Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global #============================================================================== _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'Sladek, Marianna I.' ; Fakultat f. Chemie Universitat Bielefeld 33615 Bielefeld Germany ; 'Braun, Thomas' ; Fakultat f. Chemie Universitat Bielefeld 33615 Bielefeld Germany ; 'Neumann, Beate' ; Fakultat f. Chemie Universitat Bielefeld 33615 Bielefeld Germany ; 'Stammler, Hans-Georg' ; Fakultat f. Chemie Universitat Bielefeld 33615 Bielefeld Germany ; _publ_requested_journal 'Dalton Transactions' # 1. SUBMISSION DETAILS _publ_contact_author_name 'Dr Thomas Braun' _publ_contact_author_address ; Fakultät für Chemie, ACIII Universität Bielefeld Postfach 100131 D -33501 Bielefeld Bielefeld D-33501 GERMANY ; _publ_contact_author_phone '49 521 1066165' _publ_contact_author_fax '49 521 1066146' _publ_contact_author_email THOMAS.BRAUN@UNI-BIELEFELD.DE _publ_requested_coeditor_name ? #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Aromatic C-F Activation at Ni in the Presence of a Carbon Chlorine Bond: The Nickel Mediated Synthesis of new Pyrimidines ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. #========================================================================= data_compound1 _database_code_CSD 173740 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H30 Cl F2 N2 Ni2 P2' _chemical_formula_sum 'C16 H30 Cl F3 N2 Ni P2' _chemical_formula_weight 463.52 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.87000(10) _cell_length_b 13.36900(10) _cell_length_c 14.1440(2) _cell_angle_alpha 97.9150(5) _cell_angle_beta 96.7310(5) _cell_angle_gamma 90.4950(4) _cell_volume 2207.11(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 14313 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 42.106 _exptl_crystal_description rhomb _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.395 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 1.172 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7504 _exptl_absorpt_correction_T_max 0.8532 _exptl_absorpt_process_details ? _exptl_special_details ; ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 89302 _diffrn_reflns_av_R_equivalents 0.033 _diffrn_reflns_av_sigmaI/netI 0.0285 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 30.00 _reflns_number_total 12851 _reflns_number_gt 10758 _reflns_threshold_expression >2sigma(I) _computing_data_collection KappaCCD _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0314P)^2^+0.7719P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12851 _refine_ls_number_parameters 463 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0395 _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.0710 _refine_ls_wR_factor_gt 0.0670 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.001 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.086705(14) 0.276716(12) 0.261849(12) 0.01481(4) Uani 1 1 d . . . Cl1 Cl 0.14047(3) 0.13710(3) 0.31801(3) 0.02289(7) Uani 1 1 d . . . P1 P -0.07894(3) 0.25417(3) 0.31452(3) 0.01988(7) Uani 1 1 d . . . P2 P 0.25592(3) 0.29037(3) 0.21268(2) 0.01618(7) Uani 1 1 d . . . F1 F -0.06328(8) 0.30509(7) 0.07166(7) 0.0305(2) Uani 1 1 d . . . F2 F -0.07105(9) 0.64200(8) 0.09780(9) 0.0430(3) Uani 1 1 d . . . F3 F 0.12653(8) 0.50950(7) 0.33782(7) 0.0298(2) Uani 1 1 d . . . N1 N -0.06845(11) 0.47321(10) 0.08312(10) 0.0268(3) Uani 1 1 d . . . N2 N 0.02616(11) 0.57703(9) 0.21953(10) 0.0266(3) Uani 1 1 d . . . C1 C 0.03784(11) 0.39410(10) 0.21070(10) 0.0170(2) Uani 1 1 d . . . C2 C -0.02955(12) 0.39472(11) 0.12373(10) 0.0208(3) Uani 1 1 d . . . C3 C -0.03574(13) 0.55924(12) 0.13571(13) 0.0281(3) Uani 1 1 d . . . C4 C 0.06085(11) 0.49281(11) 0.25275(11) 0.0206(3) Uani 1 1 d . . . C5 C -0.14233(13) 0.12848(12) 0.27248(13) 0.0311(4) Uani 1 1 d . . . H5A H -0.1032 0.0792 0.3103 0.037 Uiso 1 1 calc R . . H5B H -0.2230 0.1287 0.2840 0.037 Uiso 1 1 calc R . . C6 C -0.13504(15) 0.09464(14) 0.16568(14) 0.0378(4) Uani 1 1 d . . . H6A H -0.1744 0.1427 0.1278 0.057 Uiso 1 1 calc R . . H6B H -0.1708 0.0274 0.1466 0.057 Uiso 1 1 calc R . . H6C H -0.0552 0.0921 0.1542 0.057 Uiso 1 1 calc R . . C7 C -0.06059(15) 0.26009(13) 0.44521(12) 0.0323(4) Uani 1 1 d . . . H7A H -0.1358 0.2527 0.4676 0.039 Uiso 1 1 calc R . . H7B H -0.0140 0.2029 0.4630 0.039 Uiso 1 1 calc R . . C8 C -0.00378(19) 0.35864(15) 0.49563(13) 0.0447(5) Uani 1 1 d . . . H8A H 0.0701 0.3670 0.4727 0.067 Uiso 1 1 calc R . . H8B H 0.0070 0.3572 0.5652 0.067 Uiso 1 1 calc R . . H8C H -0.0518 0.4152 0.4815 0.067 Uiso 1 1 calc R . . C9 C -0.19276(12) 0.34211(12) 0.28812(13) 0.0286(3) Uani 1 1 d . . . H9A H -0.1613 0.4118 0.3065 0.034 Uiso 1 1 calc R . . H9B H -0.2150 0.3325 0.2177 0.034 Uiso 1 1 calc R . . C10 C -0.30003(15) 0.33346(15) 0.33701(17) 0.0456(5) Uani 1 1 d . . . H10A H -0.3336 0.2653 0.3187 0.068 Uiso 1 1 calc R . . H10B H -0.3547 0.3831 0.3167 0.068 Uiso 1 1 calc R . . H10C H -0.2805 0.3464 0.4069 0.068 Uiso 1 1 calc R . . C11 C 0.37393(12) 0.28725(11) 0.30783(11) 0.0230(3) Uani 1 1 d . . . H11A H 0.3645 0.2267 0.3396 0.028 Uiso 1 1 calc R . . H11B H 0.4457 0.2809 0.2785 0.028 Uiso 1 1 calc R . . C12 C 0.38278(15) 0.38043(12) 0.38348(12) 0.0307(3) Uani 1 1 d . . . H12A H 0.3980 0.4403 0.3535 0.046 Uiso 1 1 calc R . . H12B H 0.4448 0.3727 0.4340 0.046 Uiso 1 1 calc R . . H12C H 0.3113 0.3884 0.4117 0.046 Uiso 1 1 calc R . . C13 C 0.27628(12) 0.18147(10) 0.12371(10) 0.0207(3) Uani 1 1 d . . . H13A H 0.3519 0.1877 0.1018 0.025 Uiso 1 1 calc R . . H13B H 0.2749 0.1193 0.1544 0.025 Uiso 1 1 calc R . . C14 C 0.18568(13) 0.17153(12) 0.03669(11) 0.0282(3) Uani 1 1 d . . . H14A H 0.1105 0.1663 0.0580 0.042 Uiso 1 1 calc R . . H14B H 0.1987 0.1108 -0.0076 0.042 Uiso 1 1 calc R . . H14C H 0.1897 0.2311 0.0038 0.042 Uiso 1 1 calc R . . C15 C 0.28808(12) 0.40089(11) 0.15565(11) 0.0214(3) Uani 1 1 d . . . H15A H 0.2298 0.4039 0.1001 0.026 Uiso 1 1 calc R . . H15B H 0.2815 0.4624 0.2022 0.026 Uiso 1 1 calc R . . C16 C 0.40510(13) 0.40324(12) 0.12066(12) 0.0277(3) Uani 1 1 d . . . H16A H 0.4640 0.4040 0.1754 0.041 Uiso 1 1 calc R . . H16B H 0.4135 0.4640 0.0903 0.041 Uiso 1 1 calc R . . H16C H 0.4128 0.3432 0.0738 0.041 Uiso 1 1 calc R . . Ni2 Ni 0.485443(14) -0.220283(12) 0.257962(12) 0.01465(4) Uani 1 1 d . . . Cl2 Cl 0.44650(3) -0.35434(3) 0.32363(3) 0.02722(8) Uani 1 1 d . . . P3 P 0.30273(3) -0.21180(3) 0.20687(2) 0.01578(7) Uani 1 1 d . . . P4 P 0.66666(3) -0.23734(3) 0.31079(2) 0.01640(7) Uani 1 1 d . . . N3 N 0.59462(10) -0.03127(10) 0.07295(9) 0.0240(3) Uani 1 1 d . . . N4 N 0.53705(10) 0.07758(9) 0.20510(9) 0.0231(3) Uani 1 1 d . . . F4 F 0.58419(8) -0.19846(7) 0.06725(6) 0.02653(19) Uani 1 1 d . . . F5 F 0.60261(8) 0.13695(7) 0.08122(8) 0.0353(2) Uani 1 1 d . . . F6 F 0.46822(8) 0.01468(7) 0.32577(6) 0.02813(19) Uani 1 1 d . . . C17 C 0.52036(11) -0.10492(10) 0.20276(10) 0.0171(2) Uani 1 1 d . . . C18 C 0.56529(11) -0.10775(11) 0.11596(10) 0.0193(3) Uani 1 1 d . . . C19 C 0.57639(12) 0.05640(11) 0.12210(12) 0.0248(3) Uani 1 1 d . . . C20 C 0.51012(11) -0.00518(11) 0.24137(10) 0.0196(3) Uani 1 1 d . . . C21 C 0.25782(12) -0.32252(10) 0.11963(10) 0.0206(3) Uani 1 1 d . . . H21A H 0.2672 -0.3837 0.1518 0.025 Uiso 1 1 calc R . . H21B H 0.1762 -0.3175 0.0971 0.025 Uiso 1 1 calc R . . C22 C 0.32400(13) -0.33459(12) 0.03280(11) 0.0275(3) Uani 1 1 d . . . H22A H 0.3114 -0.2763 -0.0019 0.041 Uiso 1 1 calc R . . H22B H 0.2980 -0.3965 -0.0100 0.041 Uiso 1 1 calc R . . H22C H 0.4051 -0.3387 0.0545 0.041 Uiso 1 1 calc R . . C23 C 0.21066(12) -0.21612(11) 0.30066(11) 0.0225(3) Uani 1 1 d . . . H23A H 0.1305 -0.2178 0.2717 0.027 Uiso 1 1 calc R . . H23B H 0.2241 -0.2789 0.3296 0.027 Uiso 1 1 calc R . . C24 C 0.23128(15) -0.12481(12) 0.37980(12) 0.0309(3) Uani 1 1 d . . . H24A H 0.3105 -0.1230 0.4088 0.046 Uiso 1 1 calc R . . H24B H 0.1812 -0.1306 0.4292 0.046 Uiso 1 1 calc R . . H24C H 0.2153 -0.0626 0.3518 0.046 Uiso 1 1 calc R . . C25 C 0.25458(12) -0.10313(11) 0.14805(11) 0.0205(3) Uani 1 1 d . . . H25A H 0.2764 -0.0408 0.1932 0.025 Uiso 1 1 calc R . . H25B H 0.2959 -0.1015 0.0914 0.025 Uiso 1 1 calc R . . C26 C 0.12723(12) -0.10077(12) 0.11486(12) 0.0266(3) Uani 1 1 d . . . H26A H 0.1034 -0.1632 0.0720 0.040 Uiso 1 1 calc R . . H26B H 0.1116 -0.0427 0.0804 0.040 Uiso 1 1 calc R . . H26C H 0.0852 -0.0949 0.1709 0.040 Uiso 1 1 calc R . . C27 C 0.68682(13) -0.21067(12) 0.44152(10) 0.0243(3) Uani 1 1 d . . . H27A H 0.6402 -0.2592 0.4682 0.029 Uiso 1 1 calc R . . H27B H 0.7674 -0.2202 0.4650 0.029 Uiso 1 1 calc R . . C28 C 0.65391(16) -0.10311(14) 0.47750(12) 0.0357(4) Uani 1 1 d . . . H28A H 0.7008 -0.0548 0.4520 0.054 Uiso 1 1 calc R . . H28B H 0.6661 -0.0916 0.5479 0.054 Uiso 1 1 calc R . . H28C H 0.5737 -0.0939 0.4556 0.054 Uiso 1 1 calc R . . C29 C 0.71675(13) -0.36618(11) 0.28297(12) 0.0256(3) Uani 1 1 d . . . H29A H 0.8004 -0.3657 0.2972 0.031 Uiso 1 1 calc R . . H29B H 0.6848 -0.4098 0.3249 0.031 Uiso 1 1 calc R . . C30 C 0.68311(14) -0.41058(13) 0.17803(13) 0.0330(4) Uani 1 1 d . . . H30A H 0.6002 -0.4146 0.1644 0.050 Uiso 1 1 calc R . . H30B H 0.7137 -0.4784 0.1661 0.050 Uiso 1 1 calc R . . H30C H 0.7138 -0.3672 0.1362 0.050 Uiso 1 1 calc R . . C31 C 0.77384(12) -0.15704(11) 0.27155(11) 0.0219(3) Uani 1 1 d . . . H31A H 0.7759 -0.1771 0.2018 0.026 Uiso 1 1 calc R . . H31B H 0.7485 -0.0864 0.2807 0.026 Uiso 1 1 calc R . . C32 C 0.89475(13) -0.15954(13) 0.32193(14) 0.0334(4) Uani 1 1 d . . . H32A H 0.8954 -0.1361 0.3908 0.050 Uiso 1 1 calc R . . H32B H 0.9445 -0.1153 0.2944 0.050 Uiso 1 1 calc R . . H32C H 0.9219 -0.2288 0.3129 0.050 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 0.01401(8) 0.01287(8) 0.01779(8) 0.00355(6) 0.00127(6) -0.00002(6) Cl1 0.02099(16) 0.01950(16) 0.02973(18) 0.01008(13) 0.00153(13) 0.00166(12) P1 0.01688(16) 0.01738(17) 0.02652(18) 0.00532(14) 0.00484(13) -0.00071(13) P2 0.01489(15) 0.01392(15) 0.02024(16) 0.00409(13) 0.00215(12) 0.00066(12) F1 0.0339(5) 0.0259(5) 0.0278(5) 0.0001(4) -0.0090(4) 0.0013(4) F2 0.0347(5) 0.0306(5) 0.0715(8) 0.0328(5) 0.0082(5) 0.0097(4) F3 0.0322(5) 0.0222(4) 0.0313(5) -0.0045(4) -0.0013(4) -0.0011(4) N1 0.0218(6) 0.0295(7) 0.0321(7) 0.0154(6) 0.0028(5) 0.0048(5) N2 0.0219(6) 0.0157(6) 0.0442(8) 0.0071(5) 0.0096(5) 0.0017(5) C1 0.0146(6) 0.0157(6) 0.0217(6) 0.0043(5) 0.0047(5) 0.0005(5) C2 0.0187(6) 0.0205(7) 0.0238(7) 0.0052(5) 0.0020(5) 0.0015(5) C3 0.0208(7) 0.0238(8) 0.0456(9) 0.0196(7) 0.0103(6) 0.0065(6) C4 0.0167(6) 0.0180(6) 0.0279(7) 0.0035(5) 0.0062(5) 0.0005(5) C5 0.0219(7) 0.0198(7) 0.0521(10) 0.0062(7) 0.0051(7) -0.0044(6) C6 0.0274(8) 0.0303(9) 0.0507(11) -0.0069(8) -0.0011(7) -0.0076(7) C7 0.0354(9) 0.0355(9) 0.0305(8) 0.0114(7) 0.0144(7) 0.0078(7) C8 0.0667(13) 0.0387(10) 0.0268(9) -0.0029(7) 0.0053(8) 0.0117(9) C9 0.0181(7) 0.0280(8) 0.0419(9) 0.0096(7) 0.0071(6) 0.0043(6) C10 0.0232(8) 0.0421(11) 0.0777(15) 0.0190(10) 0.0185(9) 0.0069(7) C11 0.0174(6) 0.0243(7) 0.0275(7) 0.0075(6) -0.0013(5) -0.0016(5) C12 0.0354(9) 0.0276(8) 0.0279(8) 0.0062(6) -0.0037(6) -0.0068(7) C13 0.0217(7) 0.0168(6) 0.0245(7) 0.0037(5) 0.0053(5) 0.0037(5) C14 0.0277(8) 0.0289(8) 0.0258(7) -0.0034(6) 0.0018(6) 0.0035(6) C15 0.0215(7) 0.0172(6) 0.0275(7) 0.0066(5) 0.0066(5) 0.0010(5) C16 0.0255(7) 0.0240(7) 0.0361(8) 0.0076(6) 0.0110(6) -0.0015(6) Ni2 0.01495(8) 0.01252(8) 0.01693(8) 0.00366(6) 0.00204(6) -0.00045(6) Cl2 0.02481(17) 0.02219(17) 0.0373(2) 0.01506(15) 0.00226(14) -0.00195(13) P3 0.01513(15) 0.01306(15) 0.01953(16) 0.00328(12) 0.00257(12) -0.00096(12) P4 0.01680(15) 0.01478(16) 0.01751(16) 0.00291(12) 0.00073(12) 0.00101(12) N3 0.0210(6) 0.0283(7) 0.0251(6) 0.0117(5) 0.0033(5) 0.0001(5) N4 0.0187(6) 0.0178(6) 0.0338(7) 0.0088(5) 0.0008(5) 0.0007(4) F4 0.0319(5) 0.0274(5) 0.0204(4) -0.0010(3) 0.0091(3) -0.0008(4) F5 0.0333(5) 0.0301(5) 0.0476(6) 0.0228(4) 0.0057(4) -0.0029(4) F6 0.0366(5) 0.0210(4) 0.0277(5) -0.0002(3) 0.0120(4) 0.0015(4) C17 0.0128(6) 0.0177(6) 0.0206(6) 0.0043(5) 0.0000(5) 0.0000(5) C18 0.0156(6) 0.0217(7) 0.0212(6) 0.0062(5) 0.0011(5) 0.0003(5) C19 0.0169(6) 0.0232(7) 0.0358(8) 0.0135(6) -0.0011(6) -0.0018(5) C20 0.0171(6) 0.0195(7) 0.0224(7) 0.0035(5) 0.0023(5) 0.0002(5) C21 0.0207(6) 0.0154(6) 0.0249(7) 0.0023(5) 0.0001(5) -0.0035(5) C22 0.0300(8) 0.0253(8) 0.0256(7) -0.0031(6) 0.0050(6) -0.0044(6) C23 0.0203(7) 0.0180(7) 0.0314(8) 0.0064(6) 0.0089(6) -0.0009(5) C24 0.0410(9) 0.0245(8) 0.0299(8) 0.0028(6) 0.0162(7) -0.0006(7) C25 0.0191(6) 0.0173(6) 0.0257(7) 0.0066(5) 0.0010(5) 0.0007(5) C26 0.0212(7) 0.0239(7) 0.0342(8) 0.0072(6) -0.0026(6) 0.0026(6) C27 0.0259(7) 0.0287(8) 0.0178(6) 0.0045(6) -0.0011(5) 0.0006(6) C28 0.0466(10) 0.0359(9) 0.0214(7) -0.0040(7) -0.0001(7) 0.0097(8) C29 0.0231(7) 0.0187(7) 0.0340(8) 0.0020(6) 0.0008(6) 0.0049(5) C30 0.0279(8) 0.0274(8) 0.0397(9) -0.0095(7) 0.0034(7) 0.0042(6) C31 0.0175(6) 0.0228(7) 0.0262(7) 0.0061(6) 0.0028(5) -0.0004(5) C32 0.0175(7) 0.0353(9) 0.0481(10) 0.0131(8) -0.0008(7) -0.0009(6) _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 C1 1.8849(13) . ? Ni1 Cl1 2.1983(4) . ? Ni1 P1 2.2151(4) . ? Ni1 P2 2.2152(4) . ? P1 C7 1.8265(17) . ? P1 C5 1.8280(16) . ? P1 C9 1.8377(15) . ? P2 C13 1.8260(14) . ? P2 C11 1.8303(14) . ? P2 C15 1.8359(14) . ? F1 C2 1.3483(17) . ? F2 C3 1.3439(17) . ? F3 C4 1.3449(17) . ? N1 C3 1.310(2) . ? N1 C2 1.3253(18) . ? N2 C3 1.310(2) . ? N2 C4 1.3290(18) . ? C1 C4 1.3817(19) . ? C1 C2 1.3876(19) . ? C5 C6 1.529(3) . ? C7 C8 1.521(3) . ? C9 C10 1.529(2) . ? C11 C12 1.521(2) . ? C13 C14 1.527(2) . ? C15 C16 1.530(2) . ? Ni2 C17 1.8858(13) . ? Ni2 Cl2 2.1984(4) . ? Ni2 P3 2.2132(4) . ? Ni2 P4 2.2172(4) . ? P3 C23 1.8213(14) . ? P3 C21 1.8241(14) . ? P3 C25 1.8345(14) . ? P4 C27 1.8211(15) . ? P4 C29 1.8333(15) . ? P4 C31 1.8398(14) . ? N3 C19 1.311(2) . ? N3 C18 1.3235(18) . ? N4 C19 1.310(2) . ? N4 C20 1.3334(18) . ? F4 C18 1.3440(17) . ? F5 C19 1.3412(17) . ? F6 C20 1.3405(16) . ? C17 C20 1.3816(19) . ? C17 C18 1.3908(19) . ? C21 C22 1.525(2) . ? C23 C24 1.535(2) . ? C25 C26 1.5314(19) . ? C27 C28 1.528(2) . ? C29 C30 1.526(2) . ? C31 C32 1.528(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 C1 Ni1 Cl1 178.30(4) . . ? C1 Ni1 P1 92.11(4) . . ? Cl1 Ni1 P1 87.395(14) . . ? C1 Ni1 P2 91.51(4) . . ? Cl1 Ni1 P2 88.983(14) . . ? P1 Ni1 P2 176.378(15) . . ? C7 P1 C5 103.51(8) . . ? C7 P1 C9 105.30(8) . . ? C5 P1 C9 104.94(8) . . ? C7 P1 Ni1 110.28(6) . . ? C5 P1 Ni1 113.11(6) . . ? C9 P1 Ni1 118.40(5) . . ? C13 P2 C11 104.65(7) . . ? C13 P2 C15 105.02(7) . . ? C11 P2 C15 104.41(7) . . ? C13 P2 Ni1 109.16(5) . . ? C11 P2 Ni1 113.68(5) . . ? C15 P2 Ni1 118.72(5) . . ? C3 N1 C2 112.03(13) . . ? C3 N2 C4 112.59(13) . . ? C4 C1 C2 108.62(12) . . ? C4 C1 Ni1 126.57(11) . . ? C2 C1 Ni1 124.81(11) . . ? N1 C2 F1 113.27(12) . . ? N1 C2 C1 128.70(14) . . ? F1 C2 C1 118.03(12) . . ? N1 C3 N2 129.96(14) . . ? N1 C3 F2 114.99(15) . . ? N2 C3 F2 115.04(15) . . ? N2 C4 F3 113.51(13) . . ? N2 C4 C1 128.09(14) . . ? F3 C4 C1 118.40(12) . . ? C6 C5 P1 112.68(12) . . ? C8 C7 P1 112.41(12) . . ? C10 C9 P1 116.95(12) . . ? C12 C11 P2 113.35(11) . . ? C14 C13 P2 112.69(10) . . ? C16 C15 P2 115.65(10) . . ? C17 Ni2 Cl2 179.31(4) . . ? C17 Ni2 P3 91.77(4) . . ? Cl2 Ni2 P3 88.834(14) . . ? C17 Ni2 P4 91.29(4) . . ? Cl2 Ni2 P4 88.110(14) . . ? P3 Ni2 P4 176.844(14) . . ? C23 P3 C21 103.89(7) . . ? C23 P3 C25 104.55(7) . . ? C21 P3 C25 105.20(7) . . ? C23 P3 Ni2 113.75(5) . . ? C21 P3 Ni2 109.77(5) . . ? C25 P3 Ni2 118.40(5) . . ? C27 P4 C29 104.88(7) . . ? C27 P4 C31 104.72(7) . . ? C29 P4 C31 104.37(7) . . ? C27 P4 Ni2 109.43(5) . . ? C29 P4 Ni2 113.53(5) . . ? C31 P4 Ni2 118.72(5) . . ? C19 N3 C18 112.18(13) . . ? C19 N4 C20 112.40(13) . . ? C20 C17 C18 108.68(12) . . ? C20 C17 Ni2 126.95(11) . . ? C18 C17 Ni2 124.33(10) . . ? N3 C18 F4 113.23(12) . . ? N3 C18 C17 128.55(14) . . ? F4 C18 C17 118.22(12) . . ? N4 C19 N3 130.07(13) . . ? N4 C19 F5 114.98(14) . . ? N3 C19 F5 114.96(14) . . ? N4 C20 F6 113.45(12) . . ? N4 C20 C17 128.11(13) . . ? F6 C20 C17 118.44(12) . . ? C22 C21 P3 113.39(10) . . ? C24 C23 P3 112.04(10) . . ? C26 C25 P3 116.15(10) . . ? C28 C27 P4 111.90(10) . . ? C30 C29 P4 112.42(11) . . ? C32 C31 P4 116.64(11) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.928 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.064 #===END