data_global #============================================================================== # 1. SUBMISSION DETAILS #============================================================================== _publ_contact_author_name 'Denis Spasyuk' _publ_contact_author_address ; Universit\'e de Montr\'eal D\'epartement de Chimie C.P. 6128, Succ. Centre-ville Montr\'eal, Qu\'ebec Canada, H3C 3J7 ; _publ_contact_author_phone '+1 514 343 6111 3936' _publ_contact_author_fax '+1 514 343 7586' _publ_contact_author_email 'denis.spasyuk@umontreal.ca' #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) #============================================================================== _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # 3. TITLE AND AUTHOR LIST #============================================================================== _publ_section_title ; Structure of Ni(-iPrPOCsp2NBn)Br ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Spasyuk, Denis' ; D\'epartement de Chimie Universit\'e de Montr\'eal C.P. 6128, Succ. Centre-ville, Montr\'eal, Qu\'ebec Canada H3C 3J7 ; 'Zargarian, Davit' ; D\'epartement de Chimie Universit\'e de Montr\'eal C.P. 6128, Succ. Centre-ville, Montr\'eal, Qu\'ebec Canada H3C 3J7 ; #============================================================================== # 4. TEXT #============================================================================== _publ_section_abstract ; Here should be written a short abstract ; _publ_section_comment ; Here should be written the text of the article ; _publ_section_exptl_prep ; Small details about the preparation of the compound. ; _publ_section_exptl_refinement ; All non-H atoms were refined by full-matrix least-squares with anisotropic displacement parameters. The H atoms were generated geometrically (C-H 0.93 to 0.98, N-H 0.86 and O-H 0.82\%A) and were included in the refinement in the riding model approximation; their temperature factors were set to 1.5 times those of the equivalent isotropic temperature factors of the parent site (methyl) and 1.2 times for others. A final verification of possible voids was performed using the VOID routine of the PLATON program (Spek, 2000). ; _publ_section_figure_captions ; Fig 1 Ortep view of the title compound. Thermal ellipsoids are shown at 30% probability levels. ; _publ_section_table_legends ; Table 1. Selected geometric parameters (\%A, \%) for the title compound. ; _publ_section_references ; Bruker (1997). SHELXTL (1997). Release 5.10; The Complete Software Package for Single Crystal Structure Determination. Bruker AXS Inc., Madison, USA. Bruker (1999a). SAINT Release 6.06. Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, USA. Bruker (1999b). SMART Release 5.059; Bruker Molecular Analysis Research Tool, Bruker AXS Inc., Madison, USA. Flack, H. D. (1983). Acta Cryst. A39, 876-881. Flack, H. D. and Schwarzenbach, D. (1988). Acta Cryst. A44, 499-506. Sheldrick, G. M. (1986). SHELXS86. Program for Crystal Structure solution. University of G\"ottingen, Germany. Sheldrick, G. M. (1996). SADABS, Bruker Area Detector Absorption Corrections. Bruker AXS Inc., Madison, USA. Sheldrick, G. M. (1997a). SHELXS97. Program for Crystal Structure solution. University of G\"ottingen, Germany. Sheldrick, G. M. (1997b). SHELXL97. Program for crystal structure refinement. University of G\"ottingen, Germany. Spek, A. L. (2000). PLATON, 2000 version; Molecular Geometry Program, University of Utrecht, Utrecht, Holland. ; _publ_section_acknowledgements ; We are grateful to the Natural Sciences and Engineering Research Council of Canada and the Minist\`ere de l'Education du Qu\'ebec for financial support. ; data_ds74 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C49 H61 N3 Ni2 O2 P2 ' _chemical_formula_sum 'C49 H61 N3 Ni2 O2 P2' _chemical_formula_weight 903.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1827(7) _cell_length_b 12.4964(9) _cell_length_c 22.2669(17) _cell_angle_alpha 75.612(3) _cell_angle_beta 78.816(3) _cell_angle_gamma 76.488(3) _cell_volume 2381.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9843 _cell_measurement_theta_min 4.63 _cell_measurement_theta_max 69.40 _exptl_crystal_description 'Needle' _exptl_crystal_colour 'Orange' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.260 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 956 _exptl_absorpt_coefficient_mu 1.919 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6821 _exptl_absorpt_correction_T_max 0.8724 _exptl_absorpt_process_details 'Sadabs (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Helios optics' _diffrn_measurement_device_type 'Bruker Microstar' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 43552 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_av_sigmaI/netI 0.0195 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 69.72 _reflns_number_total 8793 _reflns_number_gt 8307 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'Platon Ortep' _computing_publication_material 'LinXTL v. 1.09' _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^)+(0.0941P)^2^+2.6681P] 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 8793 _refine_ls_number_parameters 533 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0545 _refine_ls_R_factor_gt 0.0530 _refine_ls_wR_factor_ref 0.1469 _refine_ls_wR_factor_gt 0.1454 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 0.85198(4) -0.07704(3) 0.245977(18) 0.01772(12) Uani 1 1 d . . . Ni2 Ni 0.87531(4) 0.12798(3) 0.263906(17) 0.01652(12) Uani 1 1 d . . . P1 P 0.92968(7) -0.25911(5) 0.26700(3) 0.02185(15) Uani 1 1 d . . . P2 P 0.80439(7) 0.12123(5) 0.36651(3) 0.01963(15) Uani 1 1 d . . . O1 O 0.8341(2) -0.30527(15) 0.33651(8) 0.0288(4) Uani 1 1 d . . . O2 O 0.9471(2) 0.15644(16) 0.38740(8) 0.0268(4) Uani 1 1 d . . . N1 N 0.7196(2) 0.07295(16) 0.23635(9) 0.0177(4) Uani 1 1 d . . . N2 N 1.0798(2) 0.16846(16) 0.14673(9) 0.0192(4) Uani 1 1 d . . . N3 N 1.0101(2) -0.01001(16) 0.18601(9) 0.0182(4) Uani 1 1 d . . . C1 C 0.6959(3) -0.1190(2) 0.30893(11) 0.0215(5) Uani 1 1 d . . . C2 C 0.7038(3) -0.2257(2) 0.34812(12) 0.0253(5) Uani 1 1 d . . . C3 C 0.5882(4) -0.2545(2) 0.39537(13) 0.0346(6) Uani 1 1 d . . . H3 H 0.5962 -0.3281 0.4211 0.042 Uiso 1 1 calc R . . C4 C 0.4606(3) -0.1719(2) 0.40375(13) 0.0337(6) Uani 1 1 d . . . H4 H 0.3796 -0.1897 0.4357 0.040 Uiso 1 1 calc R . . C5 C 0.4480(3) -0.0636(2) 0.36672(12) 0.0281(5) Uani 1 1 d . . . H5 H 0.3596 -0.0081 0.3734 0.034 Uiso 1 1 calc R . . C6 C 0.5670(3) -0.0374(2) 0.31953(11) 0.0212(5) Uani 1 1 d . . . C7 C 0.5687(3) 0.0752(2) 0.27668(11) 0.0206(5) Uani 1 1 d . . . H7A H 0.5502 0.1340 0.3015 0.025 Uiso 1 1 calc R . . H7B H 0.4877 0.0933 0.2501 0.025 Uiso 1 1 calc R . . C21 C 1.1163(3) -0.3462(2) 0.28078(13) 0.0307(6) Uani 1 1 d . . . H21 H 1.0986 -0.4215 0.3060 0.037 Uiso 1 1 calc R . . C22 C 1.1983(3) -0.2995(2) 0.31894(14) 0.0328(6) Uani 1 1 d . . . H22A H 1.2968 -0.3489 0.3246 0.049 Uiso 1 1 calc R . . H22B H 1.1375 -0.2958 0.3600 0.049 Uiso 1 1 calc R . . H22C H 1.2132 -0.2238 0.2967 0.049 Uiso 1 1 calc R . . C23 C 1.2204(3) -0.3665(2) 0.22054(15) 0.0360(6) Uani 1 1 d . . . H23A H 1.2388 -0.2943 0.1940 0.054 Uiso 1 1 calc R . . H23B H 1.1724 -0.4038 0.1980 0.054 Uiso 1 1 calc R . . H23C H 1.3169 -0.4146 0.2310 0.054 Uiso 1 1 calc R . . C24 C 0.8623(3) -0.3303(2) 0.21732(13) 0.0261(5) Uani 1 1 d . . . H24 H 0.9261 -0.3193 0.1753 0.031 Uiso 1 1 calc R . . C25 C 0.8768(4) -0.4578(2) 0.24378(15) 0.0354(6) Uani 1 1 d . . . H25A H 0.8170 -0.4708 0.2855 0.053 Uiso 1 1 calc R . . H25B H 0.9833 -0.4923 0.2467 0.053 Uiso 1 1 calc R . . H25C H 0.8393 -0.4914 0.2159 0.053 Uiso 1 1 calc R . . C26 C 0.6983(3) -0.2773(2) 0.20819(14) 0.0318(6) Uani 1 1 d . . . H26A H 0.6684 -0.3101 0.1779 0.048 Uiso 1 1 calc R . . H26B H 0.6890 -0.1958 0.1925 0.048 Uiso 1 1 calc R . . H26C H 0.6323 -0.2921 0.2483 0.048 Uiso 1 1 calc R . . C31 C 0.6901(3) 0.1165(2) 0.17054(11) 0.0199(5) Uani 1 1 d . . . H31A H 0.6256 0.0706 0.1617 0.024 Uiso 1 1 calc R . . H31B H 0.7878 0.1048 0.1426 0.024 Uiso 1 1 calc R . . C32 C 0.6149(3) 0.2396(2) 0.15337(11) 0.0202(5) Uani 1 1 d . . . C33 C 0.6317(3) 0.3212(2) 0.18270(12) 0.0237(5) Uani 1 1 d . . . H33 H 0.6863 0.2997 0.2173 0.028 Uiso 1 1 calc R . . C34 C 0.5693(3) 0.4340(2) 0.16168(14) 0.0299(6) Uani 1 1 d . . . H34 H 0.5816 0.4888 0.1822 0.036 Uiso 1 1 calc R . . C35 C 0.4890(3) 0.4679(2) 0.11098(14) 0.0343(6) Uani 1 1 d . . . H35 H 0.4467 0.5451 0.0968 0.041 Uiso 1 1 calc R . . C36 C 0.4717(3) 0.3867(3) 0.08139(13) 0.0338(6) Uani 1 1 d . . . H36 H 0.4178 0.4085 0.0465 0.041 Uiso 1 1 calc R . . C37 C 0.5330(3) 0.2738(2) 0.10266(12) 0.0263(5) Uani 1 1 d . . . H37 H 0.5191 0.2190 0.0825 0.032 Uiso 1 1 calc R . . C41 C 1.0235(3) 0.20187(19) 0.27661(11) 0.0189(5) Uani 1 1 d . . . C42 C 1.0417(3) 0.2061(2) 0.33667(11) 0.0217(5) Uani 1 1 d . . . C43 C 1.1433(3) 0.2607(2) 0.34960(12) 0.0258(5) Uani 1 1 d . . . H43 H 1.1507 0.2605 0.3916 0.031 Uiso 1 1 calc R . . C44 C 1.2340(3) 0.3157(2) 0.29985(13) 0.0253(5) Uani 1 1 d . . . H44 H 1.3069 0.3517 0.3074 0.030 Uiso 1 1 calc R . . C45 C 1.2172(3) 0.3176(2) 0.23861(12) 0.0216(5) Uani 1 1 d . . . H45 H 1.2772 0.3567 0.2043 0.026 Uiso 1 1 calc R . . C46 C 1.1127(3) 0.26240(19) 0.22752(11) 0.0189(5) Uani 1 1 d . . . C47 C 1.0853(3) 0.2754(2) 0.16154(11) 0.0208(5) Uani 1 1 d . . . H47A H 0.9884 0.3285 0.1551 0.025 Uiso 1 1 calc R . . H47B H 1.1669 0.3085 0.1322 0.025 Uiso 1 1 calc R . . C48 C 1.0028(2) 0.09558(19) 0.19000(11) 0.0174(4) Uani 1 1 d . . . C51 C 0.8072(3) -0.0165(2) 0.42058(11) 0.0250(5) Uani 1 1 d . . . H51 H 0.7201 -0.0474 0.4156 0.030 Uiso 1 1 calc R . . C52 C 0.9547(4) -0.0959(3) 0.40091(14) 0.0364(6) Uani 1 1 d . . . H52A H 1.0415 -0.0684 0.4068 0.055 Uiso 1 1 calc R . . H52B H 0.9618 -0.0979 0.3567 0.055 Uiso 1 1 calc R . . H52C H 0.9548 -0.1719 0.4267 0.055 Uiso 1 1 calc R . . C53 C 0.7937(3) -0.0115(3) 0.48962(12) 0.0329(6) Uani 1 1 d . . . H53A H 0.8141 -0.0882 0.5150 0.049 Uiso 1 1 calc R . . H53B H 0.6912 0.0263 0.5038 0.049 Uiso 1 1 calc R . . H53C H 0.8673 0.0305 0.4942 0.049 Uiso 1 1 calc R . . C54 C 0.6506(3) 0.2186(2) 0.40411(12) 0.0270(5) Uani 1 1 d . . . H54 H 0.6829 0.2219 0.4439 0.032 Uiso 1 1 calc R . . C55 C 0.4965(3) 0.1834(3) 0.42232(14) 0.0356(6) Uani 1 1 d . . . H55A H 0.4292 0.2315 0.4491 0.053 Uiso 1 1 calc R . . H55B H 0.5094 0.1047 0.4451 0.053 Uiso 1 1 calc R . . H55C H 0.4522 0.1915 0.3844 0.053 Uiso 1 1 calc R . . C56 C 0.6386(4) 0.3376(3) 0.36280(16) 0.0444(8) Uani 1 1 d . . . H56A H 0.6025 0.3393 0.3239 0.067 Uiso 1 1 calc R . . H56B H 0.7384 0.3585 0.3529 0.067 Uiso 1 1 calc R . . H56C H 0.5673 0.3912 0.3852 0.067 Uiso 1 1 calc R . . C61 C 1.1456(3) 0.1594(2) 0.08227(11) 0.0233(5) Uani 1 1 d . . . H61A H 1.1232 0.0912 0.0738 0.028 Uiso 1 1 calc R . . H61B H 1.2570 0.1501 0.0780 0.028 Uiso 1 1 calc R . . C62 C 1.0857(3) 0.2614(2) 0.03400(11) 0.0211(5) Uani 1 1 d . . . C63 C 1.1829(3) 0.3086(2) -0.01620(12) 0.0289(6) Uani 1 1 d . . . H63 H 1.2891 0.2817 -0.0183 0.035 Uiso 1 1 calc R . . C64 C 1.1256(4) 0.3952(2) -0.06361(13) 0.0363(7) Uani 1 1 d . . . H64 H 1.1928 0.4270 -0.0979 0.044 Uiso 1 1 calc R . . C65 C 0.9716(4) 0.4350(2) -0.06089(13) 0.0351(6) Uani 1 1 d . . . H65 H 0.9324 0.4929 -0.0936 0.042 Uiso 1 1 calc R . . C66 C 0.8750(3) 0.3902(2) -0.01038(13) 0.0322(6) Uani 1 1 d . . . H66 H 0.7690 0.4181 -0.0080 0.039 Uiso 1 1 calc R . . C67 C 0.9319(3) 0.3046(2) 0.03700(12) 0.0255(5) Uani 1 1 d . . . H67 H 0.8644 0.2752 0.0720 0.031 Uiso 1 1 calc R . . C71 C 1.1299(3) -0.06744(19) 0.14714(11) 0.0192(5) Uani 1 1 d . . . C72 C 1.0957(3) -0.1115(2) 0.10020(12) 0.0237(5) Uani 1 1 d . . . C73 C 1.2136(3) -0.1649(2) 0.06189(13) 0.0321(6) Uani 1 1 d . . . H73 H 1.1914 -0.1950 0.0303 0.038 Uiso 1 1 calc R . . C74 C 1.3622(3) -0.1749(3) 0.06904(15) 0.0376(7) Uani 1 1 d . . . H74 H 1.4415 -0.2108 0.0421 0.045 Uiso 1 1 calc R . . C75 C 1.3961(3) -0.1327(2) 0.11532(14) 0.0312(6) Uani 1 1 d . . . H75 H 1.4989 -0.1397 0.1198 0.037 Uiso 1 1 calc R . . C76 C 1.2811(3) -0.0799(2) 0.15570(12) 0.0233(5) Uani 1 1 d . . . C77 C 0.9355(3) -0.0922(2) 0.08719(13) 0.0288(6) Uani 1 1 d . . . H77A H 0.9086 -0.0164 0.0616 0.043 Uiso 1 1 calc R . . H77B H 0.8665 -0.0995 0.1269 0.043 Uiso 1 1 calc R . . H77C H 0.9272 -0.1482 0.0647 0.043 Uiso 1 1 calc R . . C78 C 1.3222(3) -0.0350(2) 0.20577(13) 0.0299(6) Uani 1 1 d . . . H78A H 1.4173 -0.0809 0.2190 0.045 Uiso 1 1 calc R . . H78B H 1.2416 -0.0381 0.2418 0.045 Uiso 1 1 calc R . . H78C H 1.3344 0.0432 0.1891 0.045 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 0.0167(2) 0.0157(2) 0.0195(2) -0.00284(16) -0.00321(15) -0.00130(15) Ni2 0.0147(2) 0.0191(2) 0.0161(2) -0.00408(15) -0.00231(15) -0.00333(15) P1 0.0222(3) 0.0168(3) 0.0240(3) -0.0020(2) -0.0046(2) -0.0003(2) P2 0.0176(3) 0.0258(3) 0.0158(3) -0.0042(2) -0.0016(2) -0.0056(2) O1 0.0346(10) 0.0197(9) 0.0256(9) 0.0016(7) -0.0017(8) -0.0015(7) O2 0.0251(9) 0.0412(10) 0.0175(8) -0.0041(7) -0.0025(7) -0.0155(8) N1 0.0151(9) 0.0192(9) 0.0177(9) -0.0032(7) -0.0027(7) -0.0017(7) N2 0.0210(10) 0.0191(10) 0.0167(9) -0.0043(7) -0.0006(7) -0.0037(8) N3 0.0161(9) 0.0182(9) 0.0191(9) -0.0045(7) -0.0030(7) -0.0002(7) C1 0.0227(12) 0.0229(12) 0.0200(11) -0.0042(9) -0.0043(9) -0.0062(9) C2 0.0276(13) 0.0227(12) 0.0227(12) -0.0027(10) -0.0023(10) -0.0027(10) C3 0.0439(17) 0.0285(14) 0.0258(13) 0.0021(11) 0.0024(12) -0.0105(12) C4 0.0374(15) 0.0358(15) 0.0247(13) -0.0030(11) 0.0067(11) -0.0138(12) C5 0.0254(13) 0.0320(14) 0.0259(13) -0.0077(11) 0.0014(10) -0.0063(11) C6 0.0213(12) 0.0238(12) 0.0202(11) -0.0055(9) -0.0039(9) -0.0062(9) C7 0.0155(11) 0.0225(12) 0.0246(12) -0.0068(9) -0.0031(9) -0.0029(9) C21 0.0310(14) 0.0226(13) 0.0356(14) -0.0039(11) -0.0112(11) 0.0034(10) C22 0.0313(14) 0.0348(15) 0.0359(15) -0.0087(12) -0.0167(12) -0.0024(11) C23 0.0262(14) 0.0279(14) 0.0472(17) -0.0069(12) -0.0031(12) 0.0045(11) C24 0.0276(13) 0.0189(12) 0.0313(13) -0.0060(10) -0.0054(10) -0.0019(10) C25 0.0399(16) 0.0198(13) 0.0475(17) -0.0077(12) -0.0113(13) -0.0029(11) C26 0.0315(14) 0.0271(13) 0.0405(15) -0.0110(11) -0.0119(12) -0.0037(11) C31 0.0189(11) 0.0216(11) 0.0194(11) -0.0044(9) -0.0052(9) -0.0025(9) C32 0.0129(10) 0.0226(12) 0.0208(11) -0.0018(9) 0.0002(8) -0.0006(9) C33 0.0154(11) 0.0248(12) 0.0289(12) -0.0053(10) -0.0016(9) -0.0015(9) C34 0.0237(13) 0.0217(12) 0.0413(15) -0.0070(11) 0.0027(11) -0.0042(10) C35 0.0270(14) 0.0240(13) 0.0395(15) 0.0048(11) 0.0010(11) 0.0021(11) C36 0.0255(13) 0.0373(15) 0.0280(14) 0.0047(11) -0.0058(11) 0.0033(11) C37 0.0217(12) 0.0310(13) 0.0233(12) -0.0032(10) -0.0050(10) -0.0005(10) C41 0.0151(10) 0.0194(11) 0.0208(11) -0.0043(9) -0.0029(9) -0.0006(9) C42 0.0180(11) 0.0247(12) 0.0215(12) -0.0039(9) -0.0017(9) -0.0044(9) C43 0.0226(12) 0.0329(13) 0.0248(12) -0.0067(10) -0.0072(10) -0.0076(10) C44 0.0164(11) 0.0231(12) 0.0383(14) -0.0084(10) -0.0021(10) -0.0071(9) C45 0.0178(11) 0.0194(11) 0.0256(12) -0.0033(9) -0.0024(9) -0.0024(9) C46 0.0176(11) 0.0168(11) 0.0212(11) -0.0051(9) -0.0028(9) 0.0001(9) C47 0.0228(12) 0.0184(11) 0.0203(11) -0.0034(9) -0.0013(9) -0.0049(9) C48 0.0135(10) 0.0192(11) 0.0194(11) -0.0034(9) -0.0053(8) -0.0012(8) C51 0.0266(13) 0.0294(13) 0.0193(12) -0.0017(10) -0.0068(9) -0.0069(10) C52 0.0430(17) 0.0323(15) 0.0290(14) -0.0053(11) -0.0098(12) 0.0046(12) C53 0.0358(15) 0.0405(16) 0.0199(12) 0.0020(11) -0.0058(11) -0.0101(12) C54 0.0266(13) 0.0324(14) 0.0217(12) -0.0096(10) -0.0017(10) -0.0026(11) C55 0.0213(13) 0.0541(18) 0.0302(14) -0.0151(13) -0.0003(11) -0.0012(12) C56 0.054(2) 0.0307(15) 0.0401(17) -0.0086(13) 0.0007(14) 0.0018(14) C61 0.0247(12) 0.0232(12) 0.0183(11) -0.0047(9) 0.0001(9) 0.0003(10) C62 0.0270(12) 0.0204(11) 0.0163(11) -0.0053(9) -0.0010(9) -0.0058(9) C63 0.0308(14) 0.0311(14) 0.0248(13) -0.0080(11) 0.0037(10) -0.0104(11) C64 0.0587(19) 0.0309(14) 0.0192(12) -0.0015(11) 0.0047(12) -0.0209(14) C65 0.0588(19) 0.0230(13) 0.0249(13) -0.0012(10) -0.0141(13) -0.0080(13) C66 0.0359(15) 0.0266(13) 0.0343(14) -0.0052(11) -0.0127(12) -0.0019(11) C67 0.0264(13) 0.0266(13) 0.0231(12) -0.0033(10) -0.0022(10) -0.0076(10) C71 0.0184(11) 0.0167(11) 0.0203(11) -0.0051(9) -0.0017(9) 0.0013(9) C72 0.0246(13) 0.0211(12) 0.0256(12) -0.0060(10) -0.0059(10) -0.0016(9) C73 0.0351(15) 0.0307(14) 0.0302(14) -0.0145(11) -0.0052(11) 0.0027(11) C74 0.0312(15) 0.0385(16) 0.0388(16) -0.0187(13) 0.0001(12) 0.0085(12) C75 0.0183(12) 0.0346(14) 0.0377(15) -0.0102(12) -0.0048(11) 0.0041(10) C76 0.0193(12) 0.0218(12) 0.0275(12) -0.0048(10) -0.0053(10) -0.0002(9) C77 0.0289(14) 0.0313(14) 0.0306(13) -0.0111(11) -0.0095(11) -0.0051(11) C78 0.0220(13) 0.0322(14) 0.0373(15) -0.0100(11) -0.0124(11) 0.0004(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 C1 1.871(2) . ? Ni1 N3 1.963(2) . ? Ni1 N1 1.9682(19) . ? Ni1 P1 2.1787(7) . ? Ni1 Ni2 2.7508(6) . ? Ni2 C48 1.899(2) . ? Ni2 C41 1.911(2) . ? Ni2 N1 1.9759(19) . ? Ni2 P2 2.2369(7) . ? P1 O1 1.6624(18) . ? P1 C21 1.839(3) . ? P1 C24 1.846(3) . ? P2 O2 1.6540(18) . ? P2 C51 1.837(3) . ? P2 C54 1.849(3) . ? O1 C2 1.393(3) . ? O2 C42 1.392(3) . ? N1 C31 1.485(3) . ? N1 C7 1.496(3) . ? N2 C48 1.363(3) . ? N2 C61 1.466(3) . ? N2 C47 1.467(3) . ? N3 C48 1.330(3) . ? N3 C71 1.430(3) . ? C1 C6 1.394(4) . ? C1 C2 1.396(3) . ? C2 C3 1.385(4) . ? C3 C4 1.385(4) . ? C3 H3 0.9500 . ? C4 C5 1.390(4) . ? C4 H4 0.9500 . ? C5 C6 1.399(4) . ? C5 H5 0.9500 . ? C6 C7 1.493(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C21 C22 1.527(4) . ? C21 C23 1.529(4) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C26 1.528(4) . ? C24 C25 1.539(4) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C31 C32 1.517(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.391(4) . ? C32 C37 1.401(3) . ? C33 C34 1.391(4) . ? C33 H33 0.9500 . ? C34 C35 1.392(4) . ? C34 H34 0.9500 . ? C35 C36 1.392(5) . ? C35 H35 0.9500 . ? C36 C37 1.390(4) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C41 C42 1.395(3) . ? C41 C46 1.403(3) . ? C42 C43 1.385(4) . ? C43 C44 1.387(4) . ? C43 H43 0.9500 . ? C44 C45 1.396(4) . ? C44 H44 0.9500 . ? C45 C46 1.394(3) . ? C45 H45 0.9500 . ? C46 C47 1.501(3) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C51 C53 1.534(4) . ? C51 C52 1.539(4) . ? C51 H51 1.0000 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 C55 1.530(4) . ? C54 C56 1.534(4) . ? C54 H54 1.0000 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C61 C62 1.518(3) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C67 1.385(4) . ? C62 C63 1.388(4) . ? C63 C64 1.395(4) . ? C63 H63 0.9500 . ? C64 C65 1.380(5) . ? C64 H64 0.9500 . ? C65 C66 1.377(4) . ? C65 H65 0.9500 . ? C66 C67 1.386(4) . ? C66 H66 0.9500 . ? C67 H67 0.9500 . ? C71 C76 1.405(3) . ? C71 C72 1.411(3) . ? C72 C73 1.390(4) . ? C72 C77 1.507(4) . ? C73 C74 1.378(4) . ? C73 H73 0.9500 . ? C74 C75 1.381(4) . ? C74 H74 0.9500 . ? C75 C76 1.400(4) . ? C75 H75 0.9500 . ? C76 C78 1.508(4) . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 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 C1 Ni1 N3 170.15(10) . . ? C1 Ni1 N1 83.90(9) . . ? N3 Ni1 N1 88.86(8) . . ? C1 Ni1 P1 79.96(8) . . ? N3 Ni1 P1 108.09(6) . . ? N1 Ni1 P1 161.83(6) . . ? C1 Ni1 Ni2 103.33(8) . . ? N3 Ni1 Ni2 66.82(6) . . ? N1 Ni1 Ni2 45.89(6) . . ? P1 Ni1 Ni2 147.05(3) . . ? C48 Ni2 C41 88.39(10) . . ? C48 Ni2 N1 86.63(9) . . ? C41 Ni2 N1 169.44(9) . . ? C48 Ni2 P2 157.30(7) . . ? C41 Ni2 P2 81.92(7) . . ? N1 Ni2 P2 105.94(6) . . ? C48 Ni2 Ni1 69.51(7) . . ? C41 Ni2 Ni1 139.89(7) . . ? N1 Ni2 Ni1 45.66(6) . . ? P2 Ni2 Ni1 105.59(2) . . ? O1 P1 C21 97.69(11) . . ? O1 P1 C24 100.73(11) . . ? C21 P1 C24 103.68(12) . . ? O1 P1 Ni1 105.59(7) . . ? C21 P1 Ni1 131.38(10) . . ? C24 P1 Ni1 112.78(8) . . ? O2 P2 C51 98.46(10) . . ? O2 P2 C54 97.16(11) . . ? C51 P2 C54 104.79(12) . . ? O2 P2 Ni2 103.15(7) . . ? C51 P2 Ni2 119.07(9) . . ? C54 P2 Ni2 127.43(9) . . ? C2 O1 P1 109.60(15) . . ? C42 O2 P2 113.12(15) . . ? C31 N1 C7 106.91(18) . . ? C31 N1 Ni1 110.76(14) . . ? C7 N1 Ni1 113.90(15) . . ? C31 N1 Ni2 118.02(15) . . ? C7 N1 Ni2 117.87(14) . . ? Ni1 N1 Ni2 88.44(8) . . ? C48 N2 C61 127.2(2) . . ? C48 N2 C47 118.57(19) . . ? C61 N2 C47 113.80(19) . . ? C48 N3 C71 122.29(19) . . ? C48 N3 Ni1 111.29(15) . . ? C71 N3 Ni1 126.08(15) . . ? C6 C1 C2 117.8(2) . . ? C6 C1 Ni1 118.24(18) . . ? C2 C1 Ni1 123.87(19) . . ? C3 C2 O1 120.5(2) . . ? C3 C2 C1 123.0(2) . . ? O1 C2 C1 116.5(2) . . ? C2 C3 C4 117.5(2) . . ? C2 C3 H3 121.2 . . ? C4 C3 H3 121.2 . . ? C3 C4 C5 121.8(3) . . ? C3 C4 H4 119.1 . . ? C5 C4 H4 119.1 . . ? C4 C5 C6 119.1(2) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? C1 C6 C5 120.7(2) . . ? C1 C6 C7 114.6(2) . . ? C5 C6 C7 124.8(2) . . ? C6 C7 N1 109.01(19) . . ? C6 C7 H7A 109.9 . . ? N1 C7 H7A 109.9 . . ? C6 C7 H7B 109.9 . . ? N1 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? C22 C21 C23 109.2(2) . . ? C22 C21 P1 113.07(19) . . ? C23 C21 P1 113.34(19) . . ? C22 C21 H21 106.9 . . ? C23 C21 H21 106.9 . . ? P1 C21 H21 106.9 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C26 C24 C25 109.7(2) . . ? C26 C24 P1 110.67(18) . . ? C25 C24 P1 112.66(19) . . ? C26 C24 H24 107.9 . . ? C25 C24 H24 107.9 . . ? P1 C24 H24 107.9 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N1 C31 C32 116.47(19) . . ? N1 C31 H31A 108.2 . . ? C32 C31 H31A 108.2 . . ? N1 C31 H31B 108.2 . . ? C32 C31 H31B 108.2 . . ? H31A C31 H31B 107.3 . . ? C33 C32 C37 118.4(2) . . ? C33 C32 C31 123.2(2) . . ? C37 C32 C31 118.2(2) . . ? C34 C33 C32 120.5(2) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C35 121.0(3) . . ? C33 C34 H34 119.5 . . ? C35 C34 H34 119.5 . . ? C34 C35 C36 118.8(2) . . ? C34 C35 H35 120.6 . . ? C36 C35 H35 120.6 . . ? C37 C36 C35 120.2(3) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C36 C37 C32 121.0(3) . . ? C36 C37 H37 119.5 . . ? C32 C37 H37 119.5 . . ? C42 C41 C46 115.1(2) . . ? C42 C41 Ni2 121.20(17) . . ? C46 C41 Ni2 123.49(17) . . ? C43 C42 O2 117.1(2) . . ? C43 C42 C41 124.6(2) . . ? O2 C42 C41 118.2(2) . . ? C42 C43 C44 118.5(2) . . ? C42 C43 H43 120.8 . . ? C44 C43 H43 120.8 . . ? C43 C44 C45 119.5(2) . . ? C43 C44 H44 120.3 . . ? C45 C44 H44 120.3 . . ? C46 C45 C44 120.3(2) . . ? C46 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? C45 C46 C41 121.9(2) . . ? C45 C46 C47 119.3(2) . . ? C41 C46 C47 118.6(2) . . ? N2 C47 C46 113.03(19) . . ? N2 C47 H47A 109.0 . . ? C46 C47 H47A 109.0 . . ? N2 C47 H47B 109.0 . . ? C46 C47 H47B 109.0 . . ? H47A C47 H47B 107.8 . . ? N3 C48 N2 123.5(2) . . ? N3 C48 Ni2 110.83(16) . . ? N2 C48 Ni2 125.61(17) . . ? C53 C51 C52 110.5(2) . . ? C53 C51 P2 113.64(19) . . ? C52 C51 P2 107.90(18) . . ? C53 C51 H51 108.2 . . ? C52 C51 H51 108.2 . . ? P2 C51 H51 108.2 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C55 C54 C56 111.4(3) . . ? C55 C54 P2 115.9(2) . . ? C56 C54 P2 109.32(19) . . ? C55 C54 H54 106.5 . . ? C56 C54 H54 106.5 . . ? P2 C54 H54 106.5 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N2 C61 C62 112.82(19) . . ? N2 C61 H61A 109.0 . . ? C62 C61 H61A 109.0 . . ? N2 C61 H61B 109.0 . . ? C62 C61 H61B 109.0 . . ? H61A C61 H61B 107.8 . . ? C67 C62 C63 118.7(2) . . ? C67 C62 C61 120.5(2) . . ? C63 C62 C61 120.7(2) . . ? C62 C63 C64 120.4(3) . . ? C62 C63 H63 119.8 . . ? C64 C63 H63 119.8 . . ? C65 C64 C63 120.2(3) . . ? C65 C64 H64 119.9 . . ? C63 C64 H64 119.9 . . ? C66 C65 C64 119.6(3) . . ? C66 C65 H65 120.2 . . ? C64 C65 H65 120.2 . . ? C65 C66 C67 120.3(3) . . ? C65 C66 H66 119.9 . . ? C67 C66 H66 119.9 . . ? C62 C67 C66 120.8(2) . . ? C62 C67 H67 119.6 . . ? C66 C67 H67 119.6 . . ? C76 C71 C72 120.2(2) . . ? C76 C71 N3 120.1(2) . . ? C72 C71 N3 119.7(2) . . ? C73 C72 C71 119.0(2) . . ? C73 C72 C77 119.7(2) . . ? C71 C72 C77 121.1(2) . . ? C74 C73 C72 121.1(3) . . ? C74 C73 H73 119.5 . . ? C72 C73 H73 119.5 . . ? C73 C74 C75 120.1(3) . . ? C73 C74 H74 120.0 . . ? C75 C74 H74 120.0 . . ? C74 C75 C76 121.0(2) . . ? C74 C75 H75 119.5 . . ? C76 C75 H75 119.5 . . ? C75 C76 C71 118.7(2) . . ? C75 C76 C78 119.5(2) . . ? C71 C76 C78 121.8(2) . . ? C72 C77 H77A 109.5 . . ? C72 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C72 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C76 C78 H78A 109.5 . . ? C76 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C76 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Ni1 Ni2 C48 -173.66(10) . . . . ? N3 Ni1 Ni2 C48 6.53(9) . . . . ? N1 Ni1 Ni2 C48 -106.10(11) . . . . ? P1 Ni1 Ni2 C48 94.27(8) . . . . ? C1 Ni1 Ni2 C41 125.68(14) . . . . ? N3 Ni1 Ni2 C41 -54.13(13) . . . . ? N1 Ni1 Ni2 C41 -166.76(14) . . . . ? P1 Ni1 Ni2 C41 33.62(12) . . . . ? C1 Ni1 Ni2 N1 -67.56(11) . . . . ? N3 Ni1 Ni2 N1 112.63(10) . . . . ? P1 Ni1 Ni2 N1 -159.63(9) . . . . ? C1 Ni1 Ni2 P2 29.68(8) . . . . ? N3 Ni1 Ni2 P2 -150.13(6) . . . . ? N1 Ni1 Ni2 P2 97.24(8) . . . . ? P1 Ni1 Ni2 P2 -62.39(5) . . . . ? C1 Ni1 P1 O1 -17.55(10) . . . . ? N3 Ni1 P1 O1 156.60(10) . . . . ? N1 Ni1 P1 O1 -45.2(2) . . . . ? Ni2 Ni1 P1 O1 81.50(9) . . . . ? C1 Ni1 P1 C21 -133.08(15) . . . . ? N3 Ni1 P1 C21 41.07(14) . . . . ? N1 Ni1 P1 C21 -160.7(2) . . . . ? Ni2 Ni1 P1 C21 -34.03(14) . . . . ? C1 Ni1 P1 C24 91.54(12) . . . . ? N3 Ni1 P1 C24 -94.32(11) . . . . ? N1 Ni1 P1 C24 63.9(2) . . . . ? Ni2 Ni1 P1 C24 -169.42(10) . . . . ? C48 Ni2 P2 O2 53.2(2) . . . . ? C41 Ni2 P2 O2 -12.43(10) . . . . ? N1 Ni2 P2 O2 174.80(9) . . . . ? Ni1 Ni2 P2 O2 127.24(7) . . . . ? C48 Ni2 P2 C51 -54.4(2) . . . . ? C41 Ni2 P2 C51 -120.05(12) . . . . ? N1 Ni2 P2 C51 67.18(11) . . . . ? Ni1 Ni2 P2 C51 19.62(10) . . . . ? C48 Ni2 P2 C54 163.1(2) . . . . ? C41 Ni2 P2 C54 97.45(13) . . . . ? N1 Ni2 P2 C54 -75.33(13) . . . . ? Ni1 Ni2 P2 C54 -122.88(11) . . . . ? C21 P1 O1 C2 157.96(18) . . . . ? C24 P1 O1 C2 -96.47(18) . . . . ? Ni1 P1 O1 C2 21.05(18) . . . . ? C51 P2 O2 C42 138.32(18) . . . . ? C54 P2 O2 C42 -115.49(18) . . . . ? Ni2 P2 O2 C42 15.68(17) . . . . ? C1 Ni1 N1 C31 -125.27(16) . . . . ? N3 Ni1 N1 C31 61.42(15) . . . . ? P1 Ni1 N1 C31 -97.9(2) . . . . ? Ni2 Ni1 N1 C31 119.49(17) . . . . ? C1 Ni1 N1 C7 -4.72(16) . . . . ? N3 Ni1 N1 C7 -178.03(16) . . . . ? P1 Ni1 N1 C7 22.6(3) . . . . ? Ni2 Ni1 N1 C7 -119.96(17) . . . . ? C1 Ni1 N1 Ni2 115.24(9) . . . . ? N3 Ni1 N1 Ni2 -58.07(8) . . . . ? P1 Ni1 N1 Ni2 142.60(15) . . . . ? C48 Ni2 N1 C31 -48.41(17) . . . . ? C41 Ni2 N1 C31 13.6(6) . . . . ? P2 Ni2 N1 C31 150.81(14) . . . . ? Ni1 Ni2 N1 C31 -112.78(18) . . . . ? C48 Ni2 N1 C7 -179.27(17) . . . . ? C41 Ni2 N1 C7 -117.2(5) . . . . ? P2 Ni2 N1 C7 19.96(17) . . . . ? Ni1 Ni2 N1 C7 116.37(18) . . . . ? C48 Ni2 N1 Ni1 64.37(9) . . . . ? C41 Ni2 N1 Ni1 126.4(5) . . . . ? P2 Ni2 N1 Ni1 -96.41(6) . . . . ? N1 Ni1 N3 C48 32.13(16) . . . . ? P1 Ni1 N3 C48 -154.52(14) . . . . ? Ni2 Ni1 N3 C48 -9.39(13) . . . . ? N1 Ni1 N3 C71 -154.42(19) . . . . ? P1 Ni1 N3 C71 18.93(19) . . . . ? Ni2 Ni1 N3 C71 164.1(2) . . . . ? N1 Ni1 C1 C6 1.70(19) . . . . ? P1 Ni1 C1 C6 -169.94(19) . . . . ? Ni2 Ni1 C1 C6 43.57(19) . . . . ? N1 Ni1 C1 C2 -175.0(2) . . . . ? P1 Ni1 C1 C2 13.4(2) . . . . ? Ni2 Ni1 C1 C2 -133.1(2) . . . . ? P1 O1 C2 C3 164.9(2) . . . . ? P1 O1 C2 C1 -13.5(3) . . . . ? C6 C1 C2 C3 1.9(4) . . . . ? Ni1 C1 C2 C3 178.6(2) . . . . ? C6 C1 C2 O1 -179.8(2) . . . . ? Ni1 C1 C2 O1 -3.1(3) . . . . ? O1 C2 C3 C4 -179.0(3) . . . . ? C1 C2 C3 C4 -0.7(4) . . . . ? C2 C3 C4 C5 -0.4(5) . . . . ? C3 C4 C5 C6 0.3(4) . . . . ? C2 C1 C6 C5 -2.0(4) . . . . ? Ni1 C1 C6 C5 -178.88(19) . . . . ? C2 C1 C6 C7 178.6(2) . . . . ? Ni1 C1 C6 C7 1.7(3) . . . . ? C4 C5 C6 C1 1.0(4) . . . . ? C4 C5 C6 C7 -179.7(2) . . . . ? C1 C6 C7 N1 -5.3(3) . . . . ? C5 C6 C7 N1 175.4(2) . . . . ? C31 N1 C7 C6 129.2(2) . . . . ? Ni1 N1 C7 C6 6.5(2) . . . . ? Ni2 N1 C7 C6 -95.07(19) . . . . ? O1 P1 C21 C22 -79.7(2) . . . . ? C24 P1 C21 C22 177.2(2) . . . . ? Ni1 P1 C21 C22 39.0(3) . . . . ? O1 P1 C21 C23 155.3(2) . . . . ? C24 P1 C21 C23 52.2(2) . . . . ? Ni1 P1 C21 C23 -86.0(2) . . . . ? O1 P1 C24 C26 71.9(2) . . . . ? C21 P1 C24 C26 172.63(19) . . . . ? Ni1 P1 C24 C26 -40.2(2) . . . . ? O1 P1 C24 C25 -51.3(2) . . . . ? C21 P1 C24 C25 49.4(2) . . . . ? Ni1 P1 C24 C25 -163.45(17) . . . . ? C7 N1 C31 C32 66.6(2) . . . . ? Ni1 N1 C31 C32 -168.79(15) . . . . ? Ni2 N1 C31 C32 -69.1(2) . . . . ? N1 C31 C32 C33 28.9(3) . . . . ? N1 C31 C32 C37 -155.6(2) . . . . ? C37 C32 C33 C34 -0.4(3) . . . . ? C31 C32 C33 C34 175.1(2) . . . . ? C32 C33 C34 C35 -0.1(4) . . . . ? C33 C34 C35 C36 0.1(4) . . . . ? C34 C35 C36 C37 0.5(4) . . . . ? C35 C36 C37 C32 -1.0(4) . . . . ? C33 C32 C37 C36 1.0(4) . . . . ? C31 C32 C37 C36 -174.8(2) . . . . ? C48 Ni2 C41 C42 -150.6(2) . . . . ? N1 Ni2 C41 C42 147.6(4) . . . . ? P2 Ni2 C41 C42 8.85(18) . . . . ? Ni1 Ni2 C41 C42 -95.8(2) . . . . ? C48 Ni2 C41 C46 34.5(2) . . . . ? N1 Ni2 C41 C46 -27.4(6) . . . . ? P2 Ni2 C41 C46 -166.1(2) . . . . ? Ni1 Ni2 C41 C46 89.3(2) . . . . ? P2 O2 C42 C43 166.02(19) . . . . ? P2 O2 C42 C41 -11.2(3) . . . . ? C46 C41 C42 C43 -2.7(4) . . . . ? Ni2 C41 C42 C43 -178.1(2) . . . . ? C46 C41 C42 O2 174.3(2) . . . . ? Ni2 C41 C42 O2 -1.0(3) . . . . ? O2 C42 C43 C44 -176.9(2) . . . . ? C41 C42 C43 C44 0.2(4) . . . . ? C42 C43 C44 C45 2.0(4) . . . . ? C43 C44 C45 C46 -1.5(4) . . . . ? C44 C45 C46 C41 -1.2(4) . . . . ? C44 C45 C46 C47 173.8(2) . . . . ? C42 C41 C46 C45 3.2(3) . . . . ? Ni2 C41 C46 C45 178.41(17) . . . . ? C42 C41 C46 C47 -171.9(2) . . . . ? Ni2 C41 C46 C47 3.4(3) . . . . ? C48 N2 C47 C46 42.7(3) . . . . ? C61 N2 C47 C46 -144.1(2) . . . . ? C45 C46 C47 N2 135.4(2) . . . . ? C41 C46 C47 N2 -49.4(3) . . . . ? C71 N3 C48 N2 18.7(3) . . . . ? Ni1 N3 C48 N2 -167.58(17) . . . . ? C71 N3 C48 Ni2 -160.29(17) . . . . ? Ni1 N3 C48 Ni2 13.45(19) . . . . ? C61 N2 C48 N3 18.8(4) . . . . ? C47 N2 C48 N3 -169.0(2) . . . . ? C61 N2 C48 Ni2 -162.43(18) . . . . ? C47 N2 C48 Ni2 9.8(3) . . . . ? C41 Ni2 C48 N3 136.32(17) . . . . ? N1 Ni2 C48 N3 -53.01(16) . . . . ? P2 Ni2 C48 N3 71.9(3) . . . . ? Ni1 Ni2 C48 N3 -9.50(13) . . . . ? C41 Ni2 C48 N2 -42.6(2) . . . . ? N1 Ni2 C48 N2 128.0(2) . . . . ? P2 Ni2 C48 N2 -107.1(2) . . . . ? Ni1 Ni2 C48 N2 171.6(2) . . . . ? O2 P2 C51 C53 55.8(2) . . . . ? C54 P2 C51 C53 -43.9(2) . . . . ? Ni2 P2 C51 C53 166.05(16) . . . . ? O2 P2 C51 C52 -67.04(19) . . . . ? C54 P2 C51 C52 -166.81(18) . . . . ? Ni2 P2 C51 C52 43.2(2) . . . . ? O2 P2 C54 C55 -154.2(2) . . . . ? C51 P2 C54 C55 -53.5(2) . . . . ? Ni2 P2 C54 C55 93.2(2) . . . . ? O2 P2 C54 C56 78.9(2) . . . . ? C51 P2 C54 C56 179.6(2) . . . . ? Ni2 P2 C54 C56 -33.8(2) . . . . ? C48 N2 C61 C62 122.8(2) . . . . ? C47 N2 C61 C62 -49.7(3) . . . . ? N2 C61 C62 C67 -47.4(3) . . . . ? N2 C61 C62 C63 136.8(2) . . . . ? C67 C62 C63 C64 -2.2(4) . . . . ? C61 C62 C63 C64 173.7(2) . . . . ? C62 C63 C64 C65 0.2(4) . . . . ? C63 C64 C65 C66 1.4(4) . . . . ? C64 C65 C66 C67 -1.0(4) . . . . ? C63 C62 C67 C66 2.6(4) . . . . ? C61 C62 C67 C66 -173.3(2) . . . . ? C65 C66 C67 C62 -1.0(4) . . . . ? C48 N3 C71 C76 57.6(3) . . . . ? Ni1 N3 C71 C76 -115.2(2) . . . . ? C48 N3 C71 C72 -122.4(2) . . . . ? Ni1 N3 C71 C72 64.8(3) . . . . ? C76 C71 C72 C73 -1.4(4) . . . . ? N3 C71 C72 C73 178.6(2) . . . . ? C76 C71 C72 C77 -175.7(2) . . . . ? N3 C71 C72 C77 4.3(4) . . . . ? C71 C72 C73 C74 -0.2(4) . . . . ? C77 C72 C73 C74 174.2(3) . . . . ? C72 C73 C74 C75 0.8(5) . . . . ? C73 C74 C75 C76 0.3(5) . . . . ? C74 C75 C76 C71 -1.8(4) . . . . ? C74 C75 C76 C78 179.9(3) . . . . ? C72 C71 C76 C75 2.4(4) . . . . ? N3 C71 C76 C75 -177.6(2) . . . . ? C72 C71 C76 C78 -179.4(2) . . . . ? N3 C71 C76 C78 0.6(4) . . . . ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 _platon_squeeze_void_content 1 -0.040 0.500 0.500 236 37 ' ' 2 0.371 0.018 0.963 18 1 ' ' 3 0.629 -0.018 0.037 18 1 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 69.72 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 2.447 _refine_diff_density_min -0.311 _refine_diff_density_rms 0.089