# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'David Vicic' 'Thomas J. Anderson' 'Gavin D. Jones' 'Chris McFarland' _publ_contact_author_name 'Prof David Vicic' _publ_contact_author_address ; Department of Chemistry and Biochemistry University of Arkansas Chemistry Building 101 Fayetteville Arkansas 72701 UNITED STATES OF AMERICA ; _publ_contact_author_email DVICIC@UARK.EDU _publ_requested_journal 'Chemical Communications' _publ_section_title ; Analysis of Key Steps in the Catalytic Cross-Coupling of Alkyl Electrophiles Under Negishi-like Conditions ; data_com3 _database_code_depnum_ccdc_archive 'CCDC 268664' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H50 Cl4 I N3 Ni' _chemical_formula_weight 864.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.78(2) _cell_length_b 17.04(2) _cell_length_c 19.13(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.82(2) _cell_angle_gamma 90.00 _cell_volume 4028(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 155 _cell_measurement_theta_min 1.6475 _cell_measurement_theta_max 34.9698 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1768 _exptl_absorpt_coefficient_mu 1.542 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5544 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38471 _diffrn_reflns_av_R_equivalents 0.0767 _diffrn_reflns_av_sigmaI/netI 0.0719 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 28.00 _reflns_number_total 9669 _reflns_number_gt 7651 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1282P)^2^+22.8085P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9669 _refine_ls_number_parameters 427 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1414 _refine_ls_R_factor_gt 0.1158 _refine_ls_wR_factor_ref 0.3030 _refine_ls_wR_factor_gt 0.2857 _refine_ls_goodness_of_fit_ref 1.205 _refine_ls_restrained_S_all 1.205 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.23491(5) 0.22706(3) 0.33998(3) 0.0410(2) Uani 1 1 d . . . Ni2 Ni 0.09477(8) -0.04555(6) 0.56222(6) 0.0310(3) Uani 1 1 d . . . Cl1 Cl 0.4350(3) 0.6717(4) 0.0346(2) 0.1060(15) Uani 1 1 d . . . Cl2 Cl 0.3514(5) 0.6731(9) 0.1560(4) 0.247(6) Uani 1 1 d . . . Cl3 Cl 0.3789(5) 0.4740(5) 0.2843(4) 0.168(3) Uani 1 1 d . . . Cl4 Cl 0.5408(11) 0.4409(7) 0.4179(6) 0.235(5) Uani 1 1 d . . . N1 N 0.0503(6) -0.0154(4) 0.6471(4) 0.0324(14) Uani 1 1 d . . . N2 N 0.1690(5) 0.0506(4) 0.5797(3) 0.0280(13) Uani 1 1 d . . . N3 N 0.1651(6) -0.0505(4) 0.4844(4) 0.0371(16) Uani 1 1 d . . . C1 C 0.0291(8) -0.1476(5) 0.5466(5) 0.042(2) Uani 1 1 d . . . H1A H 0.0044 -0.1578 0.4945 0.063 Uiso 1 1 calc R . . H1B H -0.0327 -0.1496 0.5680 0.063 Uiso 1 1 calc R . . H1C H 0.0823 -0.1875 0.5692 0.063 Uiso 1 1 calc R . . C2 C 0.1629(7) -0.1089(5) 0.4374(5) 0.0383(19) Uani 1 1 d . . . H2A H 0.1176 -0.1528 0.4387 0.046 Uiso 1 1 calc R . . C3 C 0.2227(7) -0.1086(5) 0.3873(5) 0.0393(19) Uani 1 1 d . . . H3A H 0.2167 -0.1513 0.3545 0.047 Uiso 1 1 calc R . . C4 C 0.2917(7) -0.0469(5) 0.3838(5) 0.0354(18) Uani 1 1 d . . . C5 C 0.2907(7) 0.0167(5) 0.4313(5) 0.0354(18) Uani 1 1 d . . . H5A H 0.3338 0.0618 0.4299 0.042 Uiso 1 1 calc R . . C6 C 0.2279(7) 0.0133(5) 0.4792(4) 0.0324(17) Uani 1 1 d . . . C7 C 0.2260(6) 0.0754(4) 0.5335(4) 0.0295(16) Uani 1 1 d . . . C8 C 0.2753(6) 0.1475(5) 0.5423(4) 0.0299(16) Uani 1 1 d . . . H8A H 0.3149 0.1647 0.5093 0.036 Uiso 1 1 calc R . . C9 C 0.2672(7) 0.1956(5) 0.6001(4) 0.0323(17) Uani 1 1 d . . . C10 C 0.2091(7) 0.1673(5) 0.6479(4) 0.0337(17) Uani 1 1 d . . . H10A H 0.2039 0.1976 0.6885 0.040 Uiso 1 1 calc R . . C11 C 0.1594(7) 0.0945(5) 0.6351(5) 0.0347(18) Uani 1 1 d . . . C12 C 0.0944(7) 0.0547(5) 0.6774(5) 0.0332(17) Uani 1 1 d . . . C13 C 0.0812(7) 0.0794(5) 0.7428(5) 0.0362(18) Uani 1 1 d . . . H13A H 0.1161 0.1263 0.7633 0.043 Uiso 1 1 calc R . . C14 C 0.0181(7) 0.0379(5) 0.7806(5) 0.0366(18) Uani 1 1 d . . . C15 C -0.0305(7) -0.0313(5) 0.7467(5) 0.040(2) Uani 1 1 d . . . H15A H -0.0749 -0.0621 0.7690 0.048 Uiso 1 1 calc R . . C16 C -0.0139(7) -0.0543(5) 0.6813(5) 0.0366(18) Uani 1 1 d . . . H16A H -0.0497 -0.1002 0.6590 0.044 Uiso 1 1 calc R . . C17 C 0.0106(9) 0.0621(5) 0.8555(5) 0.045(2) Uani 1 1 d . . . C18 C -0.0617(10) 0.0079(6) 0.8860(6) 0.058(3) Uani 1 1 d . . . H18A H -0.1351 0.0085 0.8541 0.087 Uiso 1 1 calc R . . H18B H -0.0636 0.0260 0.9343 0.087 Uiso 1 1 calc R . . H18C H -0.0329 -0.0457 0.8892 0.087 Uiso 1 1 calc R . . C19 C 0.1273(9) 0.0557(7) 0.9066(5) 0.055(3) Uani 1 1 d . . . H19A H 0.1554 0.0026 0.9037 0.083 Uiso 1 1 calc R . . H19B H 0.1249 0.0666 0.9565 0.083 Uiso 1 1 calc R . . H19C H 0.1747 0.0939 0.8917 0.083 Uiso 1 1 calc R . . C20 C -0.0303(10) 0.1466(6) 0.8529(6) 0.054(3) Uani 1 1 d . . . H20A H -0.0996 0.1509 0.8164 0.081 Uiso 1 1 calc R . . H20B H 0.0226 0.1818 0.8402 0.081 Uiso 1 1 calc R . . H20C H -0.0402 0.1612 0.9003 0.081 Uiso 1 1 calc R . . C21 C 0.3181(8) 0.2781(5) 0.6110(4) 0.0344(18) Uani 1 1 d . . . C22 C 0.3702(8) -0.0462(5) 0.3361(5) 0.040(2) Uani 1 1 d . . . C23 C 0.4856(10) -0.0489(11) 0.3822(7) 0.083(5) Uani 1 1 d . . . H23A H 0.5000 -0.0024 0.4134 0.124 Uiso 1 1 calc R . . H23B H 0.5354 -0.0497 0.3508 0.124 Uiso 1 1 calc R . . H23C H 0.4961 -0.0963 0.4121 0.124 Uiso 1 1 calc R . . C24 C 0.3543(14) -0.1171(8) 0.2847(10) 0.091(5) Uani 1 1 d . . . H24A H 0.2825 -0.1143 0.2508 0.137 Uiso 1 1 calc R . . H24B H 0.3604 -0.1657 0.3128 0.137 Uiso 1 1 calc R . . H24C H 0.4099 -0.1164 0.2576 0.137 Uiso 1 1 calc R . . C25 C 0.3538(11) 0.0270(7) 0.2875(6) 0.064(3) Uani 1 1 d . . . H25A H 0.2798 0.0274 0.2565 0.097 Uiso 1 1 calc R . . H25B H 0.4053 0.0261 0.2574 0.097 Uiso 1 1 calc R . . H25C H 0.3658 0.0742 0.3178 0.097 Uiso 1 1 calc R . . C26 C 0.2288(8) 0.3387(6) 0.6128(6) 0.048(2) Uani 1 1 d . . . H26A H 0.1700 0.3340 0.5686 0.072 Uiso 1 1 calc R . . H26B H 0.2593 0.3918 0.6160 0.072 Uiso 1 1 calc R . . H26C H 0.2006 0.3288 0.6550 0.072 Uiso 1 1 calc R . . C27 C 0.4025(8) 0.2784(6) 0.6849(6) 0.046(2) Uani 1 1 d . . . H27A H 0.4598 0.2405 0.6841 0.070 Uiso 1 1 calc R . . H27B H 0.3673 0.2640 0.7230 0.070 Uiso 1 1 calc R . . H27C H 0.4340 0.3310 0.6946 0.070 Uiso 1 1 calc R . . C28 C 0.3699(10) 0.3011(6) 0.5515(6) 0.054(3) Uani 1 1 d . . . H28A H 0.3160 0.2985 0.5048 0.081 Uiso 1 1 calc R . . H28B H 0.4295 0.2650 0.5512 0.081 Uiso 1 1 calc R . . H28C H 0.3980 0.3548 0.5598 0.081 Uiso 1 1 calc R . . C29 C 0.8291(17) 0.1944(9) 0.2202(10) 0.091(5) Uani 1 1 d . . . H29A H 0.8320 0.2029 0.2698 0.109 Uiso 1 1 calc R . . C30 C 0.7355(16) 0.1706(9) 0.1751(9) 0.085(4) Uani 1 1 d . . . H30A H 0.6751 0.1593 0.1937 0.102 Uiso 1 1 calc R . . C31 C 0.7270(12) 0.1627(7) 0.1052(9) 0.074(4) Uani 1 1 d . . . H31A H 0.6587 0.1490 0.0742 0.088 Uiso 1 1 calc R . . C32 C 0.8147(13) 0.1739(7) 0.0750(8) 0.074(4) Uani 1 1 d . . . C33 C 0.9140(12) 0.1968(7) 0.1244(10) 0.082(5) Uani 1 1 d . . . H33A H 0.9767 0.2052 0.1074 0.098 Uiso 1 1 calc R . . C34 C 0.9190(15) 0.2067(8) 0.1968(9) 0.084(5) Uani 1 1 d . . . H34A H 0.9848 0.2221 0.2298 0.101 Uiso 1 1 calc R . . C35 C 0.4486(13) 0.7088(11) 0.1213(9) 0.092(5) Uani 1 1 d . . . H35A H 0.5202 0.6942 0.1527 0.111 Uiso 1 1 calc R . . H35B H 0.4439 0.7668 0.1194 0.111 Uiso 1 1 calc R . . C37 C 0.417(2) 0.4419(15) 0.390(2) 0.194(17) Uani 1 1 d . . . H37A H 0.3858 0.4797 0.4184 0.233 Uiso 1 1 calc R . . H37B H 0.3874 0.3892 0.3952 0.233 Uiso 1 1 calc R . . C40 C 0.8007(19) 0.1619(12) -0.0029(11) 0.124(7) Uani 1 1 d . . . H40A H 0.7241 0.1529 -0.0263 0.186 Uiso 1 1 calc R . . H40B H 0.8430 0.1162 -0.0106 0.186 Uiso 1 1 calc R . . H40C H 0.8258 0.2086 -0.0238 0.186 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0475(4) 0.0410(3) 0.0362(3) 0.0070(2) 0.0137(2) 0.0081(3) Ni2 0.0317(5) 0.0300(5) 0.0300(5) -0.0014(4) 0.0055(4) -0.0034(4) Cl1 0.083(3) 0.175(5) 0.057(2) -0.017(2) 0.0125(18) -0.016(3) Cl2 0.092(4) 0.57(2) 0.094(4) -0.018(7) 0.046(3) -0.022(7) Cl3 0.097(4) 0.230(8) 0.179(7) -0.065(6) 0.042(4) -0.035(4) Cl4 0.230(11) 0.240(11) 0.210(10) 0.023(8) 0.011(8) 0.016(9) N1 0.033(3) 0.034(3) 0.030(3) 0.002(3) 0.006(3) -0.006(3) N2 0.027(3) 0.030(3) 0.026(3) 0.001(3) 0.005(3) -0.003(3) N3 0.039(4) 0.035(4) 0.031(4) 0.001(3) -0.002(3) 0.001(3) C1 0.040(5) 0.040(5) 0.044(5) -0.011(4) 0.008(4) -0.010(4) C2 0.038(5) 0.035(4) 0.039(5) -0.011(4) 0.006(4) -0.002(4) C3 0.042(5) 0.032(4) 0.043(5) -0.008(4) 0.010(4) 0.000(4) C4 0.036(4) 0.036(4) 0.032(4) -0.001(3) 0.006(3) 0.007(4) C5 0.040(4) 0.024(4) 0.038(4) -0.001(3) 0.001(4) 0.000(3) C6 0.031(4) 0.037(4) 0.029(4) -0.004(3) 0.007(3) 0.000(3) C7 0.033(4) 0.028(4) 0.026(4) 0.000(3) 0.005(3) 0.000(3) C8 0.028(4) 0.038(4) 0.021(3) 0.000(3) 0.002(3) -0.002(3) C9 0.039(4) 0.028(4) 0.028(4) 0.003(3) 0.005(3) 0.003(3) C10 0.038(4) 0.032(4) 0.030(4) -0.001(3) 0.007(3) -0.005(3) C11 0.035(4) 0.031(4) 0.036(4) -0.003(3) 0.005(3) 0.005(3) C12 0.032(4) 0.027(4) 0.037(4) 0.006(3) 0.004(3) -0.002(3) C13 0.038(4) 0.034(4) 0.036(4) 0.001(3) 0.007(4) -0.008(4) C14 0.041(5) 0.037(4) 0.034(4) 0.001(3) 0.012(4) -0.005(4) C15 0.040(5) 0.035(4) 0.048(5) -0.001(4) 0.020(4) -0.008(4) C16 0.036(4) 0.034(4) 0.040(5) -0.005(3) 0.009(4) -0.007(3) C17 0.073(7) 0.040(5) 0.028(4) 0.000(4) 0.023(4) -0.019(5) C18 0.084(8) 0.052(6) 0.047(6) 0.003(5) 0.033(6) -0.030(6) C19 0.067(7) 0.064(7) 0.033(5) -0.004(5) 0.008(5) -0.016(5) C20 0.074(7) 0.053(6) 0.048(6) 0.000(5) 0.039(5) -0.001(5) C21 0.051(5) 0.025(4) 0.029(4) -0.005(3) 0.012(4) -0.001(3) C22 0.044(5) 0.043(5) 0.039(5) 0.000(4) 0.021(4) 0.012(4) C23 0.051(7) 0.144(14) 0.062(8) 0.013(8) 0.029(6) 0.010(8) C24 0.115(12) 0.059(8) 0.125(13) -0.040(8) 0.078(11) -0.004(8) C25 0.084(8) 0.068(7) 0.051(6) 0.022(6) 0.034(6) 0.025(6) C26 0.043(5) 0.040(5) 0.063(6) 0.005(4) 0.016(5) 0.009(4) C27 0.045(5) 0.037(5) 0.054(6) -0.004(4) 0.008(4) -0.012(4) C28 0.080(8) 0.044(5) 0.045(6) -0.010(4) 0.029(5) -0.022(5) C29 0.117(14) 0.061(8) 0.094(12) 0.019(8) 0.026(11) 0.020(9) C30 0.108(13) 0.072(9) 0.082(11) 0.005(8) 0.035(10) 0.016(9) C31 0.073(9) 0.056(7) 0.097(11) 0.002(7) 0.031(8) 0.000(6) C32 0.101(11) 0.048(6) 0.083(9) 0.011(6) 0.043(8) 0.024(7) C33 0.067(9) 0.043(6) 0.140(15) 0.015(8) 0.035(9) 0.016(6) C34 0.103(12) 0.057(7) 0.072(10) 0.003(7) -0.018(9) 0.018(8) C35 0.069(9) 0.116(13) 0.087(11) -0.016(9) 0.011(8) -0.007(9) C37 0.16(2) 0.15(2) 0.35(4) 0.14(2) 0.19(3) 0.073(17) C40 0.17(2) 0.108(14) 0.125(17) 0.018(12) 0.090(15) 0.030(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni2 N2 1.880(7) . ? Ni2 C1 1.921(9) . ? Ni2 N1 1.923(8) . ? Ni2 N3 1.927(9) . ? Cl1 C35 1.741(17) . ? Cl2 C35 1.665(19) . ? Cl3 C37 2.03(3) . ? Cl4 C37 1.53(3) . ? N1 C16 1.346(11) . ? N1 C12 1.384(10) . ? N2 C11 1.328(11) . ? N2 C7 1.349(10) . ? N3 C2 1.336(11) . ? N3 C6 1.370(11) . ? C2 C3 1.370(13) . ? C3 C4 1.385(13) . ? C4 C5 1.416(12) . ? C4 C22 1.520(13) . ? C5 C6 1.364(13) . ? C6 C7 1.489(11) . ? C7 C8 1.371(11) . ? C8 C9 1.402(12) . ? C9 C10 1.401(12) . ? C9 C21 1.542(11) . ? C10 C11 1.387(12) . ? C11 C12 1.465(12) . ? C12 C13 1.370(13) . ? C13 C14 1.405(12) . ? C14 C15 1.410(12) . ? C14 C17 1.516(13) . ? C15 C16 1.379(13) . ? C17 C18 1.525(13) . ? C17 C20 1.529(15) . ? C17 C19 1.565(16) . ? C21 C28 1.508(13) . ? C21 C27 1.544(13) . ? C21 C26 1.546(13) . ? C22 C23 1.514(16) . ? C22 C25 1.537(14) . ? C22 C24 1.537(15) . ? C29 C30 1.35(2) . ? C29 C34 1.35(2) . ? C30 C31 1.32(2) . ? C31 C32 1.40(2) . ? C32 C33 1.43(2) . ? C32 C40 1.47(2) . ? C33 C34 1.38(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ni2 C1 175.8(4) . . ? N2 Ni2 N1 82.1(3) . . ? C1 Ni2 N1 99.3(4) . . ? N2 Ni2 N3 82.1(3) . . ? C1 Ni2 N3 96.4(4) . . ? N1 Ni2 N3 164.0(3) . . ? C16 N1 C12 117.1(7) . . ? C16 N1 Ni2 128.8(6) . . ? C12 N1 Ni2 114.0(6) . . ? C11 N2 C7 121.4(7) . . ? C11 N2 Ni2 119.2(6) . . ? C7 N2 Ni2 119.3(5) . . ? C2 N3 C6 116.9(8) . . ? C2 N3 Ni2 128.3(7) . . ? C6 N3 Ni2 114.8(6) . . ? N3 C2 C3 123.3(9) . . ? C2 C3 C4 120.8(8) . . ? C3 C4 C5 116.1(8) . . ? C3 C4 C22 124.1(8) . . ? C5 C4 C22 119.7(8) . . ? C6 C5 C4 120.1(8) . . ? C5 C6 N3 122.6(8) . . ? C5 C6 C7 123.8(8) . . ? N3 C6 C7 113.5(7) . . ? N2 C7 C8 120.7(7) . . ? N2 C7 C6 110.0(7) . . ? C8 C7 C6 129.3(8) . . ? C7 C8 C9 119.6(8) . . ? C10 C9 C8 118.2(8) . . ? C10 C9 C21 120.1(7) . . ? C8 C9 C21 121.7(7) . . ? C11 C10 C9 119.2(8) . . ? N2 C11 C10 120.8(8) . . ? N2 C11 C12 111.2(7) . . ? C10 C11 C12 128.0(8) . . ? C13 C12 N1 120.9(7) . . ? C13 C12 C11 125.6(7) . . ? N1 C12 C11 113.4(7) . . ? C12 C13 C14 122.5(8) . . ? C13 C14 C15 115.3(8) . . ? C13 C14 C17 122.2(8) . . ? C15 C14 C17 122.4(8) . . ? C16 C15 C14 120.2(8) . . ? N1 C16 C15 123.7(8) . . ? C14 C17 C18 112.8(8) . . ? C14 C17 C20 109.2(8) . . ? C18 C17 C20 110.3(9) . . ? C14 C17 C19 106.9(9) . . ? C18 C17 C19 107.1(9) . . ? C20 C17 C19 110.5(9) . . ? C28 C21 C9 112.8(7) . . ? C28 C21 C27 110.6(9) . . ? C9 C21 C27 107.4(7) . . ? C28 C21 C26 108.3(8) . . ? C9 C21 C26 108.9(8) . . ? C27 C21 C26 108.9(8) . . ? C23 C22 C4 110.2(8) . . ? C23 C22 C25 109.8(10) . . ? C4 C22 C25 111.1(8) . . ? C23 C22 C24 107.4(11) . . ? C4 C22 C24 112.3(9) . . ? C25 C22 C24 106.0(10) . . ? C30 C29 C34 121.7(18) . . ? C31 C30 C29 120.6(18) . . ? C30 C31 C32 122.5(16) . . ? C31 C32 C33 115.7(15) . . ? C31 C32 C40 119.8(17) . . ? C33 C32 C40 124.5(16) . . ? C34 C33 C32 120.2(15) . . ? C29 C34 C33 119.2(16) . . ? Cl2 C35 Cl1 110.1(10) . . ? Cl4 C37 Cl3 108.3(12) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.592 _refine_diff_density_min -1.109 _refine_diff_density_rms 0.180 #===END data_com1b _database_code_depnum_ccdc_archive 'CCDC 268665' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H38 N3 Ni' _chemical_formula_weight 475.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.890(10) _cell_length_b 10.947(17) _cell_length_c 20.178(19) _cell_angle_alpha 90.00 _cell_angle_beta 105.977(6) _cell_angle_gamma 90.00 _cell_volume 2525(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 173 _cell_measurement_theta_min 2.3490 _cell_measurement_theta_max 34.9698 _exptl_crystal_description prism _exptl_crystal_colour color _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.250 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1020 _exptl_absorpt_coefficient_mu 0.788 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7693 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12750 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0548 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 28.00 _reflns_number_total 5826 _reflns_number_gt 4631 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0601P)^2^+2.4443P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5826 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0775 _refine_ls_R_factor_gt 0.0597 _refine_ls_wR_factor_ref 0.1482 _refine_ls_wR_factor_gt 0.1377 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.42264(3) 0.87648(3) 0.113638(19) 0.02965(13) Uani 1 1 d . . . N1 N 0.3187(2) 0.9480(2) 0.03413(12) 0.0307(5) Uani 1 1 d . . . N2 N 0.5020(2) 1.0210(2) 0.11261(12) 0.0276(5) Uani 1 1 d . . . N3 N 0.5423(2) 0.8522(2) 0.19809(13) 0.0304(5) Uani 1 1 d . . . C1 C 0.3421(3) 0.7217(3) 0.1127(2) 0.0506(9) Uani 1 1 d . . . H1A H 0.2932 0.7049 0.0659 0.076 Uiso 1 1 calc R . . H1B H 0.2928 0.7260 0.1443 0.076 Uiso 1 1 calc R . . H1C H 0.3998 0.6561 0.1273 0.076 Uiso 1 1 calc R . . C2 C 0.2112(3) 0.9087(3) -0.00212(17) 0.0400(8) Uani 1 1 d . . . H2A H 0.1833 0.8339 0.0112 0.048 Uiso 1 1 calc R . . C3 C 0.1409(3) 0.9706(3) -0.05662(17) 0.0425(8) Uani 1 1 d . . . H3A H 0.0651 0.9398 -0.0785 0.051 Uiso 1 1 calc R . . C4 C 0.1785(2) 1.0789(3) -0.08102(15) 0.0306(6) Uani 1 1 d . . . C5 C 0.2881(2) 1.1203(3) -0.04481(14) 0.0275(6) Uani 1 1 d . . . H5A H 0.3185 1.1924 -0.0597 0.033 Uiso 1 1 calc R . . C6 C 0.3555(2) 1.0580(2) 0.01343(14) 0.0262(6) Uani 1 1 d . . . C7 C 0.0969(3) 1.1456(3) -0.14197(15) 0.0337(7) Uani 1 1 d . . . C8 C 0.0542(3) 1.0555(4) -0.20212(16) 0.0452(8) Uani 1 1 d . . . H8A H 0.1217 1.0181 -0.2132 0.068 Uiso 1 1 calc R . . H8B H 0.0069 1.0993 -0.2426 0.068 Uiso 1 1 calc R . . H8C H 0.0067 0.9917 -0.1890 0.068 Uiso 1 1 calc R . . C9 C -0.0107(3) 1.1919(4) -0.12066(18) 0.0486(9) Uani 1 1 d . . . H9A H 0.0146 1.2503 -0.0827 0.073 Uiso 1 1 calc R . . H9B H -0.0499 1.1226 -0.1057 0.073 Uiso 1 1 calc R . . H9C H -0.0650 1.2321 -0.1601 0.073 Uiso 1 1 calc R . . C10 C 0.1562(3) 1.2533(3) -0.16589(17) 0.0435(8) Uani 1 1 d . . . H10A H 0.2261 1.2249 -0.1781 0.065 Uiso 1 1 calc R . . H10B H 0.1787 1.3136 -0.1287 0.065 Uiso 1 1 calc R . . H10C H 0.1019 1.2908 -0.2063 0.065 Uiso 1 1 calc R . . C11 C 0.4628(2) 1.1024(2) 0.06057(14) 0.0260(6) Uani 1 1 d . . . C12 C 0.5176(2) 1.2150(2) 0.06223(14) 0.0267(6) Uani 1 1 d . . . H12A H 0.4914 1.2703 0.0249 0.032 Uiso 1 1 calc R . . C13 C 0.6107(2) 1.2471(3) 0.11833(14) 0.0278(6) Uani 1 1 d . . . C14 C 0.6494(2) 1.1598(3) 0.17130(15) 0.0288(6) Uani 1 1 d . . . H14A H 0.7137 1.1780 0.2099 0.035 Uiso 1 1 calc R . . C15 C 0.5941(2) 1.0483(3) 0.16716(15) 0.0278(6) Uani 1 1 d . . . C16 C 0.6681(3) 1.3736(3) 0.12687(15) 0.0309(6) Uani 1 1 d . . . C17 C 0.6652(5) 1.4291(4) 0.1953(2) 0.0746(14) Uani 1 1 d . . . H17A H 0.5839 1.4354 0.1972 0.112 Uiso 1 1 calc R . . H17B H 0.7005 1.5106 0.1999 0.112 Uiso 1 1 calc R . . H17C H 0.7093 1.3770 0.2331 0.112 Uiso 1 1 calc R . . C18 C 0.7966(3) 1.3608(4) 0.1265(3) 0.0687(13) Uani 1 1 d . . . H18A H 0.8353 1.4404 0.1357 0.103 Uiso 1 1 calc R . . H18B H 0.8002 1.3312 0.0813 0.103 Uiso 1 1 calc R . . H18C H 0.8362 1.3025 0.1621 0.103 Uiso 1 1 calc R . . C19 C 0.6095(4) 1.4591(4) 0.0695(2) 0.0728(14) Uani 1 1 d . . . H19A H 0.5276 1.4704 0.0691 0.109 Uiso 1 1 calc R . . H19B H 0.6131 1.4245 0.0253 0.109 Uiso 1 1 calc R . . H19C H 0.6497 1.5382 0.0766 0.109 Uiso 1 1 calc R . . C20 C 0.6173(2) 0.9498(3) 0.21752(15) 0.0294(6) Uani 1 1 d . . . C21 C 0.7057(2) 0.9515(3) 0.27957(15) 0.0306(6) Uani 1 1 d . . . H21A H 0.7541 1.0217 0.2914 0.037 Uiso 1 1 calc R . . C22 C 0.7241(3) 0.8529(3) 0.32417(15) 0.0333(7) Uani 1 1 d . . . C23 C 0.6476(3) 0.7543(3) 0.30347(17) 0.0381(7) Uani 1 1 d . . . H23A H 0.6562 0.6840 0.3321 0.046 Uiso 1 1 calc R . . C24 C 0.5602(3) 0.7573(3) 0.24247(16) 0.0357(7) Uani 1 1 d . . . H24A H 0.5096 0.6887 0.2309 0.043 Uiso 1 1 calc R . . C25 C 0.8204(3) 0.8535(3) 0.39244(16) 0.0378(7) Uani 1 1 d . . . C26 C 0.7635(3) 0.8805(3) 0.45025(17) 0.0418(8) Uani 1 1 d . . . H26A H 0.7048 0.8178 0.4505 0.063 Uiso 1 1 calc R . . H26B H 0.7257 0.9608 0.4426 0.063 Uiso 1 1 calc R . . H26C H 0.8235 0.8802 0.4947 0.063 Uiso 1 1 calc R . . C27 C 0.9117(3) 0.9529(5) 0.39480(19) 0.0617(12) Uani 1 1 d . . . H27A H 0.9724 0.9486 0.4388 0.093 Uiso 1 1 calc R . . H27B H 0.8739 1.0333 0.3902 0.093 Uiso 1 1 calc R . . H27C H 0.9472 0.9407 0.3569 0.093 Uiso 1 1 calc R . . C28 C 0.8803(4) 0.7299(4) 0.4047(2) 0.0741(15) Uani 1 1 d . . . H28A H 0.8232 0.6670 0.4075 0.111 Uiso 1 1 calc R . . H28B H 0.9430 0.7318 0.4480 0.111 Uiso 1 1 calc R . . H28C H 0.9136 0.7110 0.3665 0.111 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0281(2) 0.01898(19) 0.0398(2) -0.00138(15) 0.00578(16) -0.00187(15) N1 0.0284(13) 0.0250(12) 0.0368(14) -0.0045(10) 0.0055(10) -0.0051(10) N2 0.0232(12) 0.0232(12) 0.0343(13) -0.0014(9) 0.0045(10) -0.0005(9) N3 0.0294(13) 0.0227(12) 0.0392(14) 0.0005(10) 0.0092(10) 0.0031(10) C1 0.052(2) 0.0304(17) 0.060(2) 0.0050(15) -0.0015(17) -0.0038(15) C2 0.0352(17) 0.0299(16) 0.050(2) -0.0008(13) 0.0031(14) -0.0119(13) C3 0.0316(17) 0.0413(19) 0.0464(19) -0.0063(14) -0.0031(14) -0.0156(14) C4 0.0263(14) 0.0340(15) 0.0289(15) -0.0079(12) 0.0035(11) -0.0023(12) C5 0.0249(13) 0.0295(14) 0.0282(15) -0.0050(11) 0.0077(11) -0.0026(11) C6 0.0212(13) 0.0247(13) 0.0320(15) -0.0061(11) 0.0063(11) -0.0043(10) C7 0.0273(15) 0.0413(18) 0.0299(16) -0.0079(12) 0.0037(12) -0.0012(12) C8 0.0403(19) 0.061(2) 0.0311(17) -0.0114(15) 0.0040(14) -0.0111(17) C9 0.0345(18) 0.063(2) 0.046(2) -0.0031(17) 0.0065(15) 0.0131(17) C10 0.0420(19) 0.0443(19) 0.0361(18) 0.0041(14) -0.0026(14) -0.0027(15) C11 0.0194(12) 0.0250(14) 0.0329(15) -0.0025(11) 0.0061(11) 0.0006(10) C12 0.0231(13) 0.0250(13) 0.0305(15) 0.0026(11) 0.0048(11) -0.0017(11) C13 0.0205(13) 0.0264(14) 0.0352(15) 0.0020(11) 0.0056(11) -0.0022(11) C14 0.0193(13) 0.0269(14) 0.0353(16) -0.0010(11) -0.0010(11) -0.0023(10) C15 0.0206(13) 0.0240(14) 0.0363(16) 0.0012(11) 0.0034(11) 0.0034(10) C16 0.0270(14) 0.0261(14) 0.0369(16) 0.0026(12) 0.0041(12) -0.0064(12) C17 0.120(4) 0.039(2) 0.073(3) -0.011(2) 0.039(3) -0.026(3) C18 0.040(2) 0.058(3) 0.105(4) -0.004(2) 0.016(2) -0.0172(19) C19 0.068(3) 0.049(2) 0.083(3) 0.023(2) -0.011(2) -0.028(2) C20 0.0247(14) 0.0229(13) 0.0399(17) -0.0004(11) 0.0079(12) 0.0025(11) C21 0.0266(14) 0.0271(14) 0.0370(16) 0.0018(11) 0.0069(12) 0.0078(11) C22 0.0316(15) 0.0356(17) 0.0355(16) 0.0062(12) 0.0139(13) 0.0110(12) C23 0.0389(17) 0.0339(16) 0.0446(18) 0.0119(13) 0.0165(14) 0.0103(13) C24 0.0395(17) 0.0226(14) 0.0477(18) 0.0069(12) 0.0168(14) 0.0027(12) C25 0.0330(16) 0.0466(19) 0.0337(17) 0.0111(13) 0.0092(13) 0.0168(14) C26 0.0468(19) 0.0428(19) 0.0379(18) 0.0079(14) 0.0154(15) 0.0086(15) C27 0.0322(19) 0.107(4) 0.040(2) 0.020(2) 0.0000(15) -0.009(2) C28 0.079(3) 0.078(3) 0.052(2) -0.001(2) -0.005(2) 0.056(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N2 1.845(3) . ? Ni1 N1 1.903(3) . ? Ni1 N3 1.914(3) . ? Ni1 C1 1.944(4) . ? N1 C2 1.356(4) . ? N1 C6 1.385(4) . ? N2 C15 1.355(4) . ? N2 C11 1.358(4) . ? N3 C24 1.350(4) . ? N3 C20 1.377(4) . ? C2 C3 1.364(5) . ? C3 C4 1.403(5) . ? C4 C5 1.384(4) . ? C4 C7 1.526(4) . ? C5 C6 1.403(4) . ? C6 C11 1.450(4) . ? C7 C10 1.518(5) . ? C7 C8 1.537(4) . ? C7 C9 1.544(5) . ? C11 C12 1.390(4) . ? C12 C13 1.393(4) . ? C13 C14 1.413(4) . ? C13 C16 1.533(4) . ? C14 C15 1.378(4) . ? C15 C20 1.455(4) . ? C16 C19 1.503(5) . ? C16 C17 1.518(5) . ? C16 C18 1.536(5) . ? C20 C21 1.396(4) . ? C21 C22 1.384(4) . ? C22 C23 1.399(5) . ? C22 C25 1.530(4) . ? C23 C24 1.375(5) . ? C25 C28 1.518(5) . ? C25 C27 1.529(5) . ? C25 C26 1.530(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ni1 N1 81.58(12) . . ? N2 Ni1 N3 82.62(11) . . ? N1 Ni1 N3 163.44(10) . . ? N2 Ni1 C1 177.99(15) . . ? N1 Ni1 C1 98.42(14) . . ? N3 Ni1 C1 97.55(13) . . ? C2 N1 C6 116.2(3) . . ? C2 N1 Ni1 128.4(2) . . ? C6 N1 Ni1 115.23(19) . . ? C15 N2 C11 120.8(2) . . ? C15 N2 Ni1 118.78(19) . . ? C11 N2 Ni1 120.2(2) . . ? C24 N3 C20 115.9(3) . . ? C24 N3 Ni1 129.8(2) . . ? C20 N3 Ni1 114.22(19) . . ? N1 C2 C3 123.7(3) . . ? C2 C3 C4 121.3(3) . . ? C5 C4 C3 115.8(3) . . ? C5 C4 C7 124.5(3) . . ? C3 C4 C7 119.6(3) . . ? C4 C5 C6 121.4(3) . . ? N1 C6 C5 121.4(2) . . ? N1 C6 C11 112.8(2) . . ? C5 C6 C11 125.7(3) . . ? C10 C7 C4 112.4(3) . . ? C10 C7 C8 109.2(3) . . ? C4 C7 C8 109.2(3) . . ? C10 C7 C9 109.0(3) . . ? C4 C7 C9 108.9(3) . . ? C8 C7 C9 108.1(3) . . ? N2 C11 C12 120.3(3) . . ? N2 C11 C6 109.9(2) . . ? C12 C11 C6 129.4(3) . . ? C11 C12 C13 120.3(3) . . ? C12 C13 C14 117.7(3) . . ? C12 C13 C16 123.3(2) . . ? C14 C13 C16 118.9(2) . . ? C15 C14 C13 120.2(3) . . ? N2 C15 C14 120.7(3) . . ? N2 C15 C20 111.0(3) . . ? C14 C15 C20 128.2(3) . . ? C19 C16 C17 109.3(3) . . ? C19 C16 C13 112.2(3) . . ? C17 C16 C13 110.1(3) . . ? C19 C16 C18 107.7(3) . . ? C17 C16 C18 108.2(3) . . ? C13 C16 C18 109.2(3) . . ? N3 C20 C21 122.3(3) . . ? N3 C20 C15 113.1(3) . . ? C21 C20 C15 124.6(3) . . ? C22 C21 C20 121.2(3) . . ? C21 C22 C23 115.7(3) . . ? C21 C22 C25 121.8(3) . . ? C23 C22 C25 122.4(3) . . ? C24 C23 C22 121.2(3) . . ? N3 C24 C23 123.6(3) . . ? C28 C25 C27 109.4(3) . . ? C28 C25 C22 110.1(3) . . ? C27 C25 C22 112.3(3) . . ? C28 C25 C26 109.6(3) . . ? C27 C25 C26 107.3(3) . . ? C22 C25 C26 108.0(3) . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 1.030 _refine_diff_density_min -0.464 _refine_diff_density_rms 0.073 #===END