0375(12) .0346(10) .0391(11) -.0137(9) -.0064(9) .0014(9) C114 .0327(11) .0298(10) .0435(12) -.0066(8) .0000(9) .0083(9) C115 .0359(12) .0380(10) .0310(10) -.0062(9) -.0023(9) .0109(9) C116 .0288(11) .0331(10) .0269(9) -.0046(8) -.0035(8) .0033(7) C121 .0277(9) .0223(8) .0246(9) -.0027(7) -.0015(7) .0031(7) C122 .0334(11) .0376(11) .0286(10) .0032(9) -.0012(8) .0057(8) C123 .0376(13) .0449(12) .0422(12) .0091(10) .0081(10) .0080(10) C124 .0554(15) .0456(12) .0313(11) .0036(11) .0150(10) .0005(9) C125 .0557(16) .0691(16) .0235(10) .0017(12) -.0031(10) .0000(10) C126 .0339(11) .0525(12) .0282(10) .0022(10) -.0052(9) .0016(9) C131 .0316(11) .0327(10) .0426(12) .0084(8) -.0042(9) .0035(9) N11 .0354(9) .0221(7) .0202(7) .0024(6) -.0001(6) .0010(6) N12 .0275(9) .0279(7) .0251(8) .0015(6) .0008(6) .0021(6) C13 .0323(11) .0368(10) .0268(9) .0070(8) .0055(8) .0067(8) C14 .0460(13) .0354(10) .0251(9) .0137(9) .0104(9) .0060(8) C15 .0498(13) .0247(9) .0197(8) .0070(8) .0037(8) .0024(7) C16 .0316(12) .0679(16) .0439(13) .0031(11) .0081(10) .0032(11) C17 .0709(17) .0393(11) .0300(11) .0062(11) .0012(11) -.0104(9) N21 .0264(8) .0218(7) .0217(7) -.0026(6) -.0024(6) .0000(6) N22 .0261(8) .0225(7) .0214(7) -.0000(6) -.0004(6) .0008(6) C23 .0259(9) .0202(8) .0240(8) .0046(7) .0031(7) .0024(7) C24 .0296(10) .0239(8) .0292(9) -.0005(7) .0032(8) .0064(7) C25 .0271(10) .0213(8) .0318(10) -.0015(7) -.0013(8) .0033(7) C26 .0358(11) .0274(9) .0240(9) .0023(8) .0010(8) .0029(7) C27 .0471(13) .0384(11) .0394(11) -.0164(10) -.0069(10) .0026(9) N31 .0277(9) .0242(7) .0192(7) .0009(6) -.0014(6) .0004(6) N32 .0289(8) .0217(7) .0230(7) -.0003(6) -.0009(6) .0004(6) C33 .0271(10) .0239(8) .0264(9) .0022(7) .0078(7) .0051(7) C34 .0302(11) .0304(9) .0291(10) .0064(8) .0043(8) .0088(8) C35 .0244(10) .0347(9) .0198(8) .0045(7) .0017(7) .0048(7) C36 .0352(11) .0232(9) .0395(11) .0025(8) .0055(9) .0017(8) C37 .0378(12) .0497(12) .0278(10) .0083(9) -.0074(9) -.0013(9) B .0326(12) .0243(9) .0206(9) -.0010(8) -.0030(8) -.0009(8) # 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 P . . 2.1646(5) ? Cu N12 . . 2.0900(15) ? Cu N22 . . 2.0685(15) ? Cu N32 . . 2.0927(15) ? P C111 . . 1.8308(18) ? P C121 . . 1.8368(18) ? P C131 . . 1.827(2) ? C111 C112 . . 1.389(3) ? C111 C116 . . 1.390(3) ? C112 C113 . . 1.390(3) ? C112 H112 . . .9624(19) ? C113 C114 . . 1.381(3) ? C113 H113 . . .972(2) ? C114 C115 . . 1.374(3) ? C114 H114 . . .966(2) ? C115 C116 . . 1.394(3) ? C115 H115 . . .961(2) ? C116 H116 . . .961(2) ? C121 C122 . . 1.392(3) ? C121 C126 . . 1.390(3) ? C122 C123 . . 1.383(3) ? C122 H122 . . .973(2) ? C123 C124 . . 1.380(3) ? C123 H123 . . .968(2) ? C124 C125 . . 1.368(4) ? C124 H124 . . .970(2) ? C125 C126 . . 1.388(3) ? C125 H125 . . .959(2) ? C126 H126 . . .967(2) ? C131 H131a . . .956(2) ? C131 H131b . . .955(2) ? C131 H131c . . .951(2) ? N11 N12 . . 1.374(2) ? N11 C15 . . 1.359(2) ? N11 B . . 1.550(3) ? N12 C13 . . 1.341(3) ? C13 C14 . . 1.391(3) ? C13 C16 . . 1.494(3) ? C14 C15 . . 1.377(3) ? C14 H14 . . .965(2) ? C15 C17 . . 1.492(3) ? C16 H16a . . .958(3) ? C16 H16b . . .949(2) ? C16 H16c . . .960(2) ? C17 H17a . . .947(2) ? C17 H17b . . .962(2) ? C17 H17c . . .955(2) ? N21 N22 . . 1.374(2) ? N21 C25 . . 1.353(2) ? N21 B . . 1.546(2) ? N22 C23 . . 1.336(2) ? C23 C24 . . 1.394(2) ? C23 C26 . . 1.495(3) ? C24 C25 . . 1.382(3) ? C24 H24 . . .9578(18) ? C25 C27 . . 1.490(3) ? C26 H26a . . .9537(18) ? C26 H26b . . .953(2) ? C26 H26c . . .9538(19) ? C27 H27a . . .960(2) ? C27 H27b . . .955(2) ? C27 H27c . . .958(2) ? N31 N32 . . 1.377(2) ? N31 C35 . . 1.354(2) ? N31 B . . 1.548(2) ? N32 C33 . . 1.335(2) ? C33 C34 . . 1.395(3) ? C33 C36 . . 1.497(3) ? C34 C35 . . 1.374(3) ? C34 H34 . . .9623(19) ? C35 C37 . . 1.489(3) ? C36 H36a . . .961(2) ? C36 H36b . . .952(2) ? C36 H36c . . .952(2) ? C37 H37a . . .960(2) ? C37 H37b . . .957(2) ? C37 H37c . . .952(2) ? B H . . .985(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 P Cu N12 . . . 124.24(5) ? P Cu N22 . . . 120.49(4) ? P Cu N32 . . . 128.99(4) ? N12 Cu N22 . . . 92.94(6) ? N12 Cu N32 . . . 88.81(6) ? N22 Cu N32 . . . 91.22(6) ? Cu P C111 . . . 114.35(6) ? Cu P C121 . . . 113.85(6) ? Cu P C131 . . . 118.47(7) ? C111 P C121 . . . 103.21(8) ? C111 P C131 . . . 101.55(9) ? C121 P C131 . . . 103.49(9) ? P C111 C112 . . . 122.95(14) ? P C111 C116 . . . 118.16(14) ? C112 C111 C116 . . . 118.89(16) ? C111 C112 C113 . . . 120.24(18) ? C111 C112 H112 . . . 118.90(18) ? C113 C112 H112 . . . 120.86(19) ? C112 C113 C114 . . . 120.55(19) ? C112 C113 H113 . . . 119.2(2) ? C114 C113 H113 . . . 120.2(2) ? C113 C114 C115 . . . 119.58(19) ? C113 C114 H114 . . . 121.3(2) ? C115 C114 H114 . . . 119.1(2) ? C114 C115 C116 . . . 120.37(18) ? C114 C115 H115 . . . 119.6(2) ? C116 C115 H115 . . . 120.1(2) ? C111 C116 C115 . . . 120.35(18) ? C111 C116 H116 . . . 119.35(18) ? C115 C116 H116 . . . 120.30(19) ? P C121 C122 . . . 117.74(14) ? P C121 C126 . . . 124.07(15) ? C122 C121 C126 . . . 118.14(17) ? C121 C122 C123 . . . 120.84(18) ? C121 C122 H122 . . . 119.89(19) ? C123 C122 H122 . . . 119.3(2) ? C122 C123 C124 . . . 120.2(2) ? C122 C123 H123 . . . 120.8(2) ? C124 C123 H123 . . . 119.0(2) ? C123 C124 C125 . . . 119.8(2) ? C123 C124 H124 . . . 119.5(2) ? C125 C124 H124 . . . 120.8(2) ? C124 C125 C126 . . . 120.4(2) ? C124 C125 H125 . . . 120.0(2) ? C126 C125 H125 . . . 119.6(2) ? C121 C126 C125 . . . 120.7(2) ? C121 C126 H126 . . . 119.5(2) ? C125 C126 H126 . . . 119.8(2) ? P C131 H131a . . . 110.11(16) ? P C131 H131b . . . 110.04(16) ? P C131 H131c . . . 110.33(15) ? H131a C131 H131b . . . 108.5(2) ? H131a C131 H131c . . . 108.9(2) ? H131b C131 H131c . . . 108.9(2) ? N12 N11 C15 . . . 109.87(15) ? N12 N11 B . . . 119.56(14) ? C15 N11 B . . . 130.57(16) ? Cu N12 N11 . . . 113.59(11) ? Cu N12 C13 . . . 138.90(13) ? N11 N12 C13 . . . 106.37(14) ? N12 C13 C14 . . . 110.08(18) ? N12 C13 C16 . . . 120.61(17) ? C14 C13 C16 . . . 129.3(2) ? C13 C14 C15 . . . 106.24(18) ? C13 C14 H14 . . . 126.0(2) ? C15 C14 H14 . . . 127.8(2) ? N11 C15 C14 . . . 107.43(16) ? N11 C15 C17 . . . 122.8(2) ? C14 C15 C17 . . . 129.80(18) ? C13 C16 H16a . . . 109.7(2) ? C13 C16 H16b . . . 110.0(2) ? C13 C16 H16c . . . 111.6(2) ? H16a C16 H16b . . . 108.9(2) ? H16a C16 H16c . . . 108.0(2) ? H16b C16 H16c . . . 108.7(2) ? C15 C17 H17a . . . 110.4(2) ? C15 C17 H17b . . . 110.1(2) ? C15 C17 H17c . . . 110.17(19) ? H17a C17 H17b . . . 108.7(2) ? H17a C17 H17c . . . 109.3(2) ? H17b C17 H17c . . . 108.1(2) ? N22 N21 C25 . . . 110.06(14) ? N22 N21 B . . . 119.48(14) ? C25 N21 B . . . 130.46(15) ? Cu N22 N21 . . . 114.65(10) ? Cu N22 C23 . . . 138.82(12) ? N21 N22 C23 . . . 106.47(14) ? N22 C23 C24 . . . 110.09(15) ? N22 C23 C26 . . . 120.87(16) ? C24 C23 C26 . . . 129.04(16) ? C23 C24 C25 . . . 105.97(16) ? C23 C24 H24 . . . 126.63(18) ? C25 C24 H24 . . . 127.40(18) ? N21 C25 C24 . . . 107.40(16) ? N21 C25 C27 . . . 123.04(17) ? C24 C25 C27 . . . 129.56(17) ? C23 C26 H26a . . . 110.66(17) ? C23 C26 H26b . . . 110.83(17) ? C23 C26 H26c . . . 108.75(17) ? H26a C26 H26b . . . 108.85(19) ? H26a C26 H26c . . . 108.84(18) ? H26b C26 H26c . . . 108.86(19) ? C25 C27 H27a . . . 109.69(18) ? C25 C27 H27b . . . 110.10(19) ? C25 C27 H27c . . . 112.3(2) ? H27a C27 H27b . . . 108.2(2) ? H27a C27 H27c . . . 108.0(2) ? H27b C27 H27c . . . 108.4(2) ? N32 N31 C35 . . . 109.97(13) ? N32 N31 B . . . 121.21(14) ? C35 N31 B . . . 128.71(15) ? Cu N32 N31 . . . 112.53(10) ? Cu N32 C33 . . . 140.89(12) ? N31 N32 C33 . . . 106.07(14) ? N32 C33 C34 . . . 110.38(16) ? N32 C33 C36 . . . 121.88(16) ? C34 C33 C36 . . . 127.74(16) ? C33 C34 C35 . . . 105.91(16) ? C33 C34 H34 . . . 127.69(18) ? C35 C34 H34 . . . 126.40(19) ? N31 C35 C34 . . . 107.66(16) ? N31 C35 C37 . . . 123.65(17) ? C34 C35 C37 . . . 128.67(17) ? C33 C36 H36a . . . 109.36(18) ? C33 C36 H36b . . . 109.87(18) ? C33 C36 H36c . . . 111.49(16) ? H36a C36 H36b . . . 108.45(17) ? H36a C36 H36c . . . 108.4(2) ? H36b C36 H36c . . . 109.2(2) ? C35 C37 H37a . . . 110.72(18) ? C35 C37 H37b . . . 110.9(2) ? C35 C37 H37c . . . 109.96(18) ? H37a C37 H37b . . . 108.0(2) ? H37a C37 H37c . . . 108.4(2) ? H37b C37 H37c . . . 108.7(2) ? N11 B N21 . . . 109.43(15) ? N11 B N31 . . . 108.97(15) ? N11 B H . . . 109.07(17) ? N21 B N31 . . . 109.98(14) ? N21 B H . . . 109.77(17) ? N31 B H . . . 109.60(17) ? 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 C111 3.3624(18) . . ? Cu C112 4.684(2) . . ? Cu C114 4.315(2) . '7 655' ? Cu C115 4.823(2) . . ? Cu C116 3.462(2) . . ? Cu C121 3.3576(18) . . ? Cu C122 3.555(2) . . ? Cu C126 4.596(2) . . ? Cu C131 4.629(2) . 6 ? Cu C131 3.434(2) . . ? Cu N11 2.9247(15) . . ? Cu C13 3.223(2) . . ? Cu C14 4.311(2) . . ? Cu C15 4.1543(19) . . ? Cu C16 3.689(2) . . ? Cu N21 2.9215(15) . . ? Cu C23 3.1976(17) . . ? Cu C24 4.3014(19) . . ? Cu C25 4.1498(19) . . ? Cu C26 3.6618(19) . . ? Cu N31 2.9131(15) . . ? Cu C33 3.2402(18) . . ? Cu C34 4.326(2) . . ? Cu C35 4.1492(19) . . ? Cu C36 3.7560(19) . . ? Cu C37 4.798(2) . '5 756' ? Cu B 3.045(2) . . ? Cu H114 3.4418(6) . '7 655' ? Cu H116 2.8671(4) . . ? Cu H122 3.0672(4) . . ? Cu H131a 3.5439(4) . . ? Cu H131b 4.2887(6) . 6 ? Cu H131b 3.6318(5) . . ? Cu H131c 4.0964(6) . 6 ? Cu H131c 4.2382(5) . . ? Cu H16a 3.4197(5) . . ? Cu H16c 3.7672(5) . . ? Cu H26b 3.4566(5) . . ? Cu H26c 3.6569(6) . . ? Cu H36b 4.1833(6) . . ? Cu H36c 3.3167(5) . . ? Cu H37c 4.1408(6) . '5 756' ? Cu H 4.0303(4) . . ? P C112 2.837(2) . . ? P C113 4.124(2) . . ? P C114 4.621(2) . . ? P C115 4.086(2) . . ? P C116 2.773(2) . . ? P C122 2.773(2) . . ? P C123 4.080(2) . . ? P C124 4.625(2) . . ? P C125 4.141(2) . . ? P C126 2.858(2) . . ? P N12 3.7609(16) . . ? P C13 4.413(2) . . ? P C16 4.108(2) . . ? P N22 3.6753(16) . . ? P C23 4.2891(18) . . ? P C26 3.939(2) . . ? P N32 3.8425(16) . . ? P C33 4.574(2) . . ? P C36 4.364(2) . . ? P H112 2.9332(5) . . ? P H116 2.8340(6) . . ? P H122 2.8413(6) . . ? P H126 2.9735(7) . . ? P H131a 2.3353(5) . . ? P H131b 2.3339(5) . . ? P H131c 2.3347(5) . . ? P H16a 3.6077(7) . . ? P H16c 3.8825(6) . . ? P H26b 3.4214(6) . . ? P H26c 3.7281(6) . . ? P H27b 4.2709(7) . '4 745' ? P H36c 3.5659(6) . . ? C111 C113 2.409(3) . . ? C111 C114 2.791(3) . . ? C111 C115 2.416(3) . . ? C111 C121 2.875(3) . . ? C111 C122 3.637(3) . . ? C111 C122 4.379(3) . '6 455' ? C111 C123 4.007(3) . '6 455' ? C111 C126 3.715(3) . . ? C111 C131 2.834(3) . . ? C111 C16 4.360(3) . . ? C111 C24 4.241(3) . '4 745' ? C111 C27 4.389(3) . '4 745' ? C111 C36 4.092(3) . . ? C111 H112 2.0365(18) . . ? C111 H113 3.2815(18) . . ? C111 H114 3.7578(18) . . ? C111 H115 3.2826(18) . . ? C111 H116 2.0411(18) . . ? C111 H122 3.894(2) . '6 455' ? C111 H122 3.6346(19) . . ? C111 H123 3.1759(18) . '6 455' ? C111 H126 3.7567(18) . . ? C111 H131a 3.6887(18) . . ? C111 H131b 2.9622(17) . . ? C111 H131c 2.9648(18) . . ? C111 H16a 3.5533(18) . . ? C111 H24 3.4115(18) . '4 745' ? C111 H27b 3.4944(18) . '4 745' ? C111 H36c 3.3456(19) . . ? C112 C114 2.406(3) . . ? C112 C115 2.766(3) . . ? C112 C116 2.393(3) . . ? C112 C121 3.330(3) . . ? C112 C122 4.212(3) . . ? C112 C122 4.016(3) . '6 455' ? C112 C123 3.940(3) . '6 455' ? C112 C126 3.706(3) . . ? C112 C131 3.290(3) . . ? C112 C24 4.131(3) . '4 745' ? C112 C25 4.312(3) . '4 745' ? C112 C27 3.705(3) . '4 745' ? C112 C33 3.918(3) . '6 455' ? C112 C34 4.396(3) . '6 455' ? C112 C36 3.591(3) . '6 455' ? C112 H113 2.048(2) . . ? C112 H114 3.286(2) . . ? C112 H115 3.727(2) . . ? C112 H116 3.260(2) . . ? C112 H122 3.369(2) . '6 455' ? C112 H123 3.230(2) . '6 455' ? C112 H126 3.588(2) . . ? C112 H131b 3.451(2) . . ? C112 H131c 3.000(2) . . ? C112 H24 3.449(2) . '4 745' ? C112 H27b 2.766(2) . '4 745' ? C112 H36a 2.955(2) . '6 455' ? C112 H36c 3.567(2) . '6 455' ? C113 C115 2.381(3) . . ? C113 C116 2.761(3) . . ? C113 C122 4.027(3) . '6 455' ? C113 C123 3.811(3) . '6 455' ? C113 N21 4.250(3) . '7 645' ? C113 N22 3.821(3) . '7 645' ? C113 C23 3.525(3) . '7 645' ? C113 C24 4.035(3) . '4 745' ? C113 C24 3.819(3) . '7 645' ? C113 C25 4.261(3) . '7 645' ? C113 C25 4.312(3) . '4 745' ? C113 C26 3.748(3) . '7 645' ? C113 C27 3.909(3) . '4 745' ? C113 C36 3.678(3) . '6 455' ? C113 H112 2.057(2) . . ? C113 H114 2.056(2) . . ? C113 H115 3.248(2) . . ? C113 H116 3.721(2) . . ? C113 H122 3.553(2) . '6 455' ? C113 H123 3.114(2) . '6 455' ? C113 H26a 3.830(2) . '7 645' ? C113 H26b 3.337(2) . '7 645' ? C113 H24 3.390(2) . '4 745' ? C113 H27b 3.111(2) . '4 745' ? C113 H36a 2.952(2) . '6 455' ? C113 H36c 3.545(2) . '6 455' ? C114 C116 2.402(3) . . ? C114 C122 4.397(3) . '6 455' ? C114 C123 3.749(3) . '6 455' ? C114 N11 3.691(3) . '7 645' ? C114 N12 3.624(3) . '7 645' ? C114 C13 3.682(3) . '7 645' ? C114 C14 3.800(3) . '7 645' ? C114 C15 3.797(3) . '7 645' ? C114 C16 4.312(3) . '7 645' ? C114 N21 3.833(3) . '7 645' ? C114 N22 3.611(3) . '7 645' ? C114 C23 3.803(3) . '7 645' ? C114 C24 4.052(3) . '4 745' ? C114 C24 4.143(3) . '7 645' ? C114 C25 4.154(3) . '7 645' ? C114 C26 4.347(3) . '7 645' ? C114 B 4.409(3) . '7 645' ? C114 H112 3.278(2) . . ? C114 H113 2.050(2) . . ? C114 H115 2.028(2) . . ? C114 H116 3.269(2) . . ? C114 H123 2.936(2) . '6 455' ? C114 H16c 3.860(2) . '7 645' ? C114 H26b 3.915(2) . '7 645' ? C114 H24 3.291(2) . '4 745' ? C114 H27b 4.031(2) . '4 745' ? C115 C123 3.791(3) . '6 455' ? C115 N11 4.204(3) . '7 645' ? C115 N12 4.211(3) . '7 645' ? C115 C13 3.850(3) . '7 645' ? C115 C14 3.607(3) . '7 645' ? C115 C15 3.849(3) . '7 645' ? C115 C16 4.409(3) . '7 645' ? C115 C17 4.413(3) . '7 645' ? C115 C24 4.170(3) . '4 745' ? C115 C36 3.986(3) . . ? C115 C37 3.677(3) . '5 756' ? C115 H112 3.728(2) . . ? C115 H113 3.261(2) . . ? C115 H114 2.028(2) . . ? C115 H116 2.054(2) . . ? C115 H123 2.847(2) . '6 455' ? C115 H16c 3.992(2) . '7 645' ? C115 H14 3.735(2) . '7 645' ? C115 H24 3.257(2) . '4 745' ? C115 H36b 3.392(2) . . ? C115 H36c 3.679(2) . . ? C115 H37a 3.676(2) . '5 756' ? C115 H37b 3.304(2) . '5 756' ? C115 H37c 3.420(2) . '5 756' ? C116 C121 3.972(3) . . ? C116 C122 4.414(3) . . ? C116 C123 3.915(3) . '6 455' ? C116 C131 3.928(3) . . ? C116 N12 4.292(2) . . ? C116 C16 4.148(3) . . ? C116 C24 4.267(3) . '4 745' ? C116 N32 3.979(3) . . ? C116 C33 4.059(3) . . ? C116 C36 3.416(3) . . ? C116 C37 3.631(3) . '5 756' ? C116 H112 3.259(2) . . ? C116 H113 3.733(2) . . ? C116 H114 3.269(2) . . ? C116 H115 2.052(2) . . ? C116 H123 2.966(2) . '6 455' ? C116 H131b 3.839(2) . . ? C116 H16a 3.230(2) . . ? C116 H24 3.321(2) . '4 745' ? C116 H36b 3.103(2) . . ? C116 H36c 2.935(2) . . ? C116 H37a 3.952(2) . '5 756' ? C116 H37b 3.289(2) . '5 756' ? C116 H37c 3.133(2) . '5 756' ? C121 C123 2.413(3) . . ? C121 C124 2.790(3) . . ? C121 C125 2.414(3) . . ? C121 C131 2.877(3) . . ? C121 N22 4.214(2) . . ? C121 C23 4.381(2) . . ? C121 C26 3.592(3) . . ? C121 C27 4.029(3) . '4 745' ? C121 H112 3.0811(19) . . ? C121 H122 2.0575(19) . . ? C121 H123 3.289(2) . . ? C121 H124 3.7599(18) . . ? C121 H125 3.2753(18) . . ? C121 H126 2.0467(18) . . ? C121 H131a 3.1247(18) . . ? C121 H131b 3.7133(19) . . ? C121 H131c 2.913(2) . . ? C121 H26b 3.2977(18) . . ? C121 H26c 3.0130(18) . . ? C121 H27b 3.4064(18) . '4 745' ? C121 H27c 3.8274(18) . '4 745' ? C121 H36c 3.8003(18) . . ? C122 C124 2.395(3) . . ? C122 C125 2.755(3) . . ? C122 C126 2.386(3) . . ? C122 C131 4.163(3) . . ? C122 N22 4.144(2) . . ? C122 C23 4.284(3) . . ? C122 C24 4.246(3) . '4 745' ? C122 C25 4.263(3) . '4 745' ? C122 C26 3.692(3) . . ? C122 C27 4.034(3) . '4 745' ? C122 N32 4.241(3) . . ? C122 C36 4.083(3) . . ? C122 H123 2.054(2) . . ? C122 H124 3.268(2) . . ? C122 H125 3.714(2) . . ? C122 H126 3.262(2) . . ? C122 H131b 3.761(2) . 6 ? C122 H26b 3.755(2) . . ? C122 H26c 2.885(2) . . ? C122 H24 3.990(2) . '4 745' ? C122 H27b 3.662(2) . '4 745' ? C122 H27c 3.746(2) . '4 745' ? C122 H36c 3.216(2) . . ? C123 C125 2.378(3) . . ? C123 C126 2.756(3) . . ? C123 C16 3.985(3) . 6 ? C123 C25 4.208(3) . '4 745' ? C123 C26 4.214(3) . . ? C123 C27 3.960(3) . '4 745' ? C123 H122 2.044(2) . . ? C123 H124 2.040(2) . . ? C123 H125 3.245(2) . . ? C123 H126 3.723(2) . . ? C123 H131b 3.952(2) . 6 ? C123 H16a 3.400(2) . 6 ? C123 H16b 3.902(2) . 6 ? C123 H16c 4.034(2) . 6 ? C123 H17c 3.858(2) . '4 745' ? C123 H26c 3.285(2) . . ? C123 H27b 3.890(2) . '4 745' ? C123 H27c 3.395(2) . '4 745' ? C124 C124 3.876(3) . '5 755' ? C124 C125 4.140(3) . '5 755' ? C124 C126 2.392(3) . . ? C124 C16 4.231(3) . 6 ? C124 C17 4.240(3) . '4 745' ? C124 C27 3.890(3) . '4 745' ? C124 H122 3.269(2) . . ? C124 H123 2.034(2) . . ? C124 H124 3.203(2) . '5 755' ? C124 H125 3.733(2) . '5 755' ? C124 H125 2.026(2) . . ? C124 H126 3.262(2) . . ? C124 H16a 3.789(2) . 6 ? C124 H16b 3.770(2) . '2 654' ? C124 H16b 3.844(2) . 6 ? C124 H17c 3.309(2) . '4 745' ? C124 H26c 3.726(2) . . ? C124 H27b 3.893(2) . '4 745' ? C124 H27c 3.109(2) . '4 745' ? C125 C16 4.183(3) . '2 654' ? C125 C27 3.885(3) . '4 745' ? C125 C34 4.078(3) . '6 455' ? C125 C35 4.136(3) . '6 455' ? C125 C37 3.888(3) . '6 455' ? C125 H122 3.727(2) . . ? C125 H123 3.245(3) . . ? C125 H124 3.318(2) . '5 755' ? C125 H124 2.042(3) . . ? C125 H126 2.049(2) . . ? C125 H16b 3.546(2) . '2 654' ? C125 H26c 3.807(2) . . ? C125 H27b 3.659(3) . '4 745' ? C125 H27c 3.199(3) . '4 745' ? C125 H34 3.780(3) . '6 455' ? C125 H37a 3.517(3) . '6 455' ? C125 H37c 3.579(2) . '6 455' ? C126 C131 3.125(3) . . ? C126 C26 4.019(3) . . ? C126 C27 3.946(3) . '4 745' ? C126 N31 4.376(3) . '6 455' ? C126 C33 4.335(3) . '6 455' ? C126 C34 3.681(3) . '6 455' ? C126 C35 3.730(3) . '6 455' ? C126 C37 3.875(3) . '6 455' ? C126 H112 3.103(2) . . ? C126 H122 3.270(2) . . ? C126 H123 3.724(2) . . ? C126 H124 3.273(2) . . ? C126 H125 2.040(2) . . ? C126 H131a 3.260(2) . . ? C126 H131c 2.787(2) . . ? C126 H26b 3.629(2) . . ? C126 H26c 3.482(2) . . ? C126 H27b 3.400(2) . '4 745' ? C126 H27c 3.556(2) . '4 745' ? C126 H34 3.656(2) . '6 455' ? C126 H37a 3.450(2) . '6 455' ? C126 H37c 3.873(2) . '6 455' ? C131 N12 4.407(3) . . ? C131 C16 3.952(3) . . ? C131 N21 3.583(3) . '6 455' ? C131 N22 3.595(3) . '6 455' ? C131 C23 3.587(3) . '6 455' ? C131 C24 3.604(3) . '6 455' ? C131 C25 3.600(3) . '6 455' ? C131 C26 4.302(3) . '6 455' ? C131 C26 4.315(3) . . ? C131 C27 4.308(3) . '6 455' ? C131 N31 3.906(3) . '6 455' ? C131 N32 3.884(3) . '6 455' ? C131 C33 4.219(3) . '6 455' ? C131 C35 4.291(3) . '6 455' ? C131 B 4.335(3) . '6 455' ? C131 H112 3.034(2) . . ? C131 H122 3.828(2) . '6 455' ? C131 H126 2.667(2) . . ? C131 H16a 3.694(2) . . ? C131 H16c 3.343(2) . . ? C131 H26b 3.486(2) . . ? C131 H26c 3.900(2) . '6 455' ? C131 H24 4.026(2) . '6 455' ? C131 H27a 3.961(2) . '6 455' ? N11 C13 2.174(3) . . ? N11 C14 2.206(3) . . ? N11 C16 3.602(3) . . ? N11 C17 2.504(3) . . ? N11 N21 2.527(2) . . ? N11 N22 3.039(2) . . ? N11 C23 4.228(2) . . ? N11 C25 3.657(2) . . ? N11 C27 4.273(3) . . ? N11 N31 2.521(2) . . ? N11 N32 3.101(2) . . ? N11 C33 4.246(2) . . ? N11 C34 3.709(2) . '5 756' ? N11 C35 3.587(2) . . ? N11 C37 4.164(3) . . ? N11 H114 2.8001(15) . '7 655' ? N11 H115 3.8417(15) . '7 655' ? N11 H16a 3.8831(16) . . ? N11 H16c 4.0054(16) . . ? N11 H14 3.1441(16) . . ? N11 H17a 3.2656(15) . . ? N11 H17b 2.7380(15) . . ? N11 H17c 2.7821(15) . . ? N11 H27c 3.9983(16) . . ? N11 H34 3.0421(15) . '5 756' ? N11 H37b 3.7884(16) . . ? N11 H 2.0905(16) . . ? N12 C14 2.239(2) . . ? N12 C15 2.237(2) . . ? N12 C16 2.464(3) . . ? N12 C17 3.664(3) . . ? N12 N21 3.123(2) . . ? N12 N22 3.015(2) . . ? N12 C23 4.244(2) . . ? N12 C25 4.379(2) . . ? N12 N31 2.983(2) . . ? N12 N32 2.927(2) . . ? N12 C33 4.075(2) . . ? N12 C34 3.903(2) . '5 756' ? N12 C35 4.402(2) . '5 756' ? N12 C35 4.146(2) . . ? N12 C37 4.267(3) . '5 756' ? N12 B 2.528(3) . . ? N12 H114 2.7118(15) . '7 655' ? N12 H115 3.8913(16) . '7 655' ? N12 H116 3.5112(15) . . ? N12 H16a 2.6110(16) . . ? N12 H16b 3.2135(16) . . ? N12 H16c 2.8515(16) . . ? N12 H14 3.1638(15) . . ? N12 H17b 3.9893(15) . . ? N12 H17c 3.9933(15) . . ? N12 H34 3.1987(16) . '5 756' ? N12 H37c 3.5043(15) . '5 756' ? N12 H 3.3167(16) . . ? C13 C15 2.214(3) . . ? C13 C17 3.683(3) . . ? C13 N21 4.290(3) . . ? C13 N22 4.195(2) . . ? C13 N31 4.191(3) . . ? C13 N32 4.164(3) . . ? C13 C34 3.962(3) . '5 756' ? C13 C37 4.410(3) . '5 756' ? C13 B 3.643(3) . . ? C13 H114 2.975(2) . '7 655' ? C13 H115 3.314(2) . '7 655' ? C13 H116 3.988(2) . . ? C13 H125 3.817(2) . '2 655' ? C13 H16a 2.028(2) . . ? C13 H16b 2.026(2) . . ? C13 H16c 2.052(2) . . ? C13 H14 2.107(2) . . ? C13 H17a 3.999(2) . . ? C13 H34 3.088(2) . '5 756' ? C13 H37c 3.558(2) . '5 756' ? C14 C16 2.607(3) . . ? C14 C17 2.599(3) . . ? C14 C27 3.983(3) . '3 456' ? C14 C34 3.844(3) . '5 756' ? C14 B 3.732(3) . . ? C14 H114 3.231(2) . '7 655' ? C14 H115 2.842(2) . '7 655' ? C14 H16a 3.280(2) . . ? C14 H16b 2.730(2) . . ? C14 H16c 3.115(2) . . ? C14 H17a 2.712(2) . . ? C14 H17b 3.222(2) . . ? C14 H17c 3.166(2) . . ? C14 H27a 3.471(2) . '3 456' ? C14 H27c 3.637(2) . '3 456' ? C14 H34 2.891(2) . '5 756' ? C14 H37a 3.826(2) . '3 456' ? C15 C16 3.681(3) . . ? C15 N21 3.616(2) . . ? C15 N22 4.232(2) . . ? C15 N31 3.691(2) . . ? C15 N32 4.381(2) . . ? C15 C33 4.383(3) . '5 756' ? C15 C34 3.687(3) . '5 756' ? C15 C36 4.353(3) . '5 756' ? C15 B 2.644(3) . . ? C15 H114 3.1191(19) . '7 655' ? C15 H115 3.239(2) . '7 655' ? C15 H16b 3.994(2) . . ? C15 H14 2.111(2) . . ? C15 H17a 2.0279(18) . . ? C15 H17b 2.034(2) . . ? C15 H17c 2.030(2) . . ? C15 H36b 3.970(2) . '5 756' ? C15 H34 2.8681(18) . '5 756' ? C15 H 2.760(2) . . ? C16 C23 4.401(3) . '6 455' ? C16 C26 3.839(3) . '6 455' ? C16 H114 3.775(2) . '7 655' ? C16 H115 3.951(3) . '7 655' ? C16 H116 3.731(3) . . ? C16 H123 3.784(3) . '6 455' ? C16 H125 3.394(2) . '2 655' ? C16 H131b 3.218(2) . . ? C16 H14 2.927(2) . . ? C16 H26a 3.578(2) . '6 455' ? C16 H26c 3.281(2) . '6 455' ? C16 H34 4.006(2) . '5 756' ? C16 H37c 3.625(2) . '5 756' ? C17 N21 4.149(3) . . ? C17 C26 3.975(3) . 8 ? C17 N31 4.351(3) . . ? C17 C34 4.267(3) . '5 756' ? C17 C36 3.987(3) . '5 756' ? C17 B 3.176(3) . . ? C17 H114 4.030(2) . '7 655' ? C17 H115 3.813(2) . '7 655' ? C17 H124 3.579(2) . '4 755' ? C17 H16b 3.712(2) . '3 556' ? C17 H14 2.949(3) . . ? C17 H26a 3.264(2) . 8 ? C17 H26b 4.027(2) . 8 ? C17 H27c 3.815(2) . . ? C17 H36a 3.713(2) . '5 756' ? C17 H36b 3.437(2) . '5 756' ? C17 H34 3.609(2) . '5 756' ? C17 H37b 3.954(2) . . ? C17 H 2.795(2) . . ? N21 C23 2.171(2) . . ? N21 C24 2.205(2) . . ? N21 C26 3.603(2) . . ? N21 C27 2.500(3) . . ? N21 N31 2.534(2) . . ? N21 N32 3.068(2) . . ? N21 C33 4.271(2) . . ? N21 C35 3.692(2) . . ? N21 C37 4.301(3) . . ? N21 H113 3.8945(15) . '7 655' ? N21 H114 3.0690(15) . '7 655' ? N21 H131a 3.2645(15) . 6 ? N21 H131b 3.5356(15) . 6 ? N21 H131c 3.3362(15) . 6 ? N21 H17c 3.8518(15) . . ? N21 H26b 3.9166(15) . . ? N21 H26c 3.9429(16) . . ? N21 H24 3.1341(15) . . ? N21 H27a 2.7576(15) . . ? N21 H27b 3.2652(15) . . ? N21 H27c 2.7882(15) . . ? N21 H 2.0957(15) . . ? N22 C24 2.238(2) . . ? N22 C25 2.235(2) . . ? N22 C26 2.464(2) . . ? N22 C27 3.661(3) . . ? N22 N31 3.072(2) . . ? N22 N32 2.974(2) . . ? N22 C33 4.220(2) . . ? N22 C35 4.352(2) . . ? N22 B 2.523(2) . . ? N22 H113 3.2817(15) . '7 655' ? N22 H114 2.8591(15) . '7 655' ? N22 H122 3.7268(15) . . ? N22 H131a 3.5630(16) . 6 ? N22 H131b 3.2120(15) . 6 ? N22 H131c 3.4003(15) . 6 ? N22 H26a 3.2352(15) . . ? N22 H26b 2.6699(15) . . ? N22 H26c 2.7608(15) . . ? N22 H24 3.1581(15) . . ? N22 H27a 3.9834(15) . . ? N22 H 3.3220(15) . . ? C23 C25 2.217(3) . . ? C23 C27 3.683(3) . . ? C23 N31 4.255(2) . . ? C23 N32 4.166(2) . . ? C23 C36 4.203(2) . '4 755' ? C23 B 3.636(3) . . ? C23 H113 2.7455(17) . '7 655' ? C23 H114 3.3343(18) . '7 655' ? C23 H131a 3.4639(18) . 6 ? C23 H131b 2.9992(17) . 6 ? C23 H131c 3.7416(17) . 6 ? C23 H16c 3.4891(18) . 6 ? C23 H26a 2.0377(17) . . ? C23 H26b 2.0396(18) . . ? C23 H26c 2.0158(17) . . ? C23 H24 2.1105(17) . . ? C23 H27b 3.9953(17) . . ? C23 H36a 3.7753(17) . '4 755' ? C23 H36c 3.9851(17) . '4 755' ? C24 C26 2.609(3) . . ? C24 C27 2.599(3) . . ? C24 C36 3.889(3) . '4 755' ? C24 B 3.728(3) . . ? C24 H113 3.1559(19) . '7 655' ? C24 H114 3.795(2) . '7 655' ? C24 H131a 3.1245(18) . 6 ? C24 H131b 3.2482(18) . 6 ? C24 H131c 3.9239(18) . 6 ? C24 H16c 3.6607(19) . 6 ? C24 H26a 2.7217(19) . . ? C24 H26b 3.2523(19) . . ? C24 H26c 3.1367(18) . . ? C24 H27a 3.1812(19) . . ? C24 H27b 2.7040(18) . . ? C24 H27c 3.2230(19) . . ? C24 H36a 3.7546(19) . '4 755' ? C24 H36b 3.8883(19) . '4 755' ? C24 H36c 3.3990(18) . '4 755' ? C25 C26 3.685(3) . . ? C25 N31 3.658(2) . . ? C25 N32 4.291(2) . . ? C25 B 2.634(3) . . ? C25 H113 3.8463(19) . '7 655' ? C25 H114 3.639(2) . '7 655' ? C25 H131a 2.9907(18) . 6 ? C25 H131b 3.5707(18) . 6 ? C25 H131c 3.6761(18) . 6 ? C25 H26a 3.999(2) . . ? C25 H24 2.1061(18) . . ? C25 H27a 2.0261(19) . . ? C25 H27b 2.0276(18) . . ? C25 H27c 2.0552(18) . . ? C25 H 2.7596(18) . . ? C26 C36 3.938(3) . '4 755' ? C26 H113 2.818(2) . '7 655' ? C26 H122 3.846(2) . . ? C26 H131a 3.703(2) . . ? C26 H131b 3.474(2) . 6 ? C26 H16b 3.749(2) . 6 ? C26 H16c 3.095(2) . 6 ? C26 H17a 3.3775(19) . '8 554' ? C26 H17b 3.6927(19) . '8 554' ? C26 H24 2.934(2) . . ? C26 H36a 3.375(2) . '4 755' ? C26 H36b 3.766(2) . '4 755' ? C27 N31 4.245(3) . . ? C27 B 3.170(3) . . ? C27 H112 3.528(2) . '4 755' ? C27 H113 3.861(2) . '4 755' ? C27 H131a 3.490(2) . 6 ? C27 H14 3.191(2) . '3 556' ? C27 H17c 3.888(2) . . ? C27 H24 2.939(2) . . ? C27 H 2.792(2) . . ? N31 C33 2.168(2) . . ? N31 C34 2.202(2) . . ? N31 C34 3.906(2) . '5 756' ? N31 C35 4.165(2) . '5 756' ? N31 C36 3.608(2) . . ? N31 C37 2.507(3) . . ? N31 H126 3.4172(16) . 6 ? N31 H131a 3.9485(15) . 6 ? N31 H131c 3.1071(15) . 6 ? N31 H27a 3.9385(15) . . ? N31 H36c 3.8835(15) . . ? N31 H34 3.8304(15) . '5 756' ? N31 H34 3.1326(15) . . ? N31 H37a 2.8097(15) . . ? N31 H37b 2.7476(15) . . ? N31 H37c 3.2637(15) . . ? N31 H 2.0951(14) . . ? N32 C34 4.307(2) . '5 756' ? N32 C34 2.242(2) . . ? N32 C35 4.200(2) . '5 756' ? N32 C35 2.237(2) . . ? N32 C36 2.477(2) . . ? N32 C37 4.054(3) . '5 756' ? N32 C37 3.666(3) . . ? N32 B 2.550(2) . . ? N32 H112 3.7345(15) . 6 ? N32 H116 3.1675(15) . . ? N32 H122 3.3694(15) . . ? N32 H126 3.8091(16) . 6 ? N32 H131b 3.9739(15) . 6 ? N32 H131c 3.0451(15) . 6 ? N32 H36a 3.1478(15) . . ? N32 H36b 3.0049(14) . . ? N32 H36c 2.5758(14) . . ? N32 H34 3.1695(15) . . ? N32 H37b 3.6979(15) . '5 756' ? N32 H37b 3.9969(15) . . ? N32 H37c 3.7812(15) . '5 756' ? N32 H 3.3396(14) . . ? C33 C35 2.210(3) . . ? C33 C35 3.981(3) . '5 756' ? C33 C37 3.805(3) . '5 756' ? C33 C37 3.672(3) . . ? C33 B 3.646(3) . . ? C33 H112 3.0811(18) . 6 ? C33 H116 3.3246(19) . . ? C33 H122 3.622(2) . . ? C33 H126 3.5249(19) . 6 ? C33 H131c 3.2893(18) . 6 ? C33 H17b 3.8894(18) . '5 756' ? C33 H36a 2.0287(18) . . ? C33 H36b 2.0282(18) . . ? C33 H36c 2.0468(18) . . ? C33 H34 2.1243(18) . . ? C33 H37b 3.1998(18) . '5 756' ? C33 H37c 3.8305(19) . '5 756' ? C33 H37c 3.9759(19) . . ? C34 C34 4.157(3) . '5 756' ? C34 C35 3.802(3) . '5 756' ? C34 C36 2.596(3) . . ? C34 C37 2.580(3) . . ? C34 C37 4.113(3) . '5 756' ? C34 B 4.302(3) . '5 756' ? C34 B 3.719(3) . . ? C34 H112 3.446(2) . 6 ? C34 H125 3.707(2) . 6 ? C34 H126 2.935(2) . 6 ? C34 H131c 3.541(2) . 6 ? C34 H17b 3.883(2) . '5 756' ? C34 H36a 2.7878(19) . . ? C34 H36b 2.930(2) . . ? C34 H36c 3.344(2) . . ? C34 H37a 3.150(2) . . ? C34 H37b 3.607(2) . '5 756' ? C34 H37b 3.2157(19) . . ? C34 H37c 2.680(2) . . ? C34 H 4.026(2) . . ? C35 C35 3.926(3) . '5 756' ? C35 C36 3.674(3) . . ? C35 B 2.618(3) . . ? C35 H125 3.6888(19) . 6 ? C35 H126 2.8687(18) . 6 ? C35 H131c 3.4284(18) . 6 ? C35 H36a 3.9990(19) . . ? C35 H34 2.0933(19) . . ? C35 H37a 2.0371(18) . . ? C35 H37b 2.0367(18) . . ? C35 H37c 2.0220(18) . . ? C35 H 2.731(2) . . ? C36 C37 3.993(3) . '5 756' ? C36 H112 2.980(2) . 6 ? C36 H113 3.138(2) . 6 ? C36 H115 3.983(2) . . ? C36 H116 2.980(2) . . ? C36 H122 3.231(2) . . ? C36 H17b 3.251(2) . '5 756' ? C36 H26a 3.1692(18) . '4 745' ? C36 H24 3.298(2) . '4 745' ? C36 H34 2.930(2) . . ? C36 H37b 3.164(2) . '5 756' ? C37 B 3.149(3) . . ? C37 H115 3.058(2) . '5 756' ? C37 H116 2.962(2) . '5 756' ? C37 H125 3.238(2) . 6 ? C37 H126 3.204(2) . 6 ? C37 H16a 3.955(2) . '5 756' ? C37 H14 3.808(2) . '3 556' ? C37 H17b 3.959(2) . . ? C37 H36b 3.342(2) . '5 756' ? C37 H34 2.901(2) . . ? C37 H 2.755(2) . . ? B H114 3.532(2) . '7 655' ? B H131c 3.790(2) . 6 ? B H17b 3.068(2) . . ? B H17c 3.191(2) . . ? B H27a 3.139(2) . . ? B H27c 3.142(2) . . ? B H34 3.925(2) . '5 756' ? B H37a 3.204(2) . . ? B H37b 3.032(2) . . ? H112 H113 2.3582(3) . . ? H112 H122 3.3794(4) . '6 455' ? H112 H126 2.8410(3) . . ? H112 H131b 3.3549(5) . . ? H112 H131c 2.4999(4) . . ? H112 H27b 2.5892(3) . '4 745' ? H112 H36a 2.3906(2) . '6 455' ? H112 H36c 3.1391(4) . '6 455' ? H112 H34 3.5881(6) . '6 455' ? H113 H114 2.3725(4) . . ? H113 H26a 2.8584(3) . '7 645' ? H113 H26b 2.4814(3) . '7 645' ? H113 H24 3.4147(5) . '7 645' ? H113 H27b 3.1647(3) . '4 745' ? H113 H36a 2.3593(3) . '6 455' ? H113 H36c 3.0866(3) . '6 455' ? H114 H115 2.3182(2) . . ? H114 H123 3.4197(5) . '6 455' ? H114 H16c 3.4696(4) . '7 645' ? H115 H116 2.3611(3) . . ? H115 H123 3.3058(3) . '6 455' ? H115 H14 2.8362(4) . '7 645' ? H115 H36b 3.2204(4) . . ? H115 H37a 2.9146(4) . '5 756' ? H115 H37b 2.6854(3) . '5 756' ? H115 H37c 3.0080(4) . '5 756' ? H116 H123 3.4562(5) . '6 455' ? H116 H16a 2.8712(3) . . ? H116 H36b 2.7082(3) . . ? H116 H36c 2.6573(3) . . ? H116 H37a 3.4671(6) . '5 756' ? H116 H37b 2.6611(4) . '5 756' ? H116 H37c 2.4140(4) . '5 756' ? H122 H123 2.3545(3) . . ? H122 H131b 3.2796(3) . 6 ? H122 H131c 3.5143(3) . 6 ? H122 H26c 3.1027(4) . . ? H122 H36a 3.4785(4) . . ? H122 H36c 2.4365(3) . . ? H123 H124 2.3277(4) . . ? H123 H16a 3.0230(3) . 6 ? H124 H124 2.7153(3) . '5 755' ? H124 H125 2.9528(3) . '5 755' ? H124 H125 2.3439(3) . . ? H124 H16b 3.3490(4) . '2 654' ? H124 H17c 2.7135(4) . '4 745' ? H124 H27c 3.4160(3) . '4 745' ? H125 H126 2.3429(3) . . ? H125 H16a 3.1934(5) . '2 654' ? H125 H16b 2.8837(4) . '2 654' ? H125 H27c 3.5300(5) . '4 745' ? H125 H34 3.3414(4) . '6 455' ? H125 H37a 2.9913(3) . '6 455' ? H125 H37c 2.7731(3) . '6 455' ? H126 H131a 2.8087(3) . . ? H126 H131b 3.5515(5) . . ? H126 H131c 2.1174(2) . . ? H126 H34 3.1143(3) . '6 455' ? H126 H37a 2.8452(4) . '6 455' ? H126 H37c 3.3730(6) . '6 455' ? H131a H131b 1.55137(16) . . ? H131a H131c 1.5512(2) . . ? H131a H16c 3.5256(6) . . ? H131a H26b 2.7970(3) . . ? H131a H24 3.4780(4) . '6 455' ? H131a H27a 3.1259(4) . '6 455' ? H131b H131c 1.5512(2) . . ? H131b H16a 3.0054(5) . . ? H131b H16c 2.5646(4) . . ? H131b H26c 2.9947(3) . '6 455' ? H16a H16b 1.55161(15) . . ? H16a H16c 1.5514(2) . . ? H16a H26c 3.4783(4) . '6 455' ? H16a H37c 3.0066(3) . '5 756' ? H16b H16c 1.5513(3) . . ? H16b H14 2.7407(3) . . ? H16b H17b 3.4103(4) . '3 456' ? H16b H17c 3.2902(3) . '3 456' ? H16b H26a 3.3872(3) . '6 455' ? H16b H26c 3.2075(4) . '6 455' ? H16c H14 3.4034(4) . . ? H16c H26a 2.8806(3) . '6 455' ? H16c H26c 2.6409(3) . '6 455' ? H16c H24 3.4795(4) . '6 455' ? H14 H17a 2.7375(3) . . ? H14 H17b 3.6301(5) . . ? H14 H17c 3.5416(4) . . ? H14 H27a 2.6692(5) . '3 456' ? H14 H27b 3.6180(6) . '3 456' ? H14 H27c 2.8468(4) . '3 456' ? H14 H34 3.3190(4) . '5 756' ? H14 H37a 3.1533(5) . '3 456' ? H14 H37b 3.5391(5) . '3 456' ? H14 H 3.3507(3) . '3 456' ? H17a H17b 1.55136(16) . . ? H17a H17c 1.55127(19) . . ? H17a H26a 2.8168(4) . 8 ? H17a H26b 3.2713(6) . 8 ? H17a H26c 3.5065(5) . 8 ? H17a H27a 3.3387(4) . '3 456' ? H17a H36a 3.5573(4) . '5 756' ? H17a H36b 3.6348(4) . '5 756' ? H17a H37a 3.4162(4) . '3 456' ? H17b H17c 1.55143(18) . . ? H17b H26a 2.8436(5) . 8 ? H17b H36a 3.1407(4) . '5 756' ? H17b H36b 2.5828(3) . '5 756' ? H17b H34 3.4122(4) . '5 756' ? H17b H37b 3.1235(4) . . ? H17b H 2.4948(3) . . ? H17c H27c 3.0708(3) . . ? H17c H 2.7360(3) . . ? H26a H26b 1.55118(15) . . ? H26a H26c 1.5514(2) . . ? H26a H24 2.7233(3) . . ? H26a H36a 2.7028(4) . '4 755' ? H26a H36b 2.8821(4) . '4 755' ? H26a H36c 3.4138(5) . '4 755' ? H26b H26c 1.55138(16) . . ? H26b H27a 3.5895(4) . '6 455' ? H26b H36a 3.4067(5) . '4 755' ? H26c H24 3.4740(4) . . ? H24 H27a 3.5617(5) . . ? H24 H27b 2.7161(4) . . ? H24 H27c 3.5993(6) . . ? H24 H36a 3.3803(3) . '4 755' ? H24 H36b 3.2045(4) . '4 755' ? H24 H36c 2.7665(3) . '4 755' ? H27a H27b 1.5513(2) . . ? H27a H27c 1.55143(16) . . ? H27a H37a 3.3133(4) . . ? H27a H 2.6410(3) . . ? H27b H27c 1.5513(2) . . ? H27b H36a 3.6379(5) . '7 755' ? H27c H 2.6071(3) . . ? H36a H36b 1.55139(18) . . ? H36a H36c 1.55131(15) . . ? H36a H34 2.8750(4) . . ? H36b H36c 1.5513(2) . . ? H36b H34 3.1324(3) . . ? H36b H37b 2.4375(3) . '5 756' ? H36b H37c 3.5451(3) . '5 756' ? H36c H37b 3.6285(6) . '5 756' ? H34 H37a 3.4873(5) . . ? H34 H37b 3.5962(5) . . ? H34 H37c 2.6698(3) . . ? H37a H37b 1.55127(17) . . ? H37a H37c 1.55134(19) . . ? H37a H 2.6781(3) . . ? H37b H37c 1.55150(18) . . ? H37b H 2.4933(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 2352 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 19 _reflns_limit_k_min 0 _reflns_limit_k_max 24 _reflns_limit_l_min 0 _reflns_limit_l_max 29 _reflns_number_observed ? _reflns_d_resolution_high .727 _reflns_d_resolution_low 10.879 _diffrn_reflns_av_sigmaI/netI .048 _diffrn_reflns_theta_min 1.87 _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 .047 _refine_ls_goodness_of_fit_all 1.45 _refine_ls_shift/su_mean . #========================================================================== # 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 data_cpm19 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C37 H41 B1 Cu1 N8 P1' _chemical_formula_moiety ? _chemical_formula_weight 703.12 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_21/n _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 11.2796(8) _cell_length_b 15.9100(12) _cell_length_c 19.7980(15) _cell_angle_alpha 90.00000 _cell_angle_beta 100.5230(10) _cell_angle_gamma 90.00000 _cell_volume 3493.2(4) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.337 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu .71 _exptl_crystal_description plate _exptl_crystal_size_max .6 _exptl_crystal_size_mid .3 _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 .752 _exptl_absorpt_correction_T_max .928 _diffrn_reflns_number 40928 _reflns_number_total 8831 _reflns_Friedel_coverage 0 _reflns_number_gt 6649 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.28 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .033 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _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 .041 _refine_ls_wR_factor_ref .052 _refine_ls_goodness_of_fit_ref 1.596 _refine_ls_number_reflns 6649 _refine_ls_number_parameters 433 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .007 _refine_diff_density_min -.394 _refine_diff_density_max .616 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details none _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 GENTAN' _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 Cu ? 0 4 .263 1.266 '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' C ? 0 148 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 164 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 32 .004 .003 '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' 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 .45541(3) .117894(17) .165757(14) .02196(14) Uani ? ? 1.00000 ? ? P .39382(5) .24673(4) .15687(3) .0210(3) Uani ? ? 1.00000 ? ? C111 .2373(2) .25609(14) .11220(11) .0227(11) Uani ? ? 1.00000 ? ? C112 .1977(2) .31514(15) .06090(13) .0278(12) Uani ? ? 1.00000 ? ? C113 .0785(2) .31501(16) .02606(13) .0300(12) Uani ? ? 1.00000 ? ? C114 -.0044(2) .25766(16) .04189(12) .0273(12) Uani ? ? 1.00000 ? ? C1141 -.1331(2) .25744(19) .00460(14) .0390(15) Uani ? ? 1.00000 ? ? C115 .0357(2) .19889(16) .09362(13) .0316(13) Uani ? ? 1.00000 ? ? C116 .1537(2) .19775(16) .12755(13) .0297(12) Uani ? ? 1.00000 ? ? C121 .4774(2) .31761(14) .10955(11) .0229(11) Uani ? ? 1.00000 ? ? C122 .4925(2) .29666(16) .04368(12) .0295(12) Uani ? ? 1.00000 ? ? C123 .5617(2) .34591(17) .00823(12) .0301(13) Uani ? ? 1.00000 ? ? C124 .6202(3) .41684(16) .03761(14) .0358(14) Uani ? ? 1.00000 ? ? C1241 .6949(3) .47095(18) -.00119(17) .0536(19) Uani ? ? 1.00000 ? ? C125 .6091(3) .43641(17) .10494(15) .0465(16) Uani ? ? 1.00000 ? ? C126 .5373(3) .38842(16) .13957(14) .0372(14) Uani ? ? 1.00000 ? ? C131 .3978(2) .30413(14) .23693(11) .0211(11) Uani ? ? 1.00000 ? ? C132 .3168(2) .36741(16) .24538(12) .0291(12) Uani ? ? 1.00000 ? ? C133 .3301(2) .41187(16) .30666(13) .0326(13) Uani ? ? 1.00000 ? ? C134 .4252(2) .39586(15) .36034(12) .0265(12) Uani ? ? 1.00000 ? ? C1341 .4416(2) .44717(18) .42507(13) .0364(14) Uani ? ? 1.00000 ? ? C135 .5053(2) .33224(16) .35202(12) .0283(12) Uani ? ? 1.00000 ? ? C136 .4920(2) .28628(15) .29126(12) .0255(11) Uani ? ? 1.00000 ? ? N11 .48587(17) -.03757(12) .24736(9) .0234(9) Uani ? ? 1.00000 ? ? N12 .42125(18) .03568(12) .24520(9) .0247(10) Uani ? ? 1.00000 ? ? C13 .3976(2) .04651(16) .30878(12) .0283(12) Uani ? ? 1.00000 ? ? C14 .4496(2) -.01698(17) .35197(12) .0344(13) Uani ? ? 1.00000 ? ? C15 .5058(2) -.06891(17) .31193(12) .0320(13) Uani ? ? 1.00000 ? ? C16 .3177(3) .11639(18) .32350(14) .0422(15) Uani ? ? 1.00000 ? ? N21 .45188(17) -.05174(12) .11616(9) .0226(9) Uani ? ? 1.00000 ? ? N22 .40537(17) .02514(12) .09532(9) .0214(9) Uani ? ? 1.00000 ? ? C23 .3480(2) .01631(15) .03014(11) .0239(11) Uani ? ? 1.00000 ? ? C24 .3583(2) -.06688(16) .00850(12) .0289(12) Uani ? ? 1.00000 ? ? C25 .4239(2) -.10722(15) .06417(13) .0284(12) Uani ? ? 1.00000 ? ? C26 .2846(2) .08782(16) -.00888(12) .0291(12) Uani ? ? 1.00000 ? ? N31 .65368(17) -.00830(12) .18501(9) .0229(9) Uani ? ? 1.00000 ? ? N32 .63340(17) .07673(12) .17880(9) .0223(9) Uani ? ? 1.00000 ? ? C33 .7404(2) .11346(14) .18236(11) .0223(11) Uani ? ? 1.00000 ? ? C34 .8314(2) .05216(16) .19149(12) .0271(12) Uani ? ? 1.00000 ? ? C35 .7733(2) -.02363(15) .19297(12) .0254(11) Uani ? ? 1.00000 ? ? C36 .7491(2) .20642(15) .17410(12) .0279(12) Uani ? ? 1.00000 ? ? N41 .56978(18) -.15836(12) .19034(10) .0254(10) Uani ? ? 1.00000 ? ? N42 .66045(19) -.19292(12) .16117(10) .0267(10) Uani ? ? 1.00000 ? ? C43 .6374(2) -.27552(15) .15621(12) .0287(12) Uani ? ? 1.00000 ? ? C44 .5310(2) -.29491(15) .18105(13) .0314(13) Uani ? ? 1.00000 ? ? C45 .4901(2) -.21978(16) .20134(13) .0299(12) Uani ? ? 1.00000 ? ? C46 .7216(3) -.33308(16) .12916(14) .0354(14) Uani ? ? 1.00000 ? ? B .5421(2) -.06459(17) .18484(13) .0229(12) Uani ? ? 1.00000 ? ? H112 .25383 .35580 .04989 .03600 Uiso ? ? 1.00000 ? ? H113 .05389 .35531 -.01027 .03800 Uiso ? ? 1.00000 ? ? H1141a -.13622 .24010 -.04182 .05900 Uiso ? ? 1.00000 ? ? H1141b -.16543 .31320 .00435 .05900 Uiso ? ? 1.00000 ? ? H1141c -.18260 .22079 .02564 .05900 Uiso ? ? 1.00000 ? ? H115 -.02020 .15833 .10590 .03900 Uiso ? ? 1.00000 ? ? H116 .17952 .15555 .16181 .03600 Uiso ? ? 1.00000 ? ? H122 .45509 .24670 .02296 .03600 Uiso ? ? 1.00000 ? ? H123 .56971 .32943 -.03760 .03700 Uiso ? ? 1.00000 ? ? H1241a .76606 .48882 .02931 .08200 Uiso ? ? 1.00000 ? ? H1241b .65041 .51938 -.01933 .08200 Uiso ? ? 1.00000 ? ? H1241c .71986 .44165 -.03901 .08200 Uiso ? ? 1.00000 ? ? H125 .64980 .48530 .12730 .05600 Uiso ? ? 1.00000 ? ? H126 .52922 .40270 .18530 .04500 Uiso ? ? 1.00000 ? ? H132 .25272 .38069 .20823 .03600 Uiso ? ? 1.00000 ? ? H133 .27309 .45398 .31247 .04000 Uiso ? ? 1.00000 ? ? H1341a .36506 .46354 .43471 .05500 Uiso ? ? 1.00000 ? ? H1341b .48647 .49712 .41928 .05500 Uiso ? ? 1.00000 ? ? H1341c .48420 .41645 .46305 .05500 Uiso ? ? 1.00000 ? ? H135 .57152 .32045 .38944 .03500 Uiso ? ? 1.00000 ? ? H136 .54818 .24233 .28573 .03200 Uiso ? ? 1.00000 ? ? H14 .44754 -.02283 .40051 .04300 Uiso ? ? 1.00000 ? ? H15 .55159 -.11938 .32647 .04000 Uiso ? ? 1.00000 ? ? H16a .28849 .14839 .28303 .06500 Uiso ? ? 1.00000 ? ? H16b .35862 .15299 .35802 .06500 Uiso ? ? 1.00000 ? ? H16c .24900 .09306 .33953 .06500 Uiso ? ? 1.00000 ? ? H24 .32583 -.08982 -.03546 .03600 Uiso ? ? 1.00000 ? ? H25 .44833 -.16596 .06592 .03400 Uiso ? ? 1.00000 ? ? H26a .22318 .06604 -.04485 .04400 Uiso ? ? 1.00000 ? ? H26b .33983 .11964 -.02878 .04400 Uiso ? ? 1.00000 ? ? H26c .24569 .12391 .01929 .04400 Uiso ? ? 1.00000 ? ? H34 .91637 .06195 .19622 .03400 Uiso ? ? 1.00000 ? ? H35 .81124 -.07806 .19801 .03100 Uiso ? ? 1.00000 ? ? H36a .71440 .23474 .20848 .04200 Uiso ? ? 1.00000 ? ? H36b .70501 .22291 .12991 .04200 Uiso ? ? 1.00000 ? ? H36c .83042 .22386 .17766 .04200 Uiso ? ? 1.00000 ? ? H44 .49434 -.34914 .18319 .03800 Uiso ? ? 1.00000 ? ? H45 .41849 -.21202 .22118 .03700 Uiso ? ? 1.00000 ? ? H46a .78414 -.30235 .11487 .05100 Uiso ? ? 1.00000 ? ? H46b .67802 -.36373 .09065 .05100 Uiso ? ? 1.00000 ? ? H46c .75534 -.37280 .16359 .05100 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 .02520(16) .01771(15) .02247(15) .00037(12) .00299(11) -.00069(11) P .0241(3) .0176(3) .0207(3) .0002(2) .0027(2) -.0003(2) C111 .0248(12) .0203(12) .0222(11) .0020(10) .0020(9) -.0024(9) C112 .0295(14) .0228(13) .0302(13) -.0023(10) .0030(10) .0027(10) C113 .0333(14) .0267(13) .0285(13) .0049(11) .0013(11) .0023(10) C114 .0260(13) .0304(14) .0256(12) .0021(11) .0051(10) -.0058(10) C1141 .0263(14) .0477(18) .0414(15) .0018(13) .0019(12) .0042(13) C115 .0282(14) .0311(14) .0368(14) -.0041(11) .0095(11) .0048(11) C116 .0315(14) .0277(13) .0296(13) .0021(11) .0048(11) .0073(11) C121 .0268(13) .0183(11) .0228(11) .0019(10) .0023(10) .0020(9) C122 .0339(14) .0267(13) .0284(13) -.0041(11) .0071(11) -.0061(10) C123 .0330(14) .0342(14) .0237(12) .0022(12) .0070(10) .0005(11) C124 .0491(18) .0213(13) .0418(15) .0005(12) .0210(13) .0040(11) C1241 .079(2) .0306(16) .062(2) -.0083(16) .0428(18) .0038(15) C125 .073(2) .0261(14) .0468(17) -.0191(15) .0279(16) -.0101(13) C126 .0552(18) .0272(14) .0327(14) -.0096(13) .0173(13) -.0078(11) C131 .0242(12) .0178(11) .0206(11) -.0021(9) .0026(9) -.0005(9) C132 .0262(13) .0303(14) .0288(13) .0070(11) -.0008(10) -.0018(10) C133 .0309(14) .0293(14) .0374(14) .0098(11) .0058(11) -.0062(11) C134 .0271(13) .0280(13) .0257(12) -.0028(10) .0077(10) -.0048(10) C1341 .0382(16) .0394(16) .0320(14) .0023(13) .0073(11) -.0129(12) C135 .0285(13) .0308(14) .0244(12) .0023(11) .0009(10) -.0028(10) C136 .0259(13) .0232(12) .0272(12) .0042(10) .0043(10) -.0004(10) N11 .0269(11) .0189(10) .0234(10) -.0011(8) .0025(8) .0021(8) N12 .0291(11) .0228(10) .0233(10) -.0002(9) .0072(8) -.0001(8) C13 .0344(14) .0281(13) .0238(12) -.0099(11) .0090(10) -.0030(10) C14 .0458(17) .0356(15) .0222(12) -.0086(13) .0068(11) .0007(11) C15 .0382(15) .0290(14) .0270(13) -.0042(12) .0014(11) .0057(11) C16 .063(2) .0359(16) .0336(15) .0019(14) .0252(14) -.0014(12) N21 .0242(10) .0195(10) .0233(10) -.0020(8) .0027(8) -.0023(8) N22 .0244(10) .0193(10) .0202(9) -.0016(8) .0033(8) .0007(8) C23 .0232(12) .0281(13) .0201(11) -.0060(10) .0029(9) -.0003(10) C24 .0320(14) .0314(14) .0224(12) -.0046(11) .0025(10) -.0054(10) C25 .0316(14) .0221(13) .0312(13) -.0038(10) .0054(11) -.0091(10) C26 .0295(14) .0312(13) .0246(12) -.0031(11) -.0007(10) .0020(10) N31 .0263(11) .0177(10) .0237(10) .0008(8) .0019(8) .0000(8) N32 .0261(11) .0178(10) .0228(10) -.0009(8) .0035(8) -.0000(8) C33 .0249(12) .0226(12) .0185(10) -.0026(10) .0017(9) -.0024(9) C34 .0226(12) .0283(13) .0296(12) -.0022(10) .0028(10) -.0031(10) C35 .0248(13) .0240(13) .0261(12) .0039(10) .0017(10) -.0012(10) C36 .0275(13) .0247(13) .0307(13) -.0045(10) .0034(10) -.0002(10) N41 .0271(11) .0202(10) .0282(11) .0002(9) .0031(8) .0017(8) N42 .0317(12) .0203(10) .0273(10) .0018(9) .0029(9) -.0005(8) C43 .0356(15) .0224(12) .0258(12) .0012(11) -.0008(10) -.0006(10) C44 .0392(16) .0191(12) .0333(14) -.0046(11) .0001(11) .0019(10) C45 .0318(14) .0235(13) .0339(13) -.0025(11) .0044(11) .0043(11) C46 .0418(16) .0251(14) .0383(15) .0019(12) .0052(12) -.0050(11) B .0260(14) .0192(13) .0226(13) .0003(11) .0022(10) .0007(11) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Cu P . . 2.1611(7) ? Cu N12 . . 2.134(2) ? Cu N22 . . 2.0381(18) ? Cu N32 . . 2.083(2) ? P C111 . . 1.830(2) ? P C121 . . 1.833(2) ? P C131 . . 1.823(2) ? C111 C112 . . 1.396(3) ? C111 C116 . . 1.396(4) ? C112 C113 . . 1.394(3) ? C112 H112 . . .958(3) ? C113 C114 . . 1.383(4) ? C113 H113 . . .966(2) ? C114 C1141 . . 1.503(3) ? C114 C115 . . 1.399(3) ? C1141 H1141a . . .954(3) ? C1141 H1141b . . .959(3) ? C1141 H1141c . . .954(3) ? C115 C116 . . 1.377(3) ? C115 H115 . . .964(3) ? C116 H116 . . .961(2) ? C121 C122 . . 1.386(3) ? C121 C126 . . 1.390(3) ? C122 C123 . . 1.384(4) ? C122 H122 . . .956(2) ? C123 C124 . . 1.381(4) ? C123 H123 . . .965(3) ? C124 C1241 . . 1.509(5) ? C124 C125 . . 1.397(4) ? C1241 H1241a . . .956(3) ? C1241 H1241b . . .953(3) ? C1241 H1241c . . .967(3) ? C125 C126 . . 1.382(4) ? C125 H125 . . .968(3) ? C126 H126 . . .954(3) ? C131 C132 . . 1.390(3) ? C131 C136 . . 1.396(3) ? C132 C133 . . 1.389(4) ? C132 H132 . . .956(2) ? C133 C134 . . 1.389(3) ? C133 H133 . . .950(3) ? C134 C1341 . . 1.502(4) ? C134 C135 . . 1.386(4) ? C1341 H1341a . . .954(3) ? C1341 H1341b . . .960(3) ? C1341 H1341c . . .950(3) ? C135 C136 . . 1.392(3) ? C135 H135 . . .970(2) ? C136 H136 . . .963(2) ? N11 N12 . . 1.371(3) ? N11 C15 . . 1.352(3) ? N11 B . . 1.551(3) ? N12 C13 . . 1.345(3) ? C13 C14 . . 1.383(3) ? C13 C16 . . 1.493(4) ? C14 C15 . . 1.377(4) ? C14 H14 . . .970(2) ? C15 H15 . . .970(3) ? C16 H16a . . .956(3) ? C16 H16b . . .951(3) ? C16 H16c . . .964(3) ? N21 N22 . . 1.365(3) ? N21 C25 . . 1.349(3) ? N21 B . . 1.556(3) ? N22 C23 . . 1.341(3) ? C23 C24 . . 1.402(4) ? C23 C26 . . 1.484(3) ? C24 C25 . . 1.370(3) ? C24 H24 . . .953(2) ? C25 H25 . . .973(2) ? C26 H26a . . .963(2) ? C26 H26b . . .943(3) ? C26 H26c . . .961(3) ? N31 N32 . . 1.374(3) ? N31 C35 . . 1.352(3) ? N31 B . . 1.544(3) ? N32 C33 . . 1.332(3) ? C33 C34 . . 1.404(3) ? C33 C36 . . 1.493(3) ? C34 C35 . . 1.376(3) ? C34 H34 . . .958(2) ? C35 H35 . . .963(2) ? C36 H36a . . .957(3) ? C36 H36b . . .960(2) ? C36 H36c . . .949(2) ? N41 N42 . . 1.377(3) ? N41 C45 . . 1.372(3) ? N41 B . . 1.524(3) ? N42 C43 . . 1.340(3) ? C43 C44 . . 1.411(4) ? C43 C46 . . 1.488(4) ? C44 C45 . . 1.368(4) ? C44 H44 . . .961(2) ? C45 H45 . . .968(3) ? C46 H46a . . .943(3) ? C46 H46b . . .961(3) ? C46 H46c . . .956(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 P Cu N12 . . . 122.87(6) ? P Cu N22 . . . 125.90(5) ? P Cu N32 . . . 126.63(6) ? N12 Cu N22 . . . 89.76(7) ? N12 Cu N32 . . . 90.89(8) ? N22 Cu N32 . . . 89.85(7) ? Cu P C111 . . . 112.57(8) ? Cu P C121 . . . 115.94(8) ? Cu P C131 . . . 116.62(7) ? C111 P C121 . . . 104.10(10) ? C111 P C131 . . . 104.34(11) ? C121 P C131 . . . 101.71(10) ? P C111 C112 . . . 124.00(19) ? P C111 C116 . . . 118.12(17) ? C112 C111 C116 . . . 117.8(2) ? C111 C112 C113 . . . 120.7(2) ? C111 C112 H112 . . . 118.9(2) ? C113 C112 H112 . . . 120.4(2) ? C112 C113 C114 . . . 121.3(2) ? C112 C113 H113 . . . 119.2(3) ? C114 C113 H113 . . . 119.5(2) ? C113 C114 C1141 . . . 121.5(2) ? C113 C114 C115 . . . 117.7(2) ? C1141 C114 C115 . . . 120.8(2) ? C114 C1141 H1141a . . . 109.7(2) ? C114 C1141 H1141b . . . 109.4(2) ? C114 C1141 H1141c . . . 112.1(2) ? H1141a C1141 H1141b . . . 108.4(3) ? H1141a C1141 H1141c . . . 108.8(3) ? H1141b C1141 H1141c . . . 108.4(3) ? C114 C115 C116 . . . 121.4(2) ? C114 C115 H115 . . . 119.5(2) ? C116 C115 H115 . . . 119.1(2) ? C111 C116 C115 . . . 121.1(2) ? C111 C116 H116 . . . 119.2(2) ? C115 C116 H116 . . . 119.7(3) ? P C121 C122 . . . 119.71(17) ? P C121 C126 . . . 122.4(2) ? C122 C121 C126 . . . 117.6(2) ? C121 C122 C123 . . . 121.2(2) ? C121 C122 H122 . . . 118.9(3) ? C123 C122 H122 . . . 119.9(3) ? C122 C123 C124 . . . 121.3(2) ? C122 C123 H123 . . . 118.8(2) ? C124 C123 H123 . . . 119.9(3) ? C123 C124 C1241 . . . 121.4(3) ? C123 C124 C125 . . . 117.7(3) ? C1241 C124 C125 . . . 121.0(2) ? C124 C1241 H1241a . . . 109.3(3) ? C124 C1241 H1241b . . . 110.4(3) ? C124 C1241 H1241c . . . 112.8(3) ? H1241a C1241 H1241b . . . 108.7(3) ? H1241a C1241 H1241c . . . 107.6(4) ? H1241b C1241 H1241c . . . 107.8(3) ? C124 C125 C126 . . . 120.9(3) ? C124 C125 H125 . . . 119.9(3) ? C126 C125 H125 . . . 119.3(3) ? C121 C126 C125 . . . 121.2(3) ? C121 C126 H126 . . . 118.4(3) ? C125 C126 H126 . . . 120.4(3) ? P C131 C132 . . . 123.74(16) ? P C131 C136 . . . 117.53(18) ? C132 C131 C136 . . . 118.6(2) ? C131 C132 C133 . . . 120.4(2) ? C131 C132 H132 . . . 119.2(2) ? C133 C132 H132 . . . 120.4(3) ? C132 C133 C134 . . . 121.3(2) ? C132 C133 H133 . . . 119.8(2) ? C134 C133 H133 . . . 118.8(3) ? C133 C134 C1341 . . . 120.7(2) ? C133 C134 C135 . . . 118.2(2) ? C1341 C134 C135 . . . 121.1(2) ? C134 C1341 H1341a . . . 110.1(2) ? C134 C1341 H1341b . . . 109.5(2) ? C134 C1341 H1341c . . . 111.2(2) ? H1341a C1341 H1341b . . . 108.3(3) ? H1341a C1341 H1341c . . . 109.1(3) ? H1341b C1341 H1341c . . . 108.6(2) ? C134 C135 C136 . . . 121.1(2) ? C134 C135 H135 . . . 118.6(2) ? C136 C135 H135 . . . 120.3(2) ? C131 C136 C135 . . . 120.4(2) ? C131 C136 H136 . . . 119.0(2) ? C135 C136 H136 . . . 120.7(2) ? N12 N11 C15 . . . 109.8(2) ? N12 N11 B . . . 120.22(18) ? C15 N11 B . . . 129.1(2) ? Cu N12 N11 . . . 112.17(15) ? Cu N12 C13 . . . 134.82(16) ? N11 N12 C13 . . . 105.95(18) ? N12 C13 C14 . . . 110.6(2) ? N12 C13 C16 . . . 120.5(2) ? C14 C13 C16 . . . 128.8(2) ? C13 C14 C15 . . . 105.7(2) ? C13 C14 H14 . . . 126.8(3) ? C15 C14 H14 . . . 127.5(3) ? N11 C15 C14 . . . 108.0(2) ? N11 C15 H15 . . . 125.0(3) ? C14 C15 H15 . . . 127.0(2) ? C13 C16 H16a . . . 111.2(3) ? C13 C16 H16b . . . 111.4(3) ? C13 C16 H16c . . . 109.1(2) ? H16a C16 H16b . . . 108.9(3) ? H16a C16 H16c . . . 107.9(3) ? H16b C16 H16c . . . 108.2(3) ? N22 N21 C25 . . . 109.42(17) ? N22 N21 B . . . 122.41(17) ? C25 N21 B . . . 127.3(2) ? Cu N22 N21 . . . 113.52(12) ? Cu N22 C23 . . . 139.37(16) ? N21 N22 C23 . . . 106.75(18) ? N22 C23 C24 . . . 109.9(2) ? N22 C23 C26 . . . 121.5(2) ? C24 C23 C26 . . . 128.6(2) ? C23 C24 C25 . . . 105.0(2) ? C23 C24 H24 . . . 126.9(2) ? C25 C24 H24 . . . 128.0(3) ? N21 C25 C24 . . . 108.9(2) ? N21 C25 H25 . . . 125.2(2) ? C24 C25 H25 . . . 125.9(2) ? C23 C26 H26a . . . 108.8(2) ? C23 C26 H26b . . . 109.7(2) ? C23 C26 H26c . . . 112.6(2) ? H26a C26 H26b . . . 109.0(2) ? H26a C26 H26c . . . 107.5(2) ? H26b C26 H26c . . . 109.2(3) ? N32 N31 C35 . . . 109.54(18) ? N32 N31 B . . . 116.65(18) ? C35 N31 B . . . 133.7(2) ? Cu N32 N31 . . . 117.50(14) ? Cu N32 C33 . . . 135.46(16) ? N31 N32 C33 . . . 107.03(18) ? N32 C33 C34 . . . 109.7(2) ? N32 C33 C36 . . . 120.4(2) ? C34 C33 C36 . . . 129.9(2) ? C33 C34 C35 . . . 105.7(2) ? C33 C34 H34 . . . 126.5(2) ? C35 C34 H34 . . . 127.8(2) ? N31 C35 C34 . . . 108.0(2) ? N31 C35 H35 . . . 126.1(2) ? C34 C35 H35 . . . 125.9(2) ? C33 C36 H36a . . . 110.2(2) ? C33 C36 H36b . . . 109.7(2) ? C33 C36 H36c . . . 111.3(2) ? H36a C36 H36b . . . 108.0(2) ? H36a C36 H36c . . . 108.9(2) ? H36b C36 H36c . . . 108.7(3) ? N42 N41 C45 . . . 109.9(2) ? N42 N41 B . . . 121.3(2) ? C45 N41 B . . . 125.2(2) ? N41 N42 C43 . . . 105.9(2) ? N42 C43 C44 . . . 110.8(2) ? N42 C43 C46 . . . 120.1(2) ? C44 C43 C46 . . . 129.1(2) ? C43 C44 C45 . . . 105.4(2) ? C43 C44 H44 . . . 127.7(3) ? C45 C44 H44 . . . 126.9(3) ? N41 C45 C44 . . . 108.0(2) ? N41 C45 H45 . . . 126.4(2) ? C44 C45 H45 . . . 125.6(3) ? C43 C46 H46a . . . 110.5(2) ? C43 C46 H46b . . . 109.3(2) ? C43 C46 H46c . . . 110.3(3) ? H46a C46 H46b . . . 109.1(3) ? H46a C46 H46c . . . 109.5(3) ? H46b C46 H46c . . . 108.0(2) ? N11 B N21 . . . 111.3(2) ? N11 B N31 . . . 106.83(18) ? N11 B N41 . . . 108.8(2) ? N21 B N31 . . . 109.17(19) ? N21 B N41 . . . 106.49(18) ? N31 B N41 . . . 114.3(2) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? _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 1472 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 20 _reflns_limit_l_min -26 _reflns_limit_l_max 25 _reflns_number_observed ? _reflns_d_resolution_high .727 _reflns_d_resolution_low 12.288 _diffrn_reflns_av_sigmaI/netI .066 _diffrn_reflns_theta_min 1.65 _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 .06 _refine_ls_wR_factor_all .054 _refine_ls_goodness_of_fit_all 1.433 _refine_ls_shift/su_mean . #========================================================================== # 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 data_cpm46 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C32 H34 B1 Cu1 N4 P2' _chemical_formula_moiety ? _chemical_formula_weight 610.96 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _cell_length_a 9.8820(10) _cell_length_b 10.560(2) _cell_length_c 16.301(2) _cell_angle_alpha 77.826(2) _cell_angle_beta 79.893(2) _cell_angle_gamma 66.779(2) _cell_volume 1520.0(4) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 5373 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu .853 _exptl_crystal_description prism _exptl_crystal_size_max .65 _exptl_crystal_size_mid .4 _exptl_crystal_size_min .2 _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 .737 _exptl_absorpt_correction_T_max .901 _diffrn_reflns_number 17049 _reflns_number_total 7331 _reflns_Friedel_coverage 0 _reflns_number_gt 6563 _reflns_threshold_expression 'F > 4.0sig(F )' _diffrn_reflns_theta_max 29.07 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .015 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? #<< do not append units _diffrn_standards_decay_% 0 #<< do not append % _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .027 _refine_ls_wR_factor_ref .041 _refine_ls_goodness_of_fit_ref 1.567 _refine_ls_number_reflns 6563 _refine_ls_number_parameters 497 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max .008 _refine_diff_density_min -.319 _refine_diff_density_max .34 _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 64 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 68 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 8 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 4 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cu ? 0 2 .263 1.266 'Int Tables Vol IV Tables 2.2B and 2.3.1' B ? 0 2 0 .001 '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 .279483(18) .469602(16) .220427(10) .01836(15) Uani ? ? 1.00000 ? ? P1 .39619(4) .23716(4) .25038(2) .0205(3) Uani ? ? 1.00000 ? ? C111 .31435(17) .16274(15) .34901(9) .0230(12) Uani ? ? 1.00000 ? ? C112 .3938(2) .04194(16) .40065(10) .0296(13) Uani ? ? 1.00000 ? ? C113 .3231(2) -.01040(18) .47361(11) .0345(15) Uani ? ? 1.00000 ? ? C114 .1731(2) .0560(2) .49496(10) .0352(16) Uani ? ? 1.00000 ? ? C115 .0934(2) .1763(2) .44432(12) .0406(17) Uani ? ? 1.00000 ? ? C116 .16393(19) .2303(2) .37219(11) .0338(14) Uani ? ? 1.00000 ? ? C121 .59258(16) .17642(15) .26523(10) .0241(11) Uani ? ? 1.00000 ? ? C122 .69793(19) .04866(17) .24567(12) .0335(14) Uani ? ? 1.00000 ? ? C123 .8463(2) .0122(2) .25570(12) .0390(15) Uani ? ? 1.00000 ? ? C124 .89145(18) .1003(2) .28534(11) .0365(15) Uani ? ? 1.00000 ? ? C125 .7882(2) .2264(2) .30585(12) .0358(15) Uani ? ? 1.00000 ? ? C126 .63976(18) .26496(17) .29475(11) .0305(13) Uani ? ? 1.00000 ? ? C131 .3940(2) .12831(17) .17722(11) .0318(15) Uani ? ? 1.00000 ? ? P1' .05246(4) .54252(4) .17463(2) .0174(3) Uani ? ? 1.00000 ? ? C111' .00539(16) .68993(14) .08823(9) .0201(11) Uani ? ? 1.00000 ? ? C112' -.13869(18) .78674(16) .07914(10) .0274(13) Uani ? ? 1.00000 ? ? C113' -.1668(2) .89184(17) .00958(11) .0352(15) Uani ? ? 1.00000 ? ? C114' -.0535(2) .90156(17) -.05169(11) .0335(15) Uani ? ? 1.00000 ? ? C115' .0896(2) .80617(18) -.04315(10) .0317(14) Uani ? ? 1.00000 ? ? C116' .11914(18) .70201(16) .02686(9) .0253(12) Uani ? ? 1.00000 ? ? C121' -.10596(15) .59201(14) .25515(9) .0191(10) Uani ? ? 1.00000 ? ? C122' -.09446(17) .64903(16) .32178(10) .0247(12) Uani ? ? 1.00000 ? ? C123' -.21219(19) .68924(18) .38398(11) .0307(14) Uani ? ? 1.00000 ? ? C124' -.34229(18) .67086(17) .38047(10) .0281(13) Uani ? ? 1.00000 ? ? C125' -.35508(17) .61329(18) .31499(11) .0296(13) Uani ? ? 1.00000 ? ? C126' -.23777(17) .57367(17) .25234(10) .0269(13) Uani ? ? 1.00000 ? ? C131' .02068(18) .41298(16) .12879(10) .0248(13) Uani ? ? 1.00000 ? ? N11 .38409(13) .70183(12) .15606(8) .0208(10) Uani ? ? 1.00000 ? ? N12 .41265(13) .56719(12) .14867(7) .0202(9) Uani ? ? 1.00000 ? ? C13 .53090(17) .53048(17) .09143(9) .0250(12) Uani ? ? 1.00000 ? ? C14 .57805(19) .64145(19) .06066(10) .0311(14) Uani ? ? 1.00000 ? ? C15 .48264(18) .74736(17) .10310(10) .0281(13) Uani ? ? 1.00000 ? ? B1 .25010(19) .78098(17) .21621(11) .0236(13) Uani ? ? 1.00000 ? ? N21 .26395(13) .69661(12) .30662(8) .0215(10) Uani ? ? 1.00000 ? ? N22 .27322(13) .56110(12) .32242(8) .0217(10) Uani ? ? 1.00000 ? ? C23 .28348(17) .51882(18) .40541(10) .0285(13) Uani ? ? 1.00000 ? ? C24 .2796(2) .6263(2) .44399(11) .0353(15) Uani ? ? 1.00000 ? ? C25 .26682(18) .73649(19) .37933(11) .0306(14) Uani ? ? 1.00000 ? ? H112 .499(2) .001(2) .3889(12) .036(5) Uiso ? ? 1.00000 ? ? H113 .373(2) -.086(2) .5075(12) .031(5) Uiso ? ? 1.00000 ? ? H114 .119(2) .020(2) .5471(13) .048(6) Uiso ? ? 1.00000 ? ? H115 -.009(2) .224(2) .4596(13) .041(5) Uiso ? ? 1.00000 ? ? H116 .113(2) .314(2) .3450(13) .044(6) Uiso ? ? 1.00000 ? ? H122 .666(2) -.011(2) .2260(12) .033(5) Uiso ? ? 1.00000 ? ? H123 .909(2) -.068(2) .2366(13) .045(6) Uiso ? ? 1.00000 ? ? H124 .989(2) .0808(19) .2934(11) .031(5) Uiso ? ? 1.00000 ? ? H125 .815(2) .283(2) .3275(13) .039(5) Uiso ? ? 1.00000 ? ? H126 .568(2) .355(2) .3023(11) .029(5) Uiso ? ? 1.00000 ? ? H131a .449(2) .151(2) .1244(14) .046(6) Uiso ? ? 1.00000 ? ? H131b .296(2) .147(2) .1697(12) .039(5) Uiso ? ? 1.00000 ? ? H131c .444(2) .026(2) .1961(13) .041(5) Uiso ? ? 1.00000 ? ? H112' -.216(2) .779(2) .1190(12) .035(5) Uiso ? ? 1.00000 ? ? H113' -.266(2) .960(2) .0050(13) .045(6) Uiso ? ? 1.00000 ? ? H114' -.074(2) .974(2) -.0960(14) .044(6) Uiso ? ? 1.00000 ? ? H115' .169(2) .811(2) -.0858(12) .038(5) Uiso ? ? 1.00000 ? ? H116' .219(2) .641(2) .0347(12) .030(5) Uiso ? ? 1.00000 ? ? H122' -.002(2) .6598(18) .3275(11) .027(4) Uiso ? ? 1.00000 ? ? H123' -.204(3) .725(2) .4270(15) .062(7) Uiso ? ? 1.00000 ? ? H124' -.423(2) .696(2) .4223(13) .042(5) Uiso ? ? 1.00000 ? ? H125' -.443(2) .590(2) .3123(13) .043(6) Uiso ? ? 1.00000 ? ? H126' -.248(2) .5298(19) .2079(11) .030(5) Uiso ? ? 1.00000 ? ? H131'a .021(2) .3335(19) .1703(12) .028(5) Uiso ? ? 1.00000 ? ? H131'b .095(2) .3834(19) .0839(12) .032(5) Uiso ? ? 1.00000 ? ? H131'c -.074(2) .4529(17) .1064(11) .024(4) Uiso ? ? 1.00000 ? ? H13 .5719(19) .4353(18) .0773(11) .026(4) Uiso ? ? 1.00000 ? ? H14 .661(2) .645(2) .0205(13) .046(6) Uiso ? ? 1.00000 ? ? H15 .480(2) .8388(19) .1011(11) .029(5) Uiso ? ? 1.00000 ? ? H23 .291(2) .4256(19) .4296(11) .028(5) Uiso ? ? 1.00000 ? ? H24 .288(2) .620(2) .5039(14) .054(6) Uiso ? ? 1.00000 ? ? H25 .260(2) .822(2) .3771(11) .029(5) Uiso ? ? 1.00000 ? ? H1a .1478(19) .7822(17) .1936(10) .024(4) Uiso ? ? 1.00000 ? ? H1b .2551(19) .8838(17) .2177(10) .026(4) 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 .01785(10) .01714(9) .01985(10) -.00647(7) -.00184(7) -.00248(6) P1 .02043(18) .01654(17) .02286(18) -.00618(14) -.00099(14) -.00199(13) C111 .0258(7) .0218(7) .0238(7) -.0122(6) -.0018(6) -.0026(5) C112 .0310(9) .0237(7) .0312(8) -.0093(7) -.0024(7) -.0006(6) C113 .0495(11) .0294(8) .0266(8) -.0197(8) -.0068(7) .0037(7) C114 .0480(11) .0465(10) .0220(8) -.0317(9) .0017(7) -.0047(7) C115 .0295(9) .0568(12) .0335(9) -.0183(9) .0038(7) -.0043(8) C116 .0255(8) .0390(9) .0312(9) -.0102(7) -.0023(7) .0025(7) C121 .0198(7) .0187(7) .0272(7) -.0045(5) .0022(6) .0012(6) C122 .0270(8) .0242(8) .0408(10) -.0046(7) .0043(7) -.0033(7) C123 .0245(8) .0295(8) .0441(10) .0009(7) .0078(7) .0024(7) C124 .0188(8) .0414(10) .0355(9) -.0064(7) -.0014(7) .0122(7) C125 .0270(8) .0370(9) .0415(10) -.0121(7) -.0093(7) .0028(8) C126 .0240(8) .0273(8) .0360(9) -.0058(6) -.0051(7) -.0022(7) C131 .0393(10) .0254(8) .0319(9) -.0115(7) -.0033(7) -.0084(7) P1' .01728(17) .01829(17) .01677(17) -.00685(13) -.00160(13) -.00274(13) C111' .0240(7) .0213(6) .0176(6) -.0099(6) -.0054(5) -.0031(5) C112' .0253(8) .0269(8) .0270(8) -.0075(6) -.0041(6) -.0013(6) C113' .0374(10) .0257(8) .0359(9) -.0038(7) -.0127(8) .0009(7) C114' .0496(11) .0255(8) .0263(8) -.0157(7) -.0126(7) .0051(6) C115' .0417(10) .0356(9) .0221(8) -.0216(8) -.0037(7) .0012(6) C116' .0273(8) .0281(7) .0214(7) -.0118(6) -.0031(6) -.0021(6) C121' .0179(6) .0185(6) .0186(6) -.0053(5) -.0019(5) -.0006(5) C122' .0215(7) .0288(7) .0263(7) -.0113(6) .0000(6) -.0074(6) C123' .0288(8) .0382(9) .0279(8) -.0130(7) .0021(6) -.0143(7) C124' .0227(8) .0298(8) .0270(8) -.0072(6) .0039(6) -.0051(6) C125' .0186(7) .0373(9) .0331(8) -.0109(7) -.0005(6) -.0067(7) C126' .0225(7) .0361(8) .0254(8) -.0125(6) -.0028(6) -.0081(6) C131' .0276(8) .0254(7) .0250(7) -.0123(6) -.0009(6) -.0082(6) N11 .0201(6) .0205(6) .0231(6) -.0097(5) -.0027(5) -.0014(5) N12 .0187(6) .0207(6) .0211(6) -.0073(5) -.0011(5) -.0038(5) C13 .0209(7) .0332(8) .0200(7) -.0088(6) .0004(6) -.0066(6) C14 .0274(8) .0466(10) .0231(8) -.0204(7) .0028(6) -.0042(7) C15 .0307(8) .0317(8) .0265(8) -.0193(7) -.0037(6) .0021(6) B1 .0210(8) .0189(7) .0304(9) -.0065(6) -.0020(7) -.0053(6) N21 .0162(6) .0240(6) .0250(6) -.0060(5) -.0004(5) -.0097(5) N22 .0203(6) .0232(6) .0215(6) -.0074(5) -.0021(5) -.0045(5) C23 .0249(8) .0369(9) .0204(7) -.0089(7) -.0010(6) -.0039(6) C24 .0293(8) .0545(11) .0221(8) -.0117(8) .0004(6) -.0163(7) C25 .0235(8) .0365(9) .0349(9) -.0082(7) .0008(6) -.0212(7) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Cu P1 . . 2.2480(5) ? Cu P1' . . 2.2730(5) ? Cu N12 . . 2.0451(13) ? Cu N22 . . 2.0727(15) ? P1 C111 . . 1.8353(15) ? P1 C121 . . 1.8315(16) ? P1 C131 . . 1.831(2) ? C111 C112 . . 1.394(2) ? C111 C116 . . 1.393(2) ? C112 C113 . . 1.394(2) ? C112 H112 . . .95(2) ? C113 C114 . . 1.383(3) ? C113 H113 . . .885(17) ? C114 C115 . . 1.383(2) ? C114 H114 . . 1.01(2) ? C115 C116 . . 1.391(3) ? C115 H115 . . .95(2) ? C116 H116 . . .892(19) ? C121 C122 . . 1.401(2) ? C121 C126 . . 1.391(3) ? C122 C123 . . 1.391(3) ? C122 H122 . . .94(3) ? C123 C124 . . 1.375(3) ? C123 H123 . . .91(2) ? C124 C125 . . 1.387(2) ? C124 H124 . . .93(2) ? C125 C126 . . 1.394(3) ? C125 H125 . . .89(3) ? C126 H126 . . .957(17) ? C131 H131a . . .97(2) ? C131 H131b . . .94(2) ? C131 H131c . . 1.00(2) ? P1' C111' . . 1.8323(13) ? P1' C121' . . 1.8356(13) ? P1' C131' . . 1.839(2) ? C111' C112' . . 1.399(2) ? C111' C116' . . 1.395(2) ? C112' C113' . . 1.390(2) ? C112' H112' . . .93(2) ? C113' C114' . . 1.384(3) ? C113' H113' . . .963(19) ? C114' C115' . . 1.386(2) ? C114' H114' . . .92(2) ? C115' C116' . . 1.390(2) ? C115' H115' . . .96(2) ? C116' H116' . . .953(17) ? C121' C122' . . 1.389(2) ? C121' C126' . . 1.400(3) ? C122' C123' . . 1.393(2) ? C122' H122' . . .99(2) ? C123' C124' . . 1.386(3) ? C123' H123' . . .90(3) ? C124' C125' . . 1.381(3) ? C124' H124' . . .94(2) ? C125' C126' . . 1.394(2) ? C125' H125' . . 1.00(3) ? C126' H126' . . .98(2) ? C131' H131'a . . .959(18) ? C131' H131'b . . .949(18) ? C131' H131'c . . .967(19) ? N11 N12 . . 1.3636(19) ? N11 C15 . . 1.351(2) ? N11 B1 . . 1.559(2) ? N12 C13 . . 1.3413(18) ? C13 C14 . . 1.394(3) ? C13 H13 . . .986(19) ? C14 C15 . . 1.373(2) ? C14 H14 . . .96(2) ? C15 H15 . . .95(2) ? B1 N21 . . 1.551(2) ? B1 H1a . . 1.13(2) ? B1 H1b . . 1.11(2) ? N21 N22 . . 1.368(2) ? N21 C25 . . 1.347(2) ? N22 C23 . . 1.341(2) ? C23 C24 . . 1.394(3) ? C23 H23 . . .96(2) ? C24 C25 . . 1.376(2) ? C24 H24 . . .98(2) ? C25 H25 . . .87(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 P1 Cu P1' . . . 115.48(2) ? P1 Cu N12 . . . 113.06(3) ? P1 Cu N22 . . . 109.59(3) ? P1' Cu N12 . . . 113.61(4) ? P1' Cu N22 . . . 111.94(3) ? N12 Cu N22 . . . 90.47(5) ? Cu P1 C111 . . . 112.06(4) ? Cu P1 C121 . . . 115.69(6) ? Cu P1 C131 . . . 118.57(5) ? C111 P1 C121 . . . 104.08(7) ? C111 P1 C131 . . . 101.20(9) ? C121 P1 C131 . . . 103.31(8) ? P1 C111 C112 . . . 123.58(11) ? P1 C111 C116 . . . 117.69(11) ? C112 C111 C116 . . . 118.72(14) ? C111 C112 C113 . . . 120.33(15) ? C111 C112 H112 . . . 119.3(11) ? C113 C112 H112 . . . 120.1(11) ? C112 C113 C114 . . . 120.38(15) ? C112 C113 H113 . . . 121.2(12) ? C114 C113 H113 . . . 118.4(12) ? C113 C114 C115 . . . 119.71(17) ? C113 C114 H114 . . . 122.0(10) ? C115 C114 H114 . . . 118.3(10) ? C114 C115 C116 . . . 120.14(16) ? C114 C115 H115 . . . 120.1(12) ? C116 C115 H115 . . . 119.8(12) ? C111 C116 C115 . . . 120.70(14) ? C111 C116 H116 . . . 120.8(13) ? C115 C116 H116 . . . 118.1(13) ? P1 C121 C122 . . . 123.68(15) ? P1 C121 C126 . . . 117.72(10) ? C122 C121 C126 . . . 118.55(16) ? C121 C122 C123 . . . 120.3(2) ? C121 C122 H122 . . . 118.4(10) ? C123 C122 H122 . . . 121.3(10) ? C122 C123 C124 . . . 120.63(16) ? C122 C123 H123 . . . 115.2(17) ? C124 C123 H123 . . . 123.9(17) ? C123 C124 C125 . . . 119.77(18) ? C123 C124 H124 . . . 124.1(13) ? C125 C124 H124 . . . 116.1(13) ? C124 C125 C126 . . . 120.0(2) ? C124 C125 H125 . . . 120.7(12) ? C126 C125 H125 . . . 119.2(12) ? C121 C126 C125 . . . 120.70(15) ? C121 C126 H126 . . . 117.1(14) ? C125 C126 H126 . . . 122.0(14) ? P1 C131 H131a . . . 107.2(16) ? P1 C131 H131b . . . 109.3(13) ? P1 C131 H131c . . . 114.1(14) ? H131a C131 H131b . . . 111.5(18) ? H131a C131 H131c . . . 106.5(16) ? H131b C131 H131c . . . 108(2) ? Cu P1' C111' . . . 117.41(6) ? Cu P1' C121' . . . 115.81(5) ? Cu P1' C131' . . . 114.80(5) ? C111' P1' C121' . . . 103.90(6) ? C111' P1' C131' . . . 99.79(8) ? C121' P1' C131' . . . 102.88(8) ? P1' C111' C112' . . . 123.44(11) ? P1' C111' C116' . . . 117.72(10) ? C112' C111' C116' . . . 118.78(12) ? C111' C112' C113' . . . 120.07(15) ? C111' C112' H112' . . . 119.8(10) ? C113' C112' H112' . . . 120.1(10) ? C112' C113' C114' . . . 120.71(15) ? C112' C113' H113' . . . 119.3(12) ? C114' C113' H113' . . . 119.9(12) ? C113' C114' C115' . . . 119.61(15) ? C113' C114' H114' . . . 119.4(13) ? C115' C114' H114' . . . 120.9(13) ? C114' C115' C116' . . . 120.10(16) ? C114' C115' H115' . . . 120.6(10) ? C116' C115' H115' . . . 119.3(10) ? C111' C116' C115' . . . 120.71(14) ? C111' C116' H116' . . . 119.5(11) ? C115' C116' H116' . . . 119.7(11) ? P1' C121' C122' . . . 118.81(12) ? P1' C121' C126' . . . 122.56(12) ? C122' C121' C126' . . . 118.63(13) ? C121' C122' C123' . . . 120.86(17) ? C121' C122' H122' . . . 121.2(10) ? C123' C122' H122' . . . 117.9(10) ? C122' C123' C124' . . . 120.00(18) ? C122' C123' H123' . . . 120.3(16) ? C124' C123' H123' . . . 119.7(16) ? C123' C124' C125' . . . 119.85(15) ? C123' C124' H124' . . . 121.4(16) ? C125' C124' H124' . . . 118.7(17) ? C124' C125' C126' . . . 120.30(18) ? C124' C125' H125' . . . 123.0(12) ? C126' C125' H125' . . . 116.5(12) ? C121' C126' C125' . . . 120.34(18) ? C121' C126' H126' . . . 120.7(11) ? C125' C126' H126' . . . 118.9(11) ? P1' C131' H131'a . . . 111.3(14) ? P1' C131' H131'b . . . 109.8(15) ? P1' C131' H131'c . . . 110.6(12) ? H131'a C131' H131'b . . . 109.3(15) ? H131'a C131' H131'c . . . 107.8(17) ? H131'b C131' H131'c . . . 108.0(16) ? N12 N11 C15 . . . 109.47(12) ? N12 N11 B1 . . . 120.64(13) ? C15 N11 B1 . . . 129.84(14) ? Cu N12 N11 . . . 118.65(8) ? Cu N12 C13 . . . 135.03(12) ? N11 N12 C13 . . . 106.31(13) ? N12 C13 C14 . . . 110.62(15) ? N12 C13 H13 . . . 119.8(11) ? C14 C13 H13 . . . 129.6(11) ? C13 C14 C15 . . . 104.73(15) ? C13 C14 H14 . . . 129.4(14) ? C15 C14 H14 . . . 125.8(14) ? N11 C15 C14 . . . 108.86(17) ? N11 C15 H15 . . . 120.7(10) ? C14 C15 H15 . . . 130.4(10) ? N11 B1 N21 . . . 108.97(10) ? N11 B1 H1a . . . 106.4(8) ? N11 B1 H1b . . . 108.4(8) ? N21 B1 H1a . . . 107.7(8) ? N21 B1 H1b . . . 108.1(9) ? H1a B1 H1b . . . 117.0(12) ? B1 N21 N22 . . . 121.05(14) ? B1 N21 C25 . . . 129.62(15) ? N22 N21 C25 . . . 109.32(12) ? Cu N22 N21 . . . 117.64(9) ? Cu N22 C23 . . . 135.89(12) ? N21 N22 C23 . . . 106.38(14) ? N22 C23 C24 . . . 110.64(15) ? N22 C23 H23 . . . 119.5(12) ? C24 C23 H23 . . . 129.9(12) ? C23 C24 C25 . . . 104.61(16) ? C23 C24 H24 . . . 125.7(14) ? C25 C24 H24 . . . 129.7(15) ? N21 C25 C24 . . . 109.04(18) ? N21 C25 H25 . . . 117.5(12) ? C24 C25 H25 . . . 133.5(12) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cu C111 3.3942(15) . . ? Cu C112 4.6742(16) . . ? Cu C116 3.530(2) . . ? Cu C121 3.4609(13) . . ? Cu C122 4.7285(15) . . ? Cu C126 3.6271(16) . . ? Cu C131 3.513(2) . . ? Cu C111' 3.5154(14) . . ? Cu C112' 4.7719(16) . . ? Cu C116' 3.7298(15) . . ? Cu C121' 3.4884(14) . . ? Cu C122' 3.6920(14) . . ? Cu C126' 4.7417(17) . . ? Cu C131' 3.472(2) . . ? Cu N11 2.9524(15) . . ? Cu C13 3.1406(16) . . ? Cu C14 4.279(2) . . ? Cu C14 4.8013(18) . '2 665' ? Cu C15 4.150(2) . . ? Cu B1 3.172(2) . . ? Cu N21 2.9663(16) . . ? Cu C23 3.1755(18) . . ? Cu C24 4.309(2) . . ? Cu C25 4.166(2) . . ? Cu H116 3.01(2) . . ? Cu H126 3.05(2) . . ? Cu H131a 3.66(2) . . ? Cu H131b 3.61(2) . . ? Cu H131c 4.40(2) . . ? Cu H116' 3.206(17) . . ? Cu H122' 3.190(16) . . ? Cu H125' 4.05(3) . '1 655' ? Cu H131'a 3.65(2) . . ? Cu H131'b 3.56(2) . . ? Cu H131'c 4.31(2) . . ? Cu H13 3.330(17) . . ? Cu H14 4.23(2) . '2 665' ? Cu H23 3.357(18) . . ? Cu H1a 2.997(16) . . ? Cu H1b 4.28(2) . . ? P1 C112 2.8529(16) . . ? P1 C113 4.1413(18) . . ? P1 C114 4.6303(19) . . ? P1 C115 4.086(2) . . ? P1 C116 2.7725(18) . . ? P1 C122 2.8571(16) . . ? P1 C123 4.1412(17) . . ? P1 C124 4.628(2) . . ? P1 C125 4.084(2) . . ? P1 C126 2.768(2) . . ? P1 P1' 3.8231(6) . . ? P1 C131' 4.0917(18) . . ? P1 N12 3.5828(14) . . ? P1 C13 4.0910(18) . . ? P1 N22 3.5317(15) . . ? P1 C23 4.005(2) . . ? P1 H112 2.963(17) . . ? P1 H116 2.84(2) . . ? P1 H122 2.946(16) . . ? P1 H126 2.79(2) . . ? P1 H131a 2.31(2) . . ? P1 H131b 2.32(3) . . ? P1 H131c 2.42(2) . . ? P1 H131'a 3.82(2) . . ? P1 H131'b 4.01(2) . . ? P1 H13 3.743(18) . . ? P1 H23 3.65(2) . . ? C111 C113 2.418(2) . . ? C111 C114 2.797(2) . . ? C111 C115 2.420(2) . . ? C111 C121 2.891(2) . . ? C111 C122 3.697(2) . . ? C111 C126 3.691(3) . . ? C111 C131 2.833(2) . . ? C111 P1' 4.5222(14) . . ? C111 N22 3.999(2) . . ? C111 C23 3.941(3) . . ? C111 H112 2.038(17) . . ? C111 H113 3.93(2) . '2 656' ? C111 H113 3.221(18) . . ? C111 H114 3.81(2) . . ? C111 H115 3.27(2) . . ? C111 H116 2.002(18) . . ? C111 H122 3.678(17) . . ? C111 H124 3.93(2) . '1 455' ? C111 H126 3.70(2) . . ? C111 H131a 3.68(2) . . ? C111 H131b 3.01(2) . . ? C111 H131c 2.98(2) . . ? C111 H123' 3.92(3) . '2 566' ? C111 H23 3.22(2) . . ? C111 H25 3.76(2) . '1 545' ? C112 C112 3.923(3) . '2 656' ? C112 C113 3.623(3) . '2 656' ? C112 C114 2.410(3) . . ? C112 C115 2.774(2) . . ? C112 C116 2.398(2) . . ? C112 C121 3.179(2) . . ? C112 C122 3.584(2) . . ? C112 C126 3.970(3) . . ? C112 C131 3.563(2) . . ? C112 C123' 4.210(2) . '1 645' ? C112 C124' 3.801(2) . '1 645' ? C112 C25 3.990(3) . '1 545' ? C112 H112 3.65(2) . '2 656' ? C112 H113 2.002(18) . . ? C112 H113 3.19(2) . '2 656' ? C112 H114 3.33(2) . . ? C112 H115 3.72(2) . . ? C112 H116 3.206(18) . . ? C112 H122 3.528(18) . . ? C112 H131b 3.88(2) . . ? C112 H131c 3.31(2) . . ? C112 H123' 3.86(2) . '2 566' ? C112 H124' 3.35(2) . '1 645' ? C112 H23 3.88(2) . . ? C112 H25 3.20(3) . '1 545' ? C113 C113 3.840(3) . '2 656' ? C113 C115 2.392(2) . . ? C113 C116 2.767(2) . . ? C113 C121 4.340(2) . '2 656' ? C113 C123 4.435(3) . '2 656' ? C113 C124 4.234(2) . '2 656' ? C113 C125 4.059(3) . '2 656' ? C113 C126 4.129(2) . '2 656' ? C113 C123' 4.194(3) . '2 566' ? C113 C124' 4.023(2) . '1 645' ? C113 C24 4.159(3) . '1 545' ? C113 C25 3.609(3) . '1 545' ? C113 H112 3.12(2) . '2 656' ? C113 H112 2.05(2) . . ? C113 H113 3.61(2) . '2 656' ? C113 H114 2.10(2) . . ? C113 H115 3.247(19) . . ? C113 H116 3.653(18) . . ? C113 H123' 3.41(3) . '2 566' ? C113 H124' 3.291(19) . '1 645' ? C113 H24 3.98(3) . '1 545' ? C113 H25 2.89(2) . '1 545' ? C114 C114 4.005(3) . '2 556' ? C114 C115 4.134(4) . '2 556' ? C114 C116 2.404(2) . . ? C114 C122 4.419(3) . '2 656' ? C114 C123 3.959(3) . '2 656' ? C114 C124 3.673(2) . '2 656' ? C114 C125 3.878(2) . '2 656' ? C114 C126 4.363(2) . '2 656' ? C114 C123' 3.822(3) . '2 566' ? C114 C25 4.377(2) . '2 566' ? C114 C25 3.924(3) . '1 545' ? C114 H112 3.82(2) . '2 656' ? C114 H112 3.27(2) . . ? C114 H113 1.965(17) . . ? C114 H114 3.49(3) . '2 556' ? C114 H115 2.029(18) . . ? C114 H115 3.79(3) . '2 556' ? C114 H116 3.19(2) . . ? C114 H124 3.787(18) . '2 656' ? C114 H124 3.94(2) . '1 455' ? C114 H123' 2.99(3) . '2 566' ? C114 H25 3.21(2) . '1 545' ? C115 C124 3.912(3) . '1 455' ? C115 C125 3.886(3) . '1 455' ? C115 C123' 3.920(3) . '2 566' ? C115 C24 3.799(2) . '2 566' ? C115 C25 4.090(2) . '2 566' ? C115 H112 3.724(19) . . ? C115 H113 3.181(16) . . ? C115 H114 2.06(2) . . ? C115 H114 3.45(3) . '2 556' ? C115 H116 1.98(2) . . ? C115 H124 3.30(2) . '1 455' ? C115 H125 3.31(2) . '1 455' ? C115 H123' 3.05(3) . '2 566' ? C115 H23 3.79(2) . . ? C115 H24 3.58(2) . '2 566' ? C115 H25 3.76(2) . '1 545' ? C116 C121 4.151(2) . . ? C116 C124 4.027(3) . '1 455' ? C116 C125 4.062(3) . '1 455' ? C116 C131 3.662(2) . . ? C116 P1' 4.0446(17) . . ? C116 C121' 4.003(2) . . ? C116 C122' 4.129(2) . . ? C116 C123' 4.377(3) . '2 566' ? C116 C131' 4.250(2) . . ? C116 N22 3.937(3) . . ? C116 C23 3.838(3) . . ? C116 H112 3.256(18) . . ? C116 H113 3.652(17) . . ? C116 H114 3.31(2) . . ? C116 H115 2.03(2) . . ? C116 H124 3.30(3) . '1 455' ? C116 H125 3.45(2) . '1 455' ? C116 H131b 3.49(2) . . ? C116 H131c 3.96(2) . . ? C116 H123' 3.51(3) . '2 566' ? C116 H131'a 3.59(2) . . ? C116 H23 3.16(2) . . ? C116 H25 4.02(2) . '1 545' ? C121 C123 2.422(2) . . ? C121 C124 2.799(2) . . ? C121 C125 2.420(3) . . ? C121 C131 2.872(3) . . ? C121 C115' 4.380(2) . '2 665' ? C121 N12 3.9866(18) . . ? C121 C13 4.089(2) . . ? C121 N22 4.2174(18) . . ? C121 H112 2.73(2) . . ? C121 H113 3.67(2) . '2 656' ? C121 H122 2.02(2) . . ? C121 H123 3.212(18) . . ? C121 H124 3.73(2) . . ? C121 H125 3.22(3) . . ? C121 H126 2.02(2) . . ? C121 H131a 3.01(3) . . ? C121 H131b 3.70(3) . . ? C121 H131c 3.03(3) . . ? C121 H115' 3.431(19) . '2 665' ? C121 H13 3.626(16) . . ? C122 C124 2.403(3) . . ? C122 C125 2.773(3) . . ? C122 C126 2.400(3) . . ? C122 C131 3.124(3) . . ? C122 C112' 3.967(3) . '1 645' ? C122 C113' 4.299(3) . '1 645' ? C122 C114' 4.414(3) . '2 665' ? C122 C115' 3.953(3) . '2 665' ? C122 C121' 4.411(2) . '1 645' ? C122 C122' 3.926(2) . '1 645' ? C122 C123' 3.836(2) . '1 645' ? C122 C124' 4.260(3) . '1 645' ? C122 H112 2.87(2) . . ? C122 H113 4.04(2) . '2 656' ? C122 H114 3.91(2) . '2 656' ? C122 H123 1.96(2) . . ? C122 H124 3.26(2) . . ? C122 H125 3.66(3) . . ? C122 H126 3.25(2) . . ? C122 H131a 3.13(2) . . ? C122 H131c 2.88(3) . . ? C122 H112' 3.62(2) . '1 645' ? C122 H114' 4.02(2) . '2 665' ? C122 H115' 3.07(2) . '2 665' ? C122 H123' 3.93(2) . '1 645' ? C123 C125 2.389(3) . . ? C123 C126 2.768(2) . . ? C123 C111' 4.438(3) . '1 645' ? C123 C112' 4.054(3) . '1 645' ? C123 C114' 3.727(3) . '2 665' ? C123 C115' 3.670(2) . '2 665' ? C123 C121' 4.275(3) . '1 645' ? C123 C122' 3.594(3) . '1 645' ? C123 C123' 3.802(3) . '1 645' ? C123 B1 3.792(2) . '1 645' ? C123 N21 4.245(2) . '1 645' ? C123 H112 3.76(2) . . ? C123 H114 3.23(2) . '2 656' ? C123 H122 2.04(2) . . ? C123 H124 2.05(3) . . ? C123 H125 3.20(2) . . ? C123 H126 3.722(17) . . ? C123 H112' 3.93(2) . '1 645' ? C123 H114' 3.15(2) . '2 665' ? C123 H115' 2.988(18) . '2 665' ? C123 H122' 3.442(16) . '1 645' ? C123 H123' 3.79(2) . '1 645' ? C123 H1a 3.174(15) . '1 645' ? C123 H1b 3.702(17) . '1 645' ? C124 C126 2.409(2) . . ? C124 C114' 3.865(2) . '2 665' ? C124 C115' 3.852(2) . '2 665' ? C124 C131' 4.204(3) . '1 655' ? C124 B1 3.997(2) . '1 645' ? C124 N21 4.392(2) . '1 645' ? C124 C25 4.375(2) . '1 645' ? C124 H113 3.904(18) . '2 656' ? C124 H114 2.76(2) . '2 656' ? C124 H115 3.78(3) . '1 655' ? C124 H122 3.25(3) . . ? C124 H123 2.03(3) . . ? C124 H125 2.00(2) . . ? C124 H126 3.282(16) . . ? C124 H114' 3.37(2) . '2 665' ? C124 H115' 3.28(2) . '2 665' ? C124 H131'a 3.31(2) . '1 655' ? C124 H25 3.970(17) . '1 645' ? C124 H1a 3.744(16) . '1 645' ? C124 H1b 3.543(15) . '1 645' ? C125 C115' 4.289(3) . '2 665' ? C125 C121' 4.268(3) . '1 655' ? C125 C125' 3.786(3) . '1 655' ? C125 C126' 3.501(3) . '1 655' ? C125 C131' 4.041(3) . '1 655' ? C125 H113 3.499(19) . '2 656' ? C125 H114 3.10(2) . '2 656' ? C125 H115 3.47(2) . '1 655' ? C125 H116 3.86(3) . '1 655' ? C125 H122 3.71(3) . . ? C125 H123 3.23(2) . . ? C125 H124 1.981(17) . . ? C125 H126 2.067(17) . . ? C125 H115' 3.62(2) . '2 665' ? C125 H125' 3.622(19) . '1 655' ? C125 H126' 3.175(19) . '1 655' ? C125 H131'a 3.27(2) . '1 655' ? C125 H131'c 3.984(17) . '1 655' ? C125 H24 3.63(3) . '2 666' ? C126 C131 4.149(3) . . ? C126 C125' 3.782(3) . '1 655' ? C126 C126' 3.800(3) . '1 655' ? C126 N12 3.7303(18) . . ? C126 C13 3.867(2) . . ? C126 N22 3.7673(18) . . ? C126 C23 3.899(2) . . ? C126 H112 3.55(2) . . ? C126 H113 3.384(18) . '2 656' ? C126 H114 3.822(19) . '2 656' ? C126 H122 3.24(2) . . ? C126 H123 3.68(2) . . ? C126 H124 3.223(18) . . ? C126 H125 1.99(3) . . ? C126 H115' 3.67(2) . '2 665' ? C126 H125' 3.26(2) . '1 655' ? C126 H126' 3.36(2) . '1 655' ? C126 H13 3.667(16) . . ? C126 H23 3.729(16) . . ? C126 H24 3.99(3) . '2 666' ? C131 P1' 4.3424(17) . . ? C131 C113' 4.173(3) . '2 565' ? C131 C114' 4.374(3) . '2 565' ? C131 C131' 3.814(2) . . ? C131 C14 4.147(2) . '2 665' ? C131 C15 4.161(3) . '1 545' ? C131 B1 4.323(3) . '1 545' ? C131 H112 3.603(19) . . ? C131 H116 3.79(2) . . ? C131 H122 2.674(19) . . ? C131 H113' 3.84(3) . '2 565' ? C131 H131'a 3.466(16) . . ? C131 H131'b 3.445(17) . . ? C131 H14 3.57(2) . '2 665' ? C131 H15 3.28(2) . '1 545' ? C131 H1b 3.28(2) . '1 545' ? P1' C112' 2.8530(14) . . ? P1' C113' 4.1349(16) . . ? P1' C114' 4.6268(17) . . ? P1' C115' 4.0827(17) . . ? P1' C116' 2.7712(16) . . ? P1' C122' 2.7846(16) . . ? P1' C123' 4.0973(17) . . ? P1' C124' 4.6332(16) . . ? P1' C125' 4.1383(17) . . ? P1' C126' 2.8452(17) . . ? P1' N11 4.1769(16) . . ? P1' N12 3.6156(15) . . ? P1' C13 4.6430(18) . . ? P1' B1 3.959(2) . . ? P1' N21 4.1690(17) . . ? P1' N22 3.6032(16) . . ? P1' C23 4.647(2) . . ? P1' H116 3.24(2) . . ? P1' H123 4.07(2) . '1 465' ? P1' H131b 3.926(19) . . ? P1' H112' 2.962(16) . . ? P1' H116' 2.834(19) . . ? P1' H122' 2.89(2) . . ? P1' H126' 2.97(2) . . ? P1' H131'a 2.36(2) . . ? P1' H131'b 2.34(2) . . ? P1' H131'c 2.36(2) . . ? P1' H14 4.14(2) . '2 665' ? P1' H1a 3.11(2) . . ? C111' C113' 2.416(2) . . ? C111' C114' 2.797(2) . . ? C111' C114' 4.430(3) . '2 575' ? C111' C115' 2.420(2) . . ? C111' C121' 2.8885(19) . . ? C111' C122' 3.739(2) . . ? C111' C126' 3.623(2) . . ? C111' C131' 2.808(2) . . ? C111' C131' 3.990(3) . '2 565' ? C111' N11 4.138(2) . . ? C111' N12 3.948(2) . . ? C111' B1 3.946(3) . . ? C111' H123 3.63(2) . '1 465' ? C111' H112' 2.032(18) . . ? C111' H113' 3.281(18) . . ? C111' H114' 3.90(3) . '2 575' ? C111' H114' 3.71(2) . . ? C111' H115' 3.28(2) . . ? C111' H116' 2.040(19) . . ? C111' H122' 3.837(18) . . ? C111' H126' 3.63(2) . . ? C111' H131'a 3.67(2) . . ? C111' H131'b 3.01(2) . . ? C111' H131'b 3.46(2) . '2 565' ? C111' H131'c 2.85(2) . . ? C111' H131'c 3.64(2) . '2 565' ? C111' H14 3.98(3) . '1 455' ? C111' H1a 2.92(2) . . ? C112' C114' 2.411(2) . . ? C112' C114' 4.319(3) . '2 575' ? C112' C115' 4.420(3) . '2 575' ? C112' C115' 2.778(2) . . ? C112' C116' 2.404(2) . . ? C112' C121' 3.143(2) . . ? C112' C122' 3.953(2) . . ? C112' C126' 3.476(2) . . ? C112' C131' 4.121(3) . '2 565' ? C112' C131' 3.593(2) . . ? C112' C14 3.763(3) . '1 455' ? C112' C15 3.870(3) . '1 455' ? C112' H122 3.36(2) . '1 465' ? C112' H123 3.44(3) . '1 465' ? C112' H113' 2.042(18) . . ? C112' H114' 3.23(2) . . ? C112' H114' 3.94(3) . '2 575' ? C112' H115' 3.74(2) . . ? C112' H116' 3.264(18) . . ? C112' H126' 3.47(2) . . ? C112' H131'b 3.39(2) . '2 565' ? C112' H131'b 3.956(17) . . ? C112' H131'c 3.271(18) . . ? C112' H14 3.27(3) . '1 455' ? C112' H15 3.55(2) . '1 455' ? C112' H1a 3.63(2) . . ? C113' C114' 3.856(3) . '2 575' ? C113' C115' 2.394(3) . . ? C113' C115' 3.721(3) . '2 575' ? C113' C116' 2.767(2) . . ? C113' C116' 4.403(3) . '2 575' ? C113' C131' 3.973(3) . '2 565' ? C113' C14 4.200(3) . '1 455' ? C113' C15 4.161(2) . '2 575' ? C113' C15 4.241(3) . '1 455' ? C113' B1 4.429(2) . '2 575' ? C113' H122 3.79(2) . '1 465' ? C113' H131b 3.54(2) . '2 565' ? C113' H112' 2.026(19) . . ? C113' H114' 2.00(2) . . ? C113' H114' 3.78(3) . '2 575' ? C113' H115' 3.270(19) . . ? C113' H115' 3.60(2) . '2 575' ? C113' H116' 3.718(17) . . ? C113' H131'a 3.88(2) . '2 565' ? C113' H131'b 3.34(2) . '2 565' ? C113' H14 3.59(3) . '1 455' ? C113' H15 3.715(16) . '2 575' ? C113' H15 3.75(2) . '1 455' ? C113' H1b 3.988(16) . '2 575' ? C114' C114' 3.481(3) . '2 575' ? C114' C115' 3.605(3) . '2 575' ? C114' C116' 2.405(2) . . ? C114' C116' 4.073(3) . '2 575' ? C114' C131' 3.672(3) . '2 565' ? C114' N11 4.3890(19) . '2 575' ? C114' B1 3.887(2) . '2 575' ? C114' H123 3.53(2) . '2 665' ? C114' H124 3.856(18) . '2 665' ? C114' H131b 3.56(3) . '2 565' ? C114' H112' 3.25(2) . . ? C114' H113' 2.04(2) . . ? C114' H114' 3.58(3) . '2 575' ? C114' H115' 3.85(2) . '2 575' ? C114' H115' 2.053(18) . . ? C114' H116' 3.262(16) . . ? C114' H131'a 3.34(2) . '2 565' ? C114' H131'b 3.35(2) . '2 565' ? C114' H131'c 3.699(19) . '2 565' ? C114' H1a 3.524(15) . '2 575' ? C114' H1b 3.489(16) . '2 575' ? C115' C115' 4.208(3) . '2 575' ? C115' C131' 3.518(3) . '2 565' ? C115' C13 4.117(2) . '2 665' ? C115' H123 3.73(2) . '2 665' ? C115' H112' 3.71(2) . . ? C115' H113' 3.26(2) . . ? C115' H113' 3.73(3) . '2 575' ? C115' H114' 2.017(18) . . ? C115' H114' 3.52(3) . '2 575' ? C115' H116' 2.038(16) . . ? C115' H131'a 3.32(2) . '2 565' ? C115' H131'b 3.41(2) . '2 565' ? C115' H131'c 3.18(2) . '2 565' ? C115' H13 3.349(15) . '2 665' ? C115' H1a 3.942(18) . . ? C116' C121' 4.178(2) . . ? C116' C131' 3.698(3) . '2 565' ? C116' C131' 3.558(3) . . ? C116' N11 3.636(2) . . ? C116' N12 3.458(2) . . ? C116' C13 3.979(2) . . ? C116' C13 3.830(2) . '2 665' ? C116' C14 4.034(2) . '2 665' ? C116' C15 4.225(3) . . ? C116' B1 3.903(3) . . ? C116' H112' 3.249(19) . . ? C116' H113' 3.729(19) . . ? C116' H114' 3.66(3) . '2 575' ? C116' H114' 3.236(19) . . ? C116' H115' 2.044(19) . . ? C116' H131'a 3.86(2) . '2 565' ? C116' H131'b 3.39(2) . . ? C116' H131'b 3.48(2) . '2 565' ? C116' H131'c 3.16(2) . '2 565' ? C116' H131'c 3.73(2) . . ? C116' H13 3.168(16) . '2 665' ? C116' H14 3.62(2) . '2 665' ? C116' H1a 3.10(2) . . ? C121' C123' 2.419(2) . . ? C121' C124' 2.798(2) . . ? C121' C125' 2.424(2) . . ? C121' C131' 2.873(2) . . ? C121' N22 3.959(2) . . ? C121' H116 3.119(18) . . ? C121' H122 3.870(18) . '1 465' ? C121' H123 3.60(3) . '1 465' ? C121' H125 3.57(2) . '1 455' ? C121' H112' 2.705(17) . . ? C121' H122' 2.08(2) . . ? C121' H123' 3.23(3) . . ? C121' H124' 3.74(2) . . ? C121' H125' 3.30(2) . . ? C121' H126' 2.07(2) . . ? C121' H131'a 3.04(2) . . ? C121' H131'b 3.714(19) . . ? C121' H131'c 3.00(2) . . ? C121' H1a 3.68(2) . . ? C122' C124' 2.407(2) . . ? C122' C125' 2.770(3) . . ? C122' C126' 2.398(3) . . ? C122' C131' 4.150(3) . . ? C122' B1 4.144(3) . . ? C122' N21 3.728(2) . . ? C122' N22 3.378(2) . . ? C122' C23 3.827(2) . . ? C122' C24 4.401(3) . . ? C122' C25 4.315(3) . . ? C122' H116 3.29(2) . . ? C122' H122 3.630(17) . '1 465' ? C122' H123 3.03(2) . '1 465' ? C122' H112' 3.53(2) . . ? C122' H123' 2.00(2) . . ? C122' H124' 3.27(2) . . ? C122' H125' 3.77(3) . . ? C122' H126' 3.29(2) . . ? C122' H1a 3.425(19) . . ? C123' C125' 2.394(3) . . ? C123' C126' 2.774(3) . . ? C123' C23 3.782(2) . '2 566' ? C123' C24 4.070(3) . '2 566' ? C123' H112 3.409(17) . '1 465' ? C123' H114 3.95(3) . '2 566' ? C123' H122 3.572(18) . '1 465' ? C123' H123 3.55(2) . '1 465' ? C123' H122' 2.052(18) . . ? C123' H124' 2.04(2) . . ? C123' H125' 3.32(3) . . ? C123' H126' 3.75(2) . . ? C123' H23 3.110(17) . '2 566' ? C123' H24 3.67(2) . '2 566' ? C124' C126' 2.407(2) . . ? C124' N21 4.164(2) . '1 455' ? C124' C23 3.658(2) . '2 566' ? C124' C24 3.883(3) . '1 455' ? C124' C24 3.704(2) . '2 566' ? C124' C25 3.648(3) . '1 455' ? C124' H112 3.23(2) . '1 465' ? C124' H113 3.647(18) . '1 465' ? C124' H122 3.77(2) . '1 465' ? C124' H125 3.99(2) . '1 455' ? C124' H122' 3.29(2) . . ? C124' H123' 1.99(3) . . ? C124' H125' 2.10(3) . . ? C124' H126' 3.28(2) . . ? C124' H23 3.115(18) . '2 566' ? C124' H24 4.03(2) . '1 455' ? C124' H24 3.14(2) . '2 566' ? C124' H25 3.616(19) . '1 455' ? C125' N11 3.695(2) . '1 455' ? C125' N12 4.059(3) . '1 455' ? C125' C13 4.345(3) . '1 455' ? C125' C14 4.243(3) . '1 455' ? C125' C15 3.821(2) . '1 455' ? C125' B1 4.063(3) . '1 455' ? C125' N21 3.533(2) . '1 455' ? C125' N22 3.902(2) . '1 455' ? C125' C23 4.033(3) . '1 455' ? C125' C24 3.813(2) . '1 455' ? C125' C24 4.212(2) . '2 566' ? C125' C25 3.481(2) . '1 455' ? C125' H122 4.00(2) . '1 465' ? C125' H125 3.20(2) . '1 455' ? C125' H126 3.16(2) . '1 455' ? C125' H112' 3.624(19) . . ? C125' H122' 3.76(2) . . ? C125' H123' 3.20(3) . . ? C125' H124' 2.01(2) . . ? C125' H126' 2.052(18) . . ? C125' H15 3.988(17) . '1 455' ? C125' H24 3.40(2) . '2 566' ? C125' H25 3.650(17) . '1 455' ? C126' C131' 3.111(2) . . ? C126' N11 3.929(2) . '1 455' ? C126' N12 4.133(2) . '1 455' ? C126' C13 3.968(3) . '1 455' ? C126' C14 3.690(3) . '1 455' ? C126' C15 3.660(2) . '1 455' ? C126' H116 3.796(19) . . ? C126' H125 2.93(2) . '1 455' ? C126' H126 3.44(2) . '1 455' ? C126' H112' 2.770(19) . . ? C126' H122' 3.30(2) . . ? C126' H123' 3.67(3) . . ? C126' H124' 3.25(2) . . ? C126' H125' 2.05(2) . . ? C126' H131'a 3.145(17) . . ? C126' H131'c 2.864(17) . . ? C126' H14 3.92(2) . '1 455' ? C126' H15 3.876(17) . '1 455' ? C131' C131' 4.234(2) . '2 565' ? C131' C14 4.294(2) . '1 455' ? C131' H116 3.63(2) . . ? C131' H124 4.025(19) . '1 455' ? C131' H125 3.81(2) . '1 455' ? C131' H131b 3.093(17) . . ? C131' H112' 3.629(17) . . ? C131' H115' 3.77(3) . '2 565' ? C131' H116' 3.62(2) . . ? C131' H126' 2.667(16) . . ? C131' H131'b 3.776(18) . '2 565' ? C131' H131'c 3.817(17) . '2 565' ? C131' H14 3.55(2) . '2 665' ? C131' H14 3.91(2) . '1 455' ? N11 C13 2.165(2) . . ? N11 C14 2.215(2) . . ? N11 N21 2.5314(17) . . ? N11 N22 3.0504(17) . . ? N11 C23 4.246(2) . . ? N11 C25 3.670(2) . . ? N11 H126 3.868(16) . . ? N11 H131c 3.89(3) . '1 565' ? N11 H113' 3.85(2) . '2 575' ? N11 H114' 3.669(18) . '2 575' ? N11 H116' 3.08(2) . . ? N11 H125' 3.08(2) . '1 655' ? N11 H126' 3.532(18) . '1 655' ? N11 H13 3.096(17) . . ? N11 H14 3.14(2) . . ? N11 H15 2.01(2) . . ? N11 H25 3.90(2) . . ? N11 H1a 2.169(17) . . ? N11 H1b 2.182(17) . . ? N12 C13 4.145(2) . '2 665' ? N12 C14 2.249(2) . . ? N12 C14 4.405(3) . '2 665' ? N12 C15 2.216(2) . . ? N12 B1 2.541(2) . . ? N12 N21 3.0378(17) . . ? N12 N22 2.9237(16) . . ? N12 C23 4.140(2) . . ? N12 C25 4.279(2) . . ? N12 H126 3.147(17) . . ? N12 H116' 2.68(2) . . ? N12 H125' 3.33(2) . '1 655' ? N12 H126' 3.50(2) . '1 655' ? N12 H13 2.021(16) . . ? N12 H13 3.665(18) . '2 665' ? N12 H14 3.18(2) . . ? N12 H15 3.11(2) . . ? N12 H1a 2.808(15) . . ? N12 H1b 3.426(18) . . ? C13 C13 3.381(3) . '2 665' ? C13 C14 3.870(3) . '2 665' ? C13 C15 2.191(3) . . ? C13 B1 3.652(2) . . ? C13 N21 4.247(2) . . ? C13 N22 4.1552(19) . . ? C13 H126 3.548(17) . . ? C13 H115' 3.658(17) . '2 665' ? C13 H116' 3.145(17) . '2 665' ? C13 H116' 3.07(2) . . ? C13 H125' 3.85(2) . '1 655' ? C13 H126' 3.14(2) . '1 655' ? C13 H131'c 3.70(2) . '1 655' ? C13 H13 3.00(2) . '2 665' ? C13 H14 2.14(2) . . ? C13 H14 3.97(3) . '2 665' ? C13 H15 3.13(2) . . ? C13 H1a 3.986(15) . . ? C14 B1 3.746(2) . . ? C14 H131a 3.32(2) . '2 665' ? C14 H112' 3.27(3) . '1 655' ? C14 H116' 3.65(2) . . ? C14 H116' 3.392(19) . '2 665' ? C14 H125' 4.00(2) . '1 655' ? C14 H126' 2.962(19) . '1 655' ? C14 H131'b 3.602(19) . '2 665' ? C14 H131'c 3.347(17) . '1 655' ? C14 H13 3.29(2) . '2 665' ? C14 H13 2.16(2) . . ? C14 H15 2.12(2) . . ? C15 B1 2.637(2) . . ? C15 N21 3.689(2) . . ? C15 N22 4.311(2) . . ? C15 H131a 3.66(2) . '2 665' ? C15 H131c 3.44(3) . '1 565' ? C15 H112' 3.18(2) . '1 655' ? C15 H113' 3.326(18) . '2 575' ? C15 H113' 3.91(3) . '1 655' ? C15 H114' 3.958(19) . '2 575' ? C15 H116' 3.62(2) . . ? C15 H125' 3.53(2) . '1 655' ? C15 H126' 3.227(17) . '1 655' ? C15 H13 3.16(2) . . ? C15 H14 2.09(2) . . ? C15 H1a 3.289(18) . . ? C15 H1b 2.780(15) . . ? B1 N22 2.543(2) . . ? B1 C23 3.650(2) . . ? B1 C24 3.740(2) . . ? B1 C25 2.624(3) . . ? B1 H123 3.10(2) . '1 465' ? B1 H124 3.517(17) . '1 465' ? B1 H131b 3.96(2) . '1 565' ? B1 H131c 3.71(3) . '1 565' ? B1 H113' 4.06(2) . '2 575' ? B1 H114' 3.015(19) . '2 575' ? B1 H116' 3.68(2) . . ? B1 H122' 3.33(2) . . ? B1 H125' 3.35(2) . '1 655' ? B1 H15 2.862(19) . . ? B1 H25 2.77(2) . . ? N21 C23 2.169(2) . . ? N21 C24 2.218(2) . . ? N21 H123 3.62(2) . '1 465' ? N21 H124 3.878(16) . '1 465' ? N21 H126 3.675(16) . . ? N21 H122' 2.75(2) . . ? N21 H124' 3.89(3) . '1 655' ? N21 H125' 2.68(2) . '1 655' ? N21 H15 3.994(18) . . ? N21 H23 3.074(18) . . ? N21 H24 3.17(2) . . ? N21 H25 1.91(2) . . ? N21 H1a 2.180(17) . . ? N21 H1b 2.172(17) . . ? N22 C24 2.249(3) . . ? N22 C25 2.215(3) . . ? N22 H116 3.48(3) . . ? N22 H126 2.878(16) . . ? N22 H122' 2.489(18) . . ? N22 H125' 2.91(2) . '1 655' ? N22 H23 1.996(17) . . ? N22 H24 3.19(3) . . ? N22 H25 3.02(2) . . ? N22 H1a 2.821(15) . . ? N22 H1b 3.425(18) . . ? C23 C25 2.192(3) . . ? C23 H115 3.77(2) . '2 566' ? C23 H116 3.58(3) . . ? C23 H126 3.073(16) . . ? C23 H122' 2.986(18) . . ? C23 H123' 3.55(2) . '2 566' ? C23 H124' 3.337(19) . '2 566' ? C23 H125' 3.14(2) . '1 655' ? C23 H24 2.12(3) . . ? C23 H25 3.06(2) . . ? C23 H1a 4.011(15) . . ? C24 H113 3.87(2) . '1 565' ? C24 H115 2.894(19) . '2 566' ? C24 H125 3.91(2) . '2 666' ? C24 H126 3.960(17) . . ? C24 H122' 3.50(2) . . ? C24 H124' 3.535(18) . '2 566' ? C24 H124' 3.25(3) . '1 655' ? C24 H125' 3.12(2) . '1 655' ? C24 H23 2.14(2) . . ? C24 H25 2.08(2) . . ? C25 H113 3.60(2) . '1 565' ? C25 H114 3.816(18) . '2 566' ? C25 H115 3.29(2) . '2 566' ? C25 H124 3.749(16) . '1 465' ? C25 H122' 3.34(2) . . ? C25 H124' 3.11(2) . '1 655' ? C25 H125' 2.818(18) . '1 655' ? C25 H23 3.14(2) . . ? C25 H24 2.14(2) . . ? C25 H1a 3.312(19) . . ? C25 H1b 2.759(16) . . ? H112 H112 3.62(3) . '2 656' ? H112 H113 2.75(3) . '2 656' ? H112 H113 2.33(3) . . ? H112 H122 2.87(3) . . ? H112 H131c 3.22(3) . . ? H112 H123' 3.26(3) . '1 645' ? H112 H124' 2.95(3) . '1 645' ? H112 H25 3.60(4) . '1 545' ? H113 H113 3.59(3) . '2 656' ? H113 H114 2.34(3) . . ? H113 H124' 2.83(3) . '1 645' ? H113 H24 3.54(4) . '1 545' ? H113 H25 3.04(3) . '1 545' ? H114 H114 3.22(4) . '2 556' ? H114 H115 2.34(3) . . ? H114 H115 3.20(4) . '2 556' ? H114 H123 3.62(3) . '2 656' ? H114 H124 2.79(3) . '2 656' ? H114 H125 3.30(3) . '2 656' ? H114 H123' 3.24(4) . '2 566' ? H114 H25 3.57(3) . '1 545' ? H114 H25 3.56(3) . '2 566' ? H115 H116 2.28(3) . . ? H115 H124 3.38(3) . '1 455' ? H115 H125 2.82(3) . '1 455' ? H115 H123' 3.28(4) . '2 566' ? H115 H24 2.64(3) . '2 566' ? H115 H25 3.40(3) . '2 566' ? H116 H124 3.45(4) . '1 455' ? H116 H125 3.16(4) . '1 455' ? H116 H131b 3.52(3) . . ? H116 H122' 3.33(3) . . ? H116 H131'a 3.08(3) . . ? H116 H23 3.09(4) . . ? H122 H123 2.27(3) . . ? H122 H131a 2.72(3) . . ? H122 H131b 3.57(3) . . ? H122 H131c 2.20(3) . . ? H122 H112' 2.87(3) . '1 645' ? H122 H113' 3.60(3) . '1 645' ? H122 H115' 3.42(3) . '2 665' ? H123 H124 2.41(4) . . ? H123 H112' 3.40(4) . '1 645' ? H123 H114' 2.81(3) . '2 665' ? H123 H115' 3.20(3) . '2 665' ? H123 H122' 2.81(3) . '1 645' ? H123 H1a 2.34(2) . '1 645' ? H123 H1b 3.22(3) . '1 645' ? H124 H125 2.25(2) . . ? H124 H131b 3.56(3) . '1 655' ? H124 H114' 3.29(3) . '2 665' ? H124 H131'a 3.07(3) . '1 655' ? H124 H25 3.23(2) . '1 645' ? H124 H1a 3.52(3) . '1 645' ? H124 H1b 2.90(2) . '1 645' ? H125 H126 2.34(3) . . ? H125 H125' 3.23(2) . '1 655' ? H125 H126' 2.83(3) . '1 655' ? H125 H131'a 3.08(3) . '1 655' ? H125 H24 3.01(3) . '2 666' ? H126 H125' 2.47(3) . '1 655' ? H126 H126' 3.09(3) . '1 655' ? H126 H13 3.58(2) . . ? H126 H23 3.07(2) . . ? H131a H131b 1.58(3) . . ? H131a H131c 1.58(3) . . ? H131a H113' 3.63(4) . '2 565' ? H131a H113' 3.32(3) . '1 645' ? H131a H131'b 3.47(3) . . ? H131a H13 3.55(3) . . ? H131a H14 2.88(3) . '2 665' ? H131a H15 3.61(3) . '2 665' ? H131a H15 3.29(3) . '1 545' ? H131b H131c 1.57(3) . . ? H131b H113' 3.37(3) . '2 565' ? H131b H114' 3.41(4) . '2 565' ? H131b H131'a 2.65(2) . . ? H131b H131'b 2.78(2) . . ? H131b H14 3.47(3) . '2 665' ? H131b H15 3.36(3) . '1 545' ? H131b H1b 2.89(3) . '1 545' ? H131c H112' 3.56(2) . '1 645' ? H131c H15 2.64(3) . '1 545' ? H131c H1b 2.75(3) . '1 545' ? H112' H113' 2.33(3) . . ? H112' H126' 2.83(3) . . ? H112' H131'c 3.20(3) . . ? H112' H14 3.00(4) . '1 455' ? H112' H15 2.86(3) . '1 455' ? H113' H114' 2.31(3) . . ? H113' H115' 3.48(4) . '2 575' ? H113' H14 3.62(4) . '1 455' ? H113' H15 2.86(3) . '2 575' ? H113' H15 3.27(3) . '1 455' ? H114' H115' 2.35(3) . . ? H114' H131'a 3.52(3) . '2 565' ? H114' H1a 2.63(3) . '2 575' ? H114' H1b 2.70(3) . '2 575' ? H115' H116' 2.34(2) . . ? H115' H131'a 3.44(4) . '2 565' ? H115' H131'c 3.36(3) . '2 565' ? H115' H13 2.83(2) . '2 665' ? H116' H131'b 3.31(3) . . ? H116' H131'c 3.40(3) . '2 565' ? H116' H13 2.50(2) . '2 665' ? H116' H13 3.41(2) . . ? H116' H14 3.05(3) . '2 665' ? H116' H1a 3.09(3) . . ? H122' H123' 2.31(3) . . ? H122' H23 3.40(2) . . ? H122' H1a 2.79(2) . . ? H123' H124' 2.32(4) . . ? H123' H23 2.75(3) . '2 566' ? H124' H125' 2.38(3) . . ? H124' H23 2.77(3) . '2 566' ? H124' H24 3.26(3) . '1 455' ? H124' H24 3.12(3) . '2 566' ? H124' H25 3.04(3) . '1 455' ? H125' H126' 2.31(3) . . ? H125' H24 3.51(3) . '2 566' ? H125' H25 3.18(2) . '1 455' ? H125' H1b 3.64(2) . '1 455' ? H126' H131'a 2.71(2) . . ? H126' H131'b 3.57(2) . . ? H126' H131'c 2.19(2) . . ? H126' H13 3.51(3) . '1 455' ? H126' H14 3.19(3) . '1 455' ? H126' H15 3.64(2) . '1 455' ? H131'a H131'b 1.56(3) . . ? H131'a H131'c 1.56(2) . . ? H131'b H131'b 3.52(2) . '2 565' ? H131'b H131'c 3.21(2) . '2 565' ? H131'b H131'c 1.55(2) . . ? H131'b H14 2.65(3) . '2 665' ? H131'c H131'c 3.62(2) . '2 565' ? H131'c H14 2.97(3) . '1 455' ? H13 H13 2.92(2) . '2 665' ? H13 H14 2.63(3) . . ? H13 H14 3.46(4) . '2 665' ? H14 H15 2.55(3) . . ? H15 H1a 3.59(3) . . ? H15 H1b 2.62(2) . . ? H23 H24 2.58(4) . . ? H24 H25 2.61(3) . . ? H25 H1a 3.53(3) . . ? H25 H1b 2.55(2) . . ? H1a H1b 1.91(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_000 636 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 13 _reflns_limit_k_min -12 _reflns_limit_k_max 14 _reflns_limit_l_min -21 _reflns_limit_l_max 22 _reflns_number_observed ? _reflns_d_resolution_high .731 _reflns_d_resolution_low 9.566 _diffrn_reflns_av_sigmaI/netI .022 _diffrn_reflns_theta_min 2.12 _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 .033 _refine_ls_wR_factor_all .042 _refine_ls_goodness_of_fit_all 1.511 _refine_ls_shift/su_mean . #========================================================================== # 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 data_30mcp # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C34 H53 B1 Cu1 N8 P1' _chemical_formula_moiety ? _chemical_formula_weight 679.19 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_21/c _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 12.736(2) _cell_length_b 15.229(2) _cell_length_c 18.834(2) _cell_angle_alpha 90.00000 _cell_angle_beta 105.386(2) _cell_angle_gamma 90(3) _cell_volume 3522.1(8) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.281 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 6140 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu .702 _exptl_crystal_description prism _exptl_crystal_size_max .3 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .15 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .454 _exptl_absorpt_correction_T_max .831 _diffrn_reflns_number 39176 _reflns_number_total 8951 _reflns_Friedel_coverage 0 _reflns_number_gt 6791 _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 .065 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _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 .04 _refine_ls_wR_factor_ref .046 _refine_ls_goodness_of_fit_ref 1.51 _refine_ls_number_reflns 6791 _refine_ls_number_parameters 618 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max .031 _refine_diff_density_min -.709 _refine_diff_density_max .805 _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 Cu ? 0 4 .263 1.266 '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' C ? 0 136 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 212 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 32 .004 .003 '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' 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 .80179(2) .402217(15) .343638(13) .02100(12) Uani ? ? 1.00000 ? ? P .73464(4) .32604(3) .41978(3) .0205(2) Uani ? ? 1.00000 ? ? C111 .79098(16) .36187(13) .51664(11) .0220(9) Uani ? ? 1.00000 ? ? C112 .90656(17) .39942(15) .52942(12) .0259(10) Uani ? ? 1.00000 ? ? C113 .9415(2) .44591(15) .60359(13) .0300(11) Uani ? ? 1.00000 ? ? C114 .9377(2) .38418(18) .66636(13) .0352(12) Uani ? ? 1.00000 ? ? C115 .8258(2) .34151(18) .65398(13) .0343(12) Uani ? ? 1.00000 ? ? C116 .7889(2) .29684(15) .57863(12) .0287(11) Uani ? ? 1.00000 ? ? C121 .58511(16) .34172(13) .39950(11) .0219(9) Uani ? ? 1.00000 ? ? C122 .55528(18) .43841(14) .40512(14) .0278(10) Uani ? ? 1.00000 ? ? C123 .43255(19) .45374(16) .38078(14) .0324(12) Uani ? ? 1.00000 ? ? C124 .3736(2) .39541(16) .42297(15) .0346(12) Uani ? ? 1.00000 ? ? C125 .40123(19) .29920(16) .41584(15) .0350(12) Uani ? ? 1.00000 ? ? C126 .52418(19) .28385(15) .44219(13) .0298(11) Uani ? ? 1.00000 ? ? C131 .75030(18) .20562(13) .41609(12) .0246(10) Uani ? ? 1.00000 ? ? C132 .6889(2) .17294(15) .33867(12) .0311(11) Uani ? ? 1.00000 ? ? C133 .7043(2) .07459(16) .32970(15) .0396(13) Uani ? ? 1.00000 ? ? C134 .8235(3) .04909(18) .34884(16) .0470(15) Uani ? ? 1.00000 ? ? C135 .8835(2) .07987(15) .42560(15) .0396(13) Uani ? ? 1.00000 ? ? C136 .8699(2) .17877(14) .43344(15) .0323(11) Uani ? ? 1.00000 ? ? B .75324(19) .47721(15) .18690(13) .0225(10) Uani ? ? 1.00000 ? ? N11 .76027(13) .55242(10) .24341(9) .0216(8) Uani ? ? 1.00000 ? ? N12 .77092(13) .53115(11) .31567(9) .0222(8) Uani ? ? 1.00000 ? ? C13 .76722(16) .60708(12) .35126(11) .0226(9) Uani ? ? 1.00000 ? ? C14 .75389(19) .67694(14) .30146(13) .0295(11) Uani ? ? 1.00000 ? ? C15 .74997(18) .63978(14) .23431(13) .0292(11) Uani ? ? 1.00000 ? ? C16 .7790(2) .60786(16) .43214(13) .0286(11) Uani ? ? 1.00000 ? ? N21 .85882(13) .42352(11) .20592(9) .0215(8) Uani ? ? 1.00000 ? ? N22 .89540(13) .38563(10) .27420(9) .0213(8) Uani ? ? 1.00000 ? ? C23 .99048(16) .34695(13) .27599(12) .0243(9) Uani ? ? 1.00000 ? ? C24 1.01466(19) .35933(15) .20856(13) .0301(11) Uani ? ? 1.00000 ? ? C25 .93104(18) .40778(14) .16622(12) .0266(10) Uani ? ? 1.00000 ? ? C26 1.0558(2) .29935(17) .34248(14) .0315(12) Uani ? ? 1.00000 ? ? N31 .65685(14) .41903(11) .19227(9) .0232(8) Uani ? ? 1.00000 ? ? N32 .64956(14) .33308(11) .16944(10) .0261(8) Uani ? ? 1.00000 ? ? C33 .55066(17) .30608(14) .17168(11) .0262(10) Uani ? ? 1.00000 ? ? C34 .49267(17) .37440(15) .19473(12) .0276(10) Uani ? ? 1.00000 ? ? C35 .56236(17) .44433(15) .20696(12) .0262(10) Uani ? ? 1.00000 ? ? C36 .5149(2) .21381(17) .15113(16) .0370(13) Uani ? ? 1.00000 ? ? N41 .73210(14) .51553(11) .10953(9) .0260(8) Uani ? ? 1.00000 ? ? N42 .80473(15) .57226(12) .09107(10) .0292(9) Uani ? ? 1.00000 ? ? C43 .75775(19) .59623(14) .02185(12) .0293(10) Uani ? ? 1.00000 ? ? C44 .6567(2) .5569(2) -.00438(14) .0418(13) Uani ? ? 1.00000 ? ? C45 .6435(2) .50578(18) .05258(13) .0367(12) Uani ? ? 1.00000 ? ? C46 .8152(3) .65683(18) -.01819(15) .0411(13) Uani ? ? 1.00000 ? ? H111 .7446(18) .4099(14) .5206(12) .024(6) Uiso ? ? 1.00000 ? ? H112a .9589(18) .3522(15) .5290(12) .026(6) Uiso ? ? 1.00000 ? ? H112b .9088(17) .4382(15) .4907(12) .026(6) Uiso ? ? 1.00000 ? ? H113a 1.015(2) .4721(16) .6117(13) .038(7) Uiso ? ? 1.00000 ? ? H113b .8937(18) .4931(16) .6020(12) .028(6) Uiso ? ? 1.00000 ? ? H114a .991(2) .3410(16) .6718(13) .036(7) Uiso ? ? 1.00000 ? ? H114b .956(2) .4142(18) .7160(16) .056(8) Uiso ? ? 1.00000 ? ? H115a .8237(17) .2977(15) .6904(12) .026(6) Uiso ? ? 1.00000 ? ? H115b .770(2) .3857(15) .6565(12) .029(6) Uiso ? ? 1.00000 ? ? H116a .715(2) .2745(15) .5733(12) .034(6) Uiso ? ? 1.00000 ? ? H116b .8370(19) .2482(15) .5774(12) .031(6) Uiso ? ? 1.00000 ? ? H121 .5632(17) .3279(14) .3531(12) .023(6) Uiso ? ? 1.00000 ? ? H122a .5396(18) .2216(16) .4365(12) .031(6) Uiso ? ? 1.00000 ? ? H122b .551(2) .3003(16) .4951(14) .041(7) Uiso ? ? 1.00000 ? ? H123a .376(2) .2807(16) .3666(14) .035(7) Uiso ? ? 1.00000 ? ? H123b .363(2) .2573(17) .4440(14) .045(7) Uiso ? ? 1.00000 ? ? H124a .301(2) .4045(16) .4052(14) .041(7) Uiso ? ? 1.00000 ? ? H124b .395(2) .4104(15) .4756(14) .036(7) Uiso ? ? 1.00000 ? ? H125a .4037(18) .4432(15) .3301(13) .025(6) Uiso ? ? 1.00000 ? ? H125b .4142(18) .5167(16) .3895(12) .033(6) Uiso ? ? 1.00000 ? ? H126a .5789(18) .4550(15) .4570(14) .033(6) Uiso ? ? 1.00000 ? ? H126b .5855(19) .4718(16) .3761(13) .035(7) Uiso ? ? 1.00000 ? ? H131 .7203(17) .1835(15) .4500(12) .028(6) Uiso ? ? 1.00000 ? ? H132a .6104(18) .1881(14) .3265(11) .022(6) Uiso ? ? 1.00000 ? ? H132b .7162(18) .2038(16) .3029(13) .034(6) Uiso ? ? 1.00000 ? ? H133a .6647(18) .0576(16) .2792(13) .032(6) Uiso ? ? 1.00000 ? ? H133b .6687(18) .0420(15) .3624(12) .029(6) Uiso ? ? 1.00000 ? ? H134a .861(2) .0768(19) .3142(15) .051(8) Uiso ? ? 1.00000 ? ? H134b .833(2) -.009(2) .3440(15) .056(8) Uiso ? ? 1.00000 ? ? H135a .964(2) .0658(16) .4366(13) .037(7) Uiso ? ? 1.00000 ? ? H135b .8515(18) .0500(15) .4629(13) .030(6) Uiso ? ? 1.00000 ? ? H136a .906(2) .2109(17) .3988(14) .044(7) Uiso ? ? 1.00000 ? ? H136b .913(2) .2011(16) .4819(14) .040(7) Uiso ? ? 1.00000 ? ? H14 .755(2) .7352(17) .3116(14) .044(7) Uiso ? ? 1.00000 ? ? H15 .740(2) .6646(16) .1879(14) .037(7) Uiso ? ? 1.00000 ? ? H16a .725(2) .642(2) .4437(15) .056(8) Uiso ? ? 1.00000 ? ? H16b .766(2) .553(2) .4517(16) .064(9) Uiso ? ? 1.00000 ? ? H16c .844(2) .6250(18) .4558(15) .046(8) Uiso ? ? 1.00000 ? ? H24 1.077(2) .3393(17) .1990(13) .043(7) Uiso ? ? 1.00000 ? ? H25 .9200(18) .4291(16) .1181(13) .031(6) Uiso ? ? 1.00000 ? ? H26a 1.045(2) .236(2) .3377(15) .052(8) Uiso ? ? 1.00000 ? ? H26b 1.130(2) .3142(16) .3545(13) .040(7) Uiso ? ? 1.00000 ? ? H26c 1.035(2) .3139(17) .3849(15) .044(7) Uiso ? ? 1.00000 ? ? H34 .422(2) .3721(17) .2016(14) .045(7) Uiso ? ? 1.00000 ? ? H35 .554(2) .5045(17) .2228(14) .045(7) Uiso ? ? 1.00000 ? ? H36a .463(2) .2138(17) .1052(15) .047(8) Uiso ? ? 1.00000 ? ? H36b .574(3) .178(2) .1512(16) .064(9) Uiso ? ? 1.00000 ? ? H36c .481(2) .1897(17) .1869(14) .046(7) Uiso ? ? 1.00000 ? ? H44 .607(2) .5620(17) -.0489(15) .044(7) Uiso ? ? 1.00000 ? ? H45 .584(2) .4732(17) .0557(14) .046(8) Uiso ? ? 1.00000 ? ? H46a .761(3) .683(2) -.0550(19) .082(11) Uiso ? ? 1.00000 ? ? H46b .865(2) .693(2) .0144(17) .063(9) Uiso ? ? 1.00000 ? ? H46c .863(3) .625(2) -.0435(18) .075(10) 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 .02572(14) .01690(13) .02259(13) -.00022(10) .01028(10) .00177(10) P .0252(3) .0156(2) .0230(3) -.0001(2) .0103(2) .0008(2) C111 .0231(10) .0187(10) .0252(10) .0001(8) .0081(8) .0006(8) C112 .0246(11) .0238(11) .0305(11) -.0015(9) .0097(9) .0024(9) C113 .0263(12) .0276(12) .0347(13) -.0041(10) .0059(10) -.0050(9) C114 .0305(12) .0442(15) .0289(13) -.0001(11) .0044(10) -.0019(10) C115 .0342(13) .0435(15) .0261(12) -.0026(11) .0097(10) .0025(10) C116 .0310(12) .0305(12) .0249(11) -.0052(10) .0079(9) .0041(9) C121 .0258(11) .0202(10) .0209(10) -.0007(8) .0082(8) -.0027(8) C122 .0284(12) .0211(11) .0359(13) -.0001(9) .0122(10) .0001(9) C123 .0280(12) .0286(13) .0416(14) .0048(9) .0110(11) -.0003(10) C124 .0254(12) .0336(13) .0477(15) -.0010(10) .0149(11) -.0076(11) C125 .0299(12) .0292(12) .0491(16) -.0077(10) .0161(11) -.0058(11) C126 .0303(12) .0245(12) .0375(13) -.0044(9) .0140(10) .0005(10) C131 .0329(12) .0163(10) .0286(11) -.0020(8) .0152(10) .0016(8) C132 .0438(14) .0218(11) .0289(12) .0004(10) .0121(11) -.0025(9) C133 .0593(17) .0223(12) .0367(14) -.0013(11) .0119(13) -.0079(10) C134 .071(2) .0231(13) .0541(17) .0100(12) .0290(15) -.0044(12) C135 .0448(15) .0214(12) .0552(17) .0093(10) .0179(13) .0042(11) C136 .0338(13) .0190(11) .0477(15) .0039(9) .0173(11) .0015(10) B .0249(12) .0197(11) .0236(12) -.0006(9) .0080(10) .0009(9) N11 .0246(9) .0175(8) .0236(9) .0016(7) .0081(7) .0028(7) N12 .0263(9) .0189(9) .0232(9) .0001(7) .0097(7) .0016(7) C13 .0229(10) .0172(10) .0300(11) -.0006(8) .0113(8) -.0022(8) C14 .0384(13) .0170(11) .0386(13) .0028(9) .0198(10) -.0001(9) C15 .0351(12) .0195(11) .0369(13) .0058(9) .0165(10) .0094(9) C16 .0330(13) .0222(12) .0332(12) -.0001(10) .0136(10) -.0047(9) N21 .0243(9) .0196(9) .0220(9) -.0011(7) .0087(7) .0014(6) N22 .0225(8) .0191(9) .0229(9) -.0001(6) .0074(7) .0027(6) C23 .0240(10) .0179(10) .0327(11) -.0020(8) .0103(9) .0006(8) C24 .0298(12) .0265(11) .0400(13) .0032(9) .0196(10) .0031(10) C25 .0334(12) .0245(11) .0268(11) -.0006(9) .0165(9) .0012(9) C26 .0263(12) .0295(13) .0392(14) .0032(10) .0097(10) .0094(10) N31 .0237(9) .0225(9) .0243(9) -.0003(7) .0079(7) -.0009(7) N32 .0283(9) .0223(9) .0297(9) -.0021(7) .0111(8) -.0042(7) C33 .0265(11) .0289(11) .0237(11) -.0038(9) .0076(9) -.0016(8) C34 .0206(10) .0379(13) .0248(11) -.0015(9) .0069(9) -.0015(9) C35 .0257(11) .0280(12) .0263(11) .0034(9) .0095(9) .0005(9) C36 .0347(14) .0363(14) .0435(15) -.0112(11) .0163(12) -.0087(11) N41 .0281(9) .0263(10) .0250(9) .0004(7) .0094(8) .0043(7) N42 .0381(11) .0242(9) .0270(10) -.0032(8) .0117(8) .0047(7) C43 .0413(13) .0247(11) .0246(11) .0088(10) .0135(10) .0039(9) C44 .0403(14) .0598(18) .0228(12) .0080(12) .0041(11) .0097(11) C45 .0289(13) .0529(16) .0274(12) -.0043(11) .0059(10) .0026(10) C46 .065(2) .0288(13) .0317(14) .0004(13) .0174(14) .0083(11) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Cu P . . 2.1874(6) ? Cu N12 . . 2.0440(16) ? Cu N22 . . 2.006(2) ? P C111 . . 1.856(2) ? P C121 . . 1.856(2) ? P C131 . . 1.848(2) ? C111 C112 . . 1.537(3) ? C111 C116 . . 1.537(3) ? C111 H111 . . .96(2) ? C112 C113 . . 1.523(3) ? C112 H112a . . .98(2) ? C112 H112b . . .94(2) ? C113 C114 . . 1.521(4) ? C113 H113a . . .99(3) ? C113 H113b . . .94(2) ? C114 C115 . . 1.528(4) ? C114 H114a . . .93(3) ? C114 H114b . . 1.01(3) ? C115 C116 . . 1.531(3) ? C115 H115a . . .96(2) ? C115 H115b . . .99(2) ? C116 H116a . . .98(2) ? C116 H116b . . .97(2) ? C121 C122 . . 1.531(3) ? C121 C126 . . 1.535(3) ? C121 H121 . . .87(2) ? C122 C123 . . 1.526(3) ? C122 H126a . . .98(2) ? C122 H126b . . .90(3) ? C123 C124 . . 1.517(4) ? C123 H125a . . .94(2) ? C123 H125b . . 1.01(3) ? C124 C125 . . 1.521(3) ? C124 H124a . . .91(3) ? C124 H124b . . .98(3) ? C125 C126 . . 1.530(3) ? C125 H123a . . .94(2) ? C125 H123b . . 1.03(3) ? C126 H122a . . .98(2) ? C126 H122b . . 1.00(3) ? C131 C132 . . 1.543(3) ? C131 C136 . . 1.527(3) ? C131 H131 . . .89(3) ? C132 C133 . . 1.526(3) ? C132 H132a . . .99(2) ? C132 H132b . . .96(3) ? C133 C134 . . 1.515(4) ? C133 H133a . . .99(2) ? C133 H133b . . .99(3) ? C134 C135 . . 1.519(4) ? C134 H134a . . 1.00(3) ? C134 H134b . . .91(3) ? C135 C136 . . 1.528(3) ? C135 H135a . . 1.01(3) ? C135 H135b . . 1.01(3) ? C136 H136a . . 1.01(3) ? C136 H136b . . .99(2) ? B N11 . . 1.550(3) ? B N21 . . 1.533(3) ? B N31 . . 1.539(3) ? B N41 . . 1.526(3) ? N11 N12 . . 1.370(2) ? N11 C15 . . 1.343(3) ? N12 C13 . . 1.344(3) ? C13 C14 . . 1.398(3) ? C13 C16 . . 1.490(3) ? C14 C15 . . 1.374(3) ? C14 H14 . . .91(3) ? C15 H15 . . .93(3) ? C16 H16a . . .94(3) ? C16 H16b . . .94(3) ? C16 H16c . . .87(3) ? N21 N22 . . 1.373(2) ? N21 C25 . . 1.352(3) ? N22 C23 . . 1.339(3) ? C23 C24 . . 1.397(4) ? C23 C26 . . 1.494(3) ? C24 C25 . . 1.365(3) ? C24 H24 . . .91(3) ? C25 H25 . . .94(2) ? C26 H26a . . .97(3) ? C26 H26b . . .94(3) ? C26 H26c . . .93(3) ? N31 N32 . . 1.373(2) ? N31 C35 . . 1.360(3) ? N32 C33 . . 1.336(3) ? C33 C34 . . 1.409(3) ? C33 C36 . . 1.496(3) ? C34 C35 . . 1.366(3) ? C34 H34 . . .95(3) ? C35 H35 . . .98(3) ? C36 H36a . . .94(2) ? C36 H36b . . .92(3) ? C36 H36c . . .97(3) ? N41 N42 . . 1.376(3) ? N41 C45 . . 1.343(3) ? N42 C43 . . 1.333(3) ? C43 C44 . . 1.387(3) ? C43 C46 . . 1.500(4) ? C44 C45 . . 1.371(4) ? C44 H44 . . .91(2) ? C45 H45 . . .92(3) ? C46 H46a . . .93(3) ? C46 H46b . . .94(3) ? C46 H46c . . .99(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 P Cu N12 . . . 126.6(5) ? P Cu N22 . . . 139.83(11) ? N12 Cu N22 . . . 93.4(6) ? Cu P C111 . . . 111.8(3) ? Cu P C121 . . . 110.8(4) ? Cu P C131 . . . 115.9(6) ? C111 P C121 . . . 105.81(18) ? C111 P C131 . . . 108.1(9) ? C121 P C131 . . . 103.6(2) ? P C111 C112 . . . 111.6(3) ? P C111 C116 . . . 118.5(4) ? P C111 H111 . . . 102.4(14) ? C112 C111 C116 . . . 109.26(17) ? C112 C111 H111 . . . 106.8(13) ? C116 C111 H111 . . . 107.4(15) ? C111 C112 C113 . . . 110.5(3) ? C111 C112 H112a . . . 110.5(13) ? C111 C112 H112b . . . 109.6(12) ? C113 C112 H112a . . . 108.3(13) ? C113 C112 H112b . . . 110.9(14) ? H112a C112 H112b . . . 107(2) ? C112 C113 C114 . . . 111.3(3) ? C112 C113 H113a . . . 111.3(15) ? C112 C113 H113b . . . 107.3(14) ? C114 C113 H113a . . . 110.6(14) ? C114 C113 H113b . . . 110.2(16) ? H113a C113 H113b . . . 106(2) ? C113 C114 C115 . . . 111.4(2) ? C113 C114 H114a . . . 110.5(17) ? C113 C114 H114b . . . 113.2(17) ? C115 C114 H114a . . . 109.8(16) ? C115 C114 H114b . . . 107.9(18) ? H114a C114 H114b . . . 104(2) ? C114 C115 C116 . . . 112.0(4) ? C114 C115 H115a . . . 112.8(12) ? C114 C115 H115b . . . 110.7(14) ? C116 C115 H115a . . . 107.1(14) ? C116 C115 H115b . . . 107.5(14) ? H115a C115 H115b . . . 106(2) ? C111 C116 C115 . . . 110.8(3) ? C111 C116 H116a . . . 110.9(13) ? C111 C116 H116b . . . 109.7(16) ? C115 C116 H116a . . . 107.5(14) ? C115 C116 H116b . . . 108.8(14) ? H116a C116 H116b . . . 109(2) ? P C121 C122 . . . 111.7(3) ? P C121 C126 . . . 116.9(4) ? P C121 H121 . . . 102.3(15) ? C122 C121 C126 . . . 110.3(5) ? C122 C121 H121 . . . 106.5(17) ? C126 C121 H121 . . . 108.4(16) ? C121 C122 C123 . . . 112.3(4) ? C121 C122 H126a . . . 107.6(17) ? C121 C122 H126b . . . 110.2(17) ? C123 C122 H126a . . . 106.3(15) ? C123 C122 H126b . . . 107.4(15) ? H126a C122 H126b . . . 113(2) ? C122 C123 C124 . . . 111.3(5) ? C122 C123 H125a . . . 111.8(15) ? C122 C123 H125b . . . 111.0(13) ? C124 C123 H125a . . . 108.5(15) ? C124 C123 H125b . . . 107.7(15) ? H125a C123 H125b . . . 106(2) ? C123 C124 C125 . . . 111.1(5) ? C123 C124 H124a . . . 108.4(18) ? C123 C124 H124b . . . 110.6(16) ? C125 C124 H124a . . . 110.6(16) ? C125 C124 H124b . . . 107.8(17) ? H124a C124 H124b . . . 108(2) ? C124 C125 C126 . . . 111.1(4) ? C124 C125 H123a . . . 110.4(17) ? C124 C125 H123b . . . 113.6(16) ? C126 C125 H123a . . . 109.1(16) ? C126 C125 H123b . . . 108.6(14) ? H123a C125 H123b . . . 104(2) ? C121 C126 C125 . . . 111.0(5) ? C121 C126 H122a . . . 110.8(16) ? C121 C126 H122b . . . 107.3(16) ? C125 C126 H122a . . . 109.2(13) ? C125 C126 H122b . . . 109.3(15) ? H122a C126 H122b . . . 109(2) ? P C131 C132 . . . 108.8(9) ? P C131 C136 . . . 111.7(3) ? P C131 H131 . . . 106.0(16) ? C132 C131 C136 . . . 110.1(4) ? C132 C131 H131 . . . 110.4(13) ? C136 C131 H131 . . . 109.8(14) ? C131 C132 C133 . . . 111.9(9) ? C131 C132 H132a . . . 111.8(13) ? C131 C132 H132b . . . 108.6(13) ? C133 C132 H132a . . . 110.7(13) ? C133 C132 H132b . . . 108.7(16) ? H132a C132 H132b . . . 104.8(19) ? C132 C133 C134 . . . 112.1(3) ? C132 C133 H133a . . . 108.4(17) ? C132 C133 H133b . . . 109.2(15) ? C134 C133 H133a . . . 112.8(15) ? C134 C133 H133b . . . 108.6(13) ? H133a C133 H133b . . . 105(2) ? C133 C134 C135 . . . 111.5(4) ? C133 C134 H134a . . . 111.2(16) ? C133 C134 H134b . . . 112.6(18) ? C135 C134 H134a . . . 106.5(15) ? C135 C134 H134b . . . 110.5(18) ? H134a C134 H134b . . . 104(3) ? C134 C135 C136 . . . 110.8(9) ? C134 C135 H135a . . . 110.8(14) ? C134 C135 H135b . . . 109.3(12) ? C136 C135 H135a . . . 108.8(14) ? C136 C135 H135b . . . 107.5(15) ? H135a C135 H135b . . . 110(2) ? C131 C136 C135 . . . 112.0(3) ? C131 C136 H136a . . . 109.0(14) ? C131 C136 H136b . . . 112.4(16) ? C135 C136 H136a . . . 109.4(16) ? C135 C136 H136b . . . 112.2(17) ? H136a C136 H136b . . . 101(2) ? N11 B N21 . . . 110.27(16) ? N11 B N31 . . . 106.4(3) ? N11 B N41 . . . 109.7(5) ? N21 B N31 . . . 110.1(3) ? N21 B N41 . . . 110.4(5) ? N31 B N41 . . . 110.0(5) ? B N11 N12 . . . 118.7(5) ? B N11 C15 . . . 131.2(5) ? N12 N11 C15 . . . 110.0(10) ? Cu N12 N11 . . . 116.4(9) ? Cu N12 C13 . . . 136.7(2) ? N11 N12 C13 . . . 106.5(7) ? N12 C13 C14 . . . 109.5(3) ? N12 C13 C16 . . . 120.6(8) ? C14 C13 C16 . . . 129.9(6) ? C13 C14 C15 . . . 105.8(5) ? C13 C14 H14 . . . 127.7(17) ? C15 C14 H14 . . . 126.2(19) ? N11 C15 C14 . . . 108.2(9) ? N11 C15 H15 . . . 120.4(18) ? C14 C15 H15 . . . 131.4(16) ? C13 C16 H16a . . . 111.2(17) ? C13 C16 H16b . . . 114(2) ? C13 C16 H16c . . . 110(2) ? H16a C16 H16b . . . 101(3) ? H16a C16 H16c . . . 112(3) ? H16b C16 H16c . . . 108(2) ? B N21 N22 . . . 120.1(4) ? B N21 C25 . . . 130.5(4) ? N22 N21 C25 . . . 109.38(16) ? Cu N22 N21 . . . 116.42(12) ? Cu N22 C23 . . . 136.8(4) ? N21 N22 C23 . . . 106.8(4) ? N22 C23 C24 . . . 109.5(5) ? N22 C23 C26 . . . 122.2(3) ? C24 C23 C26 . . . 128.3(4) ? C23 C24 C25 . . . 106.1(5) ? C23 C24 H24 . . . 123.3(16) ? C25 C24 H24 . . . 130.5(16) ? N21 C25 C24 . . . 108.2(3) ? N21 C25 H25 . . . 121.6(15) ? C24 C25 H25 . . . 130.2(15) ? C23 C26 H26a . . . 111.7(16) ? C23 C26 H26b . . . 112.7(15) ? C23 C26 H26c . . . 112.6(15) ? H26a C26 H26b . . . 111(2) ? H26a C26 H26c . . . 105(3) ? H26b C26 H26c . . . 103(2) ? B N31 N32 . . . 121.13(18) ? B N31 C35 . . . 127.9(2) ? N32 N31 C35 . . . 110.1(2) ? N31 N32 C33 . . . 105.63(18) ? N32 C33 C34 . . . 111.0(2) ? N32 C33 C36 . . . 120.4(2) ? C34 C33 C36 . . . 128.7(3) ? C33 C34 C35 . . . 104.9(4) ? C33 C34 H34 . . . 127.7(16) ? C35 C34 H34 . . . 127.4(16) ? N31 C35 C34 . . . 108.4(3) ? N31 C35 H35 . . . 120.0(16) ? C34 C35 H35 . . . 131.7(16) ? C33 C36 H36a . . . 109.3(18) ? C33 C36 H36b . . . 111(2) ? C33 C36 H36c . . . 109.8(17) ? H36a C36 H36b . . . 112(3) ? H36a C36 H36c . . . 107(2) ? H36b C36 H36c . . . 107(3) ? B N41 N42 . . . 121.4(5) ? B N41 C45 . . . 128.2(2) ? N42 N41 C45 . . . 110.3(6) ? N41 N42 C43 . . . 105.2(6) ? N42 C43 C44 . . . 111.3(5) ? N42 C43 C46 . . . 120.5(6) ? C44 C43 C46 . . . 128.1(2) ? C43 C44 C45 . . . 105.1(2) ? C43 C44 H44 . . . 129.8(19) ? C45 C44 H44 . . . 125.1(19) ? N41 C45 C44 . . . 108.1(4) ? N41 C45 H45 . . . 122.6(16) ? C44 C45 H45 . . . 129.1(15) ? C43 C46 H46a . . . 106(2) ? C43 C46 H46b . . . 112(2) ? C43 C46 H46c . . . 113(2) ? H46a C46 H46b . . . 118(3) ? H46a C46 H46c . . . 106(3) ? H46b C46 H46c . . . 102(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 N12 Cu P C111 . . . . -70.1(7) ? N12 Cu P C121 . . . . 47.7(18) ? N12 Cu P C131 . . . . 165.3(4) ? N22 Cu P C111 . . . . 114.9(9) ? N22 Cu P C121 . . . . -127(2) ? N22 Cu P C131 . . . . -9.7(2) ? P Cu N12 N11 . . . . -141.0(5) ? P Cu N12 C13 . . . . 46.8(6) ? N22 Cu N12 N11 . . . . 35.8(5) ? N22 Cu N12 C13 . . . . -136.4(6) ? P Cu N22 N21 . . . . 134.1(16) ? P Cu N22 C23 . . . . -47.4(17) ? N12 Cu N22 N21 . . . . -41.8(16) ? N12 Cu N22 C23 . . . . 136.6(16) ? Cu P C111 C112 . . . . -28.9(13) ? Cu P C111 C116 . . . . -157.1(9) ? Cu P C111 H111 . . . . 85.1(15) ? C121 P C111 C112 . . . . -149.6(3) ? C121 P C111 C116 . . . . 82(2) ? C121 P C111 H111 . . . . -36(2) ? C131 P C111 C112 . . . . 100(2) ? C131 P C111 C116 . . . . -28.3(3) ? C131 P C111 H111 . . . . -146(2) ? Cu P C121 C122 . . . . -58.9(2) ? Cu P C121 C126 . . . . 172.79(14) ? Cu P C121 H121 . . . . 54.6(15) ? C111 P C121 C122 . . . . 62.5(3) ? C111 P C121 C126 . . . . -65.8(4) ? C111 P C121 H121 . . . . 176.0(15) ? C131 P C121 C122 . . . . 176.16(17) ? C131 P C121 C126 . . . . 47.9(2) ? C131 P C121 H121 . . . . -70.3(15) ? Cu P C131 C132 . . . . -61.9(3) ? Cu P C131 C136 . . . . 59.8(3) ? Cu P C131 H131 . . . . 179.4(13) ? C111 P C131 C132 . . . . 171.66(18) ? C111 P C131 C136 . . . . -66.6(2) ? C111 P C131 H131 . . . . 52.9(13) ? C121 P C131 C132 . . . . 59.7(2) ? C121 P C131 C136 . . . . -178.61(17) ? C121 P C131 H131 . . . . -59.1(13) ? P C111 C112 C113 . . . . 167.9(3) ? P C111 C112 H112a . . . . -72.3(14) ? P C111 C112 H112b . . . . 45.4(17) ? C116 C111 C112 C113 . . . . -59.2(9) ? C116 C111 C112 H112a . . . . 60.7(16) ? C116 C111 C112 H112b . . . . 178.4(16) ? H111 C111 C112 C113 . . . . 56.7(14) ? H111 C111 C112 H112a . . . . 177(2) ? H111 C111 C112 H112b . . . . -66(2) ? P C111 C116 C115 . . . . -173.2(3) ? P C111 C116 H116a . . . . -54(2) ? P C111 C116 H116b . . . . 66.7(15) ? C112 C111 C116 C115 . . . . 58(2) ? C112 C111 C116 H116a . . . . 176.8(16) ? C112 C111 C116 H116b . . . . -62.5(18) ? H111 C111 C116 C115 . . . . -57.9(14) ? H111 C111 C116 H116a . . . . 61(2) ? H111 C111 C116 H116b . . . . -178.0(18) ? C111 C112 C113 C114 . . . . 58(2) ? C111 C112 C113 H113a . . . . -178.1(15) ? C111 C112 C113 H113b . . . . -62.6(19) ? H112a C112 C113 C114 . . . . -63(2) ? H112a C112 C113 H113a . . . . 61(2) ? H112a C112 C113 H113b . . . . 176(2) ? H112b C112 C113 C114 . . . . 179.8(15) ? H112b C112 C113 H113a . . . . -56(3) ? H112b C112 C113 H113b . . . . 59(3) ? C112 C113 C114 C115 . . . . -54(2) ? C112 C113 C114 H114a . . . . 67.9(19) ? C112 C113 C114 H114b . . . . -176.3(18) ? H113a C113 C114 C115 . . . . -178.8(16) ? H113a C113 C114 H114a . . . . -56(2) ? H113a C113 C114 H114b . . . . 59(3) ? H113b C113 C114 C115 . . . . 64.5(18) ? H113b C113 C114 H114a . . . . -173(2) ? H113b C113 C114 H114b . . . . -57(2) ? C113 C114 C115 C116 . . . . 53.2(9) ? C113 C114 C115 H115a . . . . 174.0(16) ? C113 C114 C115 H115b . . . . -66.8(17) ? H114a C114 C115 C116 . . . . -69.6(16) ? H114a C114 C115 H115a . . . . 51(2) ? H114a C114 C115 H115b . . . . 170(2) ? H114b C114 C115 C116 . . . . 178.0(16) ? H114b C114 C115 H115a . . . . -61(2) ? H114b C114 C115 H115b . . . . 58(2) ? C114 C115 C116 C111 . . . . -55(2) ? C114 C115 C116 H116a . . . . -176.4(14) ? C114 C115 C116 H116b . . . . 65.5(18) ? H115a C115 C116 C111 . . . . -179.3(14) ? H115a C115 C116 H116a . . . . 59(3) ? H115a C115 C116 H116b . . . . -59(3) ? H115b C115 C116 C111 . . . . 67(2) ? H115b C115 C116 H116a . . . . -55(2) ? H115b C115 C116 H116b . . . . -173(2) ? P C121 C122 C123 . . . . 173.97(19) ? P C121 C122 H126a . . . . -69.5(16) ? P C121 C122 H126b . . . . 54.3(15) ? C126 C121 C122 C123 . . . . -54.3(7) ? C126 C121 C122 H126a . . . . 62.3(16) ? C126 C121 C122 H126b . . . . -174.0(14) ? H121 C121 C122 C123 . . . . 63.0(16) ? H121 C121 C122 H126a . . . . 180(2) ? H121 C121 C122 H126b . . . . -57(2) ? P C121 C126 C125 . . . . -175.87(19) ? P C121 C126 H122a . . . . -54(2) ? P C121 C126 H122b . . . . 64.8(17) ? C122 C121 C126 C125 . . . . 55.2(18) ? C122 C121 C126 H122a . . . . 176.7(12) ? C122 C121 C126 H122b . . . . -64.2(18) ? H121 C121 C126 C125 . . . . -61.0(18) ? H121 C121 C126 H122a . . . . 61(2) ? H121 C121 C126 H122b . . . . 180(2) ? C121 C122 C123 C124 . . . . 54.7(4) ? C121 C122 C123 H125a . . . . -66.9(15) ? C121 C122 C123 H125b . . . . 174.6(15) ? H126a C122 C123 C124 . . . . -62.7(15) ? H126a C122 C123 H125a . . . . 176(2) ? H126a C122 C123 H125b . . . . 57(2) ? H126b C122 C123 C124 . . . . 176.0(16) ? H126b C122 C123 H125a . . . . 54(2) ? H126b C122 C123 H125b . . . . -64(2) ? C122 C123 C124 C125 . . . . -55.4(18) ? C122 C123 C124 H124a . . . . -177.1(17) ? C122 C123 C124 H124b . . . . 64.2(18) ? H125a C123 C124 C125 . . . . 68.1(19) ? H125a C123 C124 H124a . . . . -54(2) ? H125a C123 C124 H124b . . . . -172(2) ? H125b C123 C124 C125 . . . . -177.2(12) ? H125b C123 C124 H124a . . . . 61(3) ? H125b C123 C124 H124b . . . . -58(2) ? C123 C124 C125 C126 . . . . 56.9(7) ? C123 C124 C125 H123a . . . . -64.3(18) ? C123 C124 C125 H123b . . . . 179.6(14) ? H124a C124 C125 C126 . . . . 177(2) ? H124a C124 C125 H123a . . . . 56(3) ? H124a C124 C125 H123b . . . . -60(2) ? H124b C124 C125 C126 . . . . -64.4(16) ? H124b C124 C125 H123a . . . . 174(2) ? H124b C124 C125 H123b . . . . 58(2) ? C124 C125 C126 C121 . . . . -57.0(5) ? C124 C125 C126 H122a . . . . -179.4(15) ? C124 C125 C126 H122b . . . . 61.1(16) ? H123a C125 C126 C121 . . . . 64.9(17) ? H123a C125 C126 H122a . . . . -58(2) ? H123a C125 C126 H122b . . . . -177(2) ? H123b C125 C126 C121 . . . . 177.4(16) ? H123b C125 C126 H122a . . . . 55(2) ? H123b C125 C126 H122b . . . . -64(2) ? P C131 C132 C133 . . . . 176.2(2) ? P C131 C132 H132a . . . . -59(3) ? P C131 C132 H132b . . . . 56.2(19) ? C136 C131 C132 C133 . . . . 54(2) ? C136 C131 C132 H132a . . . . 178.4(14) ? C136 C131 C132 H132b . . . . -66.5(19) ? H131 C131 C132 C133 . . . . -68(2) ? H131 C131 C132 H132a . . . . 57(2) ? H131 C131 C132 H132b . . . . 172(2) ? P C131 C136 C135 . . . . -176.3(2) ? P C131 C136 H136a . . . . -55.0(16) ? P C131 C136 H136b . . . . 56.3(17) ? C132 C131 C136 C135 . . . . -55.3(4) ? C132 C131 C136 H136a . . . . 65.9(17) ? C132 C131 C136 H136b . . . . 177.3(17) ? H131 C131 C136 C135 . . . . 66.4(16) ? H131 C131 C136 H136a . . . . -172(2) ? H131 C131 C136 H136b . . . . -61(2) ? C131 C132 C133 C134 . . . . -53.8(3) ? C131 C132 C133 H133a . . . . -179.0(16) ? C131 C132 C133 H133b . . . . 66.6(13) ? H132a C132 C133 C134 . . . . -179.3(14) ? H132a C132 C133 H133a . . . . 56(2) ? H132a C132 C133 H133b . . . . -59(2) ? H132b C132 C133 C134 . . . . 66.1(14) ? H132b C132 C133 H133a . . . . -59(2) ? H132b C132 C133 H133b . . . . -173.5(18) ? C132 C133 C134 C135 . . . . 54.6(4) ? C132 C133 C134 H134a . . . . -64.0(18) ? C132 C133 C134 H134b . . . . 179(2) ? H133a C133 C134 C135 . . . . 177.3(16) ? H133a C133 C134 H134a . . . . 59(2) ? H133a C133 C134 H134b . . . . -58(3) ? H133b C133 C134 C135 . . . . -66.1(16) ? H133b C133 C134 H134a . . . . 175(2) ? H133b C133 C134 H134b . . . . 59(2) ? C133 C134 C135 C136 . . . . -56(2) ? C133 C134 C135 H135a . . . . -176.5(15) ? C133 C134 C135 H135b . . . . 62.7(17) ? H134a C134 C135 C136 . . . . 66(2) ? H134a C134 C135 H135a . . . . -55(2) ? H134a C134 C135 H135b . . . . -176(2) ? H134b C134 C135 C136 . . . . 178(2) ? H134b C134 C135 H135a . . . . 58(3) ? H134b C134 C135 H135b . . . . -63(3) ? C134 C135 C136 C131 . . . . 56.7(3) ? C134 C135 C136 H136a . . . . -64.2(14) ? C134 C135 C136 H136b . . . . -175.8(18) ? H135a C135 C136 C131 . . . . 178.8(15) ? H135a C135 C136 H136a . . . . 58(2) ? H135a C135 C136 H136b . . . . -54(2) ? H135b C135 C136 C131 . . . . -62.6(13) ? H135b C135 C136 H136a . . . . 176.4(18) ? H135b C135 C136 H136b . . . . 65(2) ? N21 B N11 N12 . . . . -63.0(17) ? N21 B N11 C15 . . . . 122.6(17) ? N31 B N11 N12 . . . . 56.4(14) ? N31 B N11 C15 . . . . -118.1(13) ? N41 B N11 N12 . . . . 175.24(17) ? N41 B N11 C15 . . . . .8(3) ? N11 B N21 N22 . . . . 56.3(10) ? N11 B N21 C25 . . . . -120.5(11) ? N31 B N21 N22 . . . . -60.7(2) ? N31 B N21 C25 . . . . 122.4(2) ? N41 B N21 N22 . . . . 177.69(16) ? N41 B N21 C25 . . . . .9(3) ? N11 B N31 N32 . . . . -157.82(16) ? N11 B N31 C35 . . . . 33.7(3) ? N21 B N31 N32 . . . . -38.4(9) ? N21 B N31 C35 . . . . 153.2(7) ? N41 B N31 N32 . . . . 83.5(15) ? N41 B N31 C35 . . . . -85.0(13) ? N11 B N41 N42 . . . . 61(2) ? N11 B N41 C45 . . . . -114(2) ? N21 B N41 N42 . . . . -60.4(2) ? N21 B N41 C45 . . . . 123.9(3) ? N31 B N41 N42 . . . . 177.9(2) ? N31 B N41 C45 . . . . 2.3(3) ? B N11 N12 Cu . . . . 9.9(2) ? B N11 N12 C13 . . . . -175.68(17) ? C15 N11 N12 Cu . . . . -174.54(15) ? C15 N11 N12 C13 . . . . -.1(2) ? B N11 C15 C14 . . . . 174.9(2) ? B N11 C15 H15 . . . . -3.8(18) ? N12 N11 C15 C14 . . . . .0(2) ? N12 N11 C15 H15 . . . . -178.6(17) ? Cu N12 C13 C14 . . . . 172.87(18) ? Cu N12 C13 C16 . . . . -6.0(3) ? N11 N12 C13 C14 . . . . .1(2) ? N11 N12 C13 C16 . . . . -178.7(2) ? N12 C13 C14 C15 . . . . -.1(3) ? N12 C13 C14 H14 . . . . -174(2) ? C16 C13 C14 C15 . . . . 178.5(2) ? C16 C13 C14 H14 . . . . 5(2) ? N12 C13 C16 H16a . . . . -132(3) ? N12 C13 C16 H16b . . . . -19(2) ? N12 C13 C16 H16c . . . . 103(3) ? C14 C13 C16 H16a . . . . 49(3) ? C14 C13 C16 H16b . . . . 163(2) ? C14 C13 C16 H16c . . . . -76(3) ? C13 C14 C15 N11 . . . . .1(3) ? C13 C14 C15 H15 . . . . 178(2) ? H14 C14 C15 N11 . . . . 174(2) ? H14 C14 C15 H15 . . . . -8(3) ? B N21 N22 Cu . . . . 1.6(2) ? B N21 N22 C23 . . . . -177.3(2) ? C25 N21 N22 Cu . . . . 179.07(13) ? C25 N21 N22 C23 . . . . .2(2) ? B N21 C25 C24 . . . . 177.3(2) ? B N21 C25 H25 . . . . -2.4(17) ? N22 N21 C25 C24 . . . . .2(2) ? N22 N21 C25 H25 . . . . -179.5(16) ? Cu N22 C23 C24 . . . . -179.03(15) ? Cu N22 C23 C26 . . . . .8(3) ? N21 N22 C23 C24 . . . . -.5(2) ? N21 N22 C23 C26 . . . . 179.32(18) ? N22 C23 C24 C25 . . . . .6(2) ? N22 C23 C24 H24 . . . . 178.3(19) ? C26 C23 C24 C25 . . . . -179.2(2) ? C26 C23 C24 H24 . . . . -1.5(19) ? N22 C23 C26 H26a . . . . 100(3) ? N22 C23 C26 H26b . . . . -133.9(17) ? N22 C23 C26 H26c . . . . -17.6(19) ? C24 C23 C26 H26a . . . . -80(3) ? C24 C23 C26 H26b . . . . 45.9(18) ? C24 C23 C26 H26c . . . . 162.2(19) ? C23 C24 C25 N21 . . . . -.5(2) ? C23 C24 C25 H25 . . . . 179.1(18) ? H24 C24 C25 N21 . . . . -178(2) ? H24 C24 C25 H25 . . . . 2(3) ? B N31 N32 C33 . . . . -171.39(19) ? C35 N31 N32 C33 . . . . -1.1(2) ? B N31 C35 C34 . . . . 170.3(3) ? B N31 C35 H35 . . . . -9.1(17) ? N32 N31 C35 C34 . . . . .8(2) ? N32 N31 C35 H35 . . . . -178.6(16) ? N31 N32 C33 C34 . . . . 1.0(2) ? N31 N32 C33 C36 . . . . -179.09(19) ? N32 C33 C34 C35 . . . . -.5(2) ? N32 C33 C34 H34 . . . . -178.9(19) ? C36 C33 C34 C35 . . . . 179.6(2) ? C36 C33 C34 H34 . . . . 1.2(19) ? N32 C33 C36 H36a . . . . -108(2) ? N32 C33 C36 H36b . . . . 17(2) ? N32 C33 C36 H36c . . . . 134.7(15) ? C34 C33 C36 H36a . . . . 72(2) ? C34 C33 C36 H36b . . . . -163(2) ? C34 C33 C36 H36c . . . . -45.4(16) ? C33 C34 C35 N31 . . . . -.2(2) ? C33 C34 C35 H35 . . . . 179(2) ? H34 C34 C35 N31 . . . . 178.2(19) ? H34 C34 C35 H35 . . . . -2(3) ? B N41 N42 C43 . . . . -176.4(2) ? C45 N41 N42 C43 . . . . -.0(3) ? B N41 C45 C44 . . . . 175.7(3) ? B N41 C45 H45 . . . . 0(2) ? N42 N41 C45 C44 . . . . -.4(3) ? N42 N41 C45 H45 . . . . -176(2) ? N41 N42 C43 C44 . . . . .4(3) ? N41 N42 C43 C46 . . . . -178.3(2) ? N42 C43 C44 C45 . . . . -.7(3) ? N42 C43 C44 H44 . . . . 179(2) ? C46 C43 C44 C45 . . . . 177.9(3) ? C46 C43 C44 H44 . . . . -2(2) ? N42 C43 C46 H46a . . . . -157(2) ? N42 C43 C46 H46b . . . . -26(2) ? N42 C43 C46 H46c . . . . 88(3) ? C44 C43 C46 H46a . . . . 25(2) ? C44 C43 C46 H46b . . . . 155(2) ? C44 C43 C46 H46c . . . . -91(3) ? C43 C44 C45 N41 . . . . .6(3) ? C43 C44 C45 H45 . . . . 176(2) ? H44 C44 C45 N41 . . . . -179(2) ? H44 C44 C45 H45 . . . . -4(3) ? 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 C111 3.354(2) . . ? Cu C112 3.398(2) . . ? Cu C113 3.912(2) . '3 766' ? Cu C121 3.334(2) . . ? Cu C122 3.665(3) . . ? Cu C131 3.425(2) . . ? Cu C132 3.768(2) . . ? Cu C136 3.797(2) . . ? Cu B 3.071(2) . . ? Cu N11 2.9233(16) . . ? Cu C13 3.159(2) . . ? Cu C14 4.272(2) . . ? Cu C15 4.128(2) . . ? Cu C16 3.595(2) . . ? Cu N21 2.8914(19) . . ? Cu C23 3.120(2) . . ? Cu C24 4.232(3) . . ? Cu C25 4.099(3) . . ? Cu C26 3.599(3) . . ? Cu N31 2.9679(16) . . ? Cu N32 3.5009(17) . . ? Cu C33 4.167(2) . . ? Cu C34 4.205(2) . . ? Cu C35 3.489(2) . . ? Cu H111 3.60(2) . . ? Cu H112a 3.62(2) . . ? Cu H112b 2.80(2) . . ? Cu H113a 2.97(2) . '3 766' ? Cu H121 3.29(2) . . ? Cu H126b 3.16(3) . . ? Cu H132b 3.23(2) . . ? Cu H136a 3.25(3) . . ? Cu H16b 3.18(3) . . ? Cu H16c 3.96(3) . . ? Cu H26c 3.17(3) . . ? Cu H35 3.71(2) . . ? P C112 2.812(2) . . ? P C113 4.173(2) . . ? P C114 4.761(2) . . ? P C115 4.259(2) . . ? P C116 2.920(2) . . ? P C122 2.809(2) . . ? P C123 4.198(2) . . ? P C124 4.734(3) . . ? P C125 4.247(3) . . ? P C126 2.894(3) . . ? P C132 2.763(2) . . ? P C133 4.165(3) . . ? P C134 4.654(3) . . ? P C135 4.189(3) . . ? P C136 2.798(2) . . ? P N12 3.7811(18) . . ? P C13 4.521(2) . . ? P C16 4.327(2) . . ? P N22 3.939(2) . . ? P C23 4.768(3) . . ? P C26 4.709(3) . . ? P N31 4.3697(18) . . ? P N32 4.5503(19) . . ? P C33 4.648(2) . . ? P C34 4.591(2) . . ? P C35 4.411(2) . . ? P H111 2.26(2) . . ? P H112a 3.07(2) . . ? P H112b 2.84(2) . . ? P H113b 4.32(2) . . ? P H116a 3.07(2) . . ? P H116b 3.14(2) . . ? P H121 2.21(2) . . ? P H122a 3.04(2) . . ? P H122b 3.07(3) . . ? P H126a 3.00(3) . . ? P H126b 2.90(2) . . ? P H131 2.26(2) . . ? P H132a 2.92(2) . . ? P H132b 2.85(2) . . ? P H136a 2.90(3) . . ? P H136b 2.96(2) . . ? P H16b 3.52(3) . . ? P H26c 4.06(3) . . ? C111 C113 2.515(3) . . ? C111 C114 2.960(3) . . ? C111 C115 2.525(3) . . ? C111 C121 2.961(3) . . ? C111 C122 3.382(3) . . ? C111 C126 3.521(3) . . ? C111 C131 2.999(3) . . ? C111 C132 4.346(3) . . ? C111 C136 3.475(3) . . ? C111 C16 4.057(3) . . ? C111 H112a 2.09(2) . . ? C111 H112b 2.06(2) . . ? C111 H113a 3.38(2) . . ? C111 H113b 2.68(2) . . ? C111 H114a 3.34(2) . . ? C111 H114b 3.87(3) . . ? C111 H115a 3.33(2) . . ? C111 H115b 2.74(2) . . ? C111 H116a 2.09(3) . . ? C111 H116b 2.07(2) . . ? C111 H121 3.67(2) . . ? C111 H122a 3.81(2) . . ? C111 H122b 3.12(3) . . ? C111 H125b 3.98(3) . '3 666' ? C111 H126a 2.99(2) . . ? C111 H126b 3.60(2) . . ? C111 H131 3.03(2) . . ? C111 H136a 3.75(3) . . ? C111 H136b 3.06(3) . . ? C111 H16b 3.14(3) . . ? C112 C112 4.204(3) . '3 766' ? C112 C113 4.260(4) . '3 766' ? C112 C114 2.514(3) . . ? C112 C115 2.936(4) . . ? C112 C116 2.507(4) . . ? C112 C121 4.267(3) . . ? C112 C131 3.870(3) . . ? C112 C136 3.785(3) . . ? C112 C13 4.167(3) . '3 766' ? C112 C16 3.807(3) . . ? C112 C16 3.878(4) . '3 766' ? C112 H111 2.03(2) . . ? C112 H112b 3.50(2) . '3 766' ? C112 H113a 3.65(3) . '3 766' ? C112 H113a 2.10(2) . . ? C112 H113b 2.01(2) . . ? C112 H114a 2.76(2) . . ? C112 H114b 3.41(3) . . ? C112 H115a 3.80(2) . . ? C112 H115b 3.32(3) . . ? C112 H116a 3.36(3) . . ? C112 H116b 2.71(2) . . ? C112 H136a 3.78(3) . . ? C112 H136b 3.16(3) . . ? C112 H16b 3.07(3) . . ? C112 H16c 3.13(3) . '3 766' ? C112 H16c 3.71(3) . . ? C112 H26c 3.76(3) . . ? C113 C115 2.518(4) . . ? C113 C116 2.944(3) . . ? C113 N11 4.114(3) . '3 766' ? C113 N12 3.591(3) . '3 766' ? C113 C13 3.670(3) . '3 766' ? C113 C14 4.251(3) . '3 766' ? C113 C16 4.153(3) . . ? C113 C16 3.882(4) . '3 766' ? C113 N21 4.296(3) . '3 766' ? C113 N22 3.696(3) . '3 766' ? C113 C23 3.848(3) . '3 766' ? C113 C26 4.008(3) . '3 766' ? C113 H111 2.64(2) . . ? C113 H112a 2.06(2) . . ? C113 H112b 3.42(2) . '3 766' ? C113 H112b 2.06(2) . . ? C113 H114a 2.04(2) . . ? C113 H114b 2.13(3) . . ? C113 H115a 3.37(2) . . ? C113 H115b 2.78(3) . . ? C113 H116a 3.82(2) . . ? C113 H116b 3.28(2) . . ? C113 H124a 3.80(3) . '3 666' ? C113 H16b 3.53(3) . . ? C113 H16c 3.39(3) . '3 766' ? C113 H16c 3.86(3) . . ? C113 H26b 3.90(3) . '3 766' ? C113 H26c 3.67(3) . '3 766' ? C114 C116 2.536(3) . . ? C114 C134 4.197(4) . 4 ? C114 N11 3.892(3) . '3 766' ? C114 N12 3.857(3) . '3 766' ? C114 C13 3.861(4) . '3 766' ? C114 C14 3.924(4) . '3 766' ? C114 C15 3.938(3) . '3 766' ? C114 N21 4.215(3) . '3 766' ? C114 N22 4.098(3) . '3 766' ? C114 C23 4.046(3) . 4 ? C114 C23 4.273(3) . '3 766' ? C114 C24 3.864(3) . 4 ? C114 C26 4.293(4) . 4 ? C114 H111 3.19(2) . . ? C114 H112a 2.71(2) . . ? C114 H112b 3.33(2) . . ? C114 H113a 2.08(3) . . ? C114 H113b 2.04(2) . . ? C114 H115a 2.10(2) . . ? C114 H115b 2.09(2) . . ? C114 H116a 3.35(2) . . ? C114 H116b 2.76(2) . . ? C114 H134a 3.24(3) . 4 ? C114 H24 3.81(3) . 4 ? C114 H26a 3.65(3) . 4 ? C115 C132 4.290(4) . 4 ? C115 C133 4.206(4) . 4 ? C115 C134 4.038(4) . 4 ? C115 N21 4.148(3) . 4 ? C115 N22 4.100(3) . 4 ? C115 C23 3.919(3) . 4 ? C115 C24 3.858(3) . 4 ? C115 C25 4.012(3) . 4 ? C115 N32 3.541(3) . 4 ? C115 C33 4.250(4) . 4 ? C115 C36 4.034(4) . 4 ? C115 H111 2.66(2) . . ? C115 H112a 3.25(2) . . ? C115 H112b 3.80(2) . . ? C115 H113a 3.37(3) . . ? C115 H113b 2.74(2) . . ? C115 H114a 2.04(3) . . ? C115 H114b 2.08(3) . . ? C115 H116a 2.05(2) . . ? C115 H116b 2.06(2) . . ? C115 H122b 4.01(2) . . ? C115 H125b 3.65(2) . '3 666' ? C115 H132b 3.52(3) . 4 ? C115 H133a 3.83(3) . 4 ? C115 H134a 3.18(3) . 4 ? C115 H26a 4.01(2) . 4 ? C115 H36b 3.21(3) . 4 ? C116 C121 3.733(3) . . ? C116 C122 4.361(3) . . ? C116 C126 3.662(3) . . ? C116 C131 3.278(3) . . ? C116 C136 3.644(4) . . ? C116 N21 4.083(3) . 4 ? C116 C24 4.023(3) . 4 ? C116 C25 3.759(3) . 4 ? C116 N32 3.405(3) . 4 ? C116 C33 4.190(4) . 4 ? C116 C36 4.073(4) . 4 ? C116 H111 2.04(2) . . ? C116 H112a 2.71(2) . . ? C116 H112b 3.32(2) . . ? C116 H113a 3.85(2) . . ? C116 H113b 3.25(2) . . ? C116 H114a 2.79(2) . . ? C116 H114b 3.39(3) . . ? C116 H115a 2.03(2) . . ? C116 H115b 2.06(2) . . ? C116 H122a 3.75(2) . . ? C116 H122b 3.03(2) . . ? C116 H125b 3.99(2) . '3 666' ? C116 H126a 3.87(2) . . ? C116 H131 2.91(2) . . ? C116 H136b 3.08(3) . . ? C116 H25 3.81(2) . 4 ? C116 H36b 3.39(4) . 4 ? C121 C123 2.539(3) . . ? C121 C124 2.958(4) . . ? C121 C125 2.526(3) . . ? C121 C131 2.911(3) . . ? C121 C132 3.236(3) . . ? C121 C136 4.301(3) . . ? C121 N12 4.289(3) . . ? C121 N31 4.398(3) . . ? C121 C33 4.231(3) . . ? C121 C34 3.755(3) . . ? C121 C35 3.888(3) . . ? C121 H111 2.82(2) . . ? C121 H116a 3.41(2) . . ? C121 H122a 2.09(2) . . ? C121 H122b 2.06(3) . . ? C121 H123a 2.73(2) . . ? C121 H123b 3.41(3) . . ? C121 H124a 3.77(3) . . ? C121 H124b 3.30(3) . . ? C121 H125a 2.80(2) . . ? C121 H125b 3.41(2) . . ? C121 H126a 2.05(2) . . ? C121 H126b 2.03(2) . . ? C121 H131 2.97(2) . . ? C121 H132a 2.78(2) . . ? C121 H132b 3.48(3) . . ? C121 H16b 3.93(3) . . ? C121 H34 3.78(2) . . ? C122 C123 4.319(4) . '3 666' ? C122 C124 2.511(4) . . ? C122 C124 4.019(4) . '3 666' ? C122 C125 2.932(3) . . ? C122 C126 2.516(3) . . ? C122 C131 4.302(3) . . ? C122 N12 3.851(3) . . ? C122 C13 4.046(3) . . ? C122 C16 3.777(3) . . ? C122 C34 3.951(3) . . ? C122 C35 3.758(4) . . ? C122 C36 4.360(3) . '2 655' ? C122 H111 2.82(2) . . ? C122 H121 1.96(2) . . ? C122 H122a 3.37(2) . . ? C122 H122b 2.71(3) . . ? C122 H123a 3.26(2) . . ? C122 H123b 3.88(3) . . ? C122 H124a 3.28(3) . . ? C122 H124b 3.16(2) . '3 666' ? C122 H124b 2.75(3) . . ? C122 H125a 2.07(2) . . ? C122 H125b 3.84(2) . '3 666' ? C122 H125b 2.11(2) . . ? C122 H126a 3.83(3) . '3 666' ? C122 H16a 3.74(3) . . ? C122 H16b 3.13(3) . . ? C122 H34 3.89(2) . . ? C122 H35 3.57(3) . . ? C122 H36b 4.03(3) . '2 655' ? C123 C125 2.505(4) . . ? C123 C126 2.946(3) . . ? C123 C133 4.298(4) . '2 655' ? C123 C34 3.968(4) . . ? C123 C35 4.043(4) . . ? C123 C36 4.088(4) . '2 655' ? C123 H111 3.88(2) . '3 666' ? C123 H115b 3.49(2) . '3 666' ? C123 H121 2.68(2) . . ? C123 H122a 3.83(2) . . ? C123 H122b 3.26(2) . . ? C123 H123a 2.73(2) . . ? C123 H123b 3.42(3) . . ? C123 H124a 2.00(3) . . ? C123 H124b 2.08(3) . . ? C123 H124b 3.64(2) . '3 666' ? C123 H126a 3.39(3) . '3 666' ? C123 H126a 2.03(2) . . ? C123 H126b 1.99(3) . . ? C123 H133a 3.34(2) . '2 655' ? C123 H34 3.56(3) . . ? C123 H35 3.78(3) . . ? C123 H36b 3.47(3) . '2 655' ? C124 C126 2.515(3) . . ? C124 C16 3.747(4) . '3 666' ? C124 C26 4.192(3) . '1 455' ? C124 H111 3.61(2) . '3 666' ? C124 H113b 3.72(2) . '3 666' ? C124 H115b 3.91(2) . '3 666' ? C124 H121 3.21(2) . . ? C124 H122a 3.35(2) . . ? C124 H122b 2.72(2) . . ? C124 H123a 2.05(3) . . ? C124 H123b 2.15(3) . . ? C124 H125a 2.02(3) . . ? C124 H125b 2.06(3) . . ? C124 H126a 3.15(2) . '3 666' ? C124 H126a 2.68(2) . . ? C124 H126b 3.27(3) . . ? C124 H16a 3.14(3) . '3 666' ? C124 H16b 3.41(3) . '3 666' ? C124 H26b 3.27(3) . '1 455' ? C124 H36a 3.71(3) . 4 ? C125 C15 3.835(3) . '2 645' ? C125 C16 4.354(4) . '3 666' ? C125 C26 4.247(3) . '1 455' ? C125 C36 4.286(4) . 4 ? C125 N42 4.320(3) . '2 645' ? C125 C43 4.036(4) . '2 645' ? C125 C44 4.194(4) . '2 645' ? C125 C46 4.340(4) . '2 645' ? C125 H121 2.67(2) . . ? C125 H122a 2.07(2) . . ? C125 H122b 2.08(2) . . ? C125 H124a 2.03(3) . . ? C125 H124b 2.05(2) . . ? C125 H125a 2.73(2) . . ? C125 H125b 3.36(3) . . ? C125 H126a 3.23(2) . . ? C125 H126b 3.73(3) . . ? C125 H132a 3.90(2) . . ? C125 H15 3.07(2) . '2 645' ? C125 H16a 3.55(3) . '3 666' ? C125 H26b 3.35(3) . '1 455' ? C125 H36a 3.45(3) . 4 ? C126 C131 3.272(3) . . ? C126 C132 3.636(4) . . ? C126 C36 3.968(4) . 4 ? C126 H111 3.40(2) . . ? C126 H116a 2.98(2) . . ? C126 H121 1.99(2) . . ? C126 H123a 2.04(2) . . ? C126 H123b 2.10(3) . . ? C126 H124a 3.30(3) . . ? C126 H124b 2.72(3) . . ? C126 H125a 3.31(2) . . ? C126 H125b 3.85(2) . . ? C126 H126a 2.69(2) . . ? C126 H126b 3.30(3) . . ? C126 H131 2.90(2) . . ? C126 H132a 3.06(2) . . ? C126 H15 4.03(2) . '2 645' ? C126 H36a 3.37(3) . 4 ? C126 H36b 3.86(3) . 4 ? C131 C133 2.543(3) . . ? C131 C134 2.963(4) . . ? C131 C135 2.533(3) . . ? C131 H111 3.69(2) . . ? C131 H112a 3.68(2) . . ? C131 H116a 3.28(2) . . ? C131 H116b 3.01(2) . . ? C131 H121 3.01(2) . . ? C131 H122a 2.82(2) . . ? C131 H122b 3.57(3) . . ? C131 H132a 2.12(2) . . ? C131 H132b 2.06(2) . . ? C131 H133a 3.38(2) . . ? C131 H133b 2.78(2) . . ? C131 H134a 3.31(3) . . ? C131 H134b 3.80(3) . . ? C131 H135a 3.39(3) . . ? C131 H135b 2.73(2) . . ? C131 H136a 2.09(3) . . ? C131 H136b 2.11(2) . . ? C132 C134 2.522(4) . . ? C132 C135 2.946(3) . . ? C132 C136 2.516(3) . . ? C132 N32 3.938(3) . . ? C132 C33 3.763(3) . . ? C132 C34 4.406(3) . . ? C132 C36 3.690(3) . . ? C132 H115a 3.67(3) . '4 554' ? C132 H115b 3.94(3) . '4 554' ? C132 H121 2.90(2) . . ? C132 H122a 3.07(3) . . ? C132 H131 2.03(2) . . ? C132 H133a 2.06(2) . . ? C132 H133b 2.07(2) . . ? C132 H134a 2.78(3) . . ? C132 H134b 3.32(3) . . ? C132 H135a 3.86(2) . . ? C132 H135b 3.27(2) . . ? C132 H136a 2.75(2) . . ? C132 H136b 3.39(2) . . ? C132 H35 3.95(3) . '2 645' ? C132 H36b 3.45(3) . . ? C132 H36c 3.35(2) . . ? C133 C135 2.507(4) . . ? C133 C136 2.932(3) . . ? C133 C34 3.897(4) . '2 645' ? C133 C35 3.835(4) . '2 645' ? C133 C36 4.162(4) . . ? C133 C43 4.361(3) . 4 ? C133 C44 3.892(4) . 4 ? C133 H115a 3.88(2) . '4 554' ? C133 H115b 3.63(3) . '4 554' ? C133 H122a 3.96(3) . . ? C133 H125a 3.57(2) . '2 645' ? C133 H131 2.77(2) . . ? C133 H132a 2.09(2) . . ? C133 H132b 2.05(2) . . ? C133 H134a 2.10(3) . . ? C133 H134b 2.04(3) . . ? C133 H135a 3.39(2) . . ? C133 H135b 2.73(2) . . ? C133 H136a 3.29(2) . . ? C133 H136b 3.87(2) . . ? C133 H34 3.46(3) . '2 645' ? C133 H35 3.35(2) . '2 645' ? C133 H36b 3.69(3) . . ? C133 H36c 3.79(2) . . ? C133 H44 3.55(3) . 4 ? C134 C136 2.508(4) . . ? C134 C24 3.867(4) . '2 745' ? C134 C25 3.867(4) . '2 745' ? C134 C43 4.203(4) . 4 ? C134 C44 4.229(5) . 4 ? C134 C46 4.032(4) . 4 ? C134 H114b 3.41(3) . '4 554' ? C134 H115a 3.79(2) . '4 554' ? C134 H115b 3.64(2) . '4 554' ? C134 H131 3.30(2) . . ? C134 H132a 3.38(2) . . ? C134 H132b 2.75(2) . . ? C134 H133a 2.10(2) . . ? C134 H133b 2.06(2) . . ? C134 H135a 2.10(2) . . ? C134 H135b 2.08(2) . . ? C134 H136a 2.74(3) . . ? C134 H136b 3.38(2) . . ? C134 H24 3.64(3) . '2 745' ? C134 H25 3.65(2) . '2 745' ? C134 H46c 3.29(3) . 4 ? C135 C135 4.263(3) . '3 756' ? C135 C25 4.414(4) . 4 ? C135 C25 4.196(4) . '2 745' ? C135 N42 4.212(4) . 4 ? C135 N42 4.068(4) . '2 745' ? C135 C43 4.419(4) . '2 745' ? C135 C43 3.819(4) . 4 ? C135 C44 4.055(4) . 4 ? C135 C46 3.919(4) . 4 ? C135 C46 3.948(4) . '2 745' ? C135 H116b 4.00(2) . . ? C135 H131 2.74(2) . . ? C135 H132a 3.85(2) . . ? C135 H132b 3.29(2) . . ? C135 H133a 3.38(2) . . ? C135 H133b 2.74(2) . . ? C135 H134a 2.04(3) . . ? C135 H134b 2.02(3) . . ? C135 H135a 3.57(2) . '3 756' ? C135 H135b 3.99(2) . '3 756' ? C135 H136a 2.10(3) . . ? C135 H136b 2.11(3) . . ? C135 H25 3.65(2) . '2 745' ? C135 H25 3.53(2) . 4 ? C135 H26a 3.81(3) . . ? C135 H46b 3.55(3) . '2 745' ? C135 H46c 3.20(3) . 4 ? C135 H46c 3.47(3) . '2 745' ? C136 C26 3.750(4) . . ? C136 C46 3.917(4) . '2 745' ? C136 H112a 3.23(2) . . ? C136 H116a 3.96(3) . . ? C136 H116b 3.04(2) . . ? C136 H131 2.01(2) . . ? C136 H132a 3.39(2) . . ? C136 H132b 2.73(2) . . ? C136 H133a 3.83(2) . . ? C136 H133b 3.30(2) . . ? C136 H134a 2.71(3) . . ? C136 H134b 3.30(3) . . ? C136 H135a 2.09(3) . . ? C136 H135b 2.07(2) . . ? C136 H25 3.74(2) . 4 ? C136 H26a 3.34(3) . . ? C136 H26c 3.25(3) . . ? C136 H46b 3.26(3) . '2 745' ? C136 H46c 3.58(3) . '2 745' ? B N12 2.513(3) . . ? B C13 3.638(3) . . ? B C14 3.728(3) . . ? B C15 2.636(3) . . ? B N22 2.519(3) . . ? B C23 3.632(3) . . ? B C24 3.709(3) . . ? B C25 2.620(3) . . ? B N32 2.538(3) . . ? B C33 3.625(3) . . ? B C34 3.708(3) . . ? B C35 2.606(3) . . ? B N42 2.532(3) . . ? B C43 3.612(3) . . ? B C44 3.689(3) . . ? B C45 2.582(3) . . ? B H114b 4.03(3) . '3 766' ? B H15 2.86(2) . . ? B H25 2.86(3) . . ? B H35 2.82(3) . . ? B H45 2.81(2) . . ? N11 C13 2.175(3) . . ? N11 C14 2.201(3) . . ? N11 C16 3.599(3) . . ? N11 N21 2.529(2) . . ? N11 N22 3.037(2) . . ? N11 C23 4.220(3) . . ? N11 C25 3.657(3) . . ? N11 N31 2.473(2) . . ? N11 N32 3.748(2) . . ? N11 C34 4.260(3) . . ? N11 C35 2.935(3) . . ? N11 N41 2.514(2) . . ? N11 N42 3.083(3) . . ? N11 C43 4.218(3) . . ? N11 C45 3.577(3) . . ? N11 H113a 3.41(2) . '3 766' ? N11 H114a 3.54(2) . '3 766' ? N11 H114b 3.53(3) . '3 766' ? N11 H126b 3.96(3) . . ? N11 H14 3.07(3) . . ? N11 H15 1.98(2) . . ? N11 H16b 3.90(3) . . ? N11 H25 3.97(3) . . ? N11 H35 2.65(3) . . ? N11 H45 3.84(2) . . ? N12 C14 2.240(3) . . ? N12 C15 2.222(3) . . ? N12 C16 2.463(3) . . ? N12 N21 3.072(3) . . ? N12 N22 2.948(2) . . ? N12 C23 4.166(3) . . ? N12 C25 4.319(3) . . ? N12 N31 2.939(2) . . ? N12 N32 4.101(2) . . ? N12 C34 4.377(3) . . ? N12 C35 3.180(2) . . ? N12 N41 3.789(3) . . ? N12 H112b 3.59(2) . . ? N12 H113a 2.71(2) . '3 766' ? N12 H114a 3.56(3) . '3 766' ? N12 H114b 3.78(3) . '3 766' ? N12 H126b 3.02(3) . . ? N12 H14 3.11(3) . . ? N12 H15 3.09(3) . . ? N12 H16a 3.13(3) . . ? N12 H16b 2.60(3) . . ? N12 H16c 2.93(3) . . ? N12 H35 2.88(2) . . ? N12 H36c 4.00(3) . '2 655' ? C13 C15 2.212(3) . . ? C13 N21 4.285(3) . . ? C13 N22 4.172(3) . . ? C13 N31 4.112(3) . . ? C13 C35 4.071(3) . . ? C13 C36 3.933(4) . '2 655' ? C13 C46 4.307(3) . '4 565' ? C13 H112a 3.67(2) . '3 766' ? C13 H112b 3.78(2) . . ? C13 H113a 2.94(2) . '3 766' ? C13 H114a 3.32(3) . '3 766' ? C13 H126b 3.22(3) . . ? C13 H14 2.08(3) . . ? C13 H15 3.13(3) . . ? C13 H16a 2.03(3) . . ? C13 H16b 2.06(3) . . ? C13 H16c 1.97(3) . . ? C13 H35 3.49(2) . . ? C13 H36a 3.63(3) . '2 655' ? C13 H36c 3.30(3) . '2 655' ? C13 H46a 3.66(4) . '4 565' ? C14 C16 2.617(3) . . ? C14 C24 4.091(3) . '2 755' ? C14 C34 4.362(3) . '2 655' ? C14 C35 4.400(3) . . ? C14 C36 3.802(4) . '2 655' ? C14 N41 4.319(3) . . ? C14 C46 4.141(4) . '4 565' ? C14 H113a 3.74(2) . '3 766' ? C14 H114a 3.17(3) . '3 766' ? C14 H123a 3.53(2) . '2 655' ? C14 H15 2.11(3) . . ? C14 H16a 2.85(3) . . ? C14 H16b 3.37(3) . . ? C14 H16c 2.94(3) . . ? C14 H24 3.28(3) . '2 755' ? C14 H34 3.71(3) . '2 655' ? C14 H35 3.68(2) . . ? C14 H36a 3.68(3) . '2 655' ? C14 H36c 3.06(3) . '2 655' ? C14 H46a 3.43(4) . '4 565' ? C15 C16 3.678(4) . . ? C15 N21 3.667(3) . . ? C15 N22 4.271(3) . . ? C15 C24 4.428(3) . '2 755' ? C15 C26 4.002(4) . '2 755' ? C15 N31 3.583(3) . . ? C15 C35 3.766(3) . . ? C15 N41 2.979(3) . . ? C15 N42 3.134(3) . . ? C15 C43 4.083(3) . . ? C15 C45 3.906(3) . . ? C15 H113a 3.96(2) . '3 766' ? C15 H114a 3.32(2) . '3 766' ? C15 H114b 3.71(3) . '3 766' ? C15 H123a 3.03(2) . '2 655' ? C15 H123b 3.74(2) . '2 655' ? C15 H14 2.04(3) . . ? C15 H16c 4.03(3) . . ? C15 H24 3.77(2) . '2 755' ? C15 H26a 3.56(3) . '2 755' ? C15 H26b 3.68(3) . '2 755' ? C15 H35 3.20(3) . . ? C15 H36c 3.71(3) . '2 655' ? C16 C26 4.439(3) . '3 766' ? C16 C36 3.995(4) . '2 655' ? C16 C46 3.702(4) . '4 565' ? C16 H111 3.53(2) . . ? C16 H112a 3.28(2) . '3 766' ? C16 H112b 3.11(2) . . ? C16 H112b 3.92(2) . '3 766' ? C16 H113a 3.20(3) . '3 766' ? C16 H113b 3.60(2) . . ? C16 H114a 4.01(3) . '3 766' ? C16 H123b 3.90(3) . '3 666' ? C16 H124a 3.48(3) . '3 666' ? C16 H124b 3.17(3) . '3 666' ? C16 H126a 3.57(2) . . ? C16 H126b 3.18(2) . . ? C16 H14 2.94(3) . . ? C16 H26c 3.82(2) . '3 766' ? C16 H36a 3.38(3) . '2 655' ? C16 H36c 3.69(2) . '2 655' ? C16 H46a 3.21(4) . '4 565' ? C16 H46b 3.45(3) . '4 565' ? N21 C23 2.177(2) . . ? N21 C24 2.201(3) . . ? N21 C26 3.614(3) . . ? N21 N31 2.517(2) . . ? N21 N32 2.916(2) . . ? N21 C33 4.204(3) . . ? N21 C35 3.794(3) . . ? N21 N41 2.512(2) . . ? N21 N42 3.081(2) . . ? N21 C43 4.269(3) . . ? N21 C45 3.637(3) . . ? N21 H113a 3.74(2) . '3 766' ? N21 H114b 3.46(3) . '3 766' ? N21 H115a 3.40(2) . '4 554' ? N21 H116b 3.52(2) . '4 554' ? N21 H15 3.95(2) . . ? N21 H24 3.10(3) . . ? N21 H25 2.01(3) . . ? N21 H26c 3.90(2) . . ? N21 H45 3.94(2) . . ? N22 C24 2.234(3) . . ? N22 C25 2.224(3) . . ? N22 C26 2.482(3) . . ? N22 N31 3.063(2) . . ? N22 N32 3.326(2) . . ? N22 C35 4.189(3) . . ? N22 N41 3.799(2) . . ? N22 H113a 3.05(2) . '3 766' ? N22 H113b 3.57(2) . '3 766' ? N22 H114b 3.57(3) . '3 766' ? N22 H115a 3.22(2) . '4 554' ? N22 H132b 3.72(2) . . ? N22 H136a 3.53(3) . . ? N22 H24 3.10(3) . . ? N22 H25 3.11(3) . . ? N22 H26a 3.01(3) . . ? N22 H26b 3.16(2) . . ? N22 H26c 2.60(2) . . ? C23 C25 2.208(3) . . ? C23 N31 4.265(3) . . ? C23 N32 4.278(3) . . ? C23 H113a 3.48(2) . '3 766' ? C23 H113b 3.41(2) . '3 766' ? C23 H114a 3.47(3) . '4 554' ? C23 H114b 3.70(3) . '3 766' ? C23 H115a 3.19(2) . '4 554' ? C23 H116b 4.00(2) . '4 554' ? C23 H136a 3.48(3) . . ? C23 H24 2.05(3) . . ? C23 H25 3.13(2) . . ? C23 H26a 2.06(3) . . ? C23 H26b 2.05(2) . . ? C23 H26c 2.04(3) . . ? C24 C26 2.602(4) . . ? C24 N41 4.304(3) . . ? C24 N42 4.407(3) . . ? C24 H114a 3.13(3) . '4 554' ? C24 H114b 3.71(3) . '3 766' ? C24 H115a 3.36(2) . '4 554' ? C24 H116b 3.31(2) . '4 554' ? C24 H134a 3.74(3) . '2 755' ? C24 H134b 3.12(3) . '2 755' ? C24 H14 3.59(3) . '2 745' ? C24 H25 2.10(2) . . ? C24 H26a 3.01(3) . . ? C24 H26b 2.84(2) . . ? C24 H26c 3.33(3) . . ? C24 H46c 3.84(4) . '3 765' ? C25 C26 3.670(3) . . ? C25 N31 3.657(3) . . ? C25 N32 3.777(3) . . ? C25 N41 2.969(3) . . ? C25 N42 3.108(3) . . ? C25 C43 4.161(3) . . ? C25 C45 4.007(3) . . ? C25 H114a 3.86(3) . '4 554' ? C25 H114b 3.56(3) . '3 766' ? C25 H115a 3.49(2) . '4 554' ? C25 H116a 3.97(2) . '4 554' ? C25 H116b 2.97(2) . '4 554' ? C25 H134a 3.64(3) . '2 755' ? C25 H134b 3.31(3) . '2 755' ? C25 H135a 3.56(3) . '2 755' ? C25 H135b 3.75(2) . '4 554' ? C25 H136b 3.80(3) . '4 554' ? C25 H24 2.08(3) . . ? C25 H26b 4.03(2) . . ? C25 H46c 3.96(4) . '3 765' ? C26 N42 3.937(3) . '2 745' ? C26 C43 4.303(3) . '2 745' ? C26 C46 3.934(4) . '2 745' ? C26 H113a 3.75(2) . '3 766' ? C26 H113b 3.34(2) . '3 766' ? C26 H114a 3.77(2) . '4 554' ? C26 H114b 4.03(3) . '4 554' ? C26 H115a 3.82(2) . '4 554' ? C26 H123a 3.99(2) . '1 655' ? C26 H123b 3.93(2) . '1 655' ? C26 H124a 3.43(3) . '1 655' ? C26 H136a 2.77(3) . . ? C26 H136b 3.87(3) . . ? C26 H15 3.47(3) . '2 745' ? C26 H16c 3.85(3) . '3 766' ? C26 H24 2.85(3) . . ? C26 H46b 3.07(3) . '2 745' ? N31 C33 2.159(3) . . ? N31 C34 2.211(3) . . ? N31 C36 3.591(3) . . ? N31 N41 2.510(3) . . ? N31 N42 3.812(3) . . ? N31 C44 4.257(3) . . ? N31 C45 2.909(3) . . ? N31 H115a 3.93(2) . '4 554' ? N31 H116a 3.89(2) . '4 554' ? N31 H121 3.80(2) . . ? N31 H126b 3.89(3) . . ? N31 H132b 3.85(2) . . ? N31 H15 3.89(2) . . ? N31 H25 3.96(3) . . ? N31 H34 3.13(3) . . ? N31 H35 2.03(3) . . ? N31 H36b 3.84(3) . . ? N31 H44 3.73(2) . '3 665' ? N31 H45 2.62(2) . . ? N32 C34 2.263(3) . . ? N32 C35 2.240(3) . . ? N32 C36 2.459(3) . . ? N32 N41 3.275(3) . . ? N32 C45 3.417(3) . . ? N32 H115a 2.93(2) . '4 554' ? N32 H115b 3.70(2) . '4 554' ? N32 H116a 2.73(3) . '4 554' ? N32 H116b 3.53(3) . '4 554' ? N32 H121 3.90(3) . . ? N32 H122b 3.78(2) . '4 554' ? N32 H132a 3.83(2) . . ? N32 H132b 3.13(2) . . ? N32 H34 3.17(3) . . ? N32 H35 3.15(3) . . ? N32 H36a 2.98(3) . . ? N32 H36b 2.54(3) . . ? N32 H36c 3.14(3) . . ? N32 H44 3.80(2) . '3 665' ? N32 H45 2.98(3) . . ? C33 C35 2.201(3) . . ? C33 N41 4.280(3) . . ? C33 C44 4.104(3) . '3 665' ? C33 C45 4.134(4) . . ? C33 H115a 3.75(2) . '4 554' ? C33 H116a 3.38(3) . '4 554' ? C33 H121 3.39(2) . . ? C33 H122b 3.70(3) . '4 554' ? C33 H132a 3.34(2) . . ? C33 H132b 3.20(2) . . ? C33 H34 2.12(3) . . ? C33 H35 3.17(3) . . ? C33 H36a 2.01(3) . . ? C33 H36b 2.02(3) . . ? C33 H36c 2.04(3) . . ? C33 H44 3.31(2) . '3 665' ? C33 H45 3.45(3) . . ? C33 H46a 4.00(3) . '3 665' ? C34 C36 2.619(4) . . ? C34 N41 4.369(3) . . ? C34 C44 3.735(3) . '3 665' ? C34 C45 4.194(4) . . ? C34 H121 2.96(2) . . ? C34 H125a 3.23(3) . . ? C34 H126b 3.62(2) . . ? C34 H132a 3.81(2) . . ? C34 H132b 3.99(2) . . ? C34 H133a 3.54(2) . '2 655' ? C34 H133b 3.27(2) . '2 655' ? C34 H14 3.78(3) . '2 645' ? C34 H35 2.14(3) . . ? C34 H36a 2.94(3) . . ? C34 H36b 3.33(3) . . ? C34 H36c 2.82(3) . . ? C34 H44 2.87(3) . '3 665' ? C34 H45 3.48(3) . . ? C34 H46a 3.69(3) . '3 665' ? C35 C36 3.669(3) . . ? C35 N41 3.365(3) . . ? C35 C44 4.085(3) . '3 665' ? C35 C45 3.463(4) . . ? C35 H121 3.27(2) . . ? C35 H125a 3.46(3) . . ? C35 H126b 3.15(2) . . ? C35 H133a 3.44(2) . '2 655' ? C35 H133b 3.25(2) . '2 655' ? C35 H34 2.08(3) . . ? C35 H36a 4.04(3) . . ? C35 H36c 4.01(3) . . ? C35 H44 3.18(2) . '3 665' ? C35 H45 2.97(3) . . ? C36 H115a 3.81(2) . '4 554' ? C36 H115b 3.57(2) . '4 554' ? C36 H116a 3.27(3) . '4 554' ? C36 H122b 3.10(3) . '4 554' ? C36 H123b 3.89(2) . '4 554' ? C36 H124b 3.76(2) . '4 554' ? C36 H125b 3.28(3) . '2 645' ? C36 H126b 3.89(2) . '2 645' ? C36 H132a 3.23(2) . . ? C36 H132b 3.30(2) . . ? C36 H133a 3.56(2) . . ? C36 H14 3.71(3) . '2 645' ? C36 H16a 3.29(3) . '2 645' ? C36 H34 2.95(3) . . ? C36 H44 4.02(3) . '3 665' ? C36 H46a 3.84(3) . '3 665' ? N41 C43 2.152(3) . . ? N41 C44 2.197(3) . . ? N41 C46 3.590(4) . . ? N41 H123b 3.92(3) . '2 655' ? N41 H135b 3.63(3) . '4 554' ? N41 H15 2.69(3) . . ? N41 H25 2.70(2) . . ? N41 H35 3.50(3) . . ? N41 H44 3.07(3) . . ? N41 H45 1.99(2) . . ? N41 H46b 3.88(3) . . ? N42 C44 2.246(3) . . ? N42 C45 2.231(3) . . ? N42 C46 2.461(4) . . ? N42 H123b 3.49(3) . '2 655' ? N42 H135a 3.13(3) . '2 755' ? N42 H135b 3.23(2) . '4 554' ? N42 H15 2.60(3) . . ? N42 H25 2.60(2) . . ? N42 H26a 3.21(3) . '2 755' ? N42 H26b 3.86(2) . '2 755' ? N42 H44 3.13(2) . . ? N42 H45 3.10(3) . . ? N42 H46a 3.15(4) . . ? N42 H46b 2.58(3) . . ? N42 H46c 2.93(4) . . ? C43 C45 2.190(4) . . ? C43 H123b 3.05(3) . '2 655' ? C43 H133b 3.60(2) . '4 554' ? C43 H134b 3.95(3) . '4 554' ? C43 H135a 3.45(3) . '2 755' ? C43 H135b 2.88(2) . '4 554' ? C43 H15 3.36(3) . . ? C43 H25 3.47(2) . . ? C43 H26a 3.78(3) . '2 755' ? C43 H44 2.09(2) . . ? C43 H45 3.09(3) . . ? C43 H46a 1.97(4) . . ? C43 H46b 2.04(3) . . ? C43 H46c 2.09(4) . . ? C44 C44 4.394(4) . '3 665' ? C44 C45 3.809(4) . '3 665' ? C44 C46 2.596(4) . . ? C44 H122a 3.98(3) . '2 655' ? C44 H123b 3.29(3) . '2 655' ? C44 H131 3.90(2) . '4 554' ? C44 H133b 2.96(2) . '4 554' ? C44 H135b 3.16(2) . '4 554' ? C44 H15 3.86(2) . . ? C44 H25 4.03(2) . . ? C44 H34 3.74(3) . '3 665' ? C44 H45 2.08(3) . . ? C44 H45 3.00(3) . '3 665' ? C44 H46a 2.65(4) . . ? C44 H46b 3.32(3) . . ? C44 H46c 3.09(4) . . ? C45 C45 3.671(3) . '3 665' ? C45 C46 3.660(4) . . ? C45 H123b 3.83(3) . '2 655' ? C45 H131 3.74(2) . '4 554' ? C45 H133b 3.75(2) . '4 554' ? C45 H135b 3.60(3) . '4 554' ? C45 H15 3.49(2) . . ? C45 H25 3.60(2) . . ? C45 H35 3.68(3) . . ? C45 H44 3.34(3) . '3 665' ? C45 H44 2.03(3) . . ? C45 H45 3.09(2) . '3 665' ? C45 H46a 3.90(4) . . ? C46 H123b 3.34(3) . '2 655' ? C46 H133b 3.93(2) . '4 554' ? C46 H134b 3.48(3) . '4 554' ? C46 H135a 3.15(2) . '2 755' ? C46 H135b 3.22(2) . '4 554' ? C46 H136a 3.76(2) . '2 755' ? C46 H136b 3.41(2) . '2 755' ? C46 H14 3.50(3) . '4 564' ? C46 H16a 3.28(3) . '4 564' ? C46 H16c 3.39(3) . '4 564' ? C46 H24 3.99(3) . '3 765' ? C46 H26a 3.60(3) . '2 755' ? C46 H26b 3.82(2) . '2 755' ? C46 H26c 3.62(2) . '2 755' ? C46 H34 3.96(2) . '3 665' ? C46 H36a 4.00(3) . '3 665' ? C46 H44 2.93(3) . . ? H111 H112a 2.83(3) . . ? H111 H112b 2.35(3) . . ? H111 H113a 3.54(3) . . ? H111 H113b 2.45(3) . . ? H111 H115a 3.53(3) . . ? H111 H115b 2.52(3) . . ? H111 H116a 2.36(3) . . ? H111 H116b 2.82(3) . . ? H111 H121 3.60(3) . . ? H111 H122b 2.91(3) . . ? H111 H124a 3.27(3) . '3 666' ? H111 H124b 3.27(3) . '3 666' ? H111 H125b 3.17(4) . '3 666' ? H111 H126a 2.24(3) . . ? H111 H126b 3.08(3) . . ? H111 H16b 2.59(4) . . ? H112a H112b 1.55(3) . . ? H112a H113a 2.38(3) . . ? H112a H113b 2.79(3) . . ? H112a H114a 2.62(3) . . ? H112a H116a 3.62(4) . . ? H112a H116b 2.55(3) . . ? H112a H136a 3.20(3) . . ? H112a H136b 2.48(3) . . ? H112a H16c 2.47(4) . '3 766' ? H112a H26c 3.17(4) . . ? H112a H46b 3.54(4) . '2 745' ? H112b H112b 2.94(3) . '3 766' ? H112b H113a 2.75(4) . '3 766' ? H112b H113a 2.38(3) . . ? H112b H113b 2.31(3) . . ? H112b H113b 3.58(4) . '3 766' ? H112b H114a 3.61(3) . . ? H112b H116b 3.56(3) . . ? H112b H136b 3.62(3) . . ? H112b H16b 2.49(4) . . ? H112b H16c 3.19(4) . '3 766' ? H112b H16c 2.99(4) . . ? H112b H26c 3.44(4) . . ? H113a H113b 1.54(3) . . ? H113a H114a 2.35(4) . . ? H113a H114b 2.45(4) . . ? H113a H16b 3.33(4) . '3 766' ? H113a H16c 2.87(4) . '3 766' ? H113a H26c 3.32(4) . '3 766' ? H113b H114a 2.79(3) . . ? H113b H114b 2.40(4) . . ? H113b H115a 3.63(3) . . ? H113b H115b 2.66(4) . . ? H113b H124a 2.90(4) . '3 666' ? H113b H16b 3.01(3) . . ? H113b H16c 3.33(4) . . ? H113b H26b 3.08(3) . '3 766' ? H113b H26c 3.07(4) . '3 766' ? H114a H114b 1.53(4) . . ? H114a H115a 2.34(4) . . ? H114a H115b 2.83(4) . . ? H114a H116b 2.67(3) . . ? H114a H14 3.37(4) . '3 766' ? H114a H16c 3.62(4) . '3 766' ? H114a H24 2.95(4) . 4 ? H114a H26a 3.24(4) . 4 ? H114b H115a 2.40(4) . . ? H114b H115b 2.37(3) . . ? H114b H134a 2.46(5) . 4 ? H114b H134b 3.51(5) . 4 ? H114b H26a 3.23(4) . 4 ? H115a H115b 1.56(3) . . ? H115a H116a 2.30(3) . . ? H115a H116b 2.31(3) . . ? H115a H132b 2.81(4) . 4 ? H115a H134a 2.95(4) . 4 ? H115a H26a 3.43(3) . 4 ? H115a H36b 3.10(4) . 4 ? H115b H116a 2.29(3) . . ? H115b H116b 2.83(3) . . ? H115b H124a 3.44(3) . '3 666' ? H115b H125a 3.47(3) . '3 666' ? H115b H125b 2.72(3) . '3 666' ? H115b H132b 3.31(4) . 4 ? H115b H133a 3.09(4) . 4 ? H115b H134a 2.94(3) . 4 ? H115b H36b 2.67(4) . 4 ? H116a H116b 1.58(3) . . ? H116a H122a 3.04(3) . . ? H116a H122b 2.26(3) . . ? H116a H131 2.72(3) . . ? H116a H136b 3.58(4) . . ? H116a H36a 3.43(4) . 4 ? H116a H36b 2.71(4) . 4 ? H116b H131 2.65(3) . . ? H116b H136b 2.37(4) . . ? H116b H24 3.56(3) . 4 ? H116b H25 2.93(3) . 4 ? H121 H122a 2.33(3) . . ? H121 H122b 2.75(4) . . ? H121 H123a 2.57(3) . . ? H121 H123b 3.59(4) . . ? H121 H125a 2.63(3) . . ? H121 H125b 3.61(3) . . ? H121 H126a 2.72(3) . . ? H121 H126b 2.24(3) . . ? H121 H131 3.20(3) . . ? H121 H132a 2.30(3) . . ? H121 H132b 3.04(3) . . ? H121 H34 3.02(3) . . ? H121 H35 3.62(3) . . ? H122a H122b 1.61(3) . . ? H122a H123a 2.33(3) . . ? H122a H123b 2.35(4) . . ? H122a H124b 3.60(4) . . ? H122a H126a 3.60(3) . . ? H122a H131 2.32(3) . . ? H122a H132a 2.52(3) . . ? H122b H123a 2.84(3) . . ? H122b H123b 2.41(3) . . ? H122b H124a 3.55(3) . . ? H122b H124b 2.55(3) . . ? H122b H125b 3.49(3) . '3 666' ? H122b H126a 2.52(3) . . ? H122b H126b 3.55(4) . . ? H122b H131 3.09(4) . . ? H122b H36a 2.62(4) . 4 ? H122b H36b 2.90(4) . 4 ? H123a H123b 1.55(4) . . ? H123a H124a 2.32(4) . . ? H123a H124b 2.81(4) . . ? H123a H125a 2.62(3) . . ? H123a H125b 3.64(3) . . ? H123a H132a 3.56(4) . . ? H123a H14 3.40(3) . '2 645' ? H123a H15 2.36(3) . '2 645' ? H123a H26b 3.12(4) . '1 455' ? H123a H34 3.59(4) . . ? H123b H124a 2.43(4) . . ? H123b H124b 2.41(3) . . ? H123b H15 2.86(3) . '2 645' ? H123b H16a 3.05(4) . '3 666' ? H123b H26b 3.12(3) . '1 455' ? H123b H36a 3.00(4) . 4 ? H123b H44 3.53(4) . '2 645' ? H123b H46a 3.15(5) . '2 645' ? H123b H46b 3.35(4) . '2 645' ? H124a H124b 1.53(3) . . ? H124a H125a 2.25(4) . . ? H124a H125b 2.31(4) . . ? H124a H126a 3.50(4) . . ? H124a H126a 3.40(3) . '3 666' ? H124a H16a 3.03(4) . '3 666' ? H124a H16b 3.10(4) . '3 666' ? H124a H16c 3.61(4) . '3 666' ? H124a H26b 2.54(4) . '1 455' ? H124a H26c 3.58(4) . '1 455' ? H124b H125a 2.82(4) . . ? H124b H125b 3.21(3) . '3 666' ? H124b H125b 2.35(4) . . ? H124b H126a 2.39(3) . '3 666' ? H124b H126a 2.55(4) . . ? H124b H126b 3.27(4) . '3 666' ? H124b H126b 3.56(4) . . ? H124b H16a 2.55(4) . '3 666' ? H124b H16b 2.81(4) . '3 666' ? H124b H36a 3.03(4) . 4 ? H125a H125b 1.56(3) . . ? H125a H126a 2.81(3) . . ? H125a H126b 2.29(3) . . ? H125a H133a 2.66(3) . '2 655' ? H125a H34 2.72(4) . . ? H125a H35 3.27(4) . . ? H125a H36b 3.60(4) . '2 655' ? H125b H126a 2.90(4) . '3 666' ? H125b H126a 2.34(3) . . ? H125b H126b 2.36(3) . . ? H125b H133a 3.13(3) . '2 655' ? H125b H36a 3.38(4) . '2 655' ? H125b H36b 2.59(4) . '2 655' ? H125b H36c 3.44(4) . '2 655' ? H126a H126a 3.20(4) . '3 666' ? H126a H126b 1.57(4) . . ? H126a H16a 3.45(4) . . ? H126a H16b 2.84(4) . . ? H126b H16a 3.21(4) . . ? H126b H16b 2.67(4) . . ? H126b H35 2.85(4) . . ? H126b H36c 3.55(4) . '2 655' ? H131 H132a 2.38(3) . . ? H131 H132b 2.77(3) . . ? H131 H133b 2.69(3) . . ? H131 H135b 2.60(3) . . ? H131 H136a 2.81(4) . . ? H131 H136b 2.38(3) . . ? H132a H132b 1.55(4) . . ? H132a H133a 2.35(3) . . ? H132a H133b 2.39(3) . . ? H132a H35 3.47(3) . '2 645' ? H132a H36b 3.21(4) . . ? H132a H36c 2.71(3) . . ? H132b H133a 2.33(3) . . ? H132b H133b 2.84(3) . . ? H132b H134a 2.64(4) . . ? H132b H134b 3.57(4) . . ? H132b H136a 2.61(3) . . ? H132b H136b 3.63(3) . . ? H132b H36b 2.98(3) . . ? H132b H36c 3.21(3) . . ? H133a H133b 1.57(4) . . ? H133a H134a 2.43(4) . . ? H133a H134b 2.40(3) . . ? H133a H34 3.09(4) . '2 645' ? H133a H35 2.89(4) . '2 645' ? H133a H36b 3.01(4) . . ? H133a H36c 3.22(3) . . ? H133b H134a 2.88(4) . . ? H133b H134b 2.35(4) . . ? H133b H135b 2.58(3) . . ? H133b H34 2.96(3) . '2 645' ? H133b H35 2.92(3) . '2 645' ? H133b H44 2.57(4) . 4 ? H134a H134b 1.51(4) . . ? H134a H135a 2.33(3) . . ? H134a H135b 2.86(4) . . ? H134a H136a 2.56(4) . . ? H134a H136b 3.59(4) . . ? H134a H25 3.54(3) . '2 745' ? H134a H26a 3.32(4) . . ? H134b H135a 2.36(3) . . ? H134b H135b 2.37(4) . . ? H134b H136a 3.56(4) . . ? H134b H24 2.78(4) . '2 745' ? H134b H25 3.17(4) . '2 745' ? H134b H34 3.62(4) . '2 645' ? H134b H46a 3.52(5) . 4 ? H134b H46c 2.70(4) . 4 ? H135a H135a 3.07(3) . '3 756' ? H135a H135b 3.14(3) . '3 756' ? H135a H135b 1.65(4) . . ? H135a H136a 2.38(4) . . ? H135a H136b 2.38(4) . . ? H135a H25 2.90(4) . '2 745' ? H135a H25 3.61(4) . 4 ? H135a H26a 3.51(4) . . ? H135a H46b 2.88(4) . '2 745' ? H135a H46c 2.72(4) . '2 745' ? H135a H46c 3.24(4) . 4 ? H135b H136a 2.89(4) . . ? H135b H136b 2.43(3) . . ? H135b H25 2.84(3) . 4 ? H135b H44 3.50(4) . 4 ? H135b H46c 2.67(4) . 4 ? H136a H136b 1.55(4) . . ? H136a H26a 2.39(4) . . ? H136a H26b 3.55(4) . . ? H136a H26c 2.34(4) . . ? H136a H46b 2.95(4) . '2 745' ? H136b H25 3.22(4) . 4 ? H136b H26a 3.60(4) . . ? H136b H26c 3.20(4) . . ? H136b H46b 2.81(4) . '2 745' ? H136b H46c 3.02(4) . '2 745' ? H14 H15 2.53(4) . . ? H14 H16a 2.98(4) . . ? H14 H16c 3.14(4) . . ? H14 H24 2.71(4) . '2 755' ? H14 H34 3.03(4) . '2 655' ? H14 H36a 3.54(4) . '2 655' ? H14 H36c 3.09(4) . '2 655' ? H14 H46a 2.79(5) . '4 565' ? H14 H46c 3.45(4) . '4 565' ? H15 H26a 3.09(4) . '2 755' ? H15 H26b 3.04(4) . '2 755' ? H15 H35 3.58(4) . . ? H16a H16b 1.45(4) . . ? H16a H16c 1.50(4) . . ? H16a H36a 2.56(4) . '2 655' ? H16a H36c 3.16(3) . '2 655' ? H16a H46a 2.70(5) . '4 565' ? H16a H46b 3.16(4) . '4 565' ? H16b H16c 1.46(4) . . ? H16c H26b 3.62(4) . '3 766' ? H16c H26c 3.13(4) . '3 766' ? H16c H46a 3.10(4) . '4 565' ? H16c H46b 2.97(4) . '4 565' ? H24 H25 2.56(3) . . ? H24 H26a 3.16(4) . . ? H24 H26b 2.85(3) . . ? H24 H46c 3.26(5) . '3 765' ? H25 H46c 3.52(5) . '3 765' ? H26a H26b 1.58(4) . . ? H26a H26c 1.51(4) . . ? H26a H46b 2.79(4) . '2 745' ? H26b H26c 1.47(4) . . ? H26b H46b 3.07(4) . '2 745' ? H26c H46b 2.70(4) . '2 745' ? H34 H35 2.59(4) . . ? H34 H36a 3.14(4) . . ? H34 H36c 2.91(4) . . ? H34 H44 2.97(4) . '3 665' ? H34 H46a 3.22(4) . '3 665' ? H35 H36c 3.38(4) . '2 655' ? H35 H44 3.52(3) . '3 665' ? H35 H45 3.30(4) . . ? H36a H36b 1.55(4) . . ? H36a H36c 1.54(4) . . ? H36a H44 3.62(4) . '3 665' ? H36a H46a 3.17(4) . '3 665' ? H36b H36c 1.52(5) . . ? H44 H45 2.47(4) . '3 665' ? H44 H45 2.47(4) . . ? H44 H46a 2.71(5) . . ? H44 H46c 3.37(4) . . ? H45 H45 2.70(3) . '3 665' ? H46a H46b 1.60(4) . . ? H46a H46c 1.53(5) . . ? H46b H46c 1.50(5) . . ? _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 1448 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 17 _reflns_limit_k_min 0 _reflns_limit_k_max 20 _reflns_limit_l_min -24 _reflns_limit_l_max 24 _reflns_number_observed ? _reflns_d_resolution_high .726 _reflns_d_resolution_low 12.249 _diffrn_reflns_av_sigmaI/netI .063 _diffrn_reflns_theta_min 1.66 _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 .061 _refine_ls_wR_factor_all .048 _refine_ls_goodness_of_fit_all 1.369 _refine_ls_shift/su_mean .001 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end data_cpm55 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C30.5 H31.5 B1 Cl1.5 Cu1 N6 P1' _chemical_formula_moiety ? _chemical_formula_weight 640.64 _chemical_melting_point ? _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M P_-3_c_1 _symmetry_space_group_name_Hall -p_3_2"c loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -y,+x-y,+z +y,+x,1/2-z -x+y,-x,+z -x,-x+y,1/2-z +x-y,-y,1/2-z -x,-y,-z +y,-x+y,-z -y,-x,1/2+z +x-y,+x,-z +x,+x-y,1/2+z -x+y,+y,1/2+z _cell_length_a 12.7200(14) _cell_length_b 12.7200(14) _cell_length_c 22.033(2) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 120.0000 _cell_volume 3087.3(8) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu .92 _exptl_crystal_description prism _exptl_crystal_size_max .23 _exptl_crystal_size_mid .16 _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 .648 _exptl_absorpt_correction_T_max .862 _diffrn_reflns_number 36290 _reflns_number_total 2738 _reflns_Friedel_coverage 0 _reflns_number_gt 2065 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.24 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .061 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _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 .062 _refine_ls_wR_factor_ref .074 _refine_ls_goodness_of_fit_ref 1.683 _refine_ls_number_reflns 2065 _refine_ls_number_parameters 128 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .002 _refine_diff_density_min -1.438 _refine_diff_density_max 1.295 _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 ? 0 122 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 126 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 24 .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' Cu ? 0 4 .263 1.266 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 6 .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 .33333 .66666 .23862(3) .0282(3) Uani ? ? 1.00000 ? ? P .33333 .66666 .14066(5) .0252(5) Uani ? ? 1.00000 ? ? C11 .2612(3) .5157(3) .10518(13) .0290(12) Uani ? ? 1.00000 ? ? C12 .2889(3) .4276(3) .12486(14) .0330(15) Uani ? ? 1.00000 ? ? C121 .3855(4) .4520(4) .17072(16) .0400(17) Uani ? ? 1.00000 ? ? C13 .2255(4) .3118(4) .09847(17) .0407(17) Uani ? ? 1.00000 ? ? C14 .1393(4) .2848(4) .05352(17) .0442(17) Uani ? ? 1.00000 ? ? C15 .1149(4) .3716(4) .03352(16) .0430(17) Uani ? ? 1.00000 ? ? C16 .1750(3) .4871(3) .05876(14) .0348(15) Uani ? ? 1.00000 ? ? N1 .2406(3) .5396(3) .35400(12) .0350(13) Uani ? ? 1.00000 ? ? N2 .2281(3) .5168(3) .29258(12) .0336(13) Uani ? ? 1.00000 ? ? C3 .1412(3) .4029(4) .28633(16) .0371(16) Uani ? ? 1.00000 ? ? C4 .0961(4) .3498(4) .34306(18) .0429(18) Uani ? ? 1.00000 ? ? C5 .1610(4) .4391(4) .38376(16) .0397(17) Uani ? ? 1.00000 ? ? B .33333 .66666 .3777(3) .036(2) Uani ? ? 1.00000 ? ? Cl1 .00001 1.00001 .1508(3) .083(3) Uani ? ? .50000 ? ? Cl2 .00001 .8798(5) .25000 .193(6) Uani ? ? .66667 ? ? C0 .00002 1.00001 .223(2) .177(18) Uiso ? ? .50000 ? ? H121a .37112 .48185 .20736 .07028 Uiso ? ? 1.00000 ? ? H121b .38672 .38051 .17798 .06368 Uiso ? ? 1.00000 ? ? H121c .46349 .51212 .15531 .06506 Uiso ? ? 1.00000 ? ? H13 .24566 .25292 .11229 .04970 Uiso ? ? 1.00000 ? ? H14 .09353 .20198 .03884 .05030 Uiso ? ? 1.00000 ? ? H15 .05666 .35330 .00298 .06166 Uiso ? ? 1.00000 ? ? H16 .15730 .54784 .04551 .03556 Uiso ? ? 1.00000 ? ? H3 .11156 .36090 .24893 .04427 Uiso ? ? 1.00000 ? ? H4 .03471 .26909 .35110 .04764 Uiso ? ? 1.00000 ? ? H5 .15005 .43254 .42690 .04869 Uiso ? ? 1.00000 ? ? H0 -.00367 .94457 .24017 .09116 Uiso ? ? .16667 ? ? H .33333 .66666 .42741 .04500 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 .0365(3) .0365(3) .0116(3) .01824(14) .00000 .00000 P .0319(4) .0319(4) .0117(6) .0160(2) .00000 .00000 C11 .0317(17) .0353(17) .0164(12) .0140(16) .0031(13) -.0025(11) C12 .0363(19) .041(2) .0208(15) .0188(17) .0080(13) .0009(13) C121 .052(2) .048(2) .0287(17) .032(2) .0010(16) .0031(16) C13 .048(2) .036(2) .0368(19) .0202(18) .0129(17) .0001(16) C14 .042(2) .041(2) .0380(19) .013(2) .0088(18) -.0141(16) C15 .039(2) .057(2) .0252(16) .018(2) -.0006(15) -.0130(17) C16 .038(2) .044(2) .0193(15) .0183(17) .0009(13) -.0055(14) N1 .0476(18) .0433(18) .0139(12) .0226(15) .0013(11) .0041(12) N2 .0426(17) .0401(17) .0149(12) .0181(14) -.0004(11) .0021(11) C3 .038(2) .043(2) .0279(17) .0180(17) .0005(15) .0025(15) C4 .040(2) .046(2) .038(2) .0177(19) .0086(17) .0132(17) C5 .045(2) .054(2) .0240(16) .027(2) .0086(15) .0150(16) B .048(2) .048(2) .012(2) .0239(12) .00000 .00000 Cl1 .082(2) .082(2) .085(4) .0411(11) .00000 .00000 Cl2 .288(10) .149(3) .190(6) .144(5) -.053(6) -.027(3) # 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 P . . 2.1584(14) ? Cu N2 . . 2.070(3) ? Cu N2 . '2 665' 2.070(3) ? Cu N2 . '4 565' 2.070(3) ? P C11 . . 1.838(3) ? P C11 . '2 665' 1.838(3) ? P C11 . '4 565' 1.838(3) ? C11 C12 . . 1.401(5) ? C11 C16 . . 1.408(5) ? C12 C121 . . 1.498(5) ? C12 C13 . . 1.403(5) ? C121 H121a . . .948(4) ? C121 H121b . . .931(4) ? C121 H121c . . .962(4) ? C13 C14 . . 1.388(6) ? C13 H13 . . .955(4) ? C14 C15 . . 1.360(6) ? C14 H14 . . .970(4) ? C15 C16 . . 1.389(6) ? C15 H15 . . .940(4) ? C16 H16 . . .952(4) ? N1 N2 . . 1.376(4) ? N1 C5 . . 1.339(5) ? N1 B . . 1.539(4) ? N2 C3 . . 1.319(5) ? C3 C4 . . 1.400(5) ? C3 H3 . . .951(4) ? C4 C5 . . 1.356(6) ? C4 H4 . . .946(4) ? C5 H5 . . .958(3) ? B H . . 1.096(6) ? Cl1 C0 . . 1.58(4) ? Cl2 C0 . . 1.643(16) ? Cl2 H0 . . .876(6) ? Cl2 C0 . '3 465' 1.644(16) ? Cl2 H0 . 5 .876(6) ? C0 H0 . . .78(2) ? C0 H0 . '2 675' .78(2) ? C0 C0 . '3 465' 1.20(6) ? C0 H0 . '3 465' 1.07(3) ? C0 H0 . '4 465' .78(2) ? C0 H0 . 5 1.07(3) ? C0 H0 . '6 675' 1.07(3) ? H0 H0 . 5 .44076(5) ? 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 P Cu N2 . . . 125.05(7) ? P Cu N2 . . '2 665' 125.05(8) ? P Cu N2 . . '4 565' 125.04(9) ? N2 Cu N2 . . '2 665' 90.31(12) ? N2 Cu N2 . . '4 565' 90.31(13) ? N2 Cu N2 '2 665' . '4 565' 90.31(14) ? Cu P C11 . . . 115.17(10) ? Cu P C11 . . '2 665' 115.17(10) ? Cu P C11 . . '4 565' 115.17(11) ? C11 P C11 . . '2 665' 103.22(16) ? C11 P C11 . . '4 565' 103.22(17) ? C11 P C11 '2 665' . '4 565' 103.22(17) ? P C11 C12 . . . 120.7(2) ? P C11 C16 . . . 119.7(3) ? C12 C11 C16 . . . 119.6(3) ? C11 C12 C121 . . . 123.5(3) ? C11 C12 C13 . . . 117.9(4) ? C121 C12 C13 . . . 118.6(4) ? C12 C121 H121a . . . 110.8(5) ? C12 C121 H121b . . . 109.0(3) ? C12 C121 H121c . . . 109.8(3) ? H121a C121 H121b . . . 110.2(4) ? H121a C121 H121c . . . 108.1(4) ? H121b C121 H121c . . . 108.8(6) ? C12 C13 C14 . . . 121.6(5) ? C12 C13 H13 . . . 116.9(4) ? C14 C13 H13 . . . 121.5(4) ? C13 C14 C15 . . . 120.2(4) ? C13 C14 H14 . . . 118.6(5) ? C15 C14 H14 . . . 121.1(4) ? C14 C15 C16 . . . 120.0(4) ? C14 C15 H15 . . . 120.2(4) ? C16 C15 H15 . . . 119.8(5) ? C11 C16 C15 . . . 120.6(4) ? C11 C16 H16 . . . 118.9(3) ? C15 C16 H16 . . . 120.5(4) ? N2 N1 C5 . . . 109.2(3) ? N2 N1 B . . . 120.1(3) ? C5 N1 B . . . 130.8(3) ? Cu N2 N1 . . . 114.7(2) ? Cu N2 C3 . . . 138.8(2) ? N1 N2 C3 . . . 106.2(3) ? N2 C3 C4 . . . 110.7(3) ? N2 C3 H3 . . . 125.9(3) ? C4 C3 H3 . . . 123.4(3) ? C3 C4 C5 . . . 104.8(3) ? C3 C4 H4 . . . 127.4(4) ? C5 C4 H4 . . . 127.7(4) ? N1 C5 C4 . . . 109.2(3) ? N1 C5 H5 . . . 125.2(4) ? C4 C5 H5 . . . 125.6(4) ? N1 B H . . . 109.8(2) ? N1 B N1 . . '2 665' 109.1(3) ? N1 B N1 . . '4 565' 109.1(3) ? H B N1 . . '2 665' 109.8(2) ? H B N1 . . '4 565' 109.8(2) ? N1 B N1 '2 665' . '4 565' 109.1(3) ? C0 Cl2 H0 . . . 7.6(13) ? C0 Cl2 C0 . . '3 465' 43(2) ? C0 Cl2 H0 . . 5 35.9(14) ? H0 Cl2 C0 . . '3 465' 35.9(14) ? H0 Cl2 H0 . . 5 29.1(2) ? C0 Cl2 H0 '3 465' . 5 7.6(13) ? Cl1 C0 Cl2 . . . 111.5(14) ? Cl1 C0 H0 . . . 119(3) ? Cl1 C0 Cl2 . . '2 675' 111.5(14) ? Cl1 C0 H0 . . '2 675' 119(3) ? Cl1 C0 Cl2 . . '3 465' 111.4(14) ? Cl1 C0 C0 . . '3 465' 180.0000 ? Cl1 C0 H0 . . '3 465' 140.1(14) ? Cl1 C0 H0 . . '4 465' 119(3) ? Cl1 C0 H0 . . 5 140.1(14) ? Cl1 C0 H0 . . '6 675' 140.1(14) ? Cl2 C0 H0 . . . 8.5(12) ? Cl2 C0 Cl2 . . '2 675' 107.4(15) ? Cl2 C0 H0 . . '2 675' 101(2) ? Cl2 C0 Cl2 . . '3 465' 107.4(15) ? Cl2 C0 C0 . . '3 465' 68.6(14) ? Cl2 C0 H0 . . '3 465' 89(2) ? Cl2 C0 H0 . . '4 465' 105(2) ? Cl2 C0 H0 . . 5 28.80(11) ? Cl2 C0 H0 . . '6 675' 93(2) ? H0 C0 Cl2 . . '2 675' 106(2) ? H0 C0 H0 . . '2 675' 98(3) ? H0 C0 Cl2 . . '3 465' 101(2) ? H0 C0 C0 . . '3 465' 61(3) ? H0 C0 H0 . . '3 465' 81(3) ? H0 C0 H0 . . '4 465' 98(3) ? H0 C0 H0 . . 5 21.4(12) ? H0 C0 H0 . . '6 675' 88(3) ? Cl2 C0 H0 '2 675' . '2 675' 8.5(12) ? Cl2 C0 Cl2 '2 675' . '3 465' 107.4(15) ? Cl2 C0 C0 '2 675' . '3 465' 68.5(14) ? Cl2 C0 H0 '2 675' . '3 465' 93(2) ? Cl2 C0 H0 '2 675' . '4 465' 101(2) ? Cl2 C0 H0 '2 675' . 5 89(2) ? Cl2 C0 H0 '2 675' . '6 675' 28.81(10) ? H0 C0 Cl2 '2 675' . '3 465' 105(2) ? H0 C0 C0 '2 675' . '3 465' 61(3) ? H0 C0 H0 '2 675' . '3 465' 88(3) ? H0 C0 H0 '2 675' . '4 465' 98(3) ? H0 C0 H0 '2 675' . 5 81(3) ? H0 C0 H0 '2 675' . '6 675' 21.4(12) ? Cl2 C0 C0 '3 465' . '3 465' 68.5(14) ? Cl2 C0 H0 '3 465' . '3 465' 28.80(11) ? Cl2 C0 H0 '3 465' . '4 465' 8.5(12) ? Cl2 C0 H0 '3 465' . 5 93(2) ? Cl2 C0 H0 '3 465' . '6 675' 89(2) ? C0 C0 H0 '3 465' . '3 465' 39.9(14) ? C0 C0 H0 '3 465' . '4 465' 61(3) ? C0 C0 H0 '3 465' . 5 39.9(14) ? C0 C0 H0 '3 465' . '6 675' 39.9(14) ? H0 C0 H0 '3 465' . '4 465' 21.4(12) ? H0 C0 H0 '3 465' . 5 67(2) ? H0 C0 H0 '3 465' . '6 675' 67(2) ? H0 C0 H0 '4 465' . 5 88(3) ? H0 C0 H0 '4 465' . '6 675' 81(3) ? H0 C0 H0 5 . '6 675' 67(2) ? Cl2 H0 C0 . . . 164(2) ? Cl2 H0 C0 . . '3 465' 115.3(14) ? Cl2 H0 H0 . . 5 75.43(11) ? C0 H0 C0 . . '3 465' 80(3) ? C0 H0 H0 . . 5 118(3) ? C0 H0 H0 '3 465' . 5 40.4(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 ? ? ? ? ? ? _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 1324 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 30 _reflns_number_observed ? _reflns_d_resolution_high .728 _reflns_d_resolution_low 10.992 _diffrn_reflns_av_sigmaI/netI .05 _diffrn_reflns_theta_min 1.85 _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 .085 _refine_ls_wR_factor_all .078 _refine_ls_goodness_of_fit_all 1.534 _refine_ls_shift/su_mean . #========================================================================== # 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 data_cpm47l # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C22 H23 B1 Cu1 N6 P1' _chemical_formula_moiety ? _chemical_formula_weight 476.8 _chemical_melting_point ? _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P_b_c_a _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 -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 11.3840(10) _cell_length_b 19.052(2) _cell_length_c 20.467(2) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 4439.0(7) _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu 1.08 _exptl_crystal_description prism _exptl_crystal_size_max .42 _exptl_crystal_size_mid .22 _exptl_crystal_size_min .2 _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 .719 _exptl_absorpt_correction_T_max .856 _diffrn_reflns_number 51559 _reflns_number_total 5747 _reflns_Friedel_coverage 0 _reflns_number_gt 4785 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.16 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .025 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _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 .04 _refine_ls_goodness_of_fit_ref 1.534 _refine_ls_number_reflns 4785 _refine_ls_number_parameters 280 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .011 _refine_diff_density_min -.357 _refine_diff_density_max .631 _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 GENTAN' _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 Cu ? 0 8 .263 1.266 'Int Tables Vol IV Tables 2.2B and 2.3.1' C ? 0 176 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 184 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 48 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 8 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' B ? 0 8 0 .001 '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 .645367(17) .125316(10) .031607(9) .02104(11) Uani ? ? 1.00000 ? ? P .62748(3) .15614(2) -.068808(18) .0190(2) Uani ? ? 1.00000 ? ? C111 .57227(13) .24497(8) -.08161(7) .0206(7) Uani ? ? 1.00000 ? ? C112 .56176(14) .27318(9) -.14425(7) .0254(8) Uani ? ? 1.00000 ? ? C113 .51949(14) .34064(9) -.15322(8) .0296(9) Uani ? ? 1.00000 ? ? C114 .48608(15) .38088(9) -.09975(9) .0326(9) Uani ? ? 1.00000 ? ? C115 .49509(16) .35331(10) -.03746(9) .0332(9) Uani ? ? 1.00000 ? ? C116 .53818(15) .28544(9) -.02826(7) .0266(8) Uani ? ? 1.00000 ? ? C121 .75991(13) .15581(8) -.11978(7) .0200(7) Uani ? ? 1.00000 ? ? C122 .79236(15) .09712(8) -.15652(8) .0286(8) Uani ? ? 1.00000 ? ? C123 .89712(16) .09689(9) -.19141(9) .0326(9) Uani ? ? 1.00000 ? ? C124 .97012(14) .15448(9) -.19071(8) .0277(8) Uani ? ? 1.00000 ? ? C125 .93919(15) .21343(9) -.15443(8) .0284(8) Uani ? ? 1.00000 ? ? C126 .83540(14) .21349(8) -.11915(8) .0255(8) Uani ? ? 1.00000 ? ? C131 .52309(15) .10278(9) -.11520(8) .0276(8) Uani ? ? 1.00000 ? ? N11 .70041(11) .15472(6) .16803(6) .0195(6) Uani ? ? 1.00000 ? ? N12 .70697(11) .18586(7) .10799(6) .0208(6) Uani ? ? 1.00000 ? ? C13 .75040(14) .24991(8) .11832(8) .0239(8) Uani ? ? 1.00000 ? ? C14 .77167(14) .26132(8) .18462(8) .0263(8) Uani ? ? 1.00000 ? ? C15 .73942(13) .19970(8) .21442(7) .0233(8) Uani ? ? 1.00000 ? ? N21 .51806(11) .08327(6) .15069(6) .0208(6) Uani ? ? 1.00000 ? ? N22 .49535(11) .10134(7) .08694(6) .0231(7) Uani ? ? 1.00000 ? ? C23 .37890(14) .10137(9) .08105(8) .0264(8) Uani ? ? 1.00000 ? ? C24 .32457(14) .08380(9) .13997(9) .0291(9) Uani ? ? 1.00000 ? ? C25 .41577(14) .07301(8) .18285(8) .0252(8) Uani ? ? 1.00000 ? ? N31 .71688(11) .02788(6) .13306(6) .0198(6) Uani ? ? 1.00000 ? ? N32 .72709(11) .03727(6) .06705(6) .0211(6) Uani ? ? 1.00000 ? ? C33 .79228(14) -.01591(8) .04519(7) .0245(8) Uani ? ? 1.00000 ? ? C34 .82500(14) -.06044(8) .09624(8) .0272(8) Uani ? ? 1.00000 ? ? C35 .77523(14) -.03087(8) .15102(7) .0250(8) Uani ? ? 1.00000 ? ? B .64651(15) .08058(9) .17503(8) .0205(8) Uani ? ? 1.00000 ? ? H112 .58311 .24488 -.18145 .03200 Uiso ? ? 1.00000 ? ? H113 .51451 .36024 -.19635 .03700 Uiso ? ? 1.00000 ? ? H114 .45666 .42765 -.10617 .04000 Uiso ? ? 1.00000 ? ? H115 .47126 .38025 .00001 .04300 Uiso ? ? 1.00000 ? ? H116 .54351 .26668 .01493 .03300 Uiso ? ? 1.00000 ? ? H122 .74218 .05661 -.15706 .03600 Uiso ? ? 1.00000 ? ? H123 .91886 .05615 -.21638 .04000 Uiso ? ? 1.00000 ? ? H124 1.04210 .15328 -.21470 .03400 Uiso ? ? 1.00000 ? ? H125 .98960 .25388 -.15517 .03500 Uiso ? ? 1.00000 ? ? H126 .81512 .25351 -.09316 .03200 Uiso ? ? 1.00000 ? ? H131a .54402 .05434 -.11251 .04300 Uiso ? ? 1.00000 ? ? H131b .52479 .11630 -.16049 .04300 Uiso ? ? 1.00000 ? ? H131c .44590 .10898 -.09907 .04300 Uiso ? ? 1.00000 ? ? H13 .76462 .28362 .08470 .03000 Uiso ? ? 1.00000 ? ? H14 .80247 .30264 .20440 .03300 Uiso ? ? 1.00000 ? ? H15 .74369 .18978 .26006 .03000 Uiso ? ? 1.00000 ? ? H23 .33754 .11275 .04178 .03300 Uiso ? ? 1.00000 ? ? H24 .24213 .08041 .14851 .03500 Uiso ? ? 1.00000 ? ? H25 .40782 .06035 .22783 .03100 Uiso ? ? 1.00000 ? ? H33 .81288 -.02279 .00021 .03000 Uiso ? ? 1.00000 ? ? H34 .87257 -.10186 .09408 .03400 Uiso ? ? 1.00000 ? ? H35 .78173 -.04869 .19462 .03100 Uiso ? ? 1.00000 ? ? H .64993 .06606 .22135 .02600 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 .02577(12) .02055(11) .01679(11) .00102(7) -.00138(7) .00266(7) P .0226(2) .0177(2) .01683(18) -.00078(14) -.00145(14) .00121(14) C111 .0180(7) .0196(7) .0242(7) -.0012(6) -.0019(5) .0021(6) C112 .0244(8) .0270(8) .0248(8) .0000(6) -.0004(6) .0046(6) C113 .0224(8) .0309(9) .0356(9) .0015(7) -.0006(7) .0136(7) C114 .0213(8) .0242(8) .0522(11) .0039(6) .0002(7) .0049(7) C115 .0310(10) .0284(9) .0402(10) .0086(7) -.0009(7) -.0062(7) C116 .0273(9) .0265(8) .0260(8) .0044(7) -.0031(6) -.0004(6) C121 .0229(7) .0195(7) .0177(7) .0006(6) -.0030(5) .0018(6) C122 .0302(9) .0210(8) .0345(9) -.0033(7) .0024(7) -.0039(7) C123 .0310(9) .0308(9) .0359(9) .0042(7) .0046(7) -.0085(7) C124 .0228(8) .0358(9) .0246(8) .0034(7) -.0004(6) .0025(7) C125 .0242(8) .0277(8) .0331(9) -.0047(6) -.0028(6) .0037(7) C126 .0268(8) .0210(8) .0289(8) -.0008(6) -.0014(6) -.0034(6) C131 .0276(9) .0258(8) .0295(8) -.0055(7) -.0022(6) -.0024(7) N11 .0214(6) .0198(6) .0174(6) -.0005(5) -.0003(5) -.0005(5) N12 .0225(7) .0200(6) .0199(6) -.0007(5) .0000(5) .0030(5) C13 .0221(8) .0200(7) .0297(8) -.0001(6) -.0003(6) .0011(6) C14 .0232(8) .0216(8) .0343(8) -.0006(6) -.0033(6) -.0067(7) C15 .0207(8) .0265(8) .0228(7) .0003(6) -.0012(6) -.0044(6) N21 .0223(6) .0192(6) .0210(6) -.0032(5) .0011(5) -.0008(5) N22 .0233(7) .0242(7) .0217(6) -.0013(5) -.0025(5) .0006(5) C23 .0240(8) .0224(8) .0328(9) .0005(6) -.0041(6) -.0031(7) C24 .0200(8) .0243(8) .0431(10) -.0025(6) .0044(7) -.0078(7) C25 .0260(8) .0210(8) .0286(8) -.0035(6) .0081(6) -.0059(6) N31 .0220(6) .0190(6) .0183(6) -.0005(5) -.0020(5) .0022(5) N32 .0246(7) .0205(6) .0183(6) .0005(5) -.0016(5) -.0004(5) C33 .0256(8) .0218(8) .0262(8) -.0009(6) .0000(6) -.0047(6) C34 .0274(8) .0192(8) .0350(9) .0039(6) -.0039(7) -.0008(7) C35 .0265(8) .0204(8) .0282(8) .0002(6) -.0053(6) .0052(6) B .0242(8) .0196(8) .0177(8) -.0011(7) .0000(6) .0009(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 P . . 2.1472(5) ? Cu N12 . . 2.0654(12) ? Cu N22 . . 2.0995(13) ? Cu N32 . . 2.0506(13) ? P C111 . . 1.8242(15) ? P C121 . . 1.8333(15) ? P C131 . . 1.8296(17) ? C111 C112 . . 1.395(2) ? C111 C116 . . 1.392(2) ? C112 C113 . . 1.385(2) ? C112 H112 . . .9641(15) ? C113 C114 . . 1.389(3) ? C113 H113 . . .9601(17) ? C114 C115 . . 1.383(3) ? C114 H114 . . .9610(17) ? C115 C116 . . 1.396(2) ? C115 H115 . . .9619(18) ? C116 H116 . . .9554(15) ? C121 C122 . . 1.397(2) ? C121 C126 . . 1.395(2) ? C122 C123 . . 1.390(2) ? C122 H122 . . .9603(16) ? C123 C124 . . 1.376(2) ? C123 H123 . . .9618(18) ? C124 C125 . . 1.392(2) ? C124 H124 . . .9555(16) ? C125 C126 . . 1.385(2) ? C125 H125 . . .9610(17) ? C126 H126 . . .9579(16) ? C131 H131a . . .9547(16) ? C131 H131b . . .9624(16) ? C131 H131c . . .9461(17) ? N11 N12 . . 1.3667(17) ? N11 C15 . . 1.354(2) ? N11 B . . 1.547(2) ? N12 C13 . . 1.333(2) ? C13 C14 . . 1.395(2) ? C13 H13 . . .9551(15) ? C14 C15 . . 1.373(2) ? C14 H14 . . .9521(16) ? C15 H15 . . .9542(14) ? N21 N22 . . 1.3739(17) ? N21 C25 . . 1.352(2) ? N21 B . . 1.546(2) ? N22 C23 . . 1.331(2) ? C23 C24 . . 1.396(2) ? C23 H23 . . .9564(17) ? C24 C25 . . 1.375(2) ? C24 H24 . . .9568(16) ? C25 H25 . . .9559(16) ? N31 N32 . . 1.3678(16) ? N31 C35 . . 1.353(2) ? N31 B . . 1.545(2) ? N32 C33 . . 1.333(2) ? C33 C34 . . 1.396(2) ? C33 H33 . . .9589(15) ? C34 C35 . . 1.377(2) ? C34 H34 . . .9582(16) ? C35 H35 . . .9577(15) ? B H . . .9882(16) ? 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 P Cu N12 . . . 127.15(4) ? P Cu N22 . . . 119.91(4) ? P Cu N32 . . . 127.25(4) ? N12 Cu N22 . . . 89.39(5) ? N12 Cu N32 . . . 92.01(5) ? N22 Cu N32 . . . 90.02(5) ? Cu P C111 . . . 115.09(5) ? Cu P C121 . . . 117.76(5) ? Cu P C131 . . . 113.97(5) ? C111 P C121 . . . 101.82(7) ? C111 P C131 . . . 102.55(7) ? C121 P C131 . . . 103.70(7) ? P C111 C112 . . . 121.26(11) ? P C111 C116 . . . 119.82(11) ? C112 C111 C116 . . . 118.92(14) ? C111 C112 C113 . . . 120.61(14) ? C111 C112 H112 . . . 119.25(15) ? C113 C112 H112 . . . 120.13(15) ? C112 C113 C114 . . . 120.19(15) ? C112 C113 H113 . . . 120.23(16) ? C114 C113 H113 . . . 119.57(17) ? C113 C114 C115 . . . 119.76(16) ? C113 C114 H114 . . . 119.95(18) ? C115 C114 H114 . . . 120.29(18) ? C114 C115 C116 . . . 120.17(16) ? C114 C115 H115 . . . 120.76(18) ? C116 C115 H115 . . . 119.07(17) ? C111 C116 C115 . . . 120.35(14) ? C111 C116 H116 . . . 120.06(16) ? C115 C116 H116 . . . 119.59(16) ? P C121 C122 . . . 121.77(12) ? P C121 C126 . . . 119.90(11) ? C122 C121 C126 . . . 118.20(14) ? C121 C122 C123 . . . 120.39(15) ? C121 C122 H122 . . . 119.48(16) ? C123 C122 H122 . . . 120.13(16) ? C122 C123 C124 . . . 120.68(16) ? C122 C123 H123 . . . 119.76(17) ? C124 C123 H123 . . . 119.56(17) ? C123 C124 C125 . . . 119.74(15) ? C123 C124 H124 . . . 119.57(17) ? C125 C124 H124 . . . 120.69(17) ? C124 C125 C126 . . . 119.66(15) ? C124 C125 H125 . . . 119.20(16) ? C126 C125 H125 . . . 121.13(16) ? C121 C126 C125 . . . 121.34(15) ? C121 C126 H126 . . . 118.93(15) ? C125 C126 H126 . . . 119.73(16) ? P C131 H131a . . . 110.20(13) ? P C131 H131b . . . 109.76(13) ? P C131 H131c . . . 110.66(13) ? H131a C131 H131b . . . 108.01(16) ? H131a C131 H131c . . . 109.42(16) ? H131b C131 H131c . . . 108.74(16) ? N12 N11 C15 . . . 109.75(12) ? N12 N11 B . . . 120.10(11) ? C15 N11 B . . . 130.03(12) ? Cu N12 N11 . . . 114.81(9) ? Cu N12 C13 . . . 139.20(10) ? N11 N12 C13 . . . 105.95(12) ? N12 C13 C14 . . . 111.18(13) ? N12 C13 H13 . . . 124.33(15) ? C14 C13 H13 . . . 124.50(15) ? C13 C14 C15 . . . 104.62(13) ? C13 C14 H14 . . . 127.32(15) ? C15 C14 H14 . . . 128.06(16) ? N11 C15 C14 . . . 108.50(13) ? N11 C15 H15 . . . 125.30(15) ? C14 C15 H15 . . . 126.20(15) ? N22 N21 C25 . . . 109.67(12) ? N22 N21 B . . . 119.50(12) ? C25 N21 B . . . 130.77(13) ? Cu N22 N21 . . . 114.44(9) ? Cu N22 C23 . . . 139.57(11) ? N21 N22 C23 . . . 105.87(12) ? N22 C23 C24 . . . 111.28(14) ? N22 C23 H23 . . . 124.51(16) ? C24 C23 H23 . . . 124.21(16) ? C23 C24 C25 . . . 104.64(14) ? C23 C24 H24 . . . 127.48(17) ? C25 C24 H24 . . . 127.88(18) ? N21 C25 C24 . . . 108.54(14) ? N21 C25 H25 . . . 125.95(15) ? C24 C25 H25 . . . 125.51(16) ? N32 N31 C35 . . . 109.57(12) ? N32 N31 B . . . 120.55(12) ? C35 N31 B . . . 129.88(12) ? Cu N32 N31 . . . 114.70(9) ? Cu N32 C33 . . . 139.07(10) ? N31 N32 C33 . . . 106.22(12) ? N32 C33 C34 . . . 111.04(13) ? N32 C33 H33 . . . 124.21(15) ? C34 C33 H33 . . . 124.75(16) ? C33 C34 C35 . . . 104.54(14) ? C33 C34 H34 . . . 128.07(16) ? C35 C34 H34 . . . 127.38(16) ? N31 C35 C34 . . . 108.62(13) ? N31 C35 H35 . . . 125.77(15) ? C34 C35 H35 . . . 125.60(16) ? N11 B N21 . . . 108.37(12) ? N11 B N31 . . . 109.64(12) ? N11 B H . . . 109.20(14) ? N21 B N31 . . . 109.43(12) ? N21 B H . . . 110.84(14) ? N31 B H . . . 109.34(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 Cu C111 3.3554(15) . . ? Cu C112 4.6687(16) . . ? Cu C114 4.1235(18) . 3 ? Cu C115 4.0039(19) . 3 ? Cu C116 4.7846(17) . 3 ? Cu C116 3.5067(17) . . ? Cu C121 3.4115(14) . . ? Cu C122 4.2325(17) . . ? Cu C125 4.6116(17) . '3 455' ? Cu C126 4.1258(16) . . ? Cu C131 3.3391(17) . . ? Cu N11 2.9160(12) . . ? Cu C13 3.1959(15) . . ? Cu C14 4.3115(16) . . ? Cu C15 4.1419(15) . . ? Cu N21 2.9465(12) . . ? Cu C23 3.2301(16) . . ? Cu C24 4.3453(17) . . ? Cu C25 4.1722(16) . . ? Cu N31 2.9017(12) . . ? Cu C33 3.1802(16) . . ? Cu C34 4.2960(17) . . ? Cu C35 4.1247(16) . . ? Cu B 3.0568(17) . . ? Cu H114 3.9882(3) . 3 ? Cu H115 3.7675(4) . 3 ? Cu H116 2.9521(3) . . ? Cu H122 4.2236(4) . . ? Cu H125 3.8519(3) . '3 455' ? Cu H126 4.0275(3) . . ? Cu H131a 4.3710(4) . '5 655' ? Cu H131a 3.4438(3) . . ? Cu H131b 4.1679(4) . . ? Cu H131c 3.5223(3) . . ? Cu H13 3.4814(3) . . ? Cu H23 3.5186(4) . . ? Cu H33 3.4658(3) . . ? Cu H 4.0446(4) . . ? P C112 2.8135(16) . . ? P C113 4.1050(18) . . ? P C114 4.6179(18) . . ? P C115 4.720(2) . 3 ? P C115 4.0979(19) . . ? P C116 2.7911(17) . . ? P C122 2.8302(17) . . ? P C123 4.1222(18) . . ? P C124 4.6304(17) . . ? P C125 4.1054(17) . . ? P C126 2.8031(17) . . ? P N12 3.7726(13) . . ? P C13 4.7600(16) . '3 455' ? P C13 4.4517(16) . . ? P N22 3.6762(13) . . ? P C23 4.3016(17) . . ? P N32 3.7611(13) . . ? P C33 4.4394(16) . . ? P H112 2.9031(4) . . ? P H115 4.2166(5) . 3 ? P H116 2.8785(4) . . ? P H122 2.9264(4) . . ? P H126 2.8727(4) . . ? P H131a 2.3377(4) . . ? P H131b 2.3375(4) . . ? P H131c 2.3375(4) . . ? P H13 4.2670(5) . . ? P H13 4.2996(5) . '3 455' ? P H23 4.0867(5) . . ? P H33 4.2511(5) . . ? C111 C113 2.415(2) . . ? C111 C114 2.794(2) . . ? C111 C115 2.418(2) . . ? C111 C121 2.839(2) . . ? C111 C122 4.070(2) . . ? C111 C126 3.150(2) . . ? C111 C131 2.850(2) . . ? C111 N12 4.396(2) . '3 455' ? C111 N12 4.3218(19) . . ? C111 C13 3.742(2) . '3 455' ? C111 C14 4.021(2) . '3 455' ? C111 H112 2.0471(15) . . ? C111 H113 3.2818(15) . . ? C111 H114 3.7548(15) . . ? C111 H115 3.2796(15) . . ? C111 H116 2.0452(15) . . ? C111 H126 2.7794(15) . . ? C111 H131a 3.7005(15) . . ? C111 H131b 2.9846(15) . . ? C111 H131c 2.9850(15) . . ? C111 H13 3.5450(15) . '3 455' ? C111 H15 3.9817(15) . '8 554' ? C112 C114 2.405(2) . . ? C112 C115 2.772(2) . . ? C112 C116 2.401(2) . . ? C112 C121 3.215(2) . . ? C112 C122 4.267(2) . . ? C112 C124 4.197(2) . '6 454' ? C112 C126 3.356(2) . . ? C112 C131 3.330(2) . . ? C112 N11 4.364(2) . '3 455' ? C112 N11 4.375(2) . '8 554' ? C112 N12 4.180(2) . '3 455' ? C112 C13 3.611(2) . '3 455' ? C112 C14 4.291(2) . '8 554' ? C112 C14 3.467(2) . '3 455' ? C112 C15 3.567(2) . '8 554' ? C112 C15 3.974(2) . '3 455' ? C112 C24 4.048(2) . 3 ? C112 H113 2.0439(16) . . ? C112 H114 3.2711(16) . . ? C112 H115 3.7337(15) . . ? C112 H116 3.2669(15) . . ? C112 H124 3.6881(16) . '6 454' ? C112 H126 3.0908(16) . . ? C112 H131b 3.0366(17) . . ? C112 H131c 3.5187(16) . . ? C112 H13 3.7548(16) . '3 455' ? C112 H14 3.5093(16) . '3 455' ? C112 H15 2.9365(16) . '8 554' ? C112 H24 3.4648(16) . 3 ? C113 C115 2.398(2) . . ? C113 C116 2.774(2) . . ? C113 C126 4.392(2) . . ? C113 N11 3.646(2) . '3 455' ? C113 N11 4.199(2) . '8 554' ? C113 N12 3.711(2) . '3 455' ? C113 C13 3.588(2) . '3 455' ? C113 C14 3.485(2) . '3 455' ? C113 C15 3.511(2) . '3 455' ? C113 C15 3.768(2) . '8 554' ? C113 N21 4.267(2) . '8 554' ? C113 C24 3.769(2) . 3 ? C113 C25 3.919(2) . '8 554' ? C113 N31 4.279(2) . '3 455' ? C113 B 4.086(2) . '8 554' ? C113 H112 2.0461(17) . . ? C113 H114 2.0462(17) . . ? C113 H115 3.2721(17) . . ? C113 H116 3.7289(17) . . ? C113 H126 3.9488(17) . . ? C113 H13 3.9988(17) . '3 455' ? C113 H14 3.8279(17) . '3 455' ? C113 H15 3.1623(17) . '8 554' ? C113 H15 3.8698(17) . '3 455' ? C113 H24 2.9488(17) . 3 ? C113 H25 3.3319(17) . '8 554' ? C113 H 3.4576(17) . '8 554' ? C114 C116 2.408(2) . . ? C114 N11 3.604(2) . '3 455' ? C114 N12 3.427(2) . '3 455' ? C114 C13 3.681(2) . '3 455' ? C114 C14 4.039(2) . '3 455' ? C114 C15 3.969(2) . '3 455' ? C114 C24 3.997(2) . 3 ? C114 N31 3.589(2) . '3 455' ? C114 N32 3.402(2) . '3 455' ? C114 C33 3.568(2) . '3 455' ? C114 C33 4.363(2) . '7 655' ? C114 C34 3.882(2) . '3 455' ? C114 C35 3.877(2) . '3 455' ? C114 B 4.226(2) . '3 455' ? C114 H112 3.2757(18) . . ? C114 H113 2.042(2) . . ? C114 H115 2.049(2) . . ? C114 H116 3.2665(18) . . ? C114 H13 4.0340(17) . '3 455' ? C114 H24 3.1680(17) . 3 ? C114 H25 3.808(2) . '8 554' ? C114 H33 3.5765(18) . '7 655' ? C114 H33 3.9176(18) . '3 455' ? C115 C121 4.190(2) . '3 455' ? C115 C125 4.177(2) . '3 455' ? C115 C126 3.899(2) . '3 455' ? C115 N11 4.292(2) . '3 455' ? C115 N12 3.660(2) . '3 455' ? C115 C13 3.790(2) . '3 455' ? C115 N31 4.357(2) . '3 455' ? C115 N32 3.744(2) . '3 455' ? C115 C33 3.867(2) . '3 455' ? C115 C33 3.864(2) . '7 655' ? C115 C34 3.793(2) . '7 655' ? C115 H112 3.7358(18) . . ? C115 H113 3.2621(18) . . ? C115 H114 2.0433(18) . . ? C115 H116 2.0439(18) . . ? C115 H126 3.9353(18) . '3 455' ? C115 H13 3.8241(19) . '3 455' ? C115 H23 3.9527(19) . 3 ? C115 H24 3.8300(18) . 3 ? C115 H33 3.9129(19) . '3 455' ? C115 H33 3.3084(18) . '7 655' ? C115 H34 3.2012(18) . '7 655' ? C116 C121 3.997(2) . . ? C116 C125 3.905(2) . '3 455' ? C116 C126 3.799(2) . '3 455' ? C116 C126 4.097(2) . . ? C116 C131 3.912(2) . . ? C116 N12 3.882(2) . . ? C116 N12 4.145(2) . '3 455' ? C116 C13 3.911(2) . . ? C116 C13 3.819(2) . '3 455' ? C116 N22 4.254(2) . . ? C116 C34 4.188(2) . '7 655' ? C116 H112 3.2695(15) . . ? C116 H113 3.7336(15) . . ? C116 H114 3.2779(17) . . ? C116 H115 2.0440(17) . . ? C116 H125 3.8680(15) . '3 455' ? C116 H126 3.6296(16) . '3 455' ? C116 H126 3.4748(17) . . ? C116 H131c 3.8088(17) . . ? C116 H13 3.5727(17) . '3 455' ? C116 H13 3.4628(16) . . ? C116 H23 3.9310(17) . 3 ? C116 H34 3.4514(16) . '7 655' ? C121 C123 2.418(2) . . ? C121 C124 2.799(2) . . ? C121 C125 2.424(2) . . ? C121 C131 2.881(2) . . ? C121 C14 4.306(2) . '8 554' ? C121 C15 4.376(2) . '8 554' ? C121 H112 2.9195(15) . . ? C121 H115 3.5029(15) . 3 ? C121 H122 2.0481(15) . . ? C121 H123 3.2846(15) . . ? C121 H124 3.7546(15) . . ? C121 H125 3.2944(15) . . ? C121 H126 2.0388(15) . . ? C121 H131a 3.1304(15) . . ? C121 H131b 2.9026(15) . . ? C121 H131c 3.7086(16) . . ? C121 H14 3.7163(14) . '8 554' ? C121 H15 3.8389(15) . '8 554' ? C122 C124 2.404(2) . . ? C122 C125 2.776(2) . . ? C122 C126 2.396(2) . . ? C122 C131 3.182(2) . . ? C122 C14 4.231(2) . '8 554' ? C122 C24 3.711(2) . '5 655' ? C122 C25 4.051(2) . '5 655' ? C122 C35 4.207(2) . '2 654' ? C122 H112 3.7228(17) . . ? C122 H115 3.8203(17) . 3 ? C122 H123 2.0455(17) . . ? C122 H124 3.2628(17) . . ? C122 H124 4.0259(17) . '6 454' ? C122 H125 3.7366(17) . . ? C122 H126 3.2598(17) . . ? C122 H131a 3.0770(17) . . ? C122 H131b 3.0689(17) . . ? C122 H14 3.4298(17) . '8 554' ? C122 H24 3.4090(17) . '5 655' ? C122 H33 3.9451(17) . . ? C122 H34 4.0239(17) . '5 755' ? C122 H35 3.2932(17) . '2 654' ? C123 C125 2.394(2) . . ? C123 C126 2.760(2) . . ? C123 C131 4.212(2) . '6 554' ? C123 C14 3.972(2) . '8 554' ? C123 C24 4.396(2) . '5 655' ? C123 C34 3.779(2) . '5 755' ? C123 C35 4.022(2) . '5 755' ? C123 C35 3.979(2) . '2 654' ? C123 B 4.376(2) . '2 654' ? C123 H114 4.0263(18) . '7 645' ? C123 H115 4.0308(18) . 3 ? C123 H122 2.0480(18) . . ? C123 H124 2.0262(18) . . ? C123 H125 3.2564(18) . . ? C123 H126 3.7173(18) . . ? C123 H131b 3.3820(18) . '6 554' ? C123 H14 3.0615(18) . '8 554' ? C123 H24 3.8333(18) . '5 655' ? C123 H34 3.2941(18) . '5 755' ? C123 H35 3.7701(18) . '5 755' ? C123 H35 3.2296(18) . '2 654' ? C123 H 3.6213(18) . '2 654' ? C124 C126 2.400(2) . . ? C124 C131 4.137(2) . '6 554' ? C124 N12 4.403(2) . 3 ? C124 C13 3.962(2) . 3 ? C124 C14 3.791(2) . 3 ? C124 C14 3.767(2) . '8 554' ? C124 C15 4.288(2) . '8 554' ? C124 C15 4.166(2) . 3 ? C124 C34 3.520(2) . '5 755' ? C124 C35 3.822(2) . '5 755' ? C124 H112 3.3863(16) . '6 554' ? C124 H115 3.9587(16) . 3 ? C124 H116 3.9872(16) . 3 ? C124 H122 3.2687(17) . . ? C124 H123 2.0312(17) . . ? C124 H125 2.0408(17) . . ? C124 H126 3.2649(16) . . ? C124 H131b 3.1924(16) . '6 554' ? C124 H14 2.9865(16) . '8 554' ? C124 H14 3.8808(17) . 3 ? C124 H34 2.8501(16) . '5 755' ? C124 H35 3.4711(17) . '5 755' ? C125 N11 3.903(2) . 3 ? C125 N12 3.725(2) . 3 ? C125 C13 3.686(2) . 3 ? C125 C14 3.837(2) . '8 554' ? C125 C14 3.865(2) . 3 ? C125 C15 3.991(2) . 3 ? C125 C15 3.888(2) . '8 554' ? C125 N21 3.977(2) . 3 ? C125 N22 3.843(2) . 3 ? C125 C23 3.896(2) . 3 ? C125 C24 4.088(2) . 3 ? C125 C25 4.119(2) . 3 ? C125 C34 4.138(2) . '5 755' ? C125 H112 3.7850(17) . '6 554' ? C125 H115 3.6480(17) . 3 ? C125 H116 3.1155(17) . 3 ? C125 H122 3.7362(17) . . ? C125 H123 3.2619(17) . . ? C125 H124 2.0511(17) . . ? C125 H126 2.0374(17) . . ? C125 H13 3.9705(17) . 3 ? C125 H14 3.2961(17) . '8 554' ? C125 H15 3.3789(17) . '8 554' ? C125 H34 3.2613(17) . '5 755' ? C126 C131 4.135(2) . . ? C126 C14 4.109(2) . '8 554' ? C126 C15 3.941(2) . '8 554' ? C126 N22 4.024(2) . 3 ? C126 C23 3.646(2) . 3 ? C126 C24 3.887(2) . 3 ? C126 C25 4.368(2) . 3 ? C126 H112 3.1988(16) . . ? C126 H115 3.3952(16) . 3 ? C126 H116 3.2102(16) . 3 ? C126 H122 3.2652(16) . . ? C126 H123 3.7214(16) . . ? C126 H124 3.2677(16) . . ? C126 H125 2.0536(16) . . ? C126 H14 3.6439(16) . '8 554' ? C126 H15 3.2555(16) . '8 554' ? C126 H23 3.6698(16) . 3 ? C126 H34 3.9798(16) . '5 755' ? C131 C13 4.185(2) . '3 455' ? C131 C14 4.113(2) . '3 455' ? C131 N21 3.648(2) . '5 655' ? C131 N22 3.937(2) . '5 655' ? C131 N22 4.149(2) . . ? C131 C23 4.339(2) . . ? C131 C23 4.106(2) . '5 655' ? C131 C24 3.988(2) . '5 655' ? C131 C25 3.690(2) . '5 655' ? C131 N31 3.714(2) . '5 655' ? C131 N32 4.025(2) . '5 655' ? C131 C33 4.205(2) . '5 655' ? C131 C34 4.063(2) . '5 655' ? C131 C35 3.735(2) . '5 655' ? C131 B 4.175(2) . '5 655' ? C131 H112 3.1041(17) . . ? C131 H122 2.7800(17) . . ? C131 H123 3.7523(17) . '6 454' ? C131 H124 3.6185(16) . '6 454' ? C131 H13 3.7057(17) . '3 455' ? C131 H14 3.5900(17) . '3 455' ? C131 H23 3.8497(17) . . ? C131 H25 3.9487(17) . '5 655' ? C131 H35 3.9681(17) . '5 655' ? N11 C13 2.156(2) . . ? N11 C14 2.213(2) . . ? N11 N21 2.5077(18) . . ? N11 N22 3.0395(18) . . ? N11 C23 4.195(2) . . ? N11 C24 4.389(2) . 6 ? N11 C25 4.213(2) . 6 ? N11 C25 3.608(2) . . ? N11 N31 2.5272(17) . . ? N11 N32 3.0611(17) . . ? N11 C33 4.241(2) . . ? N11 C35 3.654(2) . . ? N11 H112 3.8643(12) . 8 ? N11 H113 3.5021(12) . 8 ? N11 H113 3.6335(13) . 3 ? N11 H114 3.5461(12) . 3 ? N11 H125 2.9768(12) . '3 455' ? N11 H13 3.0781(12) . . ? N11 H14 3.1379(13) . . ? N11 H15 2.0583(12) . . ? N11 H25 3.6538(12) . 6 ? N11 H25 3.9781(13) . . ? N11 H 2.0914(12) . . ? N12 C14 2.252(2) . . ? N12 C15 2.2253(19) . . ? N12 N21 3.0346(18) . . ? N12 N22 2.9295(18) . . ? N12 C23 4.104(2) . . ? N12 C25 4.238(2) . . ? N12 N31 3.0553(18) . . ? N12 N32 2.9611(18) . . ? N12 C33 4.168(2) . . ? N12 C35 4.293(2) . . ? N12 B 2.526(2) . . ? N12 H114 3.5718(13) . 3 ? N12 H115 3.9401(12) . 3 ? N12 H116 3.0759(12) . . ? N12 H125 2.8938(12) . '3 455' ? N12 H13 2.0315(13) . . ? N12 H14 3.1664(12) . . ? N12 H15 3.1413(12) . . ? N12 H 3.3188(12) . . ? C13 C15 2.191(2) . . ? C13 N21 4.185(2) . . ? C13 N22 4.105(2) . . ? C13 N31 4.258(2) . . ? C13 N32 4.193(2) . . ? C13 C34 3.741(2) . '7 655' ? C13 C35 4.240(2) . '7 655' ? C13 B 3.627(2) . . ? C13 H112 4.0031(16) . 3 ? C13 H113 3.9993(16) . 3 ? C13 H116 3.1823(16) . . ? C13 H124 3.5939(16) . '3 455' ? C13 H125 3.0641(16) . '3 455' ? C13 H131c 3.5123(15) . 3 ? C13 H14 2.1130(15) . . ? C13 H15 3.1199(16) . . ? C13 H34 3.1909(15) . '7 655' ? C14 C34 4.002(2) . '7 655' ? C14 C35 4.054(2) . '7 655' ? C14 B 3.732(2) . . ? C14 H112 3.5480(16) . 3 ? C14 H112 3.4837(16) . 8 ? C14 H113 3.6143(16) . 3 ? C14 H124 3.1395(16) . '3 455' ? C14 H125 3.2800(16) . '3 455' ? C14 H131b 3.7394(16) . 3 ? C14 H131c 3.6202(16) . 3 ? C14 H13 2.0903(16) . . ? C14 H15 2.0840(16) . . ? C14 H34 3.5952(16) . '7 655' ? C14 H35 3.6761(16) . '7 655' ? C15 N21 3.602(2) . . ? C15 N22 4.247(2) . . ? C15 C24 3.833(2) . 6 ? C15 C25 3.778(2) . 6 ? C15 N31 3.682(2) . . ? C15 N32 4.324(2) . . ? C15 B 2.630(2) . . ? C15 H112 2.9704(15) . 8 ? C15 H113 3.3538(15) . 3 ? C15 H113 3.3458(15) . 8 ? C15 H124 3.5906(16) . '3 455' ? C15 H125 4.0021(15) . 8 ? C15 H125 3.2158(15) . '3 455' ? C15 H13 3.1126(15) . . ? C15 H14 2.0985(16) . . ? C15 H24 3.6105(15) . 6 ? C15 H25 3.4814(15) . 6 ? C15 H 2.7460(16) . . ? N21 C23 2.159(2) . . ? N21 C24 2.214(2) . . ? N21 N31 2.5232(17) . . ? N21 N32 3.0595(17) . . ? N21 C33 4.240(2) . . ? N21 C35 3.647(2) . . ? N21 H113 3.3108(12) . 8 ? N21 H122 3.9869(13) . '5 655' ? N21 H123 3.8696(12) . '2 655' ? N21 H125 3.1209(13) . '3 455' ? N21 H131a 2.8255(13) . '5 655' ? N21 H131b 3.8386(13) . '5 655' ? N21 H131c 3.8340(13) . '5 655' ? N21 H15 3.9657(12) . . ? N21 H23 3.0833(12) . . ? N21 H24 3.1419(13) . . ? N21 H25 2.0636(12) . . ? N21 H 2.1102(12) . . ? N22 C24 2.252(2) . . ? N22 C25 2.228(2) . . ? N22 N31 3.0347(18) . . ? N22 N32 2.9352(18) . . ? N22 C33 4.141(2) . . ? N22 C35 4.268(2) . . ? N22 B 2.524(2) . . ? N22 H116 3.5207(13) . . ? N22 H125 3.0923(13) . '3 455' ? N22 H126 3.4457(13) . '3 455' ? N22 H131a 3.0450(13) . '5 655' ? N22 H131c 3.8512(13) . . ? N22 H23 2.0320(13) . . ? N22 H24 3.1712(13) . . ? N22 H25 3.1493(13) . . ? N22 H 3.3341(13) . . ? C23 C25 2.193(2) . . ? C23 N31 4.230(2) . . ? C23 N32 4.198(2) . '5 655' ? C23 N32 4.157(2) . . ? C23 C33 3.623(2) . '5 655' ? C23 C34 4.377(2) . '5 655' ? C23 B 3.625(2) . . ? C23 H116 3.9067(17) . . ? C23 H122 3.6578(17) . '5 655' ? C23 H125 3.3904(17) . '3 455' ? C23 H126 2.8693(17) . '3 455' ? C23 H131a 3.1599(17) . '5 655' ? C23 H131c 3.7674(17) . . ? C23 H15 3.9727(17) . '6 455' ? C23 H24 2.1190(16) . . ? C23 H25 3.1215(17) . . ? C23 H33 3.1264(16) . '5 655' ? C24 C33 4.220(2) . '5 655' ? C24 B 4.295(2) . '6 455' ? C24 B 3.735(2) . . ? C24 H113 3.8635(16) . '3 455' ? C24 H122 2.8029(17) . '5 655' ? C24 H125 3.6317(17) . '3 455' ? C24 H126 3.2460(17) . '3 455' ? C24 H131a 3.0791(17) . '5 655' ? C24 H15 3.0183(17) . '6 455' ? C24 H23 2.0892(18) . . ? C24 H25 2.0811(18) . . ? C24 H33 3.4687(18) . '5 655' ? C24 H 3.4818(17) . '6 455' ? C25 N31 3.678(2) . . ? C25 N32 4.318(2) . . ? C25 C35 4.247(2) . '6 455' ? C25 B 2.636(2) . . ? C25 B 4.228(2) . '6 455' ? C25 H113 2.9988(16) . 8 ? C25 H122 3.1001(16) . '5 655' ? C25 H123 3.7219(16) . '2 655' ? C25 H125 3.4503(16) . '3 455' ? C25 H126 3.9506(16) . '3 455' ? C25 H131a 2.8582(16) . '5 655' ? C25 H131b 3.6981(16) . '5 655' ? C25 H15 3.1862(16) . '6 455' ? C25 H23 3.1150(16) . . ? C25 H24 2.1027(16) . . ? C25 H35 3.7408(16) . '6 455' ? C25 H 3.6084(16) . '6 455' ? C25 H 2.7828(16) . . ? N31 C33 2.160(2) . . ? N31 C34 2.217(2) . . ? N31 H114 2.9106(12) . 3 ? N31 H123 3.8009(12) . '2 655' ? N31 H131a 3.3841(13) . '5 655' ? N31 H131b 3.9281(13) . '5 655' ? N31 H131c 3.2737(12) . '5 655' ? N31 H25 3.6352(12) . 6 ? N31 H33 3.0853(12) . . ? N31 H34 3.1445(12) . . ? N31 H35 2.0642(12) . . ? N31 H 2.0918(12) . . ? N32 C34 2.251(2) . . ? N32 C35 2.223(2) . . ? N32 B 2.531(2) . . ? N32 H114 2.8139(13) . 3 ? N32 H115 3.4755(13) . 3 ? N32 H131a 3.6657(13) . '5 655' ? N32 H131c 3.4745(13) . '5 655' ? N32 H23 3.6976(12) . '5 655' ? N32 H33 2.0334(12) . . ? N32 H34 3.1742(13) . . ? N32 H35 3.1443(12) . . ? N32 H 3.3236(12) . . ? C33 C35 2.193(2) . . ? C33 B 3.633(2) . . ? C33 H114 2.8084(16) . 3 ? C33 H115 3.4186(16) . 3 ? C33 H115 3.4663(16) . '7 645' ? C33 H131c 3.4224(16) . '5 655' ? C33 H13 3.9575(16) . '7 645' ? C33 H23 2.9591(16) . '5 655' ? C33 H34 2.1257(16) . . ? C33 H35 3.1239(15) . . ? C34 B 3.735(2) . . ? C34 H114 2.9476(16) . 3 ? C34 H115 3.2458(16) . '7 645' ? C34 H116 3.9823(16) . '7 645' ? C34 H123 3.8152(17) . '5 755' ? C34 H124 3.3611(16) . '5 755' ? C34 H131c 3.2201(17) . '5 655' ? C34 H13 3.1502(16) . '7 645' ? C34 H14 3.7164(16) . '7 645' ? C34 H23 3.5208(17) . '5 655' ? C34 H33 2.0967(17) . . ? C34 H35 2.0851(17) . . ? C35 B 2.626(2) . . ? C35 H114 2.9960(16) . 3 ? C35 H122 3.9635(16) . '2 655' ? C35 H123 3.7616(16) . '5 755' ? C35 H123 3.5326(16) . '2 655' ? C35 H124 3.3856(16) . '5 755' ? C35 H131a 3.7456(16) . '5 655' ? C35 H131b 3.7883(16) . '5 655' ? C35 H131c 3.1115(16) . '5 655' ? C35 H13 3.8130(16) . '7 645' ? C35 H14 3.4694(16) . '7 645' ? C35 H25 3.3834(16) . 6 ? C35 H33 3.1200(16) . . ? C35 H34 2.1012(16) . . ? C35 H 2.7418(16) . . ? B H113 3.2340(17) . 8 ? B H114 3.8049(17) . 3 ? B H123 3.5041(17) . '2 655' ? B H125 3.6474(17) . '3 455' ? B H131a 3.5985(17) . '5 655' ? B H15 2.9293(17) . . ? B H24 3.7720(17) . 6 ? B H25 3.5986(17) . 6 ? B H25 2.9495(17) . . ? B H35 2.9318(17) . . ? H112 H113 2.3523(2) . . ? H112 H124 2.7895(2) . '6 454' ? H112 H125 3.5134(3) . '6 454' ? H112 H126 3.2044(2) . . ? H112 H131b 2.5741(2) . . ? H112 H131c 3.4622(2) . . ? H112 H14 3.3537(3) . '3 455' ? H112 H14 3.5375(2) . '8 554' ? H112 H15 2.51486(14) . '8 554' ? H113 H114 2.34303(16) . . ? H113 H15 2.9173(2) . '8 554' ? H113 H15 3.4804(2) . '3 455' ? H113 H24 2.9920(2) . 3 ? H113 H25 2.48439(15) . '8 554' ? H113 H 2.68058(15) . '8 554' ? H114 H115 2.3592(2) . . ? H114 H123 3.6180(2) . '7 655' ? H114 H24 3.3669(3) . 3 ? H114 H25 3.4503(3) . '8 554' ? H114 H33 3.5377(2) . '7 655' ? H114 H33 3.2662(2) . '3 455' ? H114 H34 3.4632(3) . '3 455' ? H114 H35 3.5441(2) . '3 455' ? H115 H116 2.3348(2) . . ? H115 H33 3.0743(2) . '7 655' ? H115 H33 3.2597(3) . '3 455' ? H115 H34 2.64269(17) . '7 655' ? H116 H125 2.9612(3) . '3 455' ? H116 H126 3.0776(2) . '3 455' ? H116 H13 2.9119(2) . . ? H116 H34 3.1321(2) . '7 655' ? H122 H123 2.34937(16) . . ? H122 H131a 2.43354(19) . . ? H122 H131b 2.7245(2) . . ? H122 H24 2.6224(3) . '5 655' ? H122 H25 3.1590(2) . '5 655' ? H122 H35 3.0516(3) . '2 654' ? H122 H 3.6282(2) . '2 654' ? H123 H124 2.32248(17) . . ? H123 H131b 3.0197(2) . '6 554' ? H123 H14 3.4092(2) . '8 554' ? H123 H24 3.4724(2) . '5 655' ? H123 H25 3.1817(2) . '2 654' ? H123 H34 3.5583(2) . '5 755' ? H123 H35 2.9245(2) . '2 654' ? H123 H35 3.4404(3) . '5 755' ? H123 H 2.7674(2) . '2 654' ? H124 H125 2.34844(18) . . ? H124 H131b 2.6572(2) . '6 554' ? H124 H14 3.0879(3) . 3 ? H124 H14 3.2998(2) . '8 554' ? H124 H34 2.8281(2) . '5 755' ? H124 H35 2.8569(2) . '5 755' ? H125 H126 2.35714(16) . . ? H125 H13 3.5203(3) . 3 ? H125 H15 3.4640(2) . '8 554' ? H125 H34 3.5233(3) . '5 755' ? H126 H15 3.2945(3) . '8 554' ? H126 H23 2.7683(2) . 3 ? H126 H24 3.4620(3) . 3 ? H131a H131b 1.55105(11) . . ? H131a H131c 1.55146(10) . . ? H131a H24 3.6139(2) . '5 655' ? H131a H25 3.2628(2) . '5 655' ? H131b H131c 1.55121(11) . . ? H131b H14 3.0981(2) . '3 455' ? H131c H13 2.9210(2) . '3 455' ? H131c H14 3.18571(19) . '3 455' ? H131c H23 3.1364(3) . . ? H131c H34 3.6294(3) . '5 655' ? H131c H35 3.4437(2) . '5 655' ? H13 H14 2.5138(2) . . ? H13 H23 3.3598(2) . 3 ? H13 H34 2.6900(2) . '7 655' ? H14 H15 2.5237(2) . . ? H14 H34 3.5184(2) . '7 655' ? H14 H35 2.9970(3) . '7 655' ? H15 H24 2.8007(2) . 6 ? H15 H25 3.1037(2) . 6 ? H15 H 2.7061(2) . . ? H23 H24 2.5162(2) . . ? H23 H33 2.57067(16) . '5 655' ? H24 H25 2.51782(16) . . ? H24 H33 3.2958(3) . '5 655' ? H24 H 2.8759(2) . '6 455' ? H25 H35 2.98251(18) . '6 455' ? H25 H 3.1165(2) . '6 455' ? H25 H 2.7615(2) . . ? H33 H34 2.53422(17) . . ? H34 H35 2.51593(17) . . ? H35 H 2.7074(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 1968 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 25 _reflns_limit_l_min 0 _reflns_limit_l_max 26 _reflns_number_observed ? _reflns_d_resolution_high .729 _reflns_d_resolution_low 10.213 _diffrn_reflns_av_sigmaI/netI .032 _diffrn_reflns_theta_min 1.99 _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 .037 _refine_ls_wR_factor_all .041 _refine_ls_goodness_of_fit_all 1.44 _refine_ls_shift/su_mean . #========================================================================== # 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 data_cpm11a # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C34 H35 B1 Cu1 N8 P1' _chemical_formula_moiety ? _chemical_formula_weight 661.04 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _cell_length_a 12.405(2) _cell_length_b 12.621(2) _cell_length_c 12.948(3) _cell_angle_alpha 66.897(3) _cell_angle_beta 66.169(3) _cell_angle_gamma 67.181(3) _cell_volume 1641.1(6) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.338 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 2074 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu .751 _exptl_crystal_description prism _exptl_crystal_size_max .1 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .1 _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 .808 _exptl_absorpt_correction_T_max .928 _diffrn_reflns_number 19220 _reflns_number_total 8216 _reflns_Friedel_coverage 0 _reflns_number_gt 5854 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.41 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .038 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _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 .043 _refine_ls_wR_factor_ref .047 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_number_reflns 5854 _refine_ls_number_parameters 406 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .004 _refine_diff_density_min -.639 _refine_diff_density_max 1.263 _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 _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 68 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' B ? 0 2 0 .001 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 70 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 16 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cu ? 0 2 .263 1.266 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 2 .09 .095 '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 .80885(3) .80780(3) .30419(3) .0181(4) Uani ? ? 1.00000 ? ? P .88282(6) .87406(6) .38485(6) .0166(7) Uani ? ? 1.00000 ? ? C111 1.0196(2) .9235(2) .2878(2) .018(3) Uani ? ? 1.00000 ? ? C112 1.1181(2) .9040(2) .3253(2) .023(3) Uani ? ? 1.00000 ? ? C113 1.2168(3) .9494(3) .2479(3) .029(3) Uani ? ? 1.00000 ? ? C114 1.2173(3) 1.0150(3) .1337(3) .034(4) Uani ? ? 1.00000 ? ? C115 1.1208(3) 1.0340(3) .0948(3) .031(3) Uani ? ? 1.00000 ? ? C116 1.0228(3) .9876(2) .1710(2) .025(3) Uani ? ? 1.00000 ? ? C121 .9277(2) .7729(2) .5163(2) .018(3) Uani ? ? 1.00000 ? ? C122 .9014(3) .8090(2) .6144(3) .026(3) Uani ? ? 1.00000 ? ? C123 .9365(3) .7292(3) .7120(3) .033(4) Uani ? ? 1.00000 ? ? C124 .9997(3) .6108(3) .7132(3) .030(3) Uani ? ? 1.00000 ? ? C125 1.0267(3) .5736(3) .6161(3) .030(3) Uani ? ? 1.00000 ? ? C126 .9908(3) .6534(2) .5186(2) .025(3) Uani ? ? 1.00000 ? ? C131 .7803(2) 1.0074(2) .4326(2) .018(3) Uani ? ? 1.00000 ? ? C132 .6593(2) 1.0077(2) .4992(2) .024(3) Uani ? ? 1.00000 ? ? C133 .5773(2) 1.1068(3) .5365(3) .027(3) Uani ? ? 1.00000 ? ? C134 .6153(3) 1.2078(2) .5061(3) .027(3) Uani ? ? 1.00000 ? ? C135 .7349(3) 1.2086(2) .4406(3) .026(3) Uani ? ? 1.00000 ? ? C136 .8174(2) 1.1087(2) .4045(2) .022(3) Uani ? ? 1.00000 ? ? N11 .8421(2) .69329(19) .12797(19) .018(2) Uani ? ? 1.00000 ? ? N12 .9085(2) .71462(18) .1770(2) .019(2) Uani ? ? 1.00000 ? ? C13 1.0267(2) .6837(2) .1134(2) .022(3) Uani ? ? 1.00000 ? ? C14 1.0359(3) .6427(2) .0235(2) .026(3) Uani ? ? 1.00000 ? ? C15 .9190(3) .6499(2) .0348(2) .023(3) Uani ? ? 1.00000 ? ? C16 1.1264(3) .6915(3) .1439(3) .032(4) Uani ? ? 1.00000 ? ? N21 .68242(19) .64633(18) .32145(18) .017(2) Uani ? ? 1.00000 ? ? N22 .7009(2) .68693(19) .39562(19) .018(2) Uani ? ? 1.00000 ? ? C23 .6802(2) .6068(2) .5015(2) .020(3) Uani ? ? 1.00000 ? ? C24 .6512(3) .5136(2) .4950(2) .023(3) Uani ? ? 1.00000 ? ? C25 .6542(2) .5408(2) .3814(2) .021(3) Uani ? ? 1.00000 ? ? C26 .6860(3) .6243(3) .6061(3) .030(3) Uani ? ? 1.00000 ? ? N31 .6427(2) .85251(18) .17720(18) .018(2) Uani ? ? 1.00000 ? ? N32 .6893(2) .91618(19) .20598(19) .019(2) Uani ? ? 1.00000 ? ? C33 .6221(2) 1.0306(2) .1799(2) .022(3) Uani ? ? 1.00000 ? ? C34 .5325(2) 1.0411(2) .1347(2) .024(3) Uani ? ? 1.00000 ? ? C35 .5481(2) .9275(2) .1342(2) .023(3) Uani ? ? 1.00000 ? ? C36 .6501(3) 1.1267(2) .1968(3) .031(4) Uani ? ? 1.00000 ? ? B .7024(3) .7158(3) .1896(3) .019(3) Uani ? ? 1.00000 ? ? N41 .6366(2) .6755(2) .1404(2) .023(3) Uani ? ? 1.00000 ? ? N42 .6836(2) .6573(2) .0313(2) .028(3) Uani ? ? 1.00000 ? ? C43 .5944(3) .6383(3) .0148(3) .033(4) Uani ? ? 1.00000 ? ? C44 .4877(3) .6472(3) .1105(3) .034(4) Uani ? ? 1.00000 ? ? C45 .5175(3) .6716(3) .1880(3) .032(4) Uani ? ? 1.00000 ? ? C46 .6172(3) .6129(3) -.0971(4) .053(5) Uani ? ? 1.00000 ? ? H112 1.11729 .85806 .40547 .03200 Uiso ? ? 1.00000 ? ? H113 1.28626 .93476 .27256 .03800 Uiso ? ? 1.00000 ? ? H114 1.28490 1.04707 .07926 .04200 Uiso ? ? 1.00000 ? ? H115 1.12101 1.08003 .01548 .03900 Uiso ? ? 1.00000 ? ? H116 .95646 .99949 .14457 .03100 Uiso ? ? 1.00000 ? ? H122 .85657 .89071 .61410 .03300 Uiso ? ? 1.00000 ? ? H123 .91761 .75589 .77974 .04100 Uiso ? ? 1.00000 ? ? H124 1.02454 .55428 .78165 .03800 Uiso ? ? 1.00000 ? ? H125 1.07146 .49169 .61557 .03700 Uiso ? ? 1.00000 ? ? H126 1.00980 .62675 .45132 .03200 Uiso ? ? 1.00000 ? ? H132 .63366 .93737 .52012 .02900 Uiso ? ? 1.00000 ? ? H133 .49412 1.10580 .58338 .03300 Uiso ? ? 1.00000 ? ? H134 .55781 1.27826 .52996 .03300 Uiso ? ? 1.00000 ? ? H135 .76167 1.27816 .42021 .03300 Uiso ? ? 1.00000 ? ? H136 .90110 1.10917 .35868 .02700 Uiso ? ? 1.00000 ? ? H16a 1.15267 .75959 .08840 .04900 Uiso ? ? 1.00000 ? ? H16b 1.19250 .62108 .13489 .04900 Uiso ? ? 1.00000 ? ? H16c 1.10596 .69726 .22148 .04900 Uiso ? ? 1.00000 ? ? H14 1.10968 .61530 -.03445 .03200 Uiso ? ? 1.00000 ? ? H15 .89498 .62802 -.01412 .02800 Uiso ? ? 1.00000 ? ? H26a .76313 .57767 .61997 .04500 Uiso ? ? 1.00000 ? ? H26b .62228 .59932 .67310 .04500 Uiso ? ? 1.00000 ? ? H26c .67726 .70641 .59378 .04500 Uiso ? ? 1.00000 ? ? H24 .63255 .44452 .55795 .02800 Uiso ? ? 1.00000 ? ? H25 .63782 .49379 .34922 .02600 Uiso ? ? 1.00000 ? ? H36a .72244 1.09763 .21944 .04800 Uiso ? ? 1.00000 ? ? H36b .58353 1.16184 .25506 .04800 Uiso ? ? 1.00000 ? ? H36c .66084 1.18882 .12378 .04800 Uiso ? ? 1.00000 ? ? H34 .47249 1.11391 .10870 .03000 Uiso ? ? 1.00000 ? ? H35 .50044 .90433 .10722 .02800 Uiso ? ? 1.00000 ? ? H46a .69604 .62212 -.14921 .07900 Uiso ? ? 1.00000 ? ? H46b .55662 .66797 -.13452 .07900 Uiso ? ? 1.00000 ? ? H46c .61572 .53328 -.08355 .07900 Uiso ? ? 1.00000 ? ? H44 .41074 .63707 .11940 .04100 Uiso ? ? 1.00000 ? ? H45 .46261 .68493 .26354 .04100 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 .01918(17) .01665(17) .01962(19) -.00410(13) -.00654(14) -.00615(13) P .0168(3) .0156(3) .0172(4) -.0040(3) -.0045(3) -.0053(3) C111 .0188(13) .0152(12) .0191(14) -.0045(10) -.0024(11) -.0074(11) C112 .0204(14) .0254(14) .0231(15) -.0056(11) -.0038(12) -.0090(12) C113 .0196(14) .0345(17) .0335(18) -.0090(13) -.0038(13) -.0114(14) C114 .0268(16) .0322(17) .0325(18) -.0139(13) .0049(14) -.0077(14) C115 .0339(17) .0281(16) .0204(16) -.0089(13) -.0003(13) -.0034(13) C116 .0249(15) .0227(14) .0221(15) -.0044(12) -.0070(12) -.0043(12) C121 .0197(13) .0182(13) .0173(14) -.0077(10) -.0061(11) -.0022(11) C122 .0357(17) .0193(14) .0228(16) -.0071(12) -.0101(13) -.0041(12) C123 .0444(19) .0322(17) .0220(16) -.0106(14) -.0127(14) -.0055(13) C124 .0333(17) .0279(16) .0248(17) -.0093(13) -.0136(14) .0037(13) C125 .0262(15) .0219(14) .0326(18) -.0020(12) -.0091(13) -.0033(13) C126 .0265(15) .0219(14) .0233(15) -.0033(12) -.0055(12) -.0078(12) C131 .0190(13) .0176(13) .0199(14) -.0028(10) -.0083(11) -.0062(11) C132 .0226(14) .0201(14) .0266(16) -.0075(11) -.0032(12) -.0062(12) C133 .0183(14) .0317(16) .0281(16) -.0041(12) -.0024(12) -.0117(13) C134 .0238(15) .0228(14) .0323(17) .0037(12) -.0098(13) -.0135(13) C135 .0292(16) .0187(14) .0347(18) -.0046(12) -.0114(13) -.0105(13) C136 .0194(14) .0204(13) .0264(15) -.0048(11) -.0076(12) -.0070(12) N11 .0203(11) .0201(11) .0151(11) -.0066(9) -.0041(9) -.0057(9) N12 .0183(11) .0187(11) .0196(12) -.0046(9) -.0056(9) -.0061(9) C13 .0196(14) .0185(13) .0239(15) -.0040(11) -.0030(11) -.0058(11) C14 .0221(15) .0281(15) .0223(15) -.0051(12) .0021(12) -.0112(13) C15 .0288(15) .0225(14) .0155(14) -.0053(12) -.0033(12) -.0087(11) C16 .0206(15) .0338(17) .041(2) -.0035(12) -.0057(13) -.0186(15) N21 .0183(11) .0170(11) .0163(11) -.0050(9) -.0046(9) -.0060(9) N22 .0178(11) .0207(11) .0153(11) -.0050(9) -.0029(9) -.0072(9) C23 .0194(13) .0215(13) .0157(14) -.0059(11) -.0030(11) -.0047(11) C24 .0272(15) .0204(14) .0193(15) -.0098(12) -.0063(12) .0002(11) C25 .0236(14) .0176(13) .0240(15) -.0086(11) -.0049(12) -.0059(11) C26 .0374(17) .0389(17) .0167(15) -.0184(14) -.0064(13) -.0038(13) N31 .0188(11) .0190(11) .0153(11) -.0049(9) -.0057(9) -.0047(9) N32 .0205(11) .0172(11) .0184(12) -.0053(9) -.0054(9) -.0055(9) C33 .0223(14) .0193(13) .0200(15) -.0037(11) -.0049(12) -.0044(11) C34 .0230(14) .0217(14) .0244(16) .0008(11) -.0103(12) -.0063(12) C35 .0196(14) .0306(15) .0184(14) -.0064(12) -.0068(11) -.0069(12) C36 .0381(18) .0179(14) .0390(19) -.0032(13) -.0192(15) -.0069(13) B .0222(15) .0180(15) .0162(15) -.0054(12) -.0053(13) -.0044(13) N41 .0271(13) .0252(12) .0201(13) -.0102(10) -.0072(10) -.0065(10) N42 .0303(13) .0301(13) .0289(14) .0011(11) -.0134(11) -.0184(11) C43 .043(2) .0266(16) .042(2) -.0003(14) -.0283(16) -.0160(15) C44 .042(2) .0312(17) .041(2) -.0175(15) -.0221(16) -.0040(15) C45 .0340(17) .0376(18) .0266(17) -.0181(14) -.0090(14) -.0044(14) C46 .053(2) .060(2) .066(3) .0074(19) -.034(2) -.044(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 Cu P . . 2.1650(11) ? Cu N12 . . 2.091(2) ? Cu N22 . . 2.099(2) ? Cu N32 . . 2.067(2) ? P C111 . . 1.825(3) ? P C121 . . 1.830(3) ? P C131 . . 1.831(3) ? C111 C112 . . 1.394(5) ? C111 C116 . . 1.400(4) ? C112 C113 . . 1.391(4) ? C112 H112 . . .969(3) ? C113 C114 . . 1.381(4) ? C113 H113 . . .965(4) ? C114 C115 . . 1.383(6) ? C114 H114 . . .962(3) ? C115 C116 . . 1.386(4) ? C115 H115 . . .961(3) ? C116 H116 . . .954(4) ? C121 C122 . . 1.389(5) ? C121 C126 . . 1.398(4) ? C122 C123 . . 1.382(4) ? C122 H122 . . .963(3) ? C123 C124 . . 1.389(4) ? C123 H123 . . .971(4) ? C124 C125 . . 1.383(6) ? C124 H124 . . .972(3) ? C125 C126 . . 1.384(4) ? C125 H125 . . .967(3) ? C126 H126 . . .964(4) ? C131 C132 . . 1.396(4) ? C131 C136 . . 1.391(5) ? C132 C133 . . 1.387(4) ? C132 H132 . . .960(3) ? C133 C134 . . 1.388(5) ? C133 H133 . . .965(3) ? C134 C135 . . 1.381(4) ? C134 H134 . . .970(3) ? C135 C136 . . 1.390(4) ? C135 H135 . . .961(4) ? C136 H136 . . .966(3) ? N11 N12 . . 1.372(4) ? N11 C15 . . 1.360(4) ? N11 B . . 1.549(4) ? N12 C13 . . 1.346(3) ? C13 C14 . . 1.398(5) ? C13 C16 . . 1.489(6) ? C14 C15 . . 1.367(5) ? C14 H14 . . .961(3) ? C15 H15 . . .959(4) ? C16 H16a . . .951(3) ? C16 H16b . . .957(3) ? C16 H16c . . .957(4) ? N21 N22 . . 1.376(4) ? N21 C25 . . 1.353(4) ? N21 B . . 1.548(4) ? N22 C23 . . 1.341(3) ? C23 C24 . . 1.397(5) ? C23 C26 . . 1.488(5) ? C24 C25 . . 1.361(5) ? C24 H24 . . .961(2) ? C25 H25 . . .960(4) ? C26 H26a . . .955(3) ? C26 H26b . . .949(3) ? C26 H26c . . .953(4) ? N31 N32 . . 1.373(4) ? N31 C35 . . 1.355(4) ? N31 B . . 1.561(4) ? N32 C33 . . 1.343(3) ? C33 C34 . . 1.395(5) ? C33 C36 . . 1.496(6) ? C34 C35 . . 1.372(5) ? C34 H34 . . .970(2) ? C35 H35 . . .969(4) ? C36 H36a . . .948(4) ? C36 H36b . . .960(3) ? C36 H36c . . .961(3) ? B N41 . . 1.526(6) ? N41 N42 . . 1.369(4) ? N41 C45 . . 1.364(4) ? N42 C43 . . 1.329(6) ? C43 C44 . . 1.403(4) ? C43 C46 . . 1.499(7) ? C44 C45 . . 1.368(7) ? C44 H44 . . .967(4) ? C45 H45 . . .975(3) ? C46 H46a . . .958(4) ? C46 H46b . . .953(4) ? C46 H46c . . .956(5) ? 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 P Cu N12 . . . 126.60(8) ? P Cu N22 . . . 125.01(8) ? P Cu N32 . . . 123.86(8) ? N12 Cu N22 . . . 90.12(10) ? N12 Cu N32 . . . 89.47(9) ? N22 Cu N32 . . . 90.85(10) ? Cu P C111 . . . 114.40(12) ? Cu P C121 . . . 117.83(12) ? Cu P C131 . . . 114.72(12) ? C111 P C121 . . . 103.27(13) ? C111 P C131 . . . 101.98(13) ? C121 P C131 . . . 102.62(13) ? P C111 C112 . . . 123.3(2) ? P C111 C116 . . . 117.8(2) ? C112 C111 C116 . . . 118.9(2) ? C111 C112 C113 . . . 120.2(3) ? C111 C112 H112 . . . 119.3(3) ? C113 C112 H112 . . . 120.5(4) ? C112 C113 C114 . . . 120.2(3) ? C112 C113 H113 . . . 120.7(3) ? C114 C113 H113 . . . 119.1(3) ? C113 C114 C115 . . . 120.3(3) ? C113 C114 H114 . . . 121.1(4) ? C115 C114 H114 . . . 118.6(3) ? C114 C115 C116 . . . 119.9(3) ? C114 C115 H115 . . . 120.2(3) ? C116 C115 H115 . . . 119.9(4) ? C111 C116 C115 . . . 120.5(3) ? C111 C116 H116 . . . 119.1(3) ? C115 C116 H116 . . . 120.4(3) ? P C121 C122 . . . 123.08(19) ? P C121 C126 . . . 118.5(3) ? C122 C121 C126 . . . 118.4(3) ? C121 C122 C123 . . . 121.1(3) ? C121 C122 H122 . . . 118.9(3) ? C123 C122 H122 . . . 120.0(4) ? C122 C123 C124 . . . 120.1(3) ? C122 C123 H123 . . . 120.0(3) ? C124 C123 H123 . . . 119.9(3) ? C123 C124 C125 . . . 119.5(3) ? C123 C124 H124 . . . 120.5(4) ? C125 C124 H124 . . . 120.0(3) ? C124 C125 C126 . . . 120.4(3) ? C124 C125 H125 . . . 120.2(3) ? C126 C125 H125 . . . 119.4(4) ? C121 C126 C125 . . . 120.5(3) ? C121 C126 H126 . . . 119.6(3) ? C125 C126 H126 . . . 119.9(3) ? P C131 C132 . . . 118.5(2) ? P C131 C136 . . . 122.87(18) ? C132 C131 C136 . . . 118.7(2) ? C131 C132 C133 . . . 120.9(3) ? C131 C132 H132 . . . 119.0(3) ? C133 C132 H132 . . . 120.1(3) ? C132 C133 C134 . . . 119.7(3) ? C132 C133 H133 . . . 120.3(3) ? C134 C133 H133 . . . 120.0(3) ? C133 C134 C135 . . . 120.0(3) ? C133 C134 H134 . . . 120.1(3) ? C135 C134 H134 . . . 119.9(3) ? C134 C135 C136 . . . 120.2(3) ? C134 C135 H135 . . . 120.1(3) ? C136 C135 H135 . . . 119.6(3) ? C131 C136 C135 . . . 120.5(2) ? C131 C136 H136 . . . 119.2(3) ? C135 C136 H136 . . . 120.3(3) ? N12 N11 C15 . . . 109.5(2) ? N12 N11 B . . . 116.8(2) ? C15 N11 B . . . 133.6(3) ? Cu N12 N11 . . . 116.70(14) ? Cu N12 C13 . . . 135.8(3) ? N11 N12 C13 . . . 106.5(3) ? N12 C13 C14 . . . 109.7(3) ? N12 C13 C16 . . . 121.5(3) ? C14 C13 C16 . . . 128.7(2) ? C13 C14 C15 . . . 106.1(2) ? C13 C14 H14 . . . 126.7(4) ? C15 C14 H14 . . . 127.2(4) ? N11 C15 C14 . . . 108.1(3) ? N11 C15 H15 . . . 125.6(3) ? C14 C15 H15 . . . 126.2(3) ? C13 C16 H16a . . . 107.6(3) ? C13 C16 H16b . . . 106.9(4) ? C13 C16 H16c . . . 116.2(3) ? H16a C16 H16b . . . 108.8(3) ? H16a C16 H16c . . . 108.8(4) ? H16b C16 H16c . . . 108.3(3) ? N22 N21 C25 . . . 109.3(2) ? N22 N21 B . . . 120.5(2) ? C25 N21 B . . . 130.1(3) ? Cu N22 N21 . . . 112.40(14) ? Cu N22 C23 . . . 136.2(3) ? N21 N22 C23 . . . 106.4(3) ? N22 C23 C24 . . . 109.8(3) ? N22 C23 C26 . . . 121.6(3) ? C24 C23 C26 . . . 128.5(2) ? C23 C24 C25 . . . 105.9(2) ? C23 C24 H24 . . . 127.0(3) ? C25 C24 H24 . . . 127.0(4) ? N21 C25 C24 . . . 108.5(3) ? N21 C25 H25 . . . 125.6(3) ? C24 C25 H25 . . . 125.9(3) ? C23 C26 H26a . . . 109.7(3) ? C23 C26 H26b . . . 109.5(4) ? C23 C26 H26c . . . 110.5(3) ? H26a C26 H26b . . . 109.1(3) ? H26a C26 H26c . . . 108.8(4) ? H26b C26 H26c . . . 109.2(3) ? N32 N31 C35 . . . 109.5(2) ? N32 N31 B . . . 121.1(2) ? C35 N31 B . . . 129.4(3) ? Cu N32 N31 . . . 112.97(14) ? Cu N32 C33 . . . 139.0(3) ? N31 N32 C33 . . . 106.3(3) ? N32 C33 C34 . . . 110.3(3) ? N32 C33 C36 . . . 121.0(3) ? C34 C33 C36 . . . 128.7(2) ? C33 C34 C35 . . . 105.5(2) ? C33 C34 H34 . . . 126.8(4) ? C35 C34 H34 . . . 127.7(4) ? N31 C35 C34 . . . 108.4(3) ? N31 C35 H35 . . . 125.4(3) ? C34 C35 H35 . . . 126.2(3) ? C33 C36 H36a . . . 112.0(3) ? C33 C36 H36b . . . 111.2(3) ? C33 C36 H36c . . . 108.4(4) ? H36a C36 H36b . . . 108.8(4) ? H36a C36 H36c . . . 108.7(3) ? H36b C36 H36c . . . 107.7(3) ? N11 B N21 . . . 108.1(2) ? N11 B N31 . . . 109.3(2) ? N11 B N41 . . . 114.1(3) ? N21 B N31 . . . 109.4(2) ? N21 B N41 . . . 108.1(2) ? N31 B N41 . . . 107.7(2) ? B N41 N42 . . . 123.5(2) ? B N41 C45 . . . 125.6(3) ? N42 N41 C45 . . . 110.0(3) ? N41 N42 C43 . . . 105.6(2) ? N42 C43 C44 . . . 111.5(4) ? N42 C43 C46 . . . 119.2(3) ? C44 C43 C46 . . . 129.3(4) ? C43 C44 C45 . . . 104.7(4) ? C43 C44 H44 . . . 127.2(5) ? C45 C44 H44 . . . 128.0(3) ? N41 C45 C44 . . . 108.1(3) ? N41 C45 H45 . . . 126.2(4) ? C44 C45 H45 . . . 125.7(4) ? C43 C46 H46a . . . 109.4(5) ? C43 C46 H46b . . . 109.9(3) ? C43 C46 H46c . . . 111.9(3) ? H46a C46 H46b . . . 108.5(3) ? H46a C46 H46c . . . 108.3(4) ? H46b C46 H46c . . . 108.7(6) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 688 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 17 _reflns_limit_k_min -15 _reflns_limit_k_max 17 _reflns_limit_l_min -15 _reflns_limit_l_max 17 _reflns_number_observed ? _reflns_d_resolution_high .724 _reflns_d_resolution_low 11.346 _diffrn_reflns_av_sigmaI/netI .098 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .072 _refine_ls_wR_factor_all .052 _refine_ls_goodness_of_fit_all 1.012 _refine_ls_shift/su_mean . #========================================================================== # 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