# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_[MoCl3(tBuANA)] #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C23 H43 As2 Cl3 Mo N' _chemical_formula_moiety 'C23 H43 As2 Cl3 Mo N' _chemical_formula_weight 685.74 _chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk' #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C 2 2 21' _symmetry_space_group_name_Hall 'C 2c 2' _symmetry_Int_Tables_number 20 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 +X,-Y,-Z 3 -X,+Y,1/2-Z 4 -X,-Y,1/2+Z 5 1/2+X,1/2+Y,+Z 6 1/2+X,1/2-Y,-Z 7 1/2-X,1/2+Y,1/2-Z 8 1/2-X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 16.6959(3) _cell_length_b 25.6652(5) _cell_length_c 13.6023(3) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 5828.64(19) _cell_formula_units_Z 8 _cell_measurement_reflns_used 26449 _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 27.48 _cell_measurement_temperature 198 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.410 _exptl_crystal_size_mid 0.310 _exptl_crystal_size_min 0.170 _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2776.00 _exptl_absorpt_coefficient_mu 2.990 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR (Rigaku, 1995)' _exptl_absorpt_correction_T_min 0.409 _exptl_absorpt_correction_T_max 0.602 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 198 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_reflns_number 27848 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measured_fraction_theta_full 0.987 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_standards_number 0 _diffrn_standards_interval_count . #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6582 _reflns_number_gt 6302 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0191 _refine_ls_wR_factor_ref 0.0395 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 6582 _refine_ls_number_parameters 324 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[1.6400\s(Fo^2^)]/(4Fo^2^)' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_diff_density_max 1.320 _refine_diff_density_min -0.778 _refine_ls_extinction_method none _refine_ls_abs_structure_details 'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 2952 Friedel Pairs' _refine_ls_abs_structure_Flack 0.030(5) 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 for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.1484 0.1585 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; As As 0.0499 2.0058 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Mo Mo -1.6832 0.6857 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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(1) Mo 0.196620(10) 0.5000 1.0000 0.02011(7) Uani 1.0 4 d . . . Mo(2) Mo 0.5000 0.284510(10) 0.7500 0.02012(7) Uani 1.0 4 d . . . As(1) As 0.231030(10) 0.484260(10) 0.811540(10) 0.02399(6) Uani 1.0 8 d . . . As(2) As 0.511530(10) 0.266050(10) 0.55924(2) 0.02454(6) Uani 1.0 8 d . . . Cl(1) Cl 0.05298(4) 0.5000 1.0000 0.0340(3) Uani 1.0 4 d . . . Cl(2) Cl 0.19948(4) 0.40691(2) 1.02558(4) 0.03201(17) Uani 1.0 8 d . . . Cl(3) Cl 0.5000 0.37790(3) 0.7500 0.0388(3) Uani 1.0 4 d . . . Cl(4) Cl 0.35586(3) 0.28127(3) 0.73578(4) 0.03574(17) Uani 1.0 8 d . . . N(1) N 0.33070(14) 0.5000 1.0000 0.0236(7) Uani 1.0 4 d . . . N(2) N 0.5000 0.19850(10) 0.7500 0.0244(7) Uani 1.0 4 d . . . C(1) C 0.37254(13) 0.47357(9) 0.92996(15) 0.0272(7) Uani 1.0 8 d . . . C(2) C 0.45442(14) 0.47313(11) 0.92916(16) 0.0369(8) Uani 1.0 8 d . . . C(3) C 0.4970(2) 0.500000(10) 1.000000(10) 0.0408(11) Uani 1.0 4 d . . . C(4) C 0.32646(13) 0.44555(10) 0.84973(14) 0.0288(7) Uani 1.0 8 d . . . C(5) C 0.17289(15) 0.43293(10) 0.72531(15) 0.0343(8) Uani 1.0 8 d . . . C(6) C 0.12794(17) 0.39590(12) 0.79386(18) 0.0525(10) Uani 1.0 8 d . . . C(7) C 0.11358(17) 0.46161(13) 0.6599(2) 0.0581(10) Uani 1.0 8 d . . . C(8) C 0.23089(16) 0.40133(11) 0.66173(18) 0.0444(9) Uani 1.0 8 d . . . C(9) C 0.27586(15) 0.54252(10) 0.72800(15) 0.0341(7) Uani 1.0 8 d . . . C(10) C 0.34246(16) 0.56962(11) 0.78631(17) 0.0441(9) Uani 1.0 8 d . . . C(11) C 0.20934(16) 0.58181(11) 0.70722(18) 0.0460(9) Uani 1.0 8 d . . . C(12) C 0.31237(18) 0.52192(12) 0.63252(16) 0.0508(9) Uani 1.0 8 d . . . C(13) C 0.47855(13) 0.17111(10) 0.66795(15) 0.0264(7) Uani 1.0 8 d . . . C(14) C 0.47938(14) 0.11772(10) 0.66672(17) 0.0361(8) Uani 1.0 8 d . . . C(15) C 0.500000(10) 0.09062(14) 0.750000(10) 0.0404(11) Uani 1.0 4 d . . . C(16) C 0.45165(15) 0.20117(10) 0.57691(16) 0.0325(7) Uani 1.0 8 d . . . C(17) C 0.44663(15) 0.30575(11) 0.45863(16) 0.0372(8) Uani 1.0 8 d . . . C(18) C 0.38073(15) 0.33405(12) 0.51417(17) 0.0455(9) Uani 1.0 8 d . . . C(19) C 0.5008(2) 0.34715(11) 0.41103(18) 0.0511(9) Uani 1.0 8 d . . . C(20) C 0.40907(18) 0.26940(13) 0.38247(17) 0.0565(10) Uani 1.0 8 d . . . C(21) C 0.61537(14) 0.24322(10) 0.49711(17) 0.0333(7) Uani 1.0 8 d . . . C(22) C 0.67456(15) 0.28845(11) 0.50164(19) 0.0456(8) Uani 1.0 8 d . . . C(23) C 0.60449(19) 0.22505(12) 0.39076(16) 0.0510(10) Uani 1.0 8 d . . . C(24) C 0.64712(15) 0.19730(10) 0.55674(18) 0.0376(8) Uani 1.0 8 d . . . H(1) H 0.4816 0.4547 0.8807 0.0444 Uiso 1.0 8 calc R . . H(2) H 0.5527 0.5000 1.0000 0.0491 Uiso 1.0 4 calc R . . H(3) H 0.3213 0.4118 0.8813 0.0348 Uiso 1.0 8 calc R . . H(4) H 0.3699 0.4408 0.8032 0.0351 Uiso 1.0 8 calc R . . H(5) H 0.0985 0.3710 0.7555 0.0630 Uiso 1.0 8 calc R . . H(6) H 0.1656 0.3779 0.8350 0.0626 Uiso 1.0 8 calc R . . H(7) H 0.0915 0.4154 0.8342 0.0630 Uiso 1.0 8 calc R . . H(8) H 0.0771 0.4812 0.7000 0.0701 Uiso 1.0 8 calc R . . H(9) H 0.1420 0.4849 0.6170 0.0696 Uiso 1.0 8 calc R . . H(10) H 0.0841 0.4368 0.6213 0.0696 Uiso 1.0 8 calc R . . H(11) H 0.2595 0.4243 0.6185 0.0538 Uiso 1.0 8 calc R . . H(12) H 0.2683 0.3833 0.7033 0.0537 Uiso 1.0 8 calc R . . H(13) H 0.2013 0.3765 0.6235 0.0534 Uiso 1.0 8 calc R . . H(14) H 0.3211 0.5825 0.8472 0.0530 Uiso 1.0 8 calc R . . H(15) H 0.3846 0.5452 0.7997 0.0531 Uiso 1.0 8 calc R . . H(16) H 0.3634 0.5981 0.7486 0.0530 Uiso 1.0 8 calc R . . H(17) H 0.1679 0.5654 0.6694 0.0551 Uiso 1.0 8 calc R . . H(18) H 0.1875 0.5941 0.7682 0.0553 Uiso 1.0 8 calc R . . H(19) H 0.2308 0.6107 0.6709 0.0550 Uiso 1.0 8 calc R . . H(20) H 0.3345 0.5504 0.5957 0.0608 Uiso 1.0 8 calc R . . H(21) H 0.3540 0.4974 0.6476 0.0607 Uiso 1.0 8 calc R . . H(22) H 0.2716 0.5051 0.5942 0.0608 Uiso 1.0 8 calc R . . H(23) H 0.4660 0.0999 0.6095 0.0434 Uiso 1.0 8 calc R . . H(24) H 0.5000 0.0544 0.7500 0.0484 Uiso 1.0 4 calc R . . H(25) H 0.3947 0.2023 0.5910 0.0391 Uiso 1.0 8 calc R . . H(26) H 0.4569 0.1733 0.5292 0.0391 Uiso 1.0 8 calc R . . H(27) H 0.3471 0.3091 0.5468 0.0544 Uiso 1.0 8 calc R . . H(28) H 0.4043 0.3569 0.5620 0.0547 Uiso 1.0 8 calc R . . H(29) H 0.3492 0.3541 0.4688 0.0548 Uiso 1.0 8 calc R . . H(30) H 0.5234 0.3689 0.4613 0.0613 Uiso 1.0 8 calc R . . H(31) H 0.5431 0.3303 0.3753 0.0613 Uiso 1.0 8 calc R . . H(32) H 0.4697 0.3681 0.3668 0.0611 Uiso 1.0 8 calc R . . H(33) H 0.3776 0.2894 0.3371 0.0680 Uiso 1.0 8 calc R . . H(34) H 0.4506 0.2515 0.3473 0.0678 Uiso 1.0 8 calc R . . H(35) H 0.3754 0.2445 0.4150 0.0676 Uiso 1.0 8 calc R . . H(36) H 0.7251 0.2776 0.4750 0.0545 Uiso 1.0 8 calc R . . H(37) H 0.6542 0.3172 0.4640 0.0544 Uiso 1.0 8 calc R . . H(38) H 0.6816 0.2991 0.5688 0.0549 Uiso 1.0 8 calc R . . H(39) H 0.5670 0.1967 0.3889 0.0611 Uiso 1.0 8 calc R . . H(40) H 0.5845 0.2534 0.3517 0.0614 Uiso 1.0 8 calc R . . H(41) H 0.6551 0.2137 0.3649 0.0612 Uiso 1.0 8 calc R . . H(42) H 0.6541 0.2077 0.6240 0.0451 Uiso 1.0 8 calc R . . H(43) H 0.6096 0.1690 0.5536 0.0453 Uiso 1.0 8 calc R . . H(44) H 0.6976 0.1863 0.5303 0.0446 Uiso 1.0 8 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mo(1) 0.01849(13) 0.02212(16) 0.01973(12) 0.0000 0.0000 -0.00133(10) Mo(2) 0.02394(14) 0.01640(14) 0.02002(12) 0.0000 0.00096(11) 0.0000 As(1) 0.02212(11) 0.02977(15) 0.02008(10) 0.00110(10) 0.00012(8) -0.00376(9) As(2) 0.02886(13) 0.02438(13) 0.02037(10) 0.00306(10) -0.00037(9) -0.00180(9) Cl(1) 0.0200(4) 0.0383(6) 0.0438(5) 0.0000 0.0000 0.0038(4) Cl(2) 0.0381(4) 0.0234(4) 0.0345(3) 0.0001(3) -0.0001(3) 0.0004(3) Cl(3) 0.0520(6) 0.0179(5) 0.0464(5) 0.0000 0.0094(5) 0.0000 Cl(4) 0.0267(3) 0.0442(4) 0.0363(3) 0.0050(3) -0.0001(3) 0.0067(3) N(1) 0.0188(13) 0.0267(17) 0.0252(13) 0.0000 0.0000 -0.0013(11) N(2) 0.0244(14) 0.0192(15) 0.0296(13) 0.0000 0.0025(12) 0.0000 C(1) 0.0255(12) 0.0318(15) 0.0242(11) 0.0038(11) -0.0011(9) -0.0009(10) C(2) 0.0248(13) 0.0531(18) 0.0328(13) 0.0070(12) 0.0029(10) -0.0119(12) C(3) 0.0202(16) 0.062(3) 0.0398(19) 0.0000 0.0000 -0.0098(17) C(4) 0.0260(12) 0.0353(17) 0.0250(11) 0.0061(11) 0.0014(10) -0.0053(10) C(5) 0.0319(14) 0.0408(17) 0.0302(13) 0.0018(12) -0.0073(10) -0.0146(11) C(6) 0.0494(18) 0.061(3) 0.0472(15) -0.0225(17) 0.0018(13) -0.0222(14) C(7) 0.0443(17) 0.065(3) 0.0648(19) 0.0102(17) -0.0264(15) -0.0243(16) C(8) 0.0483(16) 0.0438(19) 0.0411(14) 0.0005(15) 0.0008(13) -0.0172(12) C(9) 0.0371(14) 0.0395(16) 0.0258(12) -0.0001(13) 0.0057(10) 0.0029(10) C(10) 0.0421(16) 0.0435(19) 0.0468(15) -0.0069(14) 0.0091(12) 0.0084(13) C(11) 0.0541(19) 0.0454(19) 0.0385(14) 0.0079(15) -0.0010(13) 0.0110(12) C(12) 0.061(2) 0.060(3) 0.0312(13) -0.0000(17) 0.0205(13) 0.0041(13) C(13) 0.0232(12) 0.0237(15) 0.0323(12) -0.0018(10) 0.0029(9) -0.0035(10) C(14) 0.0378(15) 0.0263(16) 0.0442(14) -0.0051(12) 0.0059(11) -0.0094(11) C(15) 0.039(2) 0.0170(19) 0.065(3) 0.0000 0.009(2) 0.0000 C(16) 0.0343(15) 0.0312(16) 0.0319(13) -0.0064(12) -0.0022(11) -0.0075(10) C(17) 0.0413(16) 0.0452(18) 0.0250(13) 0.0089(13) -0.0063(11) 0.0040(11) C(18) 0.0437(16) 0.060(2) 0.0329(13) 0.0196(15) -0.0042(12) 0.0104(13) C(19) 0.062(2) 0.0521(19) 0.0389(14) 0.0179(19) 0.0037(14) 0.0180(13) C(20) 0.060(2) 0.075(3) 0.0344(15) 0.0079(19) -0.0179(14) -0.0019(14) C(21) 0.0390(13) 0.0312(16) 0.0297(12) 0.0086(12) 0.0082(11) 0.0001(10) C(22) 0.0429(15) 0.0450(19) 0.0489(15) -0.0001(14) 0.0133(14) 0.0029(13) C(23) 0.068(2) 0.054(3) 0.0302(14) 0.0199(18) 0.0089(13) -0.0053(13) C(24) 0.0369(15) 0.0348(16) 0.0411(14) 0.0110(12) 0.0076(12) -0.0014(12) #============================================================================== _computing_data_collection 'RAPID AUTO (Rigaku, 2010)' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _computing_structure_solution SIR97 _computing_structure_refinement 'CRYSTALS (Carruthers, et al., 1999)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Mo(1) As(1) 2.65796(16) yes . . Mo(1) As(1) 2.65796(16) yes . 2_567 Mo(1) Cl(1) 2.3982(7) yes . . Mo(1) Cl(2) 2.4148(6) yes . . Mo(1) Cl(2) 2.4148(6) yes . 2_567 Mo(1) N(1) 2.239(3) yes . . Mo(2) As(2) 2.6447(3) yes . . Mo(2) As(2) 2.6447(3) yes . 3_656 Mo(2) Cl(3) 2.3969(9) yes . . Mo(2) Cl(4) 2.4157(5) yes . . Mo(2) Cl(4) 2.4157(5) yes . 3_656 Mo(2) N(2) 2.207(3) yes . . As(1) C(4) 1.948(3) yes . . As(1) C(5) 2.013(3) yes . . As(1) C(9) 2.022(3) yes . . As(2) C(16) 1.957(3) yes . . As(2) C(17) 2.021(3) yes . . As(2) C(21) 2.016(3) yes . . N(1) C(1) 1.362(3) yes . . N(1) C(1) 1.362(3) yes . 2_567 N(2) C(13) 1.367(3) yes . . N(2) C(13) 1.367(3) yes . 3_656 C(1) C(2) 1.367(4) yes . . C(1) C(4) 1.517(3) yes . . C(2) C(3) 1.382(3) yes . . C(5) C(6) 1.528(4) yes . . C(5) C(7) 1.521(4) yes . . C(5) C(8) 1.531(4) yes . . C(9) C(10) 1.533(4) yes . . C(9) C(11) 1.526(4) yes . . C(9) C(12) 1.529(4) yes . . C(13) C(14) 1.370(4) yes . . C(13) C(16) 1.527(4) yes . . C(14) C(15) 1.373(3) yes . . C(17) C(18) 1.519(4) yes . . C(17) C(19) 1.538(4) yes . . C(17) C(20) 1.529(4) yes . . C(21) C(22) 1.526(4) yes . . C(21) C(23) 1.531(4) yes . . C(21) C(24) 1.526(4) yes . . C(2) H(1) 0.930 no . . C(3) H(2) 0.930 no . . C(4) H(3) 0.970 no . . C(4) H(4) 0.970 no . . C(6) H(5) 0.960 no . . C(6) H(6) 0.960 no . . C(6) H(7) 0.960 no . . C(7) H(8) 0.960 no . . C(7) H(9) 0.960 no . . C(7) H(10) 0.960 no . . C(8) H(11) 0.960 no . . C(8) H(12) 0.960 no . . C(8) H(13) 0.960 no . . C(10) H(14) 0.960 no . . C(10) H(15) 0.960 no . . C(10) H(16) 0.960 no . . C(11) H(17) 0.960 no . . C(11) H(18) 0.960 no . . C(11) H(19) 0.960 no . . C(12) H(20) 0.960 no . . C(12) H(21) 0.960 no . . C(12) H(22) 0.960 no . . C(14) H(23) 0.930 no . . C(15) H(24) 0.930 no . . C(16) H(25) 0.970 no . . C(16) H(26) 0.970 no . . C(18) H(27) 0.960 no . . C(18) H(28) 0.960 no . . C(18) H(29) 0.960 no . . C(19) H(30) 0.960 no . . C(19) H(31) 0.960 no . . C(19) H(32) 0.960 no . . C(20) H(33) 0.960 no . . C(20) H(34) 0.960 no . . C(20) H(35) 0.960 no . . C(22) H(36) 0.960 no . . C(22) H(37) 0.960 no . . C(22) H(38) 0.960 no . . C(23) H(39) 0.960 no . . C(23) H(40) 0.960 no . . C(23) H(41) 0.960 no . . C(24) H(42) 0.960 no . . C(24) H(43) 0.960 no . . C(24) H(44) 0.960 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 As(1) Mo(1) As(1) 155.034(9) yes . . 2_567 As(1) Mo(1) Cl(1) 102.483(5) yes . . . As(1) Mo(1) Cl(2) 89.102(15) yes . . . As(1) Mo(1) Cl(2) 90.409(15) yes . . 2_567 As(1) Mo(1) N(1) 77.517(5) yes . . . As(1) Mo(1) Cl(1) 102.483(5) yes 2_567 . . As(1) Mo(1) Cl(2) 90.409(15) yes 2_567 . . As(1) Mo(1) Cl(2) 89.102(15) yes 2_567 . 2_567 As(1) Mo(1) N(1) 77.517(5) yes 2_567 . . Cl(1) Mo(1) Cl(2) 91.133(17) yes . . . Cl(1) Mo(1) Cl(2) 91.133(17) yes . . 2_567 Cl(1) Mo(1) N(1) 180.000 yes . . . Cl(2) Mo(1) Cl(2) 177.73(3) yes . . 2_567 Cl(2) Mo(1) N(1) 88.867(17) yes . . . Cl(2) Mo(1) N(1) 88.867(17) yes 2_567 . . As(2) Mo(2) As(2) 159.360(14) yes . . 3_656 As(2) Mo(2) Cl(3) 100.320(8) yes . . . As(2) Mo(2) Cl(4) 89.300(14) yes . . . As(2) Mo(2) Cl(4) 89.993(14) yes . . 3_656 As(2) Mo(2) N(2) 79.680(8) yes . . . As(2) Mo(2) Cl(3) 100.320(8) yes 3_656 . . As(2) Mo(2) Cl(4) 89.993(14) yes 3_656 . . As(2) Mo(2) Cl(4) 89.300(14) yes 3_656 . 3_656 As(2) Mo(2) N(2) 79.680(8) yes 3_656 . . Cl(3) Mo(2) Cl(4) 91.97(2) yes . . . Cl(3) Mo(2) Cl(4) 91.97(2) yes . . 3_656 Cl(3) Mo(2) N(2) 180.000 yes . . . Cl(4) Mo(2) Cl(4) 176.05(3) yes . . 3_656 Cl(4) Mo(2) N(2) 88.03(2) yes . . . Cl(4) Mo(2) N(2) 88.03(2) yes 3_656 . . Mo(1) As(1) C(4) 89.83(6) yes . . . Mo(1) As(1) C(5) 123.86(7) yes . . . Mo(1) As(1) C(9) 120.64(7) yes . . . C(4) As(1) C(5) 102.47(10) yes . . . C(4) As(1) C(9) 102.96(10) yes . . . C(5) As(1) C(9) 109.57(9) yes . . . Mo(2) As(2) C(16) 89.70(7) yes . . . Mo(2) As(2) C(17) 122.34(7) yes . . . Mo(2) As(2) C(21) 121.74(7) yes . . . C(16) As(2) C(17) 103.78(11) yes . . . C(16) As(2) C(21) 104.10(11) yes . . . C(17) As(2) C(21) 108.89(10) yes . . . Mo(1) N(1) C(1) 120.85(13) yes . . . Mo(1) N(1) C(1) 120.85(13) yes . . 2_567 C(1) N(1) C(1) 118.3(3) yes . . 2_567 Mo(2) N(2) C(13) 120.95(14) yes . . . Mo(2) N(2) C(13) 120.95(14) yes . . 3_656 C(13) N(2) C(13) 118.1(3) yes . . 3_656 N(1) C(1) C(2) 121.5(2) yes . . . N(1) C(1) C(4) 118.64(19) yes . . . C(2) C(1) C(4) 119.8(2) yes . . . C(1) C(2) C(3) 120.3(3) yes . . . C(2) C(3) C(2) 118.0(3) yes . . 2_567 As(1) C(4) C(1) 111.40(16) yes . . . As(1) C(5) C(6) 106.75(15) yes . . . As(1) C(5) C(7) 109.76(19) yes . . . As(1) C(5) C(8) 111.76(17) yes . . . C(6) C(5) C(7) 109.8(3) yes . . . C(6) C(5) C(8) 109.0(3) yes . . . C(7) C(5) C(8) 109.73(19) yes . . . As(1) C(9) C(10) 108.26(15) yes . . . As(1) C(9) C(11) 108.86(17) yes . . . As(1) C(9) C(12) 111.67(18) yes . . . C(10) C(9) C(11) 108.9(3) yes . . . C(10) C(9) C(12) 107.9(2) yes . . . C(11) C(9) C(12) 111.2(2) yes . . . N(2) C(13) C(14) 121.4(2) yes . . . N(2) C(13) C(16) 118.7(3) yes . . . C(14) C(13) C(16) 119.9(2) yes . . . C(13) C(14) C(15) 119.9(3) yes . . . C(14) C(15) C(14) 119.1(3) yes . . 3_656 As(2) C(16) C(13) 112.29(17) yes . . . As(2) C(17) C(18) 107.01(15) yes . . . As(2) C(17) C(19) 108.54(18) yes . . . As(2) C(17) C(20) 111.8(2) yes . . . C(18) C(17) C(19) 107.7(3) yes . . . C(18) C(17) C(20) 109.4(3) yes . . . C(19) C(17) C(20) 112.2(2) yes . . . As(2) C(21) C(22) 108.60(17) yes . . . As(2) C(21) C(23) 112.50(18) yes . . . As(2) C(21) C(24) 107.49(16) yes . . . C(22) C(21) C(23) 110.3(2) yes . . . C(22) C(21) C(24) 109.9(2) yes . . . C(23) C(21) C(24) 108.0(3) yes . . . C(1) C(2) H(1) 119.828 no . . . C(3) C(2) H(1) 119.827 no . . . C(2) C(3) H(2) 120.992 no . . . C(2) C(3) H(2) 120.992 no 2_567 . . As(1) C(4) H(3) 120.068 no . . . As(1) C(4) H(4) 120.081 no . . . C(1) C(4) H(3) 98.594 no . . . C(1) C(4) H(4) 98.601 no . . . H(3) C(4) H(4) 104.056 no . . . C(5) C(6) H(5) 109.497 no . . . C(5) C(6) H(6) 109.437 no . . . C(5) C(6) H(7) 109.560 no . . . H(5) C(6) H(6) 109.442 no . . . H(5) C(6) H(7) 109.442 no . . . H(6) C(6) H(7) 109.450 no . . . C(5) C(7) H(8) 109.504 no . . . C(5) C(7) H(9) 109.570 no . . . C(5) C(7) H(10) 109.432 no . . . H(8) C(7) H(9) 109.442 no . . . H(8) C(7) H(10) 109.441 no . . . H(9) C(7) H(10) 109.438 no . . . C(5) C(8) H(11) 109.545 no . . . C(5) C(8) H(12) 109.488 no . . . C(5) C(8) H(13) 109.462 no . . . H(11) C(8) H(12) 109.445 no . . . H(11) C(8) H(13) 109.443 no . . . H(12) C(8) H(13) 109.444 no . . . C(9) C(10) H(14) 109.504 no . . . C(9) C(10) H(15) 109.520 no . . . C(9) C(10) H(16) 109.471 no . . . H(14) C(10) H(15) 109.440 no . . . H(14) C(10) H(16) 109.446 no . . . H(15) C(10) H(16) 109.446 no . . . C(9) C(11) H(17) 109.465 no . . . C(9) C(11) H(18) 109.508 no . . . C(9) C(11) H(19) 109.529 no . . . H(17) C(11) H(18) 109.447 no . . . H(17) C(11) H(19) 109.445 no . . . H(18) C(11) H(19) 109.433 no . . . C(9) C(12) H(20) 109.484 no . . . C(9) C(12) H(21) 109.481 no . . . C(9) C(12) H(22) 109.542 no . . . H(20) C(12) H(21) 109.431 no . . . H(20) C(12) H(22) 109.443 no . . . H(21) C(12) H(22) 109.447 no . . . C(13) C(14) H(23) 120.022 no . . . C(15) C(14) H(23) 120.049 no . . . C(14) C(15) H(24) 120.432 no . . . C(14) C(15) H(24) 120.432 no 3_656 . . As(2) C(16) H(25) 119.913 no . . . As(2) C(16) H(26) 119.935 no . . . C(13) C(16) H(25) 98.249 no . . . C(13) C(16) H(26) 98.289 no . . . H(25) C(16) H(26) 104.073 no . . . C(17) C(18) H(27) 109.584 no . . . C(17) C(18) H(28) 109.416 no . . . C(17) C(18) H(29) 109.493 no . . . H(27) C(18) H(28) 109.447 no . . . H(27) C(18) H(29) 109.442 no . . . H(28) C(18) H(29) 109.445 no . . . C(17) C(19) H(30) 109.489 no . . . C(17) C(19) H(31) 109.515 no . . . C(17) C(19) H(32) 109.493 no . . . H(30) C(19) H(31) 109.439 no . . . H(30) C(19) H(32) 109.445 no . . . H(31) C(19) H(32) 109.447 no . . . C(17) C(20) H(33) 109.500 no . . . C(17) C(20) H(34) 109.476 no . . . C(17) C(20) H(35) 109.520 no . . . H(33) C(20) H(34) 109.444 no . . . H(33) C(20) H(35) 109.444 no . . . H(34) C(20) H(35) 109.444 no . . . C(21) C(22) H(36) 109.502 no . . . C(21) C(22) H(37) 109.496 no . . . C(21) C(22) H(38) 109.507 no . . . H(36) C(22) H(37) 109.444 no . . . H(36) C(22) H(38) 109.437 no . . . H(37) C(22) H(38) 109.441 no . . . C(21) C(23) H(39) 109.486 no . . . C(21) C(23) H(40) 109.472 no . . . C(21) C(23) H(41) 109.553 no . . . H(39) C(23) H(40) 109.444 no . . . H(39) C(23) H(41) 109.433 no . . . H(40) C(23) H(41) 109.439 no . . . C(21) C(24) H(42) 109.497 no . . . C(21) C(24) H(43) 109.486 no . . . C(21) C(24) H(44) 109.511 no . . . H(42) C(24) H(43) 109.438 no . . . H(42) C(24) H(44) 109.443 no . . . H(43) C(24) H(44) 109.452 no . . . _database_code_depnum_ccdc_archive 'CCDC 949577' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_[Mo(N2)2(tBuANA)]2(mu-N2).C6H14 #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C52 H100 As4 Mo2 N12' _chemical_formula_moiety 'C52 H100 As4 Mo2 N12' _chemical_formula_weight 1385.01 #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 18.4671(5) _cell_length_b 13.9179(4) _cell_length_c 25.7755(8) _cell_angle_alpha 90.0000 _cell_angle_beta 104.8817(8) _cell_angle_gamma 90.0000 _cell_volume 6402.7(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 34875 _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 27.49 _cell_measurement_temperature 183 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.330 _exptl_crystal_size_mid 0.110 _exptl_crystal_size_min 0.090 _exptl_crystal_density_diffrn 1.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2848.00 _exptl_absorpt_coefficient_mu 2.485 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'NUMABS (Rigaku, 1999)' _exptl_absorpt_correction_T_min 0.542 _exptl_absorpt_correction_T_max 0.800 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 183 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_reflns_number 56538 _diffrn_reflns_av_R_equivalents 0.0660 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measured_fraction_theta_full 0.989 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_standards_number 0 _diffrn_standards_interval_count . #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 14514 _reflns_number_gt 11998 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0603 _refine_ls_wR_factor_ref 0.0973 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 14514 _refine_ls_number_parameters 701 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[3.4050\s(Fo^2^)]/(4Fo^2^)' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_diff_density_max 2.080 _refine_diff_density_min -1.210 _refine_ls_extinction_method none 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 for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; As As 0.0499 2.0058 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Mo Mo -1.6832 0.6857 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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(1) Mo 0.29658(2) 0.81934(2) 0.25667(2) 0.02648(11) Uani 1.0 4 d . . . Mo(2) Mo 0.20517(2) 0.66394(2) 0.06528(2) 0.02765(11) Uani 1.0 4 d . . . As(1) As 0.42849(2) 0.74944(3) 0.28369(2) 0.03289(14) Uani 1.0 4 d . . . As(2) As 0.18679(2) 0.92190(3) 0.26893(2) 0.03375(14) Uani 1.0 4 d . . . As(3) As 0.17206(2) 0.83045(3) 0.02666(2) 0.03319(14) Uani 1.0 4 d . . . As(4) As 0.18717(2) 0.49959(3) 0.10098(2) 0.03067(14) Uani 1.0 4 d . . . N(1) N 0.25978(17) 0.7586(3) 0.18428(16) 0.0281(11) Uani 1.0 4 d . . . N(2) N 0.24144(17) 0.7240(3) 0.14277(16) 0.0284(11) Uani 1.0 4 d . . . N(3) N 0.25702(18) 0.7090(3) 0.29276(16) 0.0354(12) Uani 1.0 4 d . . . N(4) N 0.2371(2) 0.6501(3) 0.31490(18) 0.0467(14) Uani 1.0 4 d . . . N(5) N 0.33802(18) 0.9326(3) 0.22558(16) 0.0349(12) Uani 1.0 4 d . . . N(6) N 0.3627(2) 0.9983(3) 0.21131(19) 0.0505(15) Uani 1.0 4 d . . . N(7) N 0.3107(2) 0.6472(3) 0.06033(17) 0.0414(13) Uani 1.0 4 d . . . N(8) N 0.3705(3) 0.6351(4) 0.0594(2) 0.0733(19) Uani 1.0 4 d . . . N(9) N 0.16500(19) 0.6105(3) -0.00713(17) 0.0340(12) Uani 1.0 4 d . . . N(10) N 0.1393(2) 0.5824(3) -0.04891(18) 0.0465(14) Uani 1.0 4 d . . . N(11) N 0.34534(18) 0.8887(3) 0.33642(16) 0.0387(12) Uani 1.0 4 d . . . N(12) N 0.09026(17) 0.6795(3) 0.07321(14) 0.0283(11) Uani 1.0 4 d . . . C(1) C 0.4708(3) 0.8667(3) 0.3213(2) 0.0449(16) Uani 1.0 4 d . . . C(2) C 0.4207(3) 0.9037(4) 0.3556(2) 0.0463(16) Uani 1.0 4 d . . . C(3) C 0.4509(3) 0.9474(5) 0.4035(3) 0.076(3) Uani 1.0 4 d . . . C(4) C 0.4061(4) 0.9745(5) 0.4364(3) 0.098(3) Uani 1.0 4 d . . . C(5) C 0.3308(4) 0.9595(5) 0.4175(3) 0.081(3) Uani 1.0 4 d . . . C(6) C 0.3007(3) 0.9185(4) 0.3687(3) 0.0489(17) Uani 1.0 4 d . . . C(7) C 0.2175(3) 0.9066(4) 0.3465(2) 0.0494(17) Uani 1.0 4 d . . . C(8) C 0.4586(3) 0.6503(4) 0.3419(3) 0.0454(16) Uani 1.0 4 d . . . C(9) C 0.4242(3) 0.5549(4) 0.3218(3) 0.064(2) Uani 1.0 4 d . . . C(10) C 0.4278(3) 0.6821(4) 0.3892(3) 0.060(2) Uani 1.0 4 d . . . C(11) C 0.5436(3) 0.6392(4) 0.3640(3) 0.064(2) Uani 1.0 4 d . . . C(12) C 0.4924(3) 0.7333(4) 0.2315(2) 0.0427(16) Uani 1.0 4 d . . . C(13) C 0.4840(3) 0.6311(4) 0.2100(3) 0.063(2) Uani 1.0 4 d . . . C(14) C 0.4590(3) 0.8004(4) 0.1855(3) 0.0548(19) Uani 1.0 4 d . . . C(15) C 0.5747(3) 0.7588(4) 0.2547(3) 0.067(2) Uani 1.0 4 d . . . C(16) C 0.0789(3) 0.8782(4) 0.2533(3) 0.0447(17) Uani 1.0 4 d . . . C(17) C 0.0342(3) 0.9233(4) 0.2012(3) 0.062(2) Uani 1.0 4 d . . . C(18) C 0.0422(3) 0.9015(4) 0.2988(3) 0.067(3) Uani 1.0 4 d . . . C(19) C 0.0803(3) 0.7705(4) 0.2454(3) 0.063(2) Uani 1.0 4 d . . . C(20) C 0.1855(3) 1.0661(4) 0.2603(3) 0.0524(18) Uani 1.0 4 d . . . C(21) C 0.1761(3) 1.0879(4) 0.2016(3) 0.068(3) Uani 1.0 4 d . . . C(22) C 0.1244(3) 1.1155(4) 0.2809(3) 0.078(3) Uani 1.0 4 d . . . C(23) C 0.2616(3) 1.1041(4) 0.2922(3) 0.069(3) Uani 1.0 4 d . . . C(24) C 0.1073(3) 0.8554(3) 0.0759(2) 0.0420(16) Uani 1.0 4 d . . . C(25) C 0.0597(3) 0.7677(3) 0.07834(19) 0.0353(14) Uani 1.0 4 d . . . C(26) C -0.0122(3) 0.7777(4) 0.0843(2) 0.0393(15) Uani 1.0 4 d . . . C(27) C -0.0554(3) 0.6990(4) 0.0864(2) 0.0422(16) Uani 1.0 4 d . . . C(28) C -0.0254(3) 0.6087(4) 0.0816(2) 0.0393(15) Uani 1.0 4 d . . . C(29) C 0.0467(2) 0.6009(3) 0.07451(19) 0.0334(14) Uani 1.0 4 d . . . C(30) C 0.0783(2) 0.5019(3) 0.0675(2) 0.0357(14) Uani 1.0 4 d . . . C(31) C 0.2436(3) 0.9425(4) 0.0422(3) 0.0441(16) Uani 1.0 4 d . . . C(32) C 0.3035(3) 0.9110(4) 0.0913(3) 0.0616(19) Uani 1.0 4 d . . . C(33) C 0.2787(3) 0.9561(4) -0.0044(3) 0.067(2) Uani 1.0 4 d . . . C(34) C 0.2090(3) 1.0369(4) 0.0533(3) 0.074(3) Uani 1.0 4 d . . . C(35) C 0.0997(3) 0.8532(4) -0.0459(2) 0.0402(15) Uani 1.0 4 d . . . C(36) C 0.0313(3) 0.7899(4) -0.0495(3) 0.0541(18) Uani 1.0 4 d . . . C(37) C 0.1381(3) 0.8220(4) -0.0891(3) 0.0563(19) Uani 1.0 4 d . . . C(38) C 0.0745(3) 0.9568(4) -0.0547(3) 0.063(2) Uani 1.0 4 d . . . C(39) C 0.1893(3) 0.4745(3) 0.17797(19) 0.0349(14) Uani 1.0 4 d . . . C(40) C 0.1389(3) 0.5482(3) 0.19453(19) 0.0397(15) Uani 1.0 4 d . . . C(41) C 0.2697(3) 0.4910(4) 0.2122(2) 0.0491(17) Uani 1.0 4 d . . . C(42) C 0.1633(3) 0.3742(3) 0.1892(3) 0.0519(18) Uani 1.0 4 d . . . C(43) C 0.2196(3) 0.3775(3) 0.0706(3) 0.0404(15) Uani 1.0 4 d . . . C(44) C 0.2931(3) 0.3434(4) 0.1071(3) 0.0585(19) Uani 1.0 4 d . . . C(45) C 0.1605(3) 0.2979(4) 0.0623(3) 0.0563(18) Uani 1.0 4 d . . . C(46) C 0.2333(3) 0.4027(4) 0.0170(3) 0.0550(18) Uani 1.0 4 d . . . C(47) C 0.1985(4) 0.3804(6) 0.3563(4) 0.144(3) Uiso 1.0 4 d . . . C(48) C 0.2577(5) 0.3208(7) 0.3998(5) 0.166(4) Uiso 1.0 4 d . . . C(49) C 0.3327(6) 0.3257(8) 0.4080(5) 0.180(5) Uiso 1.0 4 d . . . C(50) C 0.3838(7) 0.2734(8) 0.4472(6) 0.195(5) Uiso 1.0 4 d . . . C(51) C 0.4640(7) 0.2553(9) 0.4582(6) 0.235(6) Uiso 1.0 4 d . . . C(52) C 0.4939(6) 0.3580(9) 0.4607(6) 0.260(6) Uiso 1.0 4 d . . . H(1) H 0.5179 0.8661 0.3488 0.0508 Uiso 1.0 4 calc R . . H(2) H 0.4736 0.9256 0.3018 0.0508 Uiso 1.0 4 calc R . . H(3) H 0.5023 0.9585 0.4146 0.0871 Uiso 1.0 4 calc R . . H(4) H 0.4259 1.0027 0.4697 0.1130 Uiso 1.0 4 calc R . . H(5) H 0.2992 0.9772 0.4387 0.0952 Uiso 1.0 4 calc R . . H(6) H 0.2025 0.9513 0.3707 0.0603 Uiso 1.0 4 calc R . . H(7) H 0.2140 0.8451 0.3635 0.0602 Uiso 1.0 4 calc R . . H(8) H 0.4258 0.5126 0.3515 0.0730 Uiso 1.0 4 calc R . . H(9) H 0.3730 0.5646 0.3022 0.0731 Uiso 1.0 4 calc R . . H(10) H 0.4516 0.5269 0.2986 0.0731 Uiso 1.0 4 calc R . . H(11) H 0.3780 0.7068 0.3756 0.0715 Uiso 1.0 4 calc R . . H(12) H 0.4266 0.6281 0.4121 0.0713 Uiso 1.0 4 calc R . . H(13) H 0.4593 0.7313 0.4093 0.0713 Uiso 1.0 4 calc R . . H(14) H 0.5646 0.6110 0.3372 0.0729 Uiso 1.0 4 calc R . . H(15) H 0.5654 0.7015 0.3735 0.0729 Uiso 1.0 4 calc R . . H(16) H 0.5542 0.5988 0.3953 0.0729 Uiso 1.0 4 calc R . . H(17) H 0.4324 0.6178 0.1928 0.0758 Uiso 1.0 4 calc R . . H(18) H 0.5135 0.6230 0.1846 0.0758 Uiso 1.0 4 calc R . . H(19) H 0.5013 0.5875 0.2394 0.0758 Uiso 1.0 4 calc R . . H(20) H 0.4064 0.7876 0.1719 0.0688 Uiso 1.0 4 calc R . . H(21) H 0.4660 0.8655 0.1979 0.0688 Uiso 1.0 4 calc R . . H(22) H 0.4837 0.7910 0.1573 0.0688 Uiso 1.0 4 calc R . . H(23) H 0.5794 0.8255 0.2646 0.0808 Uiso 1.0 4 calc R . . H(24) H 0.5947 0.7199 0.2858 0.0808 Uiso 1.0 4 calc R . . H(25) H 0.6020 0.7466 0.2283 0.0809 Uiso 1.0 4 calc R . . H(26) H 0.0635 0.9209 0.1754 0.0729 Uiso 1.0 4 calc R . . H(27) H -0.0117 0.8885 0.1877 0.0730 Uiso 1.0 4 calc R . . H(28) H 0.0230 0.9890 0.2075 0.0730 Uiso 1.0 4 calc R . . H(29) H -0.0051 0.8692 0.2928 0.0840 Uiso 1.0 4 calc R . . H(30) H 0.0746 0.8806 0.3322 0.0840 Uiso 1.0 4 calc R . . H(31) H 0.0346 0.9696 0.3000 0.0841 Uiso 1.0 4 calc R . . H(32) H 0.0302 0.7467 0.2322 0.0766 Uiso 1.0 4 calc R . . H(33) H 0.1085 0.7566 0.2198 0.0766 Uiso 1.0 4 calc R . . H(34) H 0.1036 0.7401 0.2789 0.0765 Uiso 1.0 4 calc R . . H(35) H 0.1772 1.1558 0.1953 0.0827 Uiso 1.0 4 calc R . . H(36) H 0.2160 1.0574 0.1901 0.0827 Uiso 1.0 4 calc R . . H(37) H 0.1289 1.0622 0.1817 0.0827 Uiso 1.0 4 calc R . . H(38) H 0.0803 1.0761 0.2737 0.0928 Uiso 1.0 4 calc R . . H(39) H 0.1424 1.1254 0.3190 0.0928 Uiso 1.0 4 calc R . . H(40) H 0.1125 1.1765 0.2634 0.0930 Uiso 1.0 4 calc R . . H(41) H 0.3009 1.0663 0.2842 0.0838 Uiso 1.0 4 calc R . . H(42) H 0.2677 1.1701 0.2834 0.0839 Uiso 1.0 4 calc R . . H(43) H 0.2640 1.0989 0.3297 0.0838 Uiso 1.0 4 calc R . . H(44) H 0.1284 0.8634 0.1141 0.0529 Uiso 1.0 4 calc R . . H(45) H 0.0677 0.9031 0.0677 0.0528 Uiso 1.0 4 calc R . . H(46) H -0.0309 0.8388 0.0874 0.0465 Uiso 1.0 4 calc R . . H(47) H -0.1038 0.7053 0.0905 0.0492 Uiso 1.0 4 calc R . . H(48) H -0.0532 0.5536 0.0832 0.0470 Uiso 1.0 4 calc R . . H(49) H 0.0581 0.4958 0.0290 0.0409 Uiso 1.0 4 calc R . . H(50) H 0.0437 0.4643 0.0818 0.0408 Uiso 1.0 4 calc R . . H(51) H 0.3342 0.9652 0.1058 0.0705 Uiso 1.0 4 calc R . . H(52) H 0.2803 0.8862 0.1179 0.0706 Uiso 1.0 4 calc R . . H(53) H 0.3339 0.8620 0.0814 0.0705 Uiso 1.0 4 calc R . . H(54) H 0.2972 0.8950 -0.0125 0.0786 Uiso 1.0 4 calc R . . H(55) H 0.2422 0.9796 -0.0354 0.0786 Uiso 1.0 4 calc R . . H(56) H 0.3194 1.0009 0.0054 0.0788 Uiso 1.0 4 calc R . . H(57) H 0.1895 1.0295 0.0843 0.0885 Uiso 1.0 4 calc R . . H(58) H 0.2459 1.0870 0.0599 0.0884 Uiso 1.0 4 calc R . . H(59) H 0.1689 1.0535 0.0228 0.0886 Uiso 1.0 4 calc R . . H(60) H 0.0024 0.8154 -0.0266 0.0614 Uiso 1.0 4 calc R . . H(61) H 0.0011 0.7880 -0.0858 0.0614 Uiso 1.0 4 calc R . . H(62) H 0.0476 0.7260 -0.0380 0.0612 Uiso 1.0 4 calc R . . H(63) H 0.1040 0.8282 -0.1240 0.0679 Uiso 1.0 4 calc R . . H(64) H 0.1810 0.8622 -0.0870 0.0679 Uiso 1.0 4 calc R . . H(65) H 0.1539 0.7563 -0.0833 0.0678 Uiso 1.0 4 calc R . . H(66) H 0.0503 0.9757 -0.0275 0.0717 Uiso 1.0 4 calc R . . H(67) H 0.1170 0.9976 -0.0530 0.0717 Uiso 1.0 4 calc R . . H(68) H 0.0399 0.9627 -0.0894 0.0717 Uiso 1.0 4 calc R . . H(69) H 0.1446 0.5459 0.2326 0.0478 Uiso 1.0 4 calc R . . H(70) H 0.1517 0.6112 0.1846 0.0478 Uiso 1.0 4 calc R . . H(71) H 0.0878 0.5342 0.1762 0.0479 Uiso 1.0 4 calc R . . H(72) H 0.2733 0.4772 0.2493 0.0559 Uiso 1.0 4 calc R . . H(73) H 0.3033 0.4501 0.1996 0.0560 Uiso 1.0 4 calc R . . H(74) H 0.2829 0.5570 0.2087 0.0560 Uiso 1.0 4 calc R . . H(75) H 0.1536 0.3719 0.2241 0.0633 Uiso 1.0 4 calc R . . H(76) H 0.1182 0.3589 0.1623 0.0632 Uiso 1.0 4 calc R . . H(77) H 0.2016 0.3285 0.1877 0.0635 Uiso 1.0 4 calc R . . H(78) H 0.3289 0.3948 0.1131 0.0663 Uiso 1.0 4 calc R . . H(79) H 0.2850 0.3232 0.1408 0.0664 Uiso 1.0 4 calc R . . H(80) H 0.3120 0.2903 0.0907 0.0665 Uiso 1.0 4 calc R . . H(81) H 0.1128 0.3233 0.0432 0.0659 Uiso 1.0 4 calc R . . H(82) H 0.1741 0.2459 0.0422 0.0657 Uiso 1.0 4 calc R . . H(83) H 0.1575 0.2749 0.0968 0.0659 Uiso 1.0 4 calc R . . H(84) H 0.1868 0.4215 -0.0072 0.0661 Uiso 1.0 4 calc R . . H(85) H 0.2682 0.4551 0.0215 0.0661 Uiso 1.0 4 calc R . . H(86) H 0.2534 0.3483 0.0026 0.0661 Uiso 1.0 4 calc R . . H(87) H 0.2040 0.3634 0.3214 0.1727 Uiso 1.0 4 calc R . . H(88) H 0.1482 0.3671 0.3580 0.1723 Uiso 1.0 4 calc R . . H(89) H 0.2089 0.4476 0.3625 0.1727 Uiso 1.0 4 calc R . . H(90) H 0.2601 0.3341 0.4372 0.1987 Uiso 1.0 4 calc R . . H(91) H 0.2553 0.2513 0.3968 0.1987 Uiso 1.0 4 calc R . . H(92) H 0.3376 0.3064 0.3729 0.2159 Uiso 1.0 4 calc R . . H(93) H 0.3417 0.3942 0.4122 0.2158 Uiso 1.0 4 calc R . . H(94) H 0.3771 0.3038 0.4795 0.2338 Uiso 1.0 4 calc R . . H(95) H 0.3611 0.2101 0.4435 0.2337 Uiso 1.0 4 calc R . . H(96) H 0.4818 0.2206 0.4917 0.2826 Uiso 1.0 4 calc R . . H(97) H 0.4730 0.2171 0.4290 0.2827 Uiso 1.0 4 calc R . . H(98) H 0.4820 0.3937 0.4893 0.3120 Uiso 1.0 4 calc R . . H(99) H 0.5474 0.3537 0.4669 0.3119 Uiso 1.0 4 calc R . . H(100) H 0.4733 0.3903 0.4272 0.3121 Uiso 1.0 4 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mo(1) 0.02677(18) 0.0268(2) 0.0257(3) 0.00005(15) 0.00653(16) -0.00258(17) Mo(2) 0.0330(2) 0.0239(2) 0.0246(3) -0.00009(15) 0.00468(17) -0.00135(17) As(1) 0.0280(3) 0.0375(3) 0.0307(3) 0.00263(19) 0.0029(2) -0.0052(3) As(2) 0.0340(3) 0.0348(3) 0.0338(4) 0.00554(19) 0.0112(3) -0.0031(3) As(3) 0.0388(3) 0.0267(3) 0.0325(4) -0.00047(19) 0.0063(3) 0.0044(3) As(4) 0.0350(3) 0.0236(3) 0.0308(3) -0.00022(18) 0.0036(2) 0.0001(2) N(1) 0.0286(18) 0.027(2) 0.028(3) -0.0015(15) 0.0070(17) 0.0017(18) N(2) 0.0285(18) 0.023(2) 0.033(3) -0.0011(15) 0.0075(18) 0.0026(18) N(3) 0.035(2) 0.041(3) 0.030(3) 0.0038(17) 0.0080(19) 0.001(2) N(4) 0.052(3) 0.043(3) 0.052(4) -0.000(2) 0.026(3) 0.007(3) N(5) 0.037(2) 0.037(3) 0.033(3) -0.0018(17) 0.0137(19) -0.0093(19) N(6) 0.058(3) 0.043(3) 0.054(4) -0.018(2) 0.021(3) -0.007(3) N(7) 0.040(3) 0.044(3) 0.042(3) -0.0076(18) 0.014(2) -0.012(2) N(8) 0.052(3) 0.096(4) 0.073(5) 0.000(3) 0.018(3) -0.018(3) N(9) 0.041(2) 0.031(3) 0.029(3) 0.0002(16) 0.0060(19) -0.0010(19) N(10) 0.062(3) 0.043(3) 0.030(3) -0.008(2) 0.004(3) -0.006(3) N(11) 0.039(2) 0.042(3) 0.031(3) 0.0056(17) 0.0024(19) -0.009(2) N(12) 0.0352(19) 0.024(2) 0.023(3) 0.0019(15) 0.0028(17) 0.0004(17) C(1) 0.036(3) 0.041(3) 0.049(4) -0.005(2) -0.003(3) -0.021(3) C(2) 0.040(3) 0.060(4) 0.034(4) -0.004(3) 0.001(3) -0.022(3) C(3) 0.051(4) 0.102(5) 0.065(6) 0.010(4) -0.001(4) -0.044(4) C(4) 0.067(4) 0.158(7) 0.058(6) 0.021(5) -0.006(4) -0.059(5) C(5) 0.070(4) 0.129(6) 0.038(5) 0.028(4) 0.003(4) -0.039(4) C(6) 0.054(3) 0.065(4) 0.028(4) 0.009(3) 0.011(3) -0.011(3) C(7) 0.056(3) 0.063(4) 0.032(4) 0.017(3) 0.016(3) -0.004(3) C(8) 0.042(3) 0.046(4) 0.040(4) 0.006(3) -0.004(3) -0.007(3) C(9) 0.070(4) 0.051(4) 0.062(5) 0.007(3) 0.001(4) 0.017(4) C(10) 0.059(4) 0.079(5) 0.040(4) 0.017(3) 0.008(3) 0.011(4) C(11) 0.050(3) 0.077(5) 0.056(5) 0.025(3) -0.003(3) 0.006(4) C(12) 0.031(3) 0.056(4) 0.042(4) 0.007(3) 0.012(3) -0.010(3) C(13) 0.065(4) 0.069(4) 0.056(5) 0.013(3) 0.015(4) -0.010(4) C(14) 0.055(3) 0.070(4) 0.047(4) 0.012(3) 0.027(3) 0.008(3) C(15) 0.032(3) 0.111(6) 0.058(5) -0.001(3) 0.012(3) -0.005(4) C(16) 0.033(3) 0.057(4) 0.046(4) 0.004(3) 0.013(3) 0.002(3) C(17) 0.040(3) 0.087(5) 0.055(5) 0.006(3) 0.008(3) -0.012(4) C(18) 0.051(3) 0.099(5) 0.060(5) 0.005(3) 0.033(4) 0.002(4) C(19) 0.030(3) 0.056(4) 0.105(6) -0.006(3) 0.022(3) 0.000(4) C(20) 0.059(4) 0.030(3) 0.069(5) 0.008(3) 0.018(4) -0.016(3) C(21) 0.086(4) 0.030(4) 0.091(6) 0.012(3) 0.025(4) 0.012(4) C(22) 0.081(4) 0.050(4) 0.102(7) 0.022(3) 0.021(4) -0.027(4) C(23) 0.079(4) 0.039(4) 0.092(6) -0.001(3) 0.027(4) -0.026(4) C(24) 0.056(3) 0.034(3) 0.041(4) 0.005(3) 0.023(3) 0.000(3) C(25) 0.039(3) 0.036(3) 0.027(3) 0.002(2) 0.002(3) -0.002(3) C(26) 0.039(3) 0.037(3) 0.041(4) 0.006(2) 0.007(3) -0.005(3) C(27) 0.031(3) 0.050(4) 0.042(4) 0.005(3) 0.003(3) 0.000(3) C(28) 0.034(3) 0.043(3) 0.040(4) -0.002(2) 0.009(3) 0.000(3) C(29) 0.032(3) 0.035(3) 0.029(4) 0.0012(19) 0.001(2) -0.003(3) C(30) 0.029(3) 0.033(3) 0.040(4) -0.0035(18) -0.001(2) -0.002(3) C(31) 0.058(3) 0.031(3) 0.042(4) -0.012(3) 0.010(3) 0.002(3) C(32) 0.069(4) 0.054(4) 0.053(5) -0.031(3) 0.000(3) 0.008(3) C(33) 0.070(4) 0.068(5) 0.060(5) -0.028(3) 0.007(4) 0.016(4) C(34) 0.102(5) 0.030(4) 0.089(6) -0.014(3) 0.024(4) -0.012(4) C(35) 0.047(3) 0.038(3) 0.033(4) 0.006(3) 0.005(3) 0.000(3) C(36) 0.050(3) 0.066(4) 0.038(4) 0.001(3) -0.005(3) 0.007(3) C(37) 0.071(4) 0.062(4) 0.037(4) 0.000(3) 0.015(3) 0.001(3) C(38) 0.074(4) 0.053(4) 0.052(5) 0.020(3) -0.002(3) 0.010(3) C(39) 0.037(3) 0.036(3) 0.029(3) -0.008(2) 0.003(3) 0.008(3) C(40) 0.044(3) 0.044(3) 0.032(4) -0.009(3) 0.011(3) -0.004(3) C(41) 0.048(3) 0.050(4) 0.042(4) -0.004(3) -0.002(3) 0.005(3) C(42) 0.069(4) 0.037(3) 0.052(5) -0.005(3) 0.020(3) 0.010(3) C(43) 0.045(3) 0.023(3) 0.046(4) 0.004(2) 0.001(3) -0.006(3) C(44) 0.046(3) 0.056(4) 0.065(5) 0.023(3) -0.003(3) -0.007(3) C(45) 0.068(4) 0.036(3) 0.060(5) 0.002(3) 0.009(3) -0.013(3) C(46) 0.075(4) 0.035(3) 0.055(5) 0.012(3) 0.017(4) -0.011(3) #============================================================================== _computing_data_collection 'RAPID AUTO (Rigaku, 2010)' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _computing_structure_solution SIR97 _computing_structure_refinement 'CRYSTALS (Carruthers, et al., 1999)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Mo(1) As(1) 2.5484(5) yes . . Mo(1) As(2) 2.5646(6) yes . . Mo(1) N(1) 2.002(4) yes . . Mo(1) N(3) 2.026(4) yes . . Mo(1) N(5) 2.007(4) yes . . Mo(1) N(11) 2.240(4) yes . . Mo(2) As(3) 2.5343(6) yes . . Mo(2) As(4) 2.5192(6) yes . . Mo(2) N(2) 2.110(4) yes . . Mo(2) N(7) 1.999(4) yes . . Mo(2) N(9) 1.969(4) yes . . Mo(2) N(12) 2.194(4) yes . . As(1) C(1) 1.956(5) yes . . As(1) C(8) 2.010(5) yes . . As(1) C(12) 2.017(6) yes . . As(2) C(7) 1.945(5) yes . . As(2) C(16) 2.022(5) yes . . As(2) C(20) 2.019(5) yes . . As(3) C(24) 1.985(6) yes . . As(3) C(31) 2.016(5) yes . . As(3) C(35) 2.025(5) yes . . As(4) C(30) 1.974(4) yes . . As(4) C(39) 2.005(5) yes . . As(4) C(43) 2.025(5) yes . . N(1) N(2) 1.142(6) yes . . N(3) N(4) 1.115(6) yes . . N(5) N(6) 1.125(6) yes . . N(7) N(8) 1.123(6) yes . . N(9) N(10) 1.129(6) yes . . N(11) C(2) 1.368(6) yes . . N(11) C(6) 1.377(8) yes . . N(12) C(25) 1.371(6) yes . . N(12) C(29) 1.364(6) yes . . C(1) C(2) 1.523(8) yes . . C(2) C(3) 1.362(8) yes . . C(3) C(4) 1.380(10) yes . . C(4) C(5) 1.367(8) yes . . C(5) C(6) 1.362(8) yes . . C(6) C(7) 1.506(6) yes . . C(8) C(9) 1.506(7) yes . . C(8) C(10) 1.535(9) yes . . C(8) C(11) 1.533(6) yes . . C(12) C(13) 1.521(7) yes . . C(12) C(14) 1.512(7) yes . . C(12) C(15) 1.526(6) yes . . C(16) C(17) 1.520(7) yes . . C(16) C(18) 1.531(9) yes . . C(16) C(19) 1.513(7) yes . . C(20) C(21) 1.510(10) yes . . C(20) C(22) 1.528(9) yes . . C(20) C(23) 1.529(7) yes . . C(24) C(25) 1.514(6) yes . . C(25) C(26) 1.382(7) yes . . C(26) C(27) 1.364(7) yes . . C(27) C(28) 1.392(7) yes . . C(28) C(29) 1.393(7) yes . . C(29) C(30) 1.524(6) yes . . C(31) C(32) 1.516(7) yes . . C(31) C(33) 1.516(9) yes . . C(31) C(34) 1.520(7) yes . . C(35) C(36) 1.523(7) yes . . C(35) C(37) 1.527(8) yes . . C(35) C(38) 1.515(7) yes . . C(39) C(40) 1.519(7) yes . . C(39) C(41) 1.536(6) yes . . C(39) C(42) 1.529(7) yes . . C(43) C(44) 1.517(6) yes . . C(43) C(45) 1.530(7) yes . . C(43) C(46) 1.507(9) yes . . C(47) C(48) 1.584(12) yes . . C(48) C(49) 1.349(14) yes . . C(49) C(50) 1.395(15) yes . . C(50) C(51) 1.456(17) yes . . C(51) C(52) 1.529(18) yes . . C(1) H(1) 0.970 no . . C(1) H(2) 0.970 no . . C(3) H(3) 0.930 no . . C(4) H(4) 0.930 no . . C(5) H(5) 0.930 no . . C(7) H(6) 0.970 no . . C(7) H(7) 0.970 no . . C(9) H(8) 0.960 no . . C(9) H(9) 0.960 no . . C(9) H(10) 0.960 no . . C(10) H(11) 0.960 no . . C(10) H(12) 0.960 no . . C(10) H(13) 0.960 no . . C(11) H(14) 0.960 no . . C(11) H(15) 0.960 no . . C(11) H(16) 0.960 no . . C(13) H(17) 0.960 no . . C(13) H(18) 0.960 no . . C(13) H(19) 0.960 no . . C(14) H(20) 0.960 no . . C(14) H(21) 0.960 no . . C(14) H(22) 0.960 no . . C(15) H(23) 0.960 no . . C(15) H(24) 0.960 no . . C(15) H(25) 0.960 no . . C(17) H(26) 0.960 no . . C(17) H(27) 0.960 no . . C(17) H(28) 0.960 no . . C(18) H(29) 0.960 no . . C(18) H(30) 0.960 no . . C(18) H(31) 0.960 no . . C(19) H(32) 0.960 no . . C(19) H(33) 0.960 no . . C(19) H(34) 0.960 no . . C(21) H(35) 0.960 no . . C(21) H(36) 0.960 no . . C(21) H(37) 0.960 no . . C(22) H(38) 0.960 no . . C(22) H(39) 0.960 no . . C(22) H(40) 0.960 no . . C(23) H(41) 0.960 no . . C(23) H(42) 0.960 no . . C(23) H(43) 0.960 no . . C(24) H(44) 0.970 no . . C(24) H(45) 0.970 no . . C(26) H(46) 0.930 no . . C(27) H(47) 0.930 no . . C(28) H(48) 0.930 no . . C(30) H(49) 0.970 no . . C(30) H(50) 0.970 no . . C(32) H(51) 0.960 no . . C(32) H(52) 0.960 no . . C(32) H(53) 0.960 no . . C(33) H(54) 0.960 no . . C(33) H(55) 0.960 no . . C(33) H(56) 0.960 no . . C(34) H(57) 0.960 no . . C(34) H(58) 0.960 no . . C(34) H(59) 0.960 no . . C(36) H(60) 0.960 no . . C(36) H(61) 0.960 no . . C(36) H(62) 0.960 no . . C(37) H(63) 0.960 no . . C(37) H(64) 0.960 no . . C(37) H(65) 0.960 no . . C(38) H(66) 0.960 no . . C(38) H(67) 0.960 no . . C(38) H(68) 0.960 no . . C(40) H(69) 0.960 no . . C(40) H(70) 0.960 no . . C(40) H(71) 0.960 no . . C(41) H(72) 0.960 no . . C(41) H(73) 0.960 no . . C(41) H(74) 0.960 no . . C(42) H(75) 0.960 no . . C(42) H(76) 0.960 no . . C(42) H(77) 0.960 no . . C(44) H(78) 0.960 no . . C(44) H(79) 0.960 no . . C(44) H(80) 0.960 no . . C(45) H(81) 0.960 no . . C(45) H(82) 0.960 no . . C(45) H(83) 0.960 no . . C(46) H(84) 0.960 no . . C(46) H(85) 0.960 no . . C(46) H(86) 0.960 no . . C(47) H(87) 0.960 no . . C(47) H(88) 0.960 no . . C(47) H(89) 0.960 no . . C(48) H(90) 0.970 no . . C(48) H(91) 0.970 no . . C(49) H(92) 0.970 no . . C(49) H(93) 0.970 no . . C(50) H(94) 0.970 no . . C(50) H(95) 0.970 no . . C(51) H(96) 0.970 no . . C(51) H(97) 0.970 no . . C(52) H(98) 0.960 no . . C(52) H(99) 0.960 no . . C(52) H(100) 0.960 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 As(1) Mo(1) As(2) 155.41(3) yes . . . As(1) Mo(1) N(1) 99.51(10) yes . . . As(1) Mo(1) N(3) 90.99(10) yes . . . As(1) Mo(1) N(5) 88.46(10) yes . . . As(1) Mo(1) N(11) 77.46(9) yes . . . As(2) Mo(1) N(1) 105.08(10) yes . . . As(2) Mo(1) N(3) 88.60(11) yes . . . As(2) Mo(1) N(5) 90.38(11) yes . . . As(2) Mo(1) N(11) 77.95(9) yes . . . N(1) Mo(1) N(3) 91.81(15) yes . . . N(1) Mo(1) N(5) 91.87(16) yes . . . N(1) Mo(1) N(11) 176.09(15) yes . . . N(3) Mo(1) N(5) 176.31(16) yes . . . N(3) Mo(1) N(11) 90.72(15) yes . . . N(5) Mo(1) N(11) 85.61(15) yes . . . As(3) Mo(2) As(4) 158.84(2) yes . . . As(3) Mo(2) N(2) 89.73(9) yes . . . As(3) Mo(2) N(7) 102.86(11) yes . . . As(3) Mo(2) N(9) 88.81(11) yes . . . As(3) Mo(2) N(12) 78.73(9) yes . . . As(4) Mo(2) N(2) 93.08(10) yes . . . As(4) Mo(2) N(7) 98.01(11) yes . . . As(4) Mo(2) N(9) 87.14(11) yes . . . As(4) Mo(2) N(12) 80.46(9) yes . . . N(2) Mo(2) N(7) 91.67(15) yes . . . N(2) Mo(2) N(9) 176.46(14) yes . . . N(2) Mo(2) N(12) 87.25(13) yes . . . N(7) Mo(2) N(9) 91.80(16) yes . . . N(7) Mo(2) N(12) 178.08(15) yes . . . N(9) Mo(2) N(12) 89.30(15) yes . . . Mo(1) As(1) C(1) 92.80(12) yes . . . Mo(1) As(1) C(8) 121.89(15) yes . . . Mo(1) As(1) C(12) 122.85(13) yes . . . C(1) As(1) C(8) 101.8(2) yes . . . C(1) As(1) C(12) 101.3(2) yes . . . C(8) As(1) C(12) 108.9(2) yes . . . Mo(1) As(2) C(7) 91.99(14) yes . . . Mo(1) As(2) C(16) 125.27(15) yes . . . Mo(1) As(2) C(20) 121.83(17) yes . . . C(7) As(2) C(16) 100.6(2) yes . . . C(7) As(2) C(20) 102.4(3) yes . . . C(16) As(2) C(20) 107.1(2) yes . . . Mo(2) As(3) C(24) 91.89(13) yes . . . Mo(2) As(3) C(31) 123.34(13) yes . . . Mo(2) As(3) C(35) 122.76(13) yes . . . C(24) As(3) C(31) 102.1(2) yes . . . C(24) As(3) C(35) 101.6(2) yes . . . C(31) As(3) C(35) 107.8(2) yes . . . Mo(2) As(4) C(30) 92.32(13) yes . . . Mo(2) As(4) C(39) 123.26(13) yes . . . Mo(2) As(4) C(43) 122.73(16) yes . . . C(30) As(4) C(39) 101.2(2) yes . . . C(30) As(4) C(43) 102.34(17) yes . . . C(39) As(4) C(43) 107.7(2) yes . . . Mo(1) N(1) N(2) 177.5(4) yes . . . Mo(2) N(2) N(1) 178.2(3) yes . . . Mo(1) N(3) N(4) 176.7(4) yes . . . Mo(1) N(5) N(6) 175.7(4) yes . . . Mo(2) N(7) N(8) 177.1(5) yes . . . Mo(2) N(9) N(10) 177.0(4) yes . . . Mo(1) N(11) C(2) 122.0(4) yes . . . Mo(1) N(11) C(6) 121.5(3) yes . . . C(2) N(11) C(6) 116.5(4) yes . . . Mo(2) N(12) C(25) 121.9(3) yes . . . Mo(2) N(12) C(29) 120.9(3) yes . . . C(25) N(12) C(29) 117.1(4) yes . . . As(1) C(1) C(2) 110.2(3) yes . . . N(11) C(2) C(1) 116.8(4) yes . . . N(11) C(2) C(3) 122.5(5) yes . . . C(1) C(2) C(3) 120.6(5) yes . . . C(2) C(3) C(4) 120.6(5) yes . . . C(3) C(4) C(5) 117.0(6) yes . . . C(4) C(5) C(6) 122.0(7) yes . . . N(11) C(6) C(5) 121.2(5) yes . . . N(11) C(6) C(7) 116.6(5) yes . . . C(5) C(6) C(7) 122.1(6) yes . . . As(2) C(7) C(6) 112.2(4) yes . . . As(1) C(8) C(9) 109.7(4) yes . . . As(1) C(8) C(10) 107.8(4) yes . . . As(1) C(8) C(11) 114.0(4) yes . . . C(9) C(8) C(10) 108.5(5) yes . . . C(9) C(8) C(11) 109.9(4) yes . . . C(10) C(8) C(11) 106.7(4) yes . . . As(1) C(12) C(13) 109.0(4) yes . . . As(1) C(12) C(14) 105.3(4) yes . . . As(1) C(12) C(15) 114.1(4) yes . . . C(13) C(12) C(14) 107.9(5) yes . . . C(13) C(12) C(15) 111.0(4) yes . . . C(14) C(12) C(15) 109.2(5) yes . . . As(2) C(16) C(17) 109.6(4) yes . . . As(2) C(16) C(18) 113.0(4) yes . . . As(2) C(16) C(19) 106.0(3) yes . . . C(17) C(16) C(18) 109.9(4) yes . . . C(17) C(16) C(19) 108.3(5) yes . . . C(18) C(16) C(19) 109.9(5) yes . . . As(2) C(20) C(21) 107.8(4) yes . . . As(2) C(20) C(22) 113.5(4) yes . . . As(2) C(20) C(23) 107.5(3) yes . . . C(21) C(20) C(22) 110.7(5) yes . . . C(21) C(20) C(23) 108.8(5) yes . . . C(22) C(20) C(23) 108.4(5) yes . . . As(3) C(24) C(25) 109.7(4) yes . . . N(12) C(25) C(24) 117.4(4) yes . . . N(12) C(25) C(26) 122.1(4) yes . . . C(24) C(25) C(26) 120.5(4) yes . . . C(25) C(26) C(27) 120.8(5) yes . . . C(26) C(27) C(28) 118.1(5) yes . . . C(27) C(28) C(29) 119.9(4) yes . . . N(12) C(29) C(28) 122.0(4) yes . . . N(12) C(29) C(30) 118.4(4) yes . . . C(28) C(29) C(30) 119.6(4) yes . . . As(4) C(30) C(29) 110.0(3) yes . . . As(3) C(31) C(32) 104.0(4) yes . . . As(3) C(31) C(33) 109.3(4) yes . . . As(3) C(31) C(34) 114.9(4) yes . . . C(32) C(31) C(33) 109.2(5) yes . . . C(32) C(31) C(34) 110.1(5) yes . . . C(33) C(31) C(34) 109.1(5) yes . . . As(3) C(35) C(36) 107.7(4) yes . . . As(3) C(35) C(37) 108.0(3) yes . . . As(3) C(35) C(38) 113.0(4) yes . . . C(36) C(35) C(37) 109.0(4) yes . . . C(36) C(35) C(38) 108.8(4) yes . . . C(37) C(35) C(38) 110.2(5) yes . . . As(4) C(39) C(40) 107.6(3) yes . . . As(4) C(39) C(41) 108.3(4) yes . . . As(4) C(39) C(42) 114.8(4) yes . . . C(40) C(39) C(41) 108.0(4) yes . . . C(40) C(39) C(42) 108.5(4) yes . . . C(41) C(39) C(42) 109.4(4) yes . . . As(4) C(43) C(44) 109.2(4) yes . . . As(4) C(43) C(45) 113.0(4) yes . . . As(4) C(43) C(46) 107.2(3) yes . . . C(44) C(43) C(45) 110.6(4) yes . . . C(44) C(43) C(46) 107.8(5) yes . . . C(45) C(43) C(46) 108.8(5) yes . . . C(47) C(48) C(49) 125.3(10) yes . . . C(48) C(49) C(50) 124.3(12) yes . . . C(49) C(50) C(51) 134.1(13) yes . . . C(50) C(51) C(52) 100.7(10) yes . . . As(1) C(1) H(1) 121.603 no . . . As(1) C(1) H(2) 121.055 no . . . C(2) C(1) H(1) 98.244 no . . . C(2) C(1) H(2) 97.817 no . . . H(1) C(1) H(2) 103.170 no . . . C(2) C(3) H(3) 120.036 no . . . C(4) C(3) H(3) 119.380 no . . . C(3) C(4) H(4) 121.854 no . . . C(5) C(4) H(4) 121.089 no . . . C(4) C(5) H(5) 118.973 no . . . C(6) C(5) H(5) 119.028 no . . . As(2) C(7) H(6) 122.259 no . . . As(2) C(7) H(7) 121.618 no . . . C(6) C(7) H(6) 96.720 no . . . C(6) C(7) H(7) 96.050 no . . . H(6) C(7) H(7) 102.350 no . . . C(8) C(9) H(8) 110.011 no . . . C(8) C(9) H(9) 109.254 no . . . C(8) C(9) H(10) 109.239 no . . . H(8) C(9) H(9) 109.448 no . . . H(8) C(9) H(10) 109.437 no . . . H(9) C(9) H(10) 109.438 no . . . C(8) C(10) H(11) 109.307 no . . . C(8) C(10) H(12) 109.502 no . . . C(8) C(10) H(13) 109.685 no . . . H(11) C(10) H(12) 109.443 no . . . H(11) C(10) H(13) 109.444 no . . . H(12) C(10) H(13) 109.446 no . . . C(8) C(11) H(14) 109.736 no . . . C(8) C(11) H(15) 108.987 no . . . C(8) C(11) H(16) 109.780 no . . . H(14) C(11) H(15) 109.437 no . . . H(14) C(11) H(16) 109.439 no . . . H(15) C(11) H(16) 109.448 no . . . C(12) C(13) H(17) 110.172 no . . . C(12) C(13) H(18) 109.611 no . . . C(12) C(13) H(19) 108.719 no . . . H(17) C(13) H(18) 109.437 no . . . H(17) C(13) H(19) 109.440 no . . . H(18) C(13) H(19) 109.445 no . . . C(12) C(14) H(20) 110.035 no . . . C(12) C(14) H(21) 109.099 no . . . C(12) C(14) H(22) 109.366 no . . . H(20) C(14) H(21) 109.441 no . . . H(20) C(14) H(22) 109.443 no . . . H(21) C(14) H(22) 109.441 no . . . C(12) C(15) H(23) 110.003 no . . . C(12) C(15) H(24) 108.991 no . . . C(12) C(15) H(25) 109.502 no . . . H(23) C(15) H(24) 109.444 no . . . H(23) C(15) H(25) 109.444 no . . . H(24) C(15) H(25) 109.442 no . . . C(16) C(17) H(26) 108.787 no . . . C(16) C(17) H(27) 109.963 no . . . C(16) C(17) H(28) 109.744 no . . . H(26) C(17) H(27) 109.443 no . . . H(26) C(17) H(28) 109.452 no . . . H(27) C(17) H(28) 109.436 no . . . C(16) C(18) H(29) 110.080 no . . . C(16) C(18) H(30) 109.050 no . . . C(16) C(18) H(31) 109.374 no . . . H(29) C(18) H(30) 109.446 no . . . H(29) C(18) H(31) 109.445 no . . . H(30) C(18) H(31) 109.430 no . . . C(16) C(19) H(32) 110.016 no . . . C(16) C(19) H(33) 108.936 no . . . C(16) C(19) H(34) 109.539 no . . . H(32) C(19) H(33) 109.451 no . . . H(32) C(19) H(34) 109.447 no . . . H(33) C(19) H(34) 109.436 no . . . C(20) C(21) H(35) 111.400 no . . . C(20) C(21) H(36) 108.728 no . . . C(20) C(21) H(37) 108.354 no . . . H(35) C(21) H(36) 109.443 no . . . H(35) C(21) H(37) 109.442 no . . . H(36) C(21) H(37) 109.443 no . . . C(20) C(22) H(38) 109.944 no . . . C(20) C(22) H(39) 109.056 no . . . C(20) C(22) H(40) 109.507 no . . . H(38) C(22) H(39) 109.437 no . . . H(38) C(22) H(40) 109.439 no . . . H(39) C(22) H(40) 109.444 no . . . C(20) C(23) H(41) 109.672 no . . . C(20) C(23) H(42) 110.561 no . . . C(20) C(23) H(43) 108.252 no . . . H(41) C(23) H(42) 109.439 no . . . H(41) C(23) H(43) 109.455 no . . . H(42) C(23) H(43) 109.441 no . . . As(3) C(24) H(44) 121.253 no . . . As(3) C(24) H(45) 121.701 no . . . C(25) C(24) H(44) 97.859 no . . . C(25) C(24) H(45) 98.547 no . . . H(44) C(24) H(45) 103.026 no . . . C(25) C(26) H(46) 119.501 no . . . C(27) C(26) H(46) 119.686 no . . . C(26) C(27) H(47) 121.209 no . . . C(28) C(27) H(47) 120.723 no . . . C(27) C(28) H(48) 120.237 no . . . C(29) C(28) H(48) 119.880 no . . . As(4) C(30) H(49) 121.782 no . . . As(4) C(30) H(50) 121.483 no . . . C(29) C(30) H(49) 98.195 no . . . C(29) C(30) H(50) 97.627 no . . . H(49) C(30) H(50) 102.867 no . . . C(31) C(32) H(51) 109.233 no . . . C(31) C(32) H(52) 109.659 no . . . C(31) C(32) H(53) 109.607 no . . . H(51) C(32) H(52) 109.441 no . . . H(51) C(32) H(53) 109.438 no . . . H(52) C(32) H(53) 109.447 no . . . C(31) C(33) H(54) 108.148 no . . . C(31) C(33) H(55) 110.563 no . . . C(31) C(33) H(56) 109.782 no . . . H(54) C(33) H(55) 109.439 no . . . H(54) C(33) H(56) 109.444 no . . . H(55) C(33) H(56) 109.442 no . . . C(31) C(34) H(57) 109.215 no . . . C(31) C(34) H(58) 110.275 no . . . C(31) C(34) H(59) 109.014 no . . . H(57) C(34) H(58) 109.436 no . . . H(57) C(34) H(59) 109.445 no . . . H(58) C(34) H(59) 109.440 no . . . C(35) C(36) H(60) 109.509 no . . . C(35) C(36) H(61) 109.832 no . . . C(35) C(36) H(62) 109.160 no . . . H(60) C(36) H(61) 109.444 no . . . H(60) C(36) H(62) 109.437 no . . . H(61) C(36) H(62) 109.444 no . . . C(35) C(37) H(63) 109.900 no . . . C(35) C(37) H(64) 108.915 no . . . C(35) C(37) H(65) 109.680 no . . . H(63) C(37) H(64) 109.445 no . . . H(63) C(37) H(65) 109.439 no . . . H(64) C(37) H(65) 109.447 no . . . C(35) C(38) H(66) 109.625 no . . . C(35) C(38) H(67) 109.879 no . . . C(35) C(38) H(68) 108.989 no . . . H(66) C(38) H(67) 109.436 no . . . H(66) C(38) H(68) 109.450 no . . . H(67) C(38) H(68) 109.447 no . . . C(39) C(40) H(69) 110.469 no . . . C(39) C(40) H(70) 109.234 no . . . C(39) C(40) H(71) 108.798 no . . . H(69) C(40) H(70) 109.436 no . . . H(69) C(40) H(71) 109.448 no . . . H(70) C(40) H(71) 109.437 no . . . C(39) C(41) H(72) 110.602 no . . . C(39) C(41) H(73) 109.236 no . . . C(39) C(41) H(74) 108.652 no . . . H(72) C(41) H(73) 109.451 no . . . H(72) C(41) H(74) 109.436 no . . . H(73) C(41) H(74) 109.444 no . . . C(39) C(42) H(75) 110.643 no . . . C(39) C(42) H(76) 108.836 no . . . C(39) C(42) H(77) 109.024 no . . . H(75) C(42) H(76) 109.439 no . . . H(75) C(42) H(77) 109.430 no . . . H(76) C(42) H(77) 109.450 no . . . C(43) C(44) H(78) 109.630 no . . . C(43) C(44) H(79) 109.253 no . . . C(43) C(44) H(80) 109.607 no . . . H(78) C(44) H(79) 109.442 no . . . H(78) C(44) H(80) 109.445 no . . . H(79) C(44) H(80) 109.450 no . . . C(43) C(45) H(81) 109.513 no . . . C(43) C(45) H(82) 110.246 no . . . C(43) C(45) H(83) 108.732 no . . . H(81) C(45) H(82) 109.433 no . . . H(81) C(45) H(83) 109.454 no . . . H(82) C(45) H(83) 109.446 no . . . C(43) C(46) H(84) 108.947 no . . . C(43) C(46) H(85) 109.410 no . . . C(43) C(46) H(86) 110.128 no . . . H(84) C(46) H(85) 109.437 no . . . H(84) C(46) H(86) 109.450 no . . . H(85) C(46) H(86) 109.453 no . . . C(48) C(47) H(87) 108.383 no . . . C(48) C(47) H(88) 111.447 no . . . C(48) C(47) H(89) 108.641 no . . . H(87) C(47) H(88) 109.452 no . . . H(87) C(47) H(89) 109.444 no . . . H(88) C(47) H(89) 109.443 no . . . C(47) C(48) H(90) 116.826 no . . . C(47) C(48) H(91) 117.095 no . . . C(49) C(48) H(90) 92.910 no . . . C(49) C(48) H(91) 94.942 no . . . H(90) C(48) H(91) 105.066 no . . . C(48) C(49) H(92) 100.188 no . . . C(48) C(49) H(93) 101.915 no . . . C(50) C(49) H(92) 108.813 no . . . C(50) C(49) H(93) 111.647 no . . . H(92) C(49) H(93) 108.732 no . . . C(49) C(50) H(94) 100.492 no . . . C(49) C(50) H(95) 101.983 no . . . C(51) C(50) H(94) 104.717 no . . . C(51) C(50) H(95) 104.761 no . . . H(94) C(50) H(95) 109.465 no . . . C(50) C(51) H(96) 110.805 no . . . C(50) C(51) H(97) 108.147 no . . . C(52) C(51) H(96) 113.118 no . . . C(52) C(51) H(97) 114.383 no . . . H(96) C(51) H(97) 109.307 no . . . C(51) C(52) H(98) 111.328 no . . . C(51) C(52) H(99) 107.039 no . . . C(51) C(52) H(100) 110.100 no . . . H(98) C(52) H(99) 109.454 no . . . H(98) C(52) H(100) 109.438 no . . . H(99) C(52) H(100) 109.437 no . . . _database_code_depnum_ccdc_archive 'CCDC 949578' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_[Mo(N2)2(PMe3)(tBuANA)] #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C26 H52 As2 Mo N5 P' _chemical_formula_moiety 'C26 H52 As2 Mo N5 P' _chemical_formula_weight 711.49 #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 10.6374(10) _cell_length_b 11.4503(10) _cell_length_c 15.0424(12) _cell_angle_alpha 107.8606(18) _cell_angle_beta 99.1578(17) _cell_angle_gamma 105.823(2) _cell_volume 1617.8(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 4241 _cell_measurement_theta_min 3.12 _cell_measurement_theta_max 27.47 _cell_measurement_temperature 198 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour red _exptl_crystal_size_max 0.130 _exptl_crystal_size_mid 0.070 _exptl_crystal_size_min 0.020 _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 732.00 _exptl_absorpt_coefficient_mu 2.507 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR (Rigaku, 1995)' _exptl_absorpt_correction_T_min 0.509 _exptl_absorpt_correction_T_max 0.951 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 198 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_reflns_number 15254 _diffrn_reflns_av_R_equivalents 0.0596 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_max 0.981 _diffrn_measured_fraction_theta_full 0.981 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 16 _diffrn_standards_number 0 _diffrn_standards_interval_count . #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 7273 _reflns_number_gt 4925 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.0782 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 7273 _refine_ls_number_parameters 368 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[2.1100\s(Fo^2^)]/(4Fo^2^)' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_diff_density_max 1.130 _refine_diff_density_min -1.450 _refine_ls_extinction_method none 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 for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.1023 0.0942 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; As As 0.0499 2.0058 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Mo Mo -1.6832 0.6857 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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(1) Mo 0.83058(4) 0.61338(4) 0.75778(3) 0.02561(12) Uani 1.0 2 d . . . As(1) As 0.72771(5) 0.39870(5) 0.78001(3) 0.02954(15) Uani 1.0 2 d . . . As(2) As 1.00661(5) 0.77751(4) 0.71810(3) 0.02899(15) Uani 1.0 2 d . . . P(1) P 0.66736(14) 0.72281(13) 0.78445(9) 0.0355(4) Uani 1.0 2 d . . . N(1) N 0.9855(4) 0.5138(4) 0.7297(3) 0.0275(12) Uani 1.0 2 d . . . N(2) N 0.7369(5) 0.5360(4) 0.6159(3) 0.0357(14) Uani 1.0 2 d . . . N(3) N 0.6897(6) 0.4942(5) 0.5391(4) 0.0521(16) Uani 1.0 2 d . . . N(4) N 0.9192(5) 0.6978(4) 0.9033(3) 0.0355(14) Uani 1.0 2 d . . . N(5) N 0.9665(6) 0.7453(5) 0.9794(4) 0.0567(17) Uani 1.0 2 d . . . C(1) C 0.9045(5) 0.3848(5) 0.8284(4) 0.0379(17) Uani 1.0 2 d . . . C(2) C 1.0019(5) 0.4244(5) 0.7695(3) 0.0301(14) Uani 1.0 2 d . . . C(3) C 1.0985(5) 0.3660(5) 0.7566(4) 0.0359(16) Uani 1.0 2 d . . . C(4) C 1.1817(6) 0.3953(5) 0.6984(4) 0.0405(17) Uani 1.0 2 d . . . C(5) C 1.1642(5) 0.4819(5) 0.6554(4) 0.0352(16) Uani 1.0 2 d . . . C(6) C 1.0694(5) 0.5413(5) 0.6738(3) 0.0300(14) Uani 1.0 2 d . . . C(7) C 1.0534(5) 0.6397(5) 0.6282(3) 0.0330(15) Uani 1.0 2 d . . . C(8) C 0.6343(6) 0.2337(5) 0.6601(4) 0.0365(16) Uani 1.0 2 d . . . C(9) C 0.5054(6) 0.2469(5) 0.6092(4) 0.0501(18) Uani 1.0 2 d . . . C(10) C 0.6020(7) 0.1077(5) 0.6793(4) 0.059(2) Uani 1.0 2 d . . . C(11) C 0.7312(6) 0.2295(5) 0.5939(4) 0.0465(17) Uani 1.0 2 d . . . C(12) C 0.6461(6) 0.3685(5) 0.8882(4) 0.0424(18) Uani 1.0 2 d . . . C(13) C 0.7087(6) 0.4942(5) 0.9746(4) 0.0518(19) Uani 1.0 2 d . . . C(14) C 0.4928(6) 0.3369(5) 0.8560(4) 0.0503(19) Uani 1.0 2 d . . . C(15) C 0.6747(7) 0.2600(6) 0.9177(4) 0.059(3) Uani 1.0 2 d . . . C(16) C 0.9755(6) 0.8747(5) 0.6290(4) 0.0384(17) Uani 1.0 2 d . . . C(17) C 0.8282(6) 0.8096(5) 0.5691(4) 0.0482(19) Uani 1.0 2 d . . . C(18) C 0.9966(6) 1.0163(5) 0.6867(4) 0.054(2) Uani 1.0 2 d . . . C(19) C 1.0658(6) 0.8706(5) 0.5592(4) 0.055(2) Uani 1.0 2 d . . . C(20) C 1.1848(6) 0.8888(5) 0.8167(4) 0.0388(16) Uani 1.0 2 d . . . C(21) C 1.1577(7) 0.9938(5) 0.8962(4) 0.062(2) Uani 1.0 2 d . . . C(22) C 1.2948(6) 0.9520(6) 0.7757(4) 0.059(2) Uani 1.0 2 d . . . C(23) C 1.2352(6) 0.8022(5) 0.8612(4) 0.0484(18) Uani 1.0 2 d . . . C(24) C 0.5239(6) 0.6776(6) 0.6820(4) 0.068(3) Uani 1.0 2 d . . . C(25) C 0.7248(7) 0.9002(5) 0.8228(4) 0.056(2) Uani 1.0 2 d . . . C(26) C 0.5740(6) 0.7098(6) 0.8757(4) 0.055(2) Uani 1.0 2 d . . . H(1) H 0.9148 0.3015 0.8230 0.0500 Uiso 1.0 2 calc R . . H(2) H 0.9633 0.4425 0.8921 0.0501 Uiso 1.0 2 calc R . . H(3) H 1.1076 0.3074 0.7863 0.0445 Uiso 1.0 2 calc R . . H(4) H 1.2485 0.3582 0.6892 0.0492 Uiso 1.0 2 calc R . . H(5) H 1.2155 0.4998 0.6135 0.0436 Uiso 1.0 2 calc R . . H(6) H 0.9911 0.5785 0.5667 0.0395 Uiso 1.0 2 calc R . . H(7) H 1.1398 0.6577 0.6124 0.0392 Uiso 1.0 2 calc R . . H(8) H 0.5273 0.3287 0.6000 0.0530 Uiso 1.0 2 calc R . . H(9) H 0.4429 0.2438 0.6487 0.0530 Uiso 1.0 2 calc R . . H(10) H 0.4648 0.1766 0.5474 0.0531 Uiso 1.0 2 calc R . . H(11) H 0.5558 0.1146 0.7295 0.0691 Uiso 1.0 2 calc R . . H(12) H 0.6843 0.0922 0.6993 0.0690 Uiso 1.0 2 calc R . . H(13) H 0.5448 0.0366 0.6212 0.0692 Uiso 1.0 2 calc R . . H(14) H 0.8105 0.2175 0.6246 0.0518 Uiso 1.0 2 calc R . . H(15) H 0.6868 0.1584 0.5329 0.0518 Uiso 1.0 2 calc R . . H(16) H 0.7571 0.3103 0.5833 0.0517 Uiso 1.0 2 calc R . . H(17) H 0.7050 0.5656 0.9548 0.0647 Uiso 1.0 2 calc R . . H(18) H 0.8015 0.5055 1.0009 0.0648 Uiso 1.0 2 calc R . . H(19) H 0.6601 0.4921 1.0230 0.0648 Uiso 1.0 2 calc R . . H(20) H 0.7708 0.2792 0.9368 0.0864 Uiso 1.0 2 calc R . . H(21) H 0.6374 0.2536 0.9708 0.0863 Uiso 1.0 2 calc R . . H(22) H 0.6340 0.1786 0.8635 0.0863 Uiso 1.0 2 calc R . . H(23) H 0.4536 0.2539 0.8033 0.0637 Uiso 1.0 2 calc R . . H(24) H 0.4741 0.4031 0.8350 0.0636 Uiso 1.0 2 calc R . . H(25) H 0.4544 0.3331 0.9090 0.0637 Uiso 1.0 2 calc R . . H(26) H 0.8169 0.7259 0.5227 0.0625 Uiso 1.0 2 calc R . . H(27) H 0.8036 0.8628 0.5358 0.0624 Uiso 1.0 2 calc R . . H(28) H 0.7711 0.7985 0.6114 0.0624 Uiso 1.0 2 calc R . . H(29) H 1.0527 0.7813 0.5224 0.0754 Uiso 1.0 2 calc R . . H(30) H 1.0431 0.9128 0.5159 0.0754 Uiso 1.0 2 calc R . . H(31) H 1.1588 0.9149 0.5958 0.0754 Uiso 1.0 2 calc R . . H(32) H 0.9885 1.0632 0.6442 0.0704 Uiso 1.0 2 calc R . . H(33) H 1.0857 1.0553 0.7305 0.0704 Uiso 1.0 2 calc R . . H(34) H 0.9303 1.0199 0.7230 0.0704 Uiso 1.0 2 calc R . . H(35) H 1.1579 1.0663 0.8769 0.0662 Uiso 1.0 2 calc R . . H(36) H 1.2263 1.0234 0.9558 0.0663 Uiso 1.0 2 calc R . . H(37) H 1.0706 0.9561 0.9054 0.0662 Uiso 1.0 2 calc R . . H(38) H 1.3094 0.8850 0.7260 0.0668 Uiso 1.0 2 calc R . . H(39) H 1.2659 1.0090 0.7484 0.0668 Uiso 1.0 2 calc R . . H(40) H 1.3777 1.0014 0.8259 0.0669 Uiso 1.0 2 calc R . . H(41) H 1.3014 0.8549 0.9221 0.0537 Uiso 1.0 2 calc R . . H(42) H 1.2751 0.7523 0.8181 0.0535 Uiso 1.0 2 calc R . . H(43) H 1.1598 0.7441 0.8715 0.0535 Uiso 1.0 2 calc R . . H(44) H 0.4853 0.5842 0.6521 0.0825 Uiso 1.0 2 calc R . . H(45) H 0.5546 0.7129 0.6360 0.0826 Uiso 1.0 2 calc R . . H(46) H 0.4566 0.7120 0.7035 0.0825 Uiso 1.0 2 calc R . . H(47) H 0.7478 0.9248 0.7703 0.0763 Uiso 1.0 2 calc R . . H(48) H 0.6544 0.9319 0.8412 0.0763 Uiso 1.0 2 calc R . . H(49) H 0.8033 0.9374 0.8771 0.0764 Uiso 1.0 2 calc R . . H(50) H 0.5325 0.7757 0.8885 0.0730 Uiso 1.0 2 calc R . . H(51) H 0.6363 0.7220 0.9342 0.0731 Uiso 1.0 2 calc R . . H(52) H 0.5054 0.6251 0.8525 0.0731 Uiso 1.0 2 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mo(1) 0.0266(3) 0.0251(3) 0.0255(3) 0.0086(2) 0.00641(19) 0.01037(17) As(1) 0.0296(4) 0.0298(3) 0.0323(3) 0.0093(3) 0.0116(3) 0.0146(3) As(2) 0.0309(4) 0.0263(3) 0.0325(3) 0.0096(3) 0.0094(3) 0.0142(3) P(1) 0.0331(9) 0.0405(8) 0.0360(8) 0.0174(7) 0.0096(7) 0.0140(6) N(1) 0.027(3) 0.028(2) 0.028(3) 0.0081(19) 0.0074(19) 0.0103(18) N(2) 0.034(3) 0.034(3) 0.045(3) 0.011(3) 0.020(3) 0.017(3) N(3) 0.063(4) 0.049(3) 0.037(3) 0.006(3) 0.019(3) 0.014(3) N(4) 0.030(3) 0.034(3) 0.041(3) 0.008(3) 0.011(3) 0.013(3) N(5) 0.052(4) 0.056(4) 0.050(3) 0.006(3) 0.005(3) 0.020(3) C(1) 0.034(4) 0.045(4) 0.046(4) 0.021(3) 0.008(3) 0.026(3) C(2) 0.028(4) 0.028(3) 0.030(3) 0.012(3) 0.002(3) 0.007(3) C(3) 0.035(4) 0.027(3) 0.049(4) 0.016(3) 0.009(3) 0.015(3) C(4) 0.031(4) 0.040(3) 0.052(4) 0.019(3) 0.012(3) 0.013(3) C(5) 0.033(4) 0.035(3) 0.042(3) 0.016(3) 0.016(3) 0.013(3) C(6) 0.032(4) 0.028(3) 0.029(3) 0.012(3) 0.008(3) 0.008(3) C(7) 0.036(4) 0.035(3) 0.027(3) 0.011(3) 0.016(3) 0.008(3) C(8) 0.041(4) 0.026(3) 0.037(3) 0.006(3) 0.011(3) 0.008(3) C(9) 0.036(4) 0.042(4) 0.054(4) 0.002(3) 0.005(3) 0.007(3) C(10) 0.066(5) 0.028(3) 0.078(5) 0.009(3) 0.030(4) 0.014(3) C(11) 0.054(4) 0.036(3) 0.039(3) 0.011(3) 0.019(3) 0.001(3) C(12) 0.047(4) 0.049(4) 0.047(4) 0.019(3) 0.027(3) 0.030(3) C(13) 0.055(5) 0.072(4) 0.035(3) 0.024(4) 0.022(3) 0.022(3) C(14) 0.048(4) 0.048(4) 0.063(4) 0.014(3) 0.028(4) 0.027(3) C(15) 0.077(6) 0.070(4) 0.069(4) 0.040(4) 0.045(4) 0.052(4) C(16) 0.053(4) 0.037(3) 0.040(3) 0.022(3) 0.021(3) 0.023(3) C(17) 0.058(5) 0.057(4) 0.041(4) 0.028(4) 0.008(3) 0.028(3) C(18) 0.066(5) 0.044(4) 0.065(4) 0.025(4) 0.018(4) 0.034(3) C(19) 0.062(5) 0.064(4) 0.063(4) 0.025(4) 0.031(4) 0.046(4) C(20) 0.045(4) 0.030(3) 0.042(3) 0.010(3) 0.008(3) 0.017(3) C(21) 0.079(6) 0.040(4) 0.047(4) 0.006(4) 0.001(4) 0.008(3) C(22) 0.038(4) 0.054(4) 0.075(5) -0.008(3) 0.004(4) 0.036(4) C(23) 0.038(4) 0.052(4) 0.043(4) 0.004(3) 0.004(3) 0.016(3) C(24) 0.048(5) 0.095(6) 0.063(4) 0.042(4) 0.007(4) 0.021(4) C(25) 0.073(5) 0.044(4) 0.073(5) 0.032(4) 0.043(4) 0.031(3) C(26) 0.053(5) 0.060(4) 0.070(4) 0.029(4) 0.036(4) 0.027(4) #============================================================================== _computing_data_collection 'RAPID AUTO (Rigaku, 2010)' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'CRYSTALS (Carruthers, et al., 1999)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Mo(1) As(1) 2.5506(8) yes . . Mo(1) As(2) 2.5533(7) yes . . Mo(1) P(1) 2.4177(18) yes . . Mo(1) N(1) 2.268(5) yes . . Mo(1) N(2) 2.004(4) yes . . Mo(1) N(4) 2.041(4) yes . . As(1) C(1) 1.972(6) yes . . As(1) C(8) 2.031(4) yes . . As(1) C(12) 2.038(7) yes . . As(2) C(7) 1.975(5) yes . . As(2) C(16) 2.029(6) yes . . As(2) C(20) 2.012(5) yes . . P(1) C(24) 1.817(6) yes . . P(1) C(25) 1.824(6) yes . . P(1) C(26) 1.835(7) yes . . N(1) C(2) 1.370(7) yes . . N(1) C(6) 1.360(7) yes . . N(2) N(3) 1.077(6) yes . . N(4) N(5) 1.069(6) yes . . C(1) C(2) 1.532(8) yes . . C(2) C(3) 1.378(8) yes . . C(3) C(4) 1.388(8) yes . . C(4) C(5) 1.375(9) yes . . C(5) C(6) 1.379(9) yes . . C(6) C(7) 1.520(8) yes . . C(8) C(9) 1.530(9) yes . . C(8) C(10) 1.516(8) yes . . C(8) C(11) 1.543(9) yes . . C(12) C(13) 1.502(6) yes . . C(12) C(14) 1.531(9) yes . . C(12) C(15) 1.528(10) yes . . C(16) C(17) 1.525(8) yes . . C(16) C(18) 1.520(7) yes . . C(16) C(19) 1.531(9) yes . . C(20) C(21) 1.542(8) yes . . C(20) C(22) 1.522(9) yes . . C(20) C(23) 1.516(9) yes . . C(1) H(1) 0.970 no . . C(1) H(2) 0.970 no . . C(3) H(3) 0.930 no . . C(4) H(4) 0.930 no . . C(5) H(5) 0.930 no . . C(7) H(6) 0.970 no . . C(7) H(7) 0.970 no . . C(9) H(8) 0.960 no . . C(9) H(9) 0.960 no . . C(9) H(10) 0.960 no . . C(10) H(11) 0.960 no . . C(10) H(12) 0.960 no . . C(10) H(13) 0.960 no . . C(11) H(14) 0.960 no . . C(11) H(15) 0.960 no . . C(11) H(16) 0.960 no . . C(13) H(17) 0.960 no . . C(13) H(18) 0.960 no . . C(13) H(19) 0.960 no . . C(14) H(23) 0.960 no . . C(14) H(24) 0.960 no . . C(14) H(25) 0.960 no . . C(15) H(20) 0.960 no . . C(15) H(21) 0.960 no . . C(15) H(22) 0.960 no . . C(17) H(26) 0.960 no . . C(17) H(27) 0.960 no . . C(17) H(28) 0.960 no . . C(18) H(32) 0.960 no . . C(18) H(33) 0.960 no . . C(18) H(34) 0.960 no . . C(19) H(29) 0.960 no . . C(19) H(30) 0.960 no . . C(19) H(31) 0.960 no . . C(21) H(35) 0.960 no . . C(21) H(36) 0.960 no . . C(21) H(37) 0.960 no . . C(22) H(38) 0.960 no . . C(22) H(39) 0.960 no . . C(22) H(40) 0.960 no . . C(23) H(41) 0.960 no . . C(23) H(42) 0.960 no . . C(23) H(43) 0.960 no . . C(24) H(44) 0.960 no . . C(24) H(45) 0.960 no . . C(24) H(46) 0.960 no . . C(25) H(47) 0.960 no . . C(25) H(48) 0.960 no . . C(25) H(49) 0.960 no . . C(26) H(50) 0.960 no . . C(26) H(51) 0.960 no . . C(26) H(52) 0.960 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 As(1) Mo(1) As(2) 154.93(3) yes . . . As(1) Mo(1) P(1) 104.07(4) yes . . . As(1) Mo(1) N(1) 77.42(11) yes . . . As(1) Mo(1) N(2) 92.41(13) yes . . . As(1) Mo(1) N(4) 88.59(13) yes . . . As(2) Mo(1) P(1) 100.95(5) yes . . . As(2) Mo(1) N(1) 77.54(11) yes . . . As(2) Mo(1) N(2) 86.46(13) yes . . . As(2) Mo(1) N(4) 93.85(13) yes . . . P(1) Mo(1) N(1) 178.29(12) yes . . . P(1) Mo(1) N(2) 88.97(15) yes . . . P(1) Mo(1) N(4) 88.01(15) yes . . . N(1) Mo(1) N(2) 90.13(17) yes . . . N(1) Mo(1) N(4) 92.89(17) yes . . . N(2) Mo(1) N(4) 177.0(2) yes . . . Mo(1) As(1) C(1) 94.37(16) yes . . . Mo(1) As(1) C(8) 118.51(16) yes . . . Mo(1) As(1) C(12) 128.71(15) yes . . . C(1) As(1) C(8) 103.9(3) yes . . . C(1) As(1) C(12) 96.9(3) yes . . . C(8) As(1) C(12) 106.9(2) yes . . . Mo(1) As(2) C(7) 93.01(15) yes . . . Mo(1) As(2) C(16) 128.37(16) yes . . . Mo(1) As(2) C(20) 119.80(17) yes . . . C(7) As(2) C(16) 98.0(3) yes . . . C(7) As(2) C(20) 103.0(3) yes . . . C(16) As(2) C(20) 106.5(2) yes . . . Mo(1) P(1) C(24) 116.9(3) yes . . . Mo(1) P(1) C(25) 118.7(3) yes . . . Mo(1) P(1) C(26) 121.1(3) yes . . . C(24) P(1) C(25) 100.4(3) yes . . . C(24) P(1) C(26) 98.4(3) yes . . . C(25) P(1) C(26) 97.1(3) yes . . . Mo(1) N(1) C(2) 122.0(4) yes . . . Mo(1) N(1) C(6) 121.9(4) yes . . . C(2) N(1) C(6) 116.1(5) yes . . . Mo(1) N(2) N(3) 178.1(5) yes . . . Mo(1) N(4) N(5) 177.9(5) yes . . . As(1) C(1) C(2) 110.2(4) yes . . . N(1) C(2) C(1) 117.9(5) yes . . . N(1) C(2) C(3) 123.3(5) yes . . . C(1) C(2) C(3) 118.8(5) yes . . . C(2) C(3) C(4) 119.2(6) yes . . . C(3) C(4) C(5) 118.4(6) yes . . . C(4) C(5) C(6) 119.9(6) yes . . . N(1) C(6) C(5) 123.1(5) yes . . . N(1) C(6) C(7) 117.4(5) yes . . . C(5) C(6) C(7) 119.5(5) yes . . . As(2) C(7) C(6) 109.6(4) yes . . . As(1) C(8) C(9) 107.2(4) yes . . . As(1) C(8) C(10) 114.9(4) yes . . . As(1) C(8) C(11) 107.0(3) yes . . . C(9) C(8) C(10) 110.8(5) yes . . . C(9) C(8) C(11) 109.2(5) yes . . . C(10) C(8) C(11) 107.7(5) yes . . . As(1) C(12) C(13) 106.5(4) yes . . . As(1) C(12) C(14) 108.6(4) yes . . . As(1) C(12) C(15) 114.1(5) yes . . . C(13) C(12) C(14) 109.9(5) yes . . . C(13) C(12) C(15) 108.1(5) yes . . . C(14) C(12) C(15) 109.5(5) yes . . . As(2) C(16) C(17) 107.4(4) yes . . . As(2) C(16) C(18) 111.1(4) yes . . . As(2) C(16) C(19) 113.3(5) yes . . . C(17) C(16) C(18) 107.8(6) yes . . . C(17) C(16) C(19) 108.1(4) yes . . . C(18) C(16) C(19) 108.9(5) yes . . . As(2) C(20) C(21) 107.4(4) yes . . . As(2) C(20) C(22) 114.4(4) yes . . . As(2) C(20) C(23) 107.8(3) yes . . . C(21) C(20) C(22) 110.5(4) yes . . . C(21) C(20) C(23) 108.8(5) yes . . . C(22) C(20) C(23) 107.7(5) yes . . . As(1) C(1) H(1) 122.011 no . . . As(1) C(1) H(2) 121.385 no . . . C(2) C(1) H(1) 98.106 no . . . C(2) C(1) H(2) 97.260 no . . . H(1) C(1) H(2) 102.860 no . . . C(2) C(3) H(3) 120.436 no . . . C(4) C(3) H(3) 120.350 no . . . C(3) C(4) H(4) 120.953 no . . . C(5) C(4) H(4) 120.612 no . . . C(4) C(5) H(5) 120.134 no . . . C(6) C(5) H(5) 119.968 no . . . As(2) C(7) H(6) 122.470 no . . . As(2) C(7) H(7) 121.800 no . . . C(6) C(7) H(6) 97.935 no . . . C(6) C(7) H(7) 97.275 no . . . H(6) C(7) H(7) 102.455 no . . . C(8) C(9) H(8) 109.603 no . . . C(8) C(9) H(9) 109.003 no . . . C(8) C(9) H(10) 109.808 no . . . H(8) C(9) H(9) 109.489 no . . . H(8) C(9) H(10) 109.443 no . . . H(9) C(9) H(10) 109.481 no . . . C(8) C(10) H(11) 109.174 no . . . C(8) C(10) H(12) 109.900 no . . . C(8) C(10) H(13) 109.346 no . . . H(11) C(10) H(12) 109.482 no . . . H(11) C(10) H(13) 109.441 no . . . H(12) C(10) H(13) 109.483 no . . . C(8) C(11) H(14) 109.215 no . . . C(8) C(11) H(15) 109.778 no . . . C(8) C(11) H(16) 109.435 no . . . H(14) C(11) H(15) 109.442 no . . . H(14) C(11) H(16) 109.476 no . . . H(15) C(11) H(16) 109.480 no . . . C(12) C(13) H(17) 109.290 no . . . C(12) C(13) H(18) 109.215 no . . . C(12) C(13) H(19) 109.920 no . . . H(17) C(13) H(18) 109.475 no . . . H(17) C(13) H(19) 109.447 no . . . H(18) C(13) H(19) 109.480 no . . . C(12) C(14) H(23) 108.966 no . . . C(12) C(14) H(24) 109.895 no . . . C(12) C(14) H(25) 109.560 no . . . H(23) C(14) H(24) 109.438 no . . . H(23) C(14) H(25) 109.480 no . . . H(24) C(14) H(25) 109.488 no . . . C(12) C(15) H(20) 109.409 no . . . C(12) C(15) H(21) 109.886 no . . . C(12) C(15) H(22) 109.125 no . . . H(20) C(15) H(21) 109.486 no . . . H(20) C(15) H(22) 109.440 no . . . H(21) C(15) H(22) 109.480 no . . . C(16) C(17) H(26) 109.211 no . . . C(16) C(17) H(27) 110.220 no . . . C(16) C(17) H(28) 108.988 no . . . H(26) C(17) H(27) 109.482 no . . . H(26) C(17) H(28) 109.479 no . . . H(27) C(17) H(28) 109.444 no . . . C(16) C(18) H(32) 110.543 no . . . C(16) C(18) H(33) 108.397 no . . . C(16) C(18) H(34) 109.481 no . . . H(32) C(18) H(33) 109.477 no . . . H(32) C(18) H(34) 109.477 no . . . H(33) C(18) H(34) 109.446 no . . . C(16) C(19) H(29) 109.261 no . . . C(16) C(19) H(30) 110.105 no . . . C(16) C(19) H(31) 109.055 no . . . H(29) C(19) H(30) 109.478 no . . . H(29) C(19) H(31) 109.486 no . . . H(30) C(19) H(31) 109.440 no . . . C(20) C(21) H(35) 109.875 no . . . C(20) C(21) H(36) 109.875 no . . . C(20) C(21) H(37) 108.666 no . . . H(35) C(21) H(36) 109.480 no . . . H(35) C(21) H(37) 109.485 no . . . H(36) C(21) H(37) 109.443 no . . . C(20) C(22) H(38) 109.045 no . . . C(20) C(22) H(39) 109.138 no . . . C(20) C(22) H(40) 110.232 no . . . H(38) C(22) H(39) 109.485 no . . . H(38) C(22) H(40) 109.482 no . . . H(39) C(22) H(40) 109.442 no . . . C(20) C(23) H(41) 109.932 no . . . C(20) C(23) H(42) 109.628 no . . . C(20) C(23) H(43) 108.861 no . . . H(41) C(23) H(42) 109.478 no . . . H(41) C(23) H(43) 109.481 no . . . H(42) C(23) H(43) 109.446 no . . . P(1) C(24) H(44) 109.562 no . . . P(1) C(24) H(45) 108.931 no . . . P(1) C(24) H(46) 109.934 no . . . H(44) C(24) H(45) 109.477 no . . . H(44) C(24) H(46) 109.482 no . . . H(45) C(24) H(46) 109.440 no . . . P(1) C(25) H(47) 109.389 no . . . P(1) C(25) H(48) 109.944 no . . . P(1) C(25) H(49) 109.087 no . . . H(47) C(25) H(48) 109.480 no . . . H(47) C(25) H(49) 109.485 no . . . H(48) C(25) H(49) 109.442 no . . . P(1) C(26) H(50) 109.811 no . . . P(1) C(26) H(51) 108.896 no . . . P(1) C(26) H(52) 109.712 no . . . H(50) C(26) H(51) 109.485 no . . . H(50) C(26) H(52) 109.481 no . . . H(51) C(26) H(52) 109.441 no . . . #============================================================================== # End of CIF #============================================================================== _database_code_depnum_ccdc_archive 'CCDC 949579'