# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Igor Fedushkin' _publ_contact_author_email IGORFED@IOMC.RAS.RU _publ_section_title ; 1,2-Bis(imino)acenaphthene Complexes of Molybdenum and Nickel ; loop_ _publ_author_name 'Igor Fedushkin' 'Georgy K. Fukin' 'Elisabeth Irran' 'Nalalie M. Khvoinova' 'Anton N. Lukoyanov' ; K.A.Lysenko ; 'Alexander S. Nikipelov' 'Alexander V. Piskunov' 'Herbert Schumann' 'Alexandra A. Skatova' # Attachment 'compound_3.CIF' data_fed49 _database_code_depnum_ccdc_archive 'CCDC 719953' _audit_creation_method ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H40 Mo N2 O4' _chemical_formula_weight 708.68 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' O O 0.0106 0.0060 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 21.1081(4) _cell_length_b 20.0378(3) _cell_length_c 18.0358(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.820(2) _cell_angle_gamma 90.00 _cell_volume 7302.1(2) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 14789 _cell_measurement_theta_min 2.8566 _cell_measurement_theta_max 32.4001 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.289 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2944 _exptl_absorpt_coefficient_mu 0.400 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9100 _exptl_absorpt_correction_T_max 0.9498 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Oxford Diffraction Xcalibur S Sapphire' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 74675 _diffrn_reflns_av_R_equivalents 0.0924 _diffrn_reflns_av_sigmaI/netI 0.0920 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12838 _reflns_number_gt 8314 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0332P)^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 12838 _refine_ls_number_parameters 863 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0997 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.0864 _refine_ls_wR_factor_gt 0.0748 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.980 _refine_ls_shift/su_max 0.002 _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 0.010152(15) 0.593578(14) 0.749640(19) 0.02402(9) Uani 1 1 d . . . Mo2 Mo 0.479719(16) 0.754024(16) 0.63590(2) 0.03210(10) Uani 1 1 d . . . N1 N -0.04337(13) 0.49726(12) 0.75184(17) 0.0214(7) Uani 1 1 d . . . N2 N -0.07195(13) 0.58694(13) 0.63819(16) 0.0219(7) Uani 1 1 d . . . N3 N 0.54066(14) 0.82600(14) 0.72228(18) 0.0320(8) Uani 1 1 d . . . N4 N 0.40936(14) 0.81435(14) 0.68148(18) 0.0311(8) Uani 1 1 d . . . O1 O 0.11871(14) 0.58243(15) 0.90865(17) 0.0539(8) Uani 1 1 d . . . O2 O 0.07608(14) 0.72536(13) 0.71593(17) 0.0506(8) Uani 1 1 d . . . O3 O 0.12792(14) 0.53342(13) 0.69335(17) 0.0496(8) Uani 1 1 d . . . O4 O -0.05638(15) 0.68486(13) 0.84937(17) 0.0510(8) Uani 1 1 d . . . O5 O 0.59618(15) 0.68153(15) 0.5960(2) 0.0694(10) Uani 1 1 d . . . O6 O 0.37406(14) 0.66499(14) 0.52151(18) 0.0552(8) Uani 1 1 d . . . O7 O 0.49381(15) 0.62588(15) 0.74355(19) 0.0626(9) Uani 1 1 d . . . O8 O 0.47388(15) 0.83678(15) 0.48414(19) 0.0591(9) Uani 1 1 d . . . C1 C -0.08448(16) 0.47939(16) 0.6867(2) 0.0211(8) Uani 1 1 d . . . C2 C -0.10052(16) 0.52902(16) 0.6232(2) 0.0211(8) Uani 1 1 d . . . C3 C -0.14999(16) 0.49981(15) 0.5569(2) 0.0221(8) Uani 1 1 d . . . C4 C -0.16185(16) 0.43471(16) 0.5809(2) 0.0240(8) Uani 1 1 d . . . C5 C -0.12505(16) 0.41993(15) 0.6582(2) 0.0222(8) Uani 1 1 d . . . C6 C -0.13266(17) 0.35839(16) 0.6880(2) 0.0301(9) Uani 1 1 d . . . H6 H -0.1096 0.3474 0.7401 0.036 Uiso 1 1 calc R . . C7 C -0.17550(18) 0.31169(18) 0.6396(2) 0.0364(10) Uani 1 1 d . . . H7 H -0.1799 0.2687 0.6596 0.044 Uiso 1 1 calc R . . C8 C -0.21073(18) 0.32610(17) 0.5650(2) 0.0375(10) Uani 1 1 d . . . H8 H -0.2392 0.2934 0.5345 0.045 Uiso 1 1 calc R . . C9 C -0.20514(16) 0.38911(17) 0.5332(2) 0.0278(9) Uani 1 1 d . . . C10 C -0.23744(17) 0.41183(18) 0.4565(2) 0.0346(9) Uani 1 1 d . . . H10 H -0.2672 0.3829 0.4213 0.042 Uiso 1 1 calc R . . C11 C -0.22631(17) 0.47421(19) 0.4330(2) 0.0347(10) Uani 1 1 d . . . H11 H -0.2486 0.4876 0.3815 0.042 Uiso 1 1 calc R . . C12 C -0.18288(17) 0.51963(17) 0.4824(2) 0.0303(9) Uani 1 1 d . . . H12 H -0.1764 0.5630 0.4647 0.036 Uiso 1 1 calc R . . C13 C -0.03506(16) 0.45272(16) 0.8175(2) 0.0241(8) Uani 1 1 d . . . C14 C -0.07572(16) 0.46332(16) 0.8655(2) 0.0238(8) Uani 1 1 d . . . C15 C -0.06841(18) 0.41918(18) 0.9272(2) 0.0342(10) Uani 1 1 d . . . H15 H -0.0952 0.4248 0.9610 0.041 Uiso 1 1 calc R . . C16 C -0.02331(19) 0.36758(19) 0.9406(2) 0.0375(10) Uani 1 1 d . . . H16 H -0.0199 0.3377 0.9824 0.045 Uiso 1 1 calc R . . C17 C 0.01662(17) 0.35957(17) 0.8933(2) 0.0331(10) Uani 1 1 d . . . H17 H 0.0478 0.3241 0.9031 0.040 Uiso 1 1 calc R . . C18 C 0.01247(16) 0.40226(17) 0.8311(2) 0.0271(8) Uani 1 1 d . . . C19 C 0.05843(17) 0.39295(17) 0.7817(2) 0.0326(10) Uani 1 1 d . . . H19 H 0.0472 0.4274 0.7398 0.039 Uiso 1 1 calc R . . C20 C 0.05074(19) 0.32411(17) 0.7432(2) 0.0420(11) Uani 1 1 d . . . H20A H 0.0054 0.3190 0.7094 0.063 Uiso 1 1 calc R . . H20B H 0.0599 0.2894 0.7832 0.063 Uiso 1 1 calc R . . H20C H 0.0820 0.3199 0.7125 0.063 Uiso 1 1 calc R . . C21 C 0.13089(18) 0.4038(2) 0.8300(3) 0.0514(12) Uani 1 1 d . . . H21A H 0.1357 0.4484 0.8533 0.077 Uiso 1 1 calc R . . H21B H 0.1598 0.3998 0.7965 0.077 Uiso 1 1 calc R . . H21C H 0.1432 0.3701 0.8711 0.077 Uiso 1 1 calc R . . C22 C -0.12757(17) 0.51752(17) 0.8506(2) 0.0320(9) Uani 1 1 d . . . H22 H -0.1150 0.5518 0.8171 0.038 Uiso 1 1 calc R . . C23 C -0.1309(2) 0.5529(2) 0.9242(3) 0.0531(12) Uani 1 1 d . . . H23A H -0.0866 0.5686 0.9530 0.080 Uiso 1 1 calc R . . H23B H -0.1471 0.5218 0.9565 0.080 Uiso 1 1 calc R . . H23C H -0.1611 0.5910 0.9105 0.080 Uiso 1 1 calc R . . C24 C -0.19551(17) 0.49100(19) 0.8060(2) 0.0408(11) Uani 1 1 d . . . H24A H -0.1933 0.4712 0.7572 0.061 Uiso 1 1 calc R . . H24B H -0.2275 0.5277 0.7951 0.061 Uiso 1 1 calc R . . H24C H -0.2095 0.4570 0.8371 0.061 Uiso 1 1 calc R . . C25 C -0.09615(17) 0.64094(15) 0.5840(2) 0.0243(8) Uani 1 1 d . . . C26 C -0.15148(17) 0.67713(16) 0.5913(2) 0.0277(9) Uani 1 1 d . . . C27 C -0.17224(18) 0.73083(17) 0.5414(2) 0.0351(10) Uani 1 1 d . . . H27 H -0.2090 0.7567 0.5450 0.042 Uiso 1 1 calc R . . C28 C -0.14049(19) 0.74736(18) 0.4867(2) 0.0394(10) Uani 1 1 d . . . H28 H -0.1557 0.7843 0.4532 0.047 Uiso 1 1 calc R . . C29 C -0.08736(19) 0.71101(17) 0.4802(2) 0.0341(10) Uani 1 1 d . . . H29 H -0.0668 0.7225 0.4415 0.041 Uiso 1 1 calc R . . C30 C -0.06298(17) 0.65729(16) 0.5296(2) 0.0259(9) Uani 1 1 d . . . C31 C -0.00474(17) 0.61741(17) 0.5210(2) 0.0312(9) Uani 1 1 d . . . H31 H 0.0088 0.5856 0.5656 0.037 Uiso 1 1 calc R . . C32 C -0.02385(19) 0.57647(18) 0.4467(2) 0.0424(11) Uani 1 1 d . . . H32A H -0.0596 0.5456 0.4477 0.064 Uiso 1 1 calc R . . H32B H 0.0146 0.5511 0.4425 0.064 Uiso 1 1 calc R . . H32C H -0.0389 0.6064 0.4021 0.064 Uiso 1 1 calc R . . C33 C 0.0545(2) 0.6616(2) 0.5236(3) 0.0533(12) Uani 1 1 d . . . H33A H 0.0626 0.6919 0.5680 0.080 Uiso 1 1 calc R . . H33B H 0.0454 0.6877 0.4757 0.080 Uiso 1 1 calc R . . H33C H 0.0936 0.6337 0.5287 0.080 Uiso 1 1 calc R . . C34 C -0.18886(18) 0.65895(18) 0.6489(2) 0.0366(10) Uani 1 1 d . . . H34 H -0.1594 0.6293 0.6889 0.044 Uiso 1 1 calc R . . C35 C -0.25154(19) 0.61989(19) 0.6110(3) 0.0527(13) Uani 1 1 d . . . H35A H -0.2402 0.5793 0.5873 0.079 Uiso 1 1 calc R . . H35B H -0.2815 0.6474 0.5711 0.079 Uiso 1 1 calc R . . H35C H -0.2733 0.6077 0.6503 0.079 Uiso 1 1 calc R . . C36 C -0.2070(2) 0.7181(2) 0.6910(3) 0.0653(15) Uani 1 1 d . . . H36A H -0.1672 0.7443 0.7152 0.098 Uiso 1 1 calc R . . H36B H -0.2264 0.7022 0.7310 0.098 Uiso 1 1 calc R . . H36C H -0.2392 0.7462 0.6540 0.098 Uiso 1 1 calc R . . C37 C 0.07806(19) 0.58656(19) 0.8501(2) 0.0362(10) Uani 1 1 d . . . C38 C 0.05092(19) 0.67732(19) 0.7287(2) 0.0336(10) Uani 1 1 d . . . C39 C 0.0818(2) 0.55109(17) 0.7087(2) 0.0321(9) Uani 1 1 d . . . C40 C -0.03748(19) 0.65008(17) 0.8096(2) 0.0326(9) Uani 1 1 d . . . C41 C 0.50834(18) 0.86566(17) 0.7555(2) 0.0314(9) Uani 1 1 d . . . C42 C 0.43576(18) 0.85823(18) 0.7341(2) 0.0314(9) Uani 1 1 d . . . C43 C 0.41072(18) 0.90639(18) 0.7800(2) 0.0342(9) Uani 1 1 d . . . C44 C 0.46703(19) 0.94143(18) 0.8248(2) 0.0341(9) Uani 1 1 d . . . C45 C 0.52714(18) 0.91975(17) 0.8130(2) 0.0346(10) Uani 1 1 d . . . C46 C 0.58537(19) 0.95040(19) 0.8543(2) 0.0416(11) Uani 1 1 d . . . H46 H 0.6266 0.9365 0.8482 0.050 Uiso 1 1 calc R . . C47 C 0.5825(2) 1.00237(19) 0.9053(2) 0.0453(11) Uani 1 1 d . . . H47 H 0.6224 1.0238 0.9333 0.054 Uiso 1 1 calc R . . C48 C 0.5239(2) 1.0233(2) 0.9162(2) 0.0461(11) Uani 1 1 d . . . H48 H 0.5241 1.0589 0.9510 0.055 Uiso 1 1 calc R . . C49 C 0.46331(19) 0.99266(18) 0.8763(2) 0.0378(10) Uani 1 1 d . . . C50 C 0.3997(2) 1.0074(2) 0.8829(3) 0.0473(12) Uani 1 1 d . . . H50 H 0.3945 1.0423 0.9163 0.057 Uiso 1 1 calc R . . C51 C 0.3456(2) 0.9717(2) 0.8417(2) 0.0494(12) Uani 1 1 d . . . H51 H 0.3038 0.9814 0.8491 0.059 Uiso 1 1 calc R . . C52 C 0.34925(19) 0.92108(19) 0.7883(2) 0.0429(11) Uani 1 1 d . . . H52 H 0.3107 0.8980 0.7593 0.051 Uiso 1 1 calc R . . C53 C 0.61237(18) 0.83404(19) 0.7468(2) 0.0350(10) Uani 1 1 d . . . C54 C 0.6406(2) 0.8801(2) 0.7078(3) 0.0440(11) Uani 1 1 d . . . C55 C 0.7078(2) 0.8920(2) 0.7364(3) 0.0584(13) Uani 1 1 d . . . H55 H 0.7280 0.9240 0.7117 0.070 Uiso 1 1 calc R . . C56 C 0.7455(2) 0.8581(3) 0.7997(3) 0.0702(16) Uani 1 1 d . . . H56 H 0.7915 0.8675 0.8191 0.084 Uiso 1 1 calc R . . C57 C 0.7177(2) 0.8107(3) 0.8356(3) 0.0667(15) Uani 1 1 d . . . H57 H 0.7447 0.7867 0.8786 0.080 Uiso 1 1 calc R . . C58 C 0.6496(2) 0.7974(2) 0.8091(2) 0.0451(11) Uani 1 1 d . . . C59 C 0.6194(2) 0.7451(2) 0.8497(3) 0.0582(13) Uani 1 1 d . . . H59 H 0.5720 0.7400 0.8188 0.070 Uiso 1 1 calc R . . C60 C 0.6524(3) 0.6768(3) 0.8506(3) 0.0957(19) Uani 1 1 d . . . H60A H 0.6488 0.6632 0.7973 0.144 Uiso 1 1 calc R . . H60B H 0.6302 0.6438 0.8745 0.144 Uiso 1 1 calc R . . H60C H 0.6992 0.6798 0.8804 0.144 Uiso 1 1 calc R . . C61 C 0.6199(3) 0.7675(3) 0.9313(3) 0.0855(17) Uani 1 1 d . . . H61A H 0.5968 0.8103 0.9280 0.128 Uiso 1 1 calc R . . H61B H 0.6658 0.7727 0.9637 0.128 Uiso 1 1 calc R . . H61C H 0.5976 0.7340 0.9543 0.128 Uiso 1 1 calc R . . C62 C 0.5999(2) 0.9174(2) 0.6362(3) 0.0551(13) Uani 1 1 d . . . H62 H 0.5532 0.9013 0.6238 0.066 Uiso 1 1 calc R . . C63 C 0.6254(3) 0.9019(2) 0.5668(3) 0.0826(17) Uani 1 1 d . . . H63A H 0.6267 0.8534 0.5600 0.124 Uiso 1 1 calc R . . H63B H 0.6701 0.9202 0.5760 0.124 Uiso 1 1 calc R . . H63C H 0.5958 0.9220 0.5200 0.124 Uiso 1 1 calc R . . C64 C 0.5999(3) 0.9928(2) 0.6506(3) 0.0898(19) Uani 1 1 d . . . H64A H 0.5824 1.0016 0.6944 0.135 Uiso 1 1 calc R . . H64B H 0.5721 1.0150 0.6042 0.135 Uiso 1 1 calc R . . H64C H 0.6452 1.0099 0.6624 0.135 Uiso 1 1 calc R . . C65 C 0.33786(18) 0.80686(17) 0.6586(2) 0.0302(9) Uani 1 1 d . . . C66 C 0.29937(18) 0.84448(17) 0.5963(2) 0.0315(9) Uani 1 1 d . . . C67 C 0.23126(19) 0.83573(19) 0.5765(2) 0.0403(10) Uani 1 1 d . . . H67 H 0.2038 0.8606 0.5346 0.048 Uiso 1 1 calc R . . C68 C 0.20245(19) 0.79202(19) 0.6161(3) 0.0438(11) Uani 1 1 d . . . H68 H 0.1557 0.7873 0.6016 0.053 Uiso 1 1 calc R . . C69 C 0.24137(18) 0.75547(19) 0.6761(3) 0.0430(11) Uani 1 1 d . . . H69 H 0.2211 0.7251 0.7028 0.052 Uiso 1 1 calc R . . C70 C 0.31006(18) 0.76173(18) 0.6990(2) 0.0358(10) Uani 1 1 d . . . C71 C 0.3517(2) 0.7220(2) 0.7682(3) 0.0485(12) Uani 1 1 d . . . H71 H 0.3991 0.7292 0.7704 0.058 Uiso 1 1 calc R . . C72 C 0.3392(2) 0.6483(2) 0.7595(3) 0.0767(16) Uani 1 1 d . . . H72A H 0.3491 0.6325 0.7126 0.115 Uiso 1 1 calc R . . H72B H 0.2927 0.6392 0.7554 0.115 Uiso 1 1 calc R . . H72C H 0.3677 0.6251 0.8048 0.115 Uiso 1 1 calc R . . C73 C 0.3432(2) 0.7484(2) 0.8439(3) 0.0751(15) Uani 1 1 d . . . H73A H 0.3533 0.7962 0.8483 0.113 Uiso 1 1 calc R . . H73B H 0.3735 0.7247 0.8875 0.113 Uiso 1 1 calc R . . H73C H 0.2975 0.7413 0.8447 0.113 Uiso 1 1 calc R . . C74 C 0.3295(2) 0.89399(19) 0.5529(2) 0.0444(11) Uani 1 1 d . . . H74 H 0.3781 0.8852 0.5676 0.053 Uiso 1 1 calc R . . C75 C 0.3029(3) 0.8850(3) 0.4665(3) 0.0817(17) Uani 1 1 d . . . H75A H 0.3049 0.8377 0.4536 0.123 Uiso 1 1 calc R . . H75B H 0.3297 0.9112 0.4408 0.123 Uiso 1 1 calc R . . H75C H 0.2569 0.9003 0.4490 0.123 Uiso 1 1 calc R . . C76 C 0.3199(3) 0.9661(2) 0.5757(3) 0.0818(18) Uani 1 1 d . . . H76A H 0.3373 0.9710 0.6320 0.123 Uiso 1 1 calc R . . H76B H 0.2727 0.9771 0.5593 0.123 Uiso 1 1 calc R . . H76C H 0.3437 0.9963 0.5503 0.123 Uiso 1 1 calc R . . C77 C 0.5524(2) 0.7090(2) 0.6105(2) 0.0449(11) Uani 1 1 d . . . C78 C 0.41402(19) 0.69776(19) 0.5640(2) 0.0369(10) Uani 1 1 d . . . C79 C 0.48788(19) 0.6751(2) 0.7100(3) 0.0442(11) Uani 1 1 d . . . C80 C 0.47552(19) 0.8110(2) 0.5419(3) 0.0408(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.02722(18) 0.02266(16) 0.02164(18) -0.00220(15) 0.00621(15) -0.00456(15) Mo2 0.02534(18) 0.0352(2) 0.0346(2) -0.00454(17) 0.00683(16) 0.00290(16) N1 0.0206(16) 0.0220(16) 0.0212(19) 0.0013(13) 0.0055(15) 0.0015(13) N2 0.0239(16) 0.0225(16) 0.0202(17) 0.0010(14) 0.0077(14) -0.0021(14) N3 0.0216(18) 0.0377(19) 0.036(2) -0.0010(15) 0.0074(16) 0.0016(14) N4 0.0232(18) 0.0348(18) 0.034(2) 0.0020(16) 0.0062(16) 0.0035(15) O1 0.0482(19) 0.080(2) 0.0265(18) -0.0018(17) 0.0006(15) -0.0066(17) O2 0.063(2) 0.0301(16) 0.064(2) -0.0065(15) 0.0272(18) -0.0202(15) O3 0.0421(18) 0.0582(19) 0.055(2) -0.0066(16) 0.0249(17) 0.0037(15) O4 0.081(2) 0.0328(16) 0.047(2) -0.0093(15) 0.0318(18) 0.0013(15) O5 0.057(2) 0.073(2) 0.091(3) 0.0011(19) 0.042(2) 0.0234(18) O6 0.048(2) 0.0494(19) 0.059(2) -0.0061(16) -0.0004(17) -0.0104(15) O7 0.075(2) 0.0478(18) 0.064(2) 0.0135(18) 0.0184(19) 0.0105(17) O8 0.056(2) 0.075(2) 0.043(2) 0.0061(18) 0.0095(17) -0.0072(17) C1 0.0203(19) 0.0185(18) 0.025(2) 0.0004(17) 0.0083(18) 0.0045(15) C2 0.019(2) 0.025(2) 0.021(2) 0.0002(17) 0.0091(17) 0.0006(16) C3 0.022(2) 0.023(2) 0.022(2) 0.0011(16) 0.0061(18) -0.0006(15) C4 0.024(2) 0.0228(19) 0.026(2) -0.0028(17) 0.0090(18) -0.0010(16) C5 0.0198(19) 0.020(2) 0.027(2) -0.0002(16) 0.0072(17) -0.0003(15) C6 0.030(2) 0.027(2) 0.028(2) 0.0034(18) 0.0018(19) -0.0026(17) C7 0.033(2) 0.023(2) 0.048(3) 0.005(2) 0.006(2) -0.0095(18) C8 0.029(2) 0.030(2) 0.048(3) -0.006(2) 0.002(2) -0.0116(18) C9 0.020(2) 0.030(2) 0.031(2) -0.0014(18) 0.0047(18) -0.0027(16) C10 0.028(2) 0.040(2) 0.031(2) -0.009(2) 0.0000(19) -0.0108(19) C11 0.028(2) 0.044(3) 0.026(2) 0.002(2) -0.0014(19) -0.0032(19) C12 0.032(2) 0.028(2) 0.032(3) 0.0029(19) 0.010(2) -0.0025(18) C13 0.024(2) 0.024(2) 0.021(2) 0.0032(17) 0.0022(18) -0.0048(16) C14 0.021(2) 0.029(2) 0.022(2) -0.0047(17) 0.0057(18) -0.0090(16) C15 0.033(2) 0.047(3) 0.024(2) -0.002(2) 0.0106(19) -0.0077(19) C16 0.038(2) 0.042(2) 0.027(2) 0.0114(19) -0.001(2) -0.010(2) C17 0.026(2) 0.031(2) 0.038(3) 0.0106(19) 0.003(2) 0.0031(17) C18 0.024(2) 0.026(2) 0.028(2) 0.0005(18) 0.0022(17) -0.0034(17) C19 0.036(2) 0.029(2) 0.037(3) 0.0083(18) 0.017(2) 0.0054(17) C20 0.047(3) 0.032(2) 0.049(3) 0.005(2) 0.017(2) 0.013(2) C21 0.037(3) 0.050(3) 0.071(3) 0.003(2) 0.022(2) 0.004(2) C22 0.035(2) 0.029(2) 0.036(3) -0.0023(19) 0.018(2) -0.0043(18) C23 0.053(3) 0.049(3) 0.060(3) -0.025(2) 0.021(3) -0.004(2) C24 0.031(2) 0.052(3) 0.037(3) -0.005(2) 0.007(2) 0.005(2) C25 0.026(2) 0.0179(19) 0.024(2) 0.0033(16) -0.0004(18) -0.0064(16) C26 0.024(2) 0.023(2) 0.033(2) -0.0037(18) 0.0037(19) -0.0050(17) C27 0.027(2) 0.026(2) 0.045(3) -0.0030(19) -0.002(2) 0.0011(17) C28 0.046(3) 0.021(2) 0.038(3) 0.007(2) -0.009(2) -0.007(2) C29 0.044(3) 0.029(2) 0.026(2) 0.0043(19) 0.006(2) -0.0121(19) C30 0.029(2) 0.0205(19) 0.027(2) -0.0021(18) 0.0059(19) -0.0084(16) C31 0.035(2) 0.037(2) 0.023(2) 0.0036(18) 0.0111(19) -0.0001(18) C32 0.050(3) 0.041(2) 0.041(3) -0.003(2) 0.020(2) -0.004(2) C33 0.042(3) 0.069(3) 0.054(3) -0.011(3) 0.022(2) -0.013(2) C34 0.025(2) 0.038(2) 0.048(3) 0.003(2) 0.011(2) 0.0025(18) C35 0.039(3) 0.039(2) 0.090(4) -0.005(2) 0.033(3) -0.002(2) C36 0.059(3) 0.064(3) 0.088(4) -0.030(3) 0.045(3) -0.020(3) C37 0.038(2) 0.044(2) 0.028(3) -0.002(2) 0.011(2) -0.009(2) C38 0.034(2) 0.036(2) 0.027(2) -0.0122(19) 0.003(2) -0.0012(19) C39 0.040(3) 0.027(2) 0.028(2) 0.0032(18) 0.007(2) -0.0048(19) C40 0.043(3) 0.022(2) 0.031(2) 0.0011(19) 0.008(2) -0.0052(18) C41 0.028(2) 0.033(2) 0.032(2) -0.002(2) 0.0068(19) 0.0041(18) C42 0.028(2) 0.034(2) 0.029(2) -0.0019(19) 0.0034(19) 0.0018(18) C43 0.034(2) 0.033(2) 0.035(2) -0.005(2) 0.009(2) 0.007(2) C44 0.037(2) 0.032(2) 0.032(2) -0.0039(19) 0.009(2) 0.0017(19) C45 0.030(2) 0.033(2) 0.040(3) -0.0028(19) 0.010(2) 0.0002(18) C46 0.035(3) 0.051(3) 0.039(3) -0.009(2) 0.011(2) -0.005(2) C47 0.043(3) 0.050(3) 0.040(3) -0.011(2) 0.007(2) -0.015(2) C48 0.059(3) 0.045(3) 0.033(3) -0.007(2) 0.011(2) -0.001(2) C49 0.039(3) 0.038(2) 0.034(3) -0.005(2) 0.008(2) 0.005(2) C50 0.051(3) 0.046(3) 0.041(3) -0.011(2) 0.008(2) 0.011(2) C51 0.043(3) 0.063(3) 0.041(3) -0.010(2) 0.010(2) 0.020(2) C52 0.032(2) 0.051(3) 0.042(3) -0.012(2) 0.005(2) 0.009(2) C53 0.025(2) 0.044(2) 0.035(3) -0.008(2) 0.008(2) 0.0012(19) C54 0.038(3) 0.049(3) 0.046(3) -0.015(2) 0.014(2) -0.013(2) C55 0.042(3) 0.077(3) 0.063(4) -0.019(3) 0.027(3) -0.014(3) C56 0.028(3) 0.115(5) 0.070(4) -0.036(4) 0.019(3) -0.010(3) C57 0.031(3) 0.109(4) 0.052(3) -0.020(3) -0.001(3) 0.010(3) C58 0.034(3) 0.062(3) 0.037(3) -0.010(2) 0.005(2) 0.001(2) C59 0.052(3) 0.065(3) 0.043(3) 0.010(3) -0.009(2) 0.008(3) C60 0.097(5) 0.083(4) 0.092(5) 0.022(3) 0.003(4) 0.031(3) C61 0.091(4) 0.107(4) 0.053(4) 0.015(3) 0.013(3) -0.003(3) C62 0.062(3) 0.045(3) 0.061(3) -0.004(2) 0.021(3) -0.020(2) C63 0.103(4) 0.095(4) 0.056(4) -0.006(3) 0.033(3) -0.028(4) C64 0.126(5) 0.052(3) 0.094(5) 0.005(3) 0.035(4) -0.015(3) C65 0.027(2) 0.031(2) 0.030(2) -0.0080(19) 0.0057(19) 0.0017(18) C66 0.028(2) 0.035(2) 0.031(2) -0.0012(19) 0.0071(19) 0.0063(18) C67 0.033(3) 0.046(3) 0.034(3) 0.002(2) -0.002(2) 0.012(2) C68 0.023(2) 0.046(3) 0.057(3) -0.002(2) 0.003(2) -0.002(2) C69 0.030(2) 0.039(2) 0.061(3) 0.004(2) 0.015(2) -0.003(2) C70 0.033(2) 0.035(2) 0.039(3) 0.006(2) 0.010(2) 0.0065(19) C71 0.039(3) 0.053(3) 0.056(3) 0.017(2) 0.017(2) 0.014(2) C72 0.071(4) 0.054(3) 0.096(5) 0.033(3) 0.010(3) 0.006(3) C73 0.075(4) 0.102(4) 0.046(3) 0.027(3) 0.016(3) 0.027(3) C74 0.040(2) 0.050(3) 0.046(3) 0.016(2) 0.016(2) 0.016(2) C75 0.090(4) 0.116(5) 0.046(4) 0.006(3) 0.029(3) 0.002(3) C76 0.126(5) 0.049(3) 0.089(5) 0.014(3) 0.062(4) -0.003(3) C77 0.037(3) 0.048(3) 0.049(3) 0.001(2) 0.012(2) 0.008(2) C78 0.031(2) 0.038(2) 0.042(3) -0.001(2) 0.011(2) 0.002(2) C79 0.033(3) 0.050(3) 0.047(3) -0.008(2) 0.008(2) 0.004(2) C80 0.031(2) 0.047(3) 0.043(3) -0.007(2) 0.009(2) -0.004(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 Mo1 C37 1.963(4) . ? Mo1 C38 1.971(4) . ? Mo1 C40 2.023(4) . ? Mo1 C39 2.051(4) . ? Mo1 N1 2.242(3) . ? Mo1 N2 2.246(3) . ? Mo2 C77 1.946(4) . ? Mo2 C78 1.958(4) . ? Mo2 C80 2.023(5) . ? Mo2 C79 2.045(5) . ? Mo2 N3 2.237(3) . ? Mo2 N4 2.247(3) . ? N1 C1 1.293(4) . ? N1 C13 1.452(4) . ? N2 C2 1.300(4) . ? N2 C25 1.449(4) . ? N3 C41 1.301(4) . ? N3 C53 1.458(4) . ? N4 C42 1.295(4) . ? N4 C65 1.453(4) . ? O1 C37 1.155(4) . ? O2 C38 1.154(4) . ? O3 C39 1.142(4) . ? O4 C40 1.151(4) . ? O5 C77 1.168(4) . ? O6 C78 1.164(4) . ? O7 C79 1.145(4) . ? O8 C80 1.155(4) . ? C1 C5 1.470(4) . ? C1 C2 1.480(5) . ? C2 C3 1.463(5) . ? C3 C12 1.381(5) . ? C3 C4 1.419(4) . ? C4 C9 1.399(5) . ? C4 C5 1.418(5) . ? C5 C6 1.373(4) . ? C6 C7 1.414(5) . ? C7 C8 1.366(5) . ? C8 C9 1.406(5) . ? C9 C10 1.427(5) . ? C10 C11 1.362(5) . ? C11 C12 1.410(5) . ? C13 C18 1.395(4) . ? C13 C14 1.401(4) . ? C14 C15 1.395(5) . ? C14 C22 1.510(5) . ? C15 C16 1.379(5) . ? C16 C17 1.371(5) . ? C17 C18 1.392(5) . ? C18 C19 1.508(5) . ? C19 C20 1.531(5) . ? C19 C21 1.541(5) . ? C22 C24 1.523(5) . ? C22 C23 1.525(5) . ? C25 C30 1.398(5) . ? C25 C26 1.413(4) . ? C26 C27 1.390(5) . ? C26 C34 1.519(5) . ? C27 C28 1.385(5) . ? C28 C29 1.370(5) . ? C29 C30 1.397(5) . ? C30 C31 1.512(5) . ? C31 C33 1.522(5) . ? C31 C32 1.523(5) . ? C34 C36 1.516(5) . ? C34 C35 1.519(5) . ? C41 C45 1.473(5) . ? C41 C42 1.475(5) . ? C42 C43 1.466(5) . ? C43 C52 1.381(5) . ? C43 C44 1.415(5) . ? C44 C49 1.402(5) . ? C44 C45 1.414(5) . ? C45 C46 1.383(5) . ? C46 C47 1.403(5) . ? C47 C48 1.372(5) . ? C48 C49 1.413(5) . ? C49 C50 1.412(5) . ? C50 C51 1.371(5) . ? C51 C52 1.415(5) . ? C53 C58 1.381(5) . ? C53 C54 1.394(5) . ? C54 C55 1.382(6) . ? C54 C62 1.524(6) . ? C55 C56 1.369(6) . ? C56 C57 1.374(6) . ? C57 C58 1.403(6) . ? C58 C59 1.520(6) . ? C59 C60 1.532(6) . ? C59 C61 1.537(6) . ? C62 C63 1.530(6) . ? C62 C64 1.532(6) . ? C65 C70 1.394(5) . ? C65 C66 1.400(5) . ? C66 C67 1.389(5) . ? C66 C74 1.513(5) . ? C67 C68 1.377(5) . ? C68 C69 1.367(5) . ? C69 C70 1.394(5) . ? C70 C71 1.525(5) . ? C71 C72 1.500(5) . ? C71 C73 1.522(6) . ? C74 C75 1.507(6) . ? C74 C76 1.531(5) . ? 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 C37 Mo1 C38 89.71(15) . . ? C37 Mo1 C40 83.67(15) . . ? C38 Mo1 C40 86.45(14) . . ? C37 Mo1 C39 83.37(15) . . ? C38 Mo1 C39 82.88(14) . . ? C40 Mo1 C39 163.23(15) . . ? C37 Mo1 N1 99.16(13) . . ? C38 Mo1 N1 170.40(13) . . ? C40 Mo1 N1 98.12(12) . . ? C39 Mo1 N1 94.42(11) . . ? C37 Mo1 N2 171.84(12) . . ? C38 Mo1 N2 98.37(13) . . ? C40 Mo1 N2 97.91(13) . . ? C39 Mo1 N2 96.42(12) . . ? N1 Mo1 N2 72.70(10) . . ? C77 Mo2 C78 91.85(16) . . ? C77 Mo2 C80 84.86(16) . . ? C78 Mo2 C80 85.34(16) . . ? C77 Mo2 C79 82.68(16) . . ? C78 Mo2 C79 84.12(16) . . ? C80 Mo2 C79 163.39(16) . . ? C77 Mo2 N3 97.44(14) . . ? C78 Mo2 N3 170.70(13) . . ? C80 Mo2 N3 95.55(14) . . ? C79 Mo2 N3 96.92(14) . . ? C77 Mo2 N4 170.22(15) . . ? C78 Mo2 N4 97.80(13) . . ? C80 Mo2 N4 97.45(13) . . ? C79 Mo2 N4 96.68(13) . . ? N3 Mo2 N4 72.90(11) . . ? C1 N1 C13 117.5(3) . . ? C1 N1 Mo1 115.5(2) . . ? C13 N1 Mo1 126.9(2) . . ? C2 N2 C25 118.3(3) . . ? C2 N2 Mo1 115.5(2) . . ? C25 N2 Mo1 126.1(2) . . ? C41 N3 C53 115.5(3) . . ? C41 N3 Mo2 116.2(2) . . ? C53 N3 Mo2 128.3(2) . . ? C42 N4 C65 118.0(3) . . ? C42 N4 Mo2 116.3(2) . . ? C65 N4 Mo2 125.6(2) . . ? N1 C1 C5 135.3(3) . . ? N1 C1 C2 117.4(3) . . ? C5 C1 C2 107.2(3) . . ? N2 C2 C3 134.9(3) . . ? N2 C2 C1 116.8(3) . . ? C3 C2 C1 108.2(3) . . ? C12 C3 C4 118.5(3) . . ? C12 C3 C2 136.0(3) . . ? C4 C3 C2 105.4(3) . . ? C9 C4 C5 122.9(3) . . ? C9 C4 C3 123.7(3) . . ? C5 C4 C3 113.4(3) . . ? C6 C5 C4 118.7(3) . . ? C6 C5 C1 135.5(3) . . ? C4 C5 C1 105.8(3) . . ? C5 C6 C7 118.6(3) . . ? C8 C7 C6 122.5(3) . . ? C7 C8 C9 120.4(3) . . ? C4 C9 C8 116.9(3) . . ? C4 C9 C10 115.6(3) . . ? C8 C9 C10 127.5(3) . . ? C11 C10 C9 121.2(3) . . ? C10 C11 C12 122.3(4) . . ? C3 C12 C11 118.8(3) . . ? C18 C13 C14 122.6(3) . . ? C18 C13 N1 120.0(3) . . ? C14 C13 N1 117.4(3) . . ? C15 C14 C13 116.8(3) . . ? C15 C14 C22 120.3(3) . . ? C13 C14 C22 122.8(3) . . ? C16 C15 C14 121.7(3) . . ? C17 C16 C15 119.8(4) . . ? C16 C17 C18 121.5(3) . . ? C17 C18 C13 117.5(3) . . ? C17 C18 C19 119.9(3) . . ? C13 C18 C19 122.6(3) . . ? C18 C19 C20 112.2(3) . . ? C18 C19 C21 110.5(3) . . ? C20 C19 C21 109.9(3) . . ? C14 C22 C24 111.5(3) . . ? C14 C22 C23 113.2(3) . . ? C24 C22 C23 110.4(3) . . ? C30 C25 C26 122.7(3) . . ? C30 C25 N2 119.9(3) . . ? C26 C25 N2 117.4(3) . . ? C27 C26 C25 116.8(3) . . ? C27 C26 C34 120.0(3) . . ? C25 C26 C34 123.2(3) . . ? C28 C27 C26 121.3(3) . . ? C29 C28 C27 120.7(3) . . ? C28 C29 C30 121.0(4) . . ? C29 C30 C25 117.5(3) . . ? C29 C30 C31 120.1(3) . . ? C25 C30 C31 122.3(3) . . ? C30 C31 C33 112.0(3) . . ? C30 C31 C32 111.0(3) . . ? C33 C31 C32 110.3(3) . . ? C36 C34 C35 108.4(3) . . ? C36 C34 C26 114.3(3) . . ? C35 C34 C26 111.9(3) . . ? O1 C37 Mo1 179.1(3) . . ? O2 C38 Mo1 178.1(3) . . ? O3 C39 Mo1 170.1(3) . . ? O4 C40 Mo1 171.0(3) . . ? N3 C41 C45 134.7(3) . . ? N3 C41 C42 117.4(3) . . ? C45 C41 C42 107.9(3) . . ? N4 C42 C43 135.3(3) . . ? N4 C42 C41 117.1(3) . . ? C43 C42 C41 107.6(3) . . ? C52 C43 C44 119.5(3) . . ? C52 C43 C42 134.9(4) . . ? C44 C43 C42 105.6(3) . . ? C49 C44 C45 123.3(4) . . ? C49 C44 C43 122.9(3) . . ? C45 C44 C43 113.8(3) . . ? C46 C45 C44 118.6(3) . . ? C46 C45 C41 136.3(3) . . ? C44 C45 C41 105.1(3) . . ? C45 C46 C47 118.9(4) . . ? C48 C47 C46 122.1(4) . . ? C47 C48 C49 121.0(4) . . ? C44 C49 C50 116.5(4) . . ? C44 C49 C48 116.0(4) . . ? C50 C49 C48 127.5(4) . . ? C51 C50 C49 120.6(4) . . ? C50 C51 C52 122.8(4) . . ? C43 C52 C51 117.7(4) . . ? C58 C53 C54 122.5(4) . . ? C58 C53 N3 118.9(3) . . ? C54 C53 N3 118.6(4) . . ? C55 C54 C53 117.9(4) . . ? C55 C54 C62 119.8(4) . . ? C53 C54 C62 122.3(4) . . ? C56 C55 C54 120.8(5) . . ? C55 C56 C57 120.7(5) . . ? C56 C57 C58 120.5(5) . . ? C53 C58 C57 117.5(4) . . ? C53 C58 C59 122.7(4) . . ? C57 C58 C59 119.8(4) . . ? C58 C59 C60 111.7(4) . . ? C58 C59 C61 111.7(4) . . ? C60 C59 C61 112.0(4) . . ? C54 C62 C63 110.3(4) . . ? C54 C62 C64 111.6(4) . . ? C63 C62 C64 110.9(4) . . ? C70 C65 C66 122.3(3) . . ? C70 C65 N4 118.6(3) . . ? C66 C65 N4 119.1(3) . . ? C67 C66 C65 117.1(3) . . ? C67 C66 C74 120.5(4) . . ? C65 C66 C74 122.3(3) . . ? C68 C67 C66 121.8(4) . . ? C69 C68 C67 119.8(4) . . ? C68 C69 C70 121.5(4) . . ? C69 C70 C65 117.5(4) . . ? C69 C70 C71 120.0(3) . . ? C65 C70 C71 122.4(3) . . ? C72 C71 C73 111.9(4) . . ? C72 C71 C70 112.7(4) . . ? C73 C71 C70 111.3(3) . . ? C75 C74 C66 111.8(4) . . ? C75 C74 C76 110.6(4) . . ? C66 C74 C76 111.9(3) . . ? O5 C77 Mo2 179.2(4) . . ? O6 C78 Mo2 178.8(3) . . ? O7 C79 Mo2 170.7(4) . . ? O8 C80 Mo2 172.2(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.394 _refine_diff_density_min -0.626 _refine_diff_density_rms 0.061 # Attachment 'compound_4.CIF' data_fed50 _database_code_depnum_ccdc_archive 'CCDC 719954' _audit_creation_method ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H24 Mo N2 O4 Si2' _chemical_formula_weight 532.55 _chemical_absolute_configuration ad 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' O O 0.0106 0.0060 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 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 6.8006(2) _cell_length_b 16.5995(3) _cell_length_c 20.8751(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2356.52(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8722 _cell_measurement_theta_min 3.1298 _cell_measurement_theta_max 32.3813 _exptl_crystal_description rod _exptl_crystal_colour black _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.501 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 0.689 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8149 _exptl_absorpt_correction_T_max 0.9598 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Oxford Diffraction Xcalibur S Sapphire' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22311 _diffrn_reflns_av_R_equivalents 0.0601 _diffrn_reflns_av_sigmaI/netI 0.0527 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 24.99 _reflns_number_total 4140 _reflns_number_gt 3686 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0202P)^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 0.04(3) _refine_ls_number_reflns 4140 _refine_ls_number_parameters 286 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0487 _refine_ls_wR_factor_gt 0.0469 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.969 _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 -0.05647(4) 0.053407(16) 0.346352(14) 0.01999(7) Uani 1 1 d . . . Si1 Si 0.13908(15) -0.11422(6) 0.26051(5) 0.0227(2) Uani 1 1 d . . . Si2 Si 0.13808(14) 0.09836(5) 0.50300(5) 0.0214(2) Uani 1 1 d . . . N1 N 0.0790(4) -0.07188(12) 0.33699(12) 0.0178(6) Uani 1 1 d . . . N2 N 0.0733(4) 0.02453(13) 0.44424(12) 0.0196(6) Uani 1 1 d . . . O1 O -0.4705(4) -0.02452(15) 0.37877(13) 0.0469(7) Uani 1 1 d . . . O2 O 0.3126(4) 0.15278(15) 0.29317(14) 0.0478(8) Uani 1 1 d . . . O3 O -0.2446(4) 0.07366(16) 0.21127(12) 0.0461(8) Uani 1 1 d . . . O4 O -0.2679(4) 0.21576(15) 0.37746(13) 0.0469(8) Uani 1 1 d . . . C1 C 0.0897(4) -0.10558(17) 0.39278(14) 0.0152(7) Uani 1 1 d . . . C2 C 0.0895(4) -0.05286(19) 0.45195(13) 0.0169(7) Uani 1 1 d . . . C3 C 0.1113(4) -0.10663(18) 0.50763(15) 0.0171(7) Uani 1 1 d . . . C4 C 0.1198(4) -0.18586(18) 0.48280(15) 0.0169(8) Uani 1 1 d . . . C5 C 0.1102(4) -0.18963(18) 0.41538(15) 0.0184(8) Uani 1 1 d . . . C6 C 0.1002(5) -0.26419(17) 0.38651(16) 0.0220(8) Uani 1 1 d . . . H6 H 0.0864 -0.2686 0.3414 0.026 Uiso 1 1 calc R . . C7 C 0.1109(5) -0.33426(19) 0.42525(17) 0.0267(9) Uani 1 1 d . . . H7 H 0.1090 -0.3857 0.4053 0.032 Uiso 1 1 calc R . . C8 C 0.1239(5) -0.32994(19) 0.49063(17) 0.0238(9) Uani 1 1 d . . . H8 H 0.1320 -0.3782 0.5149 0.029 Uiso 1 1 calc R . . C9 C 0.1255(5) -0.25468(19) 0.52263(16) 0.0205(8) Uani 1 1 d . . . C10 C 0.1245(5) -0.24096(19) 0.58874(16) 0.0244(9) Uani 1 1 d . . . H10 H 0.1320 -0.2855 0.6172 0.029 Uiso 1 1 calc R . . C11 C 0.1130(5) -0.16422(18) 0.61324(16) 0.0248(9) Uani 1 1 d . . . H11 H 0.1097 -0.1569 0.6584 0.030 Uiso 1 1 calc R . . C12 C 0.1060(5) -0.09604(18) 0.57300(14) 0.0223(8) Uani 1 1 d . . . H12 H 0.0977 -0.0435 0.5908 0.027 Uiso 1 1 calc R . . C13 C -0.0883(6) -0.1589(2) 0.22729(18) 0.0397(10) Uani 1 1 d . . . H13A H -0.1383 -0.2000 0.2568 0.060 Uiso 1 1 calc R . . H13B H -0.0595 -0.1838 0.1857 0.060 Uiso 1 1 calc R . . H13C H -0.1875 -0.1167 0.2217 0.060 Uiso 1 1 calc R . . C14 C 0.2338(6) -0.03197(19) 0.20888(17) 0.0352(10) Uani 1 1 d . . . H14A H 0.1271 0.0058 0.1993 0.053 Uiso 1 1 calc R . . H14B H 0.2845 -0.0548 0.1689 0.053 Uiso 1 1 calc R . . H14C H 0.3397 -0.0035 0.2312 0.053 Uiso 1 1 calc R . . C15 C 0.3496(5) -0.1849(2) 0.26637(18) 0.0351(10) Uani 1 1 d . . . H15A H 0.3068 -0.2347 0.2874 0.053 Uiso 1 1 calc R . . H15B H 0.4551 -0.1600 0.2915 0.053 Uiso 1 1 calc R . . H15C H 0.3982 -0.1974 0.2233 0.053 Uiso 1 1 calc R . . C16 C -0.0645(6) 0.10865(18) 0.56156(15) 0.0301(8) Uani 1 1 d . . . H16A H -0.0864 0.0569 0.5830 0.045 Uiso 1 1 calc R . . H16B H -0.1848 0.1250 0.5392 0.045 Uiso 1 1 calc R . . H16C H -0.0297 0.1495 0.5935 0.045 Uiso 1 1 calc R . . C17 C 0.1803(6) 0.19780(18) 0.46428(18) 0.0328(10) Uani 1 1 d . . . H17A H 0.0599 0.2152 0.4425 0.049 Uiso 1 1 calc R . . H17B H 0.2870 0.1931 0.4330 0.049 Uiso 1 1 calc R . . H17C H 0.2162 0.2375 0.4970 0.049 Uiso 1 1 calc R . . C18 C 0.3815(5) 0.0695(2) 0.53600(17) 0.0301(9) Uani 1 1 d . . . H18A H 0.3736 0.0153 0.5544 0.045 Uiso 1 1 calc R . . H18B H 0.4199 0.1079 0.5694 0.045 Uiso 1 1 calc R . . H18C H 0.4797 0.0700 0.5016 0.045 Uiso 1 1 calc R . . C19 C -0.3151(6) 0.0016(2) 0.36905(16) 0.0268(9) Uani 1 1 d . . . C20 C 0.1869(6) 0.1155(2) 0.31397(17) 0.0304(9) Uani 1 1 d . . . C21 C -0.1706(5) 0.0658(2) 0.26109(17) 0.0288(9) Uani 1 1 d . . . C22 C -0.1853(6) 0.1557(2) 0.36575(16) 0.0294(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.02321(15) 0.01929(12) 0.01748(13) 0.00274(14) -0.00048(15) 0.00097(15) Si1 0.0261(6) 0.0258(5) 0.0161(5) -0.0015(4) 0.0006(4) 0.0005(5) Si2 0.0247(6) 0.0186(5) 0.0211(5) -0.0010(4) -0.0019(4) -0.0027(4) N1 0.0173(15) 0.0208(13) 0.0152(15) 0.0005(11) 0.0002(13) -0.0033(12) N2 0.0182(16) 0.0195(13) 0.0211(15) 0.0012(11) 0.0009(14) -0.0006(14) O1 0.0297(17) 0.0559(18) 0.0550(19) 0.0104(13) 0.0037(14) -0.0081(14) O2 0.050(2) 0.0413(17) 0.052(2) 0.0038(15) 0.0196(16) -0.0191(15) O3 0.0526(19) 0.0615(19) 0.0242(16) 0.0077(14) -0.0098(14) 0.0124(15) O4 0.059(2) 0.0365(16) 0.0452(19) -0.0057(14) -0.0045(15) 0.0218(15) C1 0.0088(19) 0.0201(15) 0.0168(17) -0.0006(14) 0.0028(14) -0.0021(15) C2 0.0128(18) 0.0197(15) 0.0182(16) 0.0011(16) -0.0009(13) -0.0021(18) C3 0.012(2) 0.0225(16) 0.0163(18) 0.0010(15) 0.0006(13) 0.0005(14) C4 0.011(2) 0.0219(17) 0.0182(19) -0.0002(14) 0.0006(14) -0.0006(15) C5 0.012(2) 0.0206(16) 0.0227(19) -0.0015(14) 0.0003(14) 0.0006(15) C6 0.018(2) 0.0237(17) 0.0238(19) -0.0014(15) 0.0024(16) -0.0016(16) C7 0.023(2) 0.0215(17) 0.036(2) -0.0001(16) 0.0043(17) -0.0025(16) C8 0.018(2) 0.0200(17) 0.034(2) 0.0093(16) 0.0048(16) 0.0003(15) C9 0.0154(19) 0.0202(16) 0.026(2) 0.0047(15) 0.0030(15) -0.0014(15) C10 0.022(2) 0.0275(19) 0.024(2) 0.0103(16) -0.0018(16) -0.0003(16) C11 0.024(2) 0.0335(19) 0.0166(19) 0.0032(16) -0.0005(16) 0.0021(17) C12 0.023(2) 0.0218(16) 0.022(2) 0.0006(15) -0.0008(15) 0.0014(15) C13 0.038(3) 0.045(2) 0.037(2) -0.0132(19) -0.005(2) -0.002(2) C14 0.047(3) 0.038(2) 0.021(2) 0.0011(17) 0.0103(18) 0.0069(19) C15 0.035(2) 0.039(2) 0.031(2) -0.0033(19) 0.0097(19) 0.0072(19) C16 0.029(2) 0.0271(17) 0.034(2) -0.0019(16) -0.005(2) 0.007(2) C17 0.041(3) 0.0243(19) 0.033(2) -0.0038(17) -0.0045(19) -0.0123(18) C18 0.025(2) 0.035(2) 0.030(2) -0.0059(17) 0.0011(15) -0.0055(18) C19 0.031(2) 0.0262(19) 0.023(2) 0.0008(16) -0.0040(17) 0.0078(19) C20 0.043(3) 0.0238(19) 0.025(2) -0.0019(17) 0.0014(18) 0.007(2) C21 0.031(2) 0.030(2) 0.025(2) 0.0055(18) 0.0018(17) 0.0063(18) C22 0.037(2) 0.034(2) 0.017(2) 0.0056(16) -0.0030(17) 0.001(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 Mo1 C22 1.953(4) . ? Mo1 C21 1.953(4) . ? Mo1 C19 2.014(4) . ? Mo1 C20 2.064(4) . ? Mo1 N2 2.277(3) . ? Mo1 N1 2.283(2) . ? Si1 N1 1.792(3) . ? Si1 C13 1.850(4) . ? Si1 C14 1.855(3) . ? Si1 C15 1.855(3) . ? Si2 N2 1.789(3) . ? Si2 C16 1.850(4) . ? Si2 C18 1.856(3) . ? Si2 C17 1.860(3) . ? N1 C1 1.294(4) . ? N2 C2 1.299(4) . ? O1 C19 1.161(4) . ? O2 C20 1.141(4) . ? O3 C21 1.163(4) . ? O4 C22 1.171(4) . ? C1 C5 1.479(4) . ? C1 C2 1.514(4) . ? C2 C3 1.473(4) . ? C3 C12 1.376(4) . ? C3 C4 1.415(4) . ? C4 C5 1.410(4) . ? C4 C9 1.413(4) . ? C5 C6 1.378(4) . ? C6 C7 1.418(4) . ? C7 C8 1.370(4) . ? C8 C9 1.417(4) . ? C9 C10 1.399(5) . ? C10 C11 1.375(4) . ? C11 C12 1.410(4) . ? 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 C22 Mo1 C21 85.35(14) . . ? C22 Mo1 C19 86.03(15) . . ? C21 Mo1 C19 84.97(14) . . ? C22 Mo1 C20 89.62(14) . . ? C21 Mo1 C20 88.15(14) . . ? C19 Mo1 C20 172.13(14) . . ? C22 Mo1 N2 99.83(12) . . ? C21 Mo1 N2 173.90(12) . . ? C19 Mo1 N2 92.14(12) . . ? C20 Mo1 N2 95.07(12) . . ? C22 Mo1 N1 172.18(12) . . ? C21 Mo1 N1 100.29(12) . . ? C19 Mo1 N1 89.05(11) . . ? C20 Mo1 N1 95.93(11) . . ? N2 Mo1 N1 74.25(8) . . ? N1 Si1 C13 107.51(15) . . ? N1 Si1 C14 107.95(13) . . ? C13 Si1 C14 111.57(17) . . ? N1 Si1 C15 111.44(15) . . ? C13 Si1 C15 114.59(17) . . ? C14 Si1 C15 103.64(17) . . ? N2 Si2 C16 109.44(15) . . ? N2 Si2 C18 107.30(14) . . ? C16 Si2 C18 116.29(16) . . ? N2 Si2 C17 110.36(14) . . ? C16 Si2 C17 108.67(16) . . ? C18 Si2 C17 104.63(16) . . ? C1 N1 Si1 128.29(19) . . ? C1 N1 Mo1 109.84(19) . . ? Si1 N1 Mo1 121.72(12) . . ? C2 N2 Si2 124.8(2) . . ? C2 N2 Mo1 110.63(19) . . ? Si2 N2 Mo1 124.51(12) . . ? N1 C1 C5 134.4(3) . . ? N1 C1 C2 119.0(2) . . ? C5 C1 C2 106.6(2) . . ? N2 C2 C3 134.9(3) . . ? N2 C2 C1 118.1(3) . . ? C3 C2 C1 107.1(2) . . ? C12 C3 C4 118.9(3) . . ? C12 C3 C2 134.6(3) . . ? C4 C3 C2 106.2(3) . . ? C5 C4 C9 123.5(3) . . ? C5 C4 C3 113.9(3) . . ? C9 C4 C3 122.5(3) . . ? C6 C5 C4 118.6(3) . . ? C6 C5 C1 134.6(3) . . ? C4 C5 C1 106.3(3) . . ? C5 C6 C7 119.0(3) . . ? C8 C7 C6 121.9(3) . . ? C7 C8 C9 121.1(3) . . ? C10 C9 C4 116.7(3) . . ? C10 C9 C8 127.5(3) . . ? C4 C9 C8 115.8(3) . . ? C11 C10 C9 121.2(3) . . ? C10 C11 C12 121.6(3) . . ? C3 C12 C11 119.2(3) . . ? O1 C19 Mo1 174.9(3) . . ? O2 C20 Mo1 175.1(3) . . ? O3 C21 Mo1 177.7(3) . . ? O4 C22 Mo1 177.9(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.255 _refine_diff_density_min -0.244 _refine_diff_density_rms 0.056 # Attachment 'compound_5.cif' data_a _database_code_depnum_ccdc_archive 'CCDC 719955' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H45 N2 Ni, 0' _chemical_formula_sum 'C44 H52 N2 Ni' _chemical_formula_weight 667.59 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' N N 0.0061 0.0033 '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' 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.3259(12) _cell_length_b 12.5980(13) _cell_length_c 13.4184(13) _cell_angle_alpha 69.714(4) _cell_angle_beta 78.287(3) _cell_angle_gamma 79.081(4) _cell_volume 1897.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 3 _cell_measurement_theta_max 29 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.168 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 716 _exptl_absorpt_coefficient_mu 0.543 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.885 _exptl_absorpt_correction_T_max 0.913 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type "Bruker APEX II CCD area detector'" _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20427 _diffrn_reflns_av_R_equivalents 0.0225 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 29.00 _reflns_number_total 9999 _reflns_number_gt 8776 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+0.6781P] 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 9999 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0402 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0901 _refine_ls_wR_factor_gt 0.0862 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.009 _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 0.158175(13) 0.770541(13) 0.783259(12) 0.01330(5) Uani 1 1 d . . . N1 N 0.26107(9) 0.80028(9) 0.86069(8) 0.01335(19) Uani 1 1 d . . . C1 C 0.36612(10) 0.78241(10) 0.81901(9) 0.0126(2) Uani 1 1 d . . . N2 N 0.29576(8) 0.73330(8) 0.69361(8) 0.01233(19) Uani 1 1 d . . . C2 C 0.38555(10) 0.74496(10) 0.72550(9) 0.0121(2) Uani 1 1 d . . . C3 C 0.50664(10) 0.72709(10) 0.69087(10) 0.0137(2) Uani 1 1 d . . . C4 C 0.55593(10) 0.75591(10) 0.76417(10) 0.0137(2) Uani 1 1 d . . . C5 C 0.47485(10) 0.78901(10) 0.84396(10) 0.0141(2) Uani 1 1 d . . . C7 C 0.62855(12) 0.81463(12) 0.91524(11) 0.0235(3) Uani 1 1 d . . . H7A H 0.6541 0.8351 0.9675 0.028 Uiso 1 1 calc R . . C6 C 0.51173(11) 0.81826(11) 0.92044(11) 0.0194(3) Uani 1 1 d . . . H6A H 0.4602 0.8402 0.9751 0.023 Uiso 1 1 calc R . . C8 C 0.70629(11) 0.78289(12) 0.83819(11) 0.0212(3) Uani 1 1 d . . . H8A H 0.7836 0.7818 0.8379 0.025 Uiso 1 1 calc R . . C9 C 0.67086(10) 0.75149(10) 0.75845(10) 0.0163(2) Uani 1 1 d . . . C10 C 0.74004(11) 0.71557(11) 0.67442(11) 0.0202(3) Uani 1 1 d . . . H10A H 0.8189 0.7113 0.6669 0.024 Uiso 1 1 calc R . . C11 C 0.69318(11) 0.68684(12) 0.60382(11) 0.0208(3) Uani 1 1 d . . . H11A H 0.7412 0.6628 0.5485 0.025 Uiso 1 1 calc R . . C12 C 0.57586(11) 0.69182(11) 0.61063(10) 0.0178(2) Uani 1 1 d . . . H12A H 0.5458 0.6713 0.5610 0.021 Uiso 1 1 calc R . . C13 C 0.23793(10) 0.82793(10) 0.95875(9) 0.0132(2) Uani 1 1 d . . . C14 C 0.23813(11) 0.73841(11) 1.05697(10) 0.0169(2) Uani 1 1 d . . . C15 C 0.22388(12) 0.76721(12) 1.15085(10) 0.0222(3) Uani 1 1 d . . . H15A H 0.2252 0.7084 1.2182 0.027 Uiso 1 1 calc R . . C16 C 0.20783(12) 0.88058(13) 1.14712(11) 0.0237(3) Uani 1 1 d . . . H16A H 0.2012 0.8987 1.2114 0.028 Uiso 1 1 calc R . . C17 C 0.20150(12) 0.96754(12) 1.04995(11) 0.0210(3) Uani 1 1 d . . . H17A H 0.1880 1.0447 1.0488 0.025 Uiso 1 1 calc R . . C18 C 0.21469(11) 0.94339(10) 0.95383(10) 0.0161(2) Uani 1 1 d . . . C19 C 0.20496(13) 1.03811(11) 0.84728(11) 0.0231(3) Uani 1 1 d . . . H19A H 0.1912 1.0028 0.7954 0.028 Uiso 1 1 calc R . . C20 C 0.31314(15) 1.09102(14) 0.80102(15) 0.0411(4) Uani 1 1 d . . . H20A H 0.3752 1.0311 0.7949 0.062 Uiso 1 1 calc R . . H20B H 0.3275 1.1291 0.8486 0.062 Uiso 1 1 calc R . . H20C H 0.3064 1.1469 0.7298 0.062 Uiso 1 1 calc R . . C21 C 0.10584(13) 1.12991(13) 0.85660(13) 0.0300(3) Uani 1 1 d . . . H21A H 0.0378 1.0937 0.8896 0.045 Uiso 1 1 calc R . . H21B H 0.0961 1.1833 0.7849 0.045 Uiso 1 1 calc R . . H21C H 0.1202 1.1714 0.9013 0.045 Uiso 1 1 calc R . . C22 C 0.25212(13) 0.61408(11) 1.06163(11) 0.0230(3) Uani 1 1 d . . . H22A H 0.2505 0.6132 0.9877 0.028 Uiso 1 1 calc R . . C23 C 0.36456(14) 0.55021(13) 1.09445(15) 0.0351(4) Uani 1 1 d . . . H23A H 0.4250 0.5919 1.0471 0.053 Uiso 1 1 calc R . . H23B H 0.3744 0.4735 1.0884 0.053 Uiso 1 1 calc R . . H23C H 0.3663 0.5442 1.1689 0.053 Uiso 1 1 calc R . . C24 C 0.15603(14) 0.55268(13) 1.13648(16) 0.0370(4) Uani 1 1 d . . . H24A H 0.0848 0.5943 1.1140 0.055 Uiso 1 1 calc R . . H24B H 0.1575 0.5493 1.2103 0.055 Uiso 1 1 calc R . . H24C H 0.1642 0.4750 1.1331 0.055 Uiso 1 1 calc R . . C25 C 0.30972(10) 0.69136(10) 0.60431(10) 0.0138(2) Uani 1 1 d . . . C26 C 0.30483(11) 0.57438(11) 0.62686(11) 0.0183(2) Uani 1 1 d . . . C27 C 0.31982(13) 0.53397(13) 0.53965(12) 0.0270(3) Uani 1 1 d . . . H27A H 0.3181 0.4552 0.5524 0.032 Uiso 1 1 calc R . . C28 C 0.33708(14) 0.60665(15) 0.43495(12) 0.0315(3) Uani 1 1 d . . . H28A H 0.3471 0.5775 0.3768 0.038 Uiso 1 1 calc R . . C29 C 0.33983(13) 0.72207(14) 0.41467(11) 0.0272(3) Uani 1 1 d . . . H29A H 0.3513 0.7711 0.3425 0.033 Uiso 1 1 calc R . . C30 C 0.32599(11) 0.76739(11) 0.49870(10) 0.0186(2) Uani 1 1 d . . . C31 C 0.32806(13) 0.89397(12) 0.47634(11) 0.0266(3) Uani 1 1 d . . . H31A H 0.3309 0.9048 0.5461 0.032 Uiso 1 1 calc R . . C32 C 0.22165(14) 0.96511(14) 0.43508(16) 0.0379(4) Uani 1 1 d . . . H32A H 0.1563 0.9361 0.4856 0.057 Uiso 1 1 calc R . . H32B H 0.2186 0.9599 0.3645 0.057 Uiso 1 1 calc R . . H32C H 0.2218 1.0450 0.4287 0.057 Uiso 1 1 calc R . . C33 C 0.43055(17) 0.93820(18) 0.3985(2) 0.0595(7) Uani 1 1 d . . . H33A H 0.4982 0.8906 0.4244 0.089 Uiso 1 1 calc R . . H33B H 0.4325 1.0172 0.3937 0.089 Uiso 1 1 calc R . . H33C H 0.4268 0.9351 0.3273 0.089 Uiso 1 1 calc R . . C34 C 0.28879(13) 0.49375(11) 0.74179(12) 0.0233(3) Uani 1 1 d . . . H34A H 0.2630 0.5416 0.7901 0.028 Uiso 1 1 calc R . . C35 C 0.39986(16) 0.42327(17) 0.77187(16) 0.0443(5) Uani 1 1 d . . . H35A H 0.4548 0.4746 0.7614 0.066 Uiso 1 1 calc R . . H35B H 0.4271 0.3748 0.7262 0.066 Uiso 1 1 calc R . . H35C H 0.3889 0.3753 0.8473 0.066 Uiso 1 1 calc R . . C36 C 0.20048(15) 0.41558(13) 0.76237(15) 0.0353(4) Uani 1 1 d . . . H36A H 0.1297 0.4618 0.7435 0.053 Uiso 1 1 calc R . . H36B H 0.1901 0.3696 0.8385 0.053 Uiso 1 1 calc R . . H36C H 0.2249 0.3651 0.7183 0.053 Uiso 1 1 calc R . . C37 C -0.00655(12) 0.86636(13) 0.79894(14) 0.0273(3) Uani 1 1 d . . . H37A H -0.0235 0.9466 0.8008 0.033 Uiso 1 1 calc R . . C38 C 0.00890(11) 0.83232(14) 0.70615(12) 0.0267(3) Uani 1 1 d . . . H38A H 0.0055 0.8845 0.6309 0.032 Uiso 1 1 calc R . . C39 C 0.02444(11) 0.71203(13) 0.73905(13) 0.0262(3) Uani 1 1 d . . . H39A H 0.0345 0.6642 0.6911 0.031 Uiso 1 1 calc R . . C40 C 0.02075(12) 0.67070(13) 0.85178(13) 0.0266(3) Uani 1 1 d . . . H40A H 0.0262 0.5887 0.8977 0.032 Uiso 1 1 calc R . . C41 C -0.00050(11) 0.76628(14) 0.88908(12) 0.0272(3) Uani 1 1 d . . . H41A H -0.0121 0.7634 0.9659 0.033 Uiso 1 1 calc R . . C1S C 0.00545(17) 0.77030(16) 0.43256(15) 0.0397(4) Uani 1 1 d . . . H1SA H -0.0032 0.8354 0.3671 0.060 Uiso 1 1 calc R . . H1SB H 0.0807 0.7616 0.4502 0.060 Uiso 1 1 calc R . . H1SC H -0.0501 0.7834 0.4920 0.060 Uiso 1 1 calc R . . C2S C -0.01158(15) 0.66213(14) 0.41437(12) 0.0320(3) Uani 1 1 d . . . H2SA H 0.0408 0.6530 0.3505 0.038 Uiso 1 1 calc R . . H2SB H -0.0885 0.6708 0.3987 0.038 Uiso 1 1 calc R . . C3S C 0.00636(13) 0.55448(14) 0.50974(12) 0.0277(3) Uani 1 1 d . . . H3SA H -0.0480 0.5624 0.5729 0.033 Uiso 1 1 calc R . . H3SB H 0.0822 0.5474 0.5272 0.033 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 0.00921(8) 0.01657(8) 0.01612(8) -0.00789(6) -0.00127(6) -0.00200(5) N1 0.0130(5) 0.0149(5) 0.0137(5) -0.0067(4) -0.0007(4) -0.0029(4) C1 0.0129(5) 0.0120(5) 0.0139(5) -0.0048(4) -0.0018(4) -0.0029(4) N2 0.0123(5) 0.0128(4) 0.0133(5) -0.0060(4) -0.0012(4) -0.0022(4) C2 0.0110(5) 0.0122(5) 0.0131(5) -0.0046(4) -0.0005(4) -0.0018(4) C3 0.0116(5) 0.0128(5) 0.0164(5) -0.0041(4) -0.0017(4) -0.0026(4) C4 0.0124(6) 0.0120(5) 0.0157(5) -0.0025(4) -0.0022(4) -0.0031(4) C5 0.0125(5) 0.0141(5) 0.0161(5) -0.0043(4) -0.0019(4) -0.0040(4) C7 0.0204(7) 0.0312(7) 0.0238(7) -0.0094(6) -0.0070(5) -0.0097(5) C6 0.0178(6) 0.0244(6) 0.0187(6) -0.0087(5) -0.0024(5) -0.0063(5) C8 0.0128(6) 0.0255(7) 0.0260(7) -0.0053(5) -0.0057(5) -0.0069(5) C9 0.0131(6) 0.0151(5) 0.0190(6) -0.0018(4) -0.0030(5) -0.0039(4) C10 0.0103(6) 0.0215(6) 0.0258(7) -0.0053(5) 0.0000(5) -0.0023(5) C11 0.0130(6) 0.0245(6) 0.0239(6) -0.0105(5) 0.0023(5) -0.0004(5) C12 0.0144(6) 0.0197(6) 0.0203(6) -0.0090(5) -0.0015(5) -0.0012(5) C13 0.0100(5) 0.0175(5) 0.0143(5) -0.0078(4) -0.0005(4) -0.0030(4) C14 0.0138(6) 0.0194(6) 0.0179(6) -0.0057(5) -0.0029(5) -0.0028(4) C15 0.0213(7) 0.0295(7) 0.0139(6) -0.0049(5) -0.0029(5) -0.0027(5) C16 0.0237(7) 0.0337(7) 0.0184(6) -0.0152(6) -0.0025(5) -0.0024(6) C17 0.0222(7) 0.0230(6) 0.0221(6) -0.0137(5) -0.0012(5) -0.0033(5) C18 0.0160(6) 0.0171(6) 0.0170(6) -0.0073(5) -0.0002(5) -0.0049(4) C19 0.0357(8) 0.0144(6) 0.0190(6) -0.0059(5) -0.0021(6) -0.0039(5) C20 0.0363(9) 0.0269(8) 0.0392(9) 0.0015(7) 0.0164(7) -0.0012(7) C21 0.0272(8) 0.0215(7) 0.0346(8) -0.0013(6) -0.0037(6) -0.0032(6) C22 0.0298(7) 0.0158(6) 0.0214(6) -0.0020(5) -0.0065(6) -0.0029(5) C23 0.0241(8) 0.0216(7) 0.0466(10) -0.0002(6) 0.0019(7) 0.0001(6) C24 0.0265(8) 0.0225(7) 0.0562(11) -0.0012(7) -0.0097(8) -0.0076(6) C25 0.0105(5) 0.0181(6) 0.0154(5) -0.0087(4) -0.0024(4) -0.0008(4) C26 0.0184(6) 0.0181(6) 0.0214(6) -0.0097(5) -0.0053(5) -0.0006(5) C27 0.0312(8) 0.0246(7) 0.0324(8) -0.0190(6) -0.0100(6) 0.0033(6) C28 0.0343(8) 0.0423(9) 0.0252(7) -0.0239(7) -0.0079(6) 0.0065(7) C29 0.0265(7) 0.0398(8) 0.0147(6) -0.0104(6) -0.0028(5) 0.0005(6) C30 0.0159(6) 0.0233(6) 0.0156(6) -0.0054(5) -0.0019(5) -0.0025(5) C31 0.0342(8) 0.0232(7) 0.0195(6) 0.0010(5) -0.0055(6) -0.0106(6) C32 0.0278(8) 0.0241(7) 0.0566(11) -0.0106(7) -0.0001(8) -0.0023(6) C33 0.0286(10) 0.0382(10) 0.0817(16) 0.0183(10) -0.0038(10) -0.0094(8) C34 0.0293(7) 0.0160(6) 0.0253(7) -0.0054(5) -0.0053(6) -0.0059(5) C35 0.0349(10) 0.0440(10) 0.0424(10) 0.0097(8) -0.0179(8) -0.0093(8) C36 0.0351(9) 0.0238(7) 0.0464(10) -0.0063(7) -0.0075(7) -0.0107(6) C37 0.0131(6) 0.0282(7) 0.0457(9) -0.0204(7) -0.0030(6) 0.0002(5) C38 0.0128(6) 0.0380(8) 0.0263(7) -0.0068(6) -0.0055(5) -0.0002(5) C39 0.0135(6) 0.0375(8) 0.0378(8) -0.0245(7) -0.0047(6) -0.0032(5) C40 0.0136(6) 0.0281(7) 0.0362(8) -0.0061(6) -0.0018(6) -0.0081(5) C41 0.0117(6) 0.0481(9) 0.0258(7) -0.0179(6) 0.0015(5) -0.0060(6) C1S 0.0438(10) 0.0430(10) 0.0341(9) -0.0133(7) 0.0002(8) -0.0147(8) C2S 0.0338(9) 0.0397(9) 0.0228(7) -0.0106(6) 0.0007(6) -0.0099(7) C3S 0.0223(7) 0.0399(8) 0.0229(7) -0.0117(6) -0.0026(6) -0.0062(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N2 1.9506(10) . ? Ni1 N1 1.9528(10) . ? Ni1 C40 2.1609(14) . ? Ni1 C37 2.1675(14) . ? Ni1 C41 2.1688(14) . ? Ni1 C38 2.1757(14) . ? Ni1 C39 2.1847(13) . ? N1 C1 1.3125(16) . ? N1 C13 1.4360(15) . ? C1 C2 1.4491(16) . ? C1 C5 1.4694(16) . ? N2 C2 1.3141(15) . ? N2 C25 1.4371(14) . ? C2 C3 1.4690(16) . ? C3 C12 1.3784(17) . ? C3 C4 1.4290(16) . ? C4 C9 1.3945(17) . ? C4 C5 1.4270(17) . ? C5 C6 1.3822(17) . ? C7 C8 1.373(2) . ? C7 C6 1.4202(19) . ? C7 H7A 0.9500 . ? C6 H6A 0.9500 . ? C8 C9 1.4286(18) . ? C8 H8A 0.9500 . ? C9 C10 1.4214(19) . ? C10 C11 1.3788(19) . ? C10 H10A 0.9500 . ? C11 C12 1.4211(18) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C14 1.4065(17) . ? C13 C18 1.4090(17) . ? C14 C15 1.3973(18) . ? C14 C22 1.5235(18) . ? C15 C16 1.389(2) . ? C15 H15A 0.9500 . ? C16 C17 1.387(2) . ? C16 H16A 0.9500 . ? C17 C18 1.3967(17) . ? C17 H17A 0.9500 . ? C18 C19 1.5215(18) . ? C19 C20 1.524(2) . ? C19 C21 1.533(2) . ? C19 H19A 1.0000 . ? 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 C24 1.528(2) . ? C22 C23 1.530(2) . ? C22 H22A 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C30 1.4079(17) . ? C25 C26 1.4086(17) . ? C26 C27 1.3973(18) . ? C26 C34 1.5216(19) . ? C27 C28 1.385(2) . ? C27 H27A 0.9500 . ? C28 C29 1.389(2) . ? C28 H28A 0.9500 . ? C29 C30 1.3991(19) . ? C29 H29A 0.9500 . ? C30 C31 1.5212(19) . ? C31 C33 1.525(2) . ? C31 C32 1.528(2) . ? C31 H31A 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C36 1.525(2) . ? C34 C35 1.530(2) . ? C34 H34A 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C41 1.415(2) . ? C37 C38 1.419(2) . ? C37 H37A 1.0000 . ? C38 C39 1.410(2) . ? C38 H38A 1.0000 . ? C39 C40 1.413(2) . ? C39 H39A 1.0000 . ? C40 C41 1.419(2) . ? C40 H40A 1.0000 . ? C41 H41A 1.0000 . ? C1S C2S 1.523(2) . ? C1S H1SA 0.9800 . ? C1S H1SB 0.9800 . ? C1S H1SC 0.9800 . ? C2S C3S 1.524(2) . ? C2S H2SA 0.9900 . ? C2S H2SB 0.9900 . ? C3S C3S 1.525(3) 2_566 ? C3S H3SA 0.9900 . ? C3S H3SB 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 N2 Ni1 N1 83.13(4) . . ? N2 Ni1 C40 127.00(5) . . ? N1 Ni1 C40 127.02(5) . . ? N2 Ni1 C37 150.07(5) . . ? N1 Ni1 C37 113.24(5) . . ? C40 Ni1 C37 64.01(6) . . ? N2 Ni1 C41 164.95(5) . . ? N1 Ni1 C41 104.48(5) . . ? C40 Ni1 C41 38.27(6) . . ? C37 Ni1 C41 38.09(6) . . ? N2 Ni1 C38 116.45(5) . . ? N1 Ni1 C38 147.15(5) . . ? C40 Ni1 C38 63.65(6) . . ? C37 Ni1 C38 38.14(6) . . ? C41 Ni1 C38 63.56(6) . . ? N2 Ni1 C39 106.69(5) . . ? N1 Ni1 C39 164.96(5) . . ? C40 Ni1 C39 37.94(6) . . ? C37 Ni1 C39 63.53(5) . . ? C41 Ni1 C39 63.43(6) . . ? C38 Ni1 C39 37.73(6) . . ? C1 N1 C13 117.77(10) . . ? C1 N1 Ni1 112.72(8) . . ? C13 N1 Ni1 129.25(8) . . ? N1 C1 C2 115.69(10) . . ? N1 C1 C5 135.95(11) . . ? C2 C1 C5 108.35(10) . . ? C2 N2 C25 118.44(10) . . ? C2 N2 Ni1 112.67(8) . . ? C25 N2 Ni1 128.81(8) . . ? N2 C2 C1 115.78(11) . . ? N2 C2 C3 135.74(11) . . ? C1 C2 C3 108.46(10) . . ? C12 C3 C4 118.64(11) . . ? C12 C3 C2 136.17(11) . . ? C4 C3 C2 105.20(10) . . ? C9 C4 C5 123.81(11) . . ? C9 C4 C3 123.52(12) . . ? C5 C4 C3 112.67(11) . . ? C6 C5 C4 118.46(11) . . ? C6 C5 C1 136.23(12) . . ? C4 C5 C1 105.31(10) . . ? C8 C7 C6 123.02(12) . . ? C8 C7 H7A 118.5 . . ? C6 C7 H7A 118.5 . . ? C5 C6 C7 118.32(12) . . ? C5 C6 H6A 120.8 . . ? C7 C6 H6A 120.8 . . ? C7 C8 C9 120.00(12) . . ? C7 C8 H8A 120.0 . . ? C9 C8 H8A 120.0 . . ? C4 C9 C10 116.54(11) . . ? C4 C9 C8 116.39(12) . . ? C10 C9 C8 127.07(12) . . ? C11 C10 C9 120.30(12) . . ? C11 C10 H10A 119.8 . . ? C9 C10 H10A 119.8 . . ? C10 C11 C12 122.53(12) . . ? C10 C11 H11A 118.7 . . ? C12 C11 H11A 118.7 . . ? C3 C12 C11 118.47(12) . . ? C3 C12 H12A 120.8 . . ? C11 C12 H12A 120.8 . . ? C14 C13 C18 122.08(11) . . ? C14 C13 N1 118.73(11) . . ? C18 C13 N1 119.20(11) . . ? C15 C14 C13 117.75(12) . . ? C15 C14 C22 120.80(12) . . ? C13 C14 C22 121.44(11) . . ? C16 C15 C14 120.93(12) . . ? C16 C15 H15A 119.5 . . ? C14 C15 H15A 119.5 . . ? C17 C16 C15 120.28(12) . . ? C17 C16 H16A 119.9 . . ? C15 C16 H16A 119.9 . . ? C16 C17 C18 121.04(12) . . ? C16 C17 H17A 119.5 . . ? C18 C17 H17A 119.5 . . ? C17 C18 C13 117.65(11) . . ? C17 C18 C19 121.38(11) . . ? C13 C18 C19 120.96(11) . . ? C18 C19 C20 111.51(13) . . ? C18 C19 C21 112.05(12) . . ? C20 C19 C21 110.82(12) . . ? C18 C19 H19A 107.4 . . ? C20 C19 H19A 107.4 . . ? C21 C19 H19A 107.4 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C14 C22 C24 111.52(13) . . ? C14 C22 C23 111.80(12) . . ? C24 C22 C23 110.55(12) . . ? C14 C22 H22A 107.6 . . ? C24 C22 H22A 107.6 . . ? C23 C22 H22A 107.6 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C30 C25 C26 122.48(11) . . ? C30 C25 N2 119.66(11) . . ? C26 C25 N2 117.85(11) . . ? C27 C26 C25 117.52(12) . . ? C27 C26 C34 121.02(12) . . ? C25 C26 C34 121.41(11) . . ? C28 C27 C26 121.19(13) . . ? C28 C27 H27A 119.4 . . ? C26 C27 H27A 119.4 . . ? C27 C28 C29 120.25(13) . . ? C27 C28 H28A 119.9 . . ? C29 C28 H28A 119.9 . . ? C28 C29 C30 121.17(13) . . ? C28 C29 H29A 119.4 . . ? C30 C29 H29A 119.4 . . ? C29 C30 C25 117.37(12) . . ? C29 C30 C31 121.10(12) . . ? C25 C30 C31 121.53(11) . . ? C30 C31 C33 112.85(15) . . ? C30 C31 C32 111.39(12) . . ? C33 C31 C32 110.04(13) . . ? C30 C31 H31A 107.4 . . ? C33 C31 H31A 107.4 . . ? C32 C31 H31A 107.4 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C26 C34 C36 113.14(12) . . ? C26 C34 C35 110.60(13) . . ? C36 C34 C35 110.36(13) . . ? C26 C34 H34A 107.5 . . ? C36 C34 H34A 107.5 . . ? C35 C34 H34A 107.5 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C41 C37 C38 107.69(13) . . ? C41 C37 Ni1 71.01(8) . . ? C38 C37 Ni1 71.24(8) . . ? C41 C37 H37A 126.1 . . ? C38 C37 H37A 126.1 . . ? Ni1 C37 H37A 126.1 . . ? C39 C38 C37 108.16(13) . . ? C39 C38 Ni1 71.48(8) . . ? C37 C38 Ni1 70.61(8) . . ? C39 C38 H38A 125.9 . . ? C37 C38 H38A 125.9 . . ? Ni1 C38 H38A 125.9 . . ? C38 C39 C40 108.21(13) . . ? C38 C39 Ni1 70.79(8) . . ? C40 C39 Ni1 70.12(8) . . ? C38 C39 H39A 125.9 . . ? C40 C39 H39A 125.9 . . ? Ni1 C39 H39A 125.9 . . ? C39 C40 C41 107.82(13) . . ? C39 C40 Ni1 71.94(8) . . ? C41 C40 Ni1 71.17(8) . . ? C39 C40 H40A 126.0 . . ? C41 C40 H40A 126.0 . . ? Ni1 C40 H40A 126.0 . . ? C37 C41 C40 108.09(13) . . ? C37 C41 Ni1 70.90(8) . . ? C40 C41 Ni1 70.56(8) . . ? C37 C41 H41A 125.9 . . ? C40 C41 H41A 125.9 . . ? Ni1 C41 H41A 125.9 . . ? C2S C1S H1SA 109.5 . . ? C2S C1S H1SB 109.5 . . ? H1SA C1S H1SB 109.5 . . ? C2S C1S H1SC 109.5 . . ? H1SA C1S H1SC 109.5 . . ? H1SB C1S H1SC 109.5 . . ? C1S C2S C3S 113.63(13) . . ? C1S C2S H2SA 108.8 . . ? C3S C2S H2SA 108.8 . . ? C1S C2S H2SB 108.8 . . ? C3S C2S H2SB 108.8 . . ? H2SA C2S H2SB 107.7 . . ? C2S C3S C3S 113.77(15) . 2_566 ? C2S C3S H3SA 108.8 . . ? C3S C3S H3SA 108.8 2_566 . ? C2S C3S H3SB 108.8 . . ? C3S C3S H3SB 108.8 2_566 . ? H3SA C3S H3SB 107.7 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.456 _refine_diff_density_min -0.512 _refine_diff_density_rms 0.054 _publ_section_references ; Bruker, Programs APEX II, version 2.0-1; SAINT, version 7.23A; SADABS, version 2004/1; XPREP, version 2005/2; SHELXTL, version 6.1. Bruker AXS Inc., Madison, WI, USA, 2005. G.M. Sheldrick, Programs SHELXS97 (crystal structure solution) and SHELXL97 (crystal structure refinement), University of Gottingen, Germany, 1997. ; # Attachment 'compound_6.cif' data_nibianm _database_code_depnum_ccdc_archive 'CCDC 719956' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H48 N2 Ni P2 Si2' _chemical_formula_weight 781.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.7917(5) _cell_length_b 14.5028(4) _cell_length_c 17.5770(5) _cell_angle_alpha 90.00 _cell_angle_beta 118.5790(10) _cell_angle_gamma 90.00 _cell_volume 3982.78(19) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _exptl_crystal_description stick _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.304 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 0.661 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8791 _exptl_absorpt_correction_T_max 0.9677 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1998a)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31225 _diffrn_reflns_av_R_equivalents 0.0633 _diffrn_reflns_av_sigmaI/netI 0.0514 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7005 _reflns_number_gt 5356 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0543P)^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 7005 _refine_ls_number_parameters 466 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0684 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1031 _refine_ls_wR_factor_gt 0.0956 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 0.244145(14) 0.170216(17) 0.124940(14) 0.01819(6) Uani 1 1 d . . . Si1 Si 0.36765(3) 0.07815(4) 0.04828(3) 0.02172(14) Uani 1 1 d . . . Si2 Si 0.08176(3) 0.07125(4) -0.10262(3) 0.02542(15) Uani 1 1 d . . . P1 P 0.17397(3) 0.26050(4) 0.16720(3) 0.01935(12) Uani 1 1 d . . . P2 P 0.29244(3) 0.09376(4) 0.24657(3) 0.01937(12) Uani 1 1 d . . . N1 N 0.28295(9) 0.13659(11) 0.04527(9) 0.0209(4) Uani 1 1 d . . . N2 N 0.09722(10) 0.18944(12) -0.09581(10) 0.0237(4) Uani 1 1 d . . . C1 C 0.24915(11) 0.22298(13) 0.02322(11) 0.0187(5) Uani 1 1 d . . . C2 C 0.15921(11) 0.24250(14) -0.04733(11) 0.0202(5) Uani 1 1 d . . . C3 C 0.15272(12) 0.34509(14) -0.05508(11) 0.0218(5) Uani 1 1 d . . . C4 C 0.23385(11) 0.38210(14) -0.00175(11) 0.0211(5) Uani 1 1 d . . . C5 C 0.29544(11) 0.31329(13) 0.04385(11) 0.0205(5) Uani 1 1 d . . . C6 C 0.37870(12) 0.33943(14) 0.09370(12) 0.0247(5) Uani 1 1 d . . . H6A H 0.4220 0.2948 0.1238 0.030 Uiso 1 1 calc R . . C7 C 0.39948(13) 0.43509(15) 0.09972(13) 0.0318(6) Uani 1 1 d . . . H7A H 0.4574 0.4533 0.1346 0.038 Uiso 1 1 calc R . . C8 C 0.33920(13) 0.50156(15) 0.05723(13) 0.0310(5) Uani 1 1 d . . . H8A H 0.3555 0.5646 0.0637 0.037 Uiso 1 1 calc R . . C9 C 0.25249(12) 0.47658(14) 0.00359(12) 0.0257(5) Uani 1 1 d . . . C10 C 0.18204(13) 0.53475(15) -0.04750(12) 0.0309(5) Uani 1 1 d . . . H10A H 0.1902 0.5996 -0.0457 0.037 Uiso 1 1 calc R . . C11 C 0.10258(13) 0.49882(15) -0.09920(12) 0.0317(6) Uani 1 1 d . . . H11A H 0.0568 0.5397 -0.1325 0.038 Uiso 1 1 calc R . . C12 C 0.08597(12) 0.40336(15) -0.10498(12) 0.0274(5) Uani 1 1 d . . . H12A H 0.0304 0.3799 -0.1422 0.033 Uiso 1 1 calc R . . C13 C 0.34036(14) -0.04747(14) 0.03083(13) 0.0317(6) Uani 1 1 d . . . H13A H 0.2916 -0.0566 -0.0270 0.048 Uiso 1 1 calc R . . H13B H 0.3254 -0.0694 0.0746 0.048 Uiso 1 1 calc R . . H13C H 0.3898 -0.0822 0.0358 0.048 Uiso 1 1 calc R . . C14 C 0.47220(12) 0.08769(16) 0.14994(13) 0.0308(6) Uani 1 1 d . . . H14A H 0.4950 0.1502 0.1549 0.046 Uiso 1 1 calc R . . H14B H 0.5128 0.0431 0.1483 0.046 Uiso 1 1 calc R . . H14C H 0.4637 0.0747 0.2000 0.046 Uiso 1 1 calc R . . C15 C 0.38729(13) 0.11820(16) -0.04140(13) 0.0330(6) Uani 1 1 d . . . H15A H 0.3981 0.1848 -0.0361 0.050 Uiso 1 1 calc R . . H15B H 0.3370 0.1049 -0.0972 0.050 Uiso 1 1 calc R . . H15C H 0.4372 0.0860 -0.0381 0.050 Uiso 1 1 calc R . . C16 C -0.03633(13) 0.05693(17) -0.17068(14) 0.0383(6) Uani 1 1 d . . . H16A H -0.0554 0.0888 -0.2261 0.057 Uiso 1 1 calc R . . H16B H -0.0654 0.0833 -0.1404 0.057 Uiso 1 1 calc R . . H16C H -0.0502 -0.0088 -0.1813 0.057 Uiso 1 1 calc R . . C17 C 0.11154(13) 0.01447(15) 0.00329(12) 0.0290(5) Uani 1 1 d . . . H17A H 0.1706 -0.0079 0.0288 0.044 Uiso 1 1 calc R . . H17B H 0.0730 -0.0376 -0.0059 0.044 Uiso 1 1 calc R . . H17C H 0.1067 0.0591 0.0426 0.044 Uiso 1 1 calc R . . C18 C 0.13307(13) 0.01968(15) -0.16354(12) 0.0325(6) Uani 1 1 d . . . H18A H 0.1941 0.0352 -0.1345 0.049 Uiso 1 1 calc R . . H18B H 0.1058 0.0442 -0.2227 0.049 Uiso 1 1 calc R . . H18C H 0.1263 -0.0475 -0.1655 0.049 Uiso 1 1 calc R . . C19 C 0.18490(11) 0.38603(14) 0.16427(11) 0.0198(5) Uani 1 1 d . . . C20 C 0.26596(12) 0.42435(14) 0.21005(12) 0.0246(5) Uani 1 1 d . . . H20A H 0.3141 0.3855 0.2411 0.030 Uiso 1 1 calc R . . C21 C 0.27708(13) 0.51877(15) 0.21080(12) 0.0283(6) Uani 1 1 d . . . H21A H 0.3326 0.5445 0.2438 0.034 Uiso 1 1 calc R . . C22 C 0.20800(13) 0.57573(15) 0.16386(12) 0.0284(6) Uani 1 1 d . . . H22A H 0.2158 0.6406 0.1649 0.034 Uiso 1 1 calc R . . C23 C 0.12707(13) 0.53799(14) 0.11516(12) 0.0274(5) Uani 1 1 d . . . H23A H 0.0796 0.5770 0.0818 0.033 Uiso 1 1 calc R . . C24 C 0.11540(12) 0.44346(14) 0.11516(12) 0.0231(5) Uani 1 1 d . . . H24A H 0.0600 0.4178 0.0817 0.028 Uiso 1 1 calc R . . C25 C 0.05799(12) 0.24449(13) 0.12239(12) 0.0220(5) Uani 1 1 d . . . C26 C 0.00718(12) 0.23684(14) 0.03275(13) 0.0265(5) Uani 1 1 d . . . H26A H 0.0332 0.2378 -0.0034 0.032 Uiso 1 1 calc R . . C27 C -0.08035(13) 0.22792(14) -0.00378(14) 0.0302(6) Uani 1 1 d . . . H27A H -0.1143 0.2237 -0.0649 0.036 Uiso 1 1 calc R . . C28 C -0.11897(13) 0.22501(14) 0.04858(14) 0.0319(6) Uani 1 1 d . . . H28A H -0.1793 0.2181 0.0233 0.038 Uiso 1 1 calc R . . C29 C -0.06997(13) 0.23211(15) 0.13688(14) 0.0327(6) Uani 1 1 d . . . H29A H -0.0965 0.2298 0.1726 0.039 Uiso 1 1 calc R . . C30 C 0.01838(12) 0.24259(14) 0.17441(13) 0.0278(5) Uani 1 1 d . . . H30A H 0.0518 0.2485 0.2355 0.033 Uiso 1 1 calc R . . C31 C 0.21730(12) 0.23637(14) 0.28356(11) 0.0224(5) Uani 1 1 d . . . H31A H 0.2732 0.2674 0.3171 0.027 Uiso 1 1 calc R . . H31B H 0.1777 0.2597 0.3038 0.027 Uiso 1 1 calc R . . C32 C 0.22793(11) 0.13294(14) 0.29656(12) 0.0225(5) Uani 1 1 d . . . H32A H 0.1713 0.1023 0.2688 0.027 Uiso 1 1 calc R . . H32B H 0.2572 0.1179 0.3591 0.027 Uiso 1 1 calc R . . C33 C 0.30397(11) -0.03066(13) 0.26741(11) 0.0201(5) Uani 1 1 d . . . C34 C 0.25896(13) -0.07793(15) 0.30129(13) 0.0288(6) Uani 1 1 d . . . H34A H 0.2201 -0.0455 0.3142 0.035 Uiso 1 1 calc R . . C35 C 0.27017(13) -0.17252(15) 0.31656(14) 0.0331(6) Uani 1 1 d . . . H35A H 0.2389 -0.2040 0.3398 0.040 Uiso 1 1 calc R . . C36 C 0.32648(13) -0.22088(14) 0.29810(13) 0.0293(6) Uani 1 1 d . . . H36A H 0.3342 -0.2853 0.3086 0.035 Uiso 1 1 calc R . . C37 C 0.37102(14) -0.17426(15) 0.26435(13) 0.0334(6) Uani 1 1 d . . . H37A H 0.4101 -0.2068 0.2518 0.040 Uiso 1 1 calc R . . C38 C 0.35968(13) -0.08081(15) 0.24842(12) 0.0305(6) Uani 1 1 d . . . H38A H 0.3904 -0.0501 0.2241 0.037 Uiso 1 1 calc R . . C39 C 0.39717(11) 0.13740(14) 0.32839(11) 0.0200(5) Uani 1 1 d . . . C40 C 0.43532(12) 0.20939(14) 0.30721(12) 0.0248(5) Uani 1 1 d . . . H40A H 0.4095 0.2317 0.2494 0.030 Uiso 1 1 calc R . . C41 C 0.51020(12) 0.24886(15) 0.36910(12) 0.0272(5) Uani 1 1 d . . . H41A H 0.5355 0.2980 0.3536 0.033 Uiso 1 1 calc R . . C42 C 0.54886(12) 0.21729(14) 0.45383(12) 0.0270(6) Uani 1 1 d . . . H42A H 0.6003 0.2448 0.4965 0.032 Uiso 1 1 calc R . . C43 C 0.51165(12) 0.14503(14) 0.47583(13) 0.0267(6) Uani 1 1 d . . . H43A H 0.5378 0.1228 0.5337 0.032 Uiso 1 1 calc R . . C44 C 0.43658(12) 0.10548(14) 0.41349(12) 0.0235(5) Uani 1 1 d . . . H44A H 0.4116 0.0559 0.4289 0.028 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 0.01950(10) 0.01938(13) 0.01710(10) 0.00041(10) 0.00988(8) 0.00084(10) Si1 0.0227(2) 0.0229(3) 0.0217(2) 0.0019(2) 0.01235(19) 0.0033(2) Si2 0.0259(3) 0.0285(3) 0.0220(2) -0.0033(2) 0.0117(2) -0.0063(2) P1 0.0200(2) 0.0200(3) 0.0193(2) 0.00057(19) 0.01044(17) 0.0011(2) P2 0.0195(2) 0.0207(3) 0.0190(2) 0.0002(2) 0.01010(17) 0.0003(2) N1 0.0256(7) 0.0210(9) 0.0200(7) 0.0013(6) 0.0140(6) -0.0001(7) N2 0.0233(7) 0.0287(10) 0.0203(7) 0.0015(7) 0.0115(6) 0.0004(7) C1 0.0211(8) 0.0238(11) 0.0159(8) -0.0004(7) 0.0126(6) -0.0008(8) C2 0.0235(8) 0.0272(11) 0.0173(7) 0.0019(7) 0.0156(6) 0.0009(8) C3 0.0285(9) 0.0229(11) 0.0195(8) 0.0008(8) 0.0159(7) 0.0010(8) C4 0.0272(9) 0.0236(11) 0.0170(8) 0.0041(7) 0.0142(7) 0.0022(8) C5 0.0257(8) 0.0221(11) 0.0192(8) -0.0004(7) 0.0150(7) 0.0006(8) C6 0.0244(9) 0.0268(11) 0.0267(9) 0.0029(8) 0.0153(7) 0.0020(9) C7 0.0323(10) 0.0320(12) 0.0371(10) -0.0066(9) 0.0214(8) -0.0092(9) C8 0.0446(10) 0.0199(11) 0.0389(10) -0.0043(9) 0.0284(8) -0.0080(9) C9 0.0339(9) 0.0230(11) 0.0275(9) 0.0010(8) 0.0205(7) 0.0011(9) C10 0.0476(10) 0.0236(11) 0.0340(9) 0.0057(8) 0.0295(8) 0.0057(9) C11 0.0392(10) 0.0316(12) 0.0300(9) 0.0108(9) 0.0212(8) 0.0148(9) C12 0.0262(9) 0.0359(12) 0.0233(9) 0.0052(9) 0.0143(7) 0.0046(9) C13 0.0362(10) 0.0256(11) 0.0310(10) 0.0025(9) 0.0141(9) 0.0081(10) C14 0.0250(9) 0.0344(13) 0.0318(10) 0.0019(9) 0.0127(8) 0.0070(9) C15 0.0344(10) 0.0386(13) 0.0354(10) 0.0071(9) 0.0242(8) 0.0071(10) C16 0.0349(11) 0.0487(15) 0.0296(10) -0.0064(10) 0.0141(9) -0.0132(11) C17 0.0331(10) 0.0266(12) 0.0306(9) -0.0035(9) 0.0178(8) -0.0082(9) C18 0.0423(10) 0.0306(12) 0.0297(9) -0.0046(9) 0.0212(8) -0.0070(10) C19 0.0236(8) 0.0227(11) 0.0171(8) -0.0001(7) 0.0130(7) 0.0014(8) C20 0.0237(9) 0.0272(11) 0.0221(9) 0.0004(8) 0.0102(7) 0.0041(9) C21 0.0261(9) 0.0311(12) 0.0264(9) -0.0023(9) 0.0116(8) -0.0050(9) C22 0.0345(10) 0.0200(11) 0.0289(10) -0.0030(8) 0.0136(8) -0.0028(9) C23 0.0313(10) 0.0252(11) 0.0262(9) 0.0043(8) 0.0143(8) 0.0073(9) C24 0.0253(9) 0.0238(11) 0.0222(8) -0.0018(8) 0.0129(7) -0.0004(8) C25 0.0224(8) 0.0170(10) 0.0292(9) 0.0010(8) 0.0143(7) -0.0002(8) C26 0.0257(9) 0.0224(11) 0.0354(10) -0.0002(8) 0.0179(8) 0.0003(8) C27 0.0242(10) 0.0212(11) 0.0363(11) -0.0007(9) 0.0074(9) 0.0018(9) C28 0.0219(9) 0.0197(11) 0.0551(12) -0.0010(10) 0.0193(9) -0.0002(9) C29 0.0316(10) 0.0256(12) 0.0483(11) 0.0043(9) 0.0251(9) 0.0019(9) C30 0.0285(9) 0.0247(11) 0.0344(10) -0.0001(9) 0.0185(8) -0.0007(9) C31 0.0209(9) 0.0258(11) 0.0213(8) -0.0013(8) 0.0109(7) 0.0023(8) C32 0.0204(9) 0.0291(11) 0.0190(8) 0.0028(8) 0.0103(7) 0.0016(8) C33 0.0219(9) 0.0211(10) 0.0150(8) -0.0016(7) 0.0068(7) -0.0031(8) C34 0.0248(9) 0.0250(11) 0.0376(10) 0.0032(9) 0.0157(8) -0.0006(9) C35 0.0293(10) 0.0254(12) 0.0401(11) 0.0018(10) 0.0131(9) -0.0090(9) C36 0.0372(11) 0.0158(11) 0.0273(10) -0.0005(8) 0.0094(9) -0.0024(9) C37 0.0423(11) 0.0266(12) 0.0350(10) 0.0008(9) 0.0216(9) 0.0095(10) C38 0.0380(10) 0.0335(12) 0.0259(9) 0.0042(9) 0.0202(8) 0.0025(10) C39 0.0183(8) 0.0224(10) 0.0201(8) -0.0022(8) 0.0098(7) 0.0011(8) C40 0.0254(9) 0.0254(11) 0.0259(9) 0.0018(8) 0.0142(7) 0.0010(9) C41 0.0282(9) 0.0281(11) 0.0337(9) -0.0032(9) 0.0216(7) -0.0052(9) C42 0.0216(9) 0.0281(12) 0.0272(10) -0.0065(9) 0.0084(8) -0.0022(9) C43 0.0276(10) 0.0265(11) 0.0213(9) -0.0008(8) 0.0080(8) 0.0055(9) C44 0.0225(9) 0.0226(11) 0.0248(9) 0.0022(8) 0.0107(7) -0.0007(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 1.8976(17) . ? Ni1 C1 1.9856(19) . ? Ni1 P1 2.1708(6) . ? Ni1 P2 2.1865(5) . ? Si1 N1 1.7076(17) . ? Si1 C15 1.863(2) . ? Si1 C14 1.8687(19) . ? Si1 C13 1.873(2) . ? Si2 N2 1.7311(18) . ? Si2 C18 1.864(2) . ? Si2 C17 1.866(2) . ? Si2 C16 1.867(2) . ? P1 C19 1.834(2) . ? P1 C25 1.8377(19) . ? P1 C31 1.8415(19) . ? P2 C33 1.833(2) . ? P2 C39 1.8377(17) . ? P2 C32 1.838(2) . ? N1 C1 1.363(2) . ? N2 C2 1.279(2) . ? C1 C5 1.496(3) . ? C1 C2 1.510(2) . ? C2 C3 1.493(3) . ? C3 C12 1.377(3) . ? C3 C4 1.398(2) . ? C4 C9 1.402(3) . ? C4 C5 1.414(3) . ? C5 C6 1.365(2) . ? C6 C7 1.427(3) . ? C7 C8 1.368(3) . ? C8 C9 1.417(3) . ? C9 C10 1.419(3) . ? C10 C11 1.366(3) . ? C11 C12 1.409(3) . ? C19 C20 1.388(3) . ? C19 C24 1.395(3) . ? C20 C21 1.383(3) . ? C21 C22 1.380(3) . ? C22 C23 1.388(3) . ? C23 C24 1.387(3) . ? C25 C26 1.396(3) . ? C25 C30 1.396(3) . ? C26 C27 1.377(3) . ? C27 C28 1.388(3) . ? C28 C29 1.373(3) . ? C29 C30 1.392(3) . ? C31 C32 1.516(3) . ? C33 C34 1.386(3) . ? C33 C38 1.393(3) . ? C34 C35 1.394(3) . ? C35 C36 1.383(3) . ? C36 C37 1.374(3) . ? C37 C38 1.379(3) . ? C39 C40 1.390(3) . ? C39 C44 1.393(3) . ? C40 C41 1.378(3) . ? C41 C42 1.386(3) . ? C42 C43 1.389(3) . ? C43 C44 1.383(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 C1 41.03(7) . . ? N1 Ni1 P1 151.57(5) . . ? C1 Ni1 P1 110.89(6) . . ? N1 Ni1 P2 118.67(5) . . ? C1 Ni1 P2 155.50(6) . . ? P1 Ni1 P2 89.58(2) . . ? N1 Si1 C15 109.81(9) . . ? N1 Si1 C14 116.93(9) . . ? C15 Si1 C14 106.39(10) . . ? N1 Si1 C13 108.78(9) . . ? C15 Si1 C13 107.68(11) . . ? C14 Si1 C13 106.87(9) . . ? N2 Si2 C18 109.37(10) . . ? N2 Si2 C17 114.09(9) . . ? C18 Si2 C17 114.38(10) . . ? N2 Si2 C16 104.32(10) . . ? C18 Si2 C16 107.32(10) . . ? C17 Si2 C16 106.60(10) . . ? C19 P1 C25 103.05(9) . . ? C19 P1 C31 103.07(9) . . ? C25 P1 C31 103.87(9) . . ? C19 P1 Ni1 120.20(7) . . ? C25 P1 Ni1 119.26(7) . . ? C31 P1 Ni1 105.17(7) . . ? C33 P2 C39 102.01(8) . . ? C33 P2 C32 104.16(10) . . ? C39 P2 C32 98.67(9) . . ? C33 P2 Ni1 130.44(6) . . ? C39 P2 Ni1 111.57(7) . . ? C32 P2 Ni1 105.51(6) . . ? C1 N1 Si1 136.70(15) . . ? C1 N1 Ni1 72.95(11) . . ? Si1 N1 Ni1 137.05(9) . . ? C2 N2 Si2 134.40(14) . . ? N1 C1 C5 128.21(15) . . ? N1 C1 C2 123.77(16) . . ? C5 C1 C2 106.21(15) . . ? N1 C1 Ni1 66.02(10) . . ? C5 C1 Ni1 112.06(12) . . ? C2 C1 Ni1 108.98(13) . . ? N2 C2 C3 122.29(16) . . ? N2 C2 C1 132.20(18) . . ? C3 C2 C1 105.48(15) . . ? C12 C3 C4 119.36(18) . . ? C12 C3 C2 132.44(17) . . ? C4 C3 C2 108.14(16) . . ? C3 C4 C9 123.72(17) . . ? C3 C4 C5 112.37(17) . . ? C9 C4 C5 123.88(16) . . ? C6 C5 C4 118.46(18) . . ? C6 C5 C1 134.50(17) . . ? C4 C5 C1 107.03(15) . . ? C5 C6 C7 118.74(18) . . ? C8 C7 C6 122.50(18) . . ? C7 C8 C9 120.17(19) . . ? C4 C9 C8 116.21(17) . . ? C4 C9 C10 115.45(17) . . ? C8 C9 C10 128.3(2) . . ? C11 C10 C9 120.9(2) . . ? C10 C11 C12 122.50(19) . . ? C3 C12 C11 118.01(17) . . ? C20 C19 C24 119.16(18) . . ? C20 C19 P1 118.41(14) . . ? C24 C19 P1 122.38(14) . . ? C21 C20 C19 120.42(18) . . ? C22 C21 C20 120.32(18) . . ? C21 C22 C23 119.8(2) . . ? C24 C23 C22 120.07(18) . . ? C23 C24 C19 120.13(17) . . ? C26 C25 C30 118.70(18) . . ? C26 C25 P1 118.81(16) . . ? C30 C25 P1 122.46(14) . . ? C27 C26 C25 120.7(2) . . ? C26 C27 C28 120.11(19) . . ? C29 C28 C27 119.96(19) . . ? C28 C29 C30 120.4(2) . . ? C29 C30 C25 120.08(19) . . ? C32 C31 P1 108.14(13) . . ? C31 C32 P2 107.17(14) . . ? C34 C33 C38 117.92(19) . . ? C34 C33 P2 122.70(16) . . ? C38 C33 P2 119.38(16) . . ? C33 C34 C35 120.7(2) . . ? C36 C35 C34 120.5(2) . . ? C37 C36 C35 119.0(2) . . ? C36 C37 C38 120.9(2) . . ? C37 C38 C33 121.1(2) . . ? C40 C39 C44 118.55(16) . . ? C40 C39 P2 119.44(13) . . ? C44 C39 P2 121.80(15) . . ? C41 C40 C39 120.81(18) . . ? C40 C41 C42 120.4(2) . . ? C41 C42 C43 119.39(17) . . ? C44 C43 C42 120.02(18) . . ? C43 C44 C39 120.8(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.572 _refine_diff_density_min -0.293 _refine_diff_density_rms 0.076 _publ_section_references ; Bruker (2000) SAINTPlus Data Reduction and Correction Program v. 6.02a, Bruker AXS, Madison, Wisconsin, USA. Bruker (2000) SMART. Bruker Molecular Analysis Research Tool, v. 5.625 Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (1998a). SADABS v.2.01, Bruker/Siemens Area Detector Absorption Correction Program, Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (2000). SHELXTL v. 6.12, Structure Determination Software Suite, Bruker AXS, Madison, Wisconsin, USA. ;