# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author ; R.A. Fischer Lehrstuhl fuer Anorganische Chemie II Ruhr-Universitaet Bochum Universitaetsstrasse 150 44780 Bochum (Germany) ; _publ_contact_author_phone '049 234 32-24174' _publ_contact_author_fax '049 234 321-4174' _publ_contact_author_email roland.fischer@ruhr-uni-bochum.de #============================================================================== # 2. TITLE AND AUTHOR LIST _publ_section_title ; First Dinuclear Copper/Gallium Complexes: Supporting Cu(0) and Cu(I) Centres by Low Valent Organogallium Ligands ; loop_ _publ_author_name _publ_author_address 'Mariusz Molon' ; Lehrstuhl fuer Anorganische Chemie II Ruhr-Universitaet Bochum Universitaetsstrasse 150 44780 Bochum (Germany) ; 'Timo Bollermann' ; Lehrstuhl fuer Anorganische Chemie II Ruhr-Universitaet Bochum Universitaetsstrasse 150 44780 Bochum (Germany) ; 'Christian Gemel' ; Lehrstuhl fuer Anorganische Chemie II Ruhr-Universitaet Bochum Universitaetsstrasse 150 44780 Bochum (Germany) ; 'Roland A. Fischer' ; Lehrstuhl fuer Anorganische Chemie II Ruhr-Universitaet Bochum Universitaetsstrasse 150 44780 Bochum (Germany) ; _publ_contact_author_name 'R.A. Fischer' #============================================================================== data_Mo(GaCpstar)2(PMe3)4 _database_code_depnum_ccdc_archive 'CCDC 820859' #TrackingRef '- alle_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _space_group_name_Hall 'P 2ac 2ab ' _chemical_formula_moiety 'C12 H36 Ga2 Mo P4, 2(C10 H15)' _chemical_formula_sum 'C32 H66 Ga2 Mo P4' _chemical_formula_weight 810.11 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.6503(2) _cell_length_b 14.6989(4) _cell_length_c 23.1578(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3965.69(15) _cell_formula_units_Z 4 _cell_measurement_temperature 111(2) _cell_measurement_reflns_used 200 _cell_measurement_theta_min 3.17 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.357 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1688 _exptl_absorpt_coefficient_mu 1.841 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.580 _exptl_absorpt_correction_T_max 0.690 _exptl_absorpt_process_details abspack _exptl_special_details ; ; _diffrn_ambient_temperature 111(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 'Xcalibur, Sapphire2, large Be window' _diffrn_measurement_method '560 images at 1.0 deg. in \w and 20 sec.' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 29247 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6978 _reflns_number_gt 5668 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 171_33_34d, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 171_33_34d, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 171_33_34d, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _refine_special_details ; It was not possible to refine the molecular structure reasonably in the Pnma space group since R1 values of >0.1 resulted. Therefore the structe refinement was done in P 21 21 21 since we think the morrorplate in the molecule is not ideal resulting in a inversion twin. Severally disoerdered cocrystallized solvent molecules have been omited from the diffration data and were not taken into account by the structure refinement. 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^)+(0.0344P)^2^+0.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.462(11) _refine_ls_number_reflns 6978 _refine_ls_number_parameters 400 _refine_ls_number_restraints 81 _refine_ls_R_factor_all 0.0410 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_ref 0.0635 _refine_ls_wR_factor_gt 0.0600 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 1.014 _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 Mo1 Mo 0.19201(2) 0.50804(2) 0.140219(10) 0.01519(7) Uani 1 1 d D A . Ga1 Ga 0.21153(3) 0.49939(3) 0.033682(13) 0.02084(9) Uani 1 1 d . . . Ga2 Ga 0.40495(3) 0.51043(4) 0.144775(15) 0.02213(11) Uani 1 1 d . . . P1 P -0.01616(6) 0.50696(10) 0.13914(3) 0.0183(2) Uani 1 1 d . . . P2 P 0.20063(8) 0.51536(9) 0.24463(3) 0.0352(3) Uani 1 1 d D . . P3 P 0.18987(12) 0.34194(6) 0.13740(5) 0.0235(2) Uani 1 1 d . . . P4 P 0.18676(12) 0.67281(6) 0.12672(4) 0.0239(2) Uani 1 1 d . . . C1 C 0.3219(3) 0.4917(3) -0.05184(12) 0.0243(8) Uani 1 1 d . . . C2 C 0.2521(4) 0.4128(3) -0.05307(19) 0.0223(11) Uani 1 1 d . . . C3 C 0.1358(5) 0.4413(3) -0.06049(19) 0.0239(11) Uani 1 1 d . . . C4 C 0.1354(4) 0.5380(3) -0.06322(18) 0.0189(10) Uani 1 1 d . . . C5 C 0.2502(4) 0.5688(3) -0.05807(19) 0.0247(12) Uani 1 1 d . . . C6 C 0.4504(3) 0.4912(4) -0.05014(15) 0.0403(11) Uani 1 1 d . . . H6A H 0.4804 0.5241 -0.0837 0.060 Uiso 1 1 calc R . . H6B H 0.4781 0.4282 -0.0510 0.060 Uiso 1 1 calc R . . H6C H 0.4768 0.5208 -0.0146 0.060 Uiso 1 1 calc R . . C7 C 0.2953(6) 0.3166(2) -0.05291(18) 0.0383(11) Uani 1 1 d . . . H7A H 0.2392 0.2773 -0.0336 0.057 Uiso 1 1 calc R . . H7B H 0.3686 0.3137 -0.0322 0.057 Uiso 1 1 calc R . . H7C H 0.3062 0.2959 -0.0928 0.057 Uiso 1 1 calc R . . C8 C 0.0351(4) 0.3801(3) -0.0679(2) 0.0331(12) Uani 1 1 d . . . H8A H 0.0333 0.3571 -0.1076 0.050 Uiso 1 1 calc R . . H8B H -0.0356 0.4140 -0.0600 0.050 Uiso 1 1 calc R . . H8C H 0.0412 0.3289 -0.0410 0.050 Uiso 1 1 calc R . . C9 C 0.0314(4) 0.5956(3) -0.07491(19) 0.0325(12) Uani 1 1 d . . . H9A H 0.0439 0.6570 -0.0596 0.049 Uiso 1 1 calc R . . H9B H -0.0357 0.5685 -0.0561 0.049 Uiso 1 1 calc R . . H9C H 0.0181 0.5990 -0.1166 0.049 Uiso 1 1 calc R . . C10 C 0.2909(5) 0.6650(3) -0.06438(17) 0.0357(11) Uani 1 1 d . . . H10A H 0.3517 0.6770 -0.0362 0.054 Uiso 1 1 calc R . . H10B H 0.2267 0.7067 -0.0576 0.054 Uiso 1 1 calc R . . H10C H 0.3209 0.6742 -0.1035 0.054 Uiso 1 1 calc R . . C11 C 0.5785(3) 0.5207(4) 0.21364(16) 0.0506(15) Uani 1 1 d . . . C12 C 0.5838(4) 0.4393(4) 0.1827(3) 0.0487(16) Uani 1 1 d . . . C13 C 0.5906(4) 0.4591(3) 0.12300(18) 0.0219(9) Uani 1 1 d . . . C14 C 0.5911(4) 0.5559(3) 0.11779(18) 0.0215(9) Uani 1 1 d . . . C15 C 0.5822(4) 0.5924(3) 0.1745(2) 0.0323(11) Uani 1 1 d . . . C16 C 0.5827(4) 0.5300(7) 0.27842(18) 0.133(4) Uani 1 1 d . . . H16A H 0.6600 0.5484 0.2903 0.200 Uiso 1 1 calc R . . H16B H 0.5635 0.4715 0.2963 0.200 Uiso 1 1 calc R . . H16C H 0.5272 0.5761 0.2908 0.200 Uiso 1 1 calc R . . C17 C 0.5908(5) 0.3453(4) 0.2091(3) 0.102(3) Uani 1 1 d . . . H17A H 0.6662 0.3370 0.2270 0.153 Uiso 1 1 calc R . . H17B H 0.5798 0.2994 0.1789 0.153 Uiso 1 1 calc R . . H17C H 0.5307 0.3386 0.2384 0.153 Uiso 1 1 calc R . . C18 C 0.6106(5) 0.3933(3) 0.0749(3) 0.0543(17) Uani 1 1 d . . . H18A H 0.6521 0.3402 0.0897 0.081 Uiso 1 1 calc R . . H18B H 0.6561 0.4227 0.0446 0.081 Uiso 1 1 calc R . . H18C H 0.5367 0.3739 0.0590 0.081 Uiso 1 1 calc R . . C19 C 0.6101(5) 0.6104(3) 0.0644(2) 0.0395(13) Uani 1 1 d . . . H19A H 0.6044 0.5707 0.0306 0.059 Uiso 1 1 calc R . . H19B H 0.6866 0.6380 0.0657 0.059 Uiso 1 1 calc R . . H19C H 0.5519 0.6583 0.0619 0.059 Uiso 1 1 calc R . . C20 C 0.5917(5) 0.6919(3) 0.1884(3) 0.0706(19) Uani 1 1 d . . . H20A H 0.5420 0.7063 0.2213 0.106 Uiso 1 1 calc R . . H20B H 0.5679 0.7278 0.1549 0.106 Uiso 1 1 calc R . . H20C H 0.6714 0.7065 0.1982 0.106 Uiso 1 1 calc R . . C21 C 0.3014(10) 0.6073(7) 0.2737(4) 0.042(3) Uani 0.498(12) 1 d PDU A 1 H21A H 0.2707 0.6675 0.2640 0.063 Uiso 0.498(12) 1 calc PR A 1 H21B H 0.3775 0.6001 0.2562 0.063 Uiso 0.498(12) 1 calc PR A 1 H21C H 0.3077 0.6015 0.3157 0.063 Uiso 0.498(12) 1 calc PR A 1 C22 C 0.0783(8) 0.5624(10) 0.2891(4) 0.057(5) Uani 0.498(12) 1 d PDU A 1 H22A H 0.0418 0.6126 0.2682 0.086 Uiso 0.498(12) 1 calc PR A 1 H22B H 0.1078 0.5846 0.3261 0.086 Uiso 0.498(12) 1 calc PR A 1 H22C H 0.0217 0.5143 0.2960 0.086 Uiso 0.498(12) 1 calc PR A 1 C23 C 0.2503(13) 0.4257(8) 0.2897(5) 0.056(4) Uani 0.498(12) 1 d PDU A 1 H23A H 0.3161 0.3958 0.2713 0.083 Uiso 0.498(12) 1 calc PR A 1 H23B H 0.1886 0.3813 0.2953 0.083 Uiso 0.498(12) 1 calc PR A 1 H23C H 0.2736 0.4505 0.3271 0.083 Uiso 0.498(12) 1 calc PR A 1 C21' C 0.2341(13) 0.6132(7) 0.2856(5) 0.053(4) Uani 0.502(12) 1 d PDU A 2 H21D H 0.3003 0.6442 0.2684 0.080 Uiso 0.502(12) 1 calc PR A 2 H21E H 0.2525 0.5954 0.3253 0.080 Uiso 0.502(12) 1 calc PR A 2 H21F H 0.1680 0.6545 0.2858 0.080 Uiso 0.502(12) 1 calc PR A 2 C22' C 0.0758(7) 0.4720(8) 0.2897(4) 0.038(3) Uani 0.502(12) 1 d PDU A 2 H22D H 0.0461 0.4157 0.2728 0.057 Uiso 0.502(12) 1 calc PR A 2 H22E H 0.0149 0.5180 0.2904 0.057 Uiso 0.502(12) 1 calc PR A 2 H22F H 0.1021 0.4602 0.3292 0.057 Uiso 0.502(12) 1 calc PR A 2 C23' C 0.3067(10) 0.4343(8) 0.2795(5) 0.035(3) Uani 0.502(12) 1 d PDU A 2 H23D H 0.2996 0.3741 0.2617 0.052 Uiso 0.502(12) 1 calc PR A 2 H23E H 0.2905 0.4297 0.3209 0.052 Uiso 0.502(12) 1 calc PR A 2 H23F H 0.3849 0.4572 0.2738 0.052 Uiso 0.502(12) 1 calc PR A 2 C24 C 0.1427(5) 0.2681(3) 0.1981(2) 0.0493(15) Uani 1 1 d . A . H24A H 0.0687 0.2897 0.2128 0.074 Uiso 1 1 calc R . . H24B H 0.1999 0.2702 0.2291 0.074 Uiso 1 1 calc R . . H24C H 0.1345 0.2053 0.1844 0.074 Uiso 1 1 calc R . . C25 C 0.3247(5) 0.2816(3) 0.1211(3) 0.0642(18) Uani 1 1 d . A . H25A H 0.3853 0.3030 0.1471 0.096 Uiso 1 1 calc R . . H25B H 0.3471 0.2936 0.0810 0.096 Uiso 1 1 calc R . . H25C H 0.3135 0.2161 0.1265 0.096 Uiso 1 1 calc R . . C26 C 0.1024(4) 0.2862(3) 0.0818(2) 0.0357(12) Uani 1 1 d . A . H26A H 0.1298 0.3043 0.0434 0.054 Uiso 1 1 calc R . . H26B H 0.0220 0.3044 0.0863 0.054 Uiso 1 1 calc R . . H26C H 0.1087 0.2200 0.0859 0.054 Uiso 1 1 calc R . . C27 C 0.3194(5) 0.7329(3) 0.1067(2) 0.0535(15) Uani 1 1 d . A . H27A H 0.3015 0.7964 0.0975 0.080 Uiso 1 1 calc R . . H27B H 0.3537 0.7035 0.0728 0.080 Uiso 1 1 calc R . . H27C H 0.3736 0.7307 0.1390 0.080 Uiso 1 1 calc R . . C28 C 0.1386(5) 0.7552(3) 0.1822(2) 0.0495(15) Uani 1 1 d . A . H28A H 0.1908 0.7530 0.2154 0.074 Uiso 1 1 calc R . . H28B H 0.0608 0.7395 0.1949 0.074 Uiso 1 1 calc R . . H28C H 0.1387 0.8167 0.1658 0.074 Uiso 1 1 calc R . . C29 C 0.0977(4) 0.7184(3) 0.06753(19) 0.0313(11) Uani 1 1 d . A . H29A H 0.0177 0.7000 0.0733 0.047 Uiso 1 1 calc R . . H29B H 0.1254 0.6944 0.0306 0.047 Uiso 1 1 calc R . . H29C H 0.1028 0.7849 0.0673 0.047 Uiso 1 1 calc R . . C30 C -0.0990(5) 0.4159(3) 0.1755(2) 0.0403(13) Uani 1 1 d . . . H30A H -0.0762 0.4125 0.2161 0.060 Uiso 1 1 calc R . . H30B H -0.0835 0.3576 0.1566 0.060 Uiso 1 1 calc R . . H30C H -0.1812 0.4296 0.1729 0.060 Uiso 1 1 calc R . . C31 C -0.0988(5) 0.6014(3) 0.1700(2) 0.0358(12) Uani 1 1 d . . . H31A H -0.0775 0.6582 0.1506 0.054 Uiso 1 1 calc R . . H31B H -0.0820 0.6064 0.2114 0.054 Uiso 1 1 calc R . . H31C H -0.1809 0.5900 0.1646 0.054 Uiso 1 1 calc R . . C32 C -0.0894(2) 0.5010(3) 0.06883(13) 0.0320(8) Uani 1 1 d . . . H32A H -0.1724 0.4956 0.0749 0.048 Uiso 1 1 calc R . . H32B H -0.0617 0.4479 0.0474 0.048 Uiso 1 1 calc R . . H32C H -0.0732 0.5564 0.0467 0.048 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 Mo1 0.00971(12) 0.02427(16) 0.01158(12) 0.00017(16) 0.00002(10) 0.00043(19) Ga1 0.02080(17) 0.0292(2) 0.01253(16) -0.00089(19) 0.00108(14) -0.0015(3) Ga2 0.01071(17) 0.0327(3) 0.02296(19) 0.0008(3) -0.00033(14) -0.0003(2) P1 0.0112(4) 0.0264(6) 0.0175(4) 0.0010(7) 0.0006(3) 0.0003(5) P2 0.0210(4) 0.0721(8) 0.0126(4) -0.0025(5) 0.0002(4) 0.0038(8) P3 0.0153(6) 0.0256(5) 0.0296(5) 0.0037(4) -0.0014(6) 0.0008(5) P4 0.0182(6) 0.0256(5) 0.0279(6) -0.0012(4) -0.0001(5) -0.0010(5) C1 0.0211(17) 0.038(2) 0.0142(15) -0.0051(19) 0.0034(12) -0.001(2) C2 0.020(3) 0.031(3) 0.016(2) -0.0036(18) -0.0005(18) -0.0021(18) C3 0.031(3) 0.030(3) 0.011(2) -0.0051(19) 0.0009(19) -0.005(2) C4 0.017(2) 0.031(3) 0.009(2) 0.0032(17) -0.0013(17) 0.0025(18) C5 0.038(3) 0.026(2) 0.010(2) 0.0019(17) -0.0013(19) -0.0074(19) C6 0.0242(18) 0.070(3) 0.0268(19) -0.008(3) 0.0013(14) -0.002(3) C7 0.045(3) 0.035(2) 0.035(2) -0.0192(18) -0.004(3) 0.011(3) C8 0.026(3) 0.045(3) 0.029(3) -0.007(2) -0.010(2) -0.006(2) C9 0.033(3) 0.044(3) 0.020(3) 0.004(2) -0.003(2) 0.006(2) C10 0.043(3) 0.039(2) 0.025(2) 0.0085(18) 0.004(2) -0.009(3) C11 0.0138(19) 0.117(5) 0.020(2) 0.007(3) -0.0021(17) -0.010(3) C12 0.016(3) 0.061(4) 0.070(4) 0.045(3) -0.007(3) -0.005(3) C13 0.010(2) 0.020(2) 0.036(2) -0.0006(17) -0.0008(19) 0.0004(16) C14 0.012(2) 0.024(2) 0.029(2) 0.0019(18) -0.0010(19) 0.0010(18) C15 0.009(2) 0.054(3) 0.035(3) -0.015(2) 0.000(2) -0.003(2) C16 0.033(3) 0.347(13) 0.019(2) 0.023(5) -0.005(2) -0.036(6) C17 0.027(3) 0.100(5) 0.178(7) 0.120(5) 0.001(4) 0.002(3) C18 0.012(3) 0.036(3) 0.115(5) -0.035(3) -0.004(3) 0.002(2) C19 0.037(4) 0.043(3) 0.038(3) 0.017(2) 0.004(2) -0.007(2) C20 0.028(3) 0.074(4) 0.110(5) -0.065(4) 0.002(3) -0.008(3) C21 0.029(7) 0.085(8) 0.012(5) -0.018(4) -0.006(5) 0.015(7) C22 0.025(6) 0.133(14) 0.014(5) -0.023(6) 0.008(4) -0.012(7) C23 0.068(11) 0.080(9) 0.019(6) 0.016(6) -0.008(7) -0.015(8) C21' 0.078(12) 0.064(7) 0.016(5) -0.017(5) -0.008(7) 0.014(7) C22' 0.030(5) 0.066(9) 0.018(4) -0.004(4) 0.004(4) -0.006(5) C23' 0.036(7) 0.054(6) 0.014(5) 0.018(4) -0.002(5) -0.019(6) C24 0.075(4) 0.033(3) 0.040(3) 0.018(2) -0.007(3) 0.000(2) C25 0.033(4) 0.030(3) 0.130(5) -0.026(3) 0.004(3) 0.006(2) C26 0.031(3) 0.034(3) 0.043(3) 0.005(2) 0.001(2) -0.014(2) C27 0.017(3) 0.044(3) 0.099(4) 0.029(3) -0.002(3) -0.008(2) C28 0.075(4) 0.035(3) 0.039(3) -0.014(2) -0.010(3) 0.000(2) C29 0.034(3) 0.027(2) 0.032(3) 0.0014(19) -0.002(2) 0.008(2) C30 0.023(3) 0.045(3) 0.053(3) 0.003(2) 0.013(3) 0.001(2) C31 0.021(3) 0.045(3) 0.042(3) -0.011(2) 0.012(2) 0.005(2) C32 0.0137(16) 0.055(3) 0.0277(18) -0.004(3) -0.0024(13) 0.001(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 Mo1 P2 2.4225(8) . ? Mo1 P1 2.4255(8) . ? Mo1 P3 2.4426(10) . ? Mo1 P4 2.4427(10) . ? Mo1 Ga1 2.4809(4) . ? Mo1 Ga2 2.4833(4) . ? Ga1 C1 2.364(3) . ? Ga1 C5 2.400(4) . ? Ga1 C2 2.425(4) . ? Ga1 C4 2.479(4) . ? Ga1 C3 2.503(5) . ? Ga2 C13 2.346(4) . ? Ga2 C14 2.353(4) . ? Ga2 C15 2.488(5) . ? Ga2 C12 2.492(5) . ? P1 C31 1.834(4) . ? P1 C32 1.840(3) . ? P1 C30 1.852(5) . ? P2 C21' 1.766(8) . ? P2 C23 1.778(9) . ? P2 C22 1.889(8) . ? P2 C23' 1.897(9) . ? P2 C22' 1.900(7) . ? P2 C21 1.913(9) . ? P3 C26 1.836(5) . ? P3 C25 1.843(5) . ? P3 C24 1.859(5) . ? P4 C27 1.839(5) . ? P4 C29 1.845(4) . ? P4 C28 1.853(5) . ? C1 C5 1.415(6) . ? C1 C2 1.416(5) . ? C1 C6 1.497(4) . ? C2 C3 1.429(6) . ? C2 C7 1.501(6) . ? C3 C4 1.423(5) . ? C3 C8 1.488(6) . ? C4 C5 1.417(6) . ? C4 C9 1.504(6) . ? C5 C10 1.499(6) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C15 1.391(7) . ? C11 C12 1.396(7) . ? C11 C16 1.507(5) . ? C12 C13 1.415(6) . ? C12 C17 1.512(6) . ? C13 C14 1.428(4) . ? C13 C18 1.493(6) . ? C14 C15 1.423(6) . ? C14 C19 1.489(6) . ? C15 C20 1.501(6) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C21' H21D 0.9800 . ? C21' H21E 0.9800 . ? C21' H21F 0.9800 . ? C22' H22D 0.9800 . ? C22' H22E 0.9800 . ? C22' H22F 0.9800 . ? C23' H23D 0.9800 . ? C23' H23E 0.9800 . ? C23' H23F 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? 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 P2 Mo1 P1 92.98(3) . . ? P2 Mo1 P3 94.10(4) . . ? P1 Mo1 P3 89.02(5) . . ? P2 Mo1 P4 94.86(4) . . ? P1 Mo1 P4 88.86(5) . . ? P3 Mo1 P4 170.89(3) . . ? P2 Mo1 Ga1 172.35(3) . . ? P1 Mo1 Ga1 94.65(2) . . ? P3 Mo1 Ga1 85.59(3) . . ? P4 Mo1 Ga1 85.75(3) . . ? P2 Mo1 Ga2 85.15(3) . . ? P1 Mo1 Ga2 178.10(2) . . ? P3 Mo1 Ga2 91.46(4) . . ? P4 Mo1 Ga2 90.94(4) . . ? Ga1 Mo1 Ga2 87.214(14) . . ? C1 Ga1 C5 34.56(14) . . ? C1 Ga1 C2 34.37(13) . . ? C5 Ga1 C2 56.83(13) . . ? C1 Ga1 C4 56.44(13) . . ? C5 Ga1 C4 33.73(13) . . ? C2 Ga1 C4 55.92(14) . . ? C1 Ga1 Mo1 152.31(7) . . ? C5 Ga1 Mo1 151.16(11) . . ? C2 Ga1 Mo1 150.32(11) . . ? C4 Ga1 Mo1 148.84(10) . . ? C1 Ga1 C3 56.32(15) . . ? C5 Ga1 C3 55.93(17) . . ? C2 Ga1 C3 33.66(14) . . ? C4 Ga1 C3 33.19(12) . . ? Mo1 Ga1 C3 148.39(11) . . ? C13 Ga2 C14 35.38(11) . . ? C13 Ga2 Mo1 155.16(11) . . ? C14 Ga2 Mo1 155.95(10) . . ? C13 Ga2 C15 56.63(14) . . ? C14 Ga2 C15 34.03(13) . . ? Mo1 Ga2 C15 147.97(11) . . ? C13 Ga2 C12 33.86(16) . . ? C14 Ga2 C12 56.10(15) . . ? Mo1 Ga2 C12 147.61(11) . . ? C15 Ga2 C12 53.95(15) . . ? C31 P1 C32 97.9(2) . . ? C31 P1 C30 95.51(17) . . ? C32 P1 C30 97.2(2) . . ? C31 P1 Mo1 121.04(18) . . ? C32 P1 Mo1 118.24(10) . . ? C30 P1 Mo1 121.42(18) . . ? C21' P2 C23 102.6(6) . . ? C21' P2 C22 64.9(5) . . ? C23 P2 C22 101.4(5) . . ? C21' P2 C23' 98.0(5) . . ? C23 P2 C23' 22.0(5) . . ? C22 P2 C23' 119.3(5) . . ? C21' P2 C22' 98.4(5) . . ? C23 P2 C22' 71.2(5) . . ? C22 P2 C22' 41.0(4) . . ? C23' P2 C22' 93.1(4) . . ? C21' P2 C21 25.9(5) . . ? C23 P2 C21 96.8(5) . . ? C22 P2 C21 90.7(4) . . ? C23' P2 C21 83.9(5) . . ? C22' P2 C21 120.9(4) . . ? C21' P2 Mo1 125.5(4) . . ? C23 P2 Mo1 124.5(5) . . ? C22 P2 Mo1 121.9(3) . . ? C23' P2 Mo1 115.1(4) . . ? C22' P2 Mo1 120.1(3) . . ? C21 P2 Mo1 114.1(3) . . ? C26 P3 C25 96.6(2) . . ? C26 P3 C24 96.1(2) . . ? C25 P3 C24 97.2(3) . . ? C26 P3 Mo1 118.08(16) . . ? C25 P3 Mo1 118.55(17) . . ? C24 P3 Mo1 124.52(16) . . ? C27 P4 C29 96.3(2) . . ? C27 P4 C28 96.7(3) . . ? C29 P4 C28 96.2(2) . . ? C27 P4 Mo1 119.15(18) . . ? C29 P4 Mo1 117.98(15) . . ? C28 P4 Mo1 124.53(17) . . ? C5 C1 C2 108.3(3) . . ? C5 C1 C6 126.6(4) . . ? C2 C1 C6 124.8(4) . . ? C5 C1 Ga1 74.1(2) . . ? C2 C1 Ga1 75.2(2) . . ? C6 C1 Ga1 121.5(2) . . ? C1 C2 C3 107.9(4) . . ? C1 C2 C7 125.4(4) . . ? C3 C2 C7 126.4(4) . . ? C1 C2 Ga1 70.5(2) . . ? C3 C2 Ga1 76.2(3) . . ? C7 C2 Ga1 123.9(3) . . ? C4 C3 C2 107.5(5) . . ? C4 C3 C8 126.6(5) . . ? C2 C3 C8 125.8(4) . . ? C4 C3 Ga1 72.5(3) . . ? C2 C3 Ga1 70.2(3) . . ? C8 C3 Ga1 125.8(3) . . ? C5 C4 C3 108.2(5) . . ? C5 C4 C9 126.5(4) . . ? C3 C4 C9 125.0(5) . . ? C5 C4 Ga1 70.1(3) . . ? C3 C4 Ga1 74.3(3) . . ? C9 C4 Ga1 125.5(3) . . ? C1 C5 C4 108.0(4) . . ? C1 C5 C10 125.4(4) . . ? C4 C5 C10 126.3(4) . . ? C1 C5 Ga1 71.4(2) . . ? C4 C5 Ga1 76.2(3) . . ? C10 C5 Ga1 123.2(3) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C15 C11 C12 108.3(3) . . ? C15 C11 C16 125.3(6) . . ? C12 C11 C16 126.0(6) . . ? C11 C12 C13 109.1(4) . . ? C11 C12 C17 125.3(5) . . ? C13 C12 C17 125.4(6) . . ? C11 C12 Ga2 77.5(3) . . ? C13 C12 Ga2 67.4(3) . . ? C17 C12 Ga2 124.8(4) . . ? C12 C13 C14 106.7(4) . . ? C12 C13 C18 127.2(4) . . ? C14 C13 C18 125.6(4) . . ? C12 C13 Ga2 78.7(3) . . ? C14 C13 Ga2 72.6(3) . . ? C18 C13 Ga2 120.8(3) . . ? C15 C14 C13 107.3(4) . . ? C15 C14 C19 125.0(4) . . ? C13 C14 C19 127.4(4) . . ? C15 C14 Ga2 78.2(3) . . ? C13 C14 Ga2 72.0(3) . . ? C19 C14 Ga2 120.7(3) . . ? C11 C15 C14 108.5(4) . . ? C11 C15 C20 126.9(5) . . ? C14 C15 C20 124.1(4) . . ? C11 C15 Ga2 77.7(3) . . ? C14 C15 Ga2 67.8(3) . . ? C20 C15 Ga2 126.3(3) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? P2 C21 H21A 109.5 . . ? P2 C21 H21B 109.5 . . ? P2 C21 H21C 109.5 . . ? P2 C22 H22A 109.5 . . ? P2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? P2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? P2 C23 H23A 109.5 . . ? P2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? P2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? P2 C21' H21D 109.5 . . ? P2 C21' H21E 109.5 . . ? H21D C21' H21E 109.5 . . ? P2 C21' H21F 109.5 . . ? H21D C21' H21F 109.5 . . ? H21E C21' H21F 109.5 . . ? P2 C22' H22D 109.5 . . ? P2 C22' H22E 109.5 . . ? H22D C22' H22E 109.5 . . ? P2 C22' H22F 109.5 . . ? H22D C22' H22F 109.5 . . ? H22E C22' H22F 109.5 . . ? P2 C23' H23D 109.5 . . ? P2 C23' H23E 109.5 . . ? H23D C23' H23E 109.5 . . ? P2 C23' H23F 109.5 . . ? H23D C23' H23F 109.5 . . ? H23E C23' H23F 109.5 . . ? P3 C24 H24A 109.5 . . ? P3 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? P3 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? P3 C25 H25A 109.5 . . ? P3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? P3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? P3 C26 H26A 109.5 . . ? P3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? P3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? P4 C27 H27A 109.5 . . ? P4 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? P4 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? P4 C28 H28A 109.5 . . ? P4 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? P4 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? P4 C29 H29A 109.5 . . ? P4 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? P4 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? P1 C30 H30A 109.5 . . ? P1 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? P1 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? P1 C31 H31A 109.5 . . ? P1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? P1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? P1 C32 H32A 109.5 . . ? P1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? P1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.783 _refine_diff_density_min -0.324 _refine_diff_density_rms 0.074 data_Ni(GaCpstar)2(PPh3)2 _database_code_depnum_ccdc_archive 'CCDC 820860' #TrackingRef '- alle_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _space_group_name_Hall '-P 2ybc' _chemical_formula_moiety 'C36 H30 Ga2 Ni P2, 2(C10 H15)' _chemical_formula_sum 'C56 H60 Ga2 Ni P2' _chemical_formula_weight 993.13 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' P P 0.1023 0.0942 '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' Ga Ga 0.2307 1.6083 '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 21/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 16.5596(10) _cell_length_b 15.2068(8) _cell_length_c 23.3095(15) _cell_angle_alpha 90.00 _cell_angle_beta 101.783(6) _cell_angle_gamma 90.00 _cell_volume 5746.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 200 _cell_measurement_theta_min 2.85 _cell_measurement_theta_max 25.00 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.148 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064 _exptl_absorpt_coefficient_mu 1.342 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7752 _exptl_absorpt_correction_T_max 0.9737 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '560 images at 1.0 deg. in \w and 25 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21121 _diffrn_reflns_av_R_equivalents 0.1143 _diffrn_reflns_av_sigmaI/netI 0.2236 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10110 _reflns_number_gt 4900 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 1.171.13, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _refine_special_details ; Due to poor diffracting properties of several mounted crystals the Rint value is higher than 0.1 Several tries to obtain a better crystal quality failed. It was possible to refine the molecular structure in an acceptable way in P 21/c only. Severally disordered cocrystallized solvent molecules have been omited from the diffration data and were not taken into account by the structure refinement. 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^)+(0.0660P)^2^+0.0000P] 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 10110 _refine_ls_number_parameters 550 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.1575 _refine_ls_R_factor_gt 0.0844 _refine_ls_wR_factor_ref 0.1975 _refine_ls_wR_factor_gt 0.1697 _refine_ls_goodness_of_fit_ref 0.919 _refine_ls_restrained_S_all 0.916 _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 0.22866(6) 0.23576(7) 0.34558(5) 0.0186(3) Uani 1 1 d . . . Ga1 Ga 0.19937(6) 0.12979(6) 0.40549(4) 0.0221(3) Uani 1 1 d . . . Ga2 Ga 0.31372(5) 0.16937(6) 0.29476(4) 0.0238(3) Uani 1 1 d . . . P1 P 0.30363(13) 0.32534(15) 0.40406(10) 0.0205(5) Uani 1 1 d . . . P2 P 0.11953(12) 0.27212(14) 0.28405(9) 0.0172(5) Uani 1 1 d . . . C1 C 0.2348(5) -0.0031(6) 0.4549(4) 0.0270(10) Uani 1 1 d U . . C2 C 0.2314(5) 0.0605(6) 0.4992(4) 0.0272(10) Uani 1 1 d U . . C3 C 0.1494(5) 0.0901(6) 0.4910(4) 0.0271(10) Uani 1 1 d U . . C4 C 0.1016(5) 0.0464(5) 0.4437(4) 0.0268(10) Uani 1 1 d U . . C5 C 0.1540(5) -0.0128(5) 0.4190(4) 0.0270(10) Uani 1 1 d U . . C6 C 0.3097(5) -0.0519(6) 0.4456(4) 0.038(3) Uani 1 1 d . . . H6A H 0.3164 -0.1057 0.4692 0.057 Uiso 1 1 calc R . . H6B H 0.3586 -0.0146 0.4574 0.057 Uiso 1 1 calc R . . H6C H 0.3032 -0.0673 0.4041 0.057 Uiso 1 1 calc R . . C7 C 0.3004(6) 0.0894(7) 0.5462(4) 0.046(3) Uani 1 1 d . . . H7A H 0.3026 0.0524 0.5810 0.069 Uiso 1 1 calc R . . H7B H 0.2920 0.1508 0.5563 0.069 Uiso 1 1 calc R . . H7C H 0.3525 0.0841 0.5327 0.069 Uiso 1 1 calc R . . C8 C 0.1165(7) 0.1543(7) 0.5304(5) 0.053(3) Uani 1 1 d . . . H8A H 0.0997 0.1220 0.5624 0.079 Uiso 1 1 calc R . . H8B H 0.0688 0.1855 0.5076 0.079 Uiso 1 1 calc R . . H8C H 0.1596 0.1967 0.5466 0.079 Uiso 1 1 calc R . . C9 C 0.0084(6) 0.0564(6) 0.4196(5) 0.048(3) Uani 1 1 d . . . H9A H -0.0219 0.0167 0.4407 0.072 Uiso 1 1 calc R . . H9B H -0.0041 0.0416 0.3777 0.072 Uiso 1 1 calc R . . H9C H -0.0082 0.1172 0.4248 0.072 Uiso 1 1 calc R . . C10 C 0.1267(6) -0.0709(5) 0.3668(4) 0.037(3) Uani 1 1 d . . . H10A H 0.1098 -0.1281 0.3796 0.056 Uiso 1 1 calc R . . H10B H 0.1723 -0.0789 0.3464 0.056 Uiso 1 1 calc R . . H10C H 0.0799 -0.0435 0.3402 0.056 Uiso 1 1 calc R . . C11 C 0.3668(5) 0.0563(6) 0.2464(4) 0.0283(10) Uani 1 1 d U . . C12 C 0.4322(5) 0.0851(6) 0.2930(4) 0.0284(10) Uani 1 1 d U . . C13 C 0.4548(5) 0.1719(6) 0.2821(4) 0.0281(10) Uani 1 1 d U . . C14 C 0.4016(5) 0.2002(6) 0.2295(4) 0.0280(10) Uani 1 1 d U . . C15 C 0.3482(5) 0.1250(6) 0.2066(4) 0.0282(10) Uani 1 1 d U . . C16 C 0.3301(7) -0.0314(6) 0.2424(5) 0.054(3) Uani 1 1 d . . . H16A H 0.3603 -0.0702 0.2206 0.081 Uiso 1 1 calc R . . H16B H 0.2723 -0.0280 0.2221 0.081 Uiso 1 1 calc R . . H16C H 0.3333 -0.0551 0.2819 0.081 Uiso 1 1 calc R . . C17 C 0.4764(6) 0.0251(7) 0.3429(4) 0.050(3) Uani 1 1 d . . . H17A H 0.5240 -0.0028 0.3313 0.075 Uiso 1 1 calc R . . H17B H 0.4382 -0.0204 0.3508 0.075 Uiso 1 1 calc R . . H17C H 0.4953 0.0602 0.3783 0.075 Uiso 1 1 calc R . . C18 C 0.5206(6) 0.2281(8) 0.3195(5) 0.056(3) Uani 1 1 d . . . H18A H 0.5732 0.2194 0.3072 0.085 Uiso 1 1 calc R . . H18B H 0.5265 0.2112 0.3607 0.085 Uiso 1 1 calc R . . H18C H 0.5046 0.2902 0.3148 0.085 Uiso 1 1 calc R . . C19 C 0.4028(6) 0.2867(5) 0.1996(4) 0.039(3) Uani 1 1 d . . . H19A H 0.4437 0.2852 0.1746 0.058 Uiso 1 1 calc R . . H19B H 0.4174 0.3331 0.2291 0.058 Uiso 1 1 calc R . . H19C H 0.3482 0.2988 0.1756 0.058 Uiso 1 1 calc R . . C20 C 0.2849(5) 0.1267(7) 0.1499(4) 0.041(3) Uani 1 1 d . . . H20A H 0.3103 0.1062 0.1178 0.061 Uiso 1 1 calc R . . H20B H 0.2646 0.1869 0.1418 0.061 Uiso 1 1 calc R . . H20C H 0.2388 0.0880 0.1532 0.061 Uiso 1 1 calc R . . C21 C 0.3813(5) 0.2792(5) 0.4641(4) 0.021(2) Uani 1 1 d . . . C22 C 0.4052(5) 0.3180(5) 0.5200(4) 0.029(2) Uani 1 1 d . . . H22A H 0.3786 0.3700 0.5290 0.034 Uiso 1 1 calc R . . C23 C 0.4673(5) 0.2806(6) 0.5618(4) 0.026(2) Uani 1 1 d . . . H23A H 0.4816 0.3067 0.5995 0.031 Uiso 1 1 calc R . . C24 C 0.5086(5) 0.2069(5) 0.5500(4) 0.025(2) Uani 1 1 d . . . H24A H 0.5518 0.1833 0.5792 0.030 Uiso 1 1 calc R . . C25 C 0.4881(5) 0.1681(6) 0.4975(4) 0.037(2) Uani 1 1 d . . . H25A H 0.5161 0.1163 0.4896 0.045 Uiso 1 1 calc R . . C26 C 0.4256(5) 0.2038(5) 0.4541(4) 0.023(2) Uani 1 1 d . . . H26A H 0.4128 0.1763 0.4167 0.028 Uiso 1 1 calc R . . C27 C 0.3650(5) 0.4046(5) 0.3720(4) 0.020(2) Uani 1 1 d . . . C28 C 0.4387(5) 0.4412(5) 0.4026(4) 0.026(2) Uani 1 1 d . . . H28A H 0.4574 0.4279 0.4430 0.032 Uiso 1 1 calc R . . C29 C 0.4856(5) 0.4973(5) 0.3744(4) 0.026(2) Uani 1 1 d . . . H29A H 0.5366 0.5200 0.3953 0.032 Uiso 1 1 calc R . . C30 C 0.4575(5) 0.5195(6) 0.3164(4) 0.032(2) Uani 1 1 d . . . H30A H 0.4877 0.5594 0.2975 0.038 Uiso 1 1 calc R . . C31 C 0.3866(5) 0.4836(5) 0.2869(4) 0.027(2) Uani 1 1 d . . . H31A H 0.3678 0.4977 0.2467 0.032 Uiso 1 1 calc R . . C32 C 0.3403(6) 0.4265(6) 0.3138(4) 0.028(2) Uani 1 1 d . . . H32A H 0.2908 0.4022 0.2916 0.033 Uiso 1 1 calc R . . C33 C 0.2424(5) 0.3956(5) 0.4430(4) 0.0190(19) Uani 1 1 d . . . C34 C 0.2097(5) 0.3605(6) 0.4887(4) 0.024(2) Uani 1 1 d . . . H34A H 0.2247 0.3026 0.5020 0.029 Uiso 1 1 calc R . . C35 C 0.1569(5) 0.4070(6) 0.5145(4) 0.027(2) Uani 1 1 d . . . H35A H 0.1354 0.3813 0.5454 0.033 Uiso 1 1 calc R . . C36 C 0.1348(5) 0.4897(7) 0.4967(4) 0.037(3) Uani 1 1 d . . . H36A H 0.0996 0.5228 0.5160 0.044 Uiso 1 1 calc R . . C37 C 0.1628(6) 0.5253(6) 0.4512(5) 0.044(3) Uani 1 1 d . . . H37A H 0.1464 0.5830 0.4381 0.053 Uiso 1 1 calc R . . C38 C 0.2170(5) 0.4767(6) 0.4228(4) 0.036(3) Uani 1 1 d . . . H38A H 0.2350 0.5008 0.3900 0.044 Uiso 1 1 calc R . . C39 C 0.1264(5) 0.3777(6) 0.2467(4) 0.022(2) Uani 1 1 d . . . C40 C 0.1686(5) 0.3874(6) 0.2014(4) 0.025(2) Uani 1 1 d . . . H40A H 0.1863 0.3361 0.1842 0.030 Uiso 1 1 calc R . . C41 C 0.1860(5) 0.4685(6) 0.1803(4) 0.027(2) Uani 1 1 d . . . H41A H 0.2151 0.4728 0.1492 0.032 Uiso 1 1 calc R . . C42 C 0.1604(5) 0.5433(6) 0.2049(4) 0.030(2) Uani 1 1 d . . . H42A H 0.1720 0.5996 0.1908 0.036 Uiso 1 1 calc R . . C43 C 0.1178(5) 0.5368(5) 0.2501(4) 0.030(2) Uani 1 1 d . . . H43A H 0.0997 0.5884 0.2666 0.035 Uiso 1 1 calc R . . C44 C 0.1020(5) 0.4557(5) 0.2707(4) 0.025(2) Uani 1 1 d . . . H44A H 0.0737 0.4520 0.3023 0.029 Uiso 1 1 calc R . . C45 C 0.0829(5) 0.1964(5) 0.2217(3) 0.0187(19) Uani 1 1 d . . . C46 C 0.0981(5) 0.1094(5) 0.2299(4) 0.022(2) Uani 1 1 d . . . H46A H 0.1269 0.0900 0.2673 0.027 Uiso 1 1 calc R . . C47 C 0.0735(5) 0.0472(5) 0.1861(4) 0.022(2) Uani 1 1 d . . . H47A H 0.0841 -0.0137 0.1933 0.026 Uiso 1 1 calc R . . C48 C 0.0324(5) 0.0773(6) 0.1308(4) 0.028(2) Uani 1 1 d . . . H48A H 0.0159 0.0368 0.0996 0.033 Uiso 1 1 calc R . . C49 C 0.0163(5) 0.1649(6) 0.1220(4) 0.027(2) Uani 1 1 d . . . H49A H -0.0134 0.1838 0.0848 0.033 Uiso 1 1 calc R . . C50 C 0.0418(5) 0.2276(6) 0.1656(4) 0.027(2) Uani 1 1 d . . . H50A H 0.0321 0.2886 0.1582 0.032 Uiso 1 1 calc R . . C51 C 0.0227(5) 0.2875(5) 0.3111(3) 0.0159(18) Uani 1 1 d U . . C52 C -0.0552(5) 0.2829(5) 0.2767(4) 0.023(2) Uani 1 1 d . . . H52A H -0.0616 0.2706 0.2361 0.028 Uiso 1 1 calc R . . C53 C -0.1250(5) 0.2959(5) 0.3004(4) 0.028(2) Uani 1 1 d . . . H53A H -0.1784 0.2914 0.2761 0.033 Uiso 1 1 calc R . . C54 C -0.1164(5) 0.3155(5) 0.3595(4) 0.028(2) Uani 1 1 d . . . H54A H -0.1638 0.3241 0.3760 0.034 Uiso 1 1 calc R . . C55 C -0.0383(5) 0.3222(6) 0.3942(4) 0.029(2) Uani 1 1 d . . . H55A H -0.0322 0.3364 0.4345 0.034 Uiso 1 1 calc R . . C56 C 0.0308(5) 0.3086(5) 0.3711(4) 0.024(2) Uani 1 1 d . . . H56A H 0.0840 0.3133 0.3956 0.029 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 0.0227(6) 0.0180(6) 0.0169(6) 0.0007(5) 0.0084(4) 0.0014(5) Ga1 0.0310(6) 0.0191(5) 0.0180(5) 0.0040(5) 0.0093(4) -0.0010(4) Ga2 0.0252(5) 0.0305(6) 0.0179(5) -0.0016(5) 0.0094(4) 0.0051(4) P1 0.0241(12) 0.0212(13) 0.0186(13) -0.0001(11) 0.0101(9) 0.0012(10) P2 0.0225(12) 0.0161(12) 0.0142(12) 0.0042(10) 0.0070(9) 0.0021(9) C1 0.037(2) 0.023(2) 0.024(2) 0.014(2) 0.0155(19) 0.003(2) C2 0.038(2) 0.024(2) 0.024(2) 0.013(2) 0.0157(19) 0.002(2) C3 0.038(2) 0.024(2) 0.024(2) 0.013(2) 0.0161(19) 0.002(2) C4 0.037(2) 0.023(2) 0.024(2) 0.014(2) 0.0160(19) 0.002(2) C5 0.037(2) 0.023(2) 0.024(2) 0.013(2) 0.0155(19) 0.002(2) C6 0.031(5) 0.041(6) 0.043(7) 0.026(5) 0.013(5) 0.005(4) C7 0.058(7) 0.051(7) 0.025(6) 0.002(6) 0.003(5) -0.025(5) C8 0.073(8) 0.053(7) 0.046(7) 0.018(6) 0.044(6) 0.000(6) C9 0.041(6) 0.046(7) 0.062(8) 0.011(6) 0.019(5) -0.003(5) C10 0.077(7) 0.013(5) 0.020(5) -0.003(5) 0.010(5) -0.009(5) C11 0.035(3) 0.033(3) 0.024(2) -0.006(2) 0.0211(19) 0.007(2) C12 0.035(3) 0.033(2) 0.024(2) -0.006(2) 0.0212(19) 0.007(2) C13 0.034(3) 0.033(2) 0.024(2) -0.006(2) 0.0211(19) 0.007(2) C14 0.034(3) 0.032(3) 0.024(2) -0.006(2) 0.0209(19) 0.006(2) C15 0.034(3) 0.032(3) 0.024(2) -0.006(2) 0.0207(19) 0.007(2) C16 0.080(8) 0.026(6) 0.067(9) -0.021(6) 0.043(7) -0.016(5) C17 0.067(7) 0.059(7) 0.030(6) 0.018(6) 0.024(5) 0.040(6) C18 0.047(7) 0.084(9) 0.039(7) -0.008(7) 0.010(5) 0.005(6) C19 0.059(7) 0.016(5) 0.050(7) -0.008(5) 0.033(5) 0.003(4) C20 0.038(6) 0.072(8) 0.013(5) -0.005(5) 0.006(4) 0.002(5) C21 0.033(5) 0.019(5) 0.015(5) -0.004(4) 0.013(4) -0.011(4) C22 0.039(6) 0.016(5) 0.032(6) -0.005(5) 0.009(4) 0.000(4) C23 0.034(5) 0.032(6) 0.009(5) 0.006(4) -0.002(4) -0.007(4) C24 0.015(5) 0.024(5) 0.034(6) 0.004(5) -0.001(4) 0.000(4) C25 0.036(6) 0.036(6) 0.039(6) 0.002(5) 0.008(5) 0.001(5) C26 0.033(5) 0.025(5) 0.011(5) -0.003(4) 0.000(4) 0.007(4) C27 0.023(5) 0.019(5) 0.022(5) -0.013(4) 0.012(4) 0.003(4) C28 0.028(5) 0.025(5) 0.029(6) -0.002(5) 0.013(4) -0.011(4) C29 0.021(5) 0.024(5) 0.036(6) 0.001(5) 0.009(4) -0.009(4) C30 0.037(6) 0.021(5) 0.046(7) 0.006(5) 0.026(5) -0.004(4) C31 0.048(6) 0.026(5) 0.013(5) 0.000(4) 0.020(4) -0.003(4) C32 0.045(6) 0.020(5) 0.026(6) -0.006(5) 0.026(4) -0.005(4) C33 0.019(5) 0.026(5) 0.015(5) 0.006(4) 0.011(3) 0.001(4) C34 0.018(5) 0.022(5) 0.031(6) 0.010(5) 0.001(4) 0.002(4) C35 0.030(5) 0.030(5) 0.025(6) -0.006(5) 0.011(4) 0.005(4) C36 0.034(6) 0.053(7) 0.027(6) -0.007(5) 0.015(4) 0.011(5) C37 0.063(7) 0.023(6) 0.051(8) 0.009(6) 0.024(6) 0.012(5) C38 0.037(6) 0.039(6) 0.036(6) 0.013(5) 0.015(5) 0.008(5) C39 0.020(5) 0.028(5) 0.021(5) -0.007(4) 0.009(4) 0.001(4) C40 0.031(5) 0.025(5) 0.019(5) -0.005(4) 0.006(4) 0.004(4) C41 0.032(5) 0.034(6) 0.016(5) 0.012(5) 0.010(4) 0.001(4) C42 0.037(6) 0.031(6) 0.024(6) 0.009(5) 0.009(4) 0.002(4) C43 0.044(6) 0.012(5) 0.035(6) 0.001(5) 0.014(5) 0.004(4) C44 0.029(5) 0.026(5) 0.025(5) 0.014(4) 0.018(4) 0.004(4) C45 0.030(5) 0.018(5) 0.011(4) 0.003(4) 0.011(4) -0.010(4) C46 0.019(5) 0.031(6) 0.015(5) -0.002(4) 0.000(4) -0.005(4) C47 0.023(5) 0.022(5) 0.025(5) -0.002(4) 0.015(4) 0.001(4) C48 0.033(5) 0.034(6) 0.019(5) -0.017(5) 0.015(4) -0.010(4) C49 0.025(5) 0.035(6) 0.019(5) 0.006(5) -0.001(4) -0.001(4) C50 0.028(5) 0.040(6) 0.015(5) -0.006(5) 0.009(4) -0.009(4) C51 0.027(4) 0.010(4) 0.013(4) -0.007(4) 0.010(3) 0.001(3) C52 0.026(5) 0.030(5) 0.019(5) 0.000(4) 0.013(4) 0.002(4) C53 0.017(5) 0.023(5) 0.042(6) 0.004(5) 0.004(4) 0.000(4) C54 0.041(6) 0.024(5) 0.030(6) 0.004(5) 0.032(5) 0.003(4) C55 0.040(6) 0.029(6) 0.022(5) 0.006(5) 0.018(4) 0.000(4) C56 0.020(5) 0.030(5) 0.023(5) 0.016(4) 0.003(4) 0.003(4) _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 P1 2.136(2) . ? Ni1 P2 2.138(2) . ? Ni1 Ga1 2.2493(14) . ? Ni1 Ga2 2.2557(14) . ? Ga1 C5 2.337(8) . ? Ga1 C1 2.340(8) . ? Ga1 C4 2.368(8) . ? Ga1 C3 2.386(9) . ? Ga1 C2 2.386(8) . ? Ga2 C11 2.324(8) . ? Ga2 C15 2.342(9) . ? Ga2 C12 2.351(8) . ? Ga2 C14 2.358(9) . ? Ga2 C13 2.414(8) . ? P1 C27 1.830(9) . ? P1 C33 1.835(8) . ? P1 C21 1.835(8) . ? P2 C39 1.841(9) . ? P2 C51 1.853(8) . ? P2 C45 1.856(8) . ? C1 C2 1.425(12) . ? C1 C5 1.433(12) . ? C1 C6 1.500(12) . ? C2 C3 1.406(11) . ? C2 C7 1.479(12) . ? C3 C4 1.389(12) . ? C3 C8 1.515(13) . ? C4 C5 1.449(12) . ? C4 C9 1.538(12) . ? C5 C10 1.497(12) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C15 1.390(12) . ? C11 C12 1.437(12) . ? C11 C16 1.461(12) . ? C12 C13 1.410(12) . ? C12 C17 1.540(12) . ? C13 C14 1.423(12) . ? C13 C18 1.514(12) . ? C14 C15 1.476(12) . ? C14 C19 1.490(12) . ? C15 C20 1.510(11) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C26 1.406(11) . ? C21 C22 1.411(11) . ? C22 C23 1.387(11) . ? C22 H22A 0.9500 . ? C23 C24 1.369(11) . ? C23 H23A 0.9500 . ? C24 C25 1.340(12) . ? C24 H24A 0.9500 . ? C25 C26 1.401(11) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C27 C32 1.377(12) . ? C27 C28 1.399(10) . ? C28 C29 1.404(11) . ? C28 H28A 0.9500 . ? C29 C30 1.380(12) . ? C29 H29A 0.9500 . ? C30 C31 1.350(12) . ? C30 H30A 0.9500 . ? C31 C32 1.389(11) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? C33 C38 1.356(11) . ? C33 C34 1.396(11) . ? C34 C35 1.357(11) . ? C34 H34A 0.9500 . ? C35 C36 1.352(12) . ? C35 H35A 0.9500 . ? C36 C37 1.354(13) . ? C36 H36A 0.9500 . ? C37 C38 1.425(13) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C39 C40 1.387(11) . ? C39 C44 1.406(11) . ? C40 C41 1.381(11) . ? C40 H40A 0.9500 . ? C41 C42 1.379(12) . ? C41 H41A 0.9500 . ? C42 C43 1.385(12) . ? C42 H42A 0.9500 . ? C43 C44 1.368(11) . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? C45 C46 1.353(11) . ? C45 C50 1.427(11) . ? C46 C47 1.391(11) . ? C46 H46A 0.9500 . ? C47 C48 1.406(11) . ? C47 H47A 0.9500 . ? C48 C49 1.366(12) . ? C48 H48A 0.9500 . ? C49 C50 1.395(11) . ? C49 H49A 0.9500 . ? C50 H50A 0.9500 . ? C51 C52 1.375(10) . ? C51 C56 1.416(11) . ? C52 C53 1.393(11) . ? C52 H52A 0.9500 . ? C53 C54 1.388(12) . ? C53 H53A 0.9500 . ? C54 C55 1.382(12) . ? C54 H54A 0.9500 . ? C55 C56 1.374(11) . ? C55 H55A 0.9500 . ? C56 H56A 0.9500 . ? 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 P1 Ni1 P2 124.38(9) . . ? P1 Ni1 Ga1 103.39(8) . . ? P2 Ni1 Ga1 110.00(7) . . ? P1 Ni1 Ga2 106.06(7) . . ? P2 Ni1 Ga2 107.24(8) . . ? Ga1 Ni1 Ga2 104.02(5) . . ? Ni1 Ga1 C5 149.8(2) . . ? Ni1 Ga1 C1 149.3(2) . . ? C5 Ga1 C1 35.7(3) . . ? Ni1 Ga1 C4 150.2(2) . . ? C5 Ga1 C4 35.9(3) . . ? C1 Ga1 C4 58.3(3) . . ? Ni1 Ga1 C3 148.8(2) . . ? C5 Ga1 C3 58.5(3) . . ? C1 Ga1 C3 57.7(3) . . ? C4 Ga1 C3 34.0(3) . . ? Ni1 Ga1 C2 148.1(2) . . ? C5 Ga1 C2 58.9(3) . . ? C1 Ga1 C2 35.1(3) . . ? C4 Ga1 C2 57.4(3) . . ? C3 Ga1 C2 34.3(3) . . ? Ni1 Ga2 C11 157.5(2) . . ? Ni1 Ga2 C15 151.6(2) . . ? C11 Ga2 C15 34.7(3) . . ? Ni1 Ga2 C12 150.0(2) . . ? C11 Ga2 C12 35.8(3) . . ? C15 Ga2 C12 58.3(3) . . ? Ni1 Ga2 C14 141.6(2) . . ? C11 Ga2 C14 59.3(3) . . ? C15 Ga2 C14 36.6(3) . . ? C12 Ga2 C14 58.0(3) . . ? Ni1 Ga2 C13 141.3(2) . . ? C11 Ga2 C13 58.8(3) . . ? C15 Ga2 C13 58.8(3) . . ? C12 Ga2 C13 34.4(3) . . ? C14 Ga2 C13 34.7(3) . . ? C27 P1 C33 103.1(4) . . ? C27 P1 C21 101.7(4) . . ? C33 P1 C21 102.5(4) . . ? C27 P1 Ni1 117.3(3) . . ? C33 P1 Ni1 112.3(3) . . ? C21 P1 Ni1 117.9(3) . . ? C39 P2 C51 101.1(4) . . ? C39 P2 C45 102.2(4) . . ? C51 P2 C45 100.2(3) . . ? C39 P2 Ni1 114.7(3) . . ? C51 P2 Ni1 118.4(3) . . ? C45 P2 Ni1 117.5(3) . . ? C2 C1 C5 108.9(8) . . ? C2 C1 C6 126.7(8) . . ? C5 C1 C6 124.5(8) . . ? C2 C1 Ga1 74.2(5) . . ? C5 C1 Ga1 72.1(5) . . ? C6 C1 Ga1 119.2(6) . . ? C3 C2 C1 107.3(8) . . ? C3 C2 C7 125.8(9) . . ? C1 C2 C7 126.9(8) . . ? C3 C2 Ga1 72.8(5) . . ? C1 C2 Ga1 70.7(5) . . ? C7 C2 Ga1 122.7(6) . . ? C4 C3 C2 109.5(8) . . ? C4 C3 C8 124.9(8) . . ? C2 C3 C8 125.5(9) . . ? C4 C3 Ga1 72.3(5) . . ? C2 C3 Ga1 72.9(5) . . ? C8 C3 Ga1 124.9(6) . . ? C3 C4 C5 108.8(8) . . ? C3 C4 C9 127.6(8) . . ? C5 C4 C9 123.7(8) . . ? C3 C4 Ga1 73.7(5) . . ? C5 C4 Ga1 70.9(5) . . ? C9 C4 Ga1 121.5(6) . . ? C1 C5 C4 105.6(8) . . ? C1 C5 C10 128.8(8) . . ? C4 C5 C10 125.6(8) . . ? C1 C5 Ga1 72.3(5) . . ? C4 C5 Ga1 73.2(5) . . ? C10 C5 Ga1 119.3(6) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C15 C11 C12 107.9(8) . . ? C15 C11 C16 127.7(9) . . ? C12 C11 C16 124.4(9) . . ? C15 C11 Ga2 73.4(5) . . ? C12 C11 Ga2 73.1(5) . . ? C16 C11 Ga2 120.9(6) . . ? C13 C12 C11 109.6(8) . . ? C13 C12 C17 126.0(8) . . ? C11 C12 C17 124.0(8) . . ? C13 C12 Ga2 75.3(5) . . ? C11 C12 Ga2 71.1(5) . . ? C17 C12 Ga2 125.5(6) . . ? C12 C13 C14 107.4(8) . . ? C12 C13 C18 127.7(9) . . ? C14 C13 C18 124.9(9) . . ? C12 C13 Ga2 70.3(5) . . ? C14 C13 Ga2 70.5(5) . . ? C18 C13 Ga2 122.6(6) . . ? C13 C14 C15 107.3(8) . . ? C13 C14 C19 127.2(8) . . ? C15 C14 C19 125.4(8) . . ? C13 C14 Ga2 74.8(5) . . ? C15 C14 Ga2 71.1(5) . . ? C19 C14 Ga2 123.1(6) . . ? C11 C15 C14 107.8(8) . . ? C11 C15 C20 128.1(9) . . ? C14 C15 C20 124.1(8) . . ? C11 C15 Ga2 71.9(5) . . ? C14 C15 Ga2 72.3(5) . . ? C20 C15 Ga2 120.9(6) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C26 C21 C22 115.9(7) . . ? C26 C21 P1 119.6(6) . . ? C22 C21 P1 124.4(6) . . ? C23 C22 C21 120.3(8) . . ? C23 C22 H22A 119.8 . . ? C21 C22 H22A 119.8 . . ? C24 C23 C22 121.6(8) . . ? C24 C23 H23A 119.2 . . ? C22 C23 H23A 119.2 . . ? C25 C24 C23 120.0(8) . . ? C25 C24 H24A 120.0 . . ? C23 C24 H24A 120.0 . . ? C24 C25 C26 120.1(9) . . ? C24 C25 H25A 120.0 . . ? C26 C25 H25A 120.0 . . ? C25 C26 C21 122.1(8) . . ? C25 C26 H26A 119.0 . . ? C21 C26 H26A 119.0 . . ? C32 C27 C28 117.3(8) . . ? C32 C27 P1 119.0(6) . . ? C28 C27 P1 123.6(7) . . ? C27 C28 C29 120.8(8) . . ? C27 C28 H28A 119.6 . . ? C29 C28 H28A 119.6 . . ? C30 C29 C28 120.0(8) . . ? C30 C29 H29A 120.0 . . ? C28 C29 H29A 120.0 . . ? C31 C30 C29 119.0(8) . . ? C31 C30 H30A 120.5 . . ? C29 C30 H30A 120.5 . . ? C30 C31 C32 121.7(9) . . ? C30 C31 H31A 119.2 . . ? C32 C31 H31A 119.2 . . ? C27 C32 C31 121.1(9) . . ? C27 C32 H32A 119.4 . . ? C31 C32 H32A 119.4 . . ? C38 C33 C34 118.0(8) . . ? C38 C33 P1 121.5(7) . . ? C34 C33 P1 119.7(6) . . ? C35 C34 C33 121.7(8) . . ? C35 C34 H34A 119.1 . . ? C33 C34 H34A 119.1 . . ? C36 C35 C34 120.4(9) . . ? C36 C35 H35A 119.8 . . ? C34 C35 H35A 119.8 . . ? C35 C36 C37 119.9(9) . . ? C35 C36 H36A 120.0 . . ? C37 C36 H36A 120.0 . . ? C36 C37 C38 120.3(9) . . ? C36 C37 H37A 119.8 . . ? C38 C37 H37A 119.8 . . ? C33 C38 C37 119.5(9) . . ? C33 C38 H38A 120.3 . . ? C37 C38 H38A 120.3 . . ? C40 C39 C44 116.4(8) . . ? C40 C39 P2 122.8(7) . . ? C44 C39 P2 119.7(6) . . ? C41 C40 C39 122.7(8) . . ? C41 C40 H40A 118.7 . . ? C39 C40 H40A 118.7 . . ? C42 C41 C40 119.0(8) . . ? C42 C41 H41A 120.5 . . ? C40 C41 H41A 120.5 . . ? C41 C42 C43 120.3(9) . . ? C41 C42 H42A 119.8 . . ? C43 C42 H42A 119.8 . . ? C44 C43 C42 119.7(9) . . ? C44 C43 H43A 120.1 . . ? C42 C43 H43A 120.1 . . ? C43 C44 C39 121.9(8) . . ? C43 C44 H44A 119.0 . . ? C39 C44 H44A 119.0 . . ? C46 C45 C50 119.7(8) . . ? C46 C45 P2 118.3(6) . . ? C50 C45 P2 122.0(6) . . ? C45 C46 C47 122.9(8) . . ? C45 C46 H46A 118.6 . . ? C47 C46 H46A 118.6 . . ? C46 C47 C48 117.7(8) . . ? C46 C47 H47A 121.1 . . ? C48 C47 H47A 121.1 . . ? C49 C48 C47 120.0(8) . . ? C49 C48 H48A 120.0 . . ? C47 C48 H48A 120.0 . . ? C48 C49 C50 122.4(8) . . ? C48 C49 H49A 118.8 . . ? C50 C49 H49A 118.8 . . ? C49 C50 C45 117.2(8) . . ? C49 C50 H50A 121.4 . . ? C45 C50 H50A 121.4 . . ? C52 C51 C56 118.4(7) . . ? C52 C51 P2 124.8(6) . . ? C56 C51 P2 116.8(6) . . ? C51 C52 C53 121.2(8) . . ? C51 C52 H52A 119.4 . . ? C53 C52 H52A 119.4 . . ? C54 C53 C52 119.9(8) . . ? C54 C53 H53A 120.0 . . ? C52 C53 H53A 120.0 . . ? C55 C54 C53 119.3(8) . . ? C55 C54 H54A 120.3 . . ? C53 C54 H54A 120.3 . . ? C56 C55 C54 121.0(9) . . ? C56 C55 H55A 119.5 . . ? C54 C55 H55A 119.5 . . ? C55 C56 C51 120.2(8) . . ? C55 C56 H56A 119.9 . . ? C51 C56 H56A 119.9 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.723 _refine_diff_density_min -0.811 _refine_diff_density_rms 0.131 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.282 -0.250 0.038 677.0 34.7 2 0.718 0.250 1.005 677.0 30.4 _platon_squeeze_details ; ; data_Ni(AlCp*)2(PPh3)2 _database_code_depnum_ccdc_archive 'CCDC 820861' #TrackingRef '- alle_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _space_group_name_Hall '-P 1' _chemical_formula_moiety 'C56 H60 Al2 Ni P2 ' _chemical_formula_sum 'C56 H60 Al2 Ni P2' _chemical_formula_weight 907.65 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' Al Al 0.0645 0.0514 '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' Ni Ni 0.3393 1.1124 '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 11.5183(5) _cell_length_b 21.7943(9) _cell_length_c 22.2311(8) _cell_angle_alpha 117.737(4) _cell_angle_beta 92.013(3) _cell_angle_gamma 94.562(3) _cell_volume 4907.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 200 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.229 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 0.532 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8567 _exptl_absorpt_correction_T_max 0.9010 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '560 images at 1.0 deg. in \w and 25 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46112 _diffrn_reflns_av_R_equivalents 0.0719 _diffrn_reflns_av_sigmaI/netI 0.1042 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 25.00 _reflns_number_total 17267 _reflns_number_gt 11183 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 1.171.13, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _refine_special_details ; Severally disordered cocrystallized solvent molecules have been omited from the diffration data and were not taken into account during the structure refinement. 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^)+(0.0368P)^2^+0.0000P] 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 17267 _refine_ls_number_parameters 1119 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0987 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1065 _refine_ls_wR_factor_gt 0.0938 _refine_ls_goodness_of_fit_ref 0.970 _refine_ls_restrained_S_all 0.970 _refine_ls_shift/su_max 0.028 _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 0.60097(4) 0.27114(2) 0.25706(2) 0.01700(11) Uani 1 1 d . . . Ni2 Ni 0.00887(4) 0.78001(2) 0.23832(2) 0.01869(12) Uani 1 1 d . . . Al1 Al 0.66587(9) 0.20243(5) 0.29605(5) 0.0208(2) Uani 1 1 d . . . Al2 Al 0.44912(9) 0.20446(5) 0.18634(5) 0.0281(3) Uani 1 1 d . . . Al3 Al 0.09063(9) 0.77869(5) 0.32948(5) 0.0234(3) Uani 1 1 d . . . Al4 Al -0.15160(9) 0.70654(6) 0.21142(6) 0.0289(3) Uani 1 1 d . . . P1 P 0.72429(8) 0.28596(4) 0.19458(4) 0.0186(2) Uani 1 1 d . . . P2 P 0.54123(8) 0.35457(4) 0.34372(4) 0.0176(2) Uani 1 1 d . . . P3 P 0.11866(8) 0.73339(4) 0.15712(4) 0.0188(2) Uani 1 1 d . . . P4 P -0.05037(8) 0.87960(4) 0.26854(4) 0.0201(2) Uani 1 1 d . . . C1 C 0.6205(3) 0.11477(18) 0.32141(19) 0.0302(9) Uani 1 1 d . . . C2 C 0.6732(3) 0.17341(18) 0.38165(18) 0.0299(9) Uani 1 1 d . . . C3 C 0.7898(3) 0.18849(19) 0.36969(18) 0.0302(9) Uani 1 1 d . . . C4 C 0.8102(3) 0.13953(19) 0.30211(18) 0.0276(9) Uani 1 1 d . . . C5 C 0.7050(3) 0.09421(18) 0.27240(18) 0.0278(9) Uani 1 1 d . . . C6 C 0.4970(4) 0.0817(2) 0.3095(2) 0.0503(12) Uani 1 1 d . . . H6A H 0.4968 0.0331 0.3001 0.075 Uiso 1 1 calc R . . H6B H 0.4580 0.0832 0.2704 0.075 Uiso 1 1 calc R . . H6C H 0.4554 0.1073 0.3501 0.075 Uiso 1 1 calc R . . C7 C 0.6175(4) 0.2116(2) 0.44749(19) 0.0449(11) Uani 1 1 d . . . H7A H 0.6347 0.1912 0.4775 0.067 Uiso 1 1 calc R . . H7B H 0.5327 0.2075 0.4380 0.067 Uiso 1 1 calc R . . H7C H 0.6488 0.2609 0.4699 0.067 Uiso 1 1 calc R . . C8 C 0.8750(3) 0.2477(2) 0.42050(19) 0.0438(11) Uani 1 1 d . . . H8A H 0.8931 0.2400 0.4597 0.066 Uiso 1 1 calc R . . H8B H 0.8404 0.2917 0.4358 0.066 Uiso 1 1 calc R . . H8C H 0.9469 0.2498 0.3990 0.066 Uiso 1 1 calc R . . C9 C 0.9204(3) 0.1357(2) 0.2669(2) 0.0381(10) Uani 1 1 d . . . H9A H 0.9559 0.0937 0.2599 0.057 Uiso 1 1 calc R . . H9B H 0.9753 0.1771 0.2952 0.057 Uiso 1 1 calc R . . H9C H 0.9019 0.1339 0.2227 0.057 Uiso 1 1 calc R . . C10 C 0.6856(4) 0.03346(17) 0.20147(18) 0.0371(10) Uani 1 1 d . . . H10A H 0.6712 -0.0100 0.2043 0.056 Uiso 1 1 calc R . . H10B H 0.7550 0.0318 0.1768 0.056 Uiso 1 1 calc R . . H10C H 0.6178 0.0391 0.1773 0.056 Uiso 1 1 calc R . . C11 C 0.3247(4) 0.2051(2) 0.1058(2) 0.0496(14) Uani 1 1 d . . . C12 C 0.2570(4) 0.1962(2) 0.1535(2) 0.0603(16) Uani 1 1 d . . . C13 C 0.2787(4) 0.1321(2) 0.1520(2) 0.0535(14) Uani 1 1 d . . . C14 C 0.3597(3) 0.1015(2) 0.10235(19) 0.0374(11) Uani 1 1 d . . . C15 C 0.3887(3) 0.1462(2) 0.07398(19) 0.0348(10) Uani 1 1 d . . . C16 C 0.3350(4) 0.2675(2) 0.0933(2) 0.0798(19) Uani 1 1 d . . . H16A H 0.3231 0.2518 0.0442 0.120 Uiso 1 1 calc R . . H16B H 0.4130 0.2930 0.1105 0.120 Uiso 1 1 calc R . . H16C H 0.2757 0.2981 0.1169 0.120 Uiso 1 1 calc R . . C17 C 0.1737(4) 0.2448(3) 0.1987(2) 0.091(2) Uani 1 1 d . . . H17A H 0.0939 0.2213 0.1858 0.137 Uiso 1 1 calc R . . H17B H 0.1778 0.2869 0.1931 0.137 Uiso 1 1 calc R . . H17C H 0.1956 0.2576 0.2464 0.137 Uiso 1 1 calc R . . C18 C 0.2211(4) 0.1005(3) 0.1921(2) 0.0843(19) Uani 1 1 d . . . H18A H 0.1426 0.0786 0.1706 0.126 Uiso 1 1 calc R . . H18B H 0.2152 0.1370 0.2388 0.126 Uiso 1 1 calc R . . H18C H 0.2677 0.0652 0.1930 0.126 Uiso 1 1 calc R . . C19 C 0.4078(4) 0.03280(19) 0.08290(19) 0.0442(11) Uani 1 1 d . . . H19A H 0.3605 -0.0043 0.0432 0.066 Uiso 1 1 calc R . . H19B H 0.4051 0.0223 0.1212 0.066 Uiso 1 1 calc R . . H19C H 0.4888 0.0358 0.0716 0.066 Uiso 1 1 calc R . . C20 C 0.4704(3) 0.13308(19) 0.01924(18) 0.0387(11) Uani 1 1 d . . . H20A H 0.4336 0.0960 -0.0244 0.058 Uiso 1 1 calc R . . H20B H 0.5429 0.1189 0.0308 0.058 Uiso 1 1 calc R . . H20C H 0.4880 0.1759 0.0155 0.058 Uiso 1 1 calc R . . C21 C 0.7902(3) 0.20916(17) 0.13050(16) 0.0217(8) Uani 1 1 d . . . C22 C 0.8842(3) 0.21714(19) 0.09628(17) 0.0323(9) Uani 1 1 d . . . H22A H 0.9140 0.2625 0.1045 0.039 Uiso 1 1 calc R . . C23 C 0.9349(4) 0.1598(2) 0.05036(19) 0.0436(11) Uani 1 1 d . . . H23A H 0.9984 0.1659 0.0267 0.052 Uiso 1 1 calc R . . C24 C 0.8928(4) 0.0935(2) 0.03890(19) 0.0465(12) Uani 1 1 d . . . H24A H 0.9278 0.0540 0.0077 0.056 Uiso 1 1 calc R . . C25 C 0.7999(4) 0.08491(19) 0.07295(18) 0.0375(10) Uani 1 1 d . . . H25A H 0.7710 0.0396 0.0654 0.045 Uiso 1 1 calc R . . C26 C 0.7489(3) 0.14308(17) 0.11841(17) 0.0264(9) Uani 1 1 d . . . H26A H 0.6846 0.1370 0.1414 0.032 Uiso 1 1 calc R . . C27 C 0.8633(3) 0.34262(17) 0.23658(16) 0.0192(8) Uani 1 1 d . . . C28 C 0.9071(3) 0.39718(18) 0.22603(18) 0.0314(9) Uani 1 1 d . . . H28A H 0.8657 0.4081 0.1952 0.038 Uiso 1 1 calc R . . C29 C 1.0120(3) 0.4363(2) 0.26052(19) 0.0394(11) Uani 1 1 d . . . H29A H 1.0403 0.4745 0.2537 0.047 Uiso 1 1 calc R . . C30 C 1.0753(3) 0.4209(2) 0.30411(18) 0.0361(10) Uani 1 1 d . . . H30A H 1.1475 0.4476 0.3266 0.043 Uiso 1 1 calc R . . C31 C 1.0329(3) 0.3666(2) 0.31473(18) 0.0325(10) Uani 1 1 d . . . H31A H 1.0756 0.3556 0.3452 0.039 Uiso 1 1 calc R . . C32 C 0.9285(3) 0.32765(18) 0.28143(17) 0.0255(9) Uani 1 1 d . . . H32A H 0.9004 0.2899 0.2892 0.031 Uiso 1 1 calc R . . C33 C 0.6732(3) 0.32576(18) 0.14224(17) 0.0239(8) Uani 1 1 d . . . C34 C 0.6699(3) 0.29401(19) 0.07159(18) 0.0359(10) Uani 1 1 d . . . H34A H 0.6987 0.2500 0.0474 0.043 Uiso 1 1 calc R . . C35 C 0.6245(4) 0.3262(2) 0.0357(2) 0.0501(12) Uani 1 1 d . . . H35A H 0.6207 0.3035 -0.0127 0.060 Uiso 1 1 calc R . . C36 C 0.5853(4) 0.3906(2) 0.0704(2) 0.0461(12) Uani 1 1 d . . . H36A H 0.5566 0.4130 0.0459 0.055 Uiso 1 1 calc R . . C37 C 0.5876(3) 0.4230(2) 0.1408(2) 0.0369(10) Uani 1 1 d . . . H37A H 0.5602 0.4675 0.1647 0.044 Uiso 1 1 calc R . . C38 C 0.6299(3) 0.39023(18) 0.17628(18) 0.0275(9) Uani 1 1 d . . . H38A H 0.6295 0.4121 0.2245 0.033 Uiso 1 1 calc R . . C39 C 0.6499(3) 0.39676(16) 0.41829(16) 0.0196(8) Uani 1 1 d . . . C40 C 0.7617(3) 0.41658(17) 0.40657(17) 0.0259(9) Uani 1 1 d . . . H40A H 0.7754 0.4129 0.3632 0.031 Uiso 1 1 calc R . . C41 C 0.8533(3) 0.44159(18) 0.45717(17) 0.0296(9) Uani 1 1 d . . . H41A H 0.9286 0.4552 0.4485 0.035 Uiso 1 1 calc R . . C42 C 0.8341(3) 0.44662(18) 0.52028(18) 0.0304(9) Uani 1 1 d . . . H42A H 0.8969 0.4628 0.5547 0.036 Uiso 1 1 calc R . . C43 C 0.7242(3) 0.42824(18) 0.53327(18) 0.0298(9) Uani 1 1 d . . . H43A H 0.7108 0.4325 0.5769 0.036 Uiso 1 1 calc R . . C44 C 0.6324(3) 0.40339(17) 0.48215(17) 0.0231(8) Uani 1 1 d . . . H44A H 0.5568 0.3909 0.4914 0.028 Uiso 1 1 calc R . . C45 C 0.4979(3) 0.42952(16) 0.33407(16) 0.0187(8) Uani 1 1 d . . . C46 C 0.4096(3) 0.41537(18) 0.28356(18) 0.0253(9) Uani 1 1 d . . . H46A H 0.3712 0.3694 0.2585 0.030 Uiso 1 1 calc R . . C47 C 0.3768(3) 0.46707(19) 0.26920(19) 0.0318(9) Uani 1 1 d . . . H47A H 0.3159 0.4567 0.2348 0.038 Uiso 1 1 calc R . . C48 C 0.4326(3) 0.5338(2) 0.3049(2) 0.0366(10) Uani 1 1 d . . . H48A H 0.4111 0.5692 0.2946 0.044 Uiso 1 1 calc R . . C49 C 0.5195(4) 0.54908(18) 0.35529(19) 0.0366(10) Uani 1 1 d . . . H49A H 0.5578 0.5951 0.3799 0.044 Uiso 1 1 calc R . . C50 C 0.5513(3) 0.49740(17) 0.37036(17) 0.0275(9) Uani 1 1 d . . . H50A H 0.6103 0.5086 0.4059 0.033 Uiso 1 1 calc R . . C51 C 0.4107(3) 0.33925(16) 0.38334(16) 0.0189(8) Uani 1 1 d . . . C52 C 0.3672(3) 0.27155(18) 0.36794(18) 0.0293(9) Uani 1 1 d . . . H52A H 0.4047 0.2333 0.3368 0.035 Uiso 1 1 calc R . . C53 C 0.2709(3) 0.2593(2) 0.3972(2) 0.0399(11) Uani 1 1 d . . . H53A H 0.2422 0.2128 0.3857 0.048 Uiso 1 1 calc R . . C54 C 0.2160(3) 0.3138(2) 0.44270(19) 0.0346(10) Uani 1 1 d . . . H54A H 0.1503 0.3051 0.4634 0.042 Uiso 1 1 calc R . . C55 C 0.2564(3) 0.38148(19) 0.45845(17) 0.0277(9) Uani 1 1 d . . . H55A H 0.2181 0.4194 0.4896 0.033 Uiso 1 1 calc R . . C56 C 0.3528(3) 0.39369(17) 0.42870(16) 0.0223(8) Uani 1 1 d . . . H56A H 0.3799 0.4402 0.4395 0.027 Uiso 1 1 calc R . . C57 C 0.2333(3) 0.75357(19) 0.38540(18) 0.0312(9) Uani 1 1 d . . . C58 C 0.1235(4) 0.7247(2) 0.39269(19) 0.0360(10) Uani 1 1 d . . . C59 C 0.0546(3) 0.7805(2) 0.42962(18) 0.0332(10) Uani 1 1 d . . . C60 C 0.1235(3) 0.84378(19) 0.44553(17) 0.0274(9) Uani 1 1 d . . . C61 C 0.2333(3) 0.82705(19) 0.41799(17) 0.0262(9) Uani 1 1 d . . . C62 C 0.3329(4) 0.7141(2) 0.3518(2) 0.0510(12) Uani 1 1 d . . . H62A H 0.3710 0.6988 0.3818 0.076 Uiso 1 1 calc R . . H62B H 0.3895 0.7443 0.3429 0.076 Uiso 1 1 calc R . . H62C H 0.3035 0.6733 0.3086 0.076 Uiso 1 1 calc R . . C63 C 0.0860(4) 0.6483(2) 0.3684(2) 0.0635(15) Uani 1 1 d . . . H63A H 0.1038 0.6367 0.4051 0.095 Uiso 1 1 calc R . . H63B H 0.1282 0.6200 0.3289 0.095 Uiso 1 1 calc R . . H63C H 0.0018 0.6385 0.3554 0.095 Uiso 1 1 calc R . . C64 C -0.0682(3) 0.7725(2) 0.4480(2) 0.0476(12) Uani 1 1 d . . . H64A H -0.0676 0.7558 0.4820 0.071 Uiso 1 1 calc R . . H64B H -0.1170 0.7388 0.4071 0.071 Uiso 1 1 calc R . . H64C H -0.0997 0.8176 0.4668 0.071 Uiso 1 1 calc R . . C65 C 0.0888(3) 0.91681(18) 0.48441(17) 0.0359(10) Uani 1 1 d . . . H65A H 0.1270 0.9392 0.5308 0.054 Uiso 1 1 calc R . . H65B H 0.0038 0.9147 0.4864 0.054 Uiso 1 1 calc R . . H65C H 0.1132 0.9439 0.4612 0.054 Uiso 1 1 calc R . . C66 C 0.3346(3) 0.8786(2) 0.42504(19) 0.0366(10) Uani 1 1 d . . . H66A H 0.3894 0.8863 0.4632 0.055 Uiso 1 1 calc R . . H66B H 0.3058 0.9229 0.4337 0.055 Uiso 1 1 calc R . . H66C H 0.3745 0.8603 0.3829 0.055 Uiso 1 1 calc R . . C67 C -0.2453(3) 0.60214(19) 0.1323(2) 0.0417(11) Uani 1 1 d . . . C68 C -0.2397(4) 0.6036(2) 0.1969(2) 0.0448(12) Uani 1 1 d . . . C69 C -0.3044(3) 0.6579(2) 0.2407(2) 0.0444(11) Uani 1 1 d . . . C70 C -0.3500(3) 0.6898(2) 0.2038(2) 0.0418(11) Uani 1 1 d . . . C71 C -0.3142(3) 0.6546(2) 0.1363(2) 0.0410(11) Uani 1 1 d . . . C72 C -0.1907(4) 0.5518(2) 0.0696(2) 0.0630(15) Uani 1 1 d . . . H72A H -0.2388 0.5066 0.0484 0.094 Uiso 1 1 calc R . . H72B H -0.1120 0.5458 0.0828 0.094 Uiso 1 1 calc R . . H72C H -0.1861 0.5703 0.0371 0.094 Uiso 1 1 calc R . . C73 C -0.1769(4) 0.5559(2) 0.2156(3) 0.0699(16) Uani 1 1 d . . . H73A H -0.2171 0.5085 0.1913 0.105 Uiso 1 1 calc R . . H73B H -0.1766 0.5725 0.2649 0.105 Uiso 1 1 calc R . . H73C H -0.0962 0.5557 0.2030 0.105 Uiso 1 1 calc R . . C74 C -0.3284(4) 0.6780(3) 0.3134(2) 0.0636(14) Uani 1 1 d . . . H74A H -0.4107 0.6642 0.3152 0.095 Uiso 1 1 calc R . . H74B H -0.3110 0.7286 0.3415 0.095 Uiso 1 1 calc R . . H74C H -0.2789 0.6542 0.3308 0.095 Uiso 1 1 calc R . . C75 C -0.4255(3) 0.7485(2) 0.2310(2) 0.0567(13) Uani 1 1 d . . . H75A H -0.5028 0.7314 0.2376 0.085 Uiso 1 1 calc R . . H75B H -0.4336 0.7668 0.1984 0.085 Uiso 1 1 calc R . . H75C H -0.3893 0.7858 0.2747 0.085 Uiso 1 1 calc R . . C76 C -0.3472(4) 0.6696(2) 0.0786(2) 0.0590(14) Uani 1 1 d . . . H76A H -0.4104 0.6348 0.0484 0.089 Uiso 1 1 calc R . . H76B H -0.2792 0.6677 0.0528 0.089 Uiso 1 1 calc R . . H76C H -0.3736 0.7162 0.0972 0.089 Uiso 1 1 calc R . . C77 C 0.1991(3) 0.66100(16) 0.15195(16) 0.0182(8) Uani 1 1 d . . . C78 C 0.1438(3) 0.61391(17) 0.17029(18) 0.0280(9) Uani 1 1 d . . . H78A H 0.0687 0.6212 0.1870 0.034 Uiso 1 1 calc R . . C79 C 0.1955(3) 0.55665(19) 0.16479(19) 0.0356(10) Uani 1 1 d . . . H79A H 0.1550 0.5247 0.1767 0.043 Uiso 1 1 calc R . . C80 C 0.3056(3) 0.54573(18) 0.14209(18) 0.0321(10) Uani 1 1 d . . . H80A H 0.3411 0.5063 0.1383 0.038 Uiso 1 1 calc R . . C81 C 0.3641(3) 0.59274(18) 0.12487(19) 0.0327(10) Uani 1 1 d . . . H81A H 0.4405 0.5863 0.1099 0.039 Uiso 1 1 calc R . . C82 C 0.3096(3) 0.64951(18) 0.12978(17) 0.0271(9) Uani 1 1 d . . . H82A H 0.3498 0.6813 0.1175 0.032 Uiso 1 1 calc R . . C83 C 0.2357(3) 0.79309(16) 0.15218(16) 0.0220(8) Uani 1 1 d . . . C84 C 0.3275(3) 0.82212(18) 0.20323(18) 0.0298(9) Uani 1 1 d . . . H84A H 0.3308 0.8085 0.2381 0.036 Uiso 1 1 calc R . . C85 C 0.4143(4) 0.87067(19) 0.2039(2) 0.0412(11) Uani 1 1 d . . . H85A H 0.4774 0.8890 0.2383 0.049 Uiso 1 1 calc R . . C86 C 0.4084(4) 0.8921(2) 0.1546(2) 0.0469(12) Uani 1 1 d . . . H86A H 0.4675 0.9252 0.1549 0.056 Uiso 1 1 calc R . . C87 C 0.3169(4) 0.8654(2) 0.1049(2) 0.0472(12) Uani 1 1 d . . . H87A H 0.3116 0.8810 0.0716 0.057 Uiso 1 1 calc R . . C88 C 0.2329(3) 0.81586(18) 0.10352(18) 0.0321(10) Uani 1 1 d . . . H88A H 0.1714 0.7968 0.0682 0.038 Uiso 1 1 calc R . . C89 C 0.0513(3) 0.69297(17) 0.06895(16) 0.0220(8) Uani 1 1 d . . . C90 C -0.0385(4) 0.7247(2) 0.05584(19) 0.0509(13) Uani 1 1 d . . . H90A H -0.0652 0.7642 0.0923 0.061 Uiso 1 1 calc R . . C91 C -0.0902(4) 0.7000(2) -0.0097(2) 0.0628(16) Uani 1 1 d . . . H91A H -0.1494 0.7238 -0.0178 0.075 Uiso 1 1 calc R . . C92 C -0.0572(4) 0.6419(2) -0.06258(19) 0.0435(11) Uani 1 1 d . . . H92A H -0.0945 0.6241 -0.1071 0.052 Uiso 1 1 calc R . . C93 C 0.0306(4) 0.60975(19) -0.05031(19) 0.0426(11) Uani 1 1 d . . . H93A H 0.0548 0.5693 -0.0868 0.051 Uiso 1 1 calc R . . C94 C 0.0852(3) 0.63519(18) 0.01463(18) 0.0358(10) Uani 1 1 d . . . H94A H 0.1471 0.6123 0.0217 0.043 Uiso 1 1 calc R . . C95 C 0.0536(3) 0.95892(17) 0.31619(16) 0.0211(8) Uani 1 1 d . . . C96 C 0.1687(3) 0.95090(19) 0.32780(19) 0.0323(10) Uani 1 1 d . . . H96A H 0.1924 0.9054 0.3106 0.039 Uiso 1 1 calc R . . C97 C 0.2503(4) 1.0088(2) 0.3645(2) 0.0428(11) Uani 1 1 d . . . H97A H 0.3290 1.0027 0.3725 0.051 Uiso 1 1 calc R . . C98 C 0.2171(4) 1.07484(19) 0.38905(19) 0.0368(10) Uani 1 1 d . . . H98A H 0.2728 1.1143 0.4141 0.044 Uiso 1 1 calc R . . C99 C 0.1035(3) 1.08399(19) 0.37743(18) 0.0329(10) Uani 1 1 d . . . H99A H 0.0808 1.1297 0.3941 0.039 Uiso 1 1 calc R . . C100 C 0.0222(3) 1.02664(17) 0.34150(17) 0.0268(9) Uani 1 1 d . . . H10D H -0.0564 1.0334 0.3339 0.032 Uiso 1 1 calc R . . C101 C -0.1034(3) 0.89326(17) 0.19674(16) 0.0218(8) Uani 1 1 d U . . C102 C -0.0333(3) 0.92749(18) 0.17009(17) 0.0268(9) Uani 1 1 d . . . H10E H 0.0404 0.9511 0.1932 0.032 Uiso 1 1 calc R . . C103 C -0.0689(4) 0.92794(19) 0.11023(17) 0.0354(10) Uani 1 1 d . . . H10F H -0.0194 0.9518 0.0927 0.042 Uiso 1 1 calc R . . C104 C -0.1754(4) 0.8941(2) 0.07569(18) 0.0352(10) Uani 1 1 d . . . H10G H -0.1992 0.8941 0.0343 0.042 Uiso 1 1 calc R . . C105 C -0.2474(3) 0.86012(18) 0.10209(17) 0.0309(10) Uani 1 1 d . . . H10H H -0.3211 0.8369 0.0787 0.037 Uiso 1 1 calc R . . C106 C -0.2130(3) 0.85960(17) 0.16213(17) 0.0279(9) Uani 1 1 d . . . H10I H -0.2633 0.8365 0.1800 0.033 Uiso 1 1 calc R . . C107 C -0.1731(3) 0.90519(17) 0.32410(16) 0.0212(8) Uani 1 1 d . . . C108 C -0.2513(3) 0.95122(18) 0.32500(18) 0.0312(9) Uani 1 1 d . . . H10J H -0.2443 0.9704 0.2945 0.037 Uiso 1 1 calc R . . C109 C -0.3386(3) 0.9695(2) 0.3691(2) 0.0393(11) Uani 1 1 d . . . H10K H -0.3906 1.0011 0.3687 0.047 Uiso 1 1 calc R . . C110 C -0.3506(3) 0.9423(2) 0.4138(2) 0.0384(10) Uani 1 1 d . . . H11A H -0.4110 0.9546 0.4440 0.046 Uiso 1 1 calc R . . C111 C -0.2739(3) 0.89709(19) 0.41401(19) 0.0372(10) Uani 1 1 d . . . H11B H -0.2805 0.8787 0.4451 0.045 Uiso 1 1 calc R . . C112 C -0.1874(3) 0.87840(18) 0.36925(18) 0.0290(9) Uani 1 1 d . . . H11C H -0.1363 0.8463 0.3694 0.035 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 0.0177(2) 0.0140(2) 0.0166(2) 0.00490(19) -0.00102(19) 0.0029(2) Ni2 0.0188(3) 0.0159(2) 0.0195(2) 0.0070(2) -0.0015(2) 0.0017(2) Al1 0.0246(6) 0.0162(6) 0.0218(6) 0.0090(5) 0.0012(5) 0.0037(5) Al2 0.0210(6) 0.0221(6) 0.0255(6) -0.0016(5) -0.0047(5) 0.0040(5) Al3 0.0271(6) 0.0222(6) 0.0212(6) 0.0106(5) -0.0014(5) 0.0021(5) Al4 0.0197(6) 0.0228(6) 0.0388(7) 0.0108(5) -0.0025(5) -0.0004(5) P1 0.0227(5) 0.0176(5) 0.0149(5) 0.0069(4) 0.0001(4) 0.0050(4) P2 0.0194(5) 0.0132(5) 0.0174(5) 0.0050(4) 0.0006(4) 0.0019(4) P3 0.0206(5) 0.0163(5) 0.0183(5) 0.0074(4) -0.0021(4) 0.0017(4) P4 0.0217(5) 0.0182(5) 0.0190(5) 0.0074(4) -0.0014(4) 0.0034(4) C1 0.039(2) 0.022(2) 0.042(2) 0.0241(19) 0.010(2) 0.0058(19) C2 0.047(3) 0.023(2) 0.028(2) 0.0176(18) 0.009(2) 0.013(2) C3 0.036(2) 0.031(2) 0.029(2) 0.0181(19) -0.0054(19) 0.008(2) C4 0.032(2) 0.029(2) 0.034(2) 0.0236(19) 0.0068(19) 0.0142(19) C5 0.041(3) 0.018(2) 0.031(2) 0.0159(17) 0.0090(19) 0.0105(19) C6 0.058(3) 0.035(3) 0.065(3) 0.030(2) 0.019(3) -0.001(2) C7 0.068(3) 0.048(3) 0.032(2) 0.026(2) 0.013(2) 0.020(2) C8 0.047(3) 0.053(3) 0.034(2) 0.022(2) -0.007(2) 0.011(2) C9 0.035(2) 0.042(3) 0.045(3) 0.025(2) 0.006(2) 0.016(2) C10 0.057(3) 0.020(2) 0.035(2) 0.0118(18) 0.011(2) 0.008(2) C11 0.036(3) 0.038(3) 0.038(3) -0.014(2) -0.025(2) 0.021(2) C12 0.017(2) 0.052(3) 0.053(3) -0.024(3) -0.010(2) 0.012(2) C13 0.020(2) 0.049(3) 0.043(3) -0.016(2) 0.001(2) -0.012(2) C14 0.024(2) 0.030(2) 0.029(2) -0.0096(19) -0.0067(19) -0.0043(19) C15 0.027(2) 0.031(2) 0.024(2) -0.0061(18) -0.0141(18) 0.0090(19) C16 0.096(4) 0.058(3) 0.053(3) -0.004(3) -0.041(3) 0.050(3) C17 0.028(3) 0.091(4) 0.076(4) -0.028(3) -0.011(3) 0.026(3) C18 0.041(3) 0.076(4) 0.076(4) -0.012(3) 0.027(3) -0.024(3) C19 0.049(3) 0.027(2) 0.038(2) 0.0008(19) 0.004(2) -0.005(2) C20 0.048(3) 0.034(2) 0.025(2) 0.0074(19) -0.013(2) 0.011(2) C21 0.028(2) 0.023(2) 0.0145(18) 0.0074(16) 0.0011(16) 0.0103(17) C22 0.039(3) 0.030(2) 0.025(2) 0.0090(18) 0.0115(19) 0.013(2) C23 0.051(3) 0.045(3) 0.035(2) 0.015(2) 0.022(2) 0.019(2) C24 0.080(4) 0.035(3) 0.028(2) 0.012(2) 0.025(2) 0.034(2) C25 0.063(3) 0.026(2) 0.023(2) 0.0098(18) 0.006(2) 0.015(2) C26 0.034(2) 0.024(2) 0.021(2) 0.0084(17) 0.0012(17) 0.0097(18) C27 0.020(2) 0.0193(19) 0.0165(18) 0.0069(15) 0.0012(15) 0.0030(16) C28 0.037(2) 0.029(2) 0.027(2) 0.0129(18) -0.0021(19) -0.002(2) C29 0.041(3) 0.033(2) 0.039(2) 0.014(2) 0.006(2) -0.011(2) C30 0.023(2) 0.040(3) 0.022(2) -0.0037(19) 0.0035(18) -0.006(2) C31 0.021(2) 0.040(2) 0.026(2) 0.0066(19) -0.0020(18) 0.006(2) C32 0.027(2) 0.024(2) 0.026(2) 0.0117(17) 0.0024(17) 0.0054(18) C33 0.024(2) 0.029(2) 0.022(2) 0.0153(17) -0.0008(16) 0.0043(17) C34 0.052(3) 0.034(2) 0.024(2) 0.0137(19) 0.001(2) 0.014(2) C35 0.076(3) 0.058(3) 0.022(2) 0.022(2) -0.002(2) 0.022(3) C36 0.055(3) 0.055(3) 0.044(3) 0.035(2) -0.004(2) 0.016(2) C37 0.043(3) 0.033(2) 0.043(3) 0.024(2) 0.001(2) 0.009(2) C38 0.031(2) 0.029(2) 0.025(2) 0.0149(18) 0.0006(18) 0.0067(18) C39 0.024(2) 0.0147(18) 0.0159(19) 0.0033(15) 0.0029(16) 0.0045(16) C40 0.028(2) 0.026(2) 0.0177(19) 0.0056(16) 0.0046(17) -0.0002(18) C41 0.021(2) 0.030(2) 0.025(2) 0.0031(18) 0.0000(17) -0.0031(18) C42 0.028(2) 0.032(2) 0.025(2) 0.0087(18) -0.0056(18) 0.0042(19) C43 0.038(3) 0.029(2) 0.018(2) 0.0090(17) -0.0026(18) 0.0003(19) C44 0.021(2) 0.022(2) 0.026(2) 0.0108(17) 0.0034(17) 0.0028(17) C45 0.022(2) 0.0149(18) 0.0188(19) 0.0066(15) 0.0080(16) 0.0047(16) C46 0.021(2) 0.019(2) 0.035(2) 0.0119(17) 0.0023(17) 0.0037(17) C47 0.031(2) 0.032(2) 0.037(2) 0.018(2) 0.0041(19) 0.0121(19) C48 0.049(3) 0.029(2) 0.044(3) 0.024(2) 0.015(2) 0.018(2) C49 0.061(3) 0.014(2) 0.034(2) 0.0104(18) 0.005(2) -0.002(2) C50 0.037(2) 0.021(2) 0.023(2) 0.0095(17) 0.0021(18) -0.0008(18) C51 0.0175(19) 0.0163(19) 0.0227(19) 0.0091(16) -0.0007(16) 0.0017(16) C52 0.028(2) 0.025(2) 0.037(2) 0.0154(18) 0.0074(19) 0.0073(18) C53 0.037(3) 0.031(2) 0.057(3) 0.026(2) 0.009(2) -0.004(2) C54 0.024(2) 0.045(3) 0.046(3) 0.030(2) 0.008(2) 0.002(2) C55 0.028(2) 0.031(2) 0.025(2) 0.0128(18) 0.0063(17) 0.0072(18) C56 0.025(2) 0.0184(19) 0.024(2) 0.0103(16) 0.0047(17) 0.0027(17) C57 0.039(3) 0.028(2) 0.027(2) 0.0134(18) -0.0062(19) 0.008(2) C58 0.055(3) 0.028(2) 0.030(2) 0.0204(19) -0.014(2) -0.008(2) C59 0.037(2) 0.045(3) 0.021(2) 0.022(2) -0.0100(19) -0.012(2) C60 0.030(2) 0.033(2) 0.019(2) 0.0129(17) -0.0024(17) -0.0043(19) C61 0.030(2) 0.032(2) 0.019(2) 0.0146(17) -0.0060(17) 0.0004(19) C62 0.059(3) 0.047(3) 0.044(3) 0.017(2) -0.004(2) 0.026(2) C63 0.099(4) 0.038(3) 0.058(3) 0.031(2) -0.027(3) -0.009(3) C64 0.042(3) 0.062(3) 0.040(3) 0.029(2) -0.001(2) -0.017(2) C65 0.040(3) 0.031(2) 0.024(2) 0.0021(18) 0.0056(19) 0.001(2) C66 0.029(2) 0.042(3) 0.035(2) 0.017(2) -0.0022(19) 0.001(2) C67 0.028(2) 0.024(2) 0.053(3) 0.004(2) -0.014(2) -0.009(2) C68 0.033(3) 0.025(2) 0.072(3) 0.022(2) -0.011(2) -0.011(2) C69 0.027(2) 0.044(3) 0.059(3) 0.025(2) -0.001(2) -0.014(2) C70 0.016(2) 0.040(3) 0.058(3) 0.015(2) -0.007(2) -0.006(2) C71 0.025(2) 0.031(2) 0.048(3) 0.006(2) -0.014(2) -0.008(2) C72 0.058(3) 0.030(3) 0.066(3) -0.005(2) -0.010(3) 0.001(2) C73 0.057(3) 0.043(3) 0.117(5) 0.050(3) -0.020(3) -0.014(3) C74 0.037(3) 0.075(4) 0.081(4) 0.042(3) 0.004(3) -0.017(3) C75 0.026(3) 0.055(3) 0.072(3) 0.015(3) -0.003(2) 0.005(2) C76 0.048(3) 0.054(3) 0.059(3) 0.016(3) -0.024(3) -0.003(2) C77 0.020(2) 0.0167(18) 0.0154(18) 0.0062(15) -0.0037(15) 0.0013(16) C78 0.027(2) 0.024(2) 0.036(2) 0.0157(18) 0.0060(18) 0.0096(18) C79 0.040(3) 0.027(2) 0.049(3) 0.024(2) 0.010(2) 0.006(2) C80 0.036(2) 0.021(2) 0.040(2) 0.0134(19) 0.000(2) 0.0141(19) C81 0.023(2) 0.031(2) 0.045(3) 0.018(2) 0.0013(19) 0.0102(19) C82 0.025(2) 0.028(2) 0.034(2) 0.0204(18) 0.0019(18) 0.0035(18) C83 0.030(2) 0.0152(18) 0.0191(19) 0.0062(16) 0.0034(17) 0.0043(17) C84 0.029(2) 0.028(2) 0.032(2) 0.0138(18) 0.0006(18) -0.0010(19) C85 0.035(3) 0.026(2) 0.044(3) 0.004(2) -0.004(2) -0.010(2) C86 0.062(3) 0.026(2) 0.045(3) 0.012(2) 0.019(2) -0.014(2) C87 0.078(4) 0.030(2) 0.031(2) 0.014(2) 0.010(2) -0.010(2) C88 0.047(3) 0.019(2) 0.026(2) 0.0082(17) 0.0001(19) -0.0024(19) C89 0.024(2) 0.0172(19) 0.0195(19) 0.0042(16) -0.0002(16) 0.0012(16) C90 0.061(3) 0.050(3) 0.023(2) -0.003(2) -0.009(2) 0.036(2) C91 0.065(3) 0.075(3) 0.026(2) 0.000(2) -0.012(2) 0.048(3) C92 0.053(3) 0.043(3) 0.022(2) 0.005(2) -0.014(2) 0.011(2) C93 0.059(3) 0.031(2) 0.023(2) -0.0015(18) -0.007(2) 0.020(2) C94 0.041(3) 0.031(2) 0.026(2) 0.0043(18) -0.0060(19) 0.014(2) C95 0.026(2) 0.0193(19) 0.0178(19) 0.0089(16) 0.0000(16) 0.0008(17) C96 0.028(2) 0.022(2) 0.047(3) 0.0181(19) -0.006(2) -0.0050(19) C97 0.034(3) 0.038(3) 0.062(3) 0.030(2) -0.015(2) -0.003(2) C98 0.048(3) 0.024(2) 0.034(2) 0.0133(19) -0.005(2) -0.016(2) C99 0.046(3) 0.017(2) 0.030(2) 0.0070(17) 0.008(2) 0.000(2) C100 0.031(2) 0.020(2) 0.027(2) 0.0092(17) 0.0044(18) 0.0015(18) C101 0.026(2) 0.0189(18) 0.0182(18) 0.0057(15) -0.0011(15) 0.0114(16) C102 0.037(2) 0.026(2) 0.0158(19) 0.0062(17) 0.0032(17) 0.0118(18) C103 0.047(3) 0.042(3) 0.020(2) 0.0140(19) 0.013(2) 0.018(2) C104 0.048(3) 0.040(2) 0.014(2) 0.0071(18) 0.0016(19) 0.023(2) C105 0.034(2) 0.027(2) 0.020(2) 0.0002(17) -0.0086(18) 0.0116(19) C106 0.035(2) 0.022(2) 0.023(2) 0.0061(17) 0.0040(18) 0.0130(18) C107 0.021(2) 0.0165(19) 0.0190(19) 0.0027(16) -0.0009(16) -0.0004(16) C108 0.030(2) 0.030(2) 0.028(2) 0.0088(18) -0.0002(18) 0.0075(19) C109 0.028(2) 0.036(2) 0.040(3) 0.005(2) -0.001(2) 0.011(2) C110 0.021(2) 0.035(2) 0.039(3) 0.002(2) 0.0059(19) -0.003(2) C111 0.038(3) 0.036(2) 0.033(2) 0.012(2) 0.009(2) 0.002(2) C112 0.028(2) 0.022(2) 0.034(2) 0.0104(18) 0.0052(18) 0.0063(18) _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 P2 2.1267(10) . ? Ni1 P1 2.1294(10) . ? Ni1 Al1 2.2121(11) . ? Ni1 Al2 2.2178(11) . ? Ni2 P4 2.1302(10) . ? Ni2 P3 2.1326(10) . ? Ni2 Al4 2.2132(11) . ? Ni2 Al3 2.2178(11) . ? Al1 C5 2.253(3) . ? Al1 C1 2.259(3) . ? Al1 C2 2.269(4) . ? Al1 C3 2.275(3) . ? Al1 C4 2.276(3) . ? Al2 C11 2.260(4) . ? Al2 C15 2.263(4) . ? Al2 C12 2.272(4) . ? Al2 C14 2.276(4) . ? Al2 C13 2.281(4) . ? Al3 C58 2.253(4) . ? Al3 C59 2.262(4) . ? Al3 C57 2.276(4) . ? Al3 C61 2.291(3) . ? Al3 C60 2.292(3) . ? Al4 C69 2.253(4) . ? Al4 C68 2.260(4) . ? Al4 C70 2.273(4) . ? Al4 C67 2.277(4) . ? Al4 C71 2.294(4) . ? P1 C33 1.851(3) . ? P1 C21 1.862(3) . ? P1 C27 1.862(3) . ? P2 C45 1.847(3) . ? P2 C39 1.847(3) . ? P2 C51 1.853(3) . ? P3 C83 1.840(4) . ? P3 C89 1.843(3) . ? P3 C77 1.853(3) . ? P4 C101 1.847(3) . ? P4 C95 1.850(3) . ? P4 C107 1.855(4) . ? C1 C2 1.422(5) . ? C1 C5 1.423(5) . ? C1 C6 1.499(5) . ? C2 C3 1.420(5) . ? C2 C7 1.505(5) . ? C3 C4 1.423(5) . ? C3 C8 1.506(5) . ? C4 C5 1.424(5) . ? C4 C9 1.502(5) . ? C5 C10 1.508(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.411(7) . ? C11 C15 1.428(5) . ? C11 C16 1.505(6) . ? C12 C13 1.425(6) . ? C12 C17 1.514(6) . ? C13 C14 1.421(5) . ? C13 C18 1.499(6) . ? C14 C15 1.411(5) . ? C14 C19 1.510(5) . ? C15 C20 1.499(5) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C26 1.377(4) . ? C21 C22 1.390(5) . ? C22 C23 1.383(5) . ? C22 H22A 0.9500 . ? C23 C24 1.389(5) . ? C23 H23A 0.9500 . ? C24 C25 1.382(5) . ? C24 H24A 0.9500 . ? C25 C26 1.393(5) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C27 C28 1.377(5) . ? C27 C32 1.398(4) . ? C28 C29 1.392(5) . ? C28 H28A 0.9500 . ? C29 C30 1.369(5) . ? C29 H29A 0.9500 . ? C30 C31 1.369(5) . ? C30 H30A 0.9500 . ? C31 C32 1.381(5) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? C33 C34 1.388(5) . ? C33 C38 1.394(5) . ? C34 C35 1.396(5) . ? C34 H34A 0.9500 . ? C35 C36 1.374(5) . ? C35 H35A 0.9500 . ? C36 C37 1.384(5) . ? C36 H36A 0.9500 . ? C37 C38 1.387(4) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C39 C44 1.382(4) . ? C39 C40 1.398(5) . ? C40 C41 1.389(4) . ? C40 H40A 0.9500 . ? C41 C42 1.383(5) . ? C41 H41A 0.9500 . ? C42 C43 1.378(5) . ? C42 H42A 0.9500 . ? C43 C44 1.398(4) . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? C45 C50 1.388(4) . ? C45 C46 1.392(4) . ? C46 C47 1.381(4) . ? C46 H46A 0.9500 . ? C47 C48 1.378(5) . ? C47 H47A 0.9500 . ? C48 C49 1.375(5) . ? C48 H48A 0.9500 . ? C49 C50 1.387(5) . ? C49 H49A 0.9500 . ? C50 H50A 0.9500 . ? C51 C56 1.389(4) . ? C51 C52 1.395(4) . ? C52 C53 1.374(5) . ? C52 H52A 0.9500 . ? C53 C54 1.372(5) . ? C53 H53A 0.9500 . ? C54 C55 1.384(5) . ? C54 H54A 0.9500 . ? C55 C56 1.381(5) . ? C55 H55A 0.9500 . ? C56 H56A 0.9500 . ? C57 C58 1.415(5) . ? C57 C61 1.417(5) . ? C57 C62 1.494(5) . ? C58 C59 1.433(5) . ? C58 C63 1.512(5) . ? C59 C60 1.417(5) . ? C59 C64 1.505(5) . ? C60 C61 1.424(5) . ? C60 C65 1.512(5) . ? C61 C66 1.505(5) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 C71 1.414(5) . ? C67 C68 1.420(6) . ? C67 C72 1.513(6) . ? C68 C69 1.423(6) . ? C68 C73 1.509(5) . ? C69 C70 1.411(5) . ? C69 C74 1.507(6) . ? C70 C71 1.427(6) . ? C70 C75 1.502(5) . ? C71 C76 1.507(5) . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 C82 1.381(5) . ? C77 C78 1.389(5) . ? C78 C79 1.381(5) . ? C78 H78A 0.9500 . ? C79 C80 1.378(5) . ? C79 H79A 0.9500 . ? C80 C81 1.387(5) . ? C80 H80A 0.9500 . ? C81 C82 1.392(5) . ? C81 H81A 0.9500 . ? C82 H82A 0.9500 . ? C83 C88 1.385(4) . ? C83 C84 1.396(4) . ? C84 C85 1.391(5) . ? C84 H84A 0.9500 . ? C85 C86 1.378(5) . ? C85 H85A 0.9500 . ? C86 C87 1.375(5) . ? C86 H86A 0.9500 . ? C87 C88 1.380(5) . ? C87 H87A 0.9500 . ? C88 H88A 0.9500 . ? C89 C94 1.376(5) . ? C89 C90 1.383(5) . ? C90 C91 1.388(5) . ? C90 H90A 0.9500 . ? C91 C92 1.361(5) . ? C91 H91A 0.9500 . ? C92 C93 1.363(5) . ? C92 H92A 0.9500 . ? C93 C94 1.387(5) . ? C93 H93A 0.9500 . ? C94 H94A 0.9500 . ? C95 C96 1.382(5) . ? C95 C100 1.397(4) . ? C96 C97 1.394(5) . ? C96 H96A 0.9500 . ? C97 C98 1.373(5) . ? C97 H97A 0.9500 . ? C98 C99 1.373(5) . ? C98 H98A 0.9500 . ? C99 C100 1.382(5) . ? C99 H99A 0.9500 . ? C100 H10D 0.9500 . ? C101 C102 1.382(5) . ? C101 C106 1.408(5) . ? C102 C103 1.383(4) . ? C102 H10E 0.9500 . ? C103 C104 1.380(5) . ? C103 H10F 0.9500 . ? C104 C105 1.386(5) . ? C104 H10G 0.9500 . ? C105 C106 1.384(4) . ? C105 H10H 0.9500 . ? C106 H10I 0.9500 . ? C107 C112 1.385(5) . ? C107 C108 1.395(5) . ? C108 C109 1.378(5) . ? C108 H10J 0.9500 . ? C109 C110 1.380(5) . ? C109 H10K 0.9500 . ? C110 C111 1.377(5) . ? C110 H11A 0.9500 . ? C111 C112 1.380(5) . ? C111 H11B 0.9500 . ? C112 H11C 0.9500 . ? 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 P2 Ni1 P1 123.47(4) . . ? P2 Ni1 Al1 104.50(4) . . ? P1 Ni1 Al1 109.61(4) . . ? P2 Ni1 Al2 109.58(4) . . ? P1 Ni1 Al2 105.61(4) . . ? Al1 Ni1 Al2 102.13(4) . . ? P4 Ni2 P3 123.18(4) . . ? P4 Ni2 Al4 105.37(4) . . ? P3 Ni2 Al4 106.47(4) . . ? P4 Ni2 Al3 108.76(4) . . ? P3 Ni2 Al3 107.92(4) . . ? Al4 Ni2 Al3 103.39(4) . . ? Ni1 Al1 C5 147.28(10) . . ? Ni1 Al1 C1 146.66(11) . . ? C5 Al1 C1 36.76(12) . . ? Ni1 Al1 C2 147.59(10) . . ? C5 Al1 C2 61.05(13) . . ? C1 Al1 C2 36.60(12) . . ? Ni1 Al1 C3 148.82(10) . . ? C5 Al1 C3 60.79(13) . . ? C1 Al1 C3 60.90(13) . . ? C2 Al1 C3 36.42(13) . . ? Ni1 Al1 C4 148.32(11) . . ? C5 Al1 C4 36.64(12) . . ? C1 Al1 C4 61.28(13) . . ? C2 Al1 C4 61.05(13) . . ? C3 Al1 C4 36.43(12) . . ? Ni1 Al2 C11 138.38(14) . . ? Ni1 Al2 C15 141.40(12) . . ? C11 Al2 C15 36.80(13) . . ? Ni1 Al2 C12 146.59(12) . . ? C11 Al2 C12 36.29(17) . . ? C15 Al2 C12 60.82(16) . . ? Ni1 Al2 C14 152.82(11) . . ? C11 Al2 C14 60.73(15) . . ? C15 Al2 C14 36.23(14) . . ? C12 Al2 C14 60.51(15) . . ? Ni1 Al2 C13 156.89(14) . . ? C11 Al2 C13 60.88(19) . . ? C15 Al2 C13 60.84(16) . . ? C12 Al2 C13 36.48(16) . . ? C14 Al2 C13 36.33(14) . . ? Ni2 Al3 C58 151.30(11) . . ? Ni2 Al3 C59 144.11(11) . . ? C58 Al3 C59 37.02(14) . . ? Ni2 Al3 C57 153.13(11) . . ? C58 Al3 C57 36.42(13) . . ? C59 Al3 C57 61.27(14) . . ? Ni2 Al3 C61 147.37(10) . . ? C58 Al3 C61 60.39(13) . . ? C59 Al3 C61 60.63(13) . . ? C57 Al3 C61 36.16(12) . . ? Ni2 Al3 C60 142.33(10) . . ? C58 Al3 C60 60.72(13) . . ? C59 Al3 C60 36.26(12) . . ? C57 Al3 C60 60.66(13) . . ? C61 Al3 C60 36.20(12) . . ? Ni2 Al4 C69 151.42(12) . . ? Ni2 Al4 C68 149.16(12) . . ? C69 Al4 C68 36.76(15) . . ? Ni2 Al4 C70 148.27(12) . . ? C69 Al4 C70 36.32(14) . . ? C68 Al4 C70 60.99(15) . . ? Ni2 Al4 C67 145.18(13) . . ? C69 Al4 C67 60.88(16) . . ? C68 Al4 C67 36.46(14) . . ? C70 Al4 C67 60.81(15) . . ? Ni2 Al4 C71 145.04(13) . . ? C69 Al4 C71 60.41(16) . . ? C68 Al4 C71 60.41(15) . . ? C70 Al4 C71 36.40(14) . . ? C67 Al4 C71 36.02(13) . . ? C33 P1 C21 101.75(15) . . ? C33 P1 C27 100.60(15) . . ? C21 P1 C27 97.30(15) . . ? C33 P1 Ni1 116.24(12) . . ? C21 P1 Ni1 119.08(12) . . ? C27 P1 Ni1 118.39(11) . . ? C45 P2 C39 102.43(15) . . ? C45 P2 C51 98.41(15) . . ? C39 P2 C51 101.03(15) . . ? C45 P2 Ni1 117.40(11) . . ? C39 P2 Ni1 114.07(11) . . ? C51 P2 Ni1 120.50(11) . . ? C83 P3 C89 99.69(15) . . ? C83 P3 C77 102.20(15) . . ? C89 P3 C77 99.48(14) . . ? C83 P3 Ni2 115.51(11) . . ? C89 P3 Ni2 118.05(12) . . ? C77 P3 Ni2 118.74(11) . . ? C101 P4 C95 100.53(15) . . ? C101 P4 C107 101.63(15) . . ? C95 P4 C107 99.16(15) . . ? C101 P4 Ni2 114.12(11) . . ? C95 P4 Ni2 119.18(11) . . ? C107 P4 Ni2 119.07(11) . . ? C2 C1 C5 107.7(3) . . ? C2 C1 C6 126.9(4) . . ? C5 C1 C6 125.4(3) . . ? C2 C1 Al1 72.1(2) . . ? C5 C1 Al1 71.36(19) . . ? C6 C1 Al1 120.1(3) . . ? C3 C2 C1 107.9(3) . . ? C3 C2 C7 125.6(4) . . ? C1 C2 C7 126.4(4) . . ? C3 C2 Al1 72.1(2) . . ? C1 C2 Al1 71.3(2) . . ? C7 C2 Al1 123.8(2) . . ? C2 C3 C4 108.6(3) . . ? C2 C3 C8 124.8(4) . . ? C4 C3 C8 126.6(4) . . ? C2 C3 Al1 71.5(2) . . ? C4 C3 Al1 71.8(2) . . ? C8 C3 Al1 121.7(2) . . ? C3 C4 C5 107.2(3) . . ? C3 C4 C9 127.5(4) . . ? C5 C4 C9 125.3(3) . . ? C3 C4 Al1 71.7(2) . . ? C5 C4 Al1 70.8(2) . . ? C9 C4 Al1 122.0(2) . . ? C1 C5 C4 108.6(3) . . ? C1 C5 C10 125.1(3) . . ? C4 C5 C10 126.3(3) . . ? C1 C5 Al1 71.88(19) . . ? C4 C5 Al1 72.59(19) . . ? C10 C5 Al1 122.4(2) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C15 107.9(4) . . ? C12 C11 C16 126.8(4) . . ? C15 C11 C16 125.1(5) . . ? C12 C11 Al2 72.3(2) . . ? C15 C11 Al2 71.7(2) . . ? C16 C11 Al2 118.6(3) . . ? C11 C12 C13 108.4(4) . . ? C11 C12 C17 127.1(5) . . ? C13 C12 C17 124.4(5) . . ? C11 C12 Al2 71.4(2) . . ? C13 C12 Al2 72.1(2) . . ? C17 C12 Al2 122.9(3) . . ? C14 C13 C12 107.3(4) . . ? C14 C13 C18 126.3(5) . . ? C12 C13 C18 126.4(4) . . ? C14 C13 Al2 71.6(2) . . ? C12 C13 Al2 71.4(2) . . ? C18 C13 Al2 125.2(3) . . ? C15 C14 C13 108.7(4) . . ? C15 C14 C19 125.2(4) . . ? C13 C14 C19 126.1(4) . . ? C15 C14 Al2 71.4(2) . . ? C13 C14 Al2 72.0(2) . . ? C19 C14 Al2 122.4(3) . . ? C14 C15 C11 107.7(4) . . ? C14 C15 C20 125.9(3) . . ? C11 C15 C20 126.3(4) . . ? C14 C15 Al2 72.4(2) . . ? C11 C15 Al2 71.5(2) . . ? C20 C15 Al2 122.6(2) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C26 C21 C22 118.8(3) . . ? C26 C21 P1 119.8(3) . . ? C22 C21 P1 121.3(3) . . ? C23 C22 C21 120.9(4) . . ? C23 C22 H22A 119.6 . . ? C21 C22 H22A 119.6 . . ? C22 C23 C24 119.8(4) . . ? C22 C23 H23A 120.1 . . ? C24 C23 H23A 120.1 . . ? C25 C24 C23 119.9(4) . . ? C25 C24 H24A 120.1 . . ? C23 C24 H24A 120.1 . . ? C24 C25 C26 119.6(4) . . ? C24 C25 H25A 120.2 . . ? C26 C25 H25A 120.2 . . ? C21 C26 C25 121.1(4) . . ? C21 C26 H26A 119.5 . . ? C25 C26 H26A 119.5 . . ? C28 C27 C32 117.9(3) . . ? C28 C27 P1 125.0(3) . . ? C32 C27 P1 117.1(2) . . ? C27 C28 C29 120.1(3) . . ? C27 C28 H28A 120.0 . . ? C29 C28 H28A 120.0 . . ? C30 C29 C28 121.5(4) . . ? C30 C29 H29A 119.3 . . ? C28 C29 H29A 119.3 . . ? C29 C30 C31 118.9(4) . . ? C29 C30 H30A 120.5 . . ? C31 C30 H30A 120.5 . . ? C30 C31 C32 120.3(4) . . ? C30 C31 H31A 119.8 . . ? C32 C31 H31A 119.8 . . ? C31 C32 C27 121.3(3) . . ? C31 C32 H32A 119.4 . . ? C27 C32 H32A 119.4 . . ? C34 C33 C38 118.4(3) . . ? C34 C33 P1 124.2(3) . . ? C38 C33 P1 117.3(3) . . ? C33 C34 C35 120.6(4) . . ? C33 C34 H34A 119.7 . . ? C35 C34 H34A 119.7 . . ? C36 C35 C34 120.1(4) . . ? C36 C35 H35A 119.9 . . ? C34 C35 H35A 119.9 . . ? C35 C36 C37 120.1(4) . . ? C35 C36 H36A 120.0 . . ? C37 C36 H36A 120.0 . . ? C36 C37 C38 119.8(4) . . ? C36 C37 H37A 120.1 . . ? C38 C37 H37A 120.1 . . ? C37 C38 C33 121.0(3) . . ? C37 C38 H38A 119.5 . . ? C33 C38 H38A 119.5 . . ? C44 C39 C40 118.1(3) . . ? C44 C39 P2 125.0(3) . . ? C40 C39 P2 116.6(2) . . ? C41 C40 C39 121.3(3) . . ? C41 C40 H40A 119.4 . . ? C39 C40 H40A 119.4 . . ? C42 C41 C40 119.6(4) . . ? C42 C41 H41A 120.2 . . ? C40 C41 H41A 120.2 . . ? C43 C42 C41 120.1(3) . . ? C43 C42 H42A 120.0 . . ? C41 C42 H42A 120.0 . . ? C42 C43 C44 119.9(3) . . ? C42 C43 H43A 120.0 . . ? C44 C43 H43A 120.0 . . ? C39 C44 C43 121.0(3) . . ? C39 C44 H44A 119.5 . . ? C43 C44 H44A 119.5 . . ? C50 C45 C46 118.1(3) . . ? C50 C45 P2 124.9(3) . . ? C46 C45 P2 116.8(2) . . ? C47 C46 C45 121.1(3) . . ? C47 C46 H46A 119.4 . . ? C45 C46 H46A 119.4 . . ? C48 C47 C46 119.8(3) . . ? C48 C47 H47A 120.1 . . ? C46 C47 H47A 120.1 . . ? C49 C48 C47 120.1(3) . . ? C49 C48 H48A 120.0 . . ? C47 C48 H48A 120.0 . . ? C48 C49 C50 120.1(4) . . ? C48 C49 H49A 119.9 . . ? C50 C49 H49A 119.9 . . ? C49 C50 C45 120.7(3) . . ? C49 C50 H50A 119.6 . . ? C45 C50 H50A 119.6 . . ? C56 C51 C52 117.7(3) . . ? C56 C51 P2 122.0(3) . . ? C52 C51 P2 120.3(3) . . ? C53 C52 C51 121.0(3) . . ? C53 C52 H52A 119.5 . . ? C51 C52 H52A 119.5 . . ? C54 C53 C52 120.4(4) . . ? C54 C53 H53A 119.8 . . ? C52 C53 H53A 119.8 . . ? C53 C54 C55 119.8(4) . . ? C53 C54 H54A 120.1 . . ? C55 C54 H54A 120.1 . . ? C56 C55 C54 119.7(3) . . ? C56 C55 H55A 120.2 . . ? C54 C55 H55A 120.2 . . ? C55 C56 C51 121.3(3) . . ? C55 C56 H56A 119.4 . . ? C51 C56 H56A 119.4 . . ? C58 C57 C61 107.6(3) . . ? C58 C57 C62 126.3(4) . . ? C61 C57 C62 126.1(4) . . ? C58 C57 Al3 70.9(2) . . ? C61 C57 Al3 72.53(19) . . ? C62 C57 Al3 123.8(3) . . ? C57 C58 C59 108.5(3) . . ? C57 C58 C63 126.2(4) . . ? C59 C58 C63 125.3(4) . . ? C57 C58 Al3 72.7(2) . . ? C59 C58 Al3 71.8(2) . . ? C63 C58 Al3 123.3(2) . . ? C60 C59 C58 107.4(3) . . ? C60 C59 C64 126.9(4) . . ? C58 C59 C64 125.7(4) . . ? C60 C59 Al3 73.0(2) . . ? C58 C59 Al3 71.2(2) . . ? C64 C59 Al3 121.5(2) . . ? C59 C60 C61 108.0(3) . . ? C59 C60 C65 127.0(4) . . ? C61 C60 C65 125.0(3) . . ? C59 C60 Al3 70.73(19) . . ? C61 C60 Al3 71.90(19) . . ? C65 C60 Al3 122.8(2) . . ? C57 C61 C60 108.5(3) . . ? C57 C61 C66 125.6(3) . . ? C60 C61 C66 125.9(3) . . ? C57 C61 Al3 71.31(19) . . ? C60 C61 Al3 71.90(19) . . ? C66 C61 Al3 124.8(2) . . ? C57 C62 H62A 109.5 . . ? C57 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C57 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C58 C63 H63A 109.5 . . ? C58 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C58 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C59 C64 H64A 109.5 . . ? C59 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C59 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C60 C65 H65A 109.5 . . ? C60 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C60 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C61 C66 H66A 109.5 . . ? C61 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C61 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C71 C67 C68 108.0(4) . . ? C71 C67 C72 125.9(4) . . ? C68 C67 C72 126.1(4) . . ? C71 C67 Al4 72.7(2) . . ? C68 C67 Al4 71.1(2) . . ? C72 C67 Al4 123.5(3) . . ? C67 C68 C69 107.7(4) . . ? C67 C68 C73 126.3(4) . . ? C69 C68 C73 126.0(4) . . ? C67 C68 Al4 72.4(2) . . ? C69 C68 Al4 71.3(2) . . ? C73 C68 Al4 122.1(3) . . ? C70 C69 C68 108.5(4) . . ? C70 C69 C74 123.6(4) . . ? C68 C69 C74 127.8(4) . . ? C70 C69 Al4 72.6(2) . . ? C68 C69 Al4 71.9(2) . . ? C74 C69 Al4 123.7(3) . . ? C69 C70 C71 107.5(4) . . ? C69 C70 C75 125.6(4) . . ? C71 C70 C75 126.9(4) . . ? C69 C70 Al4 71.0(2) . . ? C71 C70 Al4 72.6(2) . . ? C75 C70 Al4 123.2(3) . . ? C67 C71 C70 108.3(4) . . ? C67 C71 C76 126.0(4) . . ? C70 C71 C76 125.6(4) . . ? C67 C71 Al4 71.3(2) . . ? C70 C71 Al4 71.0(2) . . ? C76 C71 Al4 124.7(3) . . ? C67 C72 H72A 109.5 . . ? C67 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C67 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C68 C73 H73A 109.5 . . ? C68 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C68 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C69 C74 H74A 109.5 . . ? C69 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C69 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C70 C75 H75A 109.5 . . ? C70 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C70 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C71 C76 H76A 109.5 . . ? C71 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C71 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C82 C77 C78 117.3(3) . . ? C82 C77 P3 124.7(3) . . ? C78 C77 P3 118.0(3) . . ? C79 C78 C77 121.6(4) . . ? C79 C78 H78A 119.2 . . ? C77 C78 H78A 119.2 . . ? C80 C79 C78 120.3(3) . . ? C80 C79 H79A 119.9 . . ? C78 C79 H79A 119.9 . . ? C79 C80 C81 119.5(3) . . ? C79 C80 H80A 120.3 . . ? C81 C80 H80A 120.3 . . ? C80 C81 C82 119.3(4) . . ? C80 C81 H81A 120.3 . . ? C82 C81 H81A 120.3 . . ? C77 C82 C81 122.0(3) . . ? C77 C82 H82A 119.0 . . ? C81 C82 H82A 119.0 . . ? C88 C83 C84 117.4(3) . . ? C88 C83 P3 123.4(3) . . ? C84 C83 P3 118.9(3) . . ? C85 C84 C83 121.0(4) . . ? C85 C84 H84A 119.5 . . ? C83 C84 H84A 119.5 . . ? C86 C85 C84 119.8(4) . . ? C86 C85 H85A 120.1 . . ? C84 C85 H85A 120.1 . . ? C87 C86 C85 120.0(4) . . ? C87 C86 H86A 120.0 . . ? C85 C86 H86A 120.0 . . ? C86 C87 C88 119.8(4) . . ? C86 C87 H87A 120.1 . . ? C88 C87 H87A 120.1 . . ? C87 C88 C83 121.9(4) . . ? C87 C88 H88A 119.0 . . ? C83 C88 H88A 119.0 . . ? C94 C89 C90 117.2(3) . . ? C94 C89 P3 125.5(3) . . ? C90 C89 P3 117.2(3) . . ? C89 C90 C91 121.1(4) . . ? C89 C90 H90A 119.4 . . ? C91 C90 H90A 119.4 . . ? C92 C91 C90 120.8(4) . . ? C92 C91 H91A 119.6 . . ? C90 C91 H91A 119.6 . . ? C91 C92 C93 118.7(3) . . ? C91 C92 H92A 120.7 . . ? C93 C92 H92A 120.7 . . ? C92 C93 C94 121.0(4) . . ? C92 C93 H93A 119.5 . . ? C94 C93 H93A 119.5 . . ? C89 C94 C93 121.1(3) . . ? C89 C94 H94A 119.5 . . ? C93 C94 H94A 119.5 . . ? C96 C95 C100 118.0(3) . . ? C96 C95 P4 118.3(3) . . ? C100 C95 P4 123.7(3) . . ? C95 C96 C97 120.7(4) . . ? C95 C96 H96A 119.6 . . ? C97 C96 H96A 119.6 . . ? C98 C97 C96 120.1(4) . . ? C98 C97 H97A 119.9 . . ? C96 C97 H97A 119.9 . . ? C97 C98 C99 120.1(4) . . ? C97 C98 H98A 119.9 . . ? C99 C98 H98A 119.9 . . ? C98 C99 C100 119.9(4) . . ? C98 C99 H99A 120.0 . . ? C100 C99 H99A 120.0 . . ? C99 C100 C95 121.1(3) . . ? C99 C100 H10D 119.4 . . ? C95 C100 H10D 119.4 . . ? C102 C101 C106 118.5(3) . . ? C102 C101 P4 122.2(3) . . ? C106 C101 P4 118.7(3) . . ? C101 C102 C103 120.9(3) . . ? C101 C102 H10E 119.5 . . ? C103 C102 H10E 119.5 . . ? C104 C103 C102 120.7(4) . . ? C104 C103 H10F 119.7 . . ? C102 C103 H10F 119.7 . . ? C103 C104 C105 119.2(3) . . ? C103 C104 H10G 120.4 . . ? C105 C104 H10G 120.4 . . ? C106 C105 C104 120.7(3) . . ? C106 C105 H10H 119.6 . . ? C104 C105 H10H 119.6 . . ? C105 C106 C101 120.0(4) . . ? C105 C106 H10I 120.0 . . ? C101 C106 H10I 120.0 . . ? C112 C107 C108 117.0(3) . . ? C112 C107 P4 118.4(3) . . ? C108 C107 P4 124.6(3) . . ? C109 C108 C107 121.5(4) . . ? C109 C108 H10J 119.2 . . ? C107 C108 H10J 119.2 . . ? C108 C109 C110 120.3(4) . . ? C108 C109 H10K 119.8 . . ? C110 C109 H10K 119.8 . . ? C111 C110 C109 119.1(4) . . ? C111 C110 H11A 120.4 . . ? C109 C110 H11A 120.4 . . ? C110 C111 C112 120.3(4) . . ? C110 C111 H11B 119.8 . . ? C112 C111 H11B 119.8 . . ? C111 C112 C107 121.7(3) . . ? C111 C112 H11C 119.1 . . ? C107 C112 H11C 119.1 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.414 _refine_diff_density_min -0.296 _refine_diff_density_rms 0.071 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.157 0.436 0.613 36.1 1.3 2 0.395 0.230 0.533 34.4 -0.1 3 0.500 0.500 1.000 13.4 -0.6 4 0.604 0.770 0.467 34.4 -0.1 5 0.843 0.564 0.387 36.1 1.3 _platon_squeeze_details ; ; data_Ni(GaCpstar)2(PCy3)2 _database_code_depnum_ccdc_archive 'CCDC 820862' #TrackingRef '- alle_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H66 Ga2 Ni P2, 2(C10 H15)' _space_group_name_Hall '-P 1' _chemical_formula_sum 'C56 H96 Ga2 Ni P2' _chemical_formula_weight 1029.42 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' P P 0.1023 0.0942 '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' Ga Ga 0.2307 1.6083 '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 11.9834(7) _cell_length_b 16.4634(11) _cell_length_c 17.9050(12) _cell_angle_alpha 87.267(6) _cell_angle_beta 73.270(6) _cell_angle_gamma 85.217(5) _cell_volume 3370.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 200 _cell_measurement_theta_min 2.9 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.014 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 1.145 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8033 _exptl_absorpt_correction_T_max 0.8941 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '560 images at 1.0 deg. in \w and 25 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37627 _diffrn_reflns_av_R_equivalents 0.0933 _diffrn_reflns_av_sigmaI/netI 0.1224 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11846 _reflns_number_gt 7504 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 1.171.13, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _refine_special_details ; Severally disordered cocrystallized solvent molecules have been omited from the diffration data and were not taken into account during the structure refinement. 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^)+(0.0644P)^2^+0.0000P] 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 11846 _refine_ls_number_parameters 550 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1057 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.1531 _refine_ls_wR_factor_gt 0.1377 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _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 Ni1 Ni 0.68340(5) 0.24707(4) 0.20769(4) 0.01687(17) Uani 1 1 d . . . Ga1 Ga 0.58514(5) 0.17637(4) 0.31634(3) 0.02587(17) Uani 1 1 d . . . Ga2 Ga 0.77066(5) 0.33030(3) 0.26884(3) 0.02336(16) Uani 1 1 d . . . P1 P 0.81739(10) 0.16245(7) 0.13513(7) 0.0157(3) Uani 1 1 d . . . P2 P 0.55103(11) 0.32468(8) 0.17001(7) 0.0175(3) Uani 1 1 d . . . C1 C 0.5568(5) 0.1133(4) 0.4410(3) 0.0423(16) Uani 1 1 d . . . C2 C 0.4639(5) 0.1741(4) 0.4480(3) 0.0407(16) Uani 1 1 d . . . C3 C 0.3933(5) 0.1506(4) 0.4026(3) 0.0398(16) Uani 1 1 d . . . C4 C 0.4409(5) 0.0755(4) 0.3685(3) 0.0363(15) Uani 1 1 d . . . C5 C 0.5436(5) 0.0516(3) 0.3918(3) 0.0344(14) Uani 1 1 d . . . C6 C 0.6507(6) 0.1095(4) 0.4824(3) 0.0527(18) Uani 1 1 d . . . H6A H 0.6233 0.0812 0.5331 0.079 Uiso 1 1 calc R . . H6B H 0.6683 0.1649 0.4904 0.079 Uiso 1 1 calc R . . H6C H 0.7215 0.0798 0.4507 0.079 Uiso 1 1 calc R . . C7 C 0.4402(6) 0.2470(4) 0.4985(4) 0.063(2) Uani 1 1 d . . . H7A H 0.3887 0.2332 0.5501 0.094 Uiso 1 1 calc R . . H7B H 0.4023 0.2919 0.4746 0.094 Uiso 1 1 calc R . . H7C H 0.5140 0.2637 0.5040 0.094 Uiso 1 1 calc R . . C8 C 0.2808(5) 0.1973(4) 0.3959(4) 0.0530(19) Uani 1 1 d . . . H8A H 0.2140 0.1772 0.4362 0.079 Uiso 1 1 calc R . . H8B H 0.2712 0.1891 0.3443 0.079 Uiso 1 1 calc R . . H8C H 0.2849 0.2556 0.4028 0.079 Uiso 1 1 calc R . . C9 C 0.3889(5) 0.0267(4) 0.3187(4) 0.0477(17) Uani 1 1 d . . . H9A H 0.3335 -0.0095 0.3524 0.072 Uiso 1 1 calc R . . H9B H 0.4515 -0.0059 0.2823 0.072 Uiso 1 1 calc R . . H9C H 0.3481 0.0639 0.2893 0.072 Uiso 1 1 calc R . . C10 C 0.6167(5) -0.0279(4) 0.3754(4) 0.0486(18) Uani 1 1 d . . . H10A H 0.5816 -0.0693 0.4143 0.073 Uiso 1 1 calc R . . H10B H 0.6959 -0.0206 0.3780 0.073 Uiso 1 1 calc R . . H10C H 0.6204 -0.0456 0.3232 0.073 Uiso 1 1 calc R . . C11 C 0.7765(6) 0.4033(4) 0.3796(4) 0.0448(17) Uani 1 1 d . . . C12 C 0.8740(5) 0.3463(4) 0.3626(4) 0.0418(16) Uani 1 1 d . . . C13 C 0.9484(5) 0.3683(4) 0.2885(4) 0.0351(15) Uani 1 1 d . . . C14 C 0.8997(5) 0.4387(3) 0.2605(3) 0.0348(15) Uani 1 1 d . . . C15 C 0.7910(5) 0.4617(4) 0.3166(4) 0.0410(16) Uani 1 1 d . . . C16 C 0.6759(6) 0.4078(5) 0.4526(4) 0.081(3) Uani 1 1 d . . . H16A H 0.6953 0.4403 0.4910 0.122 Uiso 1 1 calc R . . H16B H 0.6606 0.3526 0.4742 0.122 Uiso 1 1 calc R . . H16C H 0.6062 0.4333 0.4404 0.122 Uiso 1 1 calc R . . C17 C 0.8941(7) 0.2761(5) 0.4154(4) 0.066(2) Uani 1 1 d . . . H17A H 0.9376 0.2936 0.4498 0.099 Uiso 1 1 calc R . . H17B H 0.9391 0.2310 0.3837 0.099 Uiso 1 1 calc R . . H17C H 0.8187 0.2580 0.4470 0.099 Uiso 1 1 calc R . . C18 C 1.0649(5) 0.3251(4) 0.2477(4) 0.057(2) Uani 1 1 d . . . H18A H 1.1271 0.3489 0.2629 0.086 Uiso 1 1 calc R . . H18B H 1.0790 0.3312 0.1911 0.086 Uiso 1 1 calc R . . H18C H 1.0641 0.2670 0.2627 0.086 Uiso 1 1 calc R . . C19 C 0.9549(6) 0.4855(4) 0.1874(4) 0.062(2) Uani 1 1 d . . . H19A H 1.0030 0.5258 0.1988 0.092 Uiso 1 1 calc R . . H19B H 0.8938 0.5134 0.1671 0.092 Uiso 1 1 calc R . . H19C H 1.0040 0.4479 0.1484 0.092 Uiso 1 1 calc R . . C20 C 0.7136(6) 0.5384(4) 0.3151(5) 0.074(3) Uani 1 1 d . . . H20A H 0.7413 0.5828 0.3381 0.112 Uiso 1 1 calc R . . H20B H 0.6331 0.5291 0.3452 0.112 Uiso 1 1 calc R . . H20C H 0.7159 0.5533 0.2610 0.112 Uiso 1 1 calc R . . C21 C 0.7663(4) 0.0704(3) 0.1013(3) 0.0163(11) Uani 1 1 d . . . H21A H 0.8374 0.0366 0.0722 0.020 Uiso 1 1 calc R . . C22 C 0.6995(4) 0.0178(3) 0.1700(3) 0.0217(12) Uani 1 1 d . . . H22A H 0.7492 0.0031 0.2049 0.026 Uiso 1 1 calc R . . H22B H 0.6285 0.0497 0.2003 0.026 Uiso 1 1 calc R . . C23 C 0.6644(4) -0.0599(3) 0.1423(3) 0.0254(12) Uani 1 1 d . . . H23A H 0.7356 -0.0941 0.1159 0.031 Uiso 1 1 calc R . . H23B H 0.6193 -0.0914 0.1879 0.031 Uiso 1 1 calc R . . C24 C 0.5920(4) -0.0405(3) 0.0870(3) 0.0244(12) Uani 1 1 d . . . H24A H 0.5163 -0.0125 0.1152 0.029 Uiso 1 1 calc R . . H24B H 0.5758 -0.0918 0.0667 0.029 Uiso 1 1 calc R . . C25 C 0.6551(4) 0.0142(3) 0.0183(3) 0.0242(12) Uani 1 1 d . . . H25A H 0.7250 -0.0170 -0.0143 0.029 Uiso 1 1 calc R . . H25B H 0.6025 0.0298 -0.0145 0.029 Uiso 1 1 calc R . . C26 C 0.6925(4) 0.0910(3) 0.0457(3) 0.0208(11) Uani 1 1 d . . . H26A H 0.7381 0.1221 -0.0001 0.025 Uiso 1 1 calc R . . H26B H 0.6223 0.1260 0.0722 0.025 Uiso 1 1 calc R . . C27 C 0.9012(4) 0.2077(3) 0.0389(3) 0.0171(11) Uani 1 1 d . . . H27A H 0.8406 0.2288 0.0130 0.021 Uiso 1 1 calc R . . C28 C 0.9875(4) 0.1522(3) -0.0206(3) 0.0190(11) Uani 1 1 d . . . H28A H 1.0545 0.1336 -0.0007 0.023 Uiso 1 1 calc R . . H28B H 0.9486 0.1035 -0.0276 0.023 Uiso 1 1 calc R . . C29 C 1.0316(4) 0.1966(3) -0.0991(3) 0.0242(12) Uani 1 1 d . . . H29A H 0.9651 0.2136 -0.1201 0.029 Uiso 1 1 calc R . . H29B H 1.0868 0.1594 -0.1367 0.029 Uiso 1 1 calc R . . C30 C 1.0931(4) 0.2717(3) -0.0895(3) 0.0263(13) Uani 1 1 d . . . H30A H 1.1637 0.2541 -0.0731 0.032 Uiso 1 1 calc R . . H30B H 1.1182 0.3014 -0.1403 0.032 Uiso 1 1 calc R . . C31 C 1.0127(4) 0.3285(3) -0.0292(3) 0.0238(12) Uani 1 1 d . . . H31A H 0.9475 0.3520 -0.0489 0.029 Uiso 1 1 calc R . . H31B H 1.0567 0.3739 -0.0210 0.029 Uiso 1 1 calc R . . C32 C 0.9628(4) 0.2833(3) 0.0491(3) 0.0193(11) Uani 1 1 d . . . H32A H 0.9064 0.3208 0.0855 0.023 Uiso 1 1 calc R . . H32B H 1.0270 0.2661 0.0722 0.023 Uiso 1 1 calc R . . C33 C 0.9406(4) 0.1154(3) 0.1735(3) 0.0177(11) Uani 1 1 d . . . H33A H 1.0045 0.1535 0.1560 0.021 Uiso 1 1 calc R . . C34 C 0.9960(4) 0.0317(3) 0.1417(3) 0.0221(12) Uani 1 1 d . . . H34A H 0.9364 -0.0088 0.1574 0.026 Uiso 1 1 calc R . . H34B H 1.0217 0.0353 0.0839 0.026 Uiso 1 1 calc R . . C35 C 1.1000(4) 0.0028(3) 0.1710(3) 0.0278(13) Uani 1 1 d . . . H35A H 1.1291 -0.0526 0.1517 0.033 Uiso 1 1 calc R . . H35B H 1.1636 0.0395 0.1495 0.033 Uiso 1 1 calc R . . C36 C 1.0698(5) 0.0009(3) 0.2589(3) 0.0386(15) Uani 1 1 d . . . H36A H 1.1412 -0.0140 0.2752 0.046 Uiso 1 1 calc R . . H36B H 1.0136 -0.0410 0.2805 0.046 Uiso 1 1 calc R . . C37 C 1.0166(5) 0.0836(4) 0.2906(3) 0.0382(15) Uani 1 1 d . . . H37A H 1.0758 0.1242 0.2731 0.046 Uiso 1 1 calc R . . H37B H 0.9936 0.0805 0.3484 0.046 Uiso 1 1 calc R . . C38 C 0.9100(5) 0.1113(3) 0.2632(3) 0.0284(13) Uani 1 1 d . . . H38A H 0.8787 0.1658 0.2840 0.034 Uiso 1 1 calc R . . H38B H 0.8485 0.0728 0.2840 0.034 Uiso 1 1 calc R . . C39 C 0.4276(4) 0.3811(3) 0.2451(3) 0.0201(11) Uani 1 1 d . . . H39A H 0.3640 0.3426 0.2609 0.024 Uiso 1 1 calc R . . C40 C 0.3710(4) 0.4592(3) 0.2192(3) 0.0273(13) Uani 1 1 d . . . H40A H 0.3440 0.4477 0.1737 0.033 Uiso 1 1 calc R . . H40B H 0.4304 0.4997 0.2021 0.033 Uiso 1 1 calc R . . C41 C 0.2671(5) 0.4961(3) 0.2833(3) 0.0350(14) Uani 1 1 d . . . H41A H 0.2362 0.5480 0.2637 0.042 Uiso 1 1 calc R . . H41B H 0.2039 0.4582 0.2973 0.042 Uiso 1 1 calc R . . C42 C 0.3051(5) 0.5120(4) 0.3552(4) 0.0435(16) Uani 1 1 d . . . H42A H 0.2370 0.5337 0.3970 0.052 Uiso 1 1 calc R . . H42B H 0.3640 0.5531 0.3422 0.052 Uiso 1 1 calc R . . C43 C 0.3574(5) 0.4324(4) 0.3837(3) 0.0417(16) Uani 1 1 d . . . H43A H 0.3838 0.4434 0.4295 0.050 Uiso 1 1 calc R . . H43B H 0.2965 0.3929 0.4002 0.050 Uiso 1 1 calc R . . C44 C 0.4601(4) 0.3954(3) 0.3202(3) 0.0275(13) Uani 1 1 d . . . H44A H 0.4886 0.3428 0.3397 0.033 Uiso 1 1 calc R . . H44B H 0.5245 0.4322 0.3081 0.033 Uiso 1 1 calc R . . C45 C 0.6016(4) 0.4090(3) 0.0975(3) 0.0206(11) Uani 1 1 d . . . H45A H 0.5306 0.4402 0.0893 0.025 Uiso 1 1 calc R . . C46 C 0.6753(4) 0.3778(3) 0.0191(3) 0.0226(12) Uani 1 1 d . . . H46A H 0.6298 0.3418 -0.0017 0.027 Uiso 1 1 calc R . . H46B H 0.7453 0.3453 0.0257 0.027 Uiso 1 1 calc R . . C47 C 0.7136(5) 0.4493(3) -0.0393(3) 0.0272(13) Uani 1 1 d . . . H47A H 0.7662 0.4275 -0.0887 0.033 Uiso 1 1 calc R . . H47B H 0.6439 0.4774 -0.0508 0.033 Uiso 1 1 calc R . . C48 C 0.7762(4) 0.5103(3) -0.0080(3) 0.0294(13) Uani 1 1 d . . . H48A H 0.8521 0.4846 -0.0043 0.035 Uiso 1 1 calc R . . H48B H 0.7920 0.5576 -0.0448 0.035 Uiso 1 1 calc R . . C49 C 0.7046(4) 0.5399(3) 0.0718(3) 0.0273(13) Uani 1 1 d . . . H49A H 0.7507 0.5758 0.0921 0.033 Uiso 1 1 calc R . . H49B H 0.6333 0.5721 0.0670 0.033 Uiso 1 1 calc R . . C50 C 0.6704(4) 0.4693(3) 0.1280(3) 0.0256(12) Uani 1 1 d . . . H50A H 0.6216 0.4901 0.1789 0.031 Uiso 1 1 calc R . . H50B H 0.7417 0.4400 0.1363 0.031 Uiso 1 1 calc R . . C51 C 0.4675(4) 0.2689(3) 0.1175(3) 0.0162(11) Uani 1 1 d . . . H51A H 0.5278 0.2448 0.0715 0.019 Uiso 1 1 calc R . . C52 C 0.3780(4) 0.3176(3) 0.0836(3) 0.0265(13) Uani 1 1 d . . . H52A H 0.3130 0.3407 0.1267 0.032 Uiso 1 1 calc R . . H52B H 0.4155 0.3635 0.0508 0.032 Uiso 1 1 calc R . . C53 C 0.3297(5) 0.2644(3) 0.0347(3) 0.0281(13) Uani 1 1 d . . . H53A H 0.3936 0.2450 -0.0110 0.034 Uiso 1 1 calc R . . H53B H 0.2704 0.2972 0.0151 0.034 Uiso 1 1 calc R . . C54 C 0.2742(4) 0.1910(3) 0.0826(3) 0.0257(13) Uani 1 1 d . . . H54A H 0.2050 0.2102 0.1250 0.031 Uiso 1 1 calc R . . H54B H 0.2478 0.1557 0.0488 0.031 Uiso 1 1 calc R . . C55 C 0.3608(4) 0.1424(3) 0.1172(3) 0.0235(12) Uani 1 1 d . . . H55A H 0.4254 0.1179 0.0747 0.028 Uiso 1 1 calc R . . H55B H 0.3216 0.0975 0.1508 0.028 Uiso 1 1 calc R . . C56 C 0.4108(4) 0.1957(3) 0.1656(3) 0.0206(11) Uani 1 1 d . . . H56A H 0.4699 0.1626 0.1851 0.025 Uiso 1 1 calc R . . H56B H 0.3474 0.2156 0.2113 0.025 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 0.0150(3) 0.0164(3) 0.0191(4) -0.0010(3) -0.0042(3) -0.0025(3) Ga1 0.0238(3) 0.0285(3) 0.0231(3) 0.0047(3) -0.0030(3) -0.0058(3) Ga2 0.0212(3) 0.0243(3) 0.0264(3) -0.0071(3) -0.0080(3) -0.0044(3) P1 0.0118(6) 0.0146(7) 0.0214(7) 0.0000(6) -0.0055(6) -0.0028(5) P2 0.0183(7) 0.0138(7) 0.0208(7) -0.0020(6) -0.0057(6) -0.0022(5) C1 0.039(4) 0.068(5) 0.022(3) 0.014(3) -0.009(3) -0.020(3) C2 0.042(4) 0.047(4) 0.027(3) 0.008(3) -0.002(3) -0.009(3) C3 0.028(3) 0.050(4) 0.032(4) 0.007(3) 0.008(3) -0.013(3) C4 0.032(3) 0.048(4) 0.027(3) 0.015(3) -0.003(3) -0.024(3) C5 0.035(3) 0.036(3) 0.030(3) 0.017(3) -0.004(3) -0.017(3) C6 0.060(5) 0.066(5) 0.036(4) 0.012(3) -0.016(3) -0.022(4) C7 0.074(5) 0.069(5) 0.033(4) -0.001(4) 0.008(4) -0.013(4) C8 0.031(4) 0.070(5) 0.047(4) 0.006(4) 0.005(3) -0.001(3) C9 0.048(4) 0.051(4) 0.045(4) 0.009(3) -0.010(3) -0.031(3) C10 0.042(4) 0.043(4) 0.054(4) 0.028(3) -0.005(3) -0.011(3) C11 0.045(4) 0.058(4) 0.037(4) -0.026(3) -0.013(3) -0.015(4) C12 0.046(4) 0.049(4) 0.043(4) -0.013(3) -0.028(3) -0.012(3) C13 0.026(3) 0.038(4) 0.045(4) -0.013(3) -0.013(3) -0.008(3) C14 0.030(3) 0.032(3) 0.043(4) -0.012(3) -0.006(3) -0.021(3) C15 0.041(4) 0.030(3) 0.062(5) -0.028(3) -0.027(4) -0.002(3) C16 0.067(5) 0.125(7) 0.046(5) -0.053(5) 0.011(4) -0.040(5) C17 0.081(6) 0.083(6) 0.054(5) 0.005(4) -0.049(4) -0.019(5) C18 0.029(4) 0.063(5) 0.085(6) -0.024(4) -0.018(4) -0.007(3) C19 0.056(5) 0.059(5) 0.074(5) 0.005(4) -0.017(4) -0.038(4) C20 0.057(5) 0.037(4) 0.140(8) -0.042(5) -0.043(5) 0.008(4) C21 0.012(2) 0.012(3) 0.025(3) -0.005(2) -0.005(2) -0.005(2) C22 0.018(3) 0.017(3) 0.032(3) 0.001(2) -0.010(2) -0.004(2) C23 0.021(3) 0.017(3) 0.039(3) 0.001(2) -0.011(3) -0.004(2) C24 0.023(3) 0.018(3) 0.035(3) -0.010(2) -0.009(3) -0.007(2) C25 0.017(3) 0.032(3) 0.026(3) -0.007(3) -0.010(2) -0.003(2) C26 0.017(3) 0.019(3) 0.028(3) -0.001(2) -0.006(2) -0.007(2) C27 0.017(3) 0.014(3) 0.019(3) -0.002(2) -0.003(2) 0.000(2) C28 0.014(3) 0.017(3) 0.028(3) -0.004(2) -0.008(2) 0.001(2) C29 0.020(3) 0.023(3) 0.028(3) -0.002(2) -0.006(2) 0.002(2) C30 0.018(3) 0.033(3) 0.025(3) 0.005(3) -0.002(2) -0.004(2) C31 0.019(3) 0.018(3) 0.034(3) 0.001(2) -0.006(2) -0.005(2) C32 0.013(2) 0.018(3) 0.026(3) -0.005(2) -0.003(2) -0.001(2) C33 0.013(2) 0.019(3) 0.023(3) -0.005(2) -0.008(2) -0.003(2) C34 0.016(3) 0.019(3) 0.033(3) 0.001(2) -0.010(2) 0.000(2) C35 0.018(3) 0.021(3) 0.048(4) 0.006(3) -0.017(3) 0.005(2) C36 0.039(4) 0.036(4) 0.049(4) 0.007(3) -0.027(3) -0.004(3) C37 0.044(4) 0.044(4) 0.036(4) -0.004(3) -0.029(3) 0.006(3) C38 0.035(3) 0.022(3) 0.027(3) 0.000(2) -0.008(3) 0.003(3) C39 0.014(3) 0.023(3) 0.027(3) -0.005(2) -0.010(2) -0.001(2) C40 0.026(3) 0.026(3) 0.030(3) -0.005(3) -0.008(3) 0.000(2) C41 0.036(3) 0.029(3) 0.039(4) -0.009(3) -0.011(3) 0.009(3) C42 0.036(3) 0.042(4) 0.047(4) -0.025(3) -0.002(3) 0.005(3) C43 0.035(3) 0.056(4) 0.032(4) -0.017(3) -0.008(3) 0.009(3) C44 0.029(3) 0.029(3) 0.023(3) -0.009(3) -0.004(3) 0.002(3) C45 0.021(3) 0.013(3) 0.031(3) 0.002(2) -0.012(2) -0.003(2) C46 0.017(3) 0.021(3) 0.031(3) 0.004(2) -0.009(2) -0.003(2) C47 0.026(3) 0.027(3) 0.026(3) 0.006(3) -0.004(3) -0.003(2) C48 0.019(3) 0.019(3) 0.047(4) 0.007(3) -0.003(3) -0.004(2) C49 0.022(3) 0.015(3) 0.045(4) 0.004(3) -0.009(3) -0.006(2) C50 0.024(3) 0.023(3) 0.031(3) 0.001(2) -0.008(3) -0.008(2) C51 0.011(2) 0.016(3) 0.023(3) 0.000(2) -0.007(2) 0.001(2) C52 0.023(3) 0.021(3) 0.035(3) 0.001(2) -0.007(3) -0.003(2) C53 0.031(3) 0.023(3) 0.038(3) 0.005(3) -0.023(3) -0.005(2) C54 0.021(3) 0.018(3) 0.044(3) -0.010(3) -0.018(3) -0.002(2) C55 0.021(3) 0.017(3) 0.036(3) -0.003(2) -0.013(3) -0.006(2) C56 0.021(3) 0.019(3) 0.022(3) -0.003(2) -0.006(2) -0.003(2) _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 P2 2.1908(14) . ? Ni1 P1 2.1921(14) . ? Ni1 Ga2 2.2829(8) . ? Ni1 Ga1 2.2847(8) . ? Ga1 C1 2.361(6) . ? Ga1 C2 2.387(6) . ? Ga1 C5 2.411(5) . ? Ga1 C3 2.430(5) . ? Ga1 C4 2.453(5) . ? Ga2 C11 2.387(5) . ? Ga2 C12 2.391(5) . ? Ga2 C13 2.393(5) . ? Ga2 C15 2.420(5) . ? Ga2 C14 2.429(5) . ? P1 C21 1.870(4) . ? P1 C27 1.882(5) . ? P1 C33 1.896(5) . ? P2 C45 1.870(5) . ? P2 C51 1.872(5) . ? P2 C39 1.898(5) . ? C1 C2 1.415(8) . ? C1 C5 1.423(8) . ? C1 C6 1.512(8) . ? C2 C3 1.417(8) . ? C2 C7 1.496(8) . ? C3 C4 1.407(8) . ? C3 C8 1.529(8) . ? C4 C5 1.430(8) . ? C4 C9 1.517(8) . ? C5 C10 1.504(8) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.406(9) . ? C11 C15 1.428(9) . ? C11 C16 1.502(8) . ? C12 C13 1.419(8) . ? C12 C17 1.506(9) . ? C13 C14 1.391(8) . ? C13 C18 1.512(8) . ? C14 C15 1.432(8) . ? C14 C19 1.495(8) . ? C15 C20 1.508(8) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C26 1.522(6) . ? C21 C22 1.532(6) . ? C21 H21A 1.0000 . ? C22 C23 1.527(6) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.501(7) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.539(7) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.524(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.529(6) . ? C27 C32 1.543(6) . ? C27 H27A 1.0000 . ? C28 C29 1.526(7) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.531(7) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.522(7) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.538(7) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.538(6) . ? C33 C38 1.541(7) . ? C33 H33A 1.0000 . ? C34 C35 1.520(6) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.509(7) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.518(8) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.524(7) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.519(7) . ? C39 C44 1.537(7) . ? C39 H39A 1.0000 . ? C40 C41 1.535(7) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.524(8) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.534(8) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.521(7) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.515(7) . ? C45 C50 1.552(6) . ? C45 H45A 1.0000 . ? C46 C47 1.544(7) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.519(7) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.518(7) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.505(7) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.531(6) . ? C51 C56 1.535(6) . ? C51 H51A 1.0000 . ? C52 C53 1.523(7) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.532(7) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.512(7) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.530(6) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? 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 P2 Ni1 P1 126.38(5) . . ? P2 Ni1 Ga2 106.21(4) . . ? P1 Ni1 Ga2 109.05(4) . . ? P2 Ni1 Ga1 106.33(4) . . ? P1 Ni1 Ga1 107.82(4) . . ? Ga2 Ni1 Ga1 97.17(3) . . ? Ni1 Ga1 C1 155.74(15) . . ? Ni1 Ga1 C2 150.31(16) . . ? C1 Ga1 C2 34.7(2) . . ? Ni1 Ga1 C5 151.78(15) . . ? C1 Ga1 C5 34.7(2) . . ? C2 Ga1 C5 57.4(2) . . ? Ni1 Ga1 C3 144.74(15) . . ? C1 Ga1 C3 56.9(2) . . ? C2 Ga1 C3 34.19(19) . . ? C5 Ga1 C3 56.7(2) . . ? Ni1 Ga1 C4 145.61(14) . . ? C1 Ga1 C4 56.8(2) . . ? C2 Ga1 C4 56.5(2) . . ? C5 Ga1 C4 34.18(18) . . ? C3 Ga1 C4 33.49(19) . . ? Ni1 Ga2 C11 152.04(16) . . ? Ni1 Ga2 C12 149.01(16) . . ? C11 Ga2 C12 34.2(2) . . ? Ni1 Ga2 C13 147.38(14) . . ? C11 Ga2 C13 56.9(2) . . ? C12 Ga2 C13 34.5(2) . . ? Ni1 Ga2 C15 151.95(15) . . ? C11 Ga2 C15 34.5(2) . . ? C12 Ga2 C15 57.1(2) . . ? C13 Ga2 C15 56.7(2) . . ? Ni1 Ga2 C14 149.09(14) . . ? C11 Ga2 C14 57.0(2) . . ? C12 Ga2 C14 56.7(2) . . ? C13 Ga2 C14 33.52(19) . . ? C15 Ga2 C14 34.35(19) . . ? C21 P1 C27 100.4(2) . . ? C21 P1 C33 101.4(2) . . ? C27 P1 C33 101.3(2) . . ? C21 P1 Ni1 117.08(15) . . ? C27 P1 Ni1 114.24(15) . . ? C33 P1 Ni1 119.56(15) . . ? C45 P2 C51 100.2(2) . . ? C45 P2 C39 100.7(2) . . ? C51 P2 C39 101.1(2) . . ? C45 P2 Ni1 117.98(16) . . ? C51 P2 Ni1 113.88(15) . . ? C39 P2 Ni1 119.87(16) . . ? C2 C1 C5 108.6(5) . . ? C2 C1 C6 126.9(6) . . ? C5 C1 C6 124.4(6) . . ? C2 C1 Ga1 73.7(3) . . ? C5 C1 Ga1 74.6(3) . . ? C6 C1 Ga1 121.2(4) . . ? C1 C2 C3 107.6(6) . . ? C1 C2 C7 126.1(6) . . ? C3 C2 C7 126.2(6) . . ? C1 C2 Ga1 71.7(3) . . ? C3 C2 Ga1 74.6(3) . . ? C7 C2 Ga1 122.5(4) . . ? C4 C3 C2 108.6(5) . . ? C4 C3 C8 126.2(6) . . ? C2 C3 C8 125.2(6) . . ? C4 C3 Ga1 74.1(3) . . ? C2 C3 Ga1 71.2(3) . . ? C8 C3 Ga1 123.1(4) . . ? C3 C4 C5 108.2(5) . . ? C3 C4 C9 125.8(6) . . ? C5 C4 C9 126.0(6) . . ? C3 C4 Ga1 72.4(3) . . ? C5 C4 Ga1 71.3(3) . . ? C9 C4 Ga1 124.2(4) . . ? C1 C5 C4 107.0(5) . . ? C1 C5 C10 125.9(6) . . ? C4 C5 C10 126.8(6) . . ? C1 C5 Ga1 70.8(3) . . ? C4 C5 Ga1 74.5(3) . . ? C10 C5 Ga1 125.1(4) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C15 108.4(6) . . ? C12 C11 C16 127.6(7) . . ? C15 C11 C16 123.9(7) . . ? C12 C11 Ga2 73.0(3) . . ? C15 C11 Ga2 74.0(3) . . ? C16 C11 Ga2 122.0(4) . . ? C11 C12 C13 107.5(6) . . ? C11 C12 C17 125.1(7) . . ? C13 C12 C17 127.3(6) . . ? C11 C12 Ga2 72.7(3) . . ? C13 C12 Ga2 72.8(3) . . ? C17 C12 Ga2 120.7(4) . . ? C14 C13 C12 109.1(5) . . ? C14 C13 C18 125.0(6) . . ? C12 C13 C18 125.9(6) . . ? C14 C13 Ga2 74.6(3) . . ? C12 C13 Ga2 72.7(3) . . ? C18 C13 Ga2 121.2(4) . . ? C13 C14 C15 108.1(5) . . ? C13 C14 C19 126.0(6) . . ? C15 C14 C19 125.8(6) . . ? C13 C14 Ga2 71.8(3) . . ? C15 C14 Ga2 72.5(3) . . ? C19 C14 Ga2 124.6(4) . . ? C11 C15 C14 106.9(6) . . ? C11 C15 C20 125.8(6) . . ? C14 C15 C20 126.9(7) . . ? C11 C15 Ga2 71.5(3) . . ? C14 C15 Ga2 73.2(3) . . ? C20 C15 Ga2 126.3(4) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C26 C21 C22 109.9(4) . . ? C26 C21 P1 113.1(3) . . ? C22 C21 P1 111.8(3) . . ? C26 C21 H21A 107.3 . . ? C22 C21 H21A 107.3 . . ? P1 C21 H21A 107.3 . . ? C23 C22 C21 111.6(4) . . ? C23 C22 H22A 109.3 . . ? C21 C22 H22A 109.3 . . ? C23 C22 H22B 109.3 . . ? C21 C22 H22B 109.3 . . ? H22A C22 H22B 108.0 . . ? C24 C23 C22 111.1(4) . . ? C24 C23 H23A 109.4 . . ? C22 C23 H23A 109.4 . . ? C24 C23 H23B 109.4 . . ? C22 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? C23 C24 C25 111.2(4) . . ? C23 C24 H24A 109.4 . . ? C25 C24 H24A 109.4 . . ? C23 C24 H24B 109.4 . . ? C25 C24 H24B 109.4 . . ? H24A C24 H24B 108.0 . . ? C26 C25 C24 112.1(4) . . ? C26 C25 H25A 109.2 . . ? C24 C25 H25A 109.2 . . ? C26 C25 H25B 109.2 . . ? C24 C25 H25B 109.2 . . ? H25A C25 H25B 107.9 . . ? C21 C26 C25 111.2(4) . . ? C21 C26 H26A 109.4 . . ? C25 C26 H26A 109.4 . . ? C21 C26 H26B 109.4 . . ? C25 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C28 C27 C32 108.8(4) . . ? C28 C27 P1 119.1(3) . . ? C32 C27 P1 112.1(3) . . ? C28 C27 H27A 105.2 . . ? C32 C27 H27A 105.2 . . ? P1 C27 H27A 105.2 . . ? C29 C28 C27 111.2(4) . . ? C29 C28 H28A 109.4 . . ? C27 C28 H28A 109.4 . . ? C29 C28 H28B 109.4 . . ? C27 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? C28 C29 C30 110.1(4) . . ? C28 C29 H29A 109.6 . . ? C30 C29 H29A 109.6 . . ? C28 C29 H29B 109.6 . . ? C30 C29 H29B 109.6 . . ? H29A C29 H29B 108.2 . . ? C31 C30 C29 111.2(4) . . ? C31 C30 H30A 109.4 . . ? C29 C30 H30A 109.4 . . ? C31 C30 H30B 109.4 . . ? C29 C30 H30B 109.4 . . ? H30A C30 H30B 108.0 . . ? C30 C31 C32 111.5(4) . . ? C30 C31 H31A 109.3 . . ? C32 C31 H31A 109.3 . . ? C30 C31 H31B 109.3 . . ? C32 C31 H31B 109.3 . . ? H31A C31 H31B 108.0 . . ? C31 C32 C27 111.7(4) . . ? C31 C32 H32A 109.3 . . ? C27 C32 H32A 109.3 . . ? C31 C32 H32B 109.3 . . ? C27 C32 H32B 109.3 . . ? H32A C32 H32B 107.9 . . ? C34 C33 C38 108.8(4) . . ? C34 C33 P1 116.6(3) . . ? C38 C33 P1 113.8(3) . . ? C34 C33 H33A 105.5 . . ? C38 C33 H33A 105.5 . . ? P1 C33 H33A 105.5 . . ? C35 C34 C33 112.4(4) . . ? C35 C34 H34A 109.1 . . ? C33 C34 H34A 109.1 . . ? C35 C34 H34B 109.1 . . ? C33 C34 H34B 109.1 . . ? H34A C34 H34B 107.9 . . ? C36 C35 C34 112.4(4) . . ? C36 C35 H35A 109.1 . . ? C34 C35 H35A 109.1 . . ? C36 C35 H35B 109.1 . . ? C34 C35 H35B 109.1 . . ? H35A C35 H35B 107.9 . . ? C35 C36 C37 110.4(5) . . ? C35 C36 H36A 109.6 . . ? C37 C36 H36A 109.6 . . ? C35 C36 H36B 109.6 . . ? C37 C36 H36B 109.6 . . ? H36A C36 H36B 108.1 . . ? C36 C37 C38 111.5(4) . . ? C36 C37 H37A 109.3 . . ? C38 C37 H37A 109.3 . . ? C36 C37 H37B 109.3 . . ? C38 C37 H37B 109.3 . . ? H37A C37 H37B 108.0 . . ? C37 C38 C33 111.5(4) . . ? C37 C38 H38A 109.3 . . ? C33 C38 H38A 109.3 . . ? C37 C38 H38B 109.3 . . ? C33 C38 H38B 109.3 . . ? H38A C38 H38B 108.0 . . ? C40 C39 C44 109.9(4) . . ? C40 C39 P2 118.1(3) . . ? C44 C39 P2 112.2(3) . . ? C40 C39 H39A 105.1 . . ? C44 C39 H39A 105.1 . . ? P2 C39 H39A 105.1 . . ? C39 C40 C41 113.4(4) . . ? C39 C40 H40A 108.9 . . ? C41 C40 H40A 108.9 . . ? C39 C40 H40B 108.9 . . ? C41 C40 H40B 108.9 . . ? H40A C40 H40B 107.7 . . ? C42 C41 C40 110.1(5) . . ? C42 C41 H41A 109.6 . . ? C40 C41 H41A 109.6 . . ? C42 C41 H41B 109.6 . . ? C40 C41 H41B 109.6 . . ? H41A C41 H41B 108.1 . . ? C41 C42 C43 109.8(5) . . ? C41 C42 H42A 109.7 . . ? C43 C42 H42A 109.7 . . ? C41 C42 H42B 109.7 . . ? C43 C42 H42B 109.7 . . ? H42A C42 H42B 108.2 . . ? C44 C43 C42 111.5(5) . . ? C44 C43 H43A 109.3 . . ? C42 C43 H43A 109.3 . . ? C44 C43 H43B 109.3 . . ? C42 C43 H43B 109.3 . . ? H43A C43 H43B 108.0 . . ? C43 C44 C39 112.4(4) . . ? C43 C44 H44A 109.1 . . ? C39 C44 H44A 109.1 . . ? C43 C44 H44B 109.1 . . ? C39 C44 H44B 109.1 . . ? H44A C44 H44B 107.9 . . ? C46 C45 C50 109.5(4) . . ? C46 C45 P2 112.5(3) . . ? C50 C45 P2 111.7(3) . . ? C46 C45 H45A 107.6 . . ? C50 C45 H45A 107.6 . . ? P2 C45 H45A 107.6 . . ? C45 C46 C47 110.8(4) . . ? C45 C46 H46A 109.5 . . ? C47 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? C47 C46 H46B 109.5 . . ? H46A C46 H46B 108.1 . . ? C48 C47 C46 112.1(4) . . ? C48 C47 H47A 109.2 . . ? C46 C47 H47A 109.2 . . ? C48 C47 H47B 109.2 . . ? C46 C47 H47B 109.2 . . ? H47A C47 H47B 107.9 . . ? C49 C48 C47 111.8(4) . . ? C49 C48 H48A 109.3 . . ? C47 C48 H48A 109.3 . . ? C49 C48 H48B 109.3 . . ? C47 C48 H48B 109.3 . . ? H48A C48 H48B 107.9 . . ? C50 C49 C48 111.0(4) . . ? C50 C49 H49A 109.4 . . ? C48 C49 H49A 109.4 . . ? C50 C49 H49B 109.4 . . ? C48 C49 H49B 109.4 . . ? H49A C49 H49B 108.0 . . ? C49 C50 C45 111.6(4) . . ? C49 C50 H50A 109.3 . . ? C45 C50 H50A 109.3 . . ? C49 C50 H50B 109.3 . . ? C45 C50 H50B 109.3 . . ? H50A C50 H50B 108.0 . . ? C52 C51 C56 109.3(4) . . ? C52 C51 P2 118.8(3) . . ? C56 C51 P2 112.1(3) . . ? C52 C51 H51A 105.1 . . ? C56 C51 H51A 105.1 . . ? P2 C51 H51A 105.1 . . ? C53 C52 C51 111.5(4) . . ? C53 C52 H52A 109.3 . . ? C51 C52 H52A 109.3 . . ? C53 C52 H52B 109.3 . . ? C51 C52 H52B 109.3 . . ? H52A C52 H52B 108.0 . . ? C52 C53 C54 111.1(4) . . ? C52 C53 H53A 109.4 . . ? C54 C53 H53A 109.4 . . ? C52 C53 H53B 109.4 . . ? C54 C53 H53B 109.4 . . ? H53A C53 H53B 108.0 . . ? C55 C54 C53 110.7(4) . . ? C55 C54 H54A 109.5 . . ? C53 C54 H54A 109.5 . . ? C55 C54 H54B 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 108.1 . . ? C54 C55 C56 111.6(4) . . ? C54 C55 H55A 109.3 . . ? C56 C55 H55A 109.3 . . ? C54 C55 H55B 109.3 . . ? C56 C55 H55B 109.3 . . ? H55A C55 H55B 108.0 . . ? C55 C56 C51 111.6(4) . . ? C55 C56 H56A 109.3 . . ? C51 C56 H56A 109.3 . . ? C55 C56 H56B 109.3 . . ? C51 C56 H56B 109.3 . . ? H56A C56 H56B 108.0 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.639 _refine_diff_density_min -0.414 _refine_diff_density_rms 0.096 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.014 -0.008 0.500 950.1 10.1 _platon_squeeze_details ; ; data_Ni(GaCpstar)2(PMe3)2 _database_code_depnum_ccdc_archive 'CCDC 820863' #TrackingRef '- alle_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _space_group_name_Hall '-C 2yc ' _chemical_formula_moiety 'C6 H18 Ga2 Ni P2, 2(C10 H15)' _chemical_formula_sum 'C26 H48 Ga2 Ni P2' _chemical_formula_weight 620.73 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' P P 0.1023 0.0942 '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' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.8362(13) _cell_length_b 10.2222(3) _cell_length_c 16.8438(18) _cell_angle_alpha 90.00 _cell_angle_beta 121.849(10) _cell_angle_gamma 90.00 _cell_volume 3047.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 105(2) _cell_measurement_reflns_used 200 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 24.99 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.353 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 2.483 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6712 _exptl_absorpt_correction_T_max 0.7582 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 105(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '560 images at 1.0 deg. in \w and 25 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7746 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2666 _reflns_number_gt 2304 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 1.171.13, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0352P)^2^+2.7817P] 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 2666 _refine_ls_number_parameters 141 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0390 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0764 _refine_ls_wR_factor_gt 0.0725 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.097425(17) 0.45797(3) 0.32362(2) 0.01813(12) Uani 1 1 d . . . Ni1 Ni 0.0000 0.31736(5) 0.2500 0.01323(14) Uani 1 2 d S . . P1 P 0.01397(4) 0.21388(7) 0.14966(5) 0.01497(18) Uani 1 1 d . . . C13 C -0.03058(18) 0.0523(3) 0.1123(2) 0.0239(7) Uani 1 1 d . . . H13A H -0.0201 0.0154 0.0666 0.036 Uiso 1 1 calc R . . H13B H -0.0853 0.0610 0.0837 0.036 Uiso 1 1 calc R . . H13C H -0.0101 -0.0058 0.1666 0.036 Uiso 1 1 calc R . . C10 C 0.18325(18) 0.5632(3) 0.2104(2) 0.0251(7) Uani 1 1 d . . . H10A H 0.2240 0.6162 0.2141 0.038 Uiso 1 1 calc R . . H10B H 0.1344 0.5961 0.1597 0.038 Uiso 1 1 calc R . . H10C H 0.1894 0.4719 0.1980 0.038 Uiso 1 1 calc R . . C4 C 0.22880(15) 0.4901(3) 0.38026(19) 0.0167(6) Uani 1 1 d . . . C1 C 0.14755(16) 0.6658(3) 0.3233(2) 0.0184(6) Uani 1 1 d . . . C3 C 0.21529(16) 0.5320(3) 0.4509(2) 0.0174(6) Uani 1 1 d . . . C8 C 0.25127(18) 0.4774(3) 0.5484(2) 0.0287(8) Uani 1 1 d . . . H8A H 0.2994 0.5220 0.5895 0.043 Uiso 1 1 calc R . . H8B H 0.2603 0.3835 0.5473 0.043 Uiso 1 1 calc R . . H8C H 0.2175 0.4913 0.5717 0.043 Uiso 1 1 calc R . . C9 C 0.27995(16) 0.3816(3) 0.3875(2) 0.0259(7) Uani 1 1 d . . . H9A H 0.3309 0.4162 0.4122 0.039 Uiso 1 1 calc R . . H9B H 0.2609 0.3440 0.3254 0.039 Uiso 1 1 calc R . . H9C H 0.2815 0.3138 0.4295 0.039 Uiso 1 1 calc R . . C2 C 0.16533(15) 0.6398(3) 0.41590(19) 0.0180(6) Uani 1 1 d . . . C7 C 0.13922(18) 0.7164(3) 0.4705(2) 0.0274(8) Uani 1 1 d . . . H7A H 0.1748 0.7878 0.5042 0.041 Uiso 1 1 calc R . . H7B H 0.1370 0.6583 0.5153 0.041 Uiso 1 1 calc R . . H7C H 0.0889 0.7526 0.4274 0.041 Uiso 1 1 calc R . . C12 C -0.02078(18) 0.2898(3) 0.0352(2) 0.0262(7) Uani 1 1 d . . . H12A H -0.0106 0.2317 -0.0032 0.039 Uiso 1 1 calc R . . H12B H 0.0050 0.3735 0.0437 0.039 Uiso 1 1 calc R . . H12C H -0.0753 0.3048 0.0039 0.039 Uiso 1 1 calc R . . C6 C 0.09775(18) 0.7717(3) 0.2592(2) 0.0296(8) Uani 1 1 d . . . H6A H 0.1280 0.8502 0.2687 0.044 Uiso 1 1 calc R . . H6B H 0.0585 0.7920 0.2727 0.044 Uiso 1 1 calc R . . H6C H 0.0741 0.7424 0.1943 0.044 Uiso 1 1 calc R . . C5 C 0.18626(16) 0.5718(3) 0.30152(19) 0.0176(6) Uani 1 1 d . . . C11 C 0.11008(17) 0.1709(3) 0.1811(2) 0.0270(8) Uani 1 1 d . . . H11A H 0.1081 0.1242 0.1291 0.041 Uiso 1 1 calc R . . H11B H 0.1335 0.1148 0.2367 0.041 Uiso 1 1 calc R . . H11C H 0.1401 0.2509 0.1945 0.041 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 Ga1 0.01618(19) 0.0192(2) 0.0198(2) -0.00363(14) 0.01009(15) -0.00539(13) Ni1 0.0125(3) 0.0137(3) 0.0133(3) 0.000 0.0067(2) 0.000 P1 0.0147(4) 0.0162(4) 0.0134(4) 0.0000(3) 0.0070(3) 0.0006(3) C13 0.0286(17) 0.0202(18) 0.0226(17) -0.0012(13) 0.0132(15) -0.0018(14) C10 0.0295(17) 0.0315(19) 0.0176(16) -0.0033(14) 0.0147(14) -0.0063(15) C4 0.0139(14) 0.0181(16) 0.0167(15) -0.0020(13) 0.0072(12) -0.0040(12) C1 0.0169(15) 0.0161(16) 0.0196(16) 0.0002(13) 0.0079(13) -0.0039(12) C3 0.0161(14) 0.0195(17) 0.0151(15) -0.0022(13) 0.0072(13) -0.0067(12) C8 0.0296(18) 0.034(2) 0.0161(17) 0.0051(14) 0.0076(15) -0.0056(15) C9 0.0199(16) 0.0261(19) 0.0277(18) -0.0026(15) 0.0099(14) 0.0019(14) C2 0.0167(15) 0.0199(17) 0.0198(15) -0.0050(13) 0.0112(13) -0.0065(12) C7 0.0280(17) 0.0288(19) 0.0313(19) -0.0091(15) 0.0197(16) -0.0054(14) C12 0.0320(18) 0.0271(19) 0.0200(17) 0.0013(14) 0.0142(15) 0.0006(15) C6 0.0274(18) 0.0250(19) 0.0295(19) 0.0035(15) 0.0103(15) -0.0001(15) C5 0.0166(14) 0.0217(17) 0.0147(15) -0.0020(13) 0.0084(13) -0.0060(13) C11 0.0202(16) 0.034(2) 0.0271(18) -0.0043(15) 0.0125(14) 0.0043(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 Ga1 Ni1 2.2512(5) . ? Ga1 C2 2.356(3) . ? Ga1 C1 2.368(3) . ? Ga1 C3 2.375(3) . ? Ga1 C5 2.376(3) . ? Ga1 C4 2.399(3) . ? Ni1 P1 2.1399(8) . ? Ni1 P1 2.1399(8) 2 ? Ni1 Ga1 2.2512(5) 2 ? P1 C11 1.834(3) . ? P1 C13 1.835(3) . ? P1 C12 1.837(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C10 C5 1.506(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C4 C5 1.415(4) . ? C4 C3 1.425(4) . ? C4 C9 1.498(4) . ? C1 C5 1.421(4) . ? C1 C2 1.425(4) . ? C1 C6 1.494(4) . ? C3 C2 1.413(4) . ? C3 C8 1.507(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C2 C7 1.511(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? 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 Ni1 Ga1 C2 156.94(7) . . ? Ni1 Ga1 C1 147.35(7) . . ? C2 Ga1 C1 35.11(9) . . ? Ni1 Ga1 C3 154.54(7) . . ? C2 Ga1 C3 34.76(10) . . ? C1 Ga1 C3 57.93(10) . . ? Ni1 Ga1 C5 140.98(7) . . ? C2 Ga1 C5 58.04(9) . . ? C1 Ga1 C5 34.85(10) . . ? C3 Ga1 C5 57.68(10) . . ? Ni1 Ga1 C4 144.53(7) . . ? C2 Ga1 C4 57.85(10) . . ? C1 Ga1 C4 57.73(10) . . ? C3 Ga1 C4 34.73(9) . . ? C5 Ga1 C4 34.47(10) . . ? P1 Ni1 P1 120.75(5) . 2 ? P1 Ni1 Ga1 106.96(2) . . ? P1 Ni1 Ga1 109.85(2) 2 . ? P1 Ni1 Ga1 109.85(2) . 2 ? P1 Ni1 Ga1 106.96(2) 2 2 ? Ga1 Ni1 Ga1 100.64(3) . 2 ? C11 P1 C13 99.29(15) . . ? C11 P1 C12 99.79(15) . . ? C13 P1 C12 99.93(15) . . ? C11 P1 Ni1 118.22(10) . . ? C13 P1 Ni1 117.42(10) . . ? C12 P1 Ni1 118.55(11) . . ? P1 C13 H13A 109.5 . . ? P1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? P1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C5 C4 C3 107.6(3) . . ? C5 C4 C9 125.4(3) . . ? C3 C4 C9 126.9(3) . . ? C5 C4 Ga1 71.89(15) . . ? C3 C4 Ga1 71.73(16) . . ? C9 C4 Ga1 123.0(2) . . ? C5 C1 C2 107.6(3) . . ? C5 C1 C6 125.2(3) . . ? C2 C1 C6 127.3(3) . . ? C5 C1 Ga1 72.88(16) . . ? C2 C1 Ga1 71.98(16) . . ? C6 C1 Ga1 120.8(2) . . ? C2 C3 C4 108.2(2) . . ? C2 C3 C8 125.2(3) . . ? C4 C3 C8 126.5(3) . . ? C2 C3 Ga1 71.88(16) . . ? C4 C3 Ga1 73.54(16) . . ? C8 C3 Ga1 123.2(2) . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C3 C2 C1 108.1(2) . . ? C3 C2 C7 124.9(3) . . ? C1 C2 C7 126.9(3) . . ? C3 C2 Ga1 73.36(16) . . ? C1 C2 Ga1 72.91(16) . . ? C7 C2 Ga1 121.77(19) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? P1 C12 H12A 109.5 . . ? P1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? P1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C5 C1 108.5(2) . . ? C4 C5 C10 126.1(3) . . ? C1 C5 C10 125.4(3) . . ? C4 C5 Ga1 73.63(15) . . ? C1 C5 Ga1 72.27(16) . . ? C10 C5 Ga1 120.95(19) . . ? P1 C11 H11A 109.5 . . ? P1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.473 _refine_diff_density_min -0.385 _refine_diff_density_rms 0.097 data_Ni(GaCpstar)3(PCy3) _database_code_depnum_ccdc_archive 'CCDC 820864' #TrackingRef '- alle_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _space_group_name_Hall 'I -4bd 2c 3' _chemical_formula_moiety 'C48 H75 Ga3 Ni P' _chemical_formula_sum 'C48 H75 Ga3 Ni P' _chemical_formula_weight 950.92 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' Ga Ga 0.2307 1.6083 '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 cubic _symmetry_space_group_name_H-M 'I -4 3 d' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'y+1/4, -x+3/4, -z+1/4' '-x, -y+1/2, z' '-y+3/4, x+3/4, -z+1/4' 'x, -y, -z+1/2' '-y+1/4, -x+3/4, z+3/4' '-x, y+1/2, -z+1/2' 'y+3/4, x+3/4, z+3/4' 'z, x, y' 'x+1/4, -z+3/4, -y+1/4' '-z, -x+1/2, y' '-x+3/4, z+3/4, -y+1/4' 'z, -x, -y+1/2' '-x+1/4, -z+3/4, y+3/4' '-z, x+1/2, -y+1/2' 'x+3/4, z+3/4, y+3/4' 'y, z, x' 'z+3/4, y+3/4, x+3/4' 'z+3/4, -y+1/4, -x+3/4' '-z+1/4, -y+3/4, x+3/4' '-z+1/4, y+1/4, -x+3/4' 'y, -z, -x+1/2' '-y+1/2, -z, x+1/2' '-y, z+1/2, -x+1/2' 'x+1/2, y+1/2, z+1/2' 'y+3/4, -x+5/4, -z+3/4' '-x+1/2, -y+1, z+1/2' '-y+5/4, x+5/4, -z+3/4' 'x+1/2, -y+1/2, -z+1' '-y+3/4, -x+5/4, z+5/4' '-x+1/2, y+1, -z+1' 'y+5/4, x+5/4, z+5/4' 'z+1/2, x+1/2, y+1/2' 'x+3/4, -z+5/4, -y+3/4' '-z+1/2, -x+1, y+1/2' '-x+5/4, z+5/4, -y+3/4' 'z+1/2, -x+1/2, -y+1' '-x+3/4, -z+5/4, y+5/4' '-z+1/2, x+1, -y+1' 'x+5/4, z+5/4, y+5/4' 'y+1/2, z+1/2, x+1/2' 'z+5/4, y+5/4, x+5/4' 'z+5/4, -y+3/4, -x+5/4' '-z+3/4, -y+5/4, x+5/4' '-z+3/4, y+3/4, -x+5/4' 'y+1/2, -z+1/2, -x+1' '-y+1, -z+1/2, x+1' '-y+1/2, z+1, -x+1' _cell_length_a 26.9627(3) _cell_length_b 26.9627(3) _cell_length_c 26.9627(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 19601.5(4) _cell_formula_units_Z 16 _cell_measurement_temperature 105(2) _cell_measurement_reflns_used 200 _cell_measurement_theta_min 3.38 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.289 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7984 _exptl_absorpt_coefficient_mu 2.072 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6711 _exptl_absorpt_correction_T_max 0.6821 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 105(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 ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63101 _diffrn_reflns_av_R_equivalents 0.0735 _diffrn_reflns_av_sigmaI/netI 0.0294 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.38 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2878 _reflns_number_gt 2473 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 1.171.13, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _refine_special_details ; The moiety number has been reduced to one, since only one molecule is provided. Four restrains concerning C1-C bonds have been applied due to high distortion of the Phenyl-groups. Several attempts to solve the structure in a lower symmetry failed. 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^)+(0.0332P)^2^+7.4881P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(2) _refine_ls_number_reflns 2878 _refine_ls_number_parameters 258 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.0784 _refine_ls_wR_factor_gt 0.0744 _refine_ls_goodness_of_fit_ref 1.147 _refine_ls_restrained_S_all 1.176 _refine_ls_shift/su_max 0.008 _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 -0.023385(17) -0.023385(17) -0.023385(17) 0.03560(19) Uani 1 3 d S . . P1 P 0.02211(4) 0.02211(4) 0.02211(4) 0.0525(5) Uani 1 3 d S A . C1 C 0.0103(2) 0.0136(2) 0.09029(19) 0.0897(19) Uani 1 1 d D . . Ga1 Ga 0.0003(2) -0.10344(16) -0.02406(17) 0.0657(12) Uani 0.602(14) 1 d P A 1 C2 C 0.0225(12) -0.0392(5) 0.1084(10) 0.112(9) Uani 0.495(10) 1 d PD A 1 H2A H 0.0578 -0.0470 0.1018 0.134 Uiso 0.495(10) 1 calc PR A 1 H2B H 0.0017 -0.0637 0.0907 0.134 Uiso 0.495(10) 1 calc PR A 1 C3 C 0.0120(9) -0.0416(10) 0.1652(10) 0.128(9) Uani 0.495(10) 1 d P A 1 H3A H 0.0164 -0.0763 0.1763 0.154 Uiso 0.495(10) 1 calc PR A 1 H3B H 0.0373 -0.0213 0.1825 0.154 Uiso 0.495(10) 1 calc PR A 1 C4 C -0.0338(11) -0.0259(7) 0.1803(6) 0.117(7) Uani 0.495(10) 1 d P A 1 H4A H -0.0381 -0.0315 0.2164 0.140 Uiso 0.495(10) 1 calc PR A 1 H4B H -0.0602 -0.0441 0.1624 0.140 Uiso 0.495(10) 1 calc PR A 1 C5 C -0.0361(9) 0.0293(6) 0.1684(6) 0.130(7) Uani 0.495(10) 1 d P A 1 H5A H -0.0083 0.0467 0.1850 0.156 Uiso 0.495(10) 1 calc PR A 1 H5B H -0.0676 0.0433 0.1813 0.156 Uiso 0.495(10) 1 calc PR A 1 C6 C -0.0331(5) 0.0379(4) 0.1113(4) 0.103(5) Uani 0.495(10) 1 d PD A 1 H6A H -0.0634 0.0247 0.0953 0.123 Uiso 0.495(10) 1 calc PR A 1 H6B H -0.0314 0.0739 0.1045 0.123 Uiso 0.495(10) 1 calc PR A 1 C10 C 0.0467(3) -0.1700(3) -0.0564(3) 0.102(9) Uani 0.602(14) 1 d PG A 1 C11 C -0.0042(3) -0.1830(2) -0.0529(3) 0.081(5) Uani 0.602(14) 1 d PG A 1 C12 C -0.0172(3) -0.18451(18) -0.0019(3) 0.066(3) Uani 0.602(14) 1 d PG A 1 C13 C 0.0257(4) -0.1724(2) 0.0261(2) 0.105(7) Uani 0.602(14) 1 d PG A 1 C14 C 0.0652(3) -0.1635(2) -0.0075(3) 0.089(5) Uani 0.602(14) 1 d PG A 1 C15 C 0.0760(4) -0.1642(4) -0.1038(3) 0.150(9) Uani 0.602(14) 1 d PG A 1 H15A H 0.0923 -0.1956 -0.1119 0.226 Uiso 0.602(14) 1 calc PR A 1 H15B H 0.1011 -0.1383 -0.0993 0.226 Uiso 0.602(14) 1 calc PR A 1 H15C H 0.0536 -0.1548 -0.1308 0.226 Uiso 0.602(14) 1 calc PR A 1 C16 C -0.0385(4) -0.1935(4) -0.0959(4) 0.141(8) Uani 0.602(14) 1 d PG A 1 H16A H -0.0365 -0.2286 -0.1048 0.212 Uiso 0.602(14) 1 calc PR A 1 H16B H -0.0287 -0.1732 -0.1245 0.212 Uiso 0.602(14) 1 calc PR A 1 H16C H -0.0727 -0.1853 -0.0865 0.212 Uiso 0.602(14) 1 calc PR A 1 C17 C -0.0677(3) -0.1968(3) 0.0188(5) 0.155(9) Uani 0.602(14) 1 d PG A 1 H17A H -0.0698 -0.2325 0.0255 0.232 Uiso 0.602(14) 1 calc PR A 1 H17B H -0.0933 -0.1875 -0.0052 0.232 Uiso 0.602(14) 1 calc PR A 1 H17C H -0.0729 -0.1784 0.0498 0.232 Uiso 0.602(14) 1 calc PR A 1 C18 C 0.0288(6) -0.1696(3) 0.0820(2) 0.148(8) Uani 0.602(14) 1 d PG A 1 H18A H 0.0398 -0.2016 0.0951 0.222 Uiso 0.602(14) 1 calc PR A 1 H18B H -0.0040 -0.1615 0.0955 0.222 Uiso 0.602(14) 1 calc PR A 1 H18C H 0.0525 -0.1438 0.0915 0.222 Uiso 0.602(14) 1 calc PR A 1 C19 C 0.1176(3) -0.1494(4) 0.0062(5) 0.206(11) Uani 0.602(14) 1 d PG A 1 H19A H 0.1375 -0.1795 0.0102 0.310 Uiso 0.602(14) 1 calc PR A 1 H19B H 0.1174 -0.1308 0.0374 0.310 Uiso 0.602(14) 1 calc PR A 1 H19C H 0.1319 -0.1288 -0.0201 0.310 Uiso 0.602(14) 1 calc PR A 1 Ga1A Ga -0.0055(4) -0.1023(2) -0.0299(3) 0.0697(16) Uani 0.398(14) 1 d P A 2 C2A C 0.0351(5) 0.0405(4) 0.1298(4) 0.094(4) Uani 0.505(10) 1 d PD A 2 H2AA H 0.0334 0.0764 0.1226 0.112 Uiso 0.505(10) 1 calc PR A 2 H2AB H 0.0705 0.0309 0.1303 0.112 Uiso 0.505(10) 1 calc PR A 2 C3A C 0.0132(8) 0.0311(6) 0.1801(5) 0.108(6) Uani 0.505(10) 1 d P A 2 H3AA H 0.0328 0.0494 0.2052 0.129 Uiso 0.505(10) 1 calc PR A 2 H3AB H -0.0210 0.0445 0.1808 0.129 Uiso 0.505(10) 1 calc PR A 2 C4A C 0.0116(8) -0.0217(9) 0.1942(6) 0.143(8) Uani 0.505(10) 1 d P A 2 H4AA H -0.0048 -0.0248 0.2269 0.172 Uiso 0.505(10) 1 calc PR A 2 H4AB H 0.0460 -0.0341 0.1978 0.172 Uiso 0.505(10) 1 calc PR A 2 C5A C -0.0173(15) -0.0564(9) 0.1547(6) 0.159(11) Uani 0.505(10) 1 d P A 2 H5AA H -0.0534 -0.0498 0.1557 0.191 Uiso 0.505(10) 1 calc PR A 2 H5AB H -0.0117 -0.0920 0.1622 0.191 Uiso 0.505(10) 1 calc PR A 2 C6A C 0.0050(11) -0.0426(4) 0.1015(9) 0.108(8) Uani 0.505(10) 1 d PD A 2 H6AA H -0.0165 -0.0576 0.0757 0.129 Uiso 0.505(10) 1 calc PR A 2 H6AB H 0.0382 -0.0582 0.0985 0.129 Uiso 0.505(10) 1 calc PR A 2 C10A C -0.0367(3) -0.1876(2) -0.0288(4) 0.064(5) Uani 0.398(14) 1 d PG A 2 C11A C -0.0051(4) -0.1811(3) 0.0128(4) 0.090(8) Uani 0.398(14) 1 d PG A 2 C12A C 0.0435(3) -0.1714(4) -0.0049(4) 0.114(11) Uani 0.398(14) 1 d PG A 2 C13A C 0.0420(3) -0.1719(4) -0.0576(4) 0.062(9) Uani 0.398(14) 1 d PG A 2 C14A C -0.0075(3) -0.1819(4) -0.0723(4) 0.077(6) Uani 0.398(14) 1 d PG A 2 C15A C -0.0915(3) -0.1986(4) -0.0272(6) 0.084(5) Uani 0.398(14) 1 d PG A 2 H15D H -0.0966 -0.2346 -0.0254 0.126 Uiso 0.398(14) 1 calc PR A 2 H15E H -0.1074 -0.1856 -0.0572 0.126 Uiso 0.398(14) 1 calc PR A 2 H15F H -0.1062 -0.1828 0.0021 0.126 Uiso 0.398(14) 1 calc PR A 2 C16A C -0.0205(6) -0.1840(5) 0.0666(4) 0.121(8) Uani 0.398(14) 1 d PG A 2 H16D H -0.0177 -0.2184 0.0781 0.181 Uiso 0.398(14) 1 calc PR A 2 H16E H -0.0550 -0.1729 0.0699 0.181 Uiso 0.398(14) 1 calc PR A 2 H16F H 0.0011 -0.1627 0.0866 0.181 Uiso 0.398(14) 1 calc PR A 2 C17A C 0.0889(4) -0.1622(6) 0.0266(6) 0.23(2) Uani 0.398(14) 1 d PG A 2 H17D H 0.1044 -0.1940 0.0350 0.345 Uiso 0.398(14) 1 calc PR A 2 H17E H 0.0791 -0.1451 0.0571 0.345 Uiso 0.398(14) 1 calc PR A 2 H17F H 0.1125 -0.1416 0.0082 0.345 Uiso 0.398(14) 1 calc PR A 2 C18A C 0.0855(4) -0.1633(7) -0.0918(5) 0.128(11) Uani 0.398(14) 1 d PG A 2 H18D H 0.1019 -0.1950 -0.0988 0.192 Uiso 0.398(14) 1 calc PR A 2 H18E H 0.1091 -0.1406 -0.0760 0.192 Uiso 0.398(14) 1 calc PR A 2 H18F H 0.0736 -0.1487 -0.1229 0.192 Uiso 0.398(14) 1 calc PR A 2 C19A C -0.0260(5) -0.1858(6) -0.1250(4) 0.134(10) Uani 0.398(14) 1 d PG A 2 H19D H -0.0246 -0.2205 -0.1359 0.200 Uiso 0.398(14) 1 calc PR A 2 H19E H -0.0051 -0.1655 -0.1467 0.200 Uiso 0.398(14) 1 calc PR A 2 H19F H -0.0603 -0.1739 -0.1268 0.200 Uiso 0.398(14) 1 calc PR A 2 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 0.03560(19) 0.03560(19) 0.03560(19) 0.0027(2) 0.0027(2) 0.0027(2) P1 0.0525(5) 0.0525(5) 0.0525(5) -0.0062(5) -0.0062(5) -0.0062(5) C1 0.118(5) 0.098(4) 0.052(3) -0.014(3) -0.015(3) 0.017(4) Ga1 0.096(3) 0.0433(13) 0.0580(11) 0.0125(9) -0.0009(12) 0.0220(12) C2 0.118(13) 0.161(19) 0.056(11) -0.022(10) -0.063(9) 0.006(11) C3 0.17(2) 0.130(18) 0.088(16) 0.027(12) -0.054(16) -0.060(16) C4 0.20(2) 0.098(12) 0.050(9) 0.018(9) -0.023(12) -0.033(13) C5 0.19(2) 0.108(13) 0.096(11) -0.003(9) 0.022(12) -0.022(12) C6 0.181(15) 0.064(8) 0.064(7) 0.016(6) 0.025(8) 0.010(8) C10 0.111(16) 0.023(9) 0.17(3) -0.010(12) 0.010(18) 0.011(9) C11 0.143(14) 0.027(5) 0.073(8) 0.000(4) -0.004(8) 0.011(8) C12 0.081(7) 0.036(6) 0.080(8) 0.002(5) -0.012(7) 0.017(5) C13 0.21(2) 0.038(6) 0.063(7) 0.005(5) -0.034(10) 0.046(8) C14 0.100(11) 0.046(6) 0.121(14) -0.006(7) 0.007(9) 0.021(6) C15 0.205(19) 0.115(14) 0.131(12) 0.024(10) 0.078(12) 0.115(13) C16 0.158(15) 0.052(7) 0.214(18) -0.051(9) -0.081(13) 0.045(8) C17 0.145(13) 0.064(7) 0.26(2) 0.061(10) 0.068(16) 0.025(8) C18 0.29(2) 0.081(8) 0.077(8) 0.036(6) -0.009(10) 0.036(11) C19 0.095(11) 0.098(11) 0.43(3) 0.011(16) -0.124(16) 0.034(9) Ga1A 0.0635(18) 0.0316(19) 0.114(4) -0.017(2) 0.012(3) 0.0100(14) C2A 0.110(10) 0.115(10) 0.056(7) -0.034(6) -0.017(6) 0.020(7) C3A 0.163(18) 0.103(11) 0.058(8) -0.015(7) 0.005(9) 0.027(11) C4A 0.143(16) 0.21(2) 0.077(11) -0.066(14) -0.024(10) 0.048(14) C5A 0.29(4) 0.153(18) 0.033(8) 0.002(9) -0.009(13) -0.08(2) C6A 0.19(3) 0.099(11) 0.037(8) 0.037(8) -0.032(12) 0.010(11) C10A 0.094(12) 0.025(6) 0.073(12) 0.007(7) -0.001(9) 0.014(7) C11A 0.128(18) 0.055(12) 0.085(13) 0.010(9) -0.055(15) 0.031(11) C12A 0.13(2) 0.072(14) 0.15(3) 0.002(15) -0.08(2) 0.054(13) C13A 0.041(11) 0.072(18) 0.073(18) 0.001(13) -0.003(12) 0.039(10) C14A 0.054(11) 0.049(10) 0.129(15) -0.028(8) 0.024(10) 0.022(8) C15A 0.096(11) 0.065(9) 0.090(11) -0.025(8) -0.006(9) -0.019(8) C16A 0.150(19) 0.096(14) 0.116(15) 0.036(11) -0.030(15) -0.002(13) C17A 0.14(3) 0.085(16) 0.46(6) 0.00(2) -0.20(3) 0.009(16) C18A 0.099(16) 0.089(18) 0.20(3) -0.042(17) 0.039(18) -0.040(14) C19A 0.085(12) 0.104(16) 0.21(2) -0.102(17) -0.009(15) -0.001(11) _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 P1 2.1245(19) . ? Ni1 Ga1A 2.188(6) . ? Ni1 Ga1A 2.188(6) 17 ? Ni1 Ga1A 2.188(6) 9 ? Ni1 Ga1 2.251(5) . ? Ni1 Ga1 2.251(5) 9 ? Ni1 Ga1 2.251(5) 17 ? P1 C1 1.880(5) 17 ? P1 C1 1.880(5) . ? P1 C1 1.880(5) 9 ? C1 C6 1.456(9) . ? C1 C2A 1.451(8) . ? C1 C2 1.541(10) . ? C1 C6A 1.553(9) . ? Ga1 C11 2.286(8) . ? Ga1 C12 2.314(6) . ? Ga1 C10 2.356(9) . ? Ga1 C13 2.400(6) . ? Ga1 C14 2.425(8) . ? C2 C3 1.56(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.37(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.52(2) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.560(17) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C10 C11 1.4200 . ? C10 C14 1.4200 . ? C10 C15 1.5095 . ? C11 C12 1.4200 . ? C11 C16 1.5095 . ? C12 C13 1.4200 . ? C12 C17 1.5095 . ? C13 C14 1.4200 . ? C13 C18 1.5095 . ? C14 C19 1.5095 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? Ga1A C12A 2.383(12) . ? Ga1A C13A 2.391(13) . ? Ga1A C11A 2.419(10) . ? Ga1A C14A 2.433(12) . ? Ga1A C10A 2.450(9) . ? C2A C3A 1.501(18) . ? C2A H2AA 0.9900 . ? C2A H2AB 0.9900 . ? C3A C4A 1.47(3) . ? C3A H3AA 0.9900 . ? C3A H3AB 0.9900 . ? C4A C5A 1.62(2) . ? C4A H4AA 0.9900 . ? C4A H4AB 0.9900 . ? C5A C6A 1.60(3) . ? C5A H5AA 0.9900 . ? C5A H5AB 0.9900 . ? C6A H6AA 0.9900 . ? C6A H6AB 0.9900 . ? C10A C11A 1.4200 . ? C10A C14A 1.4200 . ? C10A C15A 1.5095 . ? C11A C12A 1.4200 . ? C11A C16A 1.5095 . ? C12A C13A 1.4200 . ? C12A C17A 1.5095 . ? C13A C14A 1.4200 . ? C13A C18A 1.5095 . ? C14A C19A 1.5095 . ? C15A H15D 0.9800 . ? C15A H15E 0.9800 . ? C15A H15F 0.9800 . ? C16A H16D 0.9800 . ? C16A H16E 0.9800 . ? C16A H16F 0.9800 . ? C17A H17D 0.9800 . ? C17A H17E 0.9800 . ? C17A H17F 0.9800 . ? C18A H18D 0.9800 . ? C18A H18E 0.9800 . ? C18A H18F 0.9800 . ? C19A H19D 0.9800 . ? C19A H19E 0.9800 . ? C19A H19F 0.9800 . ? 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 P1 Ni1 Ga1A 118.7(3) . . ? P1 Ni1 Ga1A 118.7(3) . 17 ? Ga1A Ni1 Ga1A 98.9(3) . 17 ? P1 Ni1 Ga1A 118.7(3) . 9 ? Ga1A Ni1 Ga1A 98.9(3) . 9 ? Ga1A Ni1 Ga1A 98.9(3) 17 9 ? P1 Ni1 Ga1 113.25(15) . . ? Ga1A Ni1 Ga1 5.5(4) . . ? Ga1A Ni1 Ga1 101.5(3) 17 . ? Ga1A Ni1 Ga1 103.1(3) 9 . ? P1 Ni1 Ga1 113.25(15) . 9 ? Ga1A Ni1 Ga1 101.5(3) . 9 ? Ga1A Ni1 Ga1 103.1(3) 17 9 ? Ga1A Ni1 Ga1 5.5(4) 9 9 ? Ga1 Ni1 Ga1 105.44(17) . 9 ? P1 Ni1 Ga1 113.25(15) . 17 ? Ga1A Ni1 Ga1 103.1(3) . 17 ? Ga1A Ni1 Ga1 5.5(4) 17 17 ? Ga1A Ni1 Ga1 101.5(3) 9 17 ? Ga1 Ni1 Ga1 105.44(17) . 17 ? Ga1 Ni1 Ga1 105.44(17) 9 17 ? C1 P1 C1 105.3(2) 17 . ? C1 P1 C1 105.3(2) 17 9 ? C1 P1 C1 105.3(2) . 9 ? C1 P1 Ni1 113.37(18) 17 . ? C1 P1 Ni1 113.37(18) . . ? C1 P1 Ni1 113.37(18) 9 . ? C6 C1 C2A 81.9(8) . . ? C6 C1 C2 117.6(16) . . ? C2A C1 C2 97.4(9) . . ? C6 C1 C6A 106.9(13) . . ? C2A C1 C6A 112.8(10) . . ? C2 C1 C6A 19.2(16) . . ? C6 C1 P1 117.5(5) . . ? C2A C1 P1 125.4(7) . . ? C2 C1 P1 112.8(13) . . ? C6A C1 P1 109.0(10) . . ? Ni1 Ga1 C11 152.6(3) . . ? Ni1 Ga1 C12 147.8(3) . . ? C11 Ga1 C12 35.95(11) . . ? Ni1 Ga1 C10 152.1(3) . . ? C11 Ga1 C10 35.58(12) . . ? C12 Ga1 C10 58.93(17) . . ? Ni1 Ga1 C13 145.0(3) . . ? C11 Ga1 C13 58.66(14) . . ? C12 Ga1 C13 35.00(9) . . ? C10 Ga1 C13 57.77(16) . . ? Ni1 Ga1 C14 147.5(3) . . ? C11 Ga1 C14 58.29(17) . . ? C12 Ga1 C14 57.94(15) . . ? C10 Ga1 C14 34.52(12) . . ? C13 Ga1 C14 34.23(10) . . ? C1 C2 C3 108(2) . . ? C1 C2 H2A 110.1 . . ? C3 C2 H2A 110.1 . . ? C1 C2 H2B 110.1 . . ? C3 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? C4 C3 C2 116.4(19) . . ? C4 C3 H3A 108.2 . . ? C2 C3 H3A 108.2 . . ? C4 C3 H3B 108.2 . . ? C2 C3 H3B 108.2 . . ? H3A C3 H3B 107.3 . . ? C3 C4 C5 106(2) . . ? C3 C4 H4A 110.5 . . ? C5 C4 H4A 110.5 . . ? C3 C4 H4B 110.5 . . ? C5 C4 H4B 110.5 . . ? H4A C4 H4B 108.7 . . ? C4 C5 C6 110.5(12) . . ? C4 C5 H5A 109.5 . . ? C6 C5 H5A 109.6 . . ? C4 C5 H5B 109.6 . . ? C6 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? C1 C6 C5 111.1(11) . . ? C1 C6 H6A 109.4 . . ? C5 C6 H6A 109.4 . . ? C1 C6 H6B 109.4 . . ? C5 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? C11 C10 C14 108.0 . . ? C11 C10 C15 126.0 . . ? C14 C10 C15 126.0 . . ? C11 C10 Ga1 69.5(2) . . ? C14 C10 Ga1 75.4(2) . . ? C15 C10 Ga1 120.80(19) . . ? C10 C11 C12 108.0 . . ? C10 C11 C16 126.0 . . ? C12 C11 C16 126.0 . . ? C10 C11 Ga1 74.9(3) . . ? C12 C11 Ga1 73.1(2) . . ? C16 C11 Ga1 118.0(2) . . ? C13 C12 C11 108.0 . . ? C13 C12 C17 126.0 . . ? C11 C12 C17 126.0 . . ? C13 C12 Ga1 75.8(3) . . ? C11 C12 Ga1 70.9(2) . . ? C17 C12 Ga1 119.1(3) . . ? C14 C13 C12 108.0 . . ? C14 C13 C18 126.0 . . ? C12 C13 C18 126.0 . . ? C14 C13 Ga1 73.8(2) . . ? C12 C13 Ga1 69.2(3) . . ? C18 C13 Ga1 122.6(2) . . ? C13 C14 C10 108.0 . . ? C13 C14 C19 126.0 . . ? C10 C14 C19 126.0 . . ? C13 C14 Ga1 71.9(2) . . ? C10 C14 Ga1 70.1(2) . . ? C19 C14 Ga1 123.6(2) . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Ni1 Ga1A C12A 149.3(5) . . ? Ni1 Ga1A C13A 155.0(4) . . ? C12A Ga1A C13A 34.61(18) . . ? Ni1 Ga1A C11A 144.8(4) . . ? C12A Ga1A C11A 34.39(15) . . ? C13A Ga1A C11A 57.1(2) . . ? Ni1 Ga1A C14A 153.0(5) . . ? C12A Ga1A C14A 57.0(2) . . ? C13A Ga1A C14A 34.22(17) . . ? C11A Ga1A C14A 56.5(2) . . ? Ni1 Ga1A C10A 146.7(5) . . ? C12A Ga1A C10A 56.8(2) . . ? C13A Ga1A C10A 56.6(2) . . ? C11A Ga1A C10A 33.90(12) . . ? C14A Ga1A C10A 33.81(13) . . ? C1 C2A C3A 113.5(11) . . ? C1 C2A H2AA 108.9 . . ? C3A C2A H2AA 108.9 . . ? C1 C2A H2AB 108.9 . . ? C3A C2A H2AB 108.9 . . ? H2AA C2A H2AB 107.7 . . ? C4A C3A C2A 114.0(12) . . ? C4A C3A H3AA 108.7 . . ? C2A C3A H3AA 108.7 . . ? C4A C3A H3AB 108.7 . . ? C2A C3A H3AB 108.7 . . ? H3AA C3A H3AB 107.6 . . ? C3A C4A C5A 113.7(17) . . ? C3A C4A H4AA 108.8 . . ? C5A C4A H4AA 108.8 . . ? C3A C4A H4AB 108.8 . . ? C5A C4A H4AB 108.8 . . ? H4AA C4A H4AB 107.7 . . ? C4A C5A C6A 105.9(17) . . ? C4A C5A H5AA 110.6 . . ? C6A C5A H5AA 110.5 . . ? C4A C5A H5AB 110.5 . . ? C6A C5A H5AB 110.6 . . ? H5AA C5A H5AB 108.7 . . ? C5A C6A C1 115.9(18) . . ? C5A C6A H6AA 108.3 . . ? C1 C6A H6AA 108.3 . . ? C5A C6A H6AB 108.3 . . ? C1 C6A H6AB 108.3 . . ? H6AA C6A H6AB 107.4 . . ? C11A C10A C14A 108.0 . . ? C11A C10A C15A 126.0 . . ? C14A C10A C15A 126.0 . . ? C11A C10A Ga1A 71.9(4) . . ? C14A C10A Ga1A 72.4(4) . . ? C15A C10A Ga1A 121.4(4) . . ? C12A C11A C10A 108.0 . . ? C12A C11A C16A 126.0 . . ? C10A C11A C16A 126.0 . . ? C12A C11A Ga1A 71.4(4) . . ? C10A C11A Ga1A 74.2(3) . . ? C16A C11A Ga1A 120.2(4) . . ? C13A C12A C11A 108.0 . . ? C13A C12A C17A 126.0 . . ? C11A C12A C17A 126.0 . . ? C13A C12A Ga1A 73.0(4) . . ? C11A C12A Ga1A 74.2(3) . . ? C17A C12A Ga1A 118.7(3) . . ? C14A C13A C12A 108.0 . . ? C14A C13A C18A 126.0 . . ? C12A C13A C18A 126.0 . . ? C14A C13A Ga1A 74.5(3) . . ? C12A C13A Ga1A 72.4(4) . . ? C18A C13A Ga1A 119.0(3) . . ? C13A C14A C10A 108.0 . . ? C13A C14A C19A 126.0 . . ? C10A C14A C19A 126.0 . . ? C13A C14A Ga1A 71.3(4) . . ? C10A C14A Ga1A 73.8(3) . . ? C19A C14A Ga1A 120.7(3) . . ? C10A C15A H15D 109.5 . . ? C10A C15A H15E 109.5 . . ? H15D C15A H15E 109.5 . . ? C10A C15A H15F 109.5 . . ? H15D C15A H15F 109.5 . . ? H15E C15A H15F 109.5 . . ? C11A C16A H16D 109.5 . . ? C11A C16A H16E 109.5 . . ? H16D C16A H16E 109.5 . . ? C11A C16A H16F 109.5 . . ? H16D C16A H16F 109.5 . . ? H16E C16A H16F 109.5 . . ? C12A C17A H17D 109.5 . . ? C12A C17A H17E 109.5 . . ? H17D C17A H17E 109.5 . . ? C12A C17A H17F 109.5 . . ? H17D C17A H17F 109.5 . . ? H17E C17A H17F 109.5 . . ? C13A C18A H18D 109.5 . . ? C13A C18A H18E 109.5 . . ? H18D C18A H18E 109.5 . . ? C13A C18A H18F 109.5 . . ? H18D C18A H18F 109.5 . . ? H18E C18A H18F 109.5 . . ? C14A C19A H19D 109.5 . . ? C14A C19A H19E 109.5 . . ? H19D C19A H19E 109.5 . . ? C14A C19A H19F 109.5 . . ? H19D C19A H19F 109.5 . . ? H19E C19A H19F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.267 _refine_diff_density_min -0.210 _refine_diff_density_rms 0.046