############################################################################ # # # This Supplementary Material is written in the Crystallographic # # Information File (CIF) format. For further details see: S.R. Hall, # # F.H. Allen and I.D. Brown, Acta Cryst. (1991) A47, 655-685. # # # ############################################################################ data_2d ############################################################################ # # _publ_requested_journal 'Journal of the American Chemical Society' _publ_section_title ; Structural Properties and Dynamics of Five-Coordinate Ni(II)-\p-Allyl Complexes Containing Monodentate Phosphorus Ligands ; loop_ _publ_author_name _publ_author_address 'Anna Rufinska' ; Max-Planck-Institut f\"ur Kohlenforschung D-45466 M\"ulheim an der Ruhr Germany ; 'Richard Goddard' ; Max-Planck-Institut f\"ur Kohlenforschung D-45466 M\"ulheim an der Ruhr Germany ; 'Claudia Weidenthaler' ; Max-Planck-Institut f\"ur Kohlenforschung D-45466 M\"ulheim an der Ruhr Germany ; 'Michael B\"uhl' ; Max-Planck-Institut f\"ur Kohlenforschung D-45466 M\"ulheim an der Ruhr Germany ; 'Klaus-Richard P\"orschke' ; Max-Planck-Institut f\"ur Kohlenforschung D-45466 M\"ulheim an der Ruhr Germany ; # # ############################################################################ _chemical_name_systematic ; \h^3^-allyl-trimethylphosphite-nickel(ii)-hexafluorophosphate ; _chemical_melting_point '>353 decomposition' _chemical_compound_source 'diethylether/dichloromethane' _chemical_formula_moiety 'C12 H32 Ni O9 P3 1+, I 1-' _chemical_formula_sum 'C12 H32 I Ni O9 P3' _chemical_formula_weight 598.90 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' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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 monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.6045(1) _cell_length_b 16.1857(3) _cell_length_c 12.2778(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.796(1) _cell_angle_gamma 90.00 _cell_volume 2298.03(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100 _cell_measurement_reflns_used 47709 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 31.51 _exptl_crystal_description prism _exptl_crystal_colour 'orange-yellow' _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.731 _exptl_crystal_density_method none _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 2.433 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details 'XPREP, Siemens (1995)' _exptl_absorpt_correction_T_min 0.904823 _exptl_absorpt_correction_T_max 1.0 _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source '0.3 mm focus rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'CCD \w-scan' _diffrn_standards_number 0 _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 47940 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_sigmaI/netI 0.0258 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 31.48 _reflns_number_total 7602 _reflns_number_gt 6606 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect software (Nonius, 1998)' _computing_cell_refinement 'Denzo / Scalepack (Otwinowski 1997)' _computing_data_reduction 'Denzo / Scalepack (Otwinowski 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Crystal Impact GbR, 1999)' _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. Highest peak 0.76 at 0.4240 0.2149 0.1122 [ 0.81 A from H9B ] Deepest hole -0.71 at 0.9088 0.2269 0.6010 [ 0.10 A from H9C ] ; _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^)+(0.0278P)^2^+2.8321P] 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_number_reflns 7602 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0332 _refine_ls_R_factor_gt 0.0251 _refine_ls_wR_factor_ref 0.0655 _refine_ls_wR_factor_gt 0.0621 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.20369(18) 0.71255(13) 0.24296(17) 0.0196(4) Uani 1 1 d . . . H1A H -0.1908 0.6784 0.3077 0.024 Uiso 1 1 calc R . . H1B H -0.2213 0.6815 0.1761 0.024 Uiso 1 1 calc R . . C2 C -0.13255(16) 0.78253(13) 0.23666(16) 0.0181(4) Uani 1 1 d . . . H2 H -0.0959 0.7956 0.1697 0.022 Uiso 1 1 calc R . . C3 C -0.11983(17) 0.83460(13) 0.32793(17) 0.0191(4) Uani 1 1 d . . . H3A H -0.0822 0.8874 0.3188 0.023 Uiso 1 1 calc R . . H3B H -0.1004 0.8088 0.3984 0.023 Uiso 1 1 calc R . . C4 C -0.50037(19) 1.05561(13) 0.2647(2) 0.0258(5) Uani 1 1 d . . . H4A H -0.5821 1.0527 0.2714 0.039 Uiso 1 1 calc R . . H4B H -0.4868 1.0802 0.1957 0.039 Uiso 1 1 calc R . . H4C H -0.4645 1.0886 0.3230 0.039 Uiso 1 1 calc R . . C5 C -0.2548(2) 0.98372(14) 0.46974(17) 0.0263(5) Uani 1 1 d . . . H5A H -0.2106 1.0222 0.5158 0.040 Uiso 1 1 calc R . . H5B H -0.2223 0.9294 0.4799 0.040 Uiso 1 1 calc R . . H5C H -0.3334 0.9833 0.4886 0.040 Uiso 1 1 calc R . . C6 C -0.18735(19) 0.99248(14) 0.10544(19) 0.0237(4) Uani 1 1 d . . . H6A H -0.1833 1.0310 0.0464 0.036 Uiso 1 1 calc R . . H6B H -0.1904 0.9372 0.0771 0.036 Uiso 1 1 calc R . . H6C H -0.1201 0.9986 0.1560 0.036 Uiso 1 1 calc R . . C7 C -0.4757(2) 0.65019(13) 0.12140(18) 0.0230(4) Uani 1 1 d . . . H7A H -0.5465 0.6196 0.1093 0.034 Uiso 1 1 calc R . . H7B H -0.4475 0.6462 0.1970 0.034 Uiso 1 1 calc R . . H7C H -0.4193 0.6278 0.0767 0.034 Uiso 1 1 calc R . . C8 C -0.58292(17) 0.89829(13) 0.06344(18) 0.0206(4) Uani 1 1 d . . . H8A H -0.6071 0.9460 0.0210 0.031 Uiso 1 1 calc R . . H8B H -0.5893 0.9095 0.1395 0.031 Uiso 1 1 calc R . . H8C H -0.6312 0.8521 0.0412 0.031 Uiso 1 1 calc R . . C9 C -0.35017(19) 0.77190(16) -0.10053(16) 0.0248(4) Uani 1 1 d . . . H9A H -0.2866 0.7577 -0.1422 0.037 Uiso 1 1 calc R . . H9B H -0.3833 0.8233 -0.1266 0.037 Uiso 1 1 calc R . . H9C H -0.4078 0.7293 -0.1085 0.037 Uiso 1 1 calc R . . C10 C -0.58851(18) 0.84723(15) 0.40205(19) 0.0244(4) Uani 1 1 d . . . H10A H -0.6355 0.8801 0.4461 0.037 Uiso 1 1 calc R . . H10B H -0.6256 0.7950 0.3866 0.037 Uiso 1 1 calc R . . H10C H -0.5788 0.8755 0.3347 0.037 Uiso 1 1 calc R . . C11 C -0.51032(19) 0.65043(13) 0.45985(17) 0.0209(4) Uani 1 1 d . . . H11A H -0.5390 0.5992 0.4290 0.031 Uiso 1 1 calc R . . H11B H -0.5742 0.6847 0.4760 0.031 Uiso 1 1 calc R . . H11C H -0.4624 0.6396 0.5259 0.031 Uiso 1 1 calc R . . C12 C -0.3096(2) 0.76864(15) 0.62128(16) 0.0232(4) Uani 1 1 d . . . H12A H -0.2375 0.7615 0.6646 0.035 Uiso 1 1 calc R . . H12B H -0.3606 0.7238 0.6350 0.035 Uiso 1 1 calc R . . H12C H -0.3443 0.8199 0.6403 0.035 Uiso 1 1 calc R . . I1 I 0.158452(11) 0.967623(8) 0.234020(10) 0.01926(4) Uani 1 1 d . . . Ni1 Ni -0.29305(2) 0.822467(14) 0.259253(18) 0.01054(5) Uani 1 1 d . . . O1 O -0.45176(12) 0.97313(8) 0.27047(12) 0.0152(3) Uani 1 1 d . . . O2 O -0.25169(13) 1.00803(9) 0.35690(12) 0.0179(3) Uani 1 1 d . . . O3 O -0.28944(12) 1.00854(9) 0.16073(11) 0.0163(3) Uani 1 1 d . . . O4 O -0.49662(12) 0.73617(9) 0.09306(12) 0.0182(3) Uani 1 1 d . . . O5 O -0.46369(12) 0.87905(9) 0.04639(11) 0.0155(3) Uani 1 1 d . . . O6 O -0.30910(12) 0.78010(9) 0.01414(11) 0.0167(3) Uani 1 1 d . . . O7 O -0.47654(12) 0.83369(9) 0.46045(11) 0.0167(3) Uani 1 1 d . . . O8 O -0.44290(14) 0.69238(9) 0.38230(12) 0.0204(3) Uani 1 1 d . . . O9 O -0.28915(12) 0.76959(10) 0.50697(11) 0.0205(3) Uani 1 1 d . . . P1 P -0.31875(4) 0.95402(3) 0.26231(4) 0.01166(8) Uani 1 1 d . . . P2 P -0.39519(4) 0.80347(3) 0.10420(4) 0.01142(8) Uani 1 1 d . . . P3 P -0.38121(4) 0.77977(3) 0.40413(4) 0.01215(9) Uani 1 1 d . . . 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 C1 0.0197(9) 0.0166(9) 0.0223(9) -0.0003(7) -0.0004(7) 0.0085(7) C2 0.0126(8) 0.0239(10) 0.0184(8) 0.0047(7) 0.0045(7) 0.0075(7) C3 0.0119(8) 0.0235(10) 0.0214(9) 0.0027(7) -0.0019(7) 0.0018(7) C4 0.0180(10) 0.0138(9) 0.0461(13) 0.0003(9) 0.0060(9) 0.0044(7) C5 0.0395(13) 0.0242(11) 0.0145(9) -0.0033(8) -0.0030(8) -0.0017(9) C6 0.0188(10) 0.0262(10) 0.0273(10) 0.0099(8) 0.0092(8) 0.0018(8) C7 0.0295(11) 0.0149(9) 0.0240(10) 0.0009(7) -0.0011(8) -0.0042(8) C8 0.0134(8) 0.0234(10) 0.0243(10) -0.0003(8) -0.0030(7) 0.0063(7) C9 0.0221(10) 0.0390(13) 0.0129(8) -0.0051(8) -0.0006(7) 0.0067(9) C10 0.0133(9) 0.0303(11) 0.0300(11) 0.0084(9) 0.0049(8) 0.0053(8) C11 0.0244(10) 0.0192(9) 0.0203(9) 0.0022(7) 0.0089(8) -0.0038(8) C12 0.0262(10) 0.0313(11) 0.0121(8) 0.0038(8) 0.0013(7) 0.0011(9) I1 0.01670(6) 0.02416(7) 0.01663(6) -0.00210(5) -0.00028(4) 0.00361(5) Ni1 0.01122(10) 0.01081(10) 0.00958(10) 0.00105(8) 0.00085(8) 0.00170(8) O1 0.0133(6) 0.0115(6) 0.0210(6) 0.0003(5) 0.0026(5) 0.0016(5) O2 0.0207(7) 0.0156(6) 0.0167(6) -0.0015(5) -0.0020(5) -0.0031(5) O3 0.0170(6) 0.0148(6) 0.0174(6) 0.0043(5) 0.0034(5) 0.0014(5) O4 0.0161(7) 0.0157(6) 0.0223(7) 0.0014(5) -0.0008(5) -0.0021(5) O5 0.0146(6) 0.0163(6) 0.0155(6) 0.0035(5) 0.0011(5) 0.0035(5) O6 0.0142(6) 0.0253(7) 0.0106(6) -0.0019(5) 0.0003(5) 0.0035(5) O7 0.0153(6) 0.0185(7) 0.0167(6) -0.0014(5) 0.0034(5) 0.0041(5) O8 0.0274(8) 0.0162(7) 0.0190(7) -0.0017(5) 0.0111(6) -0.0051(6) O9 0.0170(7) 0.0334(8) 0.0111(6) 0.0054(6) 0.0018(5) 0.0047(6) P1 0.0117(2) 0.0113(2) 0.01195(19) 0.00052(15) 0.00068(15) 0.00009(15) P2 0.0105(2) 0.0126(2) 0.01112(18) 0.00013(15) 0.00110(15) 0.00105(15) P3 0.0128(2) 0.0135(2) 0.01042(19) 0.00147(15) 0.00254(15) 0.00142(16) _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 C1 C2 1.408(3) . y C1 Ni1 2.0773(19) . y C2 C3 1.400(3) . y C2 Ni1 2.0126(19) . y C3 Ni1 2.1229(19) . y C4 O1 1.449(2) . y C5 O2 1.443(3) . y C6 O3 1.438(2) . y C7 O4 1.450(2) . y C8 O5 1.450(2) . y C9 O6 1.454(2) . y C10 O7 1.447(3) . y C11 O8 1.451(2) . y C12 O9 1.443(2) . y Ni1 P1 2.1508(5) . y Ni1 P2 2.1786(5) . y Ni1 P3 2.2344(5) . y O1 P1 1.5855(14) . y O2 P1 1.6023(15) . y O3 P1 1.5878(14) . y O4 P2 1.6012(15) . y O5 P2 1.5930(14) . y O6 P2 1.5964(14) . y O7 P3 1.6098(14) . y O8 P3 1.5977(15) . y O9 P3 1.5929(15) . y 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 C2 C1 Ni1 67.42(11) . . y C3 C2 C1 117.61(18) . . y C3 C2 Ni1 74.52(11) . . y C1 C2 Ni1 72.36(11) . . y C2 C3 Ni1 66.01(11) . . y C2 Ni1 C1 40.22(9) . . y C2 Ni1 C3 39.47(8) . . y C1 Ni1 C3 69.74(8) . . y C2 Ni1 P1 116.85(6) . . y C1 Ni1 P1 157.01(6) . . y C3 Ni1 P1 91.69(6) . . y C2 Ni1 P2 106.04(6) . . y C1 Ni1 P2 91.98(6) . . y C3 Ni1 P2 142.00(6) . . y P1 Ni1 P2 95.10(2) . . y C2 Ni1 P3 120.07(6) . . y C1 Ni1 P3 94.43(6) . . y C3 Ni1 P3 101.17(6) . . y P1 Ni1 P3 102.64(2) . . y P2 Ni1 P3 113.58(2) . . y C4 O1 P1 123.63(13) . . y C5 O2 P1 119.83(13) . . y C6 O3 P1 120.63(13) . . y C7 O4 P2 121.70(13) . . y C8 O5 P2 123.16(12) . . y C9 O6 P2 121.25(13) . . y C10 O7 P3 119.34(13) . . y C11 O8 P3 124.26(13) . . y C12 O9 P3 128.17(13) . . y O1 P1 O3 102.40(8) . . y O1 P1 O2 105.31(8) . . y O3 P1 O2 98.23(8) . . y O1 P1 Ni1 109.36(5) . . y O3 P1 Ni1 119.83(6) . . y O2 P1 Ni1 119.55(6) . . y O5 P2 O6 101.02(7) . . y O5 P2 O4 98.54(8) . . y O6 P2 O4 106.13(8) . . y O5 P2 Ni1 119.72(6) . . y O6 P2 Ni1 108.20(5) . . y O4 P2 Ni1 120.87(6) . . y O9 P3 O8 107.63(9) . . y O9 P3 O7 98.92(8) . . y O8 P3 O7 103.75(8) . . y O9 P3 Ni1 109.98(6) . . y O8 P3 Ni1 111.64(6) . . y O7 P3 Ni1 123.44(6) . . y _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 31.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.764 _refine_diff_density_min -0.713 _refine_diff_density_rms 0.094 #===END