Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Santini, Carlo' 'Lobbia, Giancarlo Gioia' 'Pellei, Maura' 'Pettinari, Claudio' 'Skelton, Brian W.' 'Somers, Neil' 'White, Allan H.' _publ_contact_author_name 'Dr Carlo Santini' _publ_contact_author_address ; Dipartimento di Scienze Chimiche Universita degli Studi di Camerino via S. Agostino 1 60232 Camerino MC ITALY ; _publ_contact_author_email CARLO.SANTINI@UNICAM.IT _publ_contact_author_fax '(+61)_08_9380_1118' _publ_contact_author_phone '(+61)_08-9380_3481' _publ_section_title ; Copper(I) coordination polymers and mononuclear copper(I) complexes built from poly(1,2,4-triazoly)borate ligands and tri-organophosphines ; _publ_section_references ; #<< references text Sheldrick, G M. (1996). SADABS. Program for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; _publ_section_figure_captions ; ? #<< figure captions ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_cpdar4 _database_code_CSD 176916 _audit_creation_method Xtal3.6 _audit_creation_date 01-10-29 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C40 H36 B1 Cu1 N6 P2' _chemical_formula_moiety ? _chemical_formula_weight 737.08 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P21/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 8.5706(5) _cell_length_b 19.2516(12) _cell_length_c 21.2925(14) _cell_angle_alpha 90.00000 _cell_angle_beta 93.471(2) _cell_angle_gamma 90.00000 _cell_volume 3506.8(4) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.396 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 5987 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu .754 _exptl_crystal_description prism _exptl_crystal_size_max .35 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .16 _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 .717 _exptl_absorpt_correction_T_max .832 _diffrn_reflns_number 73173 _reflns_number_total 18468 _reflns_Friedel_coverage 0 _reflns_number_gt 11373 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 37.61 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .051 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 36 _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 .036 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_number_reflns 11373 _refine_ls_number_parameters 595 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max .002 _refine_diff_density_min -.638 _refine_diff_density_max 1.121 _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 ? 0 160 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 144 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 8 .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' 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 1.03841(2) .674680(10) .232530(10) .01592(7) Uani ? ? 1.00000 ? ? P1 1.02846(4) .69469(2) .12737(2) .01508(15) Uani ? ? 1.00000 ? ? C111 .84298(16) .70042(8) .08056(7) .0166(6) Uani ? ? 1.00000 ? ? C112 .72060(18) .73713(8) .10556(7) .0207(7) Uani ? ? 1.00000 ? ? C113 .58217(19) .74813(9) .06978(8) .0248(8) Uani ? ? 1.00000 ? ? C114 .56473(19) .72257(10) .00881(8) .0262(8) Uani ? ? 1.00000 ? ? C115 .68290(19) .68440(9) -.01583(7) .0250(8) Uani ? ? 1.00000 ? ? C116 .82185(18) .67302(9) .02001(7) .0208(6) Uani ? ? 1.00000 ? ? C121 1.12327(16) .77566(8) .10389(7) .0166(6) Uani ? ? 1.00000 ? ? C122 1.20347(17) .81578(8) .15021(7) .0193(7) Uani ? ? 1.00000 ? ? C123 1.27699(19) .87706(8) .13430(8) .0228(7) Uani ? ? 1.00000 ? ? C124 1.2713(2) .89968(9) .07240(8) .0248(8) Uani ? ? 1.00000 ? ? C125 1.1899(2) .86117(9) .02627(8) .0253(8) Uani ? ? 1.00000 ? ? C126 1.11615(19) .79986(8) .04182(7) .0212(7) Uani ? ? 1.00000 ? ? C131 1.12768(17) .62559(8) .08593(6) .0166(6) Uani ? ? 1.00000 ? ? C132 1.0908(2) .55694(8) .10018(8) .0233(7) Uani ? ? 1.00000 ? ? C133 1.1547(2) .50178(9) .06852(8) .0275(8) Uani ? ? 1.00000 ? ? C134 1.2557(2) .51433(9) .02144(8) .0252(8) Uani ? ? 1.00000 ? ? C135 1.2952(2) .58199(9) .00759(8) .0256(8) Uani ? ? 1.00000 ? ? C136 1.23246(19) .63721(8) .03959(8) .0219(7) Uani ? ? 1.00000 ? ? P2 .92561(4) .57932(2) .27308(2) .01637(16) Uani ? ? 1.00000 ? ? C211 .79354(17) .59306(8) .33678(7) .0182(6) Uani ? ? 1.00000 ? ? C212 .8478(2) .63122(9) .38952(8) .0241(8) Uani ? ? 1.00000 ? ? C213 .7533(2) .64211(10) .43902(8) .0286(8) Uani ? ? 1.00000 ? ? C214 .6018(2) .61658(10) .43652(8) .0286(8) Uani ? ? 1.00000 ? ? C215 .54527(19) .57995(9) .38424(8) .0259(8) Uani ? ? 1.00000 ? ? C216 .64071(18) .56792(8) .33466(8) .0213(7) Uani ? ? 1.00000 ? ? C221 .79980(17) .52771(8) .21870(7) .0177(6) Uani ? ? 1.00000 ? ? C222 .69288(19) .56420(9) .17903(7) .0225(7) Uani ? ? 1.00000 ? ? C223 .5777(2) .52922(10) .14307(8) .0286(8) Uani ? ? 1.00000 ? ? C224 .5687(2) .45749(10) .14596(9) .0303(9) Uani ? ? 1.00000 ? ? C225 .6778(2) .42070(10) .18328(9) .0294(9) Uani ? ? 1.00000 ? ? C226 .79384(19) .45533(9) .21943(8) .0230(7) Uani ? ? 1.00000 ? ? C231 1.06860(17) .51651(8) .30567(7) .0200(7) Uani ? ? 1.00000 ? ? C232 1.1933(2) .49959(9) .26935(8) .0263(8) Uani ? ? 1.00000 ? ? C233 1.3041(2) .45097(10) .29046(10) .0321(9) Uani ? ? 1.00000 ? ? C234 1.2937(2) .42034(10) .34843(11) .0372(10) Uani ? ? 1.00000 ? ? C235 1.1725(2) .43721(11) .38543(11) .0408(11) Uani ? ? 1.00000 ? ? C236 1.0598(2) .48519(10) .36424(9) .0303(9) Uani ? ? 1.00000 ? ? N11 1.08698(15) .77242(7) .34157(6) .0200(6) Uani ? ? 1.00000 ? ? N12 .99013(14) .75626(7) .29011(6) .0181(6) Uani ? ? 1.00000 ? ? C13 .87232(19) .80048(9) .29313(8) .0228(7) Uani ? ? 1.00000 ? ? N14 .88390(18) .84393(8) .34291(7) .0299(7) Uani ? ? 1.00000 ? ? C15 1.0196(2) .82434(10) .37116(8) .0285(8) Uani ? ? 1.00000 ? ? N21 1.33545(14) .71862(7) .30552(6) .0188(6) Uani ? ? 1.00000 ? ? N22 1.28169(14) .68201(7) .25345(6) .0190(6) Uani ? ? 1.00000 ? ? C23 1.40262(18) .68145(9) .21752(8) .0237(7) Uani ? ? 1.00000 ? ? N24 1.53112(16) .71428(8) .24222(7) .0267(7) Uani ? ? 1.00000 ? ? C25 1.48375(18) .73605(9) .29699(8) .0235(7) Uani ? ? 1.00000 ? ? B 1.2352(2) .72927(12) .36264(8) .0251(9) Uani ? ? 1.00000 ? ? H112 .730(2) .7536(10) .1470(9) .024(5) Uiso ? ? 1.00000 ? ? H113 .504(2) .7716(10) .0868(9) .030(5) Uiso ? ? 1.00000 ? ? H114 .472(2) .7312(10) -.0148(9) .032(5) Uiso ? ? 1.00000 ? ? H115 .675(2) .6672(10) -.0575(9) .026(5) Uiso ? ? 1.00000 ? ? H116 .905(2) .6461(10) .0026(9) .025(5) Uiso ? ? 1.00000 ? ? H122 1.207(2) .8007(10) .1910(9) .024(5) Uiso ? ? 1.00000 ? ? H123 1.329(2) .9036(10) .1652(9) .028(5) Uiso ? ? 1.00000 ? ? H124 1.319(2) .9419(10) .0616(8) .023(5) Uiso ? ? 1.00000 ? ? H125 1.185(2) .8766(10) -.0170(10) .032(5) Uiso ? ? 1.00000 ? ? H126 1.062(2) .7740(10) .0103(9) .022(5) Uiso ? ? 1.00000 ? ? H132 1.024(2) .5479(11) .1295(10) .033(5) Uiso ? ? 1.00000 ? ? H133 1.128(2) .4554(11) .0791(9) .035(6) Uiso ? ? 1.00000 ? ? H134 1.297(2) .4772(9) .0019(8) .020(5) Uiso ? ? 1.00000 ? ? H135 1.364(2) .5903(10) -.0225(9) .030(5) Uiso ? ? 1.00000 ? ? H136 1.259(2) .6825(10) .0309(8) .022(5) Uiso ? ? 1.00000 ? ? H212 .944(2) .6485(10) .3921(9) .031(5) Uiso ? ? 1.00000 ? ? H213 .791(2) .6684(12) .4745(10) .044(6) Uiso ? ? 1.00000 ? ? H214 .536(2) .6236(11) .4707(9) .034(6) Uiso ? ? 1.00000 ? ? H215 .446(2) .5627(11) .3833(9) .034(6) Uiso ? ? 1.00000 ? ? H216 .600(2) .5432(10) .3007(9) .030(5) Uiso ? ? 1.00000 ? ? H222 .695(2) .6133(10) .1780(8) .019(4) Uiso ? ? 1.00000 ? ? H223 .503(2) .5544(11) .1171(10) .036(6) Uiso ? ? 1.00000 ? ? H224 .485(2) .4324(11) .1220(10) .041(6) Uiso ? ? 1.00000 ? ? H225 .673(2) .3726(11) .1859(9) .029(5) Uiso ? ? 1.00000 ? ? H226 .865(2) .4304(10) .2443(9) .029(5) Uiso ? ? 1.00000 ? ? H232 1.203(2) .5211(11) .2294(10) .040(6) Uiso ? ? 1.00000 ? ? H233 1.385(3) .4389(11) .2658(10) .042(6) Uiso ? ? 1.00000 ? ? H234 1.364(3) .3879(12) .3614(11) .050(7) Uiso ? ? 1.00000 ? ? H235 1.158(3) .4190(12) .4224(11) .051(7) Uiso ? ? 1.00000 ? ? H236 .971(2) .4943(11) .3882(10) .038(6) Uiso ? ? 1.00000 ? ? H13 .787(2) .8001(10) .2632(9) .024(5) Uiso ? ? 1.00000 ? ? H15 1.070(2) .8457(11) .4079(10) .041(6) Uiso ? ? 1.00000 ? ? H23 1.398(2) .6597(10) .1763(9) .030(5) Uiso ? ? 1.00000 ? ? H25 1.545(2) .7588(10) .3272(9) .028(5) Uiso ? ? 1.00000 ? ? H1a 1.199(2) .6775(10) .3782(9) .026(5) Uiso ? ? 1.00000 ? ? H1b 1.301(2) .7609(10) .3972(9) .031(5) Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu .01601(8) .01752(8) .01406(7) -.00079(7) -.00047(6) -.00083(7) P1 .01486(16) .01671(16) .01351(15) -.00060(13) -.00051(12) -.00090(13) C111 .0160(6) .0173(6) .0162(6) -.0022(5) -.0008(5) .0012(5) C112 .0208(7) .0234(8) .0178(7) .0003(6) .0014(5) -.0010(6) C113 .0176(7) .0293(8) .0274(8) .0026(6) .0011(6) .0026(7) C114 .0182(7) .0341(9) .0256(8) -.0049(6) -.0049(6) .0085(7) C115 .0236(8) .0332(9) .0176(7) -.0060(7) -.0045(6) -.0003(6) C116 .0200(7) .0246(7) .0174(6) -.0024(6) -.0010(5) -.0025(6) C121 .0162(6) .0167(6) .0171(6) -.0004(5) .0010(5) -.0018(5) C122 .0188(7) .0212(7) .0178(6) -.0008(5) .0007(5) -.0022(5) C123 .0222(8) .0210(7) .0253(8) -.0046(6) .0023(6) -.0065(6) C124 .0267(8) .0196(7) .0289(8) -.0046(6) .0069(6) -.0008(6) C125 .0315(9) .0238(8) .0210(7) -.0025(7) .0035(6) .0024(6) C126 .0234(7) .0219(7) .0180(7) -.0024(6) -.0015(6) -.0009(6) C131 .0159(6) .0189(7) .0148(6) .0008(5) -.0013(5) -.0013(5) C132 .0278(8) .0204(7) .0223(7) .0001(6) .0061(6) .0003(6) C133 .0347(9) .0185(8) .0297(9) -.0001(7) .0061(7) -.0009(6) C134 .0268(8) .0235(8) .0253(8) .0039(6) .0019(6) -.0066(6) C135 .0255(8) .0273(8) .0248(8) -.0000(7) .0085(6) -.0021(7) C136 .0224(7) .0195(7) .0243(8) -.0013(6) .0048(6) -.0003(6) P2 .01556(16) .01750(17) .01597(16) -.00040(13) .00031(13) .00093(14) C211 .0191(7) .0177(7) .0180(6) .0008(5) .0016(5) .0015(5) C212 .0221(8) .0282(8) .0220(7) -.0038(6) .0015(6) -.0017(6) C213 .0315(9) .0328(9) .0218(8) -.0047(7) .0047(7) -.0059(7) C214 .0306(9) .0302(9) .0262(8) -.0008(7) .0123(7) -.0028(7) C215 .0200(7) .0267(8) .0319(9) -.0023(6) .0081(6) -.0021(7) C216 .0202(7) .0208(7) .0231(7) -.0015(6) .0027(6) -.0019(6) C221 .0167(6) .0204(7) .0162(6) -.0005(5) .0031(5) -.0005(5) C222 .0221(7) .0242(8) .0210(7) .0006(6) -.0011(6) .0005(6) C223 .0246(8) .0384(10) .0221(8) .0022(7) -.0046(6) -.0025(7) C224 .0256(8) .0370(10) .0281(9) -.0045(7) -.0008(7) -.0139(8) C225 .0295(9) .0232(8) .0357(9) -.0037(7) .0031(7) -.0093(7) C226 .0222(7) .0215(7) .0254(8) .0016(6) .0022(6) -.0014(6) C231 .0172(7) .0187(7) .0236(7) -.0013(5) -.0023(5) .0016(6) C232 .0234(8) .0284(8) .0269(8) .0042(6) -.0006(6) -.0014(7) C233 .0212(8) .0280(9) .0465(11) .0046(7) -.0018(8) -.0054(8) C234 .0234(8) .0250(9) .0618(14) .0020(7) -.0099(8) .0103(9) C235 .0322(10) .0427(12) .0469(12) .0002(8) -.0037(9) .0260(10) C236 .0223(8) .0339(10) .0346(9) -.0002(7) .0009(7) .0126(8) N11 .0190(6) .0264(7) .0146(5) -.0022(5) .0007(5) -.0047(5) N12 .0181(6) .0209(6) .0153(5) -.0009(5) -.0006(4) -.0017(5) C13 .0213(7) .0253(8) .0219(7) .0034(6) .0014(6) -.0020(6) N14 .0293(7) .0311(8) .0295(7) .0045(6) .0052(6) -.0094(6) C15 .0273(8) .0356(9) .0228(7) -.0026(8) .0033(6) -.0114(7) N21 .0155(6) .0237(6) .0169(6) -.0011(5) -.0023(4) .0007(5) N22 .0163(5) .0222(6) .0183(5) .0007(5) -.0019(4) -.0011(5) C23 .0179(7) .0309(9) .0220(7) .0040(6) .0002(5) -.0043(6) N24 .0173(6) .0366(8) .0265(7) -.0005(6) .0021(5) -.0015(6) C25 .0166(7) .0288(8) .0249(8) -.0028(6) -.0015(6) -.0023(6) B .0202(8) .0399(11) .0148(7) .0000(8) -.0019(6) .0010(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 . . 2.2685(5) ? Cu P2 . . 2.2697(4) ? Cu N12 . . 2.0500(13) ? Cu N22 . . 2.1103(12) ? P1 C111 . . 1.8278(14) ? P1 C121 . . 1.8410(16) ? P1 C131 . . 1.8336(15) ? C111 C112 . . 1.397(2) ? C111 C116 . . 1.395(2) ? C112 C113 . . 1.387(2) ? C112 H112 . . .937(19) ? C113 C114 . . 1.388(2) ? C113 H113 . . .91(2) ? C114 C115 . . 1.380(2) ? C114 H114 . . .93(2) ? C115 C116 . . 1.392(2) ? C115 H115 . . .945(19) ? C116 H116 . . .971(19) ? C121 C122 . . 1.400(2) ? C121 C126 . . 1.399(2) ? C122 C123 . . 1.389(2) ? C122 H122 . . .915(19) ? C123 C124 . . 1.386(2) ? C123 H123 . . .925(19) ? C124 C125 . . 1.385(2) ? C124 H124 . . .943(19) ? C125 C126 . . 1.388(2) ? C125 H125 . . .97(2) ? C126 H126 . . .938(18) ? C131 C132 . . 1.396(2) ? C131 C136 . . 1.392(2) ? C132 C133 . . 1.388(2) ? C132 H132 . . .89(2) ? C133 C134 . . 1.385(3) ? C133 H133 . . .95(2) ? C134 C135 . . 1.382(2) ? C134 H134 . . .910(18) ? C135 C136 . . 1.388(2) ? C135 H135 . . .91(2) ? C136 H136 . . .921(19) ? P2 C211 . . 1.8376(16) ? P2 C221 . . 1.8274(15) ? P2 C231 . . 1.8283(15) ? C211 C212 . . 1.398(2) ? C211 C216 . . 1.395(2) ? C212 C213 . . 1.384(3) ? C212 H212 . . .89(2) ? C213 C214 . . 1.386(3) ? C213 H213 . . .95(2) ? C214 C215 . . 1.381(2) ? C214 H214 . . .96(2) ? C215 C216 . . 1.393(2) ? C215 H215 . . .91(2) ? C216 H216 . . .92(2) ? C221 C222 . . 1.397(2) ? C221 C226 . . 1.394(2) ? C222 C223 . . 1.387(2) ? C222 H222 . . .945(18) ? C223 C224 . . 1.385(3) ? C223 H223 . . .95(2) ? C224 C225 . . 1.385(3) ? C224 H224 . . .98(2) ? C225 C226 . . 1.390(2) ? C225 H225 . . .93(2) ? C226 H226 . . .917(19) ? C231 C232 . . 1.395(2) ? C231 C236 . . 1.391(2) ? C232 C233 . . 1.389(3) ? C232 H232 . . .95(2) ? C233 C234 . . 1.376(3) ? C233 H233 . . .93(2) ? C234 C235 . . 1.380(3) ? C234 H234 . . .90(2) ? C235 C236 . . 1.392(3) ? C235 H235 . . .88(2) ? C236 H236 . . .96(2) ? N11 N12 . . 1.3698(17) ? N11 C15 . . 1.332(2) ? N11 B . . 1.561(2) ? N12 C13 . . 1.325(2) ? C13 N14 . . 1.349(2) ? C13 H13 . . .943(18) ? N14 C15 . . 1.331(2) ? C15 H15 . . .96(2) ? N21 N22 . . 1.3698(18) ? N21 C25 . . 1.338(2) ? N21 B . . 1.545(2) ? N22 C23 . . 1.325(2) ? C23 N24 . . 1.349(2) ? C23 H23 . . .97(2) ? N24 C25 . . 1.326(2) ? C25 H25 . . .914(19) ? B H1a . . 1.099(19) ? B H1b . . 1.08(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 P2 . . . 121.427(17) ? P1 Cu N12 . . . 117.60(4) ? P1 Cu N22 . . . 100.06(4) ? P2 Cu N12 . . . 106.63(4) ? P2 Cu N22 . . . 114.33(4) ? N12 Cu N22 . . . 93.16(5) ? Cu P1 C111 . . . 121.87(5) ? Cu P1 C121 . . . 114.90(5) ? Cu P1 C131 . . . 111.16(5) ? C111 P1 C121 . . . 100.63(7) ? C111 P1 C131 . . . 101.23(7) ? C121 P1 C131 . . . 104.98(7) ? P1 C111 C112 . . . 118.11(11) ? P1 C111 C116 . . . 122.77(11) ? C112 C111 C116 . . . 119.03(13) ? C111 C112 C113 . . . 120.34(14) ? C111 C112 H112 . . . 120.5(11) ? C113 C112 H112 . . . 119.1(11) ? C112 C113 C114 . . . 119.99(15) ? C112 C113 H113 . . . 119.3(12) ? C114 C113 H113 . . . 120.7(12) ? C113 C114 C115 . . . 120.29(15) ? C113 C114 H114 . . . 118.9(12) ? C115 C114 H114 . . . 120.8(12) ? C114 C115 C116 . . . 119.89(14) ? C114 C115 H115 . . . 121.9(11) ? C116 C115 H115 . . . 118.1(11) ? C111 C116 C115 . . . 120.40(14) ? C111 C116 H116 . . . 119.8(11) ? C115 C116 H116 . . . 119.7(11) ? P1 C121 C122 . . . 118.80(11) ? P1 C121 C126 . . . 122.94(11) ? C122 C121 C126 . . . 118.25(13) ? C121 C122 C123 . . . 120.49(14) ? C121 C122 H122 . . . 118.7(11) ? C123 C122 H122 . . . 120.8(11) ? C122 C123 C124 . . . 120.56(15) ? C122 C123 H123 . . . 120.0(12) ? C124 C123 H123 . . . 119.4(12) ? C123 C124 C125 . . . 119.56(16) ? C123 C124 H124 . . . 120.8(11) ? C125 C124 H124 . . . 119.6(11) ? C124 C125 C126 . . . 120.20(15) ? C124 C125 H125 . . . 120.2(12) ? C126 C125 H125 . . . 119.6(12) ? C121 C126 C125 . . . 120.92(14) ? C121 C126 H126 . . . 119.4(11) ? C125 C126 H126 . . . 119.7(11) ? P1 C131 C132 . . . 117.67(11) ? P1 C131 C136 . . . 124.22(11) ? C132 C131 C136 . . . 118.05(14) ? C131 C132 C133 . . . 121.17(16) ? C131 C132 H132 . . . 120.1(13) ? C133 C132 H132 . . . 118.8(13) ? C132 C133 C134 . . . 120.02(16) ? C132 C133 H133 . . . 119.7(13) ? C134 C133 H133 . . . 120.3(13) ? C133 C134 C135 . . . 119.37(16) ? C133 C134 H134 . . . 118.2(12) ? C135 C134 H134 . . . 122.4(12) ? C134 C135 C136 . . . 120.68(16) ? C134 C135 H135 . . . 119.4(12) ? C136 C135 H135 . . . 119.9(12) ? C131 C136 C135 . . . 120.69(14) ? C131 C136 H136 . . . 118.0(12) ? C135 C136 H136 . . . 121.3(12) ? Cu P2 C211 . . . 117.38(5) ? Cu P2 C221 . . . 116.57(5) ? Cu P2 C231 . . . 112.84(5) ? C211 P2 C221 . . . 100.36(7) ? C211 P2 C231 . . . 104.11(7) ? C221 P2 C231 . . . 103.72(7) ? P2 C211 C212 . . . 118.62(12) ? P2 C211 C216 . . . 123.06(12) ? C212 C211 C216 . . . 118.32(15) ? C211 C212 C213 . . . 120.68(16) ? C211 C212 H212 . . . 120.6(13) ? C213 C212 H212 . . . 118.7(13) ? C212 C213 C214 . . . 120.47(16) ? C212 C213 H213 . . . 120.2(13) ? C214 C213 H213 . . . 119.3(13) ? C213 C214 C215 . . . 119.62(16) ? C213 C214 H214 . . . 121.0(12) ? C215 C214 H214 . . . 119.4(12) ? C214 C215 C216 . . . 120.15(15) ? C214 C215 H215 . . . 119.0(13) ? C216 C215 H215 . . . 120.8(13) ? C211 C216 C215 . . . 120.74(15) ? C211 C216 H216 . . . 121.2(12) ? C215 C216 H216 . . . 118.1(12) ? P2 C221 C222 . . . 116.73(12) ? P2 C221 C226 . . . 123.84(12) ? C222 C221 C226 . . . 119.07(14) ? C221 C222 C223 . . . 120.57(16) ? C221 C222 H222 . . . 120.4(10) ? C223 C222 H222 . . . 118.9(10) ? C222 C223 C224 . . . 119.96(16) ? C222 C223 H223 . . . 120.3(12) ? C224 C223 H223 . . . 119.7(12) ? C223 C224 C225 . . . 119.87(17) ? C223 C224 H224 . . . 120.6(13) ? C225 C224 H224 . . . 119.5(13) ? C224 C225 C226 . . . 120.53(18) ? C224 C225 H225 . . . 120.8(11) ? C226 C225 H225 . . . 118.6(11) ? C221 C226 C225 . . . 119.90(15) ? C221 C226 H226 . . . 120.4(12) ? C225 C226 H226 . . . 119.7(12) ? P2 C231 C232 . . . 117.54(12) ? P2 C231 C236 . . . 123.74(12) ? C232 C231 C236 . . . 118.71(15) ? C231 C232 C233 . . . 120.65(16) ? C231 C232 H232 . . . 120.1(13) ? C233 C232 H232 . . . 119.2(13) ? C232 C233 C234 . . . 119.92(18) ? C232 C233 H233 . . . 120.5(13) ? C234 C233 H233 . . . 119.6(13) ? C233 C234 C235 . . . 120.24(18) ? C233 C234 H234 . . . 119.7(15) ? C235 C234 H234 . . . 120.0(15) ? C234 C235 C236 . . . 120.2(2) ? C234 C235 H235 . . . 124.8(16) ? C236 C235 H235 . . . 115.0(15) ? C231 C236 C235 . . . 120.27(18) ? C231 C236 H236 . . . 119.2(12) ? C235 C236 H236 . . . 120.4(12) ? N12 N11 C15 . . . 106.83(13) ? N12 N11 B . . . 123.52(13) ? C15 N11 B . . . 129.22(14) ? Cu N12 N11 . . . 121.19(10) ? Cu N12 C13 . . . 134.68(11) ? N11 N12 C13 . . . 104.00(13) ? N12 C13 N14 . . . 114.61(14) ? N12 C13 H13 . . . 121.8(11) ? N14 C13 H13 . . . 123.6(11) ? C13 N14 C15 . . . 101.54(15) ? N11 C15 N14 . . . 113.02(15) ? N11 C15 H15 . . . 121.1(13) ? N14 C15 H15 . . . 125.8(13) ? N22 N21 C25 . . . 107.16(13) ? N22 N21 B . . . 121.98(12) ? C25 N21 B . . . 130.70(14) ? Cu N22 N21 . . . 119.00(9) ? Cu N22 C23 . . . 132.45(11) ? N21 N22 C23 . . . 103.59(12) ? N22 C23 N24 . . . 114.83(15) ? N22 C23 H23 . . . 122.3(11) ? N24 C23 H23 . . . 122.9(11) ? C23 N24 C25 . . . 101.82(14) ? N21 C25 N24 . . . 112.60(14) ? N21 C25 H25 . . . 122.0(13) ? N24 C25 H25 . . . 125.3(12) ? N11 B N21 . . . 109.04(13) ? N11 B H1a . . . 109.4(10) ? N11 B H1b . . . 105.9(10) ? N21 B H1a . . . 107.2(10) ? N21 B H1b . . . 108.6(11) ? H1a B H1b . . . 116.6(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 N11 2.9979(13) . . ? Cu C13 3.1271(17) . . ? Cu N21 3.0221(12) . . ? Cu C23 3.1597(16) . . ? Cu B 3.3253(18) . . ? Cu H122 2.984(19) . . ? P1 C112 2.7743(16) . . ? P1 C116 2.8364(15) . . ? P1 C122 2.7986(16) . . ? P1 C126 2.8545(16) . . ? P1 C132 2.7732(16) . . ? P1 C136 2.8584(17) . . ? C111 C113 2.415(2) . . ? C111 C114 2.786(2) . . ? C111 C115 2.418(2) . . ? C111 C121 2.823(2) . . ? C111 C131 2.830(2) . . ? C111 H112 2.039(19) . . ? C111 H116 2.058(19) . . ? C112 C114 2.403(2) . . ? C112 C115 2.777(2) . . ? C112 C116 2.405(2) . . ? C112 H113 1.99(2) . . ? C113 C115 2.401(2) . . ? C113 C116 2.774(2) . . ? C113 H112 2.017(18) . . ? C113 H114 2.01(2) . . ? C114 C116 2.400(2) . . ? C114 H113 2.01(2) . . ? C114 H115 2.04(2) . . ? C115 H114 2.02(2) . . ? C115 H116 2.055(18) . . ? C116 H115 2.018(18) . . ? C121 C123 2.421(2) . . ? C121 C124 2.804(2) . . ? C121 C125 2.425(2) . . ? C121 C131 2.915(2) . . ? C121 H122 2.007(18) . . ? C121 H126 2.030(18) . . ? C121 H136 2.682(18) . . ? C122 C124 2.410(2) . . ? C122 C125 2.776(2) . . ? C122 C126 2.402(2) . . ? C122 H123 2.018(19) . . ? C123 C125 2.395(2) . . ? C123 C126 2.767(2) . . ? C123 H122 2.017(19) . . ? C123 H124 2.037(18) . . ? C124 C126 2.404(2) . . ? C124 H123 2.009(19) . . ? C124 H125 2.05(2) . . ? C125 H124 2.024(18) . . ? C125 H126 2.024(18) . . ? C126 H125 2.05(2) . . ? C126 H136 2.586(18) . . ? C131 C133 2.425(2) . . ? C131 C134 2.804(2) . . ? C131 C135 2.416(2) . . ? C131 H116 2.558(18) . . ? C131 H132 2.00(2) . . ? C131 H136 1.997(18) . . ? C132 C134 2.402(2) . . ? C132 C135 2.758(2) . . ? C132 C136 2.391(2) . . ? C132 H133 2.03(2) . . ? C133 C135 2.389(3) . . ? C133 C136 2.770(2) . . ? C133 H132 1.98(2) . . ? C133 H134 1.985(18) . . ? C134 C136 2.407(2) . . ? C134 H133 2.04(2) . . ? C134 H135 2.00(2) . . ? C135 H134 2.021(18) . . ? C135 H136 2.026(19) . . ? C136 H135 2.01(2) . . ? P2 C212 2.7912(18) . . ? P2 C216 2.8491(17) . . ? P2 C222 2.7550(16) . . ? P2 C226 2.8499(17) . . ? P2 C232 2.7656(18) . . ? P2 C236 2.847(2) . . ? C211 C213 2.417(2) . . ? C211 C214 2.800(2) . . ? C211 C215 2.423(2) . . ? C211 C221 2.815(2) . . ? C211 C231 2.891(2) . . ? C211 H212 2.00(2) . . ? C211 H216 2.03(2) . . ? C211 H236 2.63(2) . . ? C212 C214 2.404(3) . . ? C212 C215 2.770(2) . . ? C212 C216 2.397(2) . . ? C212 H213 2.03(2) . . ? C213 C215 2.391(2) . . ? C213 C216 2.766(2) . . ? C213 H212 1.97(2) . . ? C213 H214 2.05(2) . . ? C214 C216 2.404(2) . . ? C214 H213 2.03(2) . . ? C214 H215 1.99(2) . . ? C215 H214 2.03(2) . . ? C215 H216 2.00(2) . . ? C216 C221 2.994(2) . . ? C216 H215 2.02(2) . . ? C221 C223 2.418(2) . . ? C221 C224 2.789(2) . . ? C221 C225 2.410(2) . . ? C221 C231 2.875(2) . . ? C221 H216 2.54(2) . . ? C221 H222 2.045(18) . . ? C221 H226 2.02(2) . . ? C222 C224 2.400(3) . . ? C222 C225 2.767(3) . . ? C222 C226 2.407(2) . . ? C222 H223 2.04(2) . . ? C223 C225 2.397(3) . . ? C223 C226 2.781(2) . . ? C223 H222 2.021(18) . . ? C223 H224 2.06(2) . . ? C224 C226 2.410(2) . . ? C224 H223 2.03(2) . . ? C224 H225 2.02(2) . . ? C225 H224 2.05(2) . . ? C225 H226 2.010(19) . . ? C226 H225 2.01(2) . . ? C231 C233 2.419(2) . . ? C231 C234 2.787(2) . . ? C231 C235 2.414(3) . . ? C231 H226 2.69(2) . . ? C231 H232 2.05(2) . . ? C231 H236 2.04(2) . . ? C232 C234 2.393(3) . . ? C232 C235 2.763(3) . . ? C232 C236 2.397(3) . . ? C232 H233 2.02(2) . . ? C233 C235 2.389(3) . . ? C233 C236 2.772(3) . . ? C233 H232 2.03(2) . . ? C233 H234 1.98(2) . . ? C234 C236 2.402(3) . . ? C234 H233 2.00(2) . . ? C234 H235 2.01(2) . . ? C235 H234 1.99(2) . . ? C235 H236 2.05(2) . . ? C236 H235 1.93(2) . . ? N11 C13 2.124(2) . . ? N11 N14 2.221(2) . . ? N11 N21 2.5288(18) . . ? N11 H15 2.01(2) . . ? N11 H1a 2.187(19) . . ? N11 H1b 2.130(19) . . ? N12 N14 2.251(2) . . ? N12 C15 2.170(2) . . ? N12 B 2.583(2) . . ? N12 H13 1.990(18) . . ? C13 C15 2.076(2) . . ? C13 B 3.631(2) . . ? N14 H13 2.029(18) . . ? N14 H15 2.05(2) . . ? C15 B 2.615(3) . . ? N21 C23 2.118(2) . . ? N21 N24 2.216(2) . . ? N21 H25 1.980(19) . . ? N21 H1a 2.144(19) . . ? N21 H1b 2.15(2) . . ? N22 N24 2.2528(19) . . ? N22 C25 2.179(2) . . ? N22 B 2.550(2) . . ? N22 H23 2.02(2) . . ? C23 C25 2.076(2) . . ? C23 B 3.604(3) . . ? N24 H23 2.046(19) . . ? N24 H25 2.00(2) . . ? C25 B 2.621(2) . . ? B H114 3.30(2) . '4 665' ? B H125 3.32(2) . '4 565' ? B H212 3.04(2) . . ? B H225 3.07(2) . '2 755' ? B H15 2.85(2) . . ? B H25 2.86(2) . . ? H112 H113 2.29(3) . . ? H113 H114 2.30(3) . . ? H114 H115 2.36(3) . . ? H114 H136 2.32(3) . '1 455' ? H114 H1b 2.32(3) . '4 464' ? H115 H116 2.32(3) . . ? H122 H123 2.32(3) . . ? H123 H124 2.32(3) . . ? H124 H125 2.34(3) . . ? H125 H126 2.33(3) . . ? H132 H133 2.29(3) . . ? H133 H134 2.30(3) . . ? H134 H135 2.32(3) . . ? H135 H136 2.32(3) . . ? H212 H213 2.29(3) . . ? H212 H1a 2.30(3) . . ? H213 H214 2.34(3) . . ? H214 H215 2.30(3) . . ? H215 H216 2.29(3) . . ? H222 H223 2.32(3) . . ? H223 H224 2.36(3) . . ? H224 H225 2.34(3) . . ? H225 H226 2.29(3) . . ? H232 H233 2.33(3) . . ? H233 H234 2.28(3) . . ? H234 H235 2.33(3) . . ? H235 H236 2.25(3) . . ? H1a H1b 1.86(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 1528 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 32 _reflns_limit_l_min -36 _reflns_limit_l_max 36 _reflns_number_observed ? _reflns_d_resolution_high .582 _reflns_d_resolution_low 14.228 _diffrn_reflns_av_sigmaI/netI .134 _diffrn_reflns_theta_min 1.43 _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 .086 _refine_ls_wR_factor_all .041 _refine_ls_goodness_of_fit_all .928 _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 loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_cpdar2 _database_code_CSD 176917 _audit_creation_method Xtal3.6 _audit_creation_date 01-09-28 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C27.5 H28.5 B1 Cl1.5 Cu1 N9 P1' _chemical_formula_moiety ? _chemical_formula_weight 643.6 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C2/c' _symmetry_space_group_name_Hall '-c_2yc' loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,+y,1/2-z -x,-y,-z +x,-y,1/2+z 1/2+x,1/2+y,+z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 15.708(5) _cell_length_b 14.299(4) _cell_length_c 27.283(8) _cell_angle_alpha 90.00000 _cell_angle_beta 95.611(8) _cell_angle_gamma 90.00000 _cell_volume 6099(3) _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 1.402 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 7379 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 19.3 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu .935 _exptl_crystal_description prism _exptl_crystal_size_max .35 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .16 _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 .49 _exptl_absorpt_correction_T_max .83 _diffrn_reflns_number 62156 _reflns_number_total 9944 _reflns_Friedel_coverage 0 _reflns_number_gt 6369 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 31.25 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .105 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 39 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .075 _refine_ls_wR_factor_ref .078 _refine_ls_goodness_of_fit_ref 1.383 _refine_ls_number_reflns 3583 _refine_ls_number_parameters 375 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .04 _refine_diff_density_min -1.116 _refine_diff_density_max 1.39 _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 ? 0 220 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 228 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 12 .132 .159 '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' N ? 0 72 .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 1.06085(7) .74539(6) .11936(3) .0279(6) Uani ? ? 1.00000 ? ? P .94022(15) .74244(11) .07357(5) .0234(12) Uani ? ? 1.00000 ? ? C111 .8644(6) .8325(4) .0900(2) .022(4) Uani ? ? 1.00000 ? ? C112 .8490(6) .8468(5) .1399(2) .028(5) Uani ? ? 1.00000 ? ? C1121 .8877(7) .7847(6) .1808(2) .044(6) Uani ? ? 1.00000 ? ? C113 .7973(6) .9201(5) .1509(3) .040(5) Uani ? ? 1.00000 ? ? C114 .7581(6) .9787(5) .1151(3) .039(5) Uani ? ? 1.00000 ? ? C115 .7722(6) .9640(5) .0658(3) .035(5) Uani ? ? 1.00000 ? ? C116 .8242(6) .8915(4) .0545(2) .026(5) Uani ? ? 1.00000 ? ? C121 .8823(5) .6320(4) .0749(2) .017(4) Uani ? ? 1.00000 ? ? C122 .9220(5) .5462(4) .0693(2) .021(4) Uani ? ? 1.00000 ? ? C1221 1.0156(6) .5409(5) .0626(3) .034(5) Uani ? ? 1.00000 ? ? C123 .8740(6) .4643(4) .0695(2) .031(5) Uani ? ? 1.00000 ? ? C124 .7876(6) .4658(5) .0750(3) .034(5) Uani ? ? 1.00000 ? ? C125 .7485(6) .5495(5) .0812(3) .039(5) Uani ? ? 1.00000 ? ? C126 .7953(6) .6323(4) .0804(2) .022(4) Uani ? ? 1.00000 ? ? C131 .9456(6) .7627(4) .0069(2) .023(4) Uani ? ? 1.00000 ? ? C132 .9961(6) .8352(4) -.0092(2) .028(5) Uani ? ? 1.00000 ? ? C1321 1.0502(6) .8983(5) .0251(3) .039(5) Uani ? ? 1.00000 ? ? C133 .9955(6) .8495(5) -.0601(2) .034(5) Uani ? ? 1.00000 ? ? C134 .9463(6) .7945(5) -.0940(2) .037(5) Uani ? ? 1.00000 ? ? C135 .8986(6) .7226(5) -.0779(2) .031(5) Uani ? ? 1.00000 ? ? C136 .8969(6) .7067(4) -.0274(2) .028(5) Uani ? ? 1.00000 ? ? B 1.2351(7) .7563(6) .1831(2) .030(5) Uani ? ? 1.00000 ? ? N11 1.1889(5) .8506(4) .18361(18) .031(4) Uani ? ? 1.00000 ? ? N12 1.1080(5) .8621(4) .15979(19) .034(4) Uani ? ? 1.00000 ? ? C13 1.0898(7) .9498(5) .1684(3) .046(6) Uani ? ? 1.00000 ? ? N14 1.1506(6) .9971(4) .1963(2) .050(5) Uani ? ? 1.00000 ? ? C15 1.2097(7) .9327(5) .2045(2) .046(5) Uani ? ? 1.00000 ? ? N21 1.1803(5) .6795(4) .20181(17) .026(4) Uani ? ? 1.00000 ? ? N22 1.0999(5) .6617(4) .18040(17) .024(4) Uani ? ? 1.00000 ? ? C23 1.0739(6) .5905(5) .2054(2) .034(5) Uani ? ? 1.00000 ? ? N24 1.1324(5) .5596(4) .2419(2) .041(4) Uani ? ? 1.00000 ? ? C25 1.1969(6) .6167(5) .2383(2) .037(5) Uani ? ? 1.00000 ? ? N31 1.2500(5) .7336(4) .12889(18) .026(4) Uani ? ? 1.00000 ? ? N32 1.1799(4) .7243(4) .09429(17) .022(4) Uani ? ? 1.00000 ? ? C33 1.2178(6) .7081(5) .0531(2) .028(5) Uani ? ? 1.00000 ? ? N34 1.3027(5) .7071(4) .05816(19) .032(4) Uani ? ? 1.00000 ? ? C35 1.3206(6) .7232(5) .1062(3) .039(5) Uani ? ? 1.00000 ? ? C10 1.00000 1.3045(10) .25000 .126(11) Uiso ? ? .50000 ? ? Cl11 .9701(7) 1.3634(6) .1930(3) .053(2) Uiso ? ? .25000 ? ? Cl12 1.0346(10) 1.3441(9) .2099(5) .114(5) Uiso ? ? .25000 ? ? Cl13 .983(2) 1.2096(19) .2479(7) .279(13) Uiso ? ? .25000 ? ? C20 1.00000 1.1404(8) .25000 .126(11) Uiso ? ? .50000 ? ? Cl21 .9421(9) 1.0955(11) .2070(5) .239(6) Uiso ? ? .50000 ? ? Cl22 .9291(12) 1.2064(13) .2738(7) .239(6) Uiso ? ? .25000 ? ? H1121a .86265 .80967 .20596 .11300 Uiso ? ? 1.00000 ? ? H1121b .95613 .79368 .18654 .06500 Uiso ? ? 1.00000 ? ? H1121c .87396 .72046 .17364 .04700 Uiso ? ? 1.00000 ? ? H113 .78460 .93524 .18131 .05300 Uiso ? ? 1.00000 ? ? H114 .72136 1.03032 .12149 .03000 Uiso ? ? 1.00000 ? ? H115 .74763 .99866 .04749 .04500 Uiso ? ? 1.00000 ? ? H116 .83030 .87706 .02158 .04200 Uiso ? ? 1.00000 ? ? H1221a 1.02781 .58396 .03623 .01600 Uiso ? ? 1.00000 ? ? H1221b 1.03068 .48301 .06072 .04200 Uiso ? ? 1.00000 ? ? H1221c 1.05615 .56653 .09039 .03900 Uiso ? ? 1.00000 ? ? H123 .90109 .40851 .06721 .01600 Uiso ? ? 1.00000 ? ? H124 .76365 .41066 .07573 .02800 Uiso ? ? 1.00000 ? ? H125 .69409 .55223 .08473 .03400 Uiso ? ? 1.00000 ? ? H126 .76727 .68938 .08378 .02100 Uiso ? ? 1.00000 ? ? H1321a 1.09607 .86461 .03730 .11100 Uiso ? ? 1.00000 ? ? H1321b 1.01310 .93212 .05283 .07000 Uiso ? ? 1.00000 ? ? H1321c 1.07312 .95097 .01264 .06200 Uiso ? ? 1.00000 ? ? H133 1.02839 .90058 -.07148 .02600 Uiso ? ? 1.00000 ? ? H134 .94748 .81033 -.12739 .04700 Uiso ? ? 1.00000 ? ? H135 .86075 .68652 -.09948 .03200 Uiso ? ? 1.00000 ? ? H136 .85690 .65807 -.01780 .02700 Uiso ? ? 1.00000 ? ? H13 1.04361 .97355 .15724 .03400 Uiso ? ? 1.00000 ? ? H15 1.26172 .93923 .21935 .03300 Uiso ? ? 1.00000 ? ? H23 1.02068 .56240 .19709 .02000 Uiso ? ? 1.00000 ? ? H25 1.24621 .61838 .25605 .03400 Uiso ? ? 1.00000 ? ? H33 1.18032 .70144 .02279 .01800 Uiso ? ? 1.00000 ? ? H35 1.37594 .72655 .12219 .04400 Uiso ? ? 1.00000 ? ? H 1.29049 .76010 .20453 .03600 Uiso ? ? 1.00000 ? ? H10 .95090 1.34706 .23465 .16400 Uiso ? ? .25000 ? ? H20 1.03444 1.18263 .23107 .17700 Uiso ? ? .25000 ? ? 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 .0329(10) .0300(4) .0205(3) .0004(5) .0007(4) .0007(3) P .029(2) .0230(7) .0190(6) .0008(10) .0048(8) .0007(6) C111 .016(8) .025(3) .026(3) -.003(4) .006(3) -.002(2) C112 .024(9) .036(3) .027(3) .002(4) .009(4) .001(3) C1121 .058(10) .053(4) .023(3) .013(5) .010(4) .007(3) C113 .049(9) .044(4) .030(3) .005(5) .014(4) -.008(3) C114 .047(9) .032(3) .040(4) .008(4) .013(4) -.010(3) C115 .041(9) .025(3) .038(4) .006(4) -.003(4) .001(3) C116 .025(8) .029(3) .024(3) -.004(4) .003(3) -.004(2) C121 .005(8) .027(3) .020(3) .000(3) .001(3) .004(2) C122 .009(8) .031(3) .023(3) .003(4) .005(3) .001(2) C1221 .034(9) .026(3) .041(4) .006(4) -.005(4) -.005(3) C123 .028(9) .027(3) .035(3) -.000(4) -.004(4) .004(3) C124 .022(9) .033(3) .046(4) -.014(4) .001(4) .005(3) C125 .033(9) .043(4) .041(4) -.002(5) .011(4) .009(3) C126 .008(8) .029(3) .028(3) .004(4) .003(3) .004(2) C131 .022(8) .027(3) .022(3) .007(4) .004(3) -.002(2) C132 .035(8) .029(3) .021(3) .004(4) .005(3) .003(2) C1321 .054(9) .028(3) .034(3) -.001(4) -.003(4) .010(3) C133 .041(9) .034(3) .028(3) .009(4) .011(4) .008(3) C134 .050(9) .045(4) .019(3) .008(5) .011(4) .004(3) C135 .032(9) .040(4) .023(3) .001(4) .002(4) -.006(2) C136 .030(9) .029(3) .024(3) .001(4) .002(4) .001(2) B .030(10) .036(4) .022(3) .000(5) -.005(4) -.002(3) N11 .037(7) .033(3) .022(2) -.002(3) .001(3) -.004(2) N12 .043(7) .033(3) .026(3) .000(3) .003(3) -.002(2) C13 .061(10) .037(4) .038(4) .011(5) -.000(4) -.003(3) N14 .064(8) .033(3) .050(4) .000(4) -.008(4) -.013(3) C15 .071(10) .038(4) .028(3) -.008(5) -.005(4) -.007(3) N21 .027(7) .032(3) .018(2) -.001(3) -.000(3) -.000(2) N22 .016(6) .039(3) .019(2) -.002(3) .007(3) .003(2) C23 .029(9) .041(4) .031(3) -.003(4) .003(4) .006(3) N24 .045(7) .046(4) .033(3) .005(4) .007(3) .015(3) C25 .044(9) .038(4) .028(3) .000(4) .001(4) .004(3) N31 .023(7) .032(3) .025(2) -.002(3) .008(3) .001(2) N32 .013(6) .033(3) .018(2) -.001(3) .001(3) .0000(19) C33 .029(8) .034(3) .021(3) -.001(4) .010(3) .001(2) N34 .021(7) .050(3) .027(3) -.001(4) .012(3) .003(2) C35 .044(9) .039(4) .033(3) -.002(4) .004(4) .005(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 . . 2.166(2) ? Cu N12 . . 2.096(6) ? Cu N22 . . 2.093(5) ? Cu N32 . . 2.075(7) ? P C111 . . 1.839(8) ? P C121 . . 1.825(7) ? P C131 . . 1.853(6) ? C111 C112 . . 1.421(9) ? C111 C116 . . 1.388(9) ? C112 C1121 . . 1.508(10) ? C112 C113 . . 1.377(12) ? C1121 H1121a . . .897 ? C1121 H1121b . . 1.079 ? C1121 H1121c . . .959 ? C113 C114 . . 1.384(10) ? C113 H113 . . .898 ? C114 C115 . . 1.401(10) ? C114 H114 . . .963 ? C115 C116 . . 1.375(11) ? C115 H115 . . .778 ? C116 H116 . . .935 ? C121 C122 . . 1.391(9) ? C121 C126 . . 1.390(12) ? C122 C1221 . . 1.502(13) ? C122 C123 . . 1.392(10) ? C1221 H1221a . . .979 ? C1221 H1221b . . .864 ? C1221 H1221c . . 1.010 ? C123 C124 . . 1.380(13) ? C123 H123 . . .910 ? C124 C125 . . 1.364(11) ? C124 H124 . . .874 ? C125 C126 . . 1.394(11) ? C125 H125 . . .870 ? C126 H126 . . .936 ? C131 C132 . . 1.401(10) ? C131 C136 . . 1.399(9) ? C132 C1321 . . 1.503(10) ? C132 C133 . . 1.403(9) ? C1321 H1321a . . .903 ? C1321 H1321b . . 1.108 ? C1321 H1321c . . .915 ? C133 C134 . . 1.390(10) ? C133 H133 . . .964 ? C134 C135 . . 1.370(11) ? C134 H134 . . .940 ? C135 C136 . . 1.401(9) ? C135 H135 . . .947 ? C136 H136 . . .989 ? B N11 . . 1.532(11) ? B N21 . . 1.516(11) ? B N31 . . 1.553(9) ? B H . . 1.001 ? N11 N12 . . 1.379(10) ? N11 C15 . . 1.332(9) ? N12 C13 . . 1.312(10) ? C13 N14 . . 1.344(11) ? C13 H13 . . .832 ? N14 C15 . . 1.311(12) ? C15 H15 . . .881 ? N21 N22 . . 1.363(9) ? N21 C25 . . 1.346(8) ? N22 C23 . . 1.313(9) ? C23 N24 . . 1.359(10) ? C23 H23 . . .936 ? N24 C25 . . 1.313(12) ? C25 H25 . . .873 ? N31 N32 . . 1.385(8) ? N31 C35 . . 1.330(12) ? N32 C33 . . 1.341(9) ? C33 N34 . . 1.328(12) ? C33 H33 . . .972 ? N34 C35 . . 1.333(9) ? C35 H35 . . .936 ? C10 Cl11 . . 1.793(11) ? C10 Cl12 . . 1.387(16) ? C10 Cl13 . . 1.38(3) ? C10 H10 . . 1.040 ? C10 Cl11 . 2 1.793(11) ? C10 Cl12 . 2 1.387(16) ? C10 Cl13 . 2 1.38(3) ? C10 H10 . 2 1.040 ? C20 Cl21 . . 1.553(15) ? C20 Cl22 . . 1.64(2) ? C20 H20 . . .987 ? C20 Cl21 . 2 1.553(15) ? C20 Cl22 . 2 1.64(2) ? C20 H20 . 2 .987 ? 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 . . . 124.3(2) ? P Cu N22 . . . 128.3(2) ? P Cu N32 . . . 124.96(15) ? N12 Cu N22 . . . 88.6(2) ? N12 Cu N32 . . . 90.3(3) ? N22 Cu N32 . . . 88.6(2) ? Cu P C111 . . . 113.4(2) ? Cu P C121 . . . 114.5(2) ? Cu P C131 . . . 116.3(3) ? C111 P C121 . . . 105.4(4) ? C111 P C131 . . . 102.8(3) ? C121 P C131 . . . 103.0(3) ? P C111 C112 . . . 120.6(5) ? P C111 C116 . . . 121.1(5) ? C112 C111 C116 . . . 118.2(7) ? C111 C112 C1121 . . . 122.1(7) ? C111 C112 C113 . . . 118.5(6) ? C1121 C112 C113 . . . 119.4(6) ? C112 C1121 H1121a . . . 99.0 ? C112 C1121 H1121b . . . 111.1 ? C112 C1121 H1121c . . . 110.2 ? H1121a C1121 H1121b . . . 110.3 ? H1121a C1121 H1121c . . . 115.6 ? H1121b C1121 H1121c . . . 110.2 ? C112 C113 C114 . . . 122.6(7) ? C112 C113 H113 . . . 125.0 ? C114 C113 H113 . . . 112.4 ? C113 C114 C115 . . . 119.0(7) ? C113 C114 H114 . . . 124.8 ? C115 C114 H114 . . . 116.2 ? C114 C115 C116 . . . 118.8(6) ? C114 C115 H115 . . . 114.0 ? C116 C115 H115 . . . 127.2 ? C111 C116 C115 . . . 122.8(6) ? C111 C116 H116 . . . 117.0 ? C115 C116 H116 . . . 120.0 ? P C121 C122 . . . 122.1(6) ? P C121 C126 . . . 119.8(5) ? C122 C121 C126 . . . 118.1(6) ? C121 C122 C1221 . . . 120.8(6) ? C121 C122 C123 . . . 119.5(8) ? C1221 C122 C123 . . . 119.7(6) ? C122 C1221 H1221a . . . 108.8 ? C122 C1221 H1221b . . . 109.4 ? C122 C1221 H1221c . . . 116.3 ? H1221a C1221 H1221b . . . 119.0 ? H1221a C1221 H1221c . . . 99.7 ? H1221b C1221 H1221c . . . 103.6 ? C122 C123 C124 . . . 121.7(7) ? C122 C123 H123 . . . 118.7 ? C124 C123 H123 . . . 119.5 ? C123 C124 C125 . . . 119.1(7) ? C123 C124 H124 . . . 114.7 ? C125 C124 H124 . . . 126.1 ? C124 C125 C126 . . . 119.9(9) ? C124 C125 H125 . . . 120.8 ? C126 C125 H125 . . . 119.2 ? C121 C126 C125 . . . 121.6(7) ? C121 C126 H126 . . . 119.3 ? C125 C126 H126 . . . 119.1 ? P C131 C132 . . . 120.3(5) ? P C131 C136 . . . 119.4(5) ? C132 C131 C136 . . . 120.3(5) ? C131 C132 C1321 . . . 123.5(5) ? C131 C132 C133 . . . 117.9(6) ? C1321 C132 C133 . . . 118.6(7) ? C132 C1321 H1321a . . . 106.9 ? C132 C1321 H1321b . . . 112.6 ? C132 C1321 H1321c . . . 118.7 ? H1321a C1321 H1321b . . . 115.9 ? H1321a C1321 H1321c . . . 104.3 ? H1321b C1321 H1321c . . . 98.5 ? C132 C133 C134 . . . 121.8(7) ? C132 C133 H133 . . . 118.5 ? C134 C133 H133 . . . 119.7 ? C133 C134 C135 . . . 119.8(6) ? C133 C134 H134 . . . 116.5 ? C135 C134 H134 . . . 123.7 ? C134 C135 C136 . . . 120.1(6) ? C134 C135 H135 . . . 122.6 ? C136 C135 H135 . . . 116.9 ? C131 C136 C135 . . . 120.1(7) ? C131 C136 H136 . . . 123.1 ? C135 C136 H136 . . . 116.6 ? N11 B N21 . . . 110.4(8) ? N11 B N31 . . . 108.0(5) ? N11 B H . . . 109.4 ? N21 B N31 . . . 108.3(6) ? N21 B H . . . 109.4 ? N31 B H . . . 111.4 ? B N11 N12 . . . 121.1(6) ? B N11 C15 . . . 133.1(7) ? N12 N11 C15 . . . 105.8(6) ? Cu N12 N11 . . . 114.5(4) ? Cu N12 C13 . . . 141.6(6) ? N11 N12 C13 . . . 103.7(6) ? N12 C13 N14 . . . 115.3(8) ? N12 C13 H13 . . . 121.5 ? N14 C13 H13 . . . 123.2 ? C13 N14 C15 . . . 101.2(6) ? N11 C15 N14 . . . 114.0(8) ? N11 C15 H15 . . . 117.9 ? N14 C15 H15 . . . 127.8 ? B N21 N22 . . . 121.6(5) ? B N21 C25 . . . 131.1(7) ? N22 N21 C25 . . . 107.3(6) ? Cu N22 N21 . . . 114.9(4) ? Cu N22 C23 . . . 140.9(6) ? N21 N22 C23 . . . 104.1(6) ? N22 C23 N24 . . . 114.3(8) ? N22 C23 H23 . . . 121.4(7) ? N24 C23 H23 . . . 124.2 ? C23 N24 C25 . . . 102.3(6) ? N21 C25 N24 . . . 112.0(7) ? N21 C25 H25 . . . 119.3 ? N24 C25 H25 . . . 128.7 ? B N31 N32 . . . 119.0(7) ? B N31 C35 . . . 132.6(7) ? N32 N31 C35 . . . 108.3(5) ? Cu N32 N31 . . . 116.3(4) ? Cu N32 C33 . . . 142.0(5) ? N31 N32 C33 . . . 101.5(6) ? N32 C33 N34 . . . 116.0(6) ? N32 C33 H33 . . . 116.7 ? N34 C33 H33 . . . 127.2 ? C33 N34 C35 . . . 102.3(7) ? N31 C35 N34 . . . 111.9(8) ? N31 C35 H35 . . . 123.7 ? N34 C35 H35 . . . 124.4 ? Cl11 C10 Cl12 . . . 113.7(10) ? Cl11 C10 Cl13 . . . 113.2(10) ? Cl11 C10 H10 . . . 101.2 ? Cl12 C10 Cl13 . . . 110.1(13) ? Cl12 C10 H10 . . . 76.69 ? Cl13 C10 H10 . . . 136.7 ? Cl21 C20 Cl22 . . . 107.9(9) ? Cl21 C20 Cl21 . . 2 131(1) ? Cl22 C20 Cl21 . . 2 99.8(8) ? Cl21 C20 H20 . . . 109.7 ? Cl22 C20 H20 . . . 106.6) ? H20 C20 Cl21 . . 2 99.6 ? 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 #-------------------------------------------------------------------------- _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 2648 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 22 _reflns_limit_k_min 0 _reflns_limit_k_max 20 _reflns_limit_l_min -39 _reflns_limit_l_max 39 _reflns_number_observed ? _reflns_d_resolution_high .685 _reflns_d_resolution_low 13.539 _diffrn_reflns_av_sigmaI/netI .12 _diffrn_reflns_theta_min 1.5 _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 atomblock _refine_ls_number_restraints 9 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .105 _refine_ls_wR_factor_all .084 _refine_ls_goodness_of_fit_all 1.228 _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 loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_cpdar6 _database_code_CSD 176918 _audit_creation_method Xtal3.6 _audit_creation_date 01-05-08 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C48 H49 B1 Cu1 N9 P2' _chemical_formula_moiety ? _chemical_formula_weight 888.29 _chemical_melting_point ? _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P212121' _symmetry_space_group_name_Hall 'p_2ac_2ab' loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z _cell_length_a 10.2010(8) _cell_length_b 19.5500(16) _cell_length_c 22.3910(18) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 4465.4(6) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.321 _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 .606 _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 .733 _exptl_absorpt_correction_T_max .863 _diffrn_reflns_number 23479 _reflns_number_total 12705 _reflns_Friedel_coverage .85 _reflns_number_gt 7496 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 37.57 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .076 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 38 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .049 _refine_ls_wR_factor_ref .044 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_number_reflns 7153 _refine_ls_number_parameters 551 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .002 _refine_diff_density_min -.81 _refine_diff_density_max 1.255 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack xabs refined' _refine_ls_abs_structure_Flack -.010(12) # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 192 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 196 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 36 .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' Cu ? 0 4 .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 .14846(4) .04302(2) .963816(18) .01796(17) Uani ? ? 1.00000 ? ? P1 .17172(10) -.05006(5) 1.02295(4) .0196(4) Uani ? ? 1.00000 ? ? P2 .23082(9) .03572(5) .86942(4) .0179(4) Uani ? ? 1.00000 ? ? C111 .3345(4) -.05289(18) 1.05754(16) .0251(18) Uani ? ? 1.00000 ? ? C112 .3586(5) -.0797(2) 1.11435(18) .030(2) Uani ? ? 1.00000 ? ? C113 .4879(5) -.0780(2) 1.1382(2) .033(2) Uani ? ? 1.00000 ? ? C1131 .5140(6) -.1068(3) 1.1988(2) .041(3) Uani ? ? 1.00000 ? ? C114 .5863(5) -.0497(3) 1.1038(2) .040(3) Uani ? ? 1.00000 ? ? C115 .5630(5) -.0241(3) 1.0480(2) .045(3) Uani ? ? 1.00000 ? ? C116 .4372(4) -.0252(2) 1.0249(2) .034(2) Uani ? ? 1.00000 ? ? C121 .0622(4) -.05715(19) 1.08710(16) .0220(17) Uani ? ? 1.00000 ? ? C122 .0391(4) .0024(2) 1.12028(17) .0235(18) Uani ? ? 1.00000 ? ? C123 -.0369(4) .0011(2) 1.17289(18) .029(2) Uani ? ? 1.00000 ? ? C1231 -.0593(5) .0659(3) 1.2085(2) .041(3) Uani ? ? 1.00000 ? ? C124 -.0902(4) -.0606(3) 1.19045(19) .036(2) Uani ? ? 1.00000 ? ? C125 -.0717(5) -.1195(3) 1.1576(2) .038(3) Uani ? ? 1.00000 ? ? C126 .0050(5) -.1180(2) 1.1061(2) .031(2) Uani ? ? 1.00000 ? ? C131 .1568(5) -.13339(18) .98705(16) .0275(19) Uani ? ? 1.00000 ? ? C132 .0551(5) -.1429(2) .9467(2) .034(2) Uani ? ? 1.00000 ? ? C133 .0358(6) -.2064(3) .9185(2) .042(3) Uani ? ? 1.00000 ? ? C1331 -.0708(7) -.2168(3) .8757(3) .058(4) Uani ? ? 1.00000 ? ? C134 .1214(7) -.2593(2) .9312(2) .051(3) Uani ? ? 1.00000 ? ? C135 .2217(7) -.2510(2) .9706(3) .053(3) Uani ? ? 1.00000 ? ? C136 .2393(6) -.1881(2) .9987(2) .041(3) Uani ? ? 1.00000 ? ? C211 .3902(4) -.00585(19) .86617(16) .0202(17) Uani ? ? 1.00000 ? ? C212 .3973(4) -.07741(19) .86983(18) .0229(18) Uani ? ? 1.00000 ? ? C213 .5163(4) -.1111(2) .87677(18) .027(2) Uani ? ? 1.00000 ? ? C2131 .5204(5) -.1883(2) .8800(3) .042(3) Uani ? ? 1.00000 ? ? C214 .6299(4) -.0728(2) .88097(18) .029(2) Uani ? ? 1.00000 ? ? C215 .6253(4) -.0019(2) .87707(19) .029(2) Uani ? ? 1.00000 ? ? C216 .5055(4) .0317(2) .86953(18) .0235(18) Uani ? ? 1.00000 ? ? C221 .2576(4) .11849(18) .83251(16) .0199(17) Uani ? ? 1.00000 ? ? C222 .2270(4) .17664(18) .86482(16) .0221(17) Uani ? ? 1.00000 ? ? C223 .2378(4) .2423(2) .84127(18) .0254(19) Uani ? ? 1.00000 ? ? C2231 .2029(6) .3030(2) .8798(2) .042(3) Uani ? ? 1.00000 ? ? C224 .2802(4) .2484(2) .78229(18) .028(2) Uani ? ? 1.00000 ? ? C225 .3130(5) .1908(2) .74932(18) .031(2) Uani ? ? 1.00000 ? ? C226 .3018(4) .1258(2) .77384(17) .027(2) Uani ? ? 1.00000 ? ? C231 .1323(4) -.01175(17) .81522(15) .0198(16) Uani ? ? 1.00000 ? ? C232 .1848(3) -.0398(2) .76292(15) .0213(16) Uani ? ? 1.00000 ? ? C233 .1058(4) -.0725(2) .72094(17) .025(2) Uani ? ? 1.00000 ? ? C2331 .1629(5) -.1004(2) .66381(17) .033(2) Uani ? ? 1.00000 ? ? C234 -.0270(5) -.0772(3) .73272(19) .034(2) Uani ? ? 1.00000 ? ? C235 -.0809(4) -.0506(3) .7845(2) .037(2) Uani ? ? 1.00000 ? ? C236 -.0018(4) -.0179(2) .82614(18) .027(2) Uani ? ? 1.00000 ? ? N11 .2433(3) .22775(15) 1.05117(14) .0215(15) Uani ? ? 1.00000 ? ? N12 .3700(3) .21069(15) 1.03734(16) .0248(15) Uani ? ? 1.00000 ? ? C13 .3586(4) .14979(18) 1.01189(16) .0230(17) Uani ? ? 1.00000 ? ? N14 .2321(3) .12651(15) 1.00852(13) .0212(15) Uani ? ? 1.00000 ? ? C15 .1644(4) .17742(17) 1.03353(17) .0222(16) Uani ? ? 1.00000 ? ? N21 .2926(3) .35238(16) 1.06303(14) .0218(15) Uani ? ? 1.00000 ? ? N22 .2539(4) .38994(18) 1.01426(16) .0302(18) Uani ? ? 1.00000 ? ? C23 .3563(4) .4279(2) 1.00298(17) .0277(19) Uani ? ? 1.00000 ? ? N24 .4588(3) .41833(15) 1.03987(15) .0217(14) Uani ? ? 1.00000 ? ? C25 .4143(4) .3703(2) 1.07672(19) .026(2) Uani ? ? 1.00000 ? ? N31 .2308(4) .28190(17) 1.15352(16) .0302(18) Uani ? ? 1.00000 ? ? N32 .3516(5) .2712(2) 1.17845(16) .040(2) Uani ? ? 1.00000 ? ? C33 .3213(7) .2552(3) 1.2350(2) .054(3) Uani ? ? 1.00000 ? ? N34 .1922(7) .2550(3) 1.2479(2) .064(3) Uani ? ? 1.00000 ? ? C35 .1404(7) .2718(3) 1.1962(2) .050(3) Uani ? ? 1.00000 ? ? B .2068(5) .2933(2) 1.0867(2) .024(2) Uani ? ? 1.00000 ? ? H112 .28733 -.09913 1.13777 .04200 Uiso ? ? 1.00000 ? ? H1131a .43354 -.12389 1.21608 .06400 Uiso ? ? 1.00000 ? ? H1131c .57494 -.14321 1.19693 .06400 Uiso ? ? 1.00000 ? ? H1131b .54704 -.07201 1.22475 .06400 Uiso ? ? 1.00000 ? ? H114 .67403 -.04693 1.11944 .04900 Uiso ? ? 1.00000 ? ? H115 .63299 -.00495 1.02449 .05900 Uiso ? ? 1.00000 ? ? H116 .42018 -.00635 .98616 .04300 Uiso ? ? 1.00000 ? ? H122 .07792 .04486 1.10671 .03100 Uiso ? ? 1.00000 ? ? H1231a -.13367 .09033 1.19364 .06200 Uiso ? ? 1.00000 ? ? H1231b .01575 .09646 1.20538 .06200 Uiso ? ? 1.00000 ? ? H1231c -.07203 .05543 1.24917 .06200 Uiso ? ? 1.00000 ? ? H124 -.14144 -.06243 1.22689 .04500 Uiso ? ? 1.00000 ? ? H125 -.11183 -.16182 1.16990 .04800 Uiso ? ? 1.00000 ? ? H126 .02185 -.15930 1.08416 .04100 Uiso ? ? 1.00000 ? ? H132 -.00535 -.10556 .93773 .04500 Uiso ? ? 1.00000 ? ? H1331a -.07965 -.26163 .86086 .08400 Uiso ? ? 1.00000 ? ? H1331c -.15427 -.20543 .89525 .08400 Uiso ? ? 1.00000 ? ? H1331b -.06292 -.18609 .84250 .08400 Uiso ? ? 1.00000 ? ? H134 .10903 -.30271 .91093 .06800 Uiso ? ? 1.00000 ? ? H135 .28009 -.28849 .97884 .06700 Uiso ? ? 1.00000 ? ? H136 .31296 -.18231 1.02692 .05500 Uiso ? ? 1.00000 ? ? H212 .31901 -.10438 .86663 .02900 Uiso ? ? 1.00000 ? ? H2131a .60534 -.20267 .89329 .06100 Uiso ? ? 1.00000 ? ? H2131c .45665 -.20520 .90847 .06100 Uiso ? ? 1.00000 ? ? H2131b .50216 -.20882 .84244 .06100 Uiso ? ? 1.00000 ? ? H214 .71072 -.09540 .88779 .03500 Uiso ? ? 1.00000 ? ? H215 .70493 .02409 .87861 .03600 Uiso ? ? 1.00000 ? ? H216 .50363 .08032 .86731 .02800 Uiso ? ? 1.00000 ? ? H222 .19468 .17146 .90543 .02900 Uiso ? ? 1.00000 ? ? H2231a .11881 .29484 .89750 .06500 Uiso ? ? 1.00000 ? ? H2231b .26607 .30760 .91076 .06500 Uiso ? ? 1.00000 ? ? H2231c .19841 .34519 .85810 .06500 Uiso ? ? 1.00000 ? ? H224 .28816 .29301 .76395 .03500 Uiso ? ? 1.00000 ? ? H225 .34398 .19588 .70933 .04000 Uiso ? ? 1.00000 ? ? H226 .32268 .08589 .75015 .03500 Uiso ? ? 1.00000 ? ? H232 .27649 -.03793 .75563 .02800 Uiso ? ? 1.00000 ? ? H2331a .14043 -.07208 .63065 .05000 Uiso ? ? 1.00000 ? ? H2331b .13391 -.14558 .65659 .05000 Uiso ? ? 1.00000 ? ? H2331c .25641 -.10042 .66802 .05000 Uiso ? ? 1.00000 ? ? H234 -.08300 -.09934 .70398 .04300 Uiso ? ? 1.00000 ? ? H235 -.17454 -.05449 .79114 .04700 Uiso ? ? 1.00000 ? ? H236 -.03963 .00021 .86184 .03400 Uiso ? ? 1.00000 ? ? H13 .43157 .12415 .99698 .02900 Uiso ? ? 1.00000 ? ? H15 .07034 .17738 1.03805 .02900 Uiso ? ? 1.00000 ? ? H23 .35820 .46175 .97119 .03400 Uiso ? ? 1.00000 ? ? H25 .46573 .35097 1.10885 .03300 Uiso ? ? 1.00000 ? ? H33 .38774 .24439 1.26346 .07100 Uiso ? ? 1.00000 ? ? H35 .04538 .27545 1.18897 .06400 Uiso ? ? 1.00000 ? ? H1 .11329 .30589 1.08033 .03000 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 .0218(2) .01580(16) .01630(17) .00098(19) .00048(18) -.00078(16) P1 .0264(5) .0163(4) .0161(4) -.0002(4) -.0005(3) .0000(3) P2 .0205(4) .0175(4) .0156(4) .0000(4) .0006(3) -.0008(3) C111 .035(2) .0180(16) .0228(16) .0065(16) -.0042(16) -.0036(13) C112 .040(2) .0231(17) .0269(18) .0071(19) -.005(2) .0005(14) C113 .049(3) .0239(19) .025(2) .0093(19) -.009(2) -.0025(16) C1131 .051(3) .041(3) .032(2) .010(2) -.008(2) .003(2) C114 .033(2) .042(3) .045(3) .003(2) -.008(2) .001(2) C115 .037(3) .054(3) .044(3) -.007(2) -.003(2) .008(2) C116 .030(2) .037(2) .033(2) -.0020(18) -.0018(18) .0006(18) C121 .0266(19) .0214(17) .0179(16) .0021(14) -.0014(14) .0038(13) C122 .023(2) .0300(19) .0175(17) .0019(16) -.0019(15) -.0002(14) C123 .023(2) .043(2) .0203(18) .0066(18) -.0032(16) -.0004(17) C1231 .041(3) .054(3) .027(2) .013(2) .001(2) -.010(2) C124 .030(2) .056(3) .0218(19) .008(2) .0031(17) .010(2) C125 .042(3) .041(3) .030(2) -.002(2) .003(2) .016(2) C126 .038(3) .027(2) .028(2) -.0003(18) .0007(18) .0075(16) C131 .043(2) .0190(16) .0208(16) -.0075(18) .005(2) -.0034(13) C132 .043(3) .030(2) .028(2) -.008(2) .000(2) -.0037(17) C133 .046(3) .045(3) .034(2) -.017(2) .003(2) -.009(2) C1331 .069(4) .049(3) .056(4) .001(3) -.016(3) -.014(3) C134 .080(5) .027(2) .046(3) -.007(3) .007(3) -.009(2) C135 .088(4) .024(2) .048(3) .004(2) .000(3) -.007(2) C136 .066(4) .0211(19) .036(2) .005(2) -.001(2) -.0041(17) C211 .023(2) .0225(16) .0153(15) .0016(14) .0016(14) -.0016(13) C212 .027(2) .0193(16) .0227(17) .0006(14) .0014(16) -.0012(14) C213 .031(2) .0250(19) .023(2) .0058(17) -.0005(17) .0009(15) C2131 .045(3) .025(2) .056(3) .010(2) -.001(3) .001(2) C214 .025(2) .034(2) .027(2) .0092(17) -.0007(17) -.0013(16) C215 .024(2) .033(2) .029(2) -.0005(17) .0012(17) -.0047(17) C216 .025(2) .0217(18) .0234(18) -.0012(15) .0015(15) -.0029(14) C221 .0195(18) .0201(16) .0201(16) -.0004(14) -.0007(14) .0021(13) C222 .027(2) .0220(16) .0175(16) .0010(15) .0004(15) .0011(13) C223 .032(2) .0204(16) .0244(18) .0006(16) .0008(16) .0009(14) C2231 .072(4) .0197(18) .034(2) .008(2) .008(2) .0016(17) C224 .038(2) .0221(17) .0229(18) -.0031(17) -.0013(17) .0065(14) C225 .041(3) .031(2) .0206(18) -.0056(18) .0061(17) .0033(15) C226 .034(2) .0248(18) .0211(17) -.0024(16) .0060(16) -.0012(14) C231 .024(2) .0186(14) .0174(15) -.0011(14) -.0016(14) .0010(12) C232 .0221(16) .0199(15) .0219(15) -.0018(15) .0025(13) -.0019(15) C233 .037(2) .0213(17) .0176(16) -.0009(16) .0007(16) -.0015(14) C2331 .046(3) .032(2) .0217(18) -.004(2) .006(2) -.0072(15) C234 .035(2) .046(3) .022(2) -.010(2) -.0046(18) -.0078(18) C235 .025(2) .055(3) .029(2) -.009(2) .0008(16) -.009(2) C236 .024(2) .037(2) .0208(18) -.0030(17) .0038(15) -.0049(16) N11 .0224(16) .0193(14) .0229(15) -.0013(12) .0007(12) -.0044(11) N12 .0236(16) .0233(13) .0276(15) -.0009(12) .0029(15) -.0039(13) C13 .0255(19) .0224(16) .0212(16) -.0005(16) .0020(16) -.0025(13) N14 .0286(17) .0177(13) .0174(14) -.0025(13) -.0002(13) -.0020(11) C15 .0245(19) .0201(14) .0219(15) -.0042(14) .0008(17) -.0025(13) N21 .0221(16) .0186(14) .0248(15) -.0001(12) -.0011(13) -.0045(12) N22 .0268(19) .037(2) .0268(17) -.0025(15) -.0028(14) .0035(15) C23 .026(2) .0314(19) .0261(18) .0010(18) .0006(18) .0009(15) N24 .0243(16) .0195(13) .0214(14) -.0021(12) .0028(14) -.0018(13) C25 .024(2) .0247(18) .030(2) -.0010(16) -.0024(17) .0019(16) N31 .039(2) .0245(16) .0271(17) -.0050(16) .0073(16) -.0063(13) N32 .053(3) .039(2) .0292(18) -.010(2) -.007(2) -.0019(15) C33 .095(5) .041(3) .026(2) -.007(3) -.007(3) -.004(2) N34 .102(5) .060(3) .031(2) .007(3) .026(3) -.004(2) C35 .066(4) .043(3) .041(3) .008(3) .027(3) -.002(2) B .023(2) .0198(19) .029(2) -.0010(16) .0027(17) -.0051(16) # 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 . . 2.2631(10) ? Cu P2 . . 2.2790(10) ? Cu N14 . . 2.096(3) ? Cu N24 . '3 457' 2.079(3) ? P1 C111 . . 1.833(4) ? P1 C121 . . 1.825(4) ? P1 C131 . . 1.823(4) ? P2 C211 . . 1.820(4) ? P2 C221 . . 1.837(4) ? P2 C231 . . 1.828(4) ? C111 C112 . . 1.397(5) ? C111 C116 . . 1.386(6) ? C112 C113 . . 1.423(7) ? C112 H112 . . .973 ? C113 C1131 . . 1.493(7) ? C113 C114 . . 1.381(7) ? C1131 H1131a . . .967 ? C1131 H1131c . . .946 ? C1131 H1131b . . .957 ? C114 C115 . . 1.367(7) ? C114 H114 . . .962 ? C115 C116 . . 1.384(7) ? C115 H115 . . .963 ? C116 H116 . . .960 ? C121 C122 . . 1.400(5) ? C121 C126 . . 1.391(6) ? C122 C123 . . 1.410(6) ? C122 H122 . . .969 ? C123 C1231 . . 1.513(7) ? C123 C124 . . 1.382(7) ? C1231 H1231a . . .956 ? C1231 H1231b . . .974 ? C1231 H1231c . . .942 ? C124 C125 . . 1.378(7) ? C124 H124 . . .969 ? C125 C126 . . 1.395(7) ? C125 H125 . . .963 ? C126 H126 . . .961 ? C131 C132 . . 1.387(7) ? C131 C136 . . 1.386(6) ? C132 C133 . . 1.407(7) ? C132 H132 . . .977 ? C133 C1331 . . 1.462(8) ? C133 C134 . . 1.383(8) ? C1331 H1331a . . .942 ? C1331 H1331c . . .983 ? C1331 H1331b . . .960 ? C134 C135 . . 1.361(9) ? C134 H134 . . .970 ? C135 C136 . . 1.392(6) ? C135 H135 . . .963 ? C136 H136 . . .989 ? C211 C212 . . 1.403(5) ? C211 C216 . . 1.388(5) ? C212 C213 . . 1.390(6) ? C212 H212 . . .959 ? C213 C2131 . . 1.510(6) ? C213 C214 . . 1.384(6) ? C2131 H2131a . . .958 ? C2131 H2131c . . .969 ? C2131 H2131b . . .951 ? C214 C215 . . 1.389(6) ? C214 H214 . . .948 ? C215 C216 . . 1.397(6) ? C215 H215 . . .959 ? C216 H216 . . .952 ? C221 C222 . . 1.383(5) ? C221 C226 . . 1.396(5) ? C222 C223 . . 1.393(5) ? C222 H222 . . .972 ? C223 C2231 . . 1.509(6) ? C223 C224 . . 1.395(6) ? C2231 H2231a . . .959 ? C2231 H2231b . . .951 ? C2231 H2231c . . .957 ? C224 C225 . . 1.389(6) ? C224 H224 . . .967 ? C225 C226 . . 1.389(6) ? C225 H225 . . .955 ? C226 H226 . . .967 ? C231 C232 . . 1.400(5) ? C231 C236 . . 1.395(6) ? C232 C233 . . 1.392(5) ? C232 H232 . . .951 ? C233 C2331 . . 1.508(6) ? C233 C234 . . 1.383(7) ? C2331 H2331a . . .954 ? C2331 H2331b . . .945 ? C2331 H2331c . . .958 ? C234 C235 . . 1.385(6) ? C234 H234 . . .964 ? C235 C236 . . 1.389(6) ? C235 H235 . . .969 ? C236 H236 . . .956 ? N11 N12 . . 1.371(5) ? N11 C15 . . 1.331(5) ? N11 B . . 1.553(5) ? N12 C13 . . 1.325(5) ? C13 N14 . . 1.371(5) ? C13 H13 . . .957 ? N14 C15 . . 1.335(5) ? C15 H15 . . .965 ? N21 N22 . . 1.374(5) ? N21 C25 . . 1.327(5) ? N21 B . . 1.543(5) ? N22 C23 . . 1.306(6) ? C23 N24 . . 1.346(5) ? C23 H23 . . .972 ? N24 C25 . . 1.329(5) ? C25 H25 . . .967 ? N31 N32 . . 1.369(6) ? N31 C35 . . 1.342(7) ? N31 B . . 1.532(6) ? N32 C33 . . 1.340(6) ? C33 N34 . . 1.349(10) ? C33 H33 . . .954 ? N34 C35 . . 1.314(7) ? C35 H35 . . .986 ? B H1 . . .995 ? 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 P2 . . . 116.98(4) ? P1 Cu N14 . . . 107.70(9) ? P1 Cu N24 . . '3 457' 114.40(9) ? P2 Cu N14 . . . 109.97(9) ? P2 Cu N24 . . '3 457' 109.21(10) ? N14 Cu N24 . . '3 457' 96.60(13) ? Cu P1 C111 . . . 111.49(12) ? Cu P1 C121 . . . 117.22(13) ? Cu P1 C131 . . . 116.86(12) ? C111 P1 C121 . . . 102.70(17) ? C111 P1 C131 . . . 103.6(2) ? C121 P1 C131 . . . 103.18(18) ? Cu P2 C211 . . . 113.24(12) ? Cu P2 C221 . . . 114.63(12) ? Cu P2 C231 . . . 116.40(13) ? C211 P2 C221 . . . 104.04(17) ? C211 P2 C231 . . . 103.76(17) ? C221 P2 C231 . . . 103.31(16) ? P1 C111 C112 . . . 123.7(3) ? P1 C111 C116 . . . 116.8(3) ? C112 C111 C116 . . . 119.5(4) ? C111 C112 C113 . . . 119.7(4) ? C111 C112 H112 . . . 120.4 ? C113 C112 H112 . . . 119.9 ? C112 C113 C1131 . . . 119.8(4) ? C112 C113 C114 . . . 118.3(4) ? C1131 C113 C114 . . . 121.9(5) ? C113 C1131 H1131a . . . 110.1 ? C113 C1131 H1131c . . . 111.2 ? C113 C1131 H1131b . . . 110.3 ? H1131a C1131 H1131c . . . 108.4 ? H1131a C1131 H1131b . . . 107.5 ? H1131c C1131 H1131b . . . 109.2 ? C113 C114 C115 . . . 122.0(5) ? C113 C114 H114 . . . 119.8 ? C115 C114 H114 . . . 118.3 ? C114 C115 C116 . . . 119.8(5) ? C114 C115 H115 . . . 120.9 ? C116 C115 H115 . . . 119.3 ? C111 C116 C115 . . . 120.7(4) ? C111 C116 H116 . . . 119.4 ? C115 C116 H116 . . . 119.9 ? P1 C121 C122 . . . 117.2(3) ? P1 C121 C126 . . . 124.2(3) ? C122 C121 C126 . . . 118.5(4) ? C121 C122 C123 . . . 121.4(4) ? C121 C122 H122 . . . 118.5 ? C123 C122 H122 . . . 120.1 ? C122 C123 C1231 . . . 120.6(4) ? C122 C123 C124 . . . 118.0(4) ? C1231 C123 C124 . . . 121.4(4) ? C123 C1231 H1231a . . . 110.8 ? C123 C1231 H1231b . . . 110.9 ? C123 C1231 H1231c . . . 110.4 ? H1231a C1231 H1231b . . . 106.9 ? H1231a C1231 H1231c . . . 109.6 ? H1231b C1231 H1231c . . . 108.1 ? C123 C124 C125 . . . 121.6(4) ? C123 C124 H124 . . . 118.9 ? C125 C124 H124 . . . 119.5 ? C124 C125 C126 . . . 120.0(4) ? C124 C125 H125 . . . 120.5 ? C126 C125 H125 . . . 119.5 ? C121 C126 C125 . . . 120.4(4) ? C121 C126 H126 . . . 119.2 ? C125 C126 H126 . . . 120.3 ? P1 C131 C132 . . . 118.0(3) ? P1 C131 C136 . . . 123.8(3) ? C132 C131 C136 . . . 118.2(4) ? C131 C132 C133 . . . 121.0(4) ? C131 C132 H132 . . . 120.4 ? C133 C132 H132 . . . 118.6 ? C132 C133 C1331 . . . 121.4(5) ? C132 C133 C134 . . . 118.6(5) ? C1331 C133 C134 . . . 120.0(5) ? C133 C1331 H1331a . . . 115.6 ? C133 C1331 H1331c . . . 108.8 ? C133 C1331 H1331b . . . 111.0 ? H1331a C1331 H1331c . . . 106.5 ? H1331a C1331 H1331b . . . 108.4 ? H1331c C1331 H1331b . . . 106.0 ? C133 C134 C135 . . . 121.2(5) ? C133 C134 H134 . . . 118.4 ? C135 C134 H134 . . . 120.4 ? C134 C135 C136 . . . 119.7(5) ? C134 C135 H135 . . . 119.9 ? C136 C135 H135 . . . 120.4 ? C131 C136 C135 . . . 121.2(5) ? C131 C136 H136 . . . 119.6 ? C135 C136 H136 . . . 119.2 ? P2 C211 C212 . . . 119.2(3) ? P2 C211 C216 . . . 121.2(3) ? C212 C211 C216 . . . 118.8(4) ? C211 C212 C213 . . . 121.6(4) ? C211 C212 H212 . . . 120.1 ? C213 C212 H212 . . . 118.3 ? C212 C213 C2131 . . . 120.2(4) ? C212 C213 C214 . . . 118.8(4) ? C2131 C213 C214 . . . 121.0(4) ? C213 C2131 H2131a . . . 109.5 ? C213 C2131 H2131c . . . 110.7 ? C213 C2131 H2131b . . . 112.0 ? H2131a C2131 H2131c . . . 107.6 ? H2131a C2131 H2131b . . . 109.1 ? H2131c C2131 H2131b . . . 107.8 ? C213 C214 C215 . . . 120.5(4) ? C213 C214 H214 . . . 119.1 ? C215 C214 H214 . . . 120.3 ? C214 C215 C216 . . . 120.4(4) ? C214 C215 H215 . . . 119.8 ? C216 C215 H215 . . . 119.7 ? C211 C216 C215 . . . 119.9(4) ? C211 C216 H216 . . . 120.5 ? C215 C216 H216 . . . 119.6 ? P2 C221 C222 . . . 117.1(3) ? P2 C221 C226 . . . 124.1(3) ? C222 C221 C226 . . . 118.8(3) ? C221 C222 C223 . . . 122.8(3) ? C221 C222 H222 . . . 118.7 ? C223 C222 H222 . . . 118.5 ? C222 C223 C2231 . . . 119.4(4) ? C222 C223 C224 . . . 117.5(3) ? C2231 C223 C224 . . . 123.1(4) ? C223 C2231 H2231a . . . 108.4 ? C223 C2231 H2231b . . . 109.3 ? C223 C2231 H2231c . . . 113.5 ? H2231a C2231 H2231b . . . 108.6 ? H2231a C2231 H2231c . . . 108.1 ? H2231b C2231 H2231c . . . 108.7 ? C223 C224 C225 . . . 120.6(4) ? C223 C224 H224 . . . 120.4 ? C225 C224 H224 . . . 119.1 ? C224 C225 C226 . . . 120.8(4) ? C224 C225 H225 . . . 119.6 ? C226 C225 H225 . . . 119.6 ? C221 C226 C225 . . . 119.5(4) ? C221 C226 H226 . . . 120.3 ? C225 C226 H226 . . . 120.2 ? P2 C231 C232 . . . 123.0(3) ? P2 C231 C236 . . . 117.8(3) ? C232 C231 C236 . . . 119.2(3) ? C231 C232 C233 . . . 121.6(3) ? C231 C232 H232 . . . 120.3 ? C233 C232 H232 . . . 118.1 ? C232 C233 C2331 . . . 121.0(4) ? C232 C233 C234 . . . 117.9(4) ? C2331 C233 C234 . . . 121.1(4) ? C233 C2331 H2331a . . . 110.9 ? C233 C2331 H2331b . . . 111.2 ? C233 C2331 H2331c . . . 107.5 ? H2331a C2331 H2331b . . . 109.5 ? H2331a C2331 H2331c . . . 108.4 ? H2331b C2331 H2331c . . . 109.2 ? C233 C234 C235 . . . 121.6(4) ? C233 C234 H234 . . . 118.9 ? C235 C234 H234 . . . 119.5 ? C234 C235 C236 . . . 120.2(4) ? C234 C235 H235 . . . 119.4 ? C236 C235 H235 . . . 120.4 ? C231 C236 C235 . . . 119.5(4) ? C231 C236 H236 . . . 120.7 ? C235 C236 H236 . . . 119.8 ? N12 N11 C15 . . . 108.9(3) ? N12 N11 B . . . 122.9(3) ? C15 N11 B . . . 128.1(3) ? N11 N12 C13 . . . 103.5(3) ? N12 C13 N14 . . . 113.9(3) ? N12 C13 H13 . . . 123.5 ? N14 C13 H13 . . . 122.6 ? Cu N14 C13 . . . 131.9(2) ? Cu N14 C15 . . . 124.8(3) ? C13 N14 C15 . . . 102.5(3) ? N11 C15 N14 . . . 111.3(3) ? N11 C15 H15 . . . 124.8 ? N14 C15 H15 . . . 123.9 ? N22 N21 C25 . . . 108.1(3) ? N22 N21 B . . . 120.7(3) ? C25 N21 B . . . 130.5(3) ? N21 N22 C23 . . . 103.2(3) ? N22 C23 N24 . . . 115.1(3) ? N22 C23 H23 . . . 123.0 ? N24 C23 H23 . . . 121.9 ? C23 N24 C25 . . . 102.4(3) ? C23 N24 Cu . . '3 557' 130.4(3) ? C25 N24 Cu . . '3 557' 126.8(3) ? N21 C25 N24 . . . 111.3(4) ? N21 C25 H25 . . . 125.2 ? N24 C25 H25 . . . 123.6 ? N32 N31 C35 . . . 107.8(4) ? N32 N31 B . . . 124.4(4) ? C35 N31 B . . . 127.3(4) ? N31 N32 C33 . . . 102.3(5) ? N32 C33 N34 . . . 115.4(5) ? N32 C33 H33 . . . 121.2 ? N34 C33 H33 . . . 123.4 ? C33 N34 C35 . . . 101.7(5) ? N31 C35 N34 . . . 112.8(6) ? N31 C35 H35 . . . 123.3 ? N34 C35 H35 . . . 123.9 ? N11 B N21 . . . 107.8(3) ? N11 B N31 . . . 110.0(3) ? N11 B H1 . . . 111.1 ? N21 B N31 . . . 110.7(3) ? N21 B H1 . . . 108.0 ? N31 B H1 . . . 109.2 ? 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 1856 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 33 _reflns_limit_l_min 0 _reflns_limit_l_max 38 _reflns_number_observed ? _reflns_d_resolution_high .583 _reflns_d_resolution_low 14.683 _diffrn_reflns_av_sigmaI/netI .171 _diffrn_reflns_theta_min 1.38 _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 .105 _refine_ls_wR_factor_all .055 _refine_ls_goodness_of_fit_all .983 _refine_ls_shift/su_mean .0003 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_dara13 _database_code_CSD 176919 _audit_creation_method Xtal3.6 _audit_creation_date 01-10-29 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C27 H28 B1 Cu1 N9 P1' _chemical_formula_moiety ? _chemical_formula_weight 583.91 _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 10.9114(9) _cell_length_b 11.8518(10) _cell_length_c 12.3165(11) _cell_angle_alpha 70.986(2) _cell_angle_beta 75.079(2) _cell_angle_gamma 71.896(2) _cell_volume 1409.5(2) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 7862 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu .866 _exptl_crystal_description prism _exptl_crystal_size_max .39 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .05 _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 .641 _exptl_absorpt_correction_T_max .863 _diffrn_reflns_number 28965 _reflns_number_total 14446 _reflns_Friedel_coverage 0 _reflns_number_gt 9722 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 37.89 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .028 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? #<< do not append units _diffrn_standards_decay_% 0 #<< do not append % _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .037 _refine_ls_wR_factor_ref .035 _refine_ls_goodness_of_fit_ref .994 _refine_ls_number_reflns 9722 _refine_ls_number_parameters 464 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max .001 _refine_diff_density_min -.468 _refine_diff_density_max .747 _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 54 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 56 0 0 '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' N ? 0 18 .004 .003 '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' Cu ? 0 2 .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 .37303(2) .72505(2) .19230(2) .02161(13) Uani ? ? 1.00000 ? ? P .56954(3) .60880(3) .18353(3) .0185(2) Uani ? ? 1.00000 ? ? C111 .68302(12) .65061(12) .04906(11) .0191(9) Uani ? ? 1.00000 ? ? C112 .63363(13) .71860(13) -.05355(12) .0242(11) Uani ? ? 1.00000 ? ? C113 .71762(15) .75614(14) -.15666(13) .0266(11) Uani ? ? 1.00000 ? ? C114 .85230(14) .72670(13) -.16021(12) .0249(11) Uani ? ? 1.00000 ? ? C1141 .94513(19) .76475(19) -.27110(15) .0370(16) Uani ? ? 1.00000 ? ? C115 .90084(13) .65774(13) -.05750(13) .0237(11) Uani ? ? 1.00000 ? ? C116 .81807(12) .62051(12) .04550(12) .0210(10) Uani ? ? 1.00000 ? ? C121 .58313(12) .44531(12) .20795(12) .0203(10) Uani ? ? 1.00000 ? ? C122 .49802(14) .39115(13) .30163(13) .0251(11) Uani ? ? 1.00000 ? ? C123 .51233(15) .26506(14) .33377(13) .0278(12) Uani ? ? 1.00000 ? ? C124 .61062(16) .18931(14) .27295(14) .0291(12) Uani ? ? 1.00000 ? ? C1241 .6297(3) .05152(17) .3140(2) .0477(19) Uani ? ? 1.00000 ? ? C125 .69103(16) .24444(14) .17634(14) .0314(13) Uani ? ? 1.00000 ? ? C126 .67877(14) .37089(14) .14438(13) .0258(11) Uani ? ? 1.00000 ? ? C131 .65389(12) .60511(12) .29571(11) .0192(9) Uani ? ? 1.00000 ? ? C132 .65019(14) .71802(13) .31058(12) .0234(11) Uani ? ? 1.00000 ? ? C133 .71566(15) .72236(14) .39104(13) .0258(11) Uani ? ? 1.00000 ? ? C134 .78390(13) .61548(14) .46126(12) .0243(11) Uani ? ? 1.00000 ? ? C1341 .85521(18) .62349(19) .54733(15) .0347(15) Uani ? ? 1.00000 ? ? C135 .78431(14) .50313(14) .44866(13) .0273(12) Uani ? ? 1.00000 ? ? C136 .72124(14) .49789(13) .36590(13) .0251(11) Uani ? ? 1.00000 ? ? C15 .00752(13) .69607(14) .18807(12) .0245(11) Uani ? ? 1.00000 ? ? C25 .13572(15) 1.04784(13) .02258(13) .0275(12) Uani ? ? 1.00000 ? ? C35 .08489(15) .90574(15) .41343(14) .0297(12) Uani ? ? 1.00000 ? ? N11 .09576(10) .74735(10) .19925(10) .0211(9) Uani ? ? 1.00000 ? ? N12 .21580(11) .66448(10) .18859(10) .0223(9) Uani ? ? 1.00000 ? ? C13 .19001(14) .57075(13) .17212(13) .0245(11) Uani ? ? 1.00000 ? ? N14 .06211(12) .58487(12) .17110(12) .0289(11) Uani ? ? 1.00000 ? ? N21 .16812(11) .94272(10) .10486(10) .0220(9) Uani ? ? 1.00000 ? ? N22 .30085(11) .89537(11) .07793(10) .0235(9) Uani ? ? 1.00000 ? ? C23 .33645(15) .97674(14) -.01865(13) .0274(12) Uani ? ? 1.00000 ? ? N24 .23783(14) 1.07277(12) -.05723(12) .0318(11) Uani ? ? 1.00000 ? ? N31 .13859(11) .85996(11) .32148(10) .0224(9) Uani ? ? 1.00000 ? ? N32 .26646(11) .79882(11) .33202(10) .0237(9) Uani ? ? 1.00000 ? ? C33 .27880(15) .81369(15) .42999(13) .0291(12) Uani ? ? 1.00000 ? ? N34 .16898(14) .87945(14) .48429(12) .0353(12) Uani ? ? 1.00000 ? ? B .08333(14) .87497(14) .21285(14) .0225(11) Uani ? ? 1.00000 ? ? H112 .5411(17) .7384(15) -.0505(14) .026(4) Uiso ? ? 1.00000 ? ? H113 .6823(17) .8050(16) -.2281(16) .033(5) Uiso ? ? 1.00000 ? ? H1141a 1.005(2) .802(2) -.261(2) .061(7) Uiso ? ? 1.00000 ? ? H1141b .996(2) .693(2) -.300(2) .065(7) Uiso ? ? 1.00000 ? ? H1141c .897(2) .824(2) -.332(2) .054(6) Uiso ? ? 1.00000 ? ? H115 .9928(17) .6352(16) -.0572(15) .030(5) Uiso ? ? 1.00000 ? ? H116 .8538(16) .5734(15) .1160(15) .026(4) Uiso ? ? 1.00000 ? ? H122 .4329(17) .4416(16) .3489(15) .029(4) Uiso ? ? 1.00000 ? ? H123 .4586(17) .2283(16) .3998(15) .030(5) Uiso ? ? 1.00000 ? ? H1241a .551(3) .033(3) .331(2) .086(9) Uiso ? ? 1.00000 ? ? H1241b .660(3) .014(3) .392(3) .117(12) Uiso ? ? 1.00000 ? ? H1241c .687(2) .012(2) .259(2) .060(7) Uiso ? ? 1.00000 ? ? H125 .7580(19) .1955(18) .1296(17) .043(5) Uiso ? ? 1.00000 ? ? H126 .7351(17) .4061(16) .0793(16) .031(5) Uiso ? ? 1.00000 ? ? H132 .6027(16) .7931(15) .2631(14) .025(4) Uiso ? ? 1.00000 ? ? H133 .7143(17) .7968(17) .3972(16) .034(5) Uiso ? ? 1.00000 ? ? H1341a .909(2) .544(2) .5835(18) .048(6) Uiso ? ? 1.00000 ? ? H1341b .792(2) .655(2) .612(2) .066(7) Uiso ? ? 1.00000 ? ? H1341c .912(2) .679(2) .5099(19) .055(6) Uiso ? ? 1.00000 ? ? H135 .8274(18) .4263(18) .4995(16) .039(5) Uiso ? ? 1.00000 ? ? H136 .7231(17) .4231(17) .3573(15) .030(5) Uiso ? ? 1.00000 ? ? H13 .2577(16) .4958(15) .1613(14) .026(4) Uiso ? ? 1.00000 ? ? H15 -.0808(18) .7369(16) .1913(15) .030(5) Uiso ? ? 1.00000 ? ? H23 .4267(16) .9657(15) -.0585(14) .024(4) Uiso ? ? 1.00000 ? ? H25 .0473(18) 1.0971(17) .0254(16) .035(5) Uiso ? ? 1.00000 ? ? H33 .3583(17) .7778(16) .4603(15) .028(4) Uiso ? ? 1.00000 ? ? H35 -.0029(19) .9511(17) .4241(16) .039(5) Uiso ? ? 1.00000 ? ? H1 -.0197(16) .9290(15) .2199(14) .025(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 .01520(7) .02194(8) .02483(8) .00089(6) -.00409(6) -.00727(6) P .01452(13) .01856(15) .02102(15) -.00075(11) -.00356(11) -.00621(12) C111 .0167(5) .0181(6) .0217(6) -.0018(4) -.0035(4) -.0065(5) C112 .0198(6) .0264(7) .0243(6) -.0010(5) -.0065(5) -.0066(5) C113 .0299(7) .0275(7) .0209(6) -.0050(6) -.0068(5) -.0046(5) C114 .0285(7) .0238(6) .0240(6) -.0093(5) -.0005(5) -.0092(5) C1141 .0388(9) .0476(11) .0258(8) -.0208(8) .0031(7) -.0087(7) C115 .0188(6) .0251(7) .0280(7) -.0058(5) -.0017(5) -.0097(5) C116 .0180(5) .0205(6) .0243(6) -.0025(4) -.0056(5) -.0064(5) C121 .0172(5) .0206(6) .0234(6) -.0023(4) -.0050(4) -.0077(5) C122 .0215(6) .0245(7) .0277(7) -.0039(5) -.0006(5) -.0095(5) C123 .0300(7) .0256(7) .0262(7) -.0090(6) -.0022(6) -.0052(6) C124 .0359(8) .0217(7) .0302(7) -.0057(6) -.0070(6) -.0080(6) C1241 .0682(14) .0225(8) .0454(11) -.0091(9) .0003(10) -.0101(8) C125 .0345(8) .0251(7) .0339(8) -.0036(6) -.0001(6) -.0151(6) C126 .0253(6) .0244(7) .0270(7) -.0054(5) .0003(5) -.0104(5) C131 .0170(5) .0192(6) .0198(6) -.0026(4) -.0022(4) -.0058(5) C132 .0265(6) .0192(6) .0229(6) -.0037(5) -.0053(5) -.0048(5) C133 .0308(7) .0231(7) .0261(7) -.0081(5) -.0048(5) -.0088(5) C134 .0217(6) .0321(7) .0197(6) -.0079(5) -.0022(5) -.0075(5) C1341 .0334(8) .0463(10) .0302(8) -.0107(8) -.0097(7) -.0139(7) C135 .0262(7) .0263(7) .0280(7) -.0030(5) -.0110(5) -.0039(6) C136 .0256(6) .0199(6) .0303(7) -.0021(5) -.0102(5) -.0065(5) C15 .0192(6) .0285(7) .0255(7) -.0046(5) -.0065(5) -.0060(5) C25 .0301(7) .0205(6) .0292(7) .0018(5) -.0112(6) -.0059(5) C35 .0274(7) .0317(8) .0282(7) -.0022(6) .0012(6) -.0150(6) N11 .0154(5) .0214(5) .0249(5) -.0007(4) -.0037(4) -.0076(4) N12 .0168(5) .0206(5) .0277(6) .0002(4) -.0037(4) -.0087(4) C13 .0252(6) .0216(6) .0264(7) -.0022(5) -.0065(5) -.0075(5) N14 .0274(6) .0267(6) .0360(7) -.0055(5) -.0116(5) -.0094(5) N21 .0201(5) .0191(5) .0244(5) .0008(4) -.0066(4) -.0061(4) N22 .0194(5) .0231(5) .0247(6) -.0019(4) -.0043(4) -.0050(4) C23 .0282(7) .0259(7) .0261(7) -.0068(6) -.0038(6) -.0048(6) N24 .0377(7) .0236(6) .0289(6) -.0041(5) -.0086(5) -.0015(5) N31 .0198(5) .0223(5) .0232(5) -.0001(4) -.0021(4) -.0096(4) N32 .0210(5) .0249(6) .0228(5) .0006(4) -.0053(4) -.0081(4) C33 .0291(7) .0336(8) .0238(7) -.0043(6) -.0066(6) -.0084(6) N34 .0357(7) .0445(8) .0267(6) -.0041(6) -.0034(5) -.0177(6) B .0178(6) .0213(7) .0262(7) .0008(5) -.0046(5) -.0084(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 . . 2.1562(4) ? Cu N12 . . 2.0707(14) ? Cu N22 . . 2.0999(11) ? Cu N32 . . 2.0967(13) ? P C111 . . 1.8200(12) ? P C121 . . 1.8253(15) ? P C131 . . 1.8299(16) ? C111 C112 . . 1.3979(19) ? C111 C116 . . 1.3967(18) ? C112 C113 . . 1.3916(19) ? C112 H112 . . .956(18) ? C113 C114 . . 1.393(2) ? C113 H113 . . .981(18) ? C114 C1141 . . 1.505(2) ? C114 C115 . . 1.397(2) ? C1141 H1141a . . .95(3) ? C1141 H1141b . . .98(3) ? C1141 H1141c . . .98(2) ? C115 C116 . . 1.3830(18) ? C115 H115 . . .956(18) ? C116 H116 . . .970(17) ? C121 C122 . . 1.3935(18) ? C121 C126 . . 1.392(2) ? C122 C123 . . 1.384(2) ? C122 H122 . . .975(17) ? C123 C124 . . 1.394(2) ? C123 H123 . . .936(16) ? C124 C1241 . . 1.507(2) ? C124 C125 . . 1.387(2) ? C1241 H1241a . . .91(3) ? C1241 H1241b . . 1.01(4) ? C1241 H1241c . . .94(2) ? C125 C126 . . 1.392(2) ? C125 H125 . . .97(2) ? C126 H126 . . .939(16) ? C131 C132 . . 1.396(2) ? C131 C136 . . 1.3904(17) ? C132 C133 . . 1.384(3) ? C132 H132 . . .966(15) ? C133 C134 . . 1.3923(19) ? C133 H133 . . .91(2) ? C134 C1341 . . 1.508(3) ? C134 C135 . . 1.388(3) ? C1341 H1341a . . .969(19) ? C1341 H1341b . . 1.00(2) ? C1341 H1341c . . .97(2) ? C135 C136 . . 1.395(3) ? C135 H135 . . .978(17) ? C136 H136 . . .92(2) ? C15 N11 . . 1.342(2) ? C15 N14 . . 1.328(2) ? C15 H15 . . .931(17) ? C25 N21 . . 1.3387(16) ? C25 N24 . . 1.321(2) ? C25 H25 . . .959(17) ? C35 N31 . . 1.335(2) ? C35 N34 . . 1.326(3) ? C35 H35 . . .941(18) ? N11 N12 . . 1.3760(14) ? N11 B . . 1.536(2) ? N12 C13 . . 1.313(2) ? C13 N14 . . 1.356(2) ? C13 H13 . . .985(16) ? N21 N22 . . 1.3752(15) ? N21 B . . 1.5498(18) ? N22 C23 . . 1.3203(17) ? C23 N24 . . 1.3524(19) ? C23 H23 . . .970(16) ? N31 N32 . . 1.3756(16) ? N31 B . . 1.542(2) ? N32 C33 . . 1.320(2) ? C33 N34 . . 1.355(2) ? C33 H33 . . .952(18) ? B H1 . . 1.104(15) ? 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 . . . 121.91(3) ? P Cu N22 . . . 128.69(3) ? P Cu N32 . . . 125.48(4) ? N12 Cu N22 . . . 90.04(5) ? N12 Cu N32 . . . 91.06(5) ? N22 Cu N32 . . . 88.48(4) ? Cu P C111 . . . 116.13(4) ? Cu P C121 . . . 115.52(4) ? Cu P C131 . . . 113.60(4) ? C111 P C121 . . . 105.19(6) ? C111 P C131 . . . 103.03(7) ? C121 P C131 . . . 101.60(7) ? P C111 C112 . . . 119.17(10) ? P C111 C116 . . . 122.16(10) ? C112 C111 C116 . . . 118.63(11) ? C111 C112 C113 . . . 120.45(13) ? C111 C112 H112 . . . 118.1(9) ? C113 C112 H112 . . . 121.5(9) ? C112 C113 C114 . . . 120.98(13) ? C112 C113 H113 . . . 120.1(10) ? C114 C113 H113 . . . 118.9(10) ? C113 C114 C1141 . . . 121.89(14) ? C113 C114 C115 . . . 118.15(12) ? C1141 C114 C115 . . . 119.96(14) ? C114 C1141 H1141a . . . 112.6(13) ? C114 C1141 H1141b . . . 110.3(13) ? C114 C1141 H1141c . . . 110.8(12) ? H1141a C1141 H1141b . . . 108(2) ? H1141a C1141 H1141c . . . 107(2) ? H1141b C1141 H1141c . . . 108(2) ? C114 C115 C116 . . . 121.28(13) ? C114 C115 H115 . . . 120.2(10) ? C116 C115 H115 . . . 118.5(10) ? C111 C116 C115 . . . 120.51(12) ? C111 C116 H116 . . . 119.6(10) ? C115 C116 H116 . . . 119.9(10) ? P C121 C122 . . . 117.22(11) ? P C121 C126 . . . 123.93(10) ? C122 C121 C126 . . . 118.67(13) ? C121 C122 C123 . . . 120.48(13) ? C121 C122 H122 . . . 119.5(10) ? C123 C122 H122 . . . 119.8(10) ? C122 C123 C124 . . . 121.18(13) ? C122 C123 H123 . . . 120.3(11) ? C124 C123 H123 . . . 118.5(11) ? C123 C124 C1241 . . . 120.27(15) ? C123 C124 C125 . . . 118.05(14) ? C1241 C124 C125 . . . 121.67(15) ? C124 C1241 H1241a . . . 109.8(16) ? C124 C1241 H1241b . . . 113(2) ? C124 C1241 H1241c . . . 112.2(14) ? H1241a C1241 H1241b . . . 101(3) ? H1241a C1241 H1241c . . . 110(3) ? H1241b C1241 H1241c . . . 110(2) ? C124 C125 C126 . . . 121.16(14) ? C124 C125 H125 . . . 120.7(12) ? C126 C125 H125 . . . 118.2(12) ? C121 C126 C125 . . . 120.34(13) ? C121 C126 H126 . . . 119.9(11) ? C125 C126 H126 . . . 119.7(11) ? P C131 C132 . . . 117.25(9) ? P C131 C136 . . . 124.33(13) ? C132 C131 C136 . . . 118.42(15) ? C131 C132 C133 . . . 120.36(12) ? C131 C132 H132 . . . 119.2(13) ? C133 C132 H132 . . . 120.4(13) ? C132 C133 C134 . . . 121.58(16) ? C132 C133 H133 . . . 118.7(12) ? C134 C133 H133 . . . 119.7(12) ? C133 C134 C1341 . . . 120.24(17) ? C133 C134 C135 . . . 117.95(16) ? C1341 C134 C135 . . . 121.81(13) ? C134 C1341 H1341a . . . 112.8(17) ? C134 C1341 H1341b . . . 111.0(17) ? C134 C1341 H1341c . . . 111.1(15) ? H1341a C1341 H1341b . . . 106.4(17) ? H1341a C1341 H1341c . . . 107.4(19) ? H1341b C1341 H1341c . . . 108(2) ? C134 C135 C136 . . . 120.89(13) ? C134 C135 H135 . . . 119.9(15) ? C136 C135 H135 . . . 119.2(15) ? C131 C136 C135 . . . 120.76(15) ? C131 C136 H136 . . . 118.9(12) ? C135 C136 H136 . . . 120.3(11) ? N11 C15 N14 . . . 112.06(12) ? N11 C15 H15 . . . 121.9(14) ? N14 C15 H15 . . . 126.1(14) ? N21 C25 N24 . . . 112.31(12) ? N21 C25 H25 . . . 121.3(10) ? N24 C25 H25 . . . 126.4(10) ? N31 C35 N34 . . . 112.19(13) ? N31 C35 H35 . . . 122.0(14) ? N34 C35 H35 . . . 125.8(14) ? C15 N11 N12 . . . 107.11(12) ? C15 N11 B . . . 131.87(11) ? N12 N11 B . . . 120.89(12) ? Cu N12 N11 . . . 115.28(10) ? Cu N12 C13 . . . 140.60(9) ? N11 N12 C13 . . . 103.97(12) ? N12 C13 N14 . . . 114.69(13) ? N12 C13 H13 . . . 123.1(13) ? N14 C13 H13 . . . 122.2(13) ? C15 N14 C13 . . . 102.17(15) ? C25 N21 N22 . . . 107.37(10) ? C25 N21 B . . . 131.17(11) ? N22 N21 B . . . 121.45(9) ? Cu N22 N21 . . . 114.10(8) ? Cu N22 C23 . . . 142.49(9) ? N21 N22 C23 . . . 103.33(10) ? N22 C23 N24 . . . 114.89(13) ? N22 C23 H23 . . . 121.3(9) ? N24 C23 H23 . . . 123.8(9) ? C25 N24 C23 . . . 102.10(11) ? C35 N31 N32 . . . 107.55(13) ? C35 N31 B . . . 130.77(12) ? N32 N31 B . . . 121.49(11) ? Cu N32 N31 . . . 114.18(10) ? Cu N32 C33 . . . 142.24(10) ? N31 N32 C33 . . . 103.49(11) ? N32 C33 N34 . . . 114.63(15) ? N32 C33 H33 . . . 121.6(11) ? N34 C33 H33 . . . 123.7(11) ? C35 N34 C33 . . . 102.14(15) ? N11 B N21 . . . 108.16(12) ? N11 B N31 . . . 109.55(10) ? N11 B H1 . . . 110.9(11) ? N21 B N31 . . . 107.68(13) ? N21 B H1 . . . 110.0(8) ? N31 B H1 . . . 110.4(10) ? 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 N11 2.9351(12) . . ? Cu C13 3.196(2) . . ? Cu N21 2.9426(10) . . ? Cu C23 3.2484(14) . . ? Cu N31 2.9413(11) . . ? Cu C33 3.2425(18) . . ? Cu B 3.0990(14) . . ? P C112 2.7833(13) . . ? P C116 2.8230(13) . . ? P C122 2.7569(15) . . ? P C126 2.8469(17) . . ? P C132 2.763(2) . . ? P C136 2.8551(16) . . ? C111 C113 2.4213(18) . . ? C111 C114 2.8173(17) . . ? C111 C115 2.4134(18) . . ? C111 C121 2.8957(18) . . ? C111 C131 2.857(2) . . ? C111 H112 2.032(18) . . ? C111 H116 2.057(18) . . ? C111 H126 2.691(19) . . ? C112 C114 2.424(2) . . ? C112 C115 2.769(2) . . ? C112 C116 2.403(2) . . ? C112 H113 2.066(17) . . ? C113 C1141 2.534(2) . . ? C113 C115 2.393(2) . . ? C113 C116 2.773(2) . . ? C113 H112 2.059(16) . . ? C113 H1141c 2.61(2) . . ? C114 C116 2.4228(18) . . ? C114 H113 2.055(19) . . ? C114 H1141a 2.07(2) . . ? C114 H1141b 2.06(2) . . ? C114 H1141c 2.07(2) . . ? C114 H115 2.052(18) . . ? C1141 C115 2.513(2) . . ? C1141 H113 2.695(18) . . ? C1141 H115 2.673(17) . . ? C115 H116 2.048(16) . . ? C116 H115 2.021(17) . . ? C121 C123 2.411(2) . . ? C121 C124 2.813(2) . . ? C121 C125 2.415(2) . . ? C121 C131 2.833(2) . . ? C121 H122 2.057(16) . . ? C121 H126 2.031(17) . . ? C121 H136 2.58(2) . . ? C122 C124 2.420(2) . . ? C122 C125 2.764(2) . . ? C122 C126 2.396(2) . . ? C122 H123 2.025(17) . . ? C123 C1241 2.516(3) . . ? C123 C125 2.385(2) . . ? C123 C126 2.764(2) . . ? C123 H122 2.051(18) . . ? C123 H1241a 2.66(3) . . ? C124 C126 2.421(2) . . ? C124 H123 2.016(16) . . ? C124 H1241a 2.01(3) . . ? C124 H1241b 2.12(3) . . ? C124 H1241c 2.05(2) . . ? C124 H125 2.058(18) . . ? C1241 C125 2.528(3) . . ? C1241 H123 2.643(17) . . ? C125 H1241c 2.62(2) . . ? C125 H126 2.028(18) . . ? C126 H125 2.04(2) . . ? C131 C133 2.412(3) . . ? C131 C134 2.819(2) . . ? C131 C135 2.421(2) . . ? C131 H132 2.049(17) . . ? C131 H136 2.004(17) . . ? C132 C134 2.423(2) . . ? C132 C135 2.7683(18) . . ? C132 C136 2.393(2) . . ? C132 H133 1.98(2) . . ? C133 C1341 2.516(3) . . ? C133 C135 2.383(2) . . ? C133 C136 2.757(3) . . ? C133 H132 2.050(18) . . ? C134 C136 2.421(3) . . ? C134 H133 2.002(17) . . ? C134 H1341a 2.08(2) . . ? C134 H1341b 2.09(3) . . ? C134 H1341c 2.07(3) . . ? C134 H135 2.06(2) . . ? C1341 C135 2.532(3) . . ? C1341 H133 2.651(17) . . ? C135 H1341a 2.63(3) . . ? C135 H136 2.02(2) . . ? C136 H135 2.06(2) . . ? C15 N12 2.187(2) . . ? C15 C13 2.0881(18) . . ? C15 B 2.630(3) . . ? C25 N22 2.1870(17) . . ? C25 C23 2.079(2) . . ? C25 B 2.632(2) . . ? C35 N32 2.1865(18) . . ? C35 C33 2.086(2) . . ? C35 B 2.617(3) . . ? N11 C13 2.1192(19) . . ? N11 N14 2.214(2) . . ? N11 N21 2.4992(17) . . ? N11 N31 2.515(2) . . ? N11 H15 2.00(2) . . ? N11 H1 2.189(16) . . ? N12 N14 2.247(2) . . ? N12 B 2.5346(19) . . ? N12 H13 2.03(2) . . ? C13 B 3.588(2) . . ? N14 H116 2.59(2) . '1 455' ? N14 H13 2.057(16) . . ? N14 H15 2.022(16) . . ? N21 C23 2.1147(18) . . ? N21 N24 2.2094(16) . . ? N21 N31 2.4965(16) . . ? N21 H25 2.011(16) . . ? N21 H1 2.190(16) . . ? N22 N24 2.2528(16) . . ? N22 B 2.5528(18) . . ? N22 H23 2.003(16) . . ? C23 B 3.604(2) . . ? N24 H23 2.056(16) . . ? N24 H25 2.042(18) . . ? N31 C33 2.117(2) . . ? N31 N34 2.208(2) . . ? N31 H35 1.999(18) . . ? N31 H1 2.187(18) . . ? N32 N34 2.252(2) . . ? N32 B 2.547(2) . . ? N32 H33 1.99(2) . . ? C33 B 3.597(3) . . ? N34 H33 2.044(16) . . ? N34 H35 2.598(19) . '2 576' ? N34 H35 2.03(2) . . ? B H15 2.88(2) . . ? B H25 2.878(16) . . ? B H35 2.87(2) . . ? H112 H113 2.38(2) . . ? H1141a H1141b 1.57(4) . . ? H1141a H1141c 1.56(4) . . ? H1141b H1141c 1.59(3) . . ? H115 H116 2.32(2) . . ? H122 H123 2.34(3) . . ? H1241a H1241b 1.49(5) . . ? H1241a H1241c 1.52(3) . . ? H1241b H1241c 1.59(5) . . ? H125 H126 2.31(3) . . ? H132 H133 2.31(3) . . ? H1341a H1341b 1.58(3) . . ? H1341a H1341c 1.56(3) . . ? H1341b H1341c 1.59(3) . . ? H135 H136 2.34(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_000 604 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 18 _reflns_limit_k_min -18 _reflns_limit_k_max 20 _reflns_limit_l_min -20 _reflns_limit_l_max 21 _reflns_number_observed ? _reflns_d_resolution_high .579 _reflns_d_resolution_low 11.441 _diffrn_reflns_av_sigmaI/netI .099 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 153 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .067 _refine_ls_wR_factor_all .039 _refine_ls_goodness_of_fit_all .903 _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 loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_cpdar1 _database_code_CSD 176920 _audit_creation_method Xtal3.6 _audit_creation_date 01-02-05 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C24 H40 B1 Cu1 N9 P1' _chemical_formula_moiety ? _chemical_formula_weight 559.98 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 9.2098(5) _cell_length_b 14.5388(7) _cell_length_c 21.0453(10) _cell_angle_alpha 90.00000 _cell_angle_beta 101.3770(10) _cell_angle_gamma 90.00000 _cell_volume 2762.6(2) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.346 _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 1.8 _cell_measurement_theta_max 24.0 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu .879 _exptl_crystal_description block _exptl_crystal_size_max .35 _exptl_crystal_size_mid .3 _exptl_crystal_size_min .11 _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 .736 _exptl_absorpt_correction_T_max .832 _diffrn_reflns_number 55604 _reflns_number_total 14503 _reflns_Friedel_coverage 0 _reflns_number_gt 10960 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 37.53 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .028 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 36 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .027 _refine_ls_wR_factor_ref .03 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_number_reflns 10960 _refine_ls_number_parameters 485 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max .005 _refine_diff_density_min -.577 _refine_diff_density_max .492 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 96 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 160 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 36 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cu ? 0 4 .263 1.266 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 4 .09 .095 '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 .820449(13) 1.012938(8) .252858(5) .01506(4) Uani ? ? 1.00000 ? ? P .87042(2) 1.015053(16) .155755(10) .01271(8) Uani ? ? 1.00000 ? ? C111 .73067(10) .96231(6) .08912(4) .0147(3) Uani ? ? 1.00000 ? ? C112 .79108(11) .92487(7) .03086(5) .0182(4) Uani ? ? 1.00000 ? ? C113 .66837(11) .88331(7) -.02091(5) .0202(4) Uani ? ? 1.00000 ? ? C114 .58525(11) .80859(7) .00796(5) .0209(4) Uani ? ? 1.00000 ? ? C115 .51887(11) .84753(7) .06344(5) .0195(4) Uani ? ? 1.00000 ? ? C116 .64051(10) .88796(7) .11631(4) .0172(4) Uani ? ? 1.00000 ? ? C121 .89359(10) 1.13512(6) .12903(4) .0158(3) Uani ? ? 1.00000 ? ? C122 .91180(13) 1.14729(7) .05883(5) .0225(4) Uani ? ? 1.00000 ? ? C123 .93806(14) 1.24819(8) .04366(6) .0267(5) Uani ? ? 1.00000 ? ? C124 .81284(14) 1.30906(8) .05673(6) .0276(5) Uani ? ? 1.00000 ? ? C125 .79006(16) 1.29714(8) .12613(6) .0316(5) Uani ? ? 1.00000 ? ? C126 .76741(13) 1.19622(7) .14291(5) .0239(4) Uani ? ? 1.00000 ? ? C131 1.04605(10) .95671(6) .14997(4) .0154(3) Uani ? ? 1.00000 ? ? C132 1.04052(11) .85529(7) .17019(5) .0204(4) Uani ? ? 1.00000 ? ? C133 1.18257(11) .80443(7) .16367(6) .0238(4) Uani ? ? 1.00000 ? ? C134 1.31883(11) .85120(7) .20301(5) .0230(4) Uani ? ? 1.00000 ? ? C135 1.32348(11) .95252(7) .18510(6) .0247(4) Uani ? ? 1.00000 ? ? C136 1.18159(11) 1.00324(7) .19171(6) .0226(4) Uani ? ? 1.00000 ? ? B .76289(11) 1.01435(8) .39433(5) .0168(4) Uani ? ? 1.00000 ? ? N11 .64530(9) 1.07408(5) .35065(4) .0166(3) Uani ? ? 1.00000 ? ? N12 .64858(8) 1.08689(5) .28623(4) .0157(3) Uani ? ? 1.00000 ? ? C13 .52574(10) 1.13402(6) .26398(5) .0181(4) Uani ? ? 1.00000 ? ? N14 .44211(10) 1.15191(6) .30890(5) .0224(4) Uani ? ? 1.00000 ? ? C15 .52084(11) 1.11308(7) .36183(5) .0210(4) Uani ? ? 1.00000 ? ? N21 .74747(9) .91599(5) .36629(4) .0171(3) Uani ? ? 1.00000 ? ? N22 .76786(9) .89798(5) .30461(4) .0180(3) Uani ? ? 1.00000 ? ? C23 .72706(12) .81089(7) .29506(5) .0229(4) Uani ? ? 1.00000 ? ? N24 .68124(12) .77104(6) .34591(5) .0294(4) Uani ? ? 1.00000 ? ? C25 .69524(12) .83931(7) .38869(5) .0239(4) Uani ? ? 1.00000 ? ? N31 .91900(9) 1.05174(5) .39238(4) .0164(3) Uani ? ? 1.00000 ? ? N32 .96968(9) 1.05970(6) .33545(4) .0176(3) Uani ? ? 1.00000 ? ? C33 1.10291(11) 1.09671(7) .35361(5) .0219(4) Uani ? ? 1.00000 ? ? N34 1.14341(10) 1.11314(7) .41812(5) .0259(4) Uani ? ? 1.00000 ? ? C35 1.02538(11) 1.08433(7) .43991(5) .0211(4) Uani ? ? 1.00000 ? ? H111 .6612(13) 1.0142(8) .0748(6) .015(3) Uiso ? ? 1.00000 ? ? H112a .8631(15) .8757(9) .0437(6) .024(3) Uiso ? ? 1.00000 ? ? H112b .8438(15) .9731(9) .0129(6) .023(3) Uiso ? ? 1.00000 ? ? H113a .7108(14) .8575(9) -.0565(6) .023(3) Uiso ? ? 1.00000 ? ? H113b .5969(14) .9311(9) -.0383(6) .021(3) Uiso ? ? 1.00000 ? ? H114a .6510(15) .7606(10) .0243(7) .027(3) Uiso ? ? 1.00000 ? ? H114b .5071(15) .7823(9) -.0240(7) .024(3) Uiso ? ? 1.00000 ? ? H115a .4623(14) .8002(9) .0819(6) .024(3) Uiso ? ? 1.00000 ? ? H115b .4448(14) .8963(9) .0463(6) .020(3) Uiso ? ? 1.00000 ? ? H116a .5952(13) .9131(8) .1518(6) .018(3) Uiso ? ? 1.00000 ? ? H116b .7068(14) .8360(9) .1354(6) .022(3) Uiso ? ? 1.00000 ? ? H121 .9850(14) 1.1556(9) .1557(6) .021(3) Uiso ? ? 1.00000 ? ? H122a .8204(16) 1.1275(10) .0283(7) .032(4) Uiso ? ? 1.00000 ? ? H122b .9962(16) 1.1114(10) .0517(7) .029(4) Uiso ? ? 1.00000 ? ? H123a .9497(17) 1.2545(11) -.0010(7) .037(4) Uiso ? ? 1.00000 ? ? H123b 1.0298(16) 1.2664(10) .0709(7) .027(4) Uiso ? ? 1.00000 ? ? H124a .7205(16) 1.2917(10) .0251(7) .033(4) Uiso ? ? 1.00000 ? ? H124b .8326(16) 1.3735(10) .0488(7) .031(4) Uiso ? ? 1.00000 ? ? H125a .7056(18) 1.3356(12) .1338(8) .045(4) Uiso ? ? 1.00000 ? ? H125b .8787(17) 1.3198(11) .1546(7) .038(4) Uiso ? ? 1.00000 ? ? H126a .7619(16) 1.1901(10) .1888(7) .033(4) Uiso ? ? 1.00000 ? ? H126b .6692(16) 1.1733(10) .1157(7) .031(4) Uiso ? ? 1.00000 ? ? H131 1.0591(15) .9587(9) .1040(7) .025(3) Uiso ? ? 1.00000 ? ? H132a .9542(15) .8241(9) .1443(7) .027(3) Uiso ? ? 1.00000 ? ? H132b 1.0281(14) .8538(9) .2155(6) .024(3) Uiso ? ? 1.00000 ? ? H133a 1.1917(15) .8031(9) .1163(7) .026(3) Uiso ? ? 1.00000 ? ? H133b 1.1773(16) .7428(10) .1772(7) .032(4) Uiso ? ? 1.00000 ? ? H134a 1.4122(16) .8210(10) .1981(7) .029(4) Uiso ? ? 1.00000 ? ? H134b 1.3185(15) .8469(10) .2484(7) .029(4) Uiso ? ? 1.00000 ? ? H135a 1.3365(15) .9565(10) .1392(7) .027(3) Uiso ? ? 1.00000 ? ? H135b 1.4086(18) .9807(11) .2128(8) .041(4) Uiso ? ? 1.00000 ? ? H136a 1.1692(16) 1.0034(10) .2369(7) .033(4) Uiso ? ? 1.00000 ? ? H136b 1.1873(16) 1.0660(10) .1799(7) .032(4) Uiso ? ? 1.00000 ? ? H13 .5004(14) 1.1545(9) .2205(6) .020(3) Uiso ? ? 1.00000 ? ? H15 .4959(14) 1.1114(9) .4041(6) .024(3) Uiso ? ? 1.00000 ? ? H23 .7279(15) .7805(10) .2566(7) .028(3) Uiso ? ? 1.00000 ? ? H25 .6763(14) .8382(9) .4313(6) .023(3) Uiso ? ? 1.00000 ? ? H33 1.1635(16) 1.1078(10) .3257(7) .029(4) Uiso ? ? 1.00000 ? ? H35 1.0151(14) 1.0851(9) .4834(6) .022(3) Uiso ? ? 1.00000 ? ? H .7440(14) 1.0139(8) .4436(6) .019(3) 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 .01701(5) .01637(5) .01230(4) -.00019(4) .00410(3) -.00014(4) P .01230(9) .01350(9) .01265(9) .00079(7) .00325(7) -.00057(7) C111 .0138(3) .0167(4) .0138(3) .0003(3) .0033(3) -.0016(3) C112 .0189(4) .0211(4) .0159(4) -.0018(3) .0065(3) -.0041(3) C113 .0235(4) .0219(4) .0147(4) .0005(3) .0029(3) -.0032(3) C114 .0212(4) .0191(4) .0208(4) -.0009(3) .0006(3) -.0044(3) C115 .0161(4) .0206(4) .0215(4) -.0023(3) .0028(3) -.0021(3) C116 .0153(4) .0206(4) .0161(4) -.0022(3) .0039(3) -.0009(3) C121 .0162(4) .0150(4) .0165(4) .0007(3) .0040(3) .0004(3) C122 .0309(5) .0185(4) .0219(4) -.0018(4) .0143(4) .0010(3) C123 .0335(6) .0213(5) .0292(5) -.0040(4) .0158(4) .0039(4) C124 .0322(6) .0221(5) .0301(5) .0020(4) .0097(4) .0104(4) C125 .0472(7) .0194(5) .0332(6) .0103(5) .0205(5) .0063(4) C126 .0300(5) .0197(4) .0258(5) .0085(4) .0150(4) .0067(4) C131 .0135(3) .0153(4) .0178(4) .0010(3) .0040(3) -.0010(3) C132 .0154(4) .0167(4) .0292(5) .0011(3) .0046(3) .0028(3) C133 .0185(4) .0158(4) .0364(6) .0030(3) .0042(4) -.0001(4) C134 .0165(4) .0246(5) .0274(5) .0047(3) .0030(4) .0015(4) C135 .0136(4) .0210(4) .0390(6) .0004(3) .0042(4) -.0054(4) C136 .0141(4) .0200(5) .0327(5) .0013(3) .0020(3) -.0080(4) B .0183(4) .0183(4) .0142(4) .0002(4) .0043(3) .0005(3) N11 .0177(3) .0170(3) .0162(3) .0010(3) .0059(3) .0001(3) N12 .0162(3) .0160(3) .0151(3) .0008(3) .0036(3) .0007(2) C13 .0163(4) .0156(4) .0221(4) .0004(3) .0027(3) .0012(3) N14 .0191(4) .0207(4) .0288(4) .0039(3) .0078(3) .0018(3) C15 .0207(4) .0205(4) .0242(4) .0026(3) .0100(4) -.0002(3) N21 .0195(3) .0165(3) .0155(3) -.0008(3) .0038(3) .0029(3) N22 .0234(4) .0145(3) .0162(3) -.0012(3) .0042(3) .0002(3) C23 .0294(5) .0159(4) .0215(4) -.0035(4) .0003(4) .0005(3) N24 .0405(5) .0200(4) .0256(4) -.0098(4) .0015(4) .0049(3) C25 .0279(5) .0220(4) .0213(4) -.0051(4) .0038(4) .0068(4) N31 .0180(3) .0171(3) .0136(3) .0002(3) .0021(3) -.0014(3) N32 .0169(3) .0206(4) .0158(3) -.0017(3) .0042(3) -.0019(3) C33 .0185(4) .0242(5) .0233(4) -.0034(3) .0050(3) -.0046(4) N34 .0220(4) .0294(5) .0246(4) -.0052(3) .0007(3) -.0074(3) C35 .0235(4) .0209(4) .0174(4) -.0000(3) .0005(3) -.0047(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 . . 2.1817(3) ? Cu N12 . . 2.1433(8) ? Cu N22 . . 2.1029(8) ? Cu N32 . . 2.1047(7) ? P C111 . . 1.8706(8) ? P C121 . . 1.8592(9) ? P C131 . . 1.8515(9) ? C111 C112 . . 1.5422(14) ? C111 C116 . . 1.5404(14) ? C111 H111 . . .997(12) ? C112 C113 . . 1.5308(13) ? C112 H112a . . .976(13) ? C112 H112b . . .971(14) ? C113 C114 . . 1.5228(15) ? C113 H113a . . .986(14) ? C113 H113b . . .978(13) ? C114 C115 . . 1.5294(16) ? C114 H114a . . .942(14) ? C114 H114b . . .962(12) ? C115 C116 . . 1.5319(13) ? C115 H115a . . .988(14) ? C115 H115b . . 1.000(12) ? C116 H116a . . .994(13) ? C116 H116b . . 1.004(13) ? C121 C122 . . 1.5296(15) ? C121 C126 . . 1.5359(15) ? C121 H121 . . .962(12) ? C122 C123 . . 1.5308(15) ? C122 H122a . . .995(14) ? C122 H122b . . .973(15) ? C123 C124 . . 1.5212(18) ? C123 H123a . . .972(16) ? C123 H123b . . .960(13) ? C124 C125 . . 1.5259(19) ? C124 H124a . . 1.003(14) ? C124 H124b . . .975(15) ? C125 C126 . . 1.5329(16) ? C125 H125a . . .996(17) ? C125 H125b . . .970(15) ? C126 H126a . . .982(15) ? C126 H126b . . 1.026(13) ? C131 C132 . . 1.5383(13) ? C131 C136 . . 1.5346(13) ? C131 H131 . . .998(14) ? C132 C133 . . 1.5324(15) ? C132 H132a . . .981(13) ? C132 H132b . . .983(14) ? C133 C134 . . 1.5208(14) ? C133 H133a . . 1.017(14) ? C133 H133b . . .945(15) ? C134 C135 . . 1.5233(15) ? C134 H134a . . .989(15) ? C134 H134b . . .957(15) ? C135 C136 . . 1.5305(15) ? C135 H135a . . .999(15) ? C135 H135b . . .971(15) ? C136 H136a . . .980(16) ? C136 H136b . . .950(15) ? B N11 . . 1.5426(12) ? B N21 . . 1.5428(13) ? B N31 . . 1.5452(14) ? B H . . 1.084(14) ? N11 N12 . . 1.3746(11) ? N11 C15 . . 1.3406(14) ? N12 C13 . . 1.3265(12) ? C13 N14 . . 1.3571(15) ? C13 H13 . . .947(13) ? N14 C15 . . 1.3292(13) ? C15 H15 . . .963(14) ? N21 N22 . . 1.3731(12) ? N21 C25 . . 1.3364(14) ? N22 C23 . . 1.3248(13) ? C23 N24 . . 1.3553(16) ? C23 H23 . . .924(14) ? N24 C25 . . 1.3292(14) ? C25 H25 . . .946(14) ? N31 N32 . . 1.3739(12) ? N31 C35 . . 1.3410(12) ? N32 C33 . . 1.3252(13) ? C33 N34 . . 1.3563(14) ? C33 H33 . . .902(16) ? N34 C35 . . 1.3282(15) ? C35 H35 . . .938(14) ? 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 . . . 127.29(2) ? P Cu N22 . . . 127.52(2) ? P Cu N32 . . . 123.02(3) ? N12 Cu N22 . . . 88.20(3) ? N12 Cu N32 . . . 88.37(3) ? N22 Cu N32 . . . 90.49(3) ? Cu P C111 . . . 117.09(3) ? Cu P C121 . . . 110.77(3) ? Cu P C131 . . . 113.80(3) ? C111 P C121 . . . 105.14(4) ? C111 P C131 . . . 104.11(4) ? C121 P C131 . . . 104.85(4) ? P C111 C112 . . . 115.98(6) ? P C111 C116 . . . 110.54(6) ? P C111 H111 . . . 102.9(7) ? C112 C111 C116 . . . 110.68(7) ? C112 C111 H111 . . . 109.7(8) ? C116 C111 H111 . . . 106.4(7) ? C111 C112 C113 . . . 111.95(8) ? C111 C112 H112a . . . 111.7(8) ? C111 C112 H112b . . . 109.9(8) ? C113 C112 H112a . . . 105.9(7) ? C113 C112 H112b . . . 111.4(7) ? H112a C112 H112b . . . 105.8(12) ? C112 C113 C114 . . . 110.87(8) ? C112 C113 H113a . . . 110.1(7) ? C112 C113 H113b . . . 109.5(7) ? C114 C113 H113a . . . 109.7(8) ? C114 C113 H113b . . . 107.6(8) ? H113a C113 H113b . . . 109.0(11) ? C113 C114 C115 . . . 110.40(8) ? C113 C114 H114a . . . 109.6(9) ? C113 C114 H114b . . . 111.8(8) ? C115 C114 H114a . . . 108.7(9) ? C115 C114 H114b . . . 108.9(9) ? H114a C114 H114b . . . 107.4(11) ? C114 C115 C116 . . . 110.57(8) ? C114 C115 H115a . . . 111.4(8) ? C114 C115 H115b . . . 109.5(8) ? C116 C115 H115a . . . 110.4(7) ? C116 C115 H115b . . . 109.8(7) ? H115a C115 H115b . . . 105.1(11) ? C111 C116 C115 . . . 111.72(8) ? C111 C116 H116a . . . 111.0(7) ? C111 C116 H116b . . . 110.3(8) ? C115 C116 H116a . . . 109.3(7) ? C115 C116 H116b . . . 107.6(7) ? H116a C116 H116b . . . 106.8(10) ? P C121 C122 . . . 116.22(7) ? P C121 C126 . . . 110.44(7) ? P C121 H121 . . . 104.7(8) ? C122 C121 C126 . . . 110.37(8) ? C122 C121 H121 . . . 106.2(8) ? C126 C121 H121 . . . 108.5(8) ? C121 C122 C123 . . . 111.36(9) ? C121 C122 H122a . . . 110.5(9) ? C121 C122 H122b . . . 109.3(8) ? C123 C122 H122a . . . 106.9(8) ? C123 C122 H122b . . . 108.5(9) ? H122a C122 H122b . . . 110.2(12) ? C122 C123 C124 . . . 111.29(11) ? C122 C123 H123a . . . 110.2(9) ? C122 C123 H123b . . . 107.3(8) ? C124 C123 H123a . . . 110.6(9) ? C124 C123 H123b . . . 109.9(9) ? H123a C123 H123b . . . 107.4(13) ? C123 C124 C125 . . . 111.06(10) ? C123 C124 H124a . . . 107.9(9) ? C123 C124 H124b . . . 110.8(9) ? C125 C124 H124a . . . 110.4(9) ? C125 C124 H124b . . . 109.7(9) ? H124a C124 H124b . . . 106.9(11) ? C124 C125 C126 . . . 112.32(10) ? C124 C125 H125a . . . 110.5(9) ? C124 C125 H125b . . . 107.1(10) ? C126 C125 H125a . . . 110.7(10) ? C126 C125 H125b . . . 108.6(9) ? H125a C125 H125b . . . 107.4(13) ? C121 C126 C125 . . . 111.55(10) ? C121 C126 H126a . . . 108.8(9) ? C121 C126 H126b . . . 108.9(8) ? C125 C126 H126a . . . 110.4(9) ? C125 C126 H126b . . . 109.2(8) ? H126a C126 H126b . . . 107.9(12) ? P C131 C132 . . . 110.11(7) ? P C131 C136 . . . 112.52(7) ? P C131 H131 . . . 108.9(8) ? C132 C131 C136 . . . 109.38(7) ? C132 C131 H131 . . . 108.2(8) ? C136 C131 H131 . . . 107.5(8) ? C131 C132 C133 . . . 111.24(9) ? C131 C132 H132a . . . 110.9(8) ? C131 C132 H132b . . . 107.9(8) ? C133 C132 H132a . . . 109.9(8) ? C133 C132 H132b . . . 109.9(8) ? H132a C132 H132b . . . 106.9(11) ? C132 C133 C134 . . . 111.27(9) ? C132 C133 H133a . . . 109.5(7) ? C132 C133 H133b . . . 109.6(9) ? C134 C133 H133a . . . 108.8(7) ? C134 C133 H133b . . . 110.2(8) ? H133a C133 H133b . . . 107.3(12) ? C133 C134 C135 . . . 110.98(8) ? C133 C134 H134a . . . 112.7(8) ? C133 C134 H134b . . . 110.4(8) ? C135 C134 H134a . . . 109.6(8) ? C135 C134 H134b . . . 108.4(9) ? H134a C134 H134b . . . 104.5(11) ? C134 C135 C136 . . . 112.17(9) ? C134 C135 H135a . . . 108.1(8) ? C134 C135 H135b . . . 108.6(9) ? C136 C135 H135a . . . 109.1(8) ? C136 C135 H135b . . . 110.1(10) ? H135a C135 H135b . . . 108.7(13) ? C131 C136 C135 . . . 110.38(9) ? C131 C136 H136a . . . 108.6(8) ? C131 C136 H136b . . . 110.7(8) ? C135 C136 H136a . . . 110.8(8) ? C135 C136 H136b . . . 110.3(9) ? H136a C136 H136b . . . 105.9(12) ? N11 B N21 . . . 107.04(7) ? N11 B N31 . . . 109.49(8) ? N11 B H . . . 110.3(6) ? N21 B N31 . . . 109.38(8) ? N21 B H . . . 109.9(6) ? N31 B H . . . 110.7(6) ? B N11 N12 . . . 120.97(8) ? B N11 C15 . . . 131.12(9) ? N12 N11 C15 . . . 107.56(8) ? Cu N12 N11 . . . 114.62(5) ? Cu N12 C13 . . . 140.99(7) ? N11 N12 C13 . . . 103.59(8) ? N12 C13 N14 . . . 114.50(9) ? N12 C13 H13 . . . 122.3(8) ? N14 C13 H13 . . . 123.2(8) ? C13 N14 C15 . . . 102.22(8) ? N11 C15 N14 . . . 112.11(10) ? N11 C15 H15 . . . 121.3(8) ? N14 C15 H15 . . . 126.6(8) ? B N21 N22 . . . 121.26(8) ? B N21 C25 . . . 130.60(9) ? N22 N21 C25 . . . 107.47(8) ? Cu N22 N21 . . . 115.25(6) ? Cu N22 C23 . . . 140.22(7) ? N21 N22 C23 . . . 103.76(8) ? N22 C23 N24 . . . 114.34(9) ? N22 C23 H23 . . . 122.6(9) ? N24 C23 H23 . . . 123.0(9) ? C23 N24 C25 . . . 102.23(9) ? N21 C25 N24 . . . 112.19(10) ? N21 C25 H25 . . . 119.6(8) ? N24 C25 H25 . . . 128.1(8) ? B N31 N32 . . . 122.06(7) ? B N31 C35 . . . 130.64(8) ? N32 N31 C35 . . . 107.27(8) ? Cu N32 N31 . . . 114.47(6) ? Cu N32 C33 . . . 141.81(8) ? N31 N32 C33 . . . 103.72(8) ? N32 C33 N34 . . . 114.61(10) ? N32 C33 H33 . . . 122.8(8) ? N34 C33 H33 . . . 122.6(8) ? C33 N34 C35 . . . 102.00(9) ? N31 C35 N34 . . . 112.41(9) ? N31 C35 H35 . . . 122.2(8) ? N34 C35 H35 . . . 125.4(8) ? 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 #-------------------------------------------------------------------------- _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 1184 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 24 _reflns_limit_l_min -36 _reflns_limit_l_max 35 _reflns_number_observed ? _reflns_d_resolution_high .583 _reflns_d_resolution_low 11.856 _diffrn_reflns_av_sigmaI/netI .06 _diffrn_reflns_theta_min 1.71 _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 .044 _refine_ls_wR_factor_all .032 _refine_ls_goodness_of_fit_all 1.004 _refine_ls_shift/su_mean .0002 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_cpdar8 _database_code_CSD 176921 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C48 H56 B1 Cu1 N6 O2 P2' _chemical_formula_moiety ? _chemical_formula_weight 885.32 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _cell_length_a 10.1233(6) _cell_length_b 14.0189(8) _cell_length_c 16.0319(9) _cell_angle_alpha 84.1510(10) _cell_angle_beta 86.3630(10) _cell_angle_gamma 84.8190(10) _cell_volume 2250.7(2) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.306 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 7570 _cell_measurement_theta_min 1.3 _cell_measurement_theta_max 23.1 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu .602 _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 .736 _exptl_absorpt_correction_T_max .832 _diffrn_reflns_number 45831 _reflns_number_total 22975 _reflns_Friedel_coverage 0 _reflns_number_gt 16191 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 37.67 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .021 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .037 _refine_ls_wR_factor_ref .036 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_number_reflns 16191 _refine_ls_number_parameters 749 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment mixed _refine_ls_shift/su_max .021 _refine_diff_density_min -.665 _refine_diff_density_max .721 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 96 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 112 0 0 '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' N ? 0 12 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 4 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cu ? 0 2 .263 1.266 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 4 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' 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 .858074(14) .758924(11) .270905(9) .01861(7) Uani ? ? 1.00000 ? ? P1 1.04617(3) .77574(2) .335288(18) .01842(14) Uani ? ? 1.00000 ? ? P2 .80229(3) .67099(2) .169557(18) .01851(14) Uani ? ? 1.00000 ? ? N11 .60125(10) .82434(8) .36461(7) .0224(5) Uani ? ? 1.00000 ? ? N12 .71960(10) .77000(8) .37394(6) .0224(5) Uani ? ? 1.00000 ? ? C13 .71371(13) .73500(10) .45426(8) .0259(7) Uani ? ? 1.00000 ? ? N14 .59972(12) .76174(9) .49713(7) .0309(7) Uani ? ? 1.00000 ? ? C15 .53326(14) .81713(10) .43856(9) .0289(7) Uani ? ? 1.00000 ? ? B1 .55981(14) .87991(11) .27982(10) .0260(7) Uani ? ? 1.00000 ? ? N21 .67316(10) .94269(8) .24449(6) .0220(5) Uani ? ? 1.00000 ? ? N22 .79898(10) .90400(7) .22472(6) .0213(5) Uani ? ? 1.00000 ? ? C23 .86233(12) .97927(9) .19275(8) .0231(6) Uani ? ? 1.00000 ? ? N24 .78652(12) 1.06386(8) .19021(7) .0278(6) Uani ? ? 1.00000 ? ? C25 .66983(14) 1.03714(10) .22342(9) .0276(7) Uani ? ? 1.00000 ? ? C110 1.09618(13) .68374(9) .42132(8) .0233(6) Uani ? ? 1.00000 ? ? C111 1.10486(12) .58167(9) .39871(7) .0218(6) Uani ? ? 1.00000 ? ? C112 .98950(13) .53644(10) .39051(8) .0257(7) Uani ? ? 1.00000 ? ? C113 .99646(15) .44145(10) .37285(9) .0305(8) Uani ? ? 1.00000 ? ? C114 1.11872(17) .39015(10) .36266(9) .0340(8) Uani ? ? 1.00000 ? ? C115 1.23456(16) .43409(11) .36976(9) .0336(8) Uani ? ? 1.00000 ? ? C116 1.22725(13) .52933(10) .38770(8) .0272(7) Uani ? ? 1.00000 ? ? C120 1.20581(11) .79191(9) .27561(8) .0213(6) Uani ? ? 1.00000 ? ? C121 1.19246(11) .85688(9) .19468(7) .0203(6) Uani ? ? 1.00000 ? ? C122 1.14333(12) .82354(9) .12462(8) .0233(6) Uani ? ? 1.00000 ? ? C123 1.13132(14) .88273(10) .04992(8) .0281(7) Uani ? ? 1.00000 ? ? C124 1.16819(14) .97633(11) .04430(9) .0306(7) Uani ? ? 1.00000 ? ? C125 1.21714(14) 1.01031(10) .11347(9) .0309(8) Uani ? ? 1.00000 ? ? C126 1.22930(13) .95093(10) .18810(8) .0259(7) Uani ? ? 1.00000 ? ? C130 1.01194(13) .88509(10) .39216(9) .0254(7) Uani ? ? 1.00000 ? ? C131 1.11232(12) .90895(9) .45070(8) .0239(6) Uani ? ? 1.00000 ? ? C132 1.19868(14) .97893(10) .42499(9) .0290(7) Uani ? ? 1.00000 ? ? C133 1.29043(15) 1.00367(12) .47849(10) .0340(8) Uani ? ? 1.00000 ? ? C134 1.29768(15) .95789(12) .55862(10) .0356(9) Uani ? ? 1.00000 ? ? C135 1.21162(18) .88861(11) .58595(9) .0376(9) Uani ? ? 1.00000 ? ? C136 1.11909(16) .86493(11) .53255(9) .0324(8) Uani ? ? 1.00000 ? ? C210 .63686(12) .62204(10) .18003(8) .0244(6) Uani ? ? 1.00000 ? ? C211 .62837(12) .54284(10) .25058(8) .0240(6) Uani ? ? 1.00000 ? ? C212 .60764(15) .56456(13) .33342(9) .0357(9) Uani ? ? 1.00000 ? ? C213 .60651(18) .49162(17) .39887(11) .0507(12) Uani ? ? 1.00000 ? ? C214 .62210(18) .39676(17) .38285(12) .0537(12) Uani ? ? 1.00000 ? ? C215 .64032(18) .37390(14) .30107(13) .0477(11) Uani ? ? 1.00000 ? ? C216 .64407(15) .44657(11) .23531(10) .0336(8) Uani ? ? 1.00000 ? ? C220 .79407(14) .75460(10) .07147(8) .0254(7) Uani ? ? 1.00000 ? ? C221 .68635(12) .74693(9) .01254(7) .0224(6) Uani ? ? 1.00000 ? ? C222 .57196(15) .81011(11) .01467(9) .0318(8) Uani ? ? 1.00000 ? ? C223 .47307(15) .80720(13) -.04140(10) .0387(9) Uani ? ? 1.00000 ? ? C224 .48618(15) .74070(12) -.09938(10) .0374(9) Uani ? ? 1.00000 ? ? C225 .59651(17) .67606(12) -.10086(9) .0357(9) Uani ? ? 1.00000 ? ? C226 .69666(14) .67908(10) -.04566(8) .0286(7) Uani ? ? 1.00000 ? ? C230 .90184(12) .56268(9) .13603(8) .0233(6) Uani ? ? 1.00000 ? ? C231 1.04602(12) .57480(8) .11162(7) .0211(6) Uani ? ? 1.00000 ? ? C232 1.14130(13) .55666(9) .17164(8) .0246(6) Uani ? ? 1.00000 ? ? C233 1.27483(13) .56775(10) .14992(9) .0284(7) Uani ? ? 1.00000 ? ? C234 1.31453(13) .59799(10) .06776(9) .0296(7) Uani ? ? 1.00000 ? ? C235 1.22094(14) .61621(10) .00748(8) .0283(7) Uani ? ? 1.00000 ? ? C236 1.08766(13) .60408(10) .02918(8) .0248(6) Uani ? ? 1.00000 ? ? C2 .6632(2) .81340(15) .70526(13) .0463(11) Uani ? ? 1.00000 ? ? O2 .54244(13) .82329(11) .66546(8) .0507(9) Uani ? ? 1.00000 ? ? C3 1.0129(3) .74870(19) -.20034(17) .0717(18) Uani ? ? 1.00000 ? ? O3 1.1212(2) .75276(12) -.15717(13) .1025(16) Uani ? ? 1.00000 ? ? H110a 1.1800(17) .6992(12) .4399(10) .031(4) Uiso ? ? 1.00000 ? ? H110b 1.0321(16) .6917(12) .4664(10) .031(4) Uiso ? ? 1.00000 ? ? H112 .9058(17) .5701(12) .3993(10) .031(4) Uiso ? ? 1.00000 ? ? H113 .9200(17) .4121(12) .3672(10) .031(4) Uiso ? ? 1.00000 ? ? H114 1.1259(17) .3273(13) .3515(11) .036(5) Uiso ? ? 1.00000 ? ? H115 1.3172(18) .4015(13) .3627(11) .040(5) Uiso ? ? 1.00000 ? ? H116 1.3073(17) .5575(12) .3931(10) .031(4) Uiso ? ? 1.00000 ? ? H120a 1.2651(15) .8146(11) .3120(10) .025(4) Uiso ? ? 1.00000 ? ? H120b 1.2413(15) .7305(11) .2631(9) .024(4) Uiso ? ? 1.00000 ? ? H122 1.1197(16) .7614(12) .1282(10) .028(4) Uiso ? ? 1.00000 ? ? H123 1.1008(16) .8582(12) .0032(11) .031(4) Uiso ? ? 1.00000 ? ? H124 1.1599(17) 1.0177(13) -.0081(11) .038(5) Uiso ? ? 1.00000 ? ? H125 1.2406(17) 1.0725(13) .1107(11) .039(5) Uiso ? ? 1.00000 ? ? H126 1.2650(16) .9733(11) .2343(10) .029(4) Uiso ? ? 1.00000 ? ? H132 1.1902(17) 1.0136(13) .3700(11) .037(5) Uiso ? ? 1.00000 ? ? H133 1.348(2) 1.0514(14) .4602(12) .046(5) Uiso ? ? 1.00000 ? ? H134 1.3603(19) .9729(14) .5953(12) .046(5) Uiso ? ? 1.00000 ? ? H135 1.2135(19) .8580(14) .6421(12) .046(5) Uiso ? ? 1.00000 ? ? H136 1.058(2) .8186(14) .5526(12) .047(5) Uiso ? ? 1.00000 ? ? H210a .5748(16) .6730(12) .1876(10) .030(4) Uiso ? ? 1.00000 ? ? H210b .6207(16) .6005(12) .1266(10) .030(4) Uiso ? ? 1.00000 ? ? H212 .5922(19) .6300(14) .3430(12) .046(5) Uiso ? ? 1.00000 ? ? H213 .594(2) .5093(15) .4523(14) .059(6) Uiso ? ? 1.00000 ? ? H214 .618(2) .3492(17) .4228(15) .068(7) Uiso ? ? 1.00000 ? ? H215 .652(2) .3116(16) .2854(13) .059(6) Uiso ? ? 1.00000 ? ? H216 .6619(18) .4303(13) .1808(12) .045(5) Uiso ? ? 1.00000 ? ? H222 .5648(18) .8546(13) .0546(12) .041(5) Uiso ? ? 1.00000 ? ? H223 .403(2) .8487(15) -.0375(13) .055(6) Uiso ? ? 1.00000 ? ? H224 .4210(18) .7403(13) -.1401(12) .042(5) Uiso ? ? 1.00000 ? ? H225 .608(2) .6315(15) -.1430(13) .055(6) Uiso ? ? 1.00000 ? ? H226 .7731(18) .6353(13) -.0478(11) .040(5) Uiso ? ? 1.00000 ? ? H230a .8927(17) .5150(12) .1836(11) .034(4) Uiso ? ? 1.00000 ? ? H230b .8582(17) .5435(12) .0901(11) .033(4) Uiso ? ? 1.00000 ? ? H232 1.1152(16) .5377(12) .2284(11) .032(4) Uiso ? ? 1.00000 ? ? H233 1.3377(17) .5525(12) .1910(11) .036(5) Uiso ? ? 1.00000 ? ? H234 1.4053(18) .6077(13) .0535(11) .039(5) Uiso ? ? 1.00000 ? ? H235 1.2453(16) .6394(12) -.0497(11) .032(4) Uiso ? ? 1.00000 ? ? H236 1.0254(16) .6171(12) -.0129(10) .030(4) Uiso ? ? 1.00000 ? ? H220a .8781(18) .7463(13) .0453(11) .038(5) Uiso ? ? 1.00000 ? ? H220b .7825(17) .8156(12) .0908(10) .033(4) Uiso ? ? 1.00000 ? ? H130a .9281(18) .8760(13) .4238(11) .041(5) Uiso ? ? 1.00000 ? ? H130b .9952(17) .9368(13) .3488(11) .037(5) Uiso ? ? 1.00000 ? ? H13 .7829(16) .6938(11) .4774(10) .026(4) Uiso ? ? 1.00000 ? ? H15 .4492(17) .8498(12) .4470(11) .035(5) Uiso ? ? 1.00000 ? ? H1a .4715(16) .9296(12) .2947(10) .033(4) Uiso ? ? 1.00000 ? ? H1b .5450(16) .8273(12) .2341(10) .031(4) Uiso ? ? 1.00000 ? ? H23 .9515(17) .9735(12) .1734(10) .030(4) Uiso ? ? 1.00000 ? ? H25 .5916(17) 1.0798(12) .2328(11) .036(5) Uiso ? ? 1.00000 ? ? H2 .556(3) .7852(19) .6092(17) .087(8) Uiso ? ? 1.00000 ? ? H2a .744(2) .8260(15) .6604(13) .058(6) Uiso ? ? 1.00000 ? ? H2b .679(3) .739(2) .7352(16) .088(8) Uiso ? ? 1.00000 ? ? H2c .655(3) .862(2) .7575(18) .104(9) Uiso ? ? 1.00000 ? ? H3a 1.03238 .76894 -.25830 .10700 Uiso ? ? 1.00000 ? ? H3b .94289 .79209 -.17951 .10700 Uiso ? ? 1.00000 ? ? H3c .98636 .68483 -.19557 .10700 Uiso ? ? 1.00000 ? ? H3 1.15561 .81049 -.17368 .15000 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 .01574(6) .02270(7) .01749(6) -.00080(5) -.00205(5) -.00247(5) P1 .01659(12) .02143(13) .01743(12) -.00136(10) -.00329(10) -.00161(10) P2 .01794(12) .02111(13) .01690(12) -.00391(10) -.00168(10) -.00135(10) N11 .0169(4) .0265(5) .0238(5) -.0011(4) .0019(3) -.0048(4) N12 .0186(4) .0281(5) .0203(4) -.0003(4) -.0004(3) -.0028(4) C13 .0252(6) .0311(6) .0212(5) -.0034(5) .0011(4) -.0019(5) N14 .0314(6) .0366(6) .0243(5) -.0055(5) .0074(4) -.0043(4) C15 .0247(6) .0315(7) .0301(6) -.0026(5) .0074(5) -.0067(5) B1 .0181(6) .0313(7) .0285(7) -.0002(5) -.0029(5) -.0023(5) N21 .0187(4) .0246(5) .0218(4) .0035(3) -.0023(3) -.0020(4) N22 .0177(4) .0241(5) .0214(4) .0018(3) -.0014(3) -.0023(4) C23 .0223(5) .0253(6) .0210(5) .0005(4) -.0014(4) -.0005(4) N24 .0299(5) .0241(5) .0278(5) .0018(4) -.0011(4) .0009(4) C25 .0272(6) .0258(6) .0277(6) .0058(5) -.0015(5) .0001(5) C110 .0253(5) .0267(6) .0179(5) -.0023(4) -.0047(4) -.0003(4) C111 .0245(5) .0249(5) .0156(5) -.0023(4) -.0035(4) .0023(4) C112 .0245(6) .0307(6) .0217(5) -.0042(5) -.0003(4) -.0002(5) C113 .0361(7) .0300(7) .0261(6) -.0111(5) -.0015(5) .0016(5) C114 .0478(9) .0228(6) .0305(7) -.0006(6) -.0060(6) .0016(5) C115 .0350(7) .0314(7) .0325(7) .0080(6) -.0080(6) .0011(5) C116 .0237(6) .0315(6) .0256(6) .0003(5) -.0067(4) .0024(5) C120 .0165(4) .0252(5) .0220(5) -.0007(4) -.0034(4) -.0003(4) C121 .0163(4) .0237(5) .0204(5) -.0010(4) -.0009(4) -.0008(4) C122 .0236(5) .0242(6) .0221(5) -.0014(4) -.0013(4) -.0036(4) C123 .0284(6) .0352(7) .0205(5) -.0002(5) -.0026(5) -.0030(5) C124 .0305(6) .0350(7) .0239(6) -.0009(5) .0003(5) .0064(5) C125 .0315(7) .0276(6) .0332(7) -.0079(5) -.0009(5) .0040(5) C126 .0241(5) .0285(6) .0259(6) -.0068(5) -.0040(4) -.0008(5) C130 .0229(5) .0265(6) .0275(6) .0015(4) -.0056(4) -.0074(5) C131 .0240(5) .0246(6) .0237(5) .0026(4) -.0033(4) -.0079(4) C132 .0322(7) .0291(6) .0269(6) -.0038(5) -.0023(5) -.0076(5) C133 .0303(7) .0370(8) .0378(7) -.0070(6) -.0007(6) -.0159(6) C134 .0343(7) .0395(8) .0360(7) .0056(6) -.0117(6) -.0200(6) C135 .0550(10) .0340(7) .0251(6) .0033(7) -.0127(6) -.0090(6) C136 .0434(8) .0306(7) .0247(6) -.0062(6) -.0028(5) -.0071(5) C210 .0198(5) .0283(6) .0258(6) -.0060(4) -.0046(4) -.0000(5) C211 .0177(5) .0320(6) .0229(5) -.0084(4) -.0006(4) -.0002(4) C212 .0311(7) .0519(9) .0269(6) -.0184(6) .0052(5) -.0081(6) C213 .0412(9) .0885(15) .0247(7) -.0317(9) .0006(6) .0051(8) C214 .0372(9) .0731(14) .0472(10) -.0236(9) -.0066(7) .0316(10) C215 .0421(9) .0367(9) .0611(12) -.0114(7) .0028(8) .0139(8) C216 .0356(7) .0311(7) .0341(7) -.0100(6) .0048(6) -.0008(6) C220 .0320(6) .0245(6) .0205(5) -.0080(5) -.0051(5) .0013(4) C221 .0255(5) .0230(5) .0181(5) -.0024(4) -.0015(4) .0021(4) C222 .0343(7) .0318(7) .0266(6) .0043(5) .0020(5) .0017(5) C223 .0250(6) .0461(9) .0397(8) .0052(6) -.0002(6) .0130(7) C224 .0321(7) .0463(9) .0332(7) -.0112(6) -.0123(6) .0129(6) C225 .0451(8) .0360(8) .0276(7) -.0065(6) -.0137(6) -.0010(6) C226 .0308(6) .0303(6) .0246(6) .0012(5) -.0073(5) -.0023(5) C230 .0234(5) .0226(5) .0246(5) -.0058(4) .0013(4) -.0044(4) C231 .0228(5) .0194(5) .0214(5) -.0026(4) .0009(4) -.0044(4) C232 .0269(6) .0246(6) .0212(5) -.0002(4) .0001(4) .0006(4) C233 .0246(6) .0315(7) .0285(6) .0011(5) -.0040(5) -.0016(5) C234 .0224(6) .0337(7) .0323(7) -.0026(5) .0026(5) -.0037(5) C235 .0285(6) .0332(7) .0231(6) -.0043(5) .0046(5) -.0039(5) C236 .0263(6) .0297(6) .0192(5) -.0036(5) -.0011(4) -.0051(4) C2 .0454(10) .0471(10) .0452(10) -.0020(8) .0019(8) -.0029(8) O2 .0438(7) .0678(9) .0419(7) -.0015(6) .0045(5) -.0193(6) C3 .0721(15) .0705(15) .0773(16) -.0293(12) -.0186(13) -.0004(12) O3 .1437(18) .0474(9) .1243(16) -.0404(10) -.0875(14) .0322(10) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Cu P1 . . 2.2642(4) ? Cu P2 . . 2.2647(4) ? Cu N12 . . 2.1063(10) ? Cu N22 . . 2.1383(10) ? P1 C110 . . 1.8521(12) ? P1 C120 . . 1.8451(12) ? P1 C130 . . 1.8574(14) ? P2 C210 . . 1.8579(13) ? P2 C220 . . 1.8647(13) ? P2 C230 . . 1.8524(13) ? N11 N12 . . 1.3685(14) ? N11 C15 . . 1.3319(17) ? N11 B1 . . 1.5582(18) ? N12 C13 . . 1.3302(16) ? C13 N14 . . 1.3484(17) ? C13 H13 . . .937(15) ? N14 C15 . . 1.3320(18) ? C15 H15 . . .938(17) ? B1 N21 . . 1.5526(18) ? B1 H1a . . 1.111(16) ? B1 H1b . . 1.117(17) ? N21 N22 . . 1.3697(14) ? N21 C25 . . 1.3306(17) ? N22 C23 . . 1.3258(16) ? C23 N24 . . 1.3516(16) ? C23 H23 . . .935(16) ? N24 C25 . . 1.3337(18) ? C25 H25 . . .962(17) ? C110 C111 . . 1.5052(18) ? C110 H110a . . .966(18) ? C110 H110b . . .949(16) ? C111 C112 . . 1.398(2) ? C111 C116 . . 1.3925(17) ? C112 C113 . . 1.384(2) ? C112 H112 . . .942(16) ? C113 C114 . . 1.383(2) ? C113 H113 . . .922(18) ? C114 C115 . . 1.389(2) ? C114 H114 . . .912(19) ? C115 C116 . . 1.389(2) ? C115 H115 . . .922(18) ? C116 H116 . . .945(18) ? C120 C121 . . 1.5135(16) ? C120 H120a . . .958(17) ? C120 H120b . . .938(16) ? C121 C122 . . 1.3955(18) ? C121 C126 . . 1.3943(18) ? C122 C123 . . 1.3911(18) ? C122 H122 . . .919(17) ? C123 C124 . . 1.389(2) ? C123 H123 . . .936(18) ? C124 C125 . . 1.386(2) ? C124 H124 . . .975(17) ? C125 C126 . . 1.392(2) ? C125 H125 . . .920(19) ? C126 H126 . . .937(17) ? C130 C131 . . 1.507(2) ? C130 H130a . . .973(18) ? C130 H130b . . .963(17) ? C131 C132 . . 1.387(2) ? C131 C136 . . 1.3950(18) ? C132 C133 . . 1.392(2) ? C132 H132 . . .968(17) ? C133 C134 . . 1.380(2) ? C133 H133 . . .94(2) ? C134 C135 . . 1.383(2) ? C134 H134 . . .94(2) ? C135 C136 . . 1.392(2) ? C135 H135 . . .957(19) ? C136 H136 . . .95(2) ? C210 C211 . . 1.5062(18) ? C210 H210a . . .920(16) ? C210 H210b . . .964(18) ? C211 C212 . . 1.392(2) ? C211 C216 . . 1.389(2) ? C212 C213 . . 1.389(3) ? C212 H212 . . .94(2) ? C213 C214 . . 1.373(3) ? C213 H213 . . .91(2) ? C214 C215 . . 1.378(3) ? C214 H214 . . .88(2) ? C215 C216 . . 1.391(2) ? C215 H215 . . .93(2) ? C216 H216 . . .93(2) ? C220 C221 . . 1.505(2) ? C220 H220a . . .928(18) ? C220 H220b . . .934(18) ? C221 C222 . . 1.3937(19) ? C221 C226 . . 1.392(2) ? C222 C223 . . 1.393(2) ? C222 H222 . . .93(2) ? C223 C224 . . 1.374(3) ? C223 H223 . . .88(2) ? C224 C225 . . 1.374(2) ? C224 H224 . . .96(2) ? C225 C226 . . 1.394(2) ? C225 H225 . . .96(2) ? C226 H226 . . .944(18) ? C230 C231 . . 1.5070(17) ? C230 H230a . . .967(16) ? C230 H230b . . .956(18) ? C231 C232 . . 1.3945(18) ? C231 C236 . . 1.3940(17) ? C232 C233 . . 1.3927(19) ? C232 H232 . . .950(16) ? C233 C234 . . 1.388(2) ? C233 H233 . . .940(18) ? C234 C235 . . 1.385(2) ? C234 H234 . . .951(18) ? C235 C236 . . 1.3929(19) ? C235 H235 . . .965(16) ? C236 H236 . . .946(17) ? C2 O2 . . 1.404(2) ? C2 H2a . . 1.07(2) ? C2 H2b . . 1.10(3) ? C2 H2c . . 1.13(3) ? O2 H2 . . 1.09(3) ? C3 O3 . . 1.342(4) ? C3 H3a . . .957 ? C3 H3b . . .958 ? C3 H3c . . .952 ? O3 H3 . . .9174 ? 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 P2 . . . 135.685(13) ? P1 Cu N12 . . . 99.26(3) ? P1 Cu N22 . . . 102.15(3) ? P2 Cu N12 . . . 115.90(3) ? P2 Cu N22 . . . 103.85(3) ? N12 Cu N22 . . . 90.01(4) ? Cu P1 C110 . . . 118.02(5) ? Cu P1 C120 . . . 121.90(4) ? Cu P1 C130 . . . 106.15(4) ? C110 P1 C120 . . . 101.87(6) ? C110 P1 C130 . . . 101.57(6) ? C120 P1 C130 . . . 104.91(6) ? Cu P2 C210 . . . 118.37(4) ? Cu P2 C220 . . . 106.15(5) ? Cu P2 C230 . . . 124.49(4) ? C210 P2 C220 . . . 103.44(6) ? C210 P2 C230 . . . 98.18(6) ? C220 P2 C230 . . . 103.72(6) ? N12 N11 C15 . . . 107.36(10) ? N12 N11 B1 . . . 123.47(10) ? C15 N11 B1 . . . 129.15(10) ? Cu N12 N11 . . . 120.23(7) ? Cu N12 C13 . . . 135.92(8) ? N11 N12 C13 . . . 103.85(9) ? N12 C13 N14 . . . 114.26(11) ? N12 C13 H13 . . . 121.6(9) ? N14 C13 H13 . . . 124.1(9) ? C13 N14 C15 . . . 102.09(11) ? N11 C15 N14 . . . 112.43(12) ? N11 C15 H15 . . . 122.0(10) ? N14 C15 H15 . . . 125.5(10) ? N11 B1 N21 . . . 108.58(10) ? N11 B1 H1a . . . 106.6(8) ? N11 B1 H1b . . . 109.4(8) ? N21 B1 H1a . . . 107.4(9) ? N21 B1 H1b . . . 109.1(8) ? H1a B1 H1b . . . 115.5(12) ? B1 N21 N22 . . . 122.51(10) ? B1 N21 C25 . . . 129.80(10) ? N22 N21 C25 . . . 107.59(10) ? Cu N22 N21 . . . 119.44(7) ? Cu N22 C23 . . . 135.05(8) ? N21 N22 C23 . . . 103.92(9) ? N22 C23 N24 . . . 114.13(11) ? N22 C23 H23 . . . 122.3(10) ? N24 C23 H23 . . . 123.6(10) ? C23 N24 C25 . . . 102.27(11) ? N21 C25 N24 . . . 112.09(11) ? N21 C25 H25 . . . 122.5(10) ? N24 C25 H25 . . . 125.4(10) ? P1 C110 C111 . . . 114.52(9) ? P1 C110 H110a . . . 107.8(9) ? P1 C110 H110b . . . 106.3(10) ? C111 C110 H110a . . . 111.0(10) ? C111 C110 H110b . . . 109.9(10) ? H110a C110 H110b . . . 107.0(15) ? C110 C111 C112 . . . 120.48(11) ? C110 C111 C116 . . . 121.02(12) ? C112 C111 C116 . . . 118.48(12) ? C111 C112 C113 . . . 120.86(12) ? C111 C112 H112 . . . 119.7(11) ? C113 C112 H112 . . . 119.4(11) ? C112 C113 C114 . . . 120.02(14) ? C112 C113 H113 . . . 120.5(10) ? C114 C113 H113 . . . 119.5(10) ? C113 C114 C115 . . . 120.00(14) ? C113 C114 H114 . . . 121.7(11) ? C115 C114 H114 . . . 118.3(11) ? C114 C115 C116 . . . 119.85(13) ? C114 C115 H115 . . . 121.5(12) ? C116 C115 H115 . . . 118.6(12) ? C111 C116 C115 . . . 120.79(13) ? C111 C116 H116 . . . 120.8(10) ? C115 C116 H116 . . . 118.4(10) ? P1 C120 C121 . . . 113.55(8) ? P1 C120 H120a . . . 108.1(9) ? P1 C120 H120b . . . 106.6(9) ? C121 C120 H120a . . . 112.1(9) ? C121 C120 H120b . . . 109.1(9) ? H120a C120 H120b . . . 107.0(13) ? C120 C121 C122 . . . 120.50(11) ? C120 C121 C126 . . . 121.03(11) ? C122 C121 C126 . . . 118.47(11) ? C121 C122 C123 . . . 120.80(12) ? C121 C122 H122 . . . 119.1(10) ? C123 C122 H122 . . . 120.1(10) ? C122 C123 C124 . . . 120.12(13) ? C122 C123 H123 . . . 119.3(10) ? C124 C123 H123 . . . 120.6(10) ? C123 C124 C125 . . . 119.64(13) ? C123 C124 H124 . . . 120.0(11) ? C125 C124 H124 . . . 120.3(11) ? C124 C125 C126 . . . 120.16(14) ? C124 C125 H125 . . . 120.4(11) ? C126 C125 H125 . . . 119.4(11) ? C121 C126 C125 . . . 120.81(13) ? C121 C126 H126 . . . 119.1(10) ? C125 C126 H126 . . . 120.1(10) ? P1 C130 C131 . . . 119.12(9) ? P1 C130 H130a . . . 104.5(11) ? P1 C130 H130b . . . 104.7(11) ? C131 C130 H130a . . . 109.1(11) ? C131 C130 H130b . . . 111.4(11) ? H130a C130 H130b . . . 107.1(14) ? C130 C131 C132 . . . 120.20(11) ? C130 C131 C136 . . . 122.02(12) ? C132 C131 C136 . . . 117.75(13) ? C131 C132 C133 . . . 121.29(13) ? C131 C132 H132 . . . 118.5(11) ? C133 C132 H132 . . . 120.1(11) ? C132 C133 C134 . . . 120.15(15) ? C132 C133 H133 . . . 120.2(12) ? C134 C133 H133 . . . 119.7(12) ? C133 C134 C135 . . . 119.58(16) ? C133 C134 H134 . . . 121.3(11) ? C135 C134 H134 . . . 119.1(11) ? C134 C135 C136 . . . 120.03(14) ? C134 C135 H135 . . . 120.4(12) ? C136 C135 H135 . . . 119.6(12) ? C131 C136 C135 . . . 121.18(14) ? C131 C136 H136 . . . 119.4(12) ? C135 C136 H136 . . . 119.4(12) ? P2 C210 C211 . . . 112.03(9) ? P2 C210 H210a . . . 106.9(11) ? P2 C210 H210b . . . 107.4(10) ? C211 C210 H210a . . . 112.1(10) ? C211 C210 H210b . . . 112.0(9) ? H210a C210 H210b . . . 105.9(14) ? C210 C211 C212 . . . 120.48(13) ? C210 C211 C216 . . . 121.31(12) ? C212 C211 C216 . . . 118.19(13) ? C211 C212 C213 . . . 120.57(17) ? C211 C212 H212 . . . 117.6(11) ? C213 C212 H212 . . . 121.8(11) ? C212 C213 C214 . . . 120.59(17) ? C212 C213 H213 . . . 117.5(13) ? C214 C213 H213 . . . 121.9(13) ? C213 C214 C215 . . . 119.61(18) ? C213 C214 H214 . . . 122.5(16) ? C215 C214 H214 . . . 117.8(16) ? C214 C215 C216 . . . 120.10(18) ? C214 C215 H215 . . . 124.5(13) ? C216 C215 H215 . . . 115.4(13) ? C211 C216 C215 . . . 120.91(15) ? C211 C216 H216 . . . 119.7(11) ? C215 C216 H216 . . . 119.3(11) ? P2 C220 C221 . . . 118.83(10) ? P2 C220 H220a . . . 104.4(10) ? P2 C220 H220b . . . 103.8(10) ? C221 C220 H220a . . . 111.9(12) ? C221 C220 H220b . . . 108.3(10) ? H220a C220 H220b . . . 109.1(15) ? C220 C221 C222 . . . 119.74(12) ? C220 C221 C226 . . . 122.41(11) ? C222 C221 C226 . . . 117.85(13) ? C221 C222 C223 . . . 120.97(14) ? C221 C222 H222 . . . 117.5(11) ? C223 C222 H222 . . . 121.6(11) ? C222 C223 C224 . . . 120.27(14) ? C222 C223 H223 . . . 117.4(15) ? C224 C223 H223 . . . 122.3(15) ? C223 C224 C225 . . . 119.58(15) ? C223 C224 H224 . . . 120.9(11) ? C225 C224 H224 . . . 119.5(11) ? C224 C225 C226 . . . 120.56(15) ? C224 C225 H225 . . . 120.0(12) ? C226 C225 H225 . . . 119.3(12) ? C221 C226 C225 . . . 120.73(13) ? C221 C226 H226 . . . 119.2(12) ? C225 C226 H226 . . . 120.1(12) ? P2 C230 C231 . . . 115.80(9) ? P2 C230 H230a . . . 104.0(10) ? P2 C230 H230b . . . 106.1(10) ? C231 C230 H230a . . . 111.1(10) ? C231 C230 H230b . . . 110.5(10) ? H230a C230 H230b . . . 109.0(15) ? C230 C231 C232 . . . 120.33(11) ? C230 C231 C236 . . . 121.28(11) ? C232 C231 C236 . . . 118.38(11) ? C231 C232 C233 . . . 120.90(12) ? C231 C232 H232 . . . 120.0(10) ? C233 C232 H232 . . . 119.1(10) ? C232 C233 C234 . . . 120.04(12) ? C232 C233 H233 . . . 119.3(10) ? C234 C233 H233 . . . 120.6(10) ? C233 C234 C235 . . . 119.68(12) ? C233 C234 H234 . . . 119.9(11) ? C235 C234 H234 . . . 120.4(11) ? C234 C235 C236 . . . 120.17(12) ? C234 C235 H235 . . . 121.4(10) ? C236 C235 H235 . . . 118.4(10) ? C231 C236 C235 . . . 120.82(12) ? C231 C236 H236 . . . 120.4(10) ? C235 C236 H236 . . . 118.8(10) ? O2 C2 H2a . . . 110.5(12) ? O2 C2 H2b . . . 108.7(14) ? O2 C2 H2c . . . 108.5(14) ? H2a C2 H2b . . . 108.4(17) ? H2a C2 H2c . . . 114.1(19) ? H2b C2 H2c . . . 106(2) ? C2 O2 H2 . . . 108.4(13) ? O3 C3 H3a . . . 109.2 ? O3 C3 H3b . . . 109.0 ? O3 C3 H3c . . . 110.7 ? H3a C3 H3b . . . 108.2 ? H3a C3 H3c . . . 109.0 ? H3b C3 H3c . . . 110.6 ? C3 O3 H3 . . . 107.9 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _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_000 932 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 -23 _reflns_limit_k_max 24 _reflns_limit_l_min -27 _reflns_limit_l_max 27 _reflns_number_observed ? _reflns_d_resolution_high .581 _reflns_d_resolution_low 15.874 _diffrn_reflns_av_sigmaI/netI .085 _diffrn_reflns_theta_min 1.28 _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 .066 _refine_ls_wR_factor_all .04 _refine_ls_goodness_of_fit_all .943 _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 loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end data_cpdar5 _database_code_CSD 176922 _audit_creation_method Xtal3.6 _audit_creation_date 01-09-02 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C23 H43 B1 Cu1 N6 O1 P1' _chemical_formula_moiety ? _chemical_formula_weight 524.97 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P21/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 13.7270(10) _cell_length_b 10.1806(9) _cell_length_c 19.682(2) _cell_angle_alpha 90.00000 _cell_angle_beta 105.600(2) _cell_angle_gamma 90.00000 _cell_volume 2649.2(4) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.316 _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 2.4 _cell_measurement_theta_max 20.4 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu .912 _exptl_crystal_description prism _exptl_crystal_size_max .5 _exptl_crystal_size_mid .45 _exptl_crystal_size_min .35 _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 .62 _exptl_absorpt_correction_T_max .86 _diffrn_reflns_number 53960 _reflns_number_total 6982 _reflns_Friedel_coverage 0 _reflns_number_gt 5856 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 28.9 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .075 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .057 _refine_ls_wR_factor_ref .071 _refine_ls_goodness_of_fit_ref 1.489 _refine_ls_number_reflns 5653 _refine_ls_number_parameters 470 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max .015 _refine_diff_density_min -1.233 _refine_diff_density_max 2.147 _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 92 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 172 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' O ? 0 4 .008 .006 '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' 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 .87865(3) .20903(4) .73499(2) .01669(17) Uani ? ? 1.00000 ? ? P .93587(6) .15258(8) .64318(4) .0167(3) Uani ? ? 1.00000 ? ? C111 .8940(3) .2671(3) .56740(17) .0203(14) Uani ? ? 1.00000 ? ? C112 .9066(3) .2191(4) .49664(19) .0253(15) Uani ? ? 1.00000 ? ? C113 .8772(3) .3253(4) .4399(2) .0337(18) Uani ? ? 1.00000 ? ? C114 .7702(3) .3745(4) .4327(2) .0356(19) Uani ? ? 1.00000 ? ? C115 .7598(3) .4258(4) .5025(2) .0296(16) Uani ? ? 1.00000 ? ? C116 .7867(3) .3213(4) .55992(18) .0240(15) Uani ? ? 1.00000 ? ? C121 1.0757(2) .1416(3) .65633(17) .0194(13) Uani ? ? 1.00000 ? ? C122 1.1293(3) .0965(4) .73208(18) .0240(15) Uani ? ? 1.00000 ? ? C123 1.2427(3) .0772(4) .74159(19) .0253(15) Uani ? ? 1.00000 ? ? C124 1.2909(3) .2057(4) .7273(2) .0269(15) Uani ? ? 1.00000 ? ? C125 1.2393(3) .2550(4) .6543(2) .0278(16) Uani ? ? 1.00000 ? ? C126 1.1249(3) .2700(3) .6414(2) .0246(15) Uani ? ? 1.00000 ? ? C131 .8946(3) -.0125(3) .60449(17) .0206(13) Uani ? ? 1.00000 ? ? C132 .7796(3) -.0195(4) .5761(2) .0256(15) Uani ? ? 1.00000 ? ? C133 .7423(3) -.1577(4) .5499(2) .0307(17) Uani ? ? 1.00000 ? ? C134 .7800(3) -.2587(4) .6078(2) .0326(18) Uani ? ? 1.00000 ? ? C135 .8940(3) -.2576(4) .6313(3) .0312(18) Uani ? ? 1.00000 ? ? C136 .9348(3) -.1218(3) .6585(2) .0246(15) Uani ? ? 1.00000 ? ? N11 .8912(2) .4968(3) .78161(14) .0175(11) Uani ? ? 1.00000 ? ? N12 .8266(2) .4098(2) .73970(14) .0176(11) Uani ? ? 1.00000 ? ? C13 .7373(2) .4704(3) .72491(17) .0187(13) Uani ? ? 1.00000 ? ? N14 .7414(2) .5914(3) .75475(14) .0183(11) Uani ? ? 1.00000 ? ? C15 .8386(2) .6027(3) .78962(17) .0181(12) Uani ? ? 1.00000 ? ? N21 1.00768(19) .3454(3) .86416(15) .0196(11) Uani ? ? 1.00000 ? ? N22 .9637(2) .2270(3) .84066(14) .0186(11) Uani ? ? 1.00000 ? ? C23 .9730(3) .1598(3) .89957(18) .0228(14) Uani ? ? 1.00000 ? ? N24 1.0197(2) .2248(3) .95900(16) .0272(13) Uani ? ? 1.00000 ? ? C25 1.0393(3) .3402(3) .93370(19) .0253(15) Uani ? ? 1.00000 ? ? B 1.0052(3) .4621(4) .8127(2) .0217(15) Uani ? ? 1.00000 ? ? C01 .4568(3) .3395(4) .6122(2) .0310(17) Uani ? ? 1.00000 ? ? O01 .55430(18) .3406(3) .60122(14) .0241(11) Uani ? ? 1.00000 ? ? H111 .938(3) .336(5) .582(2) .029(11) Uiso ? ? 1.00000 ? ? H112a .867(3) .143(5) .478(2) .030(11) Uiso ? ? 1.00000 ? ? H112b .973(3) .197(4) .500(2) .032(12) Uiso ? ? 1.00000 ? ? H113a .880(4) .289(5) .397(3) .052(15) Uiso ? ? 1.00000 ? ? H113b .928(3) .402(5) .455(2) .030(11) Uiso ? ? 1.00000 ? ? H114a .715(4) .299(6) .412(3) .056(16) Uiso ? ? 1.00000 ? ? H114b .751(4) .440(6) .393(3) .052(14) Uiso ? ? 1.00000 ? ? H115a .687(3) .461(4) .497(2) .031(11) Uiso ? ? 1.00000 ? ? H115b .810(3) .502(4) .515(2) .021(10) Uiso ? ? 1.00000 ? ? H116a .780(3) .343(4) .604(2) .014(9) Uiso ? ? 1.00000 ? ? H116b .732(4) .248(5) .541(3) .045(13) Uiso ? ? 1.00000 ? ? H121 1.094(3) .077(4) .6240(18) .013(8) Uiso ? ? 1.00000 ? ? H122a 1.088(3) .013(5) .741(2) .032(11) Uiso ? ? 1.00000 ? ? H122b 1.120(3) .167(5) .760(2) .034(12) Uiso ? ? 1.00000 ? ? H123a 1.256(3) .006(4) .7065(18) .012(8) Uiso ? ? 1.00000 ? ? H123b 1.269(3) .044(4) .788(2) .022(10) Uiso ? ? 1.00000 ? ? H124a 1.363(3) .193(4) .733(2) .030(11) Uiso ? ? 1.00000 ? ? H124b 1.274(4) .270(5) .761(3) .039(13) Uiso ? ? 1.00000 ? ? H125a 1.256(4) .192(5) .621(3) .051(15) Uiso ? ? 1.00000 ? ? H125b 1.268(3) .322(4) .643(2) .025(10) Uiso ? ? 1.00000 ? ? H126a 1.109(3) .337(4) .675(2) .021(10) Uiso ? ? 1.00000 ? ? H126b 1.096(3) .287(4) .593(2) .022(10) Uiso ? ? 1.00000 ? ? H131 .925(3) -.026(4) .564(2) .019(9) Uiso ? ? 1.00000 ? ? H132a .756(3) .029(4) .536(2) .030(11) Uiso ? ? 1.00000 ? ? H132b .747(3) .007(4) .6133(18) .012(8) Uiso ? ? 1.00000 ? ? H133a .767(3) -.178(4) .507(2) .029(11) Uiso ? ? 1.00000 ? ? H133b .663(4) -.160(5) .534(3) .049(14) Uiso ? ? 1.00000 ? ? H134a .749(3) -.342(4) .587(2) .028(11) Uiso ? ? 1.00000 ? ? H134b .758(3) -.242(4) .649(2) .029(11) Uiso ? ? 1.00000 ? ? H135a .913(3) -.279(4) .589(2) .024(10) Uiso ? ? 1.00000 ? ? H135b .913(4) -.295(5) .665(3) .036(14) Uiso ? ? 1.00000 ? ? H136a .917(3) -.098(4) .700(2) .022(10) Uiso ? ? 1.00000 ? ? H136b 1.007(3) -.125(4) .6690(19) .014(9) Uiso ? ? 1.00000 ? ? H13 .676(3) .437(4) .6942(18) .010(8) Uiso ? ? 1.00000 ? ? H15 .864(4) .676(5) .821(3) .053(15) Uiso ? ? 1.00000 ? ? H23 .942(3) .072(5) .898(2) .029(11) Uiso ? ? 1.00000 ? ? H25 1.073(4) .405(5) .962(2) .043(13) Uiso ? ? 1.00000 ? ? H1a 1.044(3) .429(4) .771(2) .024(10) Uiso ? ? 1.00000 ? ? H1b 1.042(3) .537(5) .843(2) .042(13) Uiso ? ? 1.00000 ? ? H01a .417(5) .401(8) .585(4) .10(3) Uiso ? ? 1.00000 ? ? H01b .464(4) .362(6) .660(3) .064(17) Uiso ? ? 1.00000 ? ? H01c .410(6) .257(8) .594(4) .10(2) Uiso ? ? 1.00000 ? ? H01 .544(3) .332(4) .561(2) .011(9) 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 .01936(19) .00977(18) .0214(2) -.00089(14) .00620(14) -.00079(15) P .0176(4) .0116(3) .0210(4) .0007(3) .0055(3) -.0000(3) C111 .0232(15) .0161(15) .0226(15) .0017(12) .0077(12) .0019(12) C112 .0288(18) .0233(17) .0256(16) .0076(14) .0103(14) .0034(14) C113 .040(2) .036(2) .0292(19) .0068(18) .0159(16) .0087(17) C114 .043(2) .034(2) .0294(19) .0127(18) .0094(17) .0098(17) C115 .0324(19) .0248(18) .0313(18) .0090(15) .0080(15) .0061(15) C116 .0268(17) .0226(17) .0220(16) .0071(13) .0057(13) .0011(13) C121 .0186(14) .0161(15) .0240(15) .0012(11) .0068(12) .0021(12) C122 .0266(17) .0200(16) .0256(16) .0008(13) .0073(13) .0038(13) C123 .0249(16) .0218(16) .0293(18) .0013(13) .0074(14) .0034(14) C124 .0193(15) .0230(17) .038(2) -.0006(13) .0071(14) -.0027(15) C125 .0241(17) .0210(16) .041(2) -.0011(14) .0135(15) .0049(16) C126 .0233(16) .0184(16) .0323(18) .0009(13) .0082(14) .0056(14) C131 .0265(16) .0139(14) .0227(15) -.0014(12) .0090(12) -.0032(12) C132 .0267(17) .0215(17) .0278(17) -.0039(13) .0062(14) -.0053(14) C133 .033(2) .0265(18) .033(2) -.0103(15) .0104(16) -.0110(16) C134 .042(2) .0220(18) .040(2) -.0107(16) .0205(18) -.0073(16) C135 .045(2) .0117(15) .042(2) -.0006(15) .0199(19) .0008(15) C136 .0267(17) .0128(14) .0352(19) .0003(12) .0098(14) .0001(13) N11 .0209(12) .0074(11) .0240(13) -.0007(10) .0056(10) -.0010(10) N12 .0210(13) .0081(11) .0231(13) -.0015(10) .0045(10) -.0010(10) C13 .0231(15) .0124(14) .0194(14) -.0010(11) .0037(12) -.0009(11) N14 .0228(13) .0110(12) .0213(12) .0008(10) .0065(10) .0005(10) C15 .0232(15) .0093(13) .0221(15) -.0003(11) .0068(12) -.0003(11) N21 .0166(12) .0114(12) .0288(14) -.0002(10) .0028(10) -.0018(11) N22 .0189(12) .0104(12) .0258(14) -.0012(10) .0046(10) -.0015(10) C23 .0260(16) .0162(15) .0245(16) .0023(13) .0040(13) .0025(13) N24 .0295(15) .0240(15) .0253(14) .0017(12) .0024(12) .0022(12) C25 .0237(16) .0173(15) .0312(18) .0008(13) .0008(14) -.0052(14) B .0157(16) .0132(16) .036(2) -.0005(13) .0063(14) .0029(15) C01 .0281(18) .0210(17) .044(2) .0005(15) .0088(16) .0052(17) O01 .0263(12) .0207(12) .0233(13) .0008(10) .0032(10) -.0019(10) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Cu P . . 2.2307(10) ? Cu N12 . . 2.175(3) ? Cu N22 . . 2.102(2) ? Cu N14 . '2 646' 2.091(3) ? P C111 . . 1.858(3) ? P C121 . . 1.869(3) ? P C131 . . 1.869(3) ? C111 C112 . . 1.529(5) ? C111 C116 . . 1.542(5) ? C111 H111 . . .92(4) ? C112 C113 . . 1.529(6) ? C112 H112a . . .97(4) ? C112 H112b . . .92(5) ? C113 C114 . . 1.522(7) ? C113 H113a . . .93(6) ? C113 H113b . . 1.04(4) ? C114 C115 . . 1.512(6) ? C114 H114a . . 1.08(6) ? C114 H114b . . 1.00(5) ? C115 C116 . . 1.524(5) ? C115 H115a . . 1.04(4) ? C115 H115b . . 1.03(4) ? C116 H116a . . .92(4) ? C116 H116b . . 1.05(5) ? C121 C122 . . 1.544(4) ? C121 C126 . . 1.535(5) ? C121 H121 . . 1.00(4) ? C122 C123 . . 1.529(5) ? C122 H122a . . 1.06(5) ? C122 H122b . . .93(5) ? C123 C124 . . 1.526(5) ? C123 H123a . . 1.05(4) ? C123 H123b . . .95(4) ? C124 C125 . . 1.507(5) ? C124 H124a . . .97(5) ? C124 H124b . . 1.00(5) ? C125 C126 . . 1.531(5) ? C125 H125a . . .99(6) ? C125 H125b . . .85(5) ? C126 H126a . . 1.02(4) ? C126 H126b . . .94(4) ? C131 C132 . . 1.528(5) ? C131 C136 . . 1.535(5) ? C131 H131 . . 1.00(4) ? C132 C133 . . 1.538(5) ? C132 H132a . . .92(4) ? C132 H132b . . .99(4) ? C133 C134 . . 1.518(6) ? C133 H133a . . 1.01(5) ? C133 H133b . . 1.05(5) ? C134 C135 . . 1.507(6) ? C134 H134a . . .99(4) ? C134 H134b . . .96(5) ? C135 C136 . . 1.533(5) ? C135 H135a . . .96(5) ? C135 H135b . . .75(5) ? C136 H136a . . .95(4) ? C136 H136b . . .96(4) ? N11 N12 . . 1.363(3) ? N11 C15 . . 1.330(4) ? N11 B . . 1.560(4) ? N12 C13 . . 1.332(4) ? C13 N14 . . 1.359(4) ? C13 H13 . . .95(3) ? N14 C15 . . 1.331(4) ? C15 H15 . . .98(5) ? N21 N22 . . 1.371(4) ? N21 C25 . . 1.321(5) ? N21 B . . 1.556(5) ? N22 C23 . . 1.323(4) ? C23 N24 . . 1.347(4) ? C23 H23 . . .98(5) ? N24 C25 . . 1.331(5) ? C25 H25 . . .90(5) ? B H1a . . 1.14(4) ? B H1b . . 1.02(5) ? C01 O01 . . 1.413(5) ? C01 H01a . . .90(7) ? C01 H01b . . .95(7) ? C01 H01c . . 1.06(8) ? O01 H01 . . .78(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 . . . 117.90(8) ? P Cu N22 . . . 126.95(9) ? P Cu N14 . . '2 646' 112.90(8) ? N12 Cu N22 . . . 88.71(10) ? N12 Cu N14 . . '2 646' 104.92(11) ? N22 Cu N14 . . '2 646' 101.36(11) ? Cu P C111 . . . 112.83(12) ? Cu P C121 . . . 118.37(11) ? Cu P C131 . . . 115.32(13) ? C111 P C121 . . . 103.50(16) ? C111 P C131 . . . 104.03(14) ? C121 P C131 . . . 100.95(15) ? P C111 C112 . . . 116.4(2) ? P C111 C116 . . . 112.5(3) ? P C111 H111 . . . 101(3) ? C112 C111 C116 . . . 111.5(3) ? C112 C111 H111 . . . 107(3) ? C116 C111 H111 . . . 107(3) ? C111 C112 C113 . . . 111.5(3) ? C111 C112 H112a . . . 115(3) ? C111 C112 H112b . . . 112(3) ? C113 C112 H112a . . . 106(3) ? C113 C112 H112b . . . 107(3) ? H112a C112 H112b . . . 106(4) ? C112 C113 C114 . . . 111.0(4) ? C112 C113 H113a . . . 108(3) ? C112 C113 H113b . . . 107(2) ? C114 C113 H113a . . . 108(3) ? C114 C113 H113b . . . 110(3) ? H113a C113 H113b . . . 112(4) ? C113 C114 C115 . . . 110.7(3) ? C113 C114 H114a . . . 111(3) ? C113 C114 H114b . . . 110(3) ? C115 C114 H114a . . . 111(3) ? C115 C114 H114b . . . 114(3) ? H114a C114 H114b . . . 100(4) ? C114 C115 C116 . . . 111.7(3) ? C114 C115 H115a . . . 110(2) ? C114 C115 H115b . . . 105(2) ? C116 C115 H115a . . . 111(3) ? C116 C115 H115b . . . 109(2) ? H115a C115 H115b . . . 110(3) ? C111 C116 C115 . . . 110.8(3) ? C111 C116 H116a . . . 109(2) ? C111 C116 H116b . . . 111(3) ? C115 C116 H116a . . . 118(2) ? C115 C116 H116b . . . 103(3) ? H116a C116 H116b . . . 105(4) ? P C121 C122 . . . 110.9(3) ? P C121 C126 . . . 114.2(2) ? P C121 H121 . . . 112(2) ? C122 C121 C126 . . . 108.5(3) ? C122 C121 H121 . . . 106(2) ? C126 C121 H121 . . . 104(2) ? C121 C122 C123 . . . 111.2(3) ? C121 C122 H122a . . . 106(2) ? C121 C122 H122b . . . 103(3) ? C123 C122 H122a . . . 116(2) ? C123 C122 H122b . . . 109(3) ? H122a C122 H122b . . . 111(4) ? C122 C123 C124 . . . 110.2(3) ? C122 C123 H123a . . . 110.9(18) ? C122 C123 H123b . . . 106(3) ? C124 C123 H123a . . . 108(2) ? C124 C123 H123b . . . 114(2) ? H123a C123 H123b . . . 107(3) ? C123 C124 C125 . . . 110.2(3) ? C123 C124 H124a . . . 110(3) ? C123 C124 H124b . . . 105(3) ? C125 C124 H124a . . . 111(3) ? C125 C124 H124b . . . 106(3) ? H124a C124 H124b . . . 115(4) ? C124 C125 C126 . . . 112.9(4) ? C124 C125 H125a . . . 106(3) ? C124 C125 H125b . . . 112(3) ? C126 C125 H125a . . . 112(3) ? C126 C125 H125b . . . 114(3) ? H125a C125 H125b . . . 98(5) ? C121 C126 C125 . . . 111.6(3) ? C121 C126 H126a . . . 105(2) ? C121 C126 H126b . . . 105(3) ? C125 C126 H126a . . . 110(2) ? C125 C126 H126b . . . 109(3) ? H126a C126 H126b . . . 116(3) ? P C131 C132 . . . 111.2(2) ? P C131 C136 . . . 110.9(2) ? P C131 H131 . . . 108(2) ? C132 C131 C136 . . . 111.2(3) ? C132 C131 H131 . . . 108(2) ? C136 C131 H131 . . . 108(2) ? C131 C132 C133 . . . 112.6(3) ? C131 C132 H132a . . . 113(3) ? C131 C132 H132b . . . 110.3(18) ? C133 C132 H132a . . . 101(3) ? C133 C132 H132b . . . 109(2) ? H132a C132 H132b . . . 111(4) ? C132 C133 C134 . . . 110.6(3) ? C132 C133 H133a . . . 108(3) ? C132 C133 H133b . . . 110(3) ? C134 C133 H133a . . . 111(2) ? C134 C133 H133b . . . 109(3) ? H133a C133 H133b . . . 107(4) ? C133 C134 C135 . . . 110.0(4) ? C133 C134 H134a . . . 104(2) ? C133 C134 H134b . . . 113(3) ? C135 C134 H134a . . . 115(3) ? C135 C134 H134b . . . 106(2) ? H134a C134 H134b . . . 108(4) ? C134 C135 C136 . . . 111.4(3) ? C134 C135 H135a . . . 103(2) ? C134 C135 H135b . . . 110(4) ? C136 C135 H135a . . . 111(3) ? C136 C135 H135b . . . 98(4) ? H135a C135 H135b . . . 123(5) ? C131 C136 C135 . . . 112.5(3) ? C131 C136 H136a . . . 107(2) ? C131 C136 H136b . . . 109(2) ? C135 C136 H136a . . . 113(3) ? C135 C136 H136b . . . 108(2) ? H136a C136 H136b . . . 108(3) ? N12 N11 C15 . . . 108.2(2) ? N12 N11 B . . . 120.8(3) ? C15 N11 B . . . 131.0(3) ? Cu N12 N11 . . . 117.92(18) ? Cu N12 C13 . . . 136.0(2) ? N11 N12 C13 . . . 104.0(2) ? N12 C13 N14 . . . 113.4(3) ? N12 C13 H13 . . . 125(2) ? N14 C13 H13 . . . 121(2) ? C13 N14 C15 . . . 102.7(3) ? C13 N14 Cu . . '2 656' 128.2(2) ? C15 N14 Cu . . '2 656' 127.4(2) ? N11 C15 N14 . . . 111.7(3) ? N11 C15 H15 . . . 126(3) ? N14 C15 H15 . . . 122(3) ? N22 N21 C25 . . . 107.9(3) ? N22 N21 B . . . 121.4(3) ? C25 N21 B . . . 130.4(3) ? Cu N22 N21 . . . 119.2(2) ? Cu N22 C23 . . . 136.0(2) ? N21 N22 C23 . . . 103.3(2) ? N22 C23 N24 . . . 114.7(3) ? N22 C23 H23 . . . 120(2) ? N24 C23 H23 . . . 125(2) ? C23 N24 C25 . . . 101.9(3) ? N21 C25 N24 . . . 112.3(3) ? N21 C25 H25 . . . 126(3) ? N24 C25 H25 . . . 122(3) ? N11 B N21 . . . 105.8(3) ? N11 B H1a . . . 113.3(17) ? N11 B H1b . . . 110(3) ? N21 B H1a . . . 108(2) ? N21 B H1b . . . 106(3) ? H1a B H1b . . . 113(4) ? O01 C01 H01a . . . 110(5) ? O01 C01 H01b . . . 108(4) ? O01 C01 H01c . . . 118(5) ? H01a C01 H01b . . . 108(6) ? H01a C01 H01c . . . 98(6) ? H01b C01 H01c . . . 115(6) ? C01 O01 H01 . . . 104(3) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? _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 1120 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 18 _reflns_limit_k_min 0 _reflns_limit_k_max 13 _reflns_limit_l_min -26 _reflns_limit_l_max 25 _reflns_number_observed ? _reflns_d_resolution_high .735 _reflns_d_resolution_low 12.51 _diffrn_reflns_av_sigmaI/netI .046 _diffrn_reflns_theta_min 1.62 _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 .076 _refine_ls_wR_factor_all .089 _refine_ls_goodness_of_fit_all 1.653 _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 loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end