Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 #=========================================================================== data_global #=========================================================================== _audit_creation_date 10-11-00 # 1. SUBMISSION DETAILS _publ_contact_author_name # Name of author for correspondance ; Richard Welter ; _publ_contact_author_address # Address of author for correspondance ; Institut Le Bel, rue Blaise Pascal, 67000 STRASBOURG, FRANCE ; _publ_contact_author_phone '0390241593' _publ_contact_author_fax '0390241232' _publ_contact_author_email welter@chimie.u-strasbg.fr _publ_requested_journal ? _publ_contact_letter ; ; _publ_requested_category FM #=========================================================================== # 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 ; First Structural Characterization of Metal Complexes Resulting from Tail-to-Tail Dimerization and C-H Activation of Methyl Acrylate by a Ni-Mo Complex : a Remarkable Case for Bimetallic Activation of an Organic Molecule ; # 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 'Braunstein, Pierre' #<--'Last name, first name' ; Laboratoire de Chimie de coordination, UMR CNRS 7513 Universit\'e Louis Pasteur Strasbourg France ; 'Chetcuti, Mickael' #<--'Last name, first name' ; Laboratoire de Chimie de coordination, UMR CNRS 7513 Universit\'e Louis Pasteur Strasbourg France ; 'Welter, Richard' #<--'Last name, first name' ; Laboratoire DECMET, UMR CNRS 7513 Universit\'e Louis Pasteur Strasbourg France ; _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. E.Dowty, ATOMS (1999), Shape Software. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. Sheldrick, G.M. (1997). SHELXL97. Program for the refinement of crystal structures. University of Gottingen. Germany. ; data_pbr22 _database_code_CSD 162868 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H11 Mo O6' _chemical_formula_sum 'C15 H11 Mo O6' _chemical_formula_weight 383.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.0224(2) _cell_length_b 18.5428(4) _cell_length_c 7.93560(10) _cell_angle_alpha 90.00 _cell_angle_beta 106.7923(10) _cell_angle_gamma 90.00 _cell_volume 1552.77(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5420 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 34.972 _exptl_crystal_description 'prism' _exptl_crystal_colour 'Yellow' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.639 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 764 _exptl_absorpt_coefficient_mu 0.869 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; ? ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11066 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 34.98 _reflns_number_total 6803 _reflns_number_gt 5384 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ATOMS (Dowty, 1995)' _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^)+(0.0398P)^2^+1.0926P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6803 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0556 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.1024 _refine_ls_wR_factor_gt 0.0951 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 O5 O 0.40284(19) 0.13824(11) 1.1030(2) 0.0449(4) Uani 1 1 d . . . C9 C 0.3598(2) 0.11982(12) 0.9583(3) 0.0304(4) Uani 1 1 d . . . O6 O 0.57357(16) 0.03919(11) 0.7997(2) 0.0434(4) Uani 1 1 d . . . O1 O 0.04966(17) 0.09865(10) 0.9956(2) 0.0390(4) Uani 1 1 d . . . C1 C -0.0610(3) 0.14040(16) 0.9926(4) 0.0456(6) Uani 1 1 d . . . C10 C 0.46854(19) 0.05684(12) 0.7683(3) 0.0294(4) Uani 1 1 d . . . C3 C 0.16805(19) 0.02821(11) 0.8596(3) 0.0264(3) Uani 1 1 d . . . C8 C 0.3521(3) -0.27751(15) 0.5379(5) 0.0536(7) Uani 1 1 d . . . C5 C 0.30206(19) -0.03916(11) 0.7215(2) 0.0272(4) Uani 1 1 d . . . C2 C 0.04618(19) 0.06308(12) 0.8464(3) 0.0277(4) Uani 1 1 d . . . O4 O 0.37586(16) -0.20113(10) 0.5327(3) 0.0434(4) Uani 1 1 d . . . O3 O 0.20154(18) -0.18130(10) 0.6158(3) 0.0486(5) Uani 1 1 d . . . C7 C 0.2919(2) -0.15848(12) 0.5761(3) 0.0313(4) Uani 1 1 d . . . C4 C 0.18179(19) -0.01206(11) 0.7142(3) 0.0266(4) Uani 1 1 d . . . Mo Mo 0.293306(15) 0.088862(9) 0.71464(2) 0.02314(5) Uani 1 1 d . . . C6 C 0.3247(2) -0.07977(12) 0.5681(3) 0.0304(4) Uani 1 1 d . . . O2 O -0.04746(15) 0.06135(11) 0.7206(2) 0.0396(4) Uani 1 1 d . . . C14 C 0.2215(4) 0.20368(16) 0.6116(4) 0.0720(12) Uani 1 1 d . . . C13 C 0.3261(3) 0.1833(3) 0.5458(7) 0.0890(17) Uani 1 1 d . . . C15 C 0.1228(2) 0.15473(18) 0.5268(4) 0.0508(7) Uani 1 1 d . . . C12 C 0.2891(5) 0.1263(3) 0.4349(6) 0.0909(17) Uani 1 1 d . . . C11 C 0.1697(4) 0.11015(19) 0.4219(4) 0.0692(11) Uani 1 1 d . . . H3 H 0.2142 0.0224 0.9830 0.010 Uiso 1 1 d . . . H1A H -0.0487 0.1644 1.1028 0.010 Uiso 1 1 d . . . H8A H 0.3535 -0.2892 0.6575 0.010 Uiso 1 1 d . . . H5 H 0.3675 -0.0548 0.8230 0.010 Uiso 1 1 d . . . H8B H 0.4167 -0.3033 0.5071 0.050 Uiso 1 1 d . . . H1B H -0.1335 0.1100 0.9681 0.050 Uiso 1 1 d . . . H1C H -0.0737 0.1766 0.9001 0.050 Uiso 1 1 d . . . H8C H 0.2708 -0.2880 0.4603 0.050 Uiso 1 1 d . . . H6A H 0.4126 -0.0760 0.5698 0.050 Uiso 1 1 d . . . H4 H 0.1138 -0.0148 0.6070 0.050 Uiso 1 1 d . . . H6B H 0.2728 -0.0599 0.4589 0.050 Uiso 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 O5 0.0520(11) 0.0506(11) 0.0292(8) -0.0072(7) 0.0074(7) -0.0095(9) C9 0.0303(9) 0.0305(10) 0.0302(9) -0.0005(8) 0.0083(7) -0.0048(8) O6 0.0264(8) 0.0543(11) 0.0474(9) 0.0086(8) 0.0073(7) 0.0056(7) O1 0.0367(9) 0.0505(10) 0.0295(7) -0.0040(7) 0.0090(6) 0.0127(7) C1 0.0473(14) 0.0472(14) 0.0463(13) -0.0002(11) 0.0197(11) 0.0162(11) C10 0.0264(9) 0.0335(10) 0.0265(8) 0.0035(8) 0.0048(7) -0.0006(7) C3 0.0256(8) 0.0292(9) 0.0251(8) 0.0024(7) 0.0084(7) -0.0018(7) C8 0.0503(15) 0.0352(13) 0.081(2) -0.0122(13) 0.0275(15) 0.0045(11) C5 0.0283(9) 0.0257(9) 0.0265(8) 0.0014(7) 0.0062(7) 0.0001(7) C2 0.0275(9) 0.0295(9) 0.0272(8) 0.0025(7) 0.0096(7) -0.0014(7) O4 0.0333(8) 0.0345(8) 0.0661(12) -0.0121(8) 0.0202(8) 0.0007(7) O3 0.0421(10) 0.0363(9) 0.0766(14) -0.0029(9) 0.0316(10) -0.0012(7) C7 0.0258(9) 0.0327(10) 0.0342(10) -0.0039(8) 0.0068(7) 0.0029(7) C4 0.0254(8) 0.0272(9) 0.0272(8) -0.0003(7) 0.0077(7) -0.0031(7) Mo 0.02175(8) 0.02512(8) 0.02169(8) 0.00323(6) 0.00493(5) -0.00033(6) C6 0.0293(9) 0.0329(10) 0.0300(9) -0.0020(8) 0.0105(8) 0.0014(7) O2 0.0248(7) 0.0553(10) 0.0357(8) -0.0058(8) 0.0040(6) 0.0003(7) C14 0.124(3) 0.0291(12) 0.0415(14) 0.0076(11) -0.0093(17) 0.0221(17) C13 0.0320(14) 0.092(3) 0.125(4) 0.087(3) -0.0052(18) -0.0126(16) C15 0.0294(11) 0.0647(18) 0.0555(15) 0.0351(14) 0.0076(10) 0.0114(11) C12 0.094(3) 0.129(4) 0.067(2) 0.069(3) 0.051(2) 0.055(3) C11 0.105(3) 0.0549(18) 0.0267(12) 0.0084(12) -0.0142(15) 0.0219(19) _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 O5 C9 1.160(3) . ? C9 Mo 1.946(2) . ? O6 C10 1.159(3) . ? O1 C2 1.346(3) . ? O1 C1 1.439(3) . ? C10 Mo 1.947(2) . ? C3 C4 1.418(3) . ? C3 C2 1.467(3) . ? C3 Mo 2.3262(19) . ? C8 O4 1.443(3) . ? C5 C4 1.403(3) . ? C5 C6 1.512(3) . ? C5 Mo 2.376(2) . ? C2 O2 1.212(2) . ? O4 C7 1.336(3) . ? O3 C7 1.204(3) . ? C7 C6 1.509(3) . ? C4 Mo 2.238(2) . ? Mo C13 2.296(3) . ? Mo C12 2.314(3) . ? Mo C14 2.336(3) . ? Mo C11 2.362(3) . ? Mo C15 2.372(2) . ? C14 C15 1.427(5) . ? C14 C13 1.446(6) . ? C13 C12 1.360(7) . ? C15 C11 1.375(5) . ? C12 C11 1.326(6) . ? 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 O5 C9 Mo 178.1(2) . . ? C2 O1 C1 116.11(19) . . ? O6 C10 Mo 178.6(2) . . ? C4 C3 C2 119.00(18) . . ? C4 C3 Mo 68.56(11) . . ? C2 C3 Mo 114.44(13) . . ? C4 C5 C6 121.23(18) . . ? C4 C5 Mo 67.02(11) . . ? C6 C5 Mo 119.62(13) . . ? O2 C2 O1 122.6(2) . . ? O2 C2 C3 126.3(2) . . ? O1 C2 C3 111.13(17) . . ? C7 O4 C8 115.3(2) . . ? O3 C7 O4 123.1(2) . . ? O3 C7 C6 125.2(2) . . ? O4 C7 C6 111.66(19) . . ? C5 C4 C3 118.46(18) . . ? C5 C4 Mo 77.73(12) . . ? C3 C4 Mo 75.30(11) . . ? C9 Mo C10 78.91(9) . . ? C9 Mo C4 107.28(8) . . ? C10 Mo C4 104.78(8) . . ? C9 Mo C13 106.10(17) . . ? C10 Mo C13 92.68(11) . . ? C4 Mo C13 144.66(13) . . ? C9 Mo C12 139.67(19) . . ? C10 Mo C12 92.57(12) . . ? C4 Mo C12 113.00(18) . . ? C13 Mo C12 34.33(18) . . ? C9 Mo C3 76.00(8) . . ? C10 Mo C3 115.94(8) . . ? C4 Mo C3 36.14(7) . . ? C13 Mo C3 150.83(12) . . ? C12 Mo C3 140.30(17) . . ? C9 Mo C14 94.09(10) . . ? C10 Mo C14 124.70(14) . . ? C4 Mo C14 129.14(13) . . ? C13 Mo C14 36.38(16) . . ? C12 Mo C14 58.65(15) . . ? C3 Mo C14 115.11(13) . . ? C9 Mo C11 150.75(11) . . ? C10 Mo C11 121.35(13) . . ? C4 Mo C11 88.72(12) . . ? C13 Mo C11 56.09(15) . . ? C12 Mo C11 32.91(16) . . ? C3 Mo C11 108.10(13) . . ? C14 Mo C11 57.47(11) . . ? C9 Mo C15 118.36(11) . . ? C10 Mo C15 148.26(9) . . ? C4 Mo C15 95.43(9) . . ? C13 Mo C15 58.01(10) . . ? C12 Mo C15 56.64(12) . . ? C3 Mo C15 94.82(8) . . ? C14 Mo C15 35.28(12) . . ? C11 Mo C15 33.77(12) . . ? C9 Mo C5 105.71(8) . . ? C10 Mo C5 70.07(8) . . ? C4 Mo C5 35.25(7) . . ? C13 Mo C5 139.76(17) . . ? C12 Mo C5 108.14(16) . . ? C3 Mo C5 62.06(7) . . ? C14 Mo C5 157.87(10) . . ? C11 Mo C5 101.40(10) . . ? C15 Mo C5 123.26(10) . . ? C7 C6 C5 110.53(18) . . ? C15 C14 C13 104.0(3) . . ? C15 C14 Mo 73.75(15) . . ? C13 C14 Mo 70.31(16) . . ? C12 C13 C14 108.4(3) . . ? C12 C13 Mo 73.57(19) . . ? C14 C13 Mo 73.31(17) . . ? C11 C15 C14 107.4(3) . . ? C11 C15 Mo 72.72(15) . . ? C14 C15 Mo 70.97(15) . . ? C11 C12 C13 109.3(4) . . ? C11 C12 Mo 75.53(18) . . ? C13 C12 Mo 72.1(2) . . ? C12 C11 C15 110.8(4) . . ? C12 C11 Mo 71.55(19) . . ? C15 C11 Mo 73.51(15) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 34.98 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.857 _refine_diff_density_min -1.046 _refine_diff_density_rms 0.095 data_pbr25 _database_code_CSD 162869 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H30 Mo2 Ni O6' _chemical_formula_sum 'C28 H30 Mo2 Ni O6' _chemical_formula_weight 713.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.3564(3) _cell_length_b 16.6644(4) _cell_length_c 15.3764(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.4249(11) _cell_angle_gamma 90.00 _cell_volume 2653.64(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8636 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description 'prism' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.785 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 1.674 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; ? ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7737 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1356 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 30.06 _reflns_number_total 7736 _reflns_number_gt 5611 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ATOMS (E.Dowty, 1999)' _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^)+(0.0000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7736 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0834 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1040 _refine_ls_wR_factor_gt 0.0922 _refine_ls_goodness_of_fit_ref 0.823 _refine_ls_restrained_S_all 0.823 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2000(3) 0.0055(2) 0.2028(2) 0.0156(7) Uani 1 1 d . . . C2 C 0.1649(4) 0.0092(2) 0.1067(3) 0.0232(8) Uani 1 1 d . . . C3 C 0.1080(4) -0.0676(2) 0.0701(2) 0.0245(8) Uani 1 1 d . . . C4 C 0.1625(5) -0.1907(3) 0.0018(4) 0.0492(14) Uani 1 1 d . . . C5 C -0.0888(4) 0.0982(3) 0.3459(3) 0.0386(11) Uani 1 1 d . . . C6 C -0.1204(4) 0.0201(3) 0.3708(4) 0.0468(14) Uani 1 1 d . . . C7 C -0.1263(4) -0.0273(3) 0.2962(5) 0.0540(17) Uani 1 1 d . . . C8 C -0.0997(4) 0.0217(4) 0.2250(4) 0.0461(14) Uani 1 1 d . . . C9 C -0.0751(4) 0.0997(3) 0.2554(3) 0.0354(11) Uani 1 1 d . . . C10 C 0.1915(4) 0.0707(2) 0.4023(3) 0.0219(8) Uani 1 1 d . . . C11 C 0.1095(4) -0.0826(2) 0.3822(3) 0.0235(8) Uani 1 1 d . . . C12 C 0.4763(4) -0.0183(2) 0.3910(3) 0.0279(9) Uani 1 1 d . . . C13 C 0.5469(4) -0.0596(2) 0.3275(3) 0.0284(9) Uani 1 1 d . . . C14 C 0.5050(4) -0.1406(2) 0.3257(3) 0.0306(9) Uani 1 1 d . . . C15 C 0.4062(4) -0.1485(2) 0.3878(3) 0.0282(9) Uani 1 1 d . . . C16 C 0.3877(4) -0.0732(2) 0.4290(3) 0.0260(9) Uani 1 1 d . . . C17 C 0.2373(4) -0.1554(2) 0.2322(3) 0.0256(8) Uani 1 1 d . . . C18 C 0.4198(4) -0.0550(2) 0.1640(3) 0.0243(8) Uani 1 1 d . . . C19 C 0.4106(4) 0.1879(2) 0.3030(2) 0.0196(7) Uani 1 1 d . . . C20 C 0.2839(4) 0.2179(2) 0.2810(3) 0.0201(8) Uani 1 1 d . . . C21 C 0.2636(4) 0.2053(2) 0.1903(3) 0.0204(8) Uani 1 1 d . . . C22 C 0.3739(4) 0.1660(2) 0.1565(2) 0.0211(8) Uani 1 1 d . . . C23 C 0.4634(3) 0.1547(2) 0.2260(2) 0.0192(7) Uani 1 1 d . . . C24 C 0.4804(5) 0.1999(3) 0.3869(3) 0.0345(10) Uani 1 1 d . . . C25 C 0.1992(5) 0.2643(2) 0.3413(3) 0.0354(11) Uani 1 1 d . . . C26 C 0.1518(4) 0.2357(3) 0.1370(3) 0.0382(11) Uani 1 1 d . . . C27 C 0.3999(5) 0.1498(3) 0.0623(3) 0.0358(11) Uani 1 1 d . . . C28 C 0.5990(4) 0.1241(2) 0.2153(3) 0.0312(10) Uani 1 1 d . . . Ni Ni 0.28879(4) 0.09225(2) 0.25520(3) 0.01263(10) Uani 1 1 d . . . Mo1 Mo 0.08647(3) 0.014723(18) 0.31409(2) 0.01610(8) Uani 1 1 d . . . Mo2 Mo 0.33584(3) -0.061483(17) 0.27809(2) 0.01343(8) Uani 1 1 d . . . O1 O -0.0030(3) -0.08542(19) 0.0657(2) 0.0400(8) Uani 1 1 d . . . O2 O 0.2020(3) -0.11438(19) 0.0384(2) 0.0398(8) Uani 1 1 d . . . O3 O 0.2371(3) 0.10021(17) 0.46317(19) 0.0325(7) Uani 1 1 d . . . O4 O 0.1048(3) -0.13955(18) 0.4272(2) 0.0369(7) Uani 1 1 d . . . O5 O 0.1833(4) -0.21176(18) 0.2105(2) 0.0447(9) Uani 1 1 d . . . O6 O 0.4749(3) -0.0528(2) 0.0997(2) 0.0443(9) Uani 1 1 d . . . H1 H 0.2424 0.0216 0.0755 0.031 Uiso 1 1 d . . . H2 H 0.1050 0.0510 0.0993 0.031 Uiso 1 1 d . . . H3 H 0.2362 -0.2198 -0.0172 0.062 Uiso 1 1 d . . . H4 H 0.1200 -0.2224 0.0458 0.062 Uiso 1 1 d . . . H5 H 0.1044 -0.1836 -0.0454 0.062 Uiso 1 1 d . . . H6 H -0.0759 0.1439 0.3842 0.043 Uiso 1 1 d . . . H7 H -0.1353 0.0050 0.4283 0.055 Uiso 1 1 d . . . H8 H -0.1423 -0.0832 0.2938 0.061 Uiso 1 1 d . . . H9 H -0.0972 0.0058 0.1643 0.056 Uiso 1 1 d . . . H10 H -0.0539 0.1463 0.2223 0.044 Uiso 1 1 d . . . H11 H 0.4878 0.0387 0.4072 0.037 Uiso 1 1 d . . . H12 H 0.6137 -0.0368 0.2899 0.039 Uiso 1 1 d . . . H13 H 0.5402 -0.1821 0.2883 0.040 Uiso 1 1 d . . . H14 H 0.3583 -0.1979 0.3994 0.036 Uiso 1 1 d . . . H15 H 0.3245 -0.0604 0.4746 0.034 Uiso 1 1 d . . . H16 H 0.4229 0.2231 0.4294 0.042 Uiso 1 1 d . . . H17 H 0.5109 0.1501 0.4099 0.042 Uiso 1 1 d . . . H18 H 0.5520 0.2354 0.3807 0.042 Uiso 1 1 d . . . H19 H 0.1191 0.2772 0.3127 0.045 Uiso 1 1 d . . . H20 H 0.1795 0.2318 0.3911 0.045 Uiso 1 1 d . . . H21 H 0.2399 0.3118 0.3597 0.045 Uiso 1 1 d . . . H22 H 0.1603 0.2188 0.0786 0.046 Uiso 1 1 d . . . H23 H 0.0728 0.2151 0.1599 0.046 Uiso 1 1 d . . . H24 H 0.1493 0.2928 0.1393 0.046 Uiso 1 1 d . . . H25 H 0.4798 0.1240 0.0553 0.048 Uiso 1 1 d . . . H26 H 0.3324 0.1179 0.0377 0.048 Uiso 1 1 d . . . H27 H 0.4017 0.2001 0.0304 0.048 Uiso 1 1 d . . . H28 H 0.6436 0.1223 0.2682 0.039 Uiso 1 1 d . . . H29 H 0.5982 0.0728 0.1882 0.039 Uiso 1 1 d . . . H30 H 0.6464 0.1602 0.1761 0.039 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0139(16) 0.0141(16) 0.0188(18) 0.0006(13) -0.0017(13) -0.0017(13) C2 0.032(2) 0.0201(18) 0.0179(18) -0.0003(15) -0.0063(16) -0.0030(16) C3 0.034(2) 0.0226(19) 0.0170(18) -0.0015(15) -0.0098(17) -0.0044(16) C4 0.057(3) 0.035(3) 0.055(3) -0.026(2) -0.010(3) -0.001(2) C5 0.023(2) 0.041(3) 0.052(3) -0.009(2) 0.004(2) 0.014(2) C6 0.019(2) 0.064(4) 0.058(3) 0.026(3) 0.019(2) 0.010(2) C7 0.014(2) 0.029(3) 0.118(6) 0.003(3) -0.003(3) 0.0003(18) C8 0.018(2) 0.072(4) 0.048(3) -0.020(3) -0.009(2) 0.018(2) C9 0.019(2) 0.037(2) 0.050(3) 0.014(2) 0.000(2) 0.0078(18) C10 0.0240(19) 0.0164(17) 0.025(2) 0.0007(15) 0.0067(16) 0.0034(14) C11 0.0227(19) 0.0164(17) 0.031(2) 0.0044(16) 0.0020(17) -0.0017(14) C12 0.029(2) 0.025(2) 0.030(2) -0.0013(17) -0.0188(18) 0.0001(17) C13 0.0126(18) 0.032(2) 0.040(2) 0.0083(19) -0.0064(17) 0.0018(16) C14 0.029(2) 0.0205(19) 0.042(3) 0.0037(18) -0.0056(19) 0.0149(17) C15 0.032(2) 0.0175(18) 0.035(2) 0.0069(16) -0.0112(18) 0.0026(16) C16 0.027(2) 0.033(2) 0.0180(19) 0.0018(16) -0.0088(16) 0.0057(17) C17 0.030(2) 0.0194(19) 0.027(2) 0.0014(16) -0.0081(17) 0.0003(16) C18 0.024(2) 0.0240(19) 0.025(2) -0.0052(16) 0.0032(16) 0.0011(16) C19 0.0248(19) 0.0110(16) 0.0230(19) -0.0026(14) -0.0020(15) -0.0065(14) C20 0.0235(19) 0.0101(16) 0.027(2) -0.0018(14) 0.0033(16) -0.0006(14) C21 0.0216(19) 0.0129(16) 0.027(2) 0.0067(14) -0.0046(15) -0.0023(14) C22 0.031(2) 0.0127(16) 0.0200(18) 0.0018(14) 0.0045(16) -0.0070(15) C23 0.0184(17) 0.0135(16) 0.0256(19) -0.0006(14) 0.0019(15) -0.0058(13) C24 0.048(3) 0.025(2) 0.030(2) -0.0029(18) -0.012(2) -0.0118(19) C25 0.045(3) 0.0199(19) 0.041(3) -0.0061(18) 0.015(2) 0.0097(19) C26 0.037(3) 0.030(2) 0.047(3) 0.015(2) -0.013(2) -0.0014(19) C27 0.053(3) 0.034(2) 0.020(2) 0.0036(18) 0.012(2) -0.011(2) C28 0.020(2) 0.027(2) 0.046(3) 0.0023(19) 0.0045(19) -0.0074(16) Ni 0.0138(2) 0.0103(2) 0.0138(2) -0.00033(16) -0.00056(17) -0.00054(16) Mo1 0.01208(14) 0.01495(15) 0.02129(16) 0.00252(12) 0.00180(12) 0.00118(11) Mo2 0.01318(14) 0.01132(14) 0.01578(15) -0.00087(11) -0.00135(11) 0.00153(11) O1 0.0332(18) 0.0384(18) 0.048(2) -0.0135(16) -0.0035(15) -0.0110(14) O2 0.0382(18) 0.0350(18) 0.046(2) -0.0220(15) -0.0073(15) -0.0033(14) O3 0.0446(18) 0.0311(16) 0.0218(15) -0.0083(13) 0.0043(13) -0.0054(14) O4 0.0356(17) 0.0310(16) 0.0440(19) 0.0154(15) 0.0070(15) -0.0018(14) O5 0.060(2) 0.0245(16) 0.050(2) -0.0027(15) -0.0152(18) -0.0142(15) O6 0.053(2) 0.049(2) 0.0317(18) -0.0069(16) 0.0187(16) -0.0025(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken= into account individually in the estimation of esds in distances, angles= and torsion angles; correlations between esds in cell parameters are only= used when they are defined by crystal symmetry. An approximate (isotropic= ) treatment of cell esds is used for estimating esds involving l.s. planes.= ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.519(5) . ? C1 Ni 1.891(3) . ? C1 Mo1 2.090(4) . ? C1 Mo2 2.131(3) . ? C2 C3 1.516(5) . ? C3 O1 1.189(5) . ? C3 O2 1.342(5) . ? C4 O2 1.449(5) . ? C5 C6 1.395(7) . ? C5 C9 1.400(7) . ? C5 Mo1 2.341(4) . ? C6 C7 1.395(8) . ? C6 Mo1 2.321(4) . ? C7 C8 1.395(8) . ? C7 Mo1 2.327(5) . ? C8 C9 1.404(7) . ? C8 Mo1 2.360(5) . ? C9 Mo1 2.366(4) . ? C10 O3 1.156(5) . ? C10 Mo1 1.967(4) . ? C10 Ni 2.509(4) . ? C11 O4 1.176(5) . ? C11 Mo1 1.944(4) . ? C12 C13 1.405(6) . ? C12 C16 1.424(6) . ? C12 Mo2 2.369(4) . ? C13 C14 1.417(6) . ? C13 Mo2 2.309(4) . ? C14 C15 1.410(6) . ? C14 Mo2 2.307(4) . ? C15 C16 1.420(6) . ? C15 Mo2 2.337(4) . ? C16 Mo2 2.385(4) . ? C17 O5 1.142(5) . ? C17 Mo2 1.994(4) . ? C18 O6 1.146(5) . ? C18 Mo2 1.967(4) . ? C19 C23 1.419(5) . ? C19 C20 1.443(5) . ? C19 C24 1.489(6) . ? C19 Ni 2.158(3) . ? C20 C21 1.424(5) . ? C20 C25 1.496(5) . ? C20 Ni 2.132(3) . ? C21 C22 1.418(5) . ? C21 C26 1.502(6) . ? C21 Ni 2.146(3) . ? C22 C23 1.422(6) . ? C22 C27 1.500(5) . ? C22 Ni 2.147(4) . ? C23 C28 1.504(5) . ? C23 Ni 2.136(3) . ? Ni Mo1 2.6282(5) . ? Ni Mo2 2.6309(5) . ? Mo1 Mo2 2.9343(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 C2 C1 Ni 119.6(2) . . ? C2 C1 Mo1 131.4(3) . . ? Ni C1 Mo1 82.47(14) . . ? C2 C1 Mo2 134.6(3) . . ? Ni C1 Mo2 81.47(13) . . ? Mo1 C1 Mo2 88.08(13) . . ? C3 C2 C1 114.6(3) . . ? O1 C3 O2 122.5(4) . . ? O1 C3 C2 127.3(4) . . ? O2 C3 C2 110.1(3) . . ? C6 C5 C9 108.4(5) . . ? C6 C5 Mo1 71.8(3) . . ? C9 C5 Mo1 73.7(2) . . ? C7 C6 C5 108.2(5) . . ? C7 C6 Mo1 72.8(3) . . ? C5 C6 Mo1 73.4(2) . . ? C6 C7 C8 107.8(4) . . ? C6 C7 Mo1 72.3(3) . . ? C8 C7 Mo1 74.0(3) . . ? C7 C8 C9 108.5(5) . . ? C7 C8 Mo1 71.4(3) . . ? C9 C8 Mo1 73.0(3) . . ? C5 C9 C8 107.1(4) . . ? C5 C9 Mo1 71.7(2) . . ? C8 C9 Mo1 72.5(3) . . ? O3 C10 Mo1 168.8(3) . . ? O3 C10 Ni 120.3(3) . . ? Mo1 C10 Ni 70.74(12) . . ? O4 C11 Mo1 170.0(3) . . ? C13 C12 C16 108.1(4) . . ? C13 C12 Mo2 70.2(2) . . ? C16 C12 Mo2 73.2(2) . . ? C12 C13 C14 108.6(4) . . ? C12 C13 Mo2 74.9(2) . . ? C14 C13 Mo2 72.0(2) . . ? C15 C14 C13 107.4(4) . . ? C15 C14 Mo2 73.5(2) . . ? C13 C14 Mo2 72.2(2) . . ? C14 C15 C16 108.7(4) . . ? C14 C15 Mo2 71.2(2) . . ? C16 C15 Mo2 74.4(2) . . ? C15 C16 C12 107.2(4) . . ? C15 C16 Mo2 70.6(2) . . ? C12 C16 Mo2 72.0(2) . . ? O5 C17 Mo2 175.8(4) . . ? O6 C18 Mo2 176.1(4) . . ? C23 C19 C20 107.2(3) . . ? C23 C19 C24 126.0(4) . . ? C20 C19 C24 126.2(4) . . ? C23 C19 Ni 69.9(2) . . ? C20 C19 Ni 69.39(19) . . ? C24 C19 Ni 132.4(3) . . ? C21 C20 C19 107.8(3) . . ? C21 C20 C25 126.9(4) . . ? C19 C20 C25 124.8(4) . . ? C21 C20 Ni 71.1(2) . . ? C19 C20 Ni 71.31(19) . . ? C25 C20 Ni 129.6(3) . . ? C22 C21 C20 108.2(3) . . ? C22 C21 C26 125.1(4) . . ? C20 C21 C26 126.3(4) . . ? C22 C21 Ni 70.7(2) . . ? C20 C21 Ni 70.0(2) . . ? C26 C21 Ni 129.9(3) . . ? C21 C22 C23 108.0(3) . . ? C21 C22 C27 126.0(4) . . ? C23 C22 C27 125.5(4) . . ? C21 C22 Ni 70.7(2) . . ? C23 C22 Ni 70.2(2) . . ? C27 C22 Ni 131.1(3) . . ? C19 C23 C22 108.8(3) . . ? C19 C23 C28 126.1(4) . . ? C22 C23 C28 124.5(4) . . ? C19 C23 Ni 71.5(2) . . ? C22 C23 Ni 71.0(2) . . ? C28 C23 Ni 130.6(3) . . ? C1 Ni C20 144.93(15) . . ? C1 Ni C23 133.82(15) . . ? C20 Ni C23 65.31(14) . . ? C1 Ni C21 114.57(15) . . ? C20 Ni C21 38.89(14) . . ? C23 Ni C21 64.89(14) . . ? C1 Ni C22 109.72(15) . . ? C20 Ni C22 65.14(14) . . ? C23 Ni C22 38.78(15) . . ? C21 Ni C22 38.59(14) . . ? C1 Ni C19 172.32(15) . . ? C20 Ni C19 39.29(14) . . ? C23 Ni C19 38.58(14) . . ? C21 Ni C19 65.11(14) . . ? C22 Ni C19 64.89(14) . . ? C1 Ni C10 94.45(14) . . ? C20 Ni C10 87.86(13) . . ? C23 Ni C10 127.24(14) . . ? C21 Ni C10 119.76(14) . . ? C22 Ni C10 152.72(13) . . ? C19 Ni C10 92.10(13) . . ? C1 Ni Mo1 52.02(11) . . ? C20 Ni Mo1 113.49(10) . . ? C23 Ni Mo1 171.79(11) . . ? C21 Ni Mo1 119.79(10) . . ? C22 Ni Mo1 149.03(11) . . ? C19 Ni Mo1 135.35(10) . . ? C10 Ni Mo1 44.96(9) . . ? C1 Ni Mo2 53.22(10) . . ? C20 Ni Mo2 159.42(11) . . ? C23 Ni Mo2 110.23(10) . . ? C21 Ni Mo2 159.79(11) . . ? C22 Ni Mo2 125.13(10) . . ? C19 Ni Mo2 124.49(10) . . ? C10 Ni Mo2 79.35(8) . . ? Mo1 Ni Mo2 67.827(14) . . ? C11 Mo1 C10 87.65(16) . . ? C11 Mo1 C1 108.18(15) . . ? C10 Mo1 C1 106.75(14) . . ? C11 Mo1 C6 86.56(17) . . ? C10 Mo1 C6 103.27(19) . . ? C1 Mo1 C6 146.87(18) . . ? C11 Mo1 C7 85.69(18) . . ? C10 Mo1 C7 137.9(2) . . ? C1 Mo1 C7 114.8(2) . . ? C6 Mo1 C7 34.9(2) . . ? C11 Mo1 C5 118.37(17) . . ? C10 Mo1 C5 89.98(16) . . ? C1 Mo1 C5 131.08(16) . . ? C6 Mo1 C5 34.82(17) . . ? C7 Mo1 C5 57.90(17) . . ? C11 Mo1 C8 116.77(19) . . ? C10 Mo1 C8 145.28(17) . . ? C1 Mo1 C8 89.46(16) . . ? C6 Mo1 C8 57.57(19) . . ? C7 Mo1 C8 34.6(2) . . ? C5 Mo1 C8 57.36(17) . . ? C11 Mo1 C9 142.04(16) . . ? C10 Mo1 C9 111.39(17) . . ? C1 Mo1 C9 97.63(15) . . ? C6 Mo1 C9 57.84(16) . . ? C7 Mo1 C9 57.91(17) . . ? C5 Mo1 C9 34.60(17) . . ? C8 Mo1 C9 34.58(17) . . ? C11 Mo1 Ni 120.03(11) . . ? C10 Mo1 Ni 64.30(11) . . ? C1 Mo1 Ni 45.51(9) . . ? C6 Mo1 Ni 148.31(14) . . ? C7 Mo1 Ni 149.79(17) . . ? C5 Mo1 Ni 113.66(12) . . ? C8 Mo1 Ni 115.21(15) . . ? C9 Mo1 Ni 97.92(11) . . ? C11 Mo1 Mo2 68.65(11) . . ? C10 Mo1 Mo2 81.51(11) . . ? C1 Mo1 Mo2 46.54(9) . . ? C6 Mo1 Mo2 154.68(13) . . ? C7 Mo1 Mo2 132.96(13) . . ? C5 Mo1 Mo2 168.91(12) . . ? C8 Mo1 Mo2 128.93(12) . . ? C9 Mo1 Mo2 143.93(12) . . ? Ni Mo1 Mo2 56.131(12) . . ? C18 Mo2 C17 87.50(17) . . ? C18 Mo2 C1 77.32(15) . . ? C17 Mo2 C1 83.38(14) . . ? C18 Mo2 C14 88.57(16) . . ? C17 Mo2 C14 92.82(16) . . ? C1 Mo2 C14 165.51(15) . . ? C18 Mo2 C13 82.48(16) . . ? C17 Mo2 C13 127.40(15) . . ? C1 Mo2 C13 142.32(14) . . ? C14 Mo2 C13 35.75(14) . . ? C18 Mo2 C15 122.72(16) . . ? C17 Mo2 C15 85.65(15) . . ? C1 Mo2 C15 156.69(14) . . ? C14 Mo2 C15 35.35(15) . . ? C13 Mo2 C15 58.75(14) . . ? C18 Mo2 C12 111.34(17) . . ? C17 Mo2 C12 143.84(15) . . ? C1 Mo2 C12 129.69(13) . . ? C14 Mo2 C12 58.68(15) . . ? C13 Mo2 C12 34.92(15) . . ? C15 Mo2 C12 58.19(14) . . ? C18 Mo2 C16 140.75(16) . . ? C17 Mo2 C16 112.99(15) . . ? C1 Mo2 C16 135.58(13) . . ? C14 Mo2 C16 58.66(15) . . ? C13 Mo2 C16 58.36(15) . . ? C15 Mo2 C16 34.98(14) . . ? C12 Mo2 C16 34.86(14) . . ? C18 Mo2 Ni 84.81(11) . . ? C17 Mo2 Ni 128.55(11) . . ? C1 Mo2 Ni 45.30(9) . . ? C14 Mo2 Ni 137.57(11) . . ? C13 Mo2 Ni 101.83(10) . . ? C15 Mo2 Ni 139.22(11) . . ? C12 Mo2 Ni 85.08(10) . . ? C16 Mo2 Ni 104.45(10) . . ? C18 Mo2 Mo1 122.67(12) . . ? C17 Mo2 Mo1 87.57(12) . . ? C1 Mo2 Mo1 45.38(10) . . ? C14 Mo2 Mo1 148.72(12) . . ? C13 Mo2 Mo1 139.87(11) . . ? C15 Mo2 Mo1 113.75(11) . . ? C12 Mo2 Mo1 105.48(11) . . ? C16 Mo2 Mo1 92.51(10) . . ? Ni Mo2 Mo1 56.042(12) . . ? C3 O2 C4 116.6(4) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 30.06 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.535 _refine_diff_density_min -0.694 _refine_diff_density_rms 0.115