Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global # *** Added by check_cif _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' _publ_requested_coeditor_name 'Rothwell' _publ_section_title ; Mono- and dinickellaazaphosphiranes of mono- and bis(tert-butylamido)cyclodiphosph(III)azanes ; loop_ _publ_author_name 'G.R.Lief' 'C.J.Carrow' 'L.Stahl' 'R.J.Staples' _publ_contact_author_name 'Dr Lothar Stahl' _publ_contact_author_address ; Department of Chemistry University of North Dakota Grand Forks ND 58202-9024 UNITED STATES OF AMERICA ; _publ_contact_author_email 'ISTAHL@CHEM.UND.EDU' _publ_section_title ; Mono- and dinickellaazaphosphiranes of mono- and bis (amido) cyclodiphosph (III) azanes ; data_2 _database_code_CSD 166955 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H63 Cl N3 Ni O P3' _chemical_formula_weight 644.88 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' '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' 'Cl' 'Cl' 0.1484 0.1585 '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 Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 20.538(2) _cell_length_b 13.6862(15) _cell_length_c 13.1024(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3682.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.163 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 0.753 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Data was collected using a BRUKER SMART CCD (charge coupled device) based diffractometer equipped with an LT-2 low-temperature apparatus operating at 213 K. A suitable crystal was chosen and mounted on a glass fiber using grease. Data were measured using omega scans of 0.3\% per frame for 30 s , such that a hemisphere was collected. A total of 1271 frames were collected with a final resolution of 0.75 \%A. The first 50 frames were recollected at the end of data collection to monitor for decay. Cell parameters were retrieved using SMART software and refined using SAINT on all observed reflections. Data reduction was performed using the SAINT software which corrects for Lp and decay. Absorption corrections were applied using SADABS based on Blessing, (1995). The structures are solved by the direct method using the SHELX-90 program and refined by least squares method on F2 SHELXL-93, incorporated in SHELXTL V5.1. Carbon-bound H atoms were placed in idealized positions and refined as a riding model. ; _diffrn_ambient_temperature 213(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 ? _diffrn_measurement_method '\w, 0.3 deg' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 24068 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_sigmaI/netI 0.0200 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 28.31 _reflns_number_total 4736 _reflns_number_gt 4182 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'ASTRO (BRUKER, V5.007, 1997)' _computing_cell_refinement 'SMART (BRUKER, V5.054, 1998)' _computing_data_reduction 'SAINT (BRUKER, V6.01, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (BRUKER, 1998, V5.1)' _computing_publication_material 'XCIF (Sheldrick and BRUKER, 1997, V5.1)' _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^)+(0.0806P)^2^+2.7319P] 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 4736 _refine_ls_number_parameters 196 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0638 _refine_ls_R_factor_gt 0.0569 _refine_ls_wR_factor_ref 0.1549 _refine_ls_wR_factor_gt 0.1497 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.117 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.002 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 0.32371(2) 0.2500 0.68660(3) 0.03376(15) Uani 1 2 d S . . Cl1 Cl 0.28096(6) 0.2500 0.84201(7) 0.0504(3) Uani 1 2 d S . . P1 P 0.31399(4) 0.2500 0.52861(6) 0.02877(19) Uani 1 2 d S . . P2 P 0.35167(4) 0.2500 0.34184(6) 0.0314(2) Uani 1 2 d S . . P3 P 0.42195(6) 0.2500 0.74377(9) 0.0614(3) Uani 1 2 d S . . O1 O 0.28702(12) 0.2500 0.27039(18) 0.0419(6) Uani 1 2 d S . . N1 N 0.25075(14) 0.2500 0.5944(2) 0.0380(6) Uani 1 2 d S . . N2 N 0.33204(10) 0.16860(14) 0.43719(14) 0.0337(4) Uani 1 1 d . . . C1 C 0.18003(18) 0.2500 0.5972(3) 0.0445(9) Uani 1 2 d S . . C2 C 0.15744(18) 0.1590(3) 0.6537(3) 0.0698(10) Uani 1 1 d . . . H2A H 0.1748 0.1596 0.7225 0.105 Uiso 1 1 calc R . . H2B H 0.1729 0.1013 0.6181 0.105 Uiso 1 1 calc R . . H2C H 0.1102 0.1580 0.6564 0.105 Uiso 1 1 calc R . . C3 C 0.1539(2) 0.2500 0.4887(4) 0.0667(13) Uani 1 2 d S . . H3A H 0.1683 0.3078 0.4537 0.100 Uiso 1 1 d R . . H3B H 0.1072 0.2500 0.4910 0.100 Uiso 1 2 d SR . . C4 C 0.33061(15) 0.06083(19) 0.4348(2) 0.0456(6) Uani 1 1 d . . . C5 C 0.3384(2) 0.0213(2) 0.5423(3) 0.0736(11) Uani 1 1 d . . . H5A H 0.3798 0.0427 0.5701 0.110 Uiso 1 1 calc R . . H5B H 0.3371 -0.0495 0.5407 0.110 Uiso 1 1 calc R . . H5C H 0.3032 0.0455 0.5848 0.110 Uiso 1 1 calc R . . C6 C 0.38549(19) 0.0240(2) 0.3672(3) 0.0613(8) Uani 1 1 d . . . H6A H 0.4269 0.0455 0.3948 0.092 Uiso 1 1 calc R . . H6B H 0.3801 0.0499 0.2988 0.092 Uiso 1 1 calc R . . H6C H 0.3845 -0.0468 0.3650 0.092 Uiso 1 1 calc R . . C7 C 0.2653(2) 0.0262(3) 0.3913(3) 0.0728(10) Uani 1 1 d . . . H7A H 0.2601 0.0512 0.3225 0.109 Uiso 1 1 calc R . . H7B H 0.2301 0.0501 0.4338 0.109 Uiso 1 1 calc R . . H7C H 0.2644 -0.0446 0.3899 0.109 Uiso 1 1 calc R . . C8 C 0.28915(19) 0.2500 0.1578(3) 0.0431(8) Uani 1 2 d S . . C9 C 0.2180(2) 0.2500 0.1274(4) 0.0621(12) Uani 1 2 d S . . H9A H 0.1975 0.3083 0.1525 0.093 Uiso 1 1 d R . . H9B H 0.2145 0.2500 0.0544 0.093 Uiso 1 2 d SR . . C10 C 0.3226(2) 0.1578(3) 0.1186(2) 0.0705(11) Uani 1 1 d . . . H10A H 0.3681 0.1587 0.1385 0.106 Uiso 1 1 calc R . . H10B H 0.3194 0.1555 0.0448 0.106 Uiso 1 1 calc R . . H10C H 0.3016 0.1008 0.1476 0.106 Uiso 1 1 calc R . . C11 C 0.4899(3) 0.2500 0.6554(5) 0.140(4) Uani 1 2 d S . . H11A H 0.5261 0.2247 0.6935 0.168 Uiso 0.50 1 d PR . . H11B H 0.4995 0.3177 0.6433 0.168 Uiso 0.50 1 d PR . . C12 C 0.4939(3) 0.2095(6) 0.5667(7) 0.082(3) Uani 0.50 1 d P . . H12A H 0.4526 0.2169 0.5334 0.098 Uiso 0.50 1 d PR . . H12B H 0.5011 0.1408 0.5765 0.098 Uiso 0.50 1 d PR . . C13 C 0.5480(3) 0.2500 0.4903(7) 0.119(3) Uani 1 2 d S . . H13A H 0.5904 0.2427 0.5201 0.143 Uiso 0.50 1 d PR . . H13B H 0.5408 0.3176 0.4744 0.143 Uiso 0.50 1 d PR . . C14 C 0.5418(5) 0.1921(10) 0.4061(11) 0.125(5) Uani 0.50 1 d P . . H14A H 0.5734 0.2110 0.3559 0.187 Uiso 0.50 1 d PR . . H14B H 0.5484 0.1249 0.4245 0.187 Uiso 0.50 1 d PR . . H14C H 0.4988 0.2001 0.3786 0.187 Uiso 0.50 1 d PR . . C15 C 0.4388(2) 0.1474(5) 0.8327(3) 0.1012(18) Uani 1 1 d . . . H15A H 0.4850 0.1491 0.8514 0.121 Uiso 1 1 calc R . . H15B H 0.4134 0.1573 0.8951 0.121 Uiso 1 1 calc R . . C16 C 0.4238(4) 0.0509(5) 0.7919(5) 0.134(2) Uani 1 1 d . . . H16A H 0.4478 0.0416 0.7281 0.161 Uiso 1 1 calc R . . H16B H 0.3772 0.0480 0.7759 0.161 Uiso 1 1 calc R . . C17 C 0.4404(6) -0.0322(7) 0.8645(6) 0.184(4) Uani 1 1 d . . . H17A H 0.4476 -0.0023 0.9315 0.221 Uiso 1 1 calc R . . H17B H 0.4009 -0.0720 0.8706 0.221 Uiso 1 1 calc R . . C18 C 0.4831(7) -0.0865(11) 0.8518(11) 0.343(13) Uani 1 1 d . . . H18A H 0.4853 -0.1339 0.9057 0.515 Uiso 1 1 d R . . H18B H 0.4793 -0.1194 0.7874 0.515 Uiso 1 1 d R . . H18C H 0.5220 -0.0474 0.8522 0.515 Uiso 1 1 d 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 0.0375(3) 0.0395(3) 0.0242(2) 0.000 -0.00003(15) 0.000 Cl1 0.0645(6) 0.0598(6) 0.0269(4) 0.000 0.0062(4) 0.000 P1 0.0329(4) 0.0294(4) 0.0240(4) 0.000 0.0005(3) 0.000 P2 0.0361(4) 0.0337(4) 0.0245(4) 0.000 0.0010(3) 0.000 P3 0.0442(6) 0.0936(10) 0.0463(6) 0.000 -0.0090(5) 0.000 O1 0.0398(13) 0.0575(16) 0.0286(12) 0.000 -0.0037(10) 0.000 N1 0.0349(14) 0.0477(17) 0.0312(14) 0.000 0.0009(11) 0.000 N2 0.0487(11) 0.0267(9) 0.0258(9) 0.0013(7) 0.0036(8) 0.0019(8) C1 0.0356(18) 0.050(2) 0.048(2) 0.000 0.0002(15) 0.000 C2 0.0504(17) 0.076(2) 0.083(2) 0.018(2) 0.0074(17) -0.0172(17) C3 0.044(2) 0.092(4) 0.064(3) 0.000 -0.011(2) 0.000 C4 0.0650(17) 0.0298(12) 0.0420(14) -0.0015(10) 0.0046(12) -0.0001(11) C5 0.134(3) 0.0334(15) 0.0531(18) 0.0099(14) 0.009(2) 0.0062(18) C6 0.080(2) 0.0410(15) 0.0629(18) -0.0059(14) 0.0096(17) 0.0158(15) C7 0.080(2) 0.0494(18) 0.089(3) -0.0155(18) 0.000(2) -0.0203(17) C8 0.047(2) 0.056(2) 0.0265(15) 0.000 -0.0054(14) 0.000 C9 0.063(3) 0.074(3) 0.049(2) 0.000 -0.018(2) 0.000 C10 0.091(3) 0.085(3) 0.0356(15) -0.0104(16) -0.0039(15) 0.029(2) C11 0.037(3) 0.318(14) 0.065(4) 0.000 0.000(2) 0.000 C12 0.045(3) 0.111(7) 0.088(5) -0.018(5) 0.006(3) 0.009(3) C13 0.047(3) 0.205(11) 0.104(6) 0.000 0.024(4) 0.000 C14 0.054(5) 0.147(10) 0.172(13) 0.006(10) -0.017(6) 0.009(6) C15 0.074(3) 0.161(6) 0.069(3) 0.009(3) -0.021(2) 0.033(3) C16 0.186(7) 0.127(5) 0.091(4) 0.016(4) -0.018(4) 0.031(5) C17 0.259(12) 0.170(8) 0.123(6) 0.068(6) 0.023(7) 0.088(8) C18 0.309(15) 0.368(19) 0.353(18) 0.265(16) 0.242(14) 0.239(15) _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 N1 1.925(3) . ? Ni1 P1 2.0796(9) . ? Ni1 P3 2.1522(12) . ? Ni1 Cl1 2.2175(10) . ? P1 N1 1.559(3) . ? P1 N2 1.677(2) 7_565 ? P1 N2 1.677(2) . ? P1 P2 2.5667(12) . ? P2 O1 1.625(3) . ? P2 N2 1.722(2) . ? P2 N2 1.722(2) 7_565 ? P3 C11 1.813(6) . ? P3 C15 1.857(5) 7_565 ? P3 C15 1.857(5) . ? O1 C8 1.476(4) . ? N1 C1 1.453(5) . ? N2 C4 1.476(3) . ? C1 C2 1.521(4) . ? C1 C2 1.521(4) 7_565 ? C1 C3 1.520(6) . ? C4 C5 1.516(4) . ? C4 C6 1.519(4) . ? C4 C7 1.532(5) . ? C8 C9 1.515(6) . ? C8 C10 1.525(4) 7_565 ? C8 C10 1.525(4) . ? C11 C12 1.290(10) 7_565 ? C11 C12 1.290(10) . ? C12 C12 1.109(18) 7_565 ? C12 C13 1.595(10) . ? C13 C14 1.363(14) . ? C13 C14 1.363(14) 7_565 ? C13 C12 1.595(10) 7_565 ? C14 C14 1.58(3) 7_565 ? C15 C16 1.457(9) . ? C16 C17 1.521(9) . ? C17 C18 1.162(10) . ? 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 N1 Ni1 P1 45.62(9) . . ? N1 Ni1 P3 161.50(10) . . ? P1 Ni1 P3 115.88(5) . . ? N1 Ni1 Cl1 105.55(9) . . ? P1 Ni1 Cl1 151.17(4) . . ? P3 Ni1 Cl1 92.95(5) . . ? N1 P1 N2 125.39(10) . 7_565 ? N1 P1 N2 125.39(10) . . ? N2 P1 N2 83.23(13) 7_565 . ? N1 P1 Ni1 61.93(11) . . ? N2 P1 Ni1 133.60(7) 7_565 . ? N2 P1 Ni1 133.60(7) . . ? N1 P1 P2 141.13(12) . . ? N2 P1 P2 41.62(7) 7_565 . ? N2 P1 P2 41.62(7) . . ? Ni1 P1 P2 156.94(5) . . ? O1 P2 N2 103.11(10) . . ? O1 P2 N2 103.11(10) . 7_565 ? N2 P2 N2 80.64(13) . 7_565 ? O1 P2 P1 107.64(10) . . ? N2 P2 P1 40.32(7) . . ? N2 P2 P1 40.32(7) 7_565 . ? C11 P3 C15 104.9(2) . 7_565 ? C11 P3 C15 104.9(2) . . ? C15 P3 C15 98.3(4) 7_565 . ? C11 P3 Ni1 119.9(2) . . ? C15 P3 Ni1 113.15(17) 7_565 . ? C15 P3 Ni1 113.15(17) . . ? C8 O1 P2 123.5(2) . . ? C1 N1 P1 147.9(3) . . ? C1 N1 Ni1 139.7(3) . . ? P1 N1 Ni1 72.45(12) . . ? C4 N2 P1 132.40(17) . . ? C4 N2 P2 129.52(17) . . ? P1 N2 P2 98.06(10) . . ? N1 C1 C2 108.5(2) . . ? N1 C1 C2 108.5(2) . 7_565 ? C2 C1 C2 109.9(4) . 7_565 ? N1 C1 C3 109.2(3) . . ? C2 C1 C3 110.3(3) . . ? C2 C1 C3 110.3(3) 7_565 . ? N2 C4 C5 109.6(2) . . ? N2 C4 C6 109.2(2) . . ? C5 C4 C6 110.2(3) . . ? N2 C4 C7 109.5(3) . . ? C5 C4 C7 109.1(3) . . ? C6 C4 C7 109.2(3) . . ? O1 C8 C9 103.5(3) . . ? O1 C8 C10 110.5(2) . 7_565 ? C9 C8 C10 110.3(2) . 7_565 ? O1 C8 C10 110.5(2) . . ? C9 C8 C10 110.3(2) . . ? C10 C8 C10 111.5(4) 7_565 . ? C12 C11 C12 50.9(9) 7_565 . ? C12 C11 P3 128.6(5) 7_565 . ? C12 C11 P3 128.6(5) . . ? C12 C12 C11 64.5(4) 7_565 . ? C12 C12 C13 69.7(3) 7_565 . ? C11 C12 C13 117.4(7) . . ? C14 C13 C14 71.1(12) . 7_565 ? C14 C13 C12 103.9(7) . . ? C14 C13 C12 130.2(7) 7_565 . ? C14 C13 C12 130.2(7) . 7_565 ? C14 C13 C12 103.9(7) 7_565 7_565 ? C12 C13 C12 40.7(6) . 7_565 ? C13 C14 C14 54.5(6) . 7_565 ? C16 C15 P3 114.6(3) . . ? C15 C16 C17 113.6(7) . . ? C18 C17 C16 124.0(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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P3 Ni1 P1 N1 180.0 . . . . ? Cl1 Ni1 P1 N1 0.0 . . . . ? N1 Ni1 P1 N2 113.49(11) . . . 7_565 ? P3 Ni1 P1 N2 -66.51(11) . . . 7_565 ? Cl1 Ni1 P1 N2 113.49(11) . . . 7_565 ? N1 Ni1 P1 N2 -113.49(11) . . . . ? P3 Ni1 P1 N2 66.51(11) . . . . ? Cl1 Ni1 P1 N2 -113.49(11) . . . . ? N1 Ni1 P1 P2 180.0 . . . . ? P3 Ni1 P1 P2 0.0 . . . . ? Cl1 Ni1 P1 P2 180.0 . . . . ? N1 P1 P2 O1 0.0 . . . . ? N2 P1 P2 O1 -89.61(11) 7_565 . . . ? N2 P1 P2 O1 89.61(11) . . . . ? Ni1 P1 P2 O1 180.0 . . . . ? N1 P1 P2 N2 -89.61(11) . . . . ? N2 P1 P2 N2 -179.2(2) 7_565 . . . ? Ni1 P1 P2 N2 90.39(11) . . . . ? N1 P1 P2 N2 89.61(11) . . . 7_565 ? N2 P1 P2 N2 179.2(2) . . . 7_565 ? Ni1 P1 P2 N2 -90.39(11) . . . 7_565 ? N1 Ni1 P3 C11 0.0 . . . . ? P1 Ni1 P3 C11 0.0 . . . . ? Cl1 Ni1 P3 C11 180.0 . . . . ? N1 Ni1 P3 C15 124.7(2) . . . 7_565 ? P1 Ni1 P3 C15 124.7(2) . . . 7_565 ? Cl1 Ni1 P3 C15 -55.3(2) . . . 7_565 ? N1 Ni1 P3 C15 -124.7(2) . . . . ? P1 Ni1 P3 C15 -124.7(2) . . . . ? Cl1 Ni1 P3 C15 55.3(2) . . . . ? N2 P2 O1 C8 -138.37(7) . . . . ? N2 P2 O1 C8 138.37(7) 7_565 . . . ? P1 P2 O1 C8 180.0 . . . . ? N2 P1 N1 C1 54.56(11) 7_565 . . . ? N2 P1 N1 C1 -54.56(11) . . . . ? Ni1 P1 N1 C1 180.0 . . . . ? P2 P1 N1 C1 0.000(1) . . . . ? N2 P1 N1 Ni1 -125.44(11) 7_565 . . . ? N2 P1 N1 Ni1 125.44(11) . . . . ? P2 P1 N1 Ni1 180.0 . . . . ? P1 Ni1 N1 C1 180.0 . . . . ? P3 Ni1 N1 C1 180.0 . . . . ? Cl1 Ni1 N1 C1 0.0 . . . . ? P3 Ni1 N1 P1 0.0 . . . . ? Cl1 Ni1 N1 P1 180.0 . . . . ? N1 P1 N2 C4 -48.9(3) . . . . ? N2 P1 N2 C4 -178.0(2) 7_565 . . . ? Ni1 P1 N2 C4 34.2(3) . . . . ? P2 P1 N2 C4 -178.6(3) . . . . ? N1 P1 N2 P2 129.66(13) . . . . ? N2 P1 N2 P2 0.52(15) 7_565 . . . ? Ni1 P1 N2 P2 -147.26(7) . . . . ? O1 P2 N2 C4 76.7(2) . . . . ? N2 P2 N2 C4 178.11(19) 7_565 . . . ? P1 P2 N2 C4 178.6(3) . . . . ? O1 P2 N2 P1 -101.91(11) . . . . ? N2 P2 N2 P1 -0.51(15) 7_565 . . . ? P1 N1 C1 C2 120.3(3) . . . . ? Ni1 N1 C1 C2 -59.7(3) . . . . ? P1 N1 C1 C2 -120.3(3) . . . 7_565 ? Ni1 N1 C1 C2 59.7(3) . . . 7_565 ? P1 N1 C1 C3 0.0 . . . . ? Ni1 N1 C1 C3 180.0 . . . . ? P1 N2 C4 C5 -25.4(4) . . . . ? P2 N2 C4 C5 156.5(3) . . . . ? P1 N2 C4 C6 -146.1(2) . . . . ? P2 N2 C4 C6 35.8(4) . . . . ? P1 N2 C4 C7 94.3(3) . . . . ? P2 N2 C4 C7 -83.8(3) . . . . ? P2 O1 C8 C9 180.0 . . . . ? P2 O1 C8 C10 -62.0(3) . . . 7_565 ? P2 O1 C8 C10 62.0(3) . . . . ? C15 P3 C11 C12 -95.1(7) 7_565 . . 7_565 ? C15 P3 C11 C12 161.9(6) . . . 7_565 ? Ni1 P3 C11 C12 33.4(6) . . . 7_565 ? C15 P3 C11 C12 -161.9(6) 7_565 . . . ? C15 P3 C11 C12 95.1(7) . . . . ? Ni1 P3 C11 C12 -33.4(6) . . . . ? P3 C11 C12 C12 112.4(6) . . . 7_565 ? C12 C11 C12 C13 47.1(7) 7_565 . . . ? P3 C11 C12 C13 159.5(4) . . . . ? C12 C12 C13 C14 -136.9(7) 7_565 . . . ? C11 C12 C13 C14 178.2(8) . . . . ? C12 C12 C13 C14 -60.1(8) 7_565 . . 7_565 ? C11 C12 C13 C14 -105.0(11) . . . 7_565 ? C11 C12 C13 C12 -44.8(8) . . . 7_565 ? C12 C13 C14 C14 128.1(7) . . . 7_565 ? C12 C13 C14 C14 92.5(9) 7_565 . . 7_565 ? C11 P3 C15 C16 -78.3(5) . . . . ? C15 P3 C15 C16 173.8(4) 7_565 . . . ? Ni1 P3 C15 C16 54.1(5) . . . . ? P3 C15 C16 C17 177.8(6) . . . . ? C15 C16 C17 C18 -109.0(18) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.701 _refine_diff_density_min -0.423 _refine_diff_density_rms 0.074 #====END=== data_3 _database_code_CSD 166956 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H90 Cl2 N4 Ni2 P4' _chemical_formula_weight 939.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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' 'N' 'N' 0.0061 0.0033 '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' '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 13.905(3) _cell_length_b 18.186(4) _cell_length_c 21.592(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.13(3) _cell_angle_gamma 90.00 _cell_volume 5405.3(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.154 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 0.942 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8647 _diffrn_reflns_av_R_equivalents 0.0876 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 22.50 _reflns_number_total 7028 _reflns_number_gt 5509 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0567P)^2^+9.5083P] 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 7028 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0757 _refine_ls_R_factor_gt 0.0532 _refine_ls_wR_factor_ref 0.1486 _refine_ls_wR_factor_gt 0.1304 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.090 _refine_ls_shift/su_mean 0.001 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 0.13173(5) 0.71007(3) 0.20615(3) 0.0608(2) Uani 1 1 d . . . Ni2 Ni 0.35662(5) 0.40901(4) 0.20590(3) 0.0666(2) Uani 1 1 d . . . Cl1 Cl 0.04162(14) 0.80998(9) 0.19907(8) 0.1025(5) Uani 1 1 d . . . Cl2 Cl 0.44508(13) 0.30986(9) 0.19896(9) 0.1060(6) Uani 1 1 d . . . N1 N 0.1638(3) 0.5271(2) 0.16367(17) 0.0553(9) Uani 1 1 d . . . N2 N 0.3006(3) 0.5898(2) 0.16018(18) 0.0583(10) Uani 1 1 d . . . N3 N 0.1263(3) 0.6746(2) 0.12106(17) 0.0622(10) Uani 1 1 d . . . N4 N 0.3167(3) 0.4414(2) 0.12031(19) 0.0691(11) Uani 1 1 d . . . P1 P 0.18657(9) 0.61874(7) 0.16528(5) 0.0517(3) Uani 1 1 d . . . P2 P 0.27923(9) 0.49816(7) 0.16490(6) 0.0544(3) Uani 1 1 d . . . P3 P 0.17669(12) 0.71768(8) 0.30564(6) 0.0761(4) Uani 1 1 d . . . P4 P 0.36284(13) 0.40413(9) 0.30626(8) 0.0858(5) Uani 1 1 d . . . C10 C 0.0709(4) 0.4869(3) 0.1682(2) 0.0652(13) Uani 1 1 d . . . C11 C 0.0926(5) 0.4052(3) 0.1755(4) 0.104(2) Uani 1 1 d . . . H11A H 0.1164 0.3872 0.1387 0.155 Uiso 1 1 calc R . . H11B H 0.0343 0.3793 0.1811 0.155 Uiso 1 1 calc R . . H11C H 0.1409 0.3974 0.2113 0.155 Uiso 1 1 calc R . . C12 C 0.0010(5) 0.4999(4) 0.1089(3) 0.108(2) Uani 1 1 d . . . H12A H -0.0168 0.5510 0.1062 0.162 Uiso 1 1 calc R . . H12B H -0.0561 0.4705 0.1096 0.162 Uiso 1 1 calc R . . H12C H 0.0316 0.4866 0.0734 0.162 Uiso 1 1 calc R . . C13 C 0.0273(4) 0.5156(4) 0.2241(3) 0.0952(19) Uani 1 1 d . . . H13A H 0.0723 0.5079 0.2615 0.143 Uiso 1 1 calc R . . H13B H -0.0321 0.4899 0.2272 0.143 Uiso 1 1 calc R . . H13C H 0.0141 0.5673 0.2188 0.143 Uiso 1 1 calc R . . C20 C 0.3936(4) 0.6303(3) 0.1607(3) 0.0702(14) Uani 1 1 d . . . C21 C 0.3743(4) 0.7124(3) 0.1672(4) 0.097(2) Uani 1 1 d . . . H21A H 0.3293 0.7288 0.1321 0.145 Uiso 1 1 calc R . . H21B H 0.4342 0.7390 0.1686 0.145 Uiso 1 1 calc R . . H21C H 0.3474 0.7211 0.2051 0.145 Uiso 1 1 calc R . . C22 C 0.4318(5) 0.6159(4) 0.0994(3) 0.119(3) Uani 1 1 d . . . H22A H 0.4463 0.5646 0.0963 0.178 Uiso 1 1 calc R . . H22B H 0.4897 0.6442 0.0981 0.178 Uiso 1 1 calc R . . H22C H 0.3835 0.6299 0.0652 0.178 Uiso 1 1 calc R . . C23 C 0.4655(4) 0.6042(4) 0.2156(4) 0.106(2) Uani 1 1 d . . . H23A H 0.4389 0.6121 0.2537 0.159 Uiso 1 1 calc R . . H23B H 0.5250 0.6313 0.2169 0.159 Uiso 1 1 calc R . . H23C H 0.4781 0.5528 0.2109 0.159 Uiso 1 1 calc R . . C30 C 0.0939(4) 0.7012(3) 0.0570(2) 0.0760(15) Uani 1 1 d . . . C31 C 0.1278(6) 0.6461(4) 0.0108(3) 0.117(2) Uani 1 1 d . . . H31A H 0.1971 0.6407 0.0194 0.176 Uiso 1 1 calc R . . H31B H 0.1101 0.6637 -0.0312 0.176 Uiso 1 1 calc R . . H31C H 0.0975 0.5994 0.0153 0.176 Uiso 1 1 calc R . . C32 C 0.1413(6) 0.7757(4) 0.0498(3) 0.109(2) Uani 1 1 d . . . H32A H 0.1284 0.8077 0.0831 0.163 Uiso 1 1 calc R . . H32B H 0.1151 0.7970 0.0103 0.163 Uiso 1 1 calc R . . H32C H 0.2101 0.7694 0.0516 0.163 Uiso 1 1 calc R . . C33 C -0.0152(5) 0.7097(4) 0.0479(3) 0.111(2) Uani 1 1 d . . . H33A H -0.0448 0.6625 0.0516 0.167 Uiso 1 1 calc R . . H33B H -0.0366 0.7296 0.0071 0.167 Uiso 1 1 calc R . . H33C H -0.0335 0.7423 0.0791 0.167 Uiso 1 1 calc R . . C40 C 0.3138(5) 0.4116(3) 0.0566(3) 0.0874(17) Uani 1 1 d . . . C41 C 0.2690(5) 0.3352(4) 0.0545(3) 0.110(2) Uani 1 1 d . . . H41A H 0.3053 0.3048 0.0858 0.164 Uiso 1 1 calc R . . H41B H 0.2704 0.3140 0.0140 0.164 Uiso 1 1 calc R . . H41C H 0.2029 0.3387 0.0625 0.164 Uiso 1 1 calc R . . C42 C 0.4157(6) 0.4059(4) 0.0412(4) 0.128(3) Uani 1 1 d . . . H42A H 0.4430 0.4543 0.0397 0.192 Uiso 1 1 calc R . . H42B H 0.4146 0.3825 0.0013 0.192 Uiso 1 1 calc R . . H42C H 0.4546 0.3774 0.0728 0.192 Uiso 1 1 calc R . . C43 C 0.2521(7) 0.4627(4) 0.0115(3) 0.130(3) Uani 1 1 d . . . H43A H 0.1884 0.4667 0.0233 0.195 Uiso 1 1 calc R . . H43B H 0.2473 0.4433 -0.0302 0.195 Uiso 1 1 calc R . . H43C H 0.2818 0.5105 0.0128 0.195 Uiso 1 1 calc R . . C50 C 0.0951(6) 0.6690(5) 0.3518(3) 0.120(3) Uani 1 1 d . . . H50A H 0.0978 0.6169 0.3426 0.144 Uiso 1 1 calc R . . H50B H 0.1199 0.6753 0.3958 0.144 Uiso 1 1 calc R . . C51 C -0.0051(6) 0.6915(5) 0.3420(4) 0.134(3) Uani 1 1 d . . . H51A H -0.0290 0.6901 0.2975 0.161 Uiso 1 1 calc R . . H51B H -0.0096 0.7419 0.3560 0.161 Uiso 1 1 calc R . . C52 C -0.0697(8) 0.6425(6) 0.3769(5) 0.163(4) Uani 1 1 d . . . H52A H -0.0687 0.5928 0.3607 0.196 Uiso 1 1 calc R . . H52B H -0.0427 0.6411 0.4208 0.196 Uiso 1 1 calc R . . C54 C 0.2944(5) 0.6768(4) 0.3345(3) 0.105(2) Uani 1 1 d . . . H54A H 0.2899 0.6244 0.3261 0.126 Uiso 1 1 calc R . . H54B H 0.3416 0.6966 0.3098 0.126 Uiso 1 1 calc R . . C55 C 0.3350(7) 0.6867(6) 0.4032(3) 0.147(3) Uani 1 1 d . . . H55A H 0.3284 0.7379 0.4144 0.177 Uiso 1 1 calc R . . H55B H 0.2966 0.6576 0.4283 0.177 Uiso 1 1 calc R . . C56 C 0.4391(8) 0.6649(6) 0.4186(4) 0.170(4) Uani 1 1 d . . . H56A H 0.4442 0.6126 0.4108 0.204 Uiso 1 1 calc R . . H56B H 0.4759 0.6903 0.3902 0.204 Uiso 1 1 calc R . . C57 C 0.4842(10) 0.6798(7) 0.4824(5) 0.230(6) Uani 1 1 d . . . H57A H 0.4850 0.7318 0.4898 0.345 Uiso 1 1 calc R . . H57B H 0.5496 0.6613 0.4883 0.345 Uiso 1 1 calc R . . H57C H 0.4478 0.6559 0.5112 0.345 Uiso 1 1 calc R . . C58 C 0.1892(5) 0.8111(3) 0.3363(3) 0.098(2) Uani 1 1 d . . . H58A H 0.1273 0.8361 0.3264 0.118 Uiso 1 1 calc R . . H58B H 0.2043 0.8087 0.3815 0.118 Uiso 1 1 calc R . . C59 C 0.2647(5) 0.8552(4) 0.3119(4) 0.119(3) Uani 1 1 d . . . H59A H 0.2453 0.8650 0.2677 0.143 Uiso 1 1 calc R . . H59B H 0.3254 0.8281 0.3166 0.143 Uiso 1 1 calc R . . C61 C 0.3458(8) 0.9704(7) 0.3392(8) 0.242(8) Uani 1 1 d . . . H61A H 0.4056 0.9433 0.3434 0.363 Uiso 1 1 calc R . . H61B H 0.3512 1.0096 0.3693 0.363 Uiso 1 1 calc R . . H61C H 0.3326 0.9905 0.2978 0.363 Uiso 1 1 calc R . . C62 C 0.2654(6) 0.4506(4) 0.3383(3) 0.123(3) Uani 1 1 d . . . H62A H 0.2682 0.5023 0.3276 0.148 Uiso 1 1 calc R . . H62B H 0.2044 0.4317 0.3169 0.148 Uiso 1 1 calc R . . C63 C 0.2613(9) 0.4459(6) 0.4092(4) 0.188(5) Uani 1 1 d . . . H63A H 0.3106 0.4779 0.4311 0.225 Uiso 1 1 calc R . . H63B H 0.2760 0.3960 0.4233 0.225 Uiso 1 1 calc R . . C66 C 0.3581(5) 0.3119(4) 0.3372(3) 0.103(2) Uani 1 1 d . . . H66A H 0.4140 0.2847 0.3273 0.123 Uiso 1 1 calc R . . H66B H 0.3636 0.3149 0.3824 0.123 Uiso 1 1 calc R . . C67 C 0.2700(5) 0.2702(4) 0.3139(4) 0.113(2) Uani 1 1 d . . . H67A H 0.2675 0.2619 0.2693 0.136 Uiso 1 1 calc R . . H67B H 0.2133 0.2986 0.3204 0.136 Uiso 1 1 calc R . . C68 C 0.2680(7) 0.1951(5) 0.3479(6) 0.158(4) Uani 1 1 d . . . H68A H 0.3266 0.1682 0.3428 0.190 Uiso 1 1 calc R . . H68B H 0.2693 0.2042 0.3923 0.190 Uiso 1 1 calc R . . C69 C 0.1898(8) 0.1519(6) 0.3276(6) 0.178(4) Uani 1 1 d . . . H69A H 0.1312 0.1795 0.3284 0.268 Uiso 1 1 calc R . . H69B H 0.1898 0.1098 0.3544 0.268 Uiso 1 1 calc R . . H69C H 0.1933 0.1359 0.2856 0.268 Uiso 1 1 calc R . . C70 C 0.4692(7) 0.4492(6) 0.3512(4) 0.148(3) Uani 1 1 d . . . H70A H 0.4613 0.5019 0.3457 0.178 Uiso 1 1 calc R . . H70B H 0.4681 0.4389 0.3952 0.178 Uiso 1 1 calc R . . C71 C 0.5583(7) 0.4310(7) 0.3376(5) 0.165(4) Uani 1 1 d . . . H71A H 0.5599 0.4394 0.2934 0.198 Uiso 1 1 calc R . . H71B H 0.5692 0.3790 0.3455 0.198 Uiso 1 1 calc R . . C72 C 0.6440(8) 0.4762(8) 0.3769(7) 0.214(6) Uani 1 1 d . . . H72A H 0.6393 0.5274 0.3643 0.257 Uiso 1 1 calc R . . H72B H 0.6374 0.4736 0.4209 0.257 Uiso 1 1 calc R . . C73 C 0.7310(14) 0.4498(10) 0.3682(11) 0.358(14) Uani 1 1 d . . . H73A H 0.7227 0.4119 0.3369 0.537 Uiso 1 1 calc R . . H73B H 0.7631 0.4297 0.4068 0.537 Uiso 1 1 calc R . . H73C H 0.7697 0.4888 0.3547 0.537 Uiso 1 1 calc R . . C60 C 0.2792(8) 0.9291(5) 0.3483(8) 0.227(7) Uani 1 1 d . . . H60A H 0.2191 0.9566 0.3394 0.272 Uiso 1 1 calc R . . H60B H 0.2878 0.9175 0.3926 0.272 Uiso 1 1 calc R . . C64 C 0.1607(16) 0.4681(9) 0.4263(7) 0.283(12) Uani 1 1 d . . . H64A H 0.1698 0.5155 0.4469 0.340 Uiso 1 1 calc R . . H64B H 0.1193 0.4768 0.3869 0.340 Uiso 1 1 calc R . . C53 C -0.1652(12) 0.6664(8) 0.3715(7) 0.251(7) Uani 1 1 d . . . H53A H -0.1677 0.7126 0.3926 0.377 Uiso 1 1 calc R . . H53B H -0.2034 0.6307 0.3899 0.377 Uiso 1 1 calc R . . H53C H -0.1906 0.6723 0.3280 0.377 Uiso 1 1 calc R . . C65 C 0.119(2) 0.4357(13) 0.4540(14) 0.419(18) Uani 1 1 d . . . H65A H 0.1105 0.3871 0.4367 0.629 Uiso 1 1 calc R . . H65B H 0.0562 0.4581 0.4541 0.629 Uiso 1 1 calc R . . H65C H 0.1518 0.4328 0.4961 0.629 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 0.0740(4) 0.0564(4) 0.0545(4) -0.0032(3) 0.0171(3) 0.0037(3) Ni2 0.0683(4) 0.0597(4) 0.0732(4) 0.0016(3) 0.0147(3) 0.0052(3) Cl1 0.1271(14) 0.0827(10) 0.0985(11) -0.0034(8) 0.0185(10) 0.0390(10) Cl2 0.1111(13) 0.0859(11) 0.1223(14) 0.0009(9) 0.0216(10) 0.0367(9) N1 0.054(2) 0.055(2) 0.060(2) -0.0022(18) 0.0159(18) -0.0054(18) N2 0.054(2) 0.057(2) 0.067(2) -0.0019(19) 0.0192(18) -0.0077(18) N3 0.076(3) 0.063(2) 0.049(2) -0.0009(19) 0.0135(19) 0.000(2) N4 0.080(3) 0.068(3) 0.063(3) -0.005(2) 0.023(2) 0.007(2) P1 0.0571(7) 0.0535(7) 0.0463(6) -0.0016(5) 0.0138(5) -0.0037(6) P2 0.0550(7) 0.0557(7) 0.0547(7) -0.0014(6) 0.0153(6) -0.0030(6) P3 0.0962(11) 0.0774(10) 0.0575(8) -0.0152(7) 0.0211(7) -0.0044(8) P4 0.0976(11) 0.0827(10) 0.0755(10) 0.0150(8) 0.0061(8) -0.0009(9) C10 0.061(3) 0.063(3) 0.073(3) -0.002(3) 0.017(3) -0.011(2) C11 0.089(4) 0.067(4) 0.164(7) 0.004(4) 0.049(4) -0.021(3) C12 0.087(4) 0.126(6) 0.104(5) 0.001(4) -0.003(4) -0.035(4) C13 0.072(4) 0.107(5) 0.116(5) -0.014(4) 0.045(3) -0.020(3) C20 0.060(3) 0.072(3) 0.081(4) 0.003(3) 0.020(3) -0.014(3) C21 0.075(4) 0.074(4) 0.140(6) 0.002(4) 0.014(4) -0.024(3) C22 0.109(5) 0.140(6) 0.122(6) -0.011(5) 0.066(5) -0.040(5) C23 0.065(4) 0.111(5) 0.141(6) 0.006(4) 0.006(4) -0.015(4) C30 0.094(4) 0.082(4) 0.051(3) 0.010(3) 0.006(3) 0.001(3) C31 0.176(7) 0.123(6) 0.053(3) 0.001(4) 0.016(4) 0.010(5) C32 0.145(6) 0.100(5) 0.081(4) 0.032(4) 0.018(4) -0.006(4) C33 0.092(5) 0.134(6) 0.098(5) 0.025(4) -0.021(4) 0.011(4) C40 0.107(5) 0.089(4) 0.070(4) -0.014(3) 0.027(3) 0.020(4) C41 0.133(6) 0.098(5) 0.099(5) -0.036(4) 0.022(4) -0.003(4) C42 0.148(7) 0.131(6) 0.124(6) -0.028(5) 0.082(5) 0.010(5) C43 0.197(8) 0.134(6) 0.060(4) -0.008(4) 0.020(4) 0.038(6) C50 0.147(7) 0.154(7) 0.063(4) -0.008(4) 0.034(4) -0.040(6) C51 0.123(7) 0.155(8) 0.137(7) -0.009(6) 0.061(6) -0.005(6) C52 0.141(8) 0.200(10) 0.166(9) -0.016(8) 0.084(7) -0.041(8) C54 0.140(6) 0.099(5) 0.069(4) -0.012(3) -0.012(4) 0.024(4) C55 0.180(9) 0.175(9) 0.079(5) -0.013(5) -0.012(5) 0.019(7) C56 0.199(10) 0.170(9) 0.117(7) -0.011(6) -0.062(7) 0.027(8) C57 0.265(14) 0.262(15) 0.130(9) 0.018(9) -0.081(9) -0.010(12) C58 0.091(4) 0.093(4) 0.114(5) -0.045(4) 0.021(4) 0.004(4) C59 0.095(5) 0.084(5) 0.176(8) -0.022(5) 0.014(5) -0.008(4) C61 0.126(8) 0.163(10) 0.45(2) -0.107(13) 0.071(11) -0.019(8) C62 0.186(8) 0.102(5) 0.091(5) 0.008(4) 0.054(5) 0.034(5) C63 0.284(14) 0.194(11) 0.100(6) 0.019(6) 0.079(8) 0.053(10) C66 0.103(5) 0.090(4) 0.119(5) 0.034(4) 0.029(4) 0.018(4) C67 0.109(5) 0.087(5) 0.149(7) 0.020(4) 0.041(5) -0.001(4) C68 0.126(7) 0.104(6) 0.249(12) 0.032(7) 0.039(7) -0.012(5) C69 0.144(8) 0.137(8) 0.256(13) 0.035(8) 0.036(8) -0.015(7) C70 0.150(8) 0.189(10) 0.099(6) 0.011(6) -0.005(6) -0.033(7) C71 0.123(7) 0.230(12) 0.140(8) -0.001(8) 0.008(6) -0.005(8) C72 0.100(7) 0.237(15) 0.288(16) -0.007(12) -0.035(9) -0.048(9) C73 0.237(19) 0.27(2) 0.52(4) -0.11(2) -0.11(2) 0.019(18) C60 0.123(8) 0.107(7) 0.46(2) -0.097(10) 0.094(11) -0.044(6) C64 0.47(3) 0.255(18) 0.178(11) 0.084(12) 0.221(16) 0.16(2) C53 0.246(16) 0.244(16) 0.294(19) 0.005(13) 0.144(15) -0.031(14) C65 0.42(3) 0.36(3) 0.53(5) 0.14(3) 0.24(3) -0.01(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 N3 1.939(4) . ? Ni1 P1 2.0759(13) . ? Ni1 P3 2.1551(16) . ? Ni1 Cl1 2.2001(16) . ? Ni2 N4 1.944(4) . ? Ni2 P2 2.0739(14) . ? Ni2 P4 2.1584(18) . ? Ni2 Cl2 2.1996(17) . ? N1 C10 1.500(6) . ? N1 P2 1.686(4) . ? N1 P1 1.695(4) . ? N2 C20 1.487(6) . ? N2 P1 1.689(4) . ? N2 P2 1.698(4) . ? N3 C30 1.475(6) . ? N3 P1 1.556(4) . ? N4 C40 1.473(7) . ? N4 P2 1.551(4) . ? P1 P2 2.5440(18) . ? P3 C58 1.823(6) . ? P3 C54 1.826(7) . ? P3 C50 1.840(7) . ? P4 C66 1.811(6) . ? P4 C62 1.816(7) . ? P4 C70 1.842(9) . ? C10 C12 1.512(8) . ? C10 C13 1.516(7) . ? C10 C11 1.521(7) . ? C20 C23 1.514(8) . ? C20 C22 1.516(8) . ? C20 C21 1.528(8) . ? C30 C33 1.509(8) . ? C30 C32 1.523(8) . ? C30 C31 1.535(8) . ? C40 C42 1.505(9) . ? C40 C41 1.521(9) . ? C40 C43 1.521(9) . ? C50 C51 1.439(10) . ? C51 C52 1.537(11) . ? C52 C53 1.386(15) . ? C54 C55 1.522(9) . ? C55 C56 1.492(12) . ? C56 C57 1.456(12) . ? C58 C59 1.477(9) . ? C59 C60 1.555(11) . ? C61 C60 1.231(13) . ? C62 C63 1.542(10) . ? C63 C64 1.549(18) . ? C66 C67 1.468(9) . ? C67 C68 1.552(10) . ? C68 C69 1.364(12) . ? C70 C71 1.355(11) . ? C71 C72 1.590(13) . ? C72 C73 1.340(19) . ? C64 C65 1.071(19) . ? 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 N3 Ni1 P1 45.44(12) . . ? N3 Ni1 P3 158.91(13) . . ? P1 Ni1 P3 113.76(6) . . ? N3 Ni1 Cl1 105.27(13) . . ? P1 Ni1 Cl1 150.58(6) . . ? P3 Ni1 Cl1 95.64(7) . . ? N4 Ni2 P2 45.27(12) . . ? N4 Ni2 P4 158.79(13) . . ? P2 Ni2 P4 113.91(6) . . ? N4 Ni2 Cl2 105.72(13) . . ? P2 Ni2 Cl2 150.83(7) . . ? P4 Ni2 Cl2 95.24(7) . . ? C10 N1 P2 132.3(3) . . ? C10 N1 P1 129.6(3) . . ? P2 N1 P1 97.61(19) . . ? C20 N2 P1 131.9(3) . . ? C20 N2 P2 130.1(3) . . ? P1 N2 P2 97.39(19) . . ? C30 N3 P1 149.0(4) . . ? C30 N3 Ni1 138.2(3) . . ? P1 N3 Ni1 71.95(15) . . ? C40 N4 P2 149.0(4) . . ? C40 N4 Ni2 137.9(4) . . ? P2 N4 Ni2 71.79(16) . . ? N3 P1 N2 126.4(2) . . ? N3 P1 N1 123.1(2) . . ? N2 P1 N1 82.31(18) . . ? N3 P1 Ni1 62.61(14) . . ? N2 P1 Ni1 133.00(14) . . ? N1 P1 Ni1 135.75(14) . . ? N3 P1 P2 142.20(15) . . ? N2 P1 P2 41.44(13) . . ? N1 P1 P2 41.06(13) . . ? Ni1 P1 P2 155.19(6) . . ? N4 P2 N1 126.9(2) . . ? N4 P2 N2 122.6(2) . . ? N1 P2 N2 82.32(18) . . ? N4 P2 Ni2 62.94(16) . . ? N1 P2 Ni2 133.35(14) . . ? N2 P2 Ni2 135.09(15) . . ? N4 P2 P1 142.22(17) . . ? N1 P2 P1 41.33(13) . . ? N2 P2 P1 41.17(13) . . ? Ni2 P2 P1 154.82(7) . . ? C58 P3 C54 102.8(3) . . ? C58 P3 C50 106.6(3) . . ? C54 P3 C50 102.2(4) . . ? C58 P3 Ni1 114.9(3) . . ? C54 P3 Ni1 115.7(2) . . ? C50 P3 Ni1 113.3(2) . . ? C66 P4 C62 102.9(3) . . ? C66 P4 C70 106.6(4) . . ? C62 P4 C70 100.3(5) . . ? C66 P4 Ni2 114.2(3) . . ? C62 P4 Ni2 116.0(2) . . ? C70 P4 Ni2 115.2(3) . . ? N1 C10 C12 108.9(4) . . ? N1 C10 C13 109.2(4) . . ? C12 C10 C13 109.7(5) . . ? N1 C10 C11 108.8(4) . . ? C12 C10 C11 109.6(5) . . ? C13 C10 C11 110.5(5) . . ? N2 C20 C23 109.2(4) . . ? N2 C20 C22 108.7(5) . . ? C23 C20 C22 110.8(5) . . ? N2 C20 C21 108.7(4) . . ? C23 C20 C21 109.8(5) . . ? C22 C20 C21 109.7(5) . . ? N3 C30 C33 108.9(5) . . ? N3 C30 C32 107.9(5) . . ? C33 C30 C32 109.7(5) . . ? N3 C30 C31 108.3(5) . . ? C33 C30 C31 112.2(5) . . ? C32 C30 C31 109.8(5) . . ? N4 C40 C42 109.2(5) . . ? N4 C40 C41 108.7(5) . . ? C42 C40 C41 109.0(5) . . ? N4 C40 C43 108.2(5) . . ? C42 C40 C43 111.3(6) . . ? C41 C40 C43 110.4(6) . . ? C51 C50 P3 116.2(6) . . ? C50 C51 C52 112.5(8) . . ? C53 C52 C51 113.3(11) . . ? C55 C54 P3 118.3(5) . . ? C56 C55 C54 113.5(7) . . ? C57 C56 C55 115.9(10) . . ? C59 C58 P3 114.3(4) . . ? C58 C59 C60 109.6(7) . . ? C63 C62 P4 119.1(6) . . ? C62 C63 C64 112.5(10) . . ? C67 C66 P4 115.1(5) . . ? C66 C67 C68 111.2(7) . . ? C69 C68 C67 114.9(9) . . ? C71 C70 P4 117.9(8) . . ? C70 C71 C72 113.4(10) . . ? C73 C72 C71 111.3(14) . . ? C61 C60 C59 119.5(11) . . ? C65 C64 C63 125(2) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.365 _refine_diff_density_min -0.540 _refine_diff_density_rms 0.081