#------------------------------------------------------------------------------ #$Date: 2012-02-26 23:34:47 +0200 (Sun, 26 Feb 2012) $ #$Revision: 35909 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/01/54/7015473.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7015473 loop_ _publ_author_name 'R\"omer, Ren\'e' 'Gradert, Christian' 'Bannwarth, Alexander' 'Peters, Gerhard' 'N\"ather, Christian' 'Tuczek, Felix' _publ_section_title ; One-step synthesis of Mo(0) and W(0) bis(dinitrogen) complexes with the linear tetraphosphine ligand prP4: stereoselective formation of cis-[M(N2)2(rac-prP4)] and trans-[M(N2)2(meso-prP4)]; M = Mo, W. ; _journal_issue 13 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 3229 _journal_page_last 3236 _journal_volume 40 _journal_year 2011 _chemical_formula_sum 'C15 H20 N2 O3' _chemical_formula_weight 276.33 _chemical_name_common Hdapp _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 85.485(6) _cell_angle_beta 78.375(6) _cell_angle_gamma 69.760(5) _cell_formula_units_Z 2 _cell_length_a 7.5438(8) _cell_length_b 9.0878(9) _cell_length_c 11.3719(12) _cell_measurement_reflns_used 3617 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 27.87 _cell_measurement_theta_min 2.39 _cell_volume 716.44(13) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Bruker X8 APEX II' _diffrn_measurement_method 'area deteector' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.0323 _diffrn_reflns_av_sigmaI/netI 0.0316 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 14821 _diffrn_reflns_theta_full 28.13 _diffrn_reflns_theta_max 28.13 _diffrn_reflns_theta_min 1.83 _exptl_absorpt_coefficient_mu 0.090 _exptl_absorpt_correction_T_max 0.996 _exptl_absorpt_correction_T_min 0.894 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker Nonius, 2003)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.281 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 296 _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.246 _refine_diff_density_min -0.213 _refine_diff_density_rms 0.044 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 193 _refine_ls_number_reflns 3490 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.067 _refine_ls_R_factor_all 0.0676 _refine_ls_R_factor_gt 0.0459 _refine_ls_shift/su_max 0.022 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0601P)^2^+0.1306P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1173 _refine_ls_wR_factor_ref 0.1281 _reflns_number_gt 2533 _reflns_number_total 3490 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file c0dt01646b.txt _[local]_cod_data_source_block co335 _cod_database_code 7015473 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 C1 C -0.0354(2) 0.39438(19) 0.76236(14) 0.0343(3) Uani 1 1 d . . . H1A H 0.0315 0.4709 0.7545 0.051 Uiso 1 1 calc R . . H1B H 0.0250 0.3064 0.8130 0.051 Uiso 1 1 calc R . . H1C H -0.1706 0.4446 0.7991 0.051 Uiso 1 1 calc R . . C2 C -0.02311(19) 0.33541(16) 0.64102(12) 0.0253(3) Uani 1 1 d . . . C3 C -0.17080(19) 0.39357(15) 0.57936(12) 0.0258(3) Uani 1 1 d . . . C4 C -0.16317(19) 0.33624(16) 0.46415(12) 0.0263(3) Uani 1 1 d . . . C5 C 0.0102(2) 0.21777(18) 0.41738(13) 0.0322(3) Uani 1 1 d . . . H5 H 0.0259 0.1762 0.3404 0.039 Uiso 1 1 calc R . . C6 C 0.1551(2) 0.16217(18) 0.48062(13) 0.0326(3) Uani 1 1 d . . . H6 H 0.2697 0.0817 0.4469 0.039 Uiso 1 1 calc R . . C7 C 0.29628(19) 0.14620(16) 0.65558(12) 0.0253(3) Uani 1 1 d . . . C8 C 0.3218(2) -0.00196(17) 0.70402(13) 0.0291(3) Uani 1 1 d . . . H8 H 0.2423 -0.0580 0.6905 0.035 Uiso 1 1 calc R . . C9 C 0.4623(2) -0.06910(17) 0.77209(13) 0.0299(3) Uani 1 1 d . . . H9 H 0.4784 -0.1712 0.8052 0.036 Uiso 1 1 calc R . . C10 C 0.58166(19) 0.01082(16) 0.79318(12) 0.0252(3) Uani 1 1 d . . . C11 C 0.5549(2) 0.16000(16) 0.74017(13) 0.0278(3) Uani 1 1 d . . . H11 H 0.6355 0.2163 0.7513 0.033 Uiso 1 1 calc R . . C12 C 0.4144(2) 0.22631(16) 0.67239(13) 0.0288(3) Uani 1 1 d . . . H12 H 0.3989 0.3273 0.6372 0.035 Uiso 1 1 calc R . . C13 C 0.7306(2) -0.19952(19) 0.92735(15) 0.0404(4) Uani 1 1 d . . . H13A H 0.6112 -0.1832 0.9861 0.061 Uiso 1 1 calc R . . H13B H 0.8398 -0.2306 0.9692 0.061 Uiso 1 1 calc R . . H13C H 0.7471 -0.2824 0.8718 0.061 Uiso 1 1 calc R . . C14 C 0.8387(2) 0.0294(2) 0.88660(17) 0.0441(4) Uani 1 1 d . . . H14A H 0.8850 0.0789 0.8127 0.066 Uiso 1 1 calc R . . H14B H 0.9487 -0.0431 0.9185 0.066 Uiso 1 1 calc R . . H14C H 0.7620 0.1104 0.9461 0.066 Uiso 1 1 calc R . . C15 C -0.3171(3) 0.4383(2) 0.10181(15) 0.0500(5) Uani 1 1 d . . . H15A H -0.4546 0.4611 0.1333 0.075 Uiso 1 1 calc R . . H15B H -0.2868 0.4022 0.0188 0.075 Uiso 1 1 calc R . . H15C H -0.2848 0.5335 0.1040 0.075 Uiso 1 1 calc R . . N1 N 0.14098(16) 0.21796(14) 0.59010(10) 0.0264(3) Uani 1 1 d . . . N2 N 0.72161(19) -0.05551(15) 0.86083(12) 0.0355(3) Uani 1 1 d . . . O1 O -0.30534(14) 0.39286(12) 0.41058(9) 0.0328(3) Uani 1 1 d . . . O2 O -0.33095(15) 0.50904(12) 0.63044(10) 0.0356(3) Uani 1 1 d . . . O3 O -0.21082(18) 0.32174(14) 0.17193(11) 0.0449(3) Uani 1 1 d . . . H2O H -0.418(3) 0.526(2) 0.5830(18) 0.060(6) Uiso 1 1 d . . . H3O H -0.252(3) 0.352(2) 0.250(2) 0.071(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0289(8) 0.0391(8) 0.0327(8) -0.0081(6) -0.0076(6) -0.0062(6) C2 0.0226(7) 0.0259(7) 0.0264(7) -0.0001(5) -0.0033(5) -0.0078(5) C3 0.0214(7) 0.0247(7) 0.0287(7) 0.0001(5) -0.0026(6) -0.0058(5) C4 0.0231(7) 0.0299(7) 0.0261(7) 0.0057(5) -0.0069(5) -0.0092(6) C5 0.0283(8) 0.0391(8) 0.0253(7) -0.0046(6) -0.0068(6) -0.0048(6) C6 0.0256(7) 0.0382(8) 0.0280(7) -0.0062(6) -0.0042(6) -0.0024(6) C7 0.0201(7) 0.0287(7) 0.0248(7) -0.0003(5) -0.0061(5) -0.0043(5) C8 0.0256(7) 0.0292(7) 0.0347(8) -0.0001(6) -0.0073(6) -0.0110(6) C9 0.0292(7) 0.0257(7) 0.0346(8) 0.0049(6) -0.0080(6) -0.0091(6) C10 0.0215(7) 0.0271(7) 0.0235(7) -0.0026(5) -0.0029(5) -0.0041(5) C11 0.0245(7) 0.0282(7) 0.0324(7) -0.0002(6) -0.0073(6) -0.0101(6) C12 0.0281(7) 0.0258(7) 0.0324(7) 0.0038(6) -0.0067(6) -0.0093(6) C13 0.0349(9) 0.0400(9) 0.0397(9) 0.0089(7) -0.0126(7) -0.0035(7) C14 0.0373(9) 0.0455(10) 0.0541(11) -0.0023(8) -0.0246(8) -0.0104(8) C15 0.0670(13) 0.0448(10) 0.0335(9) 0.0035(7) -0.0139(9) -0.0113(9) N1 0.0216(6) 0.0305(6) 0.0257(6) -0.0003(5) -0.0064(5) -0.0057(5) N2 0.0342(7) 0.0355(7) 0.0398(7) 0.0065(6) -0.0186(6) -0.0103(6) O1 0.0261(5) 0.0387(6) 0.0314(5) 0.0027(4) -0.0116(4) -0.0051(4) O2 0.0257(5) 0.0369(6) 0.0384(6) -0.0091(5) -0.0101(5) 0.0007(4) O3 0.0455(7) 0.0427(7) 0.0369(7) 0.0002(5) -0.0073(5) -0.0034(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 Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 N1 118.92(12) . . ? C3 C2 C1 121.80(12) . . ? N1 C2 C1 119.28(12) . . ? O2 C3 C2 118.24(12) . . ? O2 C3 C4 119.19(12) . . ? C2 C3 C4 122.56(12) . . ? O1 C4 C5 124.49(13) . . ? O1 C4 C3 120.35(12) . . ? C5 C4 C3 115.15(12) . . ? C6 C5 C4 121.05(13) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? N1 C6 C5 121.94(13) . . ? N1 C6 H6 119.0 . . ? C5 C6 H6 119.0 . . ? C8 C7 C12 120.08(13) . . ? C8 C7 N1 119.26(12) . . ? C12 C7 N1 120.63(12) . . ? C7 C8 C9 120.19(13) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C8 C9 C10 121.07(13) . . ? C8 C9 H9 119.5 . . ? C10 C9 H9 119.5 . . ? N2 C10 C9 121.27(12) . . ? N2 C10 C11 121.43(13) . . ? C9 C10 C11 117.29(12) . . ? C12 C11 C10 121.32(13) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C11 C12 C7 120.00(13) . . ? C11 C12 H12 120.0 . . ? C7 C12 H12 120.0 . . ? N2 C13 H13A 109.5 . . ? N2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N2 C14 H14A 109.5 . . ? N2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O3 C15 H15A 109.5 . . ? O3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C6 N1 C2 120.36(12) . . ? C6 N1 C7 118.86(11) . . ? C2 N1 C7 120.69(11) . . ? C10 N2 C14 121.15(13) . . ? C10 N2 C13 120.47(13) . . ? C14 N2 C13 117.31(13) . . ? C3 O2 H2O 107.1(13) . . ? C15 O3 H3O 108.4(13) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.494(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.3644(19) . ? C2 N1 1.3788(17) . ? C3 O2 1.3544(16) . ? C3 C4 1.431(2) . ? C4 O1 1.2721(16) . ? C4 C5 1.410(2) . ? C5 C6 1.358(2) . ? C5 H5 0.9500 . ? C6 N1 1.3518(18) . ? C6 H6 0.9500 . ? C7 C8 1.378(2) . ? C7 C12 1.379(2) . ? C7 N1 1.4487(17) . ? C8 C9 1.380(2) . ? C8 H8 0.9500 . ? C9 C10 1.401(2) . ? C9 H9 0.9500 . ? C10 N2 1.3725(18) . ? C10 C11 1.4047(19) . ? C11 C12 1.3765(19) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 N2 1.4466(19) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 N2 1.440(2) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 O3 1.392(2) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? O2 H2O 0.90(2) . ? O3 H3O 0.91(2) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 O2 -179.92(12) . . . . ? C1 C2 C3 O2 0.7(2) . . . . ? N1 C2 C3 C4 0.7(2) . . . . ? C1 C2 C3 C4 -178.67(13) . . . . ? O2 C3 C4 O1 -0.2(2) . . . . ? C2 C3 C4 O1 179.19(13) . . . . ? O2 C3 C4 C5 179.11(12) . . . . ? C2 C3 C4 C5 -1.5(2) . . . . ? O1 C4 C5 C6 -179.35(14) . . . . ? C3 C4 C5 C6 1.4(2) . . . . ? C4 C5 C6 N1 -0.5(2) . . . . ? C12 C7 C8 C9 1.7(2) . . . . ? N1 C7 C8 C9 -176.57(12) . . . . ? C7 C8 C9 C10 -0.1(2) . . . . ? C8 C9 C10 N2 179.99(13) . . . . ? C8 C9 C10 C11 -1.3(2) . . . . ? N2 C10 C11 C12 -179.98(13) . . . . ? C9 C10 C11 C12 1.4(2) . . . . ? C10 C11 C12 C7 0.1(2) . . . . ? C8 C7 C12 C11 -1.6(2) . . . . ? N1 C7 C12 C11 176.56(12) . . . . ? C5 C6 N1 C2 -0.4(2) . . . . ? C5 C6 N1 C7 176.12(14) . . . . ? C3 C2 N1 C6 0.3(2) . . . . ? C1 C2 N1 C6 179.69(14) . . . . ? C3 C2 N1 C7 -176.16(12) . . . . ? C1 C2 N1 C7 3.24(19) . . . . ? C8 C7 N1 C6 -71.69(18) . . . . ? C12 C7 N1 C6 110.09(16) . . . . ? C8 C7 N1 C2 104.81(15) . . . . ? C12 C7 N1 C2 -73.41(17) . . . . ? C9 C10 N2 C14 -177.35(14) . . . . ? C11 C10 N2 C14 4.0(2) . . . . ? C9 C10 N2 C13 -9.5(2) . . . . ? C11 C10 N2 C13 171.90(13) . . . . ?