Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Armando Pombeiro' 'Alegria,Elisabete C. B. A.' 'Frausto da Silva,Joao J. R.' 'David L. Hughes' 'Luisa M. D. R. S. Martins' _publ_contact_author_name 'Prof Armando Pombeiro' _publ_contact_author_address ; Centro de Quimica Estrutural Instituto Superior Tecnico Av. Rovisco Pais Lisboa 1049-001 PORTUGAL ; _publ_contact_author_email POMBEIRO@IST.UTL.PT _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Syntheses and Properties of Hydride-cyanamide and Derived Hydrogen-cyanamide Complexes of Molybdenum(IV). Crystal Structure of [MoH2(NCNH2)2 Ph2PCH2CH2PPh2)2][BF4]2 ; data_luisa1 _database_code_CSD 212459 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H54 Mo N4 P4, 2(B F4), C4 H8 O, (?)' _chemical_formula_structural [Mo(H)2(NCNH2)2(dppe)2](BF4)2.thf.(solvent?) _chemical_formula_sum 'C58 H62 B2 F8 Mo N4 O P4' _chemical_formula_weight 1224.56 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/a' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 32.620(5) _cell_length_b 14.848(2) _cell_length_c 12.440(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.06(2) _cell_angle_gamma 90.00 _cell_volume 5991.5(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 9 _exptl_crystal_description parallelipipeds _exptl_crystal_colour 'dull yellow' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.358 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2520 _exptl_absorpt_coefficient_mu 0.393 _exptl_absorpt_correction_type 'semi-empirical psi-scans' _exptl_absorpt_correction_T_min 0.006 _exptl_absorpt_correction_T_max 0.015 _exptl_absorpt_process_details ; EMPABS, (Sheldrick et al,' 1977) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method 'scintillation counter; \w/\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '10000 s' _diffrn_standards_decay_% 21.9 _diffrn_reflns_number 4416 _diffrn_reflns_av_R_equivalents 0.073 _diffrn_reflns_av_sigmaI/netI 0.1256 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 17.98 _reflns_number_total 4060 _reflns_number_gt 1942 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_cell_refinement 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_data_reduction 'CAD4 (Hursthouse, 1976)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _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^)+(0.1529P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _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 4060 _refine_ls_number_parameters 692 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1559 _refine_ls_R_factor_gt 0.0940 _refine_ls_wR_factor_ref 0.2903 _refine_ls_wR_factor_gt 0.2333 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.095 _refine_ls_shift/su_mean 0.006 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 Mo Mo 0.37057(5) 0.34194(12) 0.40383(16) 0.0708(8) Uani 1 1 d . . . P1 P 0.42341(16) 0.3546(4) 0.5621(5) 0.0730(18) Uani 1 1 d . . . C11A C 0.4399(8) 0.2515(15) 0.6329(18) 0.077(8) Uani 1 1 d . . . C12A C 0.4785(8) 0.2106(18) 0.634(2) 0.096(8) Uani 1 1 d . . . H12A H 0.4994 0.2371 0.5997 0.115 Uiso 1 1 calc R . . C13A C 0.4849(9) 0.125(2) 0.691(2) 0.109(9) Uani 1 1 d . . . H13A H 0.5109 0.0992 0.6983 0.131 Uiso 1 1 calc R . . C14A C 0.4535(14) 0.0846(17) 0.732(2) 0.125(15) Uani 1 1 d . . . H14A H 0.4568 0.0290 0.7658 0.151 Uiso 1 1 calc R . . C15A C 0.4148(8) 0.130(3) 0.721(3) 0.128(15) Uani 1 1 d . . . H15A H 0.3921 0.1005 0.7444 0.153 Uiso 1 1 calc R . . C16A C 0.4096(12) 0.2093(19) 0.680(3) 0.141(17) Uani 1 1 d . . . H16A H 0.3844 0.2383 0.6824 0.169 Uiso 1 1 calc R . . C11B C 0.4189(6) 0.4359(19) 0.670(2) 0.079(7) Uani 1 1 d . . . C12B C 0.4166(6) 0.529(2) 0.643(2) 0.092(8) Uani 1 1 d . . . H12B H 0.4169 0.5496 0.5726 0.111 Uiso 1 1 calc R . . C13B C 0.4138(7) 0.5880(15) 0.731(3) 0.100(9) Uani 1 1 d . . . H13B H 0.4094 0.6487 0.7153 0.120 Uiso 1 1 calc R . . C14B C 0.4170(8) 0.563(2) 0.834(3) 0.105(9) Uani 1 1 d . . . H14B H 0.4164 0.6058 0.8889 0.126 Uiso 1 1 calc R . . C15B C 0.4210(8) 0.478(3) 0.858(2) 0.103(8) Uani 1 1 d . . . H15B H 0.4230 0.4591 0.9300 0.124 Uiso 1 1 calc R . . C16B C 0.4223(6) 0.4157(16) 0.777(3) 0.085(7) Uani 1 1 d . . . H16B H 0.4258 0.3556 0.7969 0.102 Uiso 1 1 calc R . . C1 C 0.4698(5) 0.3971(13) 0.5108(16) 0.065(6) Uani 1 1 d . . . H1A H 0.4681 0.4622 0.5052 0.078 Uiso 1 1 calc R . . H1B H 0.4935 0.3824 0.5616 0.078 Uiso 1 1 calc R . . C2 C 0.4760(5) 0.3582(13) 0.4013(17) 0.071(6) Uani 1 1 d . . . H2A H 0.4810 0.2940 0.4083 0.085 Uiso 1 1 calc R . . H2B H 0.5001 0.3856 0.3752 0.085 Uiso 1 1 calc R . . P2 P 0.43143(16) 0.3778(4) 0.3041(5) 0.0751(18) Uani 1 1 d . . . C21A C 0.4410(11) 0.3065(17) 0.190(2) 0.097(8) Uani 1 1 d . . . C22A C 0.4120(8) 0.3072(16) 0.096(3) 0.083(7) Uani 1 1 d . . . H22A H 0.3886 0.3431 0.0947 0.100 Uiso 1 1 calc R . . C23A C 0.4181(13) 0.257(2) 0.011(2) 0.113(10) Uani 1 1 d . . . H23A H 0.3971 0.2533 -0.0455 0.136 Uiso 1 1 calc R . . C24A C 0.4543(15) 0.211(2) 0.004(3) 0.133(12) Uani 1 1 d . . . H24A H 0.4594 0.1797 -0.0585 0.159 Uiso 1 1 calc R . . C25A C 0.4803(12) 0.213(3) 0.088(4) 0.154(14) Uani 1 1 d . . . H25A H 0.5049 0.1816 0.0846 0.185 Uiso 1 1 calc R . . C26A C 0.4753(10) 0.259(2) 0.185(3) 0.116(9) Uani 1 1 d . . . H26A H 0.4954 0.2554 0.2436 0.139 Uiso 1 1 calc R . . C21B C 0.4414(8) 0.4943(17) 0.256(2) 0.082(7) Uani 1 1 d . . . C22B C 0.4642(7) 0.505(2) 0.166(2) 0.097(8) Uani 1 1 d . . . H22B H 0.4737 0.4547 0.1320 0.116 Uiso 1 1 calc R . . C23B C 0.4725(8) 0.592(3) 0.127(2) 0.103(9) Uani 1 1 d . . . H23B H 0.4879 0.5990 0.0693 0.124 Uiso 1 1 calc R . . C24B C 0.4576(9) 0.665(2) 0.177(3) 0.113(9) Uani 1 1 d . . . H24B H 0.4613 0.7230 0.1503 0.135 Uiso 1 1 calc R . . C25B C 0.4371(8) 0.6521(18) 0.265(3) 0.099(8) Uani 1 1 d . . . H25B H 0.4291 0.7031 0.3015 0.118 Uiso 1 1 calc R . . C26B C 0.4271(6) 0.570(2) 0.306(2) 0.097(8) Uani 1 1 d . . . H26B H 0.4115 0.5650 0.3639 0.116 Uiso 1 1 calc R . . P3 P 0.31847(17) 0.4597(4) 0.3519(5) 0.080(2) Uani 1 1 d . . . C31A C 0.3250(7) 0.5722(18) 0.406(3) 0.089(8) Uani 1 1 d . . . C32A C 0.3330(7) 0.650(3) 0.348(3) 0.131(11) Uani 1 1 d . . . H32A H 0.3353 0.6415 0.2749 0.158 Uiso 1 1 calc R . . C33A C 0.3379(12) 0.735(3) 0.384(4) 0.163(18) Uani 1 1 d . . . H33A H 0.3397 0.7834 0.3372 0.195 Uiso 1 1 calc R . . C34A C 0.3401(10) 0.748(2) 0.492(5) 0.17(2) Uani 1 1 d . . . H34A H 0.3474 0.8037 0.5211 0.203 Uiso 1 1 calc R . . C35A C 0.3315(7) 0.676(3) 0.560(3) 0.146(14) Uani 1 1 d . . . H35A H 0.3300 0.6843 0.6332 0.175 Uiso 1 1 calc R . . C36A C 0.3253(7) 0.5904(17) 0.508(3) 0.095(8) Uani 1 1 d . . . H36A H 0.3209 0.5420 0.5528 0.114 Uiso 1 1 calc R . . C31B C 0.3033(9) 0.4733(12) 0.212(2) 0.076(6) Uani 1 1 d . . . C32B C 0.2638(11) 0.4643(17) 0.166(3) 0.136(12) Uani 1 1 d . . . H32B H 0.2441 0.4473 0.2110 0.164 Uiso 1 1 calc R . . C33B C 0.2507(10) 0.478(2) 0.059(3) 0.143(11) Uani 1 1 d . . . H33B H 0.2231 0.4705 0.0339 0.172 Uiso 1 1 calc R . . C34B C 0.2784(13) 0.504(2) -0.011(2) 0.130(10) Uani 1 1 d . . . H34B H 0.2710 0.5145 -0.0843 0.156 Uiso 1 1 calc R . . C35B C 0.3197(11) 0.5138(19) 0.039(4) 0.128(10) Uani 1 1 d . . . H35B H 0.3396 0.5338 -0.0033 0.154 Uiso 1 1 calc R . . C36B C 0.3320(9) 0.4961(16) 0.144(3) 0.099(8) Uani 1 1 d . . . H36B H 0.3598 0.4992 0.1693 0.118 Uiso 1 1 calc R . . C3 C 0.2710(6) 0.4288(15) 0.4110(17) 0.084(7) Uani 1 1 d . . . H3A H 0.2727 0.4499 0.4851 0.101 Uiso 1 1 calc R . . H3B H 0.2476 0.4582 0.3708 0.101 Uiso 1 1 calc R . . C4 C 0.2642(5) 0.3265(13) 0.4086(18) 0.079(7) Uani 1 1 d . . . H4A H 0.2592 0.3060 0.3343 0.095 Uiso 1 1 calc R . . H4B H 0.2402 0.3116 0.4451 0.095 Uiso 1 1 calc R . . P4 P 0.30956(18) 0.2702(4) 0.4756(5) 0.0772(19) Uani 1 1 d . . . C41A C 0.2980(8) 0.1552(14) 0.438(2) 0.079(7) Uani 1 1 d . . . C42A C 0.2692(7) 0.118(2) 0.358(2) 0.096(8) Uani 1 1 d . . . H42A H 0.2511 0.1578 0.3205 0.115 Uiso 1 1 calc R . . C43A C 0.2652(9) 0.031(2) 0.332(2) 0.096(9) Uani 1 1 d . . . H43A H 0.2441 0.0124 0.2809 0.116 Uiso 1 1 calc R . . C44A C 0.2920(10) -0.0279(18) 0.380(3) 0.107(10) Uani 1 1 d . . . H44A H 0.2903 -0.0879 0.3590 0.128 Uiso 1 1 calc R . . C45A C 0.3231(11) -0.002(2) 0.463(3) 0.134(10) Uani 1 1 d . . . H45A H 0.3413 -0.0434 0.4973 0.161 Uiso 1 1 calc R . . C46A C 0.3252(9) 0.091(2) 0.492(2) 0.119(9) Uani 1 1 d . . . H46A H 0.3448 0.1101 0.5466 0.142 Uiso 1 1 calc R . . C41B C 0.3010(7) 0.2783(18) 0.614(2) 0.090(8) Uani 1 1 d . . . C42B C 0.3173(7) 0.3447(18) 0.688(3) 0.101(8) Uani 1 1 d . . . H42B H 0.3343 0.3884 0.6628 0.122 Uiso 1 1 calc R . . C43B C 0.3103(9) 0.350(2) 0.795(2) 0.112(10) Uani 1 1 d . . . H43B H 0.3241 0.3909 0.8430 0.134 Uiso 1 1 calc R . . C44B C 0.2803(9) 0.288(3) 0.828(3) 0.132(11) Uani 1 1 d . . . H44B H 0.2714 0.2922 0.8968 0.159 Uiso 1 1 calc R . . C45B C 0.2656(10) 0.2254(19) 0.760(3) 0.128(13) Uani 1 1 d . . . H45B H 0.2480 0.1835 0.7864 0.154 Uiso 1 1 calc R . . C46B C 0.2728(8) 0.2149(19) 0.659(2) 0.109(9) Uani 1 1 d . . . H46B H 0.2603 0.1686 0.6166 0.131 Uiso 1 1 calc R . . N5 N 0.4004(7) 0.2096(13) 0.4008(18) 0.094(7) Uani 1 1 d . . . C51 C 0.4175(8) 0.140(3) 0.409(2) 0.103(10) Uani 1 1 d . . . N52 N 0.4383(7) 0.0634(13) 0.4072(19) 0.124(9) Uani 1 1 d . . . N6 N 0.3391(7) 0.2850(15) 0.255(2) 0.109(9) Uani 1 1 d . . . C61 C 0.3249(10) 0.2386(18) 0.194(4) 0.114(13) Uani 1 1 d . . . N62 N 0.3056(7) 0.1878(19) 0.107(2) 0.143(10) Uani 1 1 d . . . H7 H 0.362(3) 0.332(8) 0.528(10) 0.04(4) Uiso 1 1 d . . . H8 H 0.426(4) 0.357(9) 0.448(12) 0.06(5) Uiso 1 1 d . . . B9 B 0.1896(6) 0.2369(15) 0.1183(18) 0.22(3) Uiso 1 1 d D . . F91 F 0.1577(7) 0.236(2) 0.044(2) 0.37(2) Uani 1 1 d D . . F92 F 0.1884(9) 0.1628(15) 0.1765(19) 0.293(14) Uani 1 1 d D . . F93 F 0.2237(7) 0.2382(19) 0.070(2) 0.311(16) Uani 1 1 d D . . F94 F 0.1885(10) 0.3092(16) 0.180(3) 0.41(3) Uani 1 1 d D . . B10 B 0.0563(14) 0.346(4) 0.435(4) 0.132(12) Uiso 1 1 d . . . F101 F 0.0566(5) 0.2670(12) 0.468(2) 0.209(10) Uani 1 1 d . . . F102 F 0.0215(5) 0.3917(13) 0.4114(19) 0.204(9) Uani 1 1 d . . . F103 F 0.0760(10) 0.349(2) 0.347(2) 0.295(16) Uani 1 1 d . . . F104 F 0.0807(7) 0.4032(15) 0.496(3) 0.31(2) Uani 1 1 d . . . C111 C 0.415(3) -0.073(6) 0.029(8) 0.27(4) Uiso 0.60 1 d P . . C112 C 0.3745(14) -0.003(3) -0.003(4) 0.211(16) Uiso 1 1 d . . . O113 O 0.3521(10) 0.032(2) 0.083(3) 0.254(13) Uiso 1 1 d . . . C114 C 0.368(6) -0.186(13) 0.243(15) 0.28(8) Uiso 0.30 1 d P . . C115 C 0.388(2) -0.101(5) 0.150(5) 0.22(2) Uiso 0.75 1 d P . . C116 C 0.411(3) -0.020(6) 0.137(7) 0.26(3) Uiso 0.65 1 d P . . C117 C 0.3540(19) -0.033(5) 0.174(5) 0.21(2) Uiso 0.70 1 d P . . C121 C 0.086(3) 0.334(7) 0.133(8) 0.27(4) Uiso 0.50 1 d P . . C123 C 0.1515(17) 0.425(4) 0.268(4) 0.26(2) Uiso 0.90 1 d P . . 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 Mo 0.0678(13) 0.0530(13) 0.0905(17) 0.0031(11) 0.0029(10) -0.0015(9) P1 0.079(4) 0.058(4) 0.083(5) 0.005(4) 0.013(3) -0.003(3) C11A 0.10(2) 0.056(17) 0.078(18) 0.008(13) 0.028(14) -0.026(16) C12A 0.085(19) 0.08(2) 0.13(2) -0.017(18) 0.023(15) 0.023(15) C13A 0.14(3) 0.049(18) 0.13(2) -0.023(17) -0.01(2) 0.048(19) C14A 0.23(4) 0.059(19) 0.08(2) 0.003(14) 0.00(2) -0.09(3) C15A 0.042(15) 0.19(4) 0.16(3) -0.06(3) 0.033(16) -0.017(18) C16A 0.24(5) 0.031(16) 0.14(3) 0.026(17) -0.04(3) 0.03(2) C11B 0.072(15) 0.10(3) 0.06(2) 0.004(16) -0.013(12) 0.003(13) C12B 0.105(18) 0.053(18) 0.11(2) -0.01(2) -0.025(15) -0.015(13) C13B 0.13(2) 0.031(15) 0.13(3) -0.03(2) -0.045(19) -0.003(13) C14B 0.15(2) 0.08(3) 0.09(3) 0.009(19) 0.029(19) 0.012(17) C15B 0.14(2) 0.08(2) 0.08(2) 0.00(2) -0.022(16) 0.007(17) C16B 0.099(17) 0.048(16) 0.10(3) -0.01(2) -0.005(16) 0.000(12) C1 0.055(12) 0.067(14) 0.070(17) 0.000(12) -0.003(11) 0.014(10) C2 0.066(13) 0.052(13) 0.094(18) 0.008(13) 0.014(12) -0.019(10) P2 0.072(4) 0.067(4) 0.088(5) 0.000(3) 0.016(3) -0.005(3) C21A 0.09(2) 0.09(2) 0.11(3) 0.021(17) 0.02(2) -0.011(18) C22A 0.088(19) 0.069(19) 0.10(2) 0.013(19) 0.04(2) -0.007(13) C23A 0.19(4) 0.08(2) 0.07(2) -0.040(18) 0.01(2) -0.02(2) C24A 0.20(4) 0.12(2) 0.08(3) -0.03(2) 0.02(3) 0.04(3) C25A 0.17(3) 0.19(4) 0.12(3) 0.03(3) 0.06(3) 0.09(3) C26A 0.11(2) 0.12(2) 0.13(3) 0.00(2) 0.04(2) 0.02(2) C21B 0.097(17) 0.07(2) 0.08(2) -0.008(15) 0.004(15) -0.025(15) C22B 0.086(16) 0.11(3) 0.10(2) -0.017(18) 0.021(16) 0.005(15) C23B 0.11(2) 0.10(2) 0.10(2) 0.03(2) 0.033(16) -0.056(19) C24B 0.14(2) 0.07(2) 0.13(3) 0.00(2) 0.03(2) 0.000(18) C25B 0.13(2) 0.05(2) 0.11(2) -0.008(17) 0.021(18) -0.023(15) C26B 0.081(16) 0.07(2) 0.14(2) -0.01(2) 0.014(15) -0.011(15) P3 0.074(4) 0.054(4) 0.109(6) 0.005(4) 0.004(4) 0.005(3) C31A 0.074(16) 0.07(2) 0.12(3) 0.00(2) 0.039(17) -0.002(14) C32A 0.061(16) 0.18(4) 0.16(3) -0.06(3) 0.028(17) 0.01(2) C33A 0.17(3) 0.06(3) 0.24(5) -0.02(3) -0.05(4) 0.01(2) C34A 0.09(2) 0.05(2) 0.35(7) -0.03(4) -0.05(3) -0.050(17) C35A 0.047(15) 0.15(3) 0.24(4) -0.11(3) 0.016(19) 0.006(18) C36A 0.093(18) 0.05(2) 0.13(3) -0.016(19) -0.003(18) 0.038(14) C31B 0.107(18) 0.039(13) 0.07(2) -0.010(13) -0.02(2) 0.001(12) C32B 0.18(4) 0.11(2) 0.09(3) -0.002(18) -0.08(2) -0.01(2) C33B 0.12(2) 0.20(4) 0.11(3) 0.00(3) 0.00(3) -0.01(2) C34B 0.14(3) 0.17(3) 0.08(2) 0.00(2) 0.00(2) 0.05(2) C35B 0.11(3) 0.14(3) 0.14(3) 0.03(2) 0.06(2) 0.018(19) C36B 0.14(2) 0.091(19) 0.07(2) 0.041(16) 0.03(2) 0.017(16) C3 0.082(15) 0.10(2) 0.067(16) 0.015(13) -0.009(12) 0.008(13) C4 0.056(13) 0.060(16) 0.12(2) 0.025(13) 0.003(12) -0.012(11) P4 0.088(4) 0.054(4) 0.090(5) 0.004(3) 0.012(4) -0.005(3) C41A 0.076(15) 0.059(16) 0.10(2) 0.042(16) 0.016(15) 0.004(15) C42A 0.074(17) 0.11(3) 0.09(2) 0.005(17) -0.013(15) -0.029(16) C43A 0.12(2) 0.052(18) 0.13(2) -0.04(2) 0.068(19) -0.04(2) C44A 0.10(2) 0.041(18) 0.18(3) -0.01(2) 0.03(2) -0.011(18) C45A 0.16(3) 0.08(3) 0.16(3) 0.00(2) 0.00(2) -0.01(2) C46A 0.15(2) 0.08(2) 0.12(3) -0.05(2) 0.00(2) -0.03(2) C41B 0.079(16) 0.071(17) 0.12(2) 0.036(19) 0.025(16) -0.021(13) C42B 0.097(18) 0.067(18) 0.14(3) 0.014(19) 0.011(19) -0.017(15) C43B 0.14(3) 0.14(3) 0.05(2) -0.042(18) 0.029(17) 0.00(2) C44B 0.09(2) 0.16(3) 0.15(3) 0.04(3) 0.05(2) 0.03(2) C45B 0.21(3) 0.08(2) 0.11(3) -0.025(19) 0.06(2) -0.07(2) C46B 0.14(2) 0.12(2) 0.07(2) 0.026(18) 0.012(17) 0.03(2) N5 0.121(18) 0.047(14) 0.111(18) -0.011(13) 0.001(13) -0.021(12) C51 0.09(2) 0.15(3) 0.071(19) -0.04(2) 0.011(15) -0.06(2) N52 0.15(2) 0.044(13) 0.18(2) -0.007(13) 0.006(16) 0.050(13) N6 0.111(17) 0.039(16) 0.17(3) 0.008(15) -0.008(15) -0.022(13) C61 0.11(3) 0.03(2) 0.22(5) 0.04(2) 0.06(3) -0.004(16) N62 0.125(18) 0.16(2) 0.15(2) -0.067(19) 0.018(15) -0.049(17) F91 0.26(3) 0.36(4) 0.45(5) 0.02(4) -0.17(3) 0.08(3) F92 0.37(4) 0.27(3) 0.24(3) -0.03(3) 0.02(3) 0.01(3) F93 0.24(3) 0.22(3) 0.49(5) -0.01(3) 0.08(3) -0.02(2) F94 0.32(4) 0.21(3) 0.67(8) -0.14(4) -0.07(4) -0.03(3) F101 0.155(15) 0.101(14) 0.36(3) 0.036(16) -0.006(16) -0.016(11) F102 0.096(11) 0.174(17) 0.34(3) 0.064(17) 0.018(14) 0.021(11) F103 0.34(3) 0.33(4) 0.25(3) 0.10(3) 0.17(3) 0.09(3) F104 0.21(2) 0.17(2) 0.52(5) -0.18(3) -0.15(3) 0.082(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 Mo N6 2.19(3) . ? Mo N5 2.20(2) . ? Mo P3 2.476(6) . ? Mo P1 2.483(6) . ? Mo P4 2.503(6) . ? Mo P2 2.506(6) . ? Mo H7 1.61(12) . ? Mo H8 1.84(13) . ? P1 C1 1.817(18) . ? P1 C11A 1.82(2) . ? P1 C11B 1.82(2) . ? P1 H8 1.44(15) . ? C11A C16A 1.35(4) . ? C11A C12A 1.39(3) . ? C12A C13A 1.45(3) . ? C12A H12A 0.9300 . ? C13A C14A 1.34(3) . ? C13A H13A 0.9300 . ? C14A C15A 1.42(4) . ? C14A H14A 0.9300 . ? C15A C16A 1.29(4) . ? C15A H15A 0.9300 . ? C16A H16A 0.9300 . ? C11B C16B 1.36(3) . ? C11B C12B 1.42(3) . ? C12B C13B 1.41(3) . ? C12B H12B 0.9300 . ? C13B C14B 1.34(3) . ? C13B H13B 0.9300 . ? C14B C15B 1.30(3) . ? C14B H14B 0.9300 . ? C15B C16B 1.37(3) . ? C15B H15B 0.9300 . ? C16B H16B 0.9300 . ? C1 C2 1.51(2) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 P2 1.81(2) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? P2 C21A 1.83(3) . ? P2 C21B 1.87(2) . ? P2 H8 1.84(15) . ? C21A C26A 1.33(3) . ? C21A C22A 1.42(3) . ? C22A C23A 1.32(3) . ? C22A H22A 0.9300 . ? C23A C24A 1.38(4) . ? C23A H23A 0.9300 . ? C24A C25A 1.28(4) . ? C24A H24A 0.9300 . ? C25A C26A 1.41(4) . ? C25A H25A 0.9300 . ? C26A H26A 0.9300 . ? C21B C26B 1.38(3) . ? C21B C22B 1.42(3) . ? C22B C23B 1.41(3) . ? C22B H22B 0.9300 . ? C23B C24B 1.36(3) . ? C23B H23B 0.9300 . ? C24B C25B 1.36(3) . ? C24B H24B 0.9300 . ? C25B C26B 1.37(3) . ? C25B H25B 0.9300 . ? C26B H26B 0.9300 . ? P3 C31B 1.77(2) . ? P3 C31A 1.80(3) . ? P3 C3 1.84(2) . ? C31A C36A 1.30(3) . ? C31A C32A 1.39(4) . ? C32A C33A 1.35(4) . ? C32A H32A 0.9300 . ? C33A C34A 1.34(5) . ? C33A H33A 0.9300 . ? C34A C35A 1.40(5) . ? C34A H34A 0.9300 . ? C35A C36A 1.43(4) . ? C35A H35A 0.9300 . ? C36A H36A 0.9300 . ? C31B C32B 1.36(3) . ? C31B C36B 1.37(3) . ? C32B C33B 1.37(3) . ? C32B H32B 0.9300 . ? C33B C34B 1.38(4) . ? C33B H33B 0.9300 . ? C34B C35B 1.43(4) . ? C34B H34B 0.9300 . ? C35B C36B 1.34(4) . ? C35B H35B 0.9300 . ? C36B H36B 0.9300 . ? C3 C4 1.54(3) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 P4 1.823(19) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? P4 C41B 1.78(3) . ? P4 C41A 1.80(2) . ? C41A C42A 1.40(3) . ? C41A C46A 1.42(3) . ? C42A C43A 1.33(3) . ? C42A H42A 0.9300 . ? C43A C44A 1.34(3) . ? C43A H43A 0.9300 . ? C44A C45A 1.42(3) . ? C44A H44A 0.9300 . ? C45A C46A 1.42(3) . ? C45A H45A 0.9300 . ? C46A H46A 0.9300 . ? C41B C42B 1.42(3) . ? C41B C46B 1.47(3) . ? C42B C43B 1.38(3) . ? C42B H42B 0.9300 . ? C43B C44B 1.43(3) . ? C43B H43B 0.9300 . ? C44B C45B 1.32(4) . ? C44B H44B 0.9300 . ? C45B C46B 1.31(3) . ? C45B H45B 0.9300 . ? C46B H46B 0.9300 . ? N5 C51 1.17(4) . ? C51 N52 1.33(4) . ? N6 C61 1.09(4) . ? C61 N62 1.42(4) . ? B9 F93 1.316(10) . ? B9 F91 1.320(10) . ? B9 F92 1.320(10) . ? B9 F94 1.321(10) . ? B10 F101 1.24(5) . ? B10 F103 1.33(4) . ? B10 F102 1.33(4) . ? B10 F104 1.35(4) . ? C111 C116 1.58(10) . ? C111 C112 1.70(9) . ? C111 C115 1.88(10) . ? C112 O113 1.45(4) . ? C112 C116 2.01(9) . ? O113 C117 1.49(6) . ? C114 C115 1.87(19) . ? C115 C116 1.43(9) . ? C115 C117 1.54(7) . ? C116 C117 1.95(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Mo N5 79.0(8) . . ? N6 Mo P3 78.8(6) . . ? N5 Mo P3 157.1(6) . . ? N6 Mo P1 157.4(6) . . ? N5 Mo P1 79.0(6) . . ? P3 Mo P1 123.6(2) . . ? N6 Mo P4 79.6(7) . . ? N5 Mo P4 89.7(6) . . ? P3 Mo P4 81.0(2) . . ? P1 Mo P4 105.1(2) . . ? N6 Mo P2 89.2(7) . . ? N5 Mo P2 78.8(6) . . ? P3 Mo P2 106.2(2) . . ? P1 Mo P2 81.7(2) . . ? P4 Mo P2 165.4(2) . . ? N6 Mo H7 132(4) . . ? N5 Mo H7 94(4) . . ? P3 Mo H7 97(4) . . ? P1 Mo H7 55(4) . . ? P4 Mo H7 52(4) . . ? P2 Mo H7 137(4) . . ? N6 Mo H8 131(5) . . ? N5 Mo H8 72(4) . . ? P3 Mo H8 128(4) . . ? P1 Mo H8 35(5) . . ? P4 Mo H8 137(5) . . ? P2 Mo H8 47(5) . . ? H7 Mo H8 90(6) . . ? C1 P1 C11A 104.3(10) . . ? C1 P1 C11B 99.4(11) . . ? C11A P1 C11B 104.1(13) . . ? C1 P1 Mo 106.4(7) . . ? C11A P1 Mo 117.8(8) . . ? C11B P1 Mo 122.0(8) . . ? C1 P1 H8 60(5) . . ? C11A P1 H8 117(6) . . ? C11B P1 H8 137(6) . . ? Mo P1 H8 47(5) . . ? C16A C11A C12A 120(2) . . ? C16A C11A P1 114(2) . . ? C12A C11A P1 126(2) . . ? C11A C12A C13A 118(2) . . ? C11A C12A H12A 121.1 . . ? C13A C12A H12A 121.1 . . ? C14A C13A C12A 120(2) . . ? C14A C13A H13A 119.9 . . ? C12A C13A H13A 119.9 . . ? C13A C14A C15A 117(3) . . ? C13A C14A H14A 121.4 . . ? C15A C14A H14A 121.3 . . ? C16A C15A C14A 123(3) . . ? C16A C15A H15A 118.5 . . ? C14A C15A H15A 118.5 . . ? C15A C16A C11A 121(3) . . ? C15A C16A H16A 119.3 . . ? C11A C16A H16A 119.3 . . ? C16B C11B C12B 116(2) . . ? C16B C11B P1 125(2) . . ? C12B C11B P1 119(2) . . ? C13B C12B C11B 116(2) . . ? C13B C12B H12B 122.2 . . ? C11B C12B H12B 122.3 . . ? C14B C13B C12B 125(2) . . ? C14B C13B H13B 117.6 . . ? C12B C13B H13B 117.6 . . ? C15B C14B C13B 119(3) . . ? C15B C14B H14B 120.5 . . ? C13B C14B H14B 120.5 . . ? C14B C15B C16B 120(3) . . ? C14B C15B H15B 120.2 . . ? C16B C15B H15B 120.1 . . ? C11B C16B C15B 125(2) . . ? C11B C16B H16B 117.6 . . ? C15B C16B H16B 117.6 . . ? C2 C1 P1 112.2(13) . . ? C2 C1 H1A 109.2 . . ? P1 C1 H1A 109.2 . . ? C2 C1 H1B 109.2 . . ? P1 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? C1 C2 P2 111.4(13) . . ? C1 C2 H2A 109.3 . . ? P2 C2 H2A 109.3 . . ? C1 C2 H2B 109.3 . . ? P2 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? C2 P2 C21A 103.6(15) . . ? C2 P2 C21B 101.9(9) . . ? C21A P2 C21B 103.8(12) . . ? C2 P2 Mo 104.9(7) . . ? C21A P2 Mo 118.2(8) . . ? C21B P2 Mo 121.8(10) . . ? C2 P2 H8 59(4) . . ? C21A P2 H8 135(4) . . ? C21B P2 H8 120(4) . . ? Mo P2 H8 47(4) . . ? C26A C21A C22A 117(3) . . ? C26A C21A P2 124(3) . . ? C22A C21A P2 119(3) . . ? C23A C22A C21A 121(3) . . ? C23A C22A H22A 119.7 . . ? C21A C22A H22A 119.7 . . ? C22A C23A C24A 122(3) . . ? C22A C23A H23A 118.8 . . ? C24A C23A H23A 118.8 . . ? C25A C24A C23A 116(3) . . ? C25A C24A H24A 122.2 . . ? C23A C24A H24A 122.2 . . ? C24A C25A C26A 126(3) . . ? C24A C25A H25A 117.0 . . ? C26A C25A H25A 117.0 . . ? C21A C26A C25A 118(3) . . ? C21A C26A H26A 121.0 . . ? C25A C26A H26A 121.0 . . ? C26B C21B C22B 119(2) . . ? C26B C21B P2 122(2) . . ? C22B C21B P2 119(2) . . ? C23B C22B C21B 120(2) . . ? C23B C22B H22B 119.8 . . ? C21B C22B H22B 119.8 . . ? C24B C23B C22B 119(2) . . ? C24B C23B H23B 120.4 . . ? C22B C23B H23B 120.4 . . ? C23B C24B C25B 118(3) . . ? C23B C24B H24B 120.8 . . ? C25B C24B H24B 120.7 . . ? C24B C25B C26B 125(3) . . ? C24B C25B H25B 117.3 . . ? C26B C25B H25B 117.3 . . ? C25B C26B C21B 117(2) . . ? C25B C26B H26B 121.5 . . ? C21B C26B H26B 121.5 . . ? C31B P3 C31A 105.6(13) . . ? C31B P3 C3 105.1(12) . . ? C31A P3 C3 98.9(12) . . ? C31B P3 Mo 116.7(8) . . ? C31A P3 Mo 120.5(9) . . ? C3 P3 Mo 107.7(7) . . ? C36A C31A C32A 110(3) . . ? C36A C31A P3 123(2) . . ? C32A C31A P3 127(3) . . ? C33A C32A C31A 129(3) . . ? C33A C32A H32A 115.6 . . ? C31A C32A H32A 115.6 . . ? C34A C33A C32A 117(4) . . ? C34A C33A H33A 121.6 . . ? C32A C33A H33A 121.6 . . ? C33A C34A C35A 120(3) . . ? C33A C34A H34A 119.8 . . ? C35A C34A H34A 119.9 . . ? C34A C35A C36A 115(3) . . ? C34A C35A H35A 122.2 . . ? C36A C35A H35A 122.3 . . ? C31A C36A C35A 128(3) . . ? C31A C36A H36A 116.2 . . ? C35A C36A H36A 116.2 . . ? C32B C31B C36B 116(3) . . ? C32B C31B P3 124(3) . . ? C36B C31B P3 120(2) . . ? C31B C32B C33B 125(3) . . ? C31B C32B H32B 117.4 . . ? C33B C32B H32B 117.3 . . ? C32B C33B C34B 120(3) . . ? C32B C33B H33B 120.0 . . ? C34B C33B H33B 119.9 . . ? C33B C34B C35B 114(3) . . ? C33B C34B H34B 123.2 . . ? C35B C34B H34B 123.2 . . ? C36B C35B C34B 125(3) . . ? C36B C35B H35B 117.4 . . ? C34B C35B H35B 117.5 . . ? C35B C36B C31B 120(3) . . ? C35B C36B H36B 120.2 . . ? C31B C36B H36B 120.1 . . ? C4 C3 P3 111.4(14) . . ? C4 C3 H3A 109.4 . . ? P3 C3 H3A 109.4 . . ? C4 C3 H3B 109.4 . . ? P3 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? C3 C4 P4 109.7(13) . . ? C3 C4 H4A 109.7 . . ? P4 C4 H4A 109.7 . . ? C3 C4 H4B 109.7 . . ? P4 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C41B P4 C41A 105.4(12) . . ? C41B P4 C4 102.0(10) . . ? C41A P4 C4 100.3(11) . . ? C41B P4 Mo 121.9(9) . . ? C41A P4 Mo 117.6(7) . . ? C4 P4 Mo 106.3(6) . . ? C42A C41A C46A 114(2) . . ? C42A C41A P4 131(2) . . ? C46A C41A P4 114(2) . . ? C43A C42A C41A 127(3) . . ? C43A C42A H42A 116.7 . . ? C41A C42A H42A 116.7 . . ? C42A C43A C44A 119(3) . . ? C42A C43A H43A 120.6 . . ? C44A C43A H43A 120.5 . . ? C43A C44A C45A 122(3) . . ? C43A C44A H44A 119.1 . . ? C45A C44A H44A 119.1 . . ? C46A C45A C44A 117(3) . . ? C46A C45A H45A 121.4 . . ? C44A C45A H45A 121.4 . . ? C45A C46A C41A 122(3) . . ? C45A C46A H46A 119.3 . . ? C41A C46A H46A 119.2 . . ? C42B C41B C46B 114(2) . . ? C42B C41B P4 126(2) . . ? C46B C41B P4 119(2) . . ? C43B C42B C41B 126(2) . . ? C43B C42B H42B 117.2 . . ? C41B C42B H42B 117.2 . . ? C42B C43B C44B 115(3) . . ? C42B C43B H43B 122.3 . . ? C44B C43B H43B 122.3 . . ? C45B C44B C43B 119(3) . . ? C45B C44B H44B 120.6 . . ? C43B C44B H44B 120.6 . . ? C46B C45B C44B 128(3) . . ? C46B C45B H45B 116.1 . . ? C44B C45B H45B 116.1 . . ? C45B C46B C41B 118(3) . . ? C45B C46B H46B 121.0 . . ? C41B C46B H46B 121.0 . . ? C51 N5 Mo 174(2) . . ? N5 C51 N52 174(3) . . ? C61 N6 Mo 163(3) . . ? N6 C61 N62 173(3) . . ? F93 B9 F91 108.8(15) . . ? F93 B9 F92 109.7(15) . . ? F91 B9 F92 108.0(15) . . ? F93 B9 F94 109.1(15) . . ? F91 B9 F94 110.4(15) . . ? F92 B9 F94 110.8(15) . . ? F101 B10 F103 109(4) . . ? F101 B10 F102 122(4) . . ? F103 B10 F102 106(4) . . ? F101 B10 F104 115(4) . . ? F103 B10 F104 97(4) . . ? F102 B10 F104 104(4) . . ? C116 C111 C112 76(5) . . ? C116 C111 C115 48(4) . . ? C112 C111 C115 84(5) . . ? O113 C112 C111 119(5) . . ? O113 C112 C116 73(3) . . ? C111 C112 C116 50(4) . . ? C112 O113 C117 110(4) . . ? C116 C115 C117 82(6) . . ? C116 C115 C114 148(9) . . ? C117 C115 C114 92(7) . . ? C116 C115 C111 55(5) . . ? C117 C115 C111 115(6) . . ? C114 C115 C111 150(8) . . ? C115 C116 C111 77(6) . . ? C115 C116 C117 51(4) . . ? C111 C116 C117 109(6) . . ? C115 C116 C112 86(5) . . ? C111 C116 C112 55(4) . . ? C117 C116 C112 75(4) . . ? O113 C117 C115 105(5) . . ? O113 C117 C116 74(4) . . ? C115 C117 C116 46(4) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 17.98 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.444 _refine_diff_density_min -0.371 _refine_diff_density_rms 0.098