# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # 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_13rwz711b _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2013-07-22 # yyyy-mm-dd _chemical_name_systematic ; trifluorooxidobis(triphenylphosphineoxide)niobium(V) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H30 F3 Nb O3 P2' _chemical_formula_sum 'C36 H30 F3 Nb O3 P2' _chemical_formula_structural '(((C6 H5)3 P O)2 Nb O F3)' _chemical_formula_weight 722.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_name_H-M_alt 'F d d 2' _space_group_IT_number 43 _space_group_name_Hall 'F 2 -2d' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 18.762(9) _cell_length_b 33.289(14) _cell_length_c 10.152(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6340(5) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5625 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 34.6 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2944 _exptl_absorpt_coefficient_mu 0.534 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.861 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, VHF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ Superbright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7136 _diffrn_reflns_av_R_equivalents 0.0849 # _diffrn_reflns_av_sigmaI/netI 0.1458 _diffrn_reflns_av_unetI/netI 0.1458 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3000 _reflns_number_gt 2484 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1997)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. There is an F/O disorder problem. Based on the displacement ellipsoids this was modelled with O1 and F2 disorder the atoms having the same coordinates and ADPs. DELU was used to control the C1 ADP. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0259P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(6) _chemical_absolute_configuration ad _refine_ls_number_reflns 3000 _refine_ls_number_parameters 204 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0888 _refine_ls_R_factor_gt 0.0719 _refine_ls_wR_factor_ref 0.1148 _refine_ls_wR_factor_gt 0.1062 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 0.5000 0.0000 -0.00625(7) 0.0234(3) Uani 1 2 d S . . P1 P 0.40609(10) 0.06746(5) 0.20178(17) 0.0174(4) Uani 1 1 d U . . F1 F 0.5821(2) 0.03443(9) 0.0147(4) 0.0268(10) Uani 1 1 d . . . F2 F 0.4501(3) 0.03513(14) -0.1131(5) 0.0538(16) Uani 0.50 1 d P . . O1 O 0.4501(3) 0.03513(14) -0.1131(5) 0.0538(16) Uani 0.50 1 d P . . O2 O 0.4575(3) 0.03390(11) 0.1610(4) 0.0199(11) Uani 1 1 d U . . C1 C 0.4210(4) 0.08070(18) 0.3713(6) 0.0146(13) Uani 1 1 d U . . C2 C 0.4588(4) 0.05425(19) 0.4509(7) 0.0249(16) Uani 1 1 d U . . H2 H 0.4772 0.0300 0.4153 0.030 Uiso 1 1 calc R . . C3 C 0.4698(5) 0.0636(2) 0.5840(7) 0.037(2) Uani 1 1 d U . . H3 H 0.4953 0.0455 0.6387 0.044 Uiso 1 1 calc R . . C4 C 0.4438(4) 0.0985(2) 0.6353(7) 0.033(2) Uani 1 1 d . . . H4 H 0.4511 0.1044 0.7259 0.040 Uiso 1 1 calc R . . C5 C 0.4075(4) 0.12523(19) 0.5580(7) 0.0297(19) Uani 1 1 d U . . H5 H 0.3896 0.1494 0.5948 0.036 Uiso 1 1 calc R . . C6 C 0.3969(4) 0.11684(18) 0.4260(6) 0.0214(16) Uani 1 1 d U . . H6 H 0.3731 0.1358 0.3718 0.026 Uiso 1 1 calc R . . C7 C 0.3155(4) 0.05167(17) 0.1919(6) 0.0168(14) Uani 1 1 d U . . C8 C 0.2761(4) 0.04031(17) 0.3043(6) 0.0185(16) Uani 1 1 d . . . H8 H 0.2971 0.0430 0.3890 0.022 Uiso 1 1 calc R . . C9 C 0.2071(4) 0.02524(16) 0.2939(7) 0.0200(17) Uani 1 1 d . . . H9 H 0.1812 0.0178 0.3706 0.024 Uiso 1 1 calc R . . C10 C 0.1763(4) 0.02116(17) 0.1693(7) 0.0246(19) Uani 1 1 d . . . H10 H 0.1294 0.0107 0.1613 0.029 Uiso 1 1 calc R . . C11 C 0.2138(4) 0.03232(17) 0.0568(7) 0.0230(17) Uani 1 1 d . . . H11 H 0.1924 0.0292 -0.0274 0.028 Uiso 1 1 calc R . . C12 C 0.2810(4) 0.04775(19) 0.0663(7) 0.0271(19) Uani 1 1 d . . . H12 H 0.3053 0.0560 -0.0112 0.033 Uiso 1 1 calc R . . C13 C 0.4174(4) 0.11192(17) 0.1025(6) 0.0149(15) Uani 1 1 d U . . C14 C 0.3620(4) 0.13944(16) 0.0867(6) 0.0210(17) Uani 1 1 d . . . H14 H 0.3164 0.1336 0.1226 0.025 Uiso 1 1 calc R . . C15 C 0.3725(4) 0.17494(17) 0.0199(7) 0.0207(16) Uani 1 1 d . . . H15 H 0.3349 0.1939 0.0117 0.025 Uiso 1 1 calc R . . C16 C 0.4397(4) 0.18284(17) -0.0361(6) 0.0193(16) Uani 1 1 d . . . H16 H 0.4469 0.2066 -0.0861 0.023 Uiso 1 1 calc R . . C17 C 0.4948(4) 0.15619(16) -0.0187(9) 0.0239(17) Uani 1 1 d . . . H17 H 0.5404 0.1622 -0.0544 0.029 Uiso 1 1 calc R . . C18 C 0.4848(4) 0.12102(19) 0.0498(6) 0.0225(17) Uani 1 1 d . . . H18 H 0.5234 0.1029 0.0615 0.027 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nb1 0.0230(6) 0.0333(5) 0.0138(4) 0.000 0.000 -0.0116(5) P1 0.0142(11) 0.0176(9) 0.0204(9) 0.0052(7) 0.0022(8) -0.0002(8) F1 0.022(3) 0.035(2) 0.024(2) -0.0074(18) 0.008(2) -0.0070(18) F2 0.039(4) 0.068(3) 0.055(3) 0.051(3) -0.035(3) -0.027(3) O1 0.039(4) 0.068(3) 0.055(3) 0.051(3) -0.035(3) -0.027(3) O2 0.016(3) 0.022(2) 0.021(3) 0.0001(18) 0.005(2) 0.001(2) C1 0.004(4) 0.022(3) 0.017(3) 0.002(2) 0.000(3) -0.004(3) C2 0.018(4) 0.031(4) 0.026(3) 0.007(3) 0.006(3) 0.009(3) C3 0.030(6) 0.053(5) 0.028(4) 0.016(4) -0.009(4) -0.008(4) C4 0.032(6) 0.048(5) 0.020(4) 0.000(4) 0.007(4) -0.008(4) C5 0.038(6) 0.019(4) 0.032(4) -0.005(3) -0.006(4) -0.005(4) C6 0.029(5) 0.016(3) 0.019(3) 0.010(2) 0.002(4) -0.004(3) C7 0.012(3) 0.018(3) 0.021(3) 0.000(3) 0.001(3) 0.003(2) C8 0.019(4) 0.017(3) 0.019(4) 0.004(3) -0.001(3) 0.001(3) C9 0.019(5) 0.011(3) 0.030(4) -0.003(3) -0.004(3) -0.001(3) C10 0.017(5) 0.011(3) 0.046(5) 0.000(3) 0.004(4) 0.000(3) C11 0.018(5) 0.025(4) 0.026(4) -0.002(3) 0.001(4) -0.003(3) C12 0.019(5) 0.033(4) 0.029(4) 0.001(3) 0.007(4) 0.000(4) C13 0.014(4) 0.019(3) 0.012(3) 0.004(2) 0.003(3) 0.001(3) C14 0.034(5) 0.010(3) 0.019(4) -0.004(3) 0.004(4) -0.006(3) C15 0.013(4) 0.021(3) 0.027(4) 0.002(3) -0.005(3) 0.002(3) C16 0.020(4) 0.010(3) 0.028(4) 0.003(3) 0.004(3) -0.006(3) C17 0.017(4) 0.019(3) 0.036(5) 0.001(4) 0.006(3) -0.004(3) C18 0.018(4) 0.029(4) 0.020(4) 0.001(3) -0.001(3) 0.011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 O1 1.850(4) 2_655 ? Nb1 F2 1.850(4) 2_655 ? Nb1 F2 1.850(4) . ? Nb1 F1 1.932(4) . ? Nb1 F1 1.932(4) 2_655 ? Nb1 O2 2.189(4) 2_655 ? Nb1 O2 2.189(4) . ? P1 O2 1.532(4) . ? P1 C7 1.782(7) . ? P1 C1 1.798(6) . ? P1 C13 1.803(6) . ? C1 C2 1.390(8) . ? C1 C6 1.400(8) . ? C2 C3 1.401(9) . ? C2 H2 0.9500 . ? C3 C4 1.365(10) . ? C3 H3 0.9500 . ? C4 C5 1.368(9) . ? C4 H4 0.9500 . ? C5 C6 1.383(8) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.411(8) . ? C7 C12 1.435(8) . ? C8 C9 1.393(9) . ? C8 H8 0.9500 . ? C9 C10 1.397(8) . ? C9 H9 0.9500 . ? C10 C11 1.392(8) . ? C10 H10 0.9500 . ? C11 C12 1.366(9) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.395(9) . ? C13 C18 1.406(9) . ? C14 C15 1.377(7) . ? C14 H14 0.9500 . ? C15 C16 1.408(8) . ? C15 H15 0.9500 . ? C16 C17 1.375(8) . ? C16 H16 0.9500 . ? C17 C18 1.374(8) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? 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 # O1 Nb1 F2 0.0(4) 2_655 2_655 ? O1 Nb1 F2 108.2(4) 2_655 . ? F2 Nb1 F2 108.2(4) 2_655 . ? O1 Nb1 F1 92.06(19) 2_655 . ? F2 Nb1 F1 92.06(19) 2_655 . ? F2 Nb1 F1 95.36(18) . . ? O1 Nb1 F1 95.36(18) 2_655 2_655 ? F2 Nb1 F1 95.36(18) 2_655 2_655 ? F2 Nb1 F1 92.06(19) . 2_655 ? F1 Nb1 F1 167.3(2) . 2_655 ? O1 Nb1 O2 86.8(2) 2_655 2_655 ? F2 Nb1 O2 86.8(2) 2_655 2_655 ? F2 Nb1 O2 164.9(2) . 2_655 ? F1 Nb1 O2 85.97(17) . 2_655 ? F1 Nb1 O2 84.23(16) 2_655 2_655 ? O1 Nb1 O2 164.9(2) 2_655 . ? F2 Nb1 O2 164.9(2) 2_655 . ? F2 Nb1 O2 86.8(2) . . ? F1 Nb1 O2 84.23(16) . . ? F1 Nb1 O2 85.97(17) 2_655 . ? O2 Nb1 O2 78.3(2) 2_655 . ? O2 P1 C7 111.7(3) . . ? O2 P1 C1 109.8(3) . . ? C7 P1 C1 105.9(3) . . ? O2 P1 C13 111.9(3) . . ? C7 P1 C13 108.8(3) . . ? C1 P1 C13 108.4(3) . . ? P1 O2 Nb1 144.5(3) . . ? C2 C1 C6 118.6(6) . . ? C2 C1 P1 118.7(5) . . ? C6 C1 P1 122.7(5) . . ? C1 C2 C3 119.7(7) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C4 C3 C2 120.3(7) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 120.8(7) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C4 C5 C6 119.8(7) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C5 C6 C1 120.8(6) . . ? C5 C6 H6 119.6 . . ? C1 C6 H6 119.6 . . ? C8 C7 C12 117.3(6) . . ? C8 C7 P1 122.2(5) . . ? C12 C7 P1 120.4(5) . . ? C9 C8 C7 121.5(7) . . ? C9 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C10 C9 C8 119.2(7) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C11 C10 C9 120.6(7) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C12 C11 C10 120.6(7) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C7 120.9(7) . . ? C11 C12 H12 119.6 . . ? C7 C12 H12 119.6 . . ? C14 C13 C18 119.1(6) . . ? C14 C13 P1 121.0(5) . . ? C18 C13 P1 119.7(5) . . ? C15 C14 C13 120.9(7) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 119.2(6) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? C17 C16 C15 120.1(6) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 120.8(7) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C17 C18 C13 119.9(6) . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.045 _refine_diff_density_min -0.495 _refine_diff_density_rms 0.109 _iucr_refine_instruction_details ; Add final .res file here for Acta Cryst publications or if required. ; _database_code_depnum_ccdc_archive 'CCDC 973570' ####################################################################### # # 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_13rwz1003d _audit_creation_method 'SHELXL-2013 + hand edit' _audit_creation_date 2013-12-18 # yyyy-mm-dd _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H18 F3 Nb O3 P2, 0.33(C H2 Cl2)' _chemical_formula_sum 'C6.33 H18.67 Cl0.67 F3 Nb O3 P2' _chemical_formula_weight 378.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.8890(15) _cell_length_b 14.584(3) _cell_length_c 20.046(4) _cell_angle_alpha 102.497(4) _cell_angle_beta 99.803(4) _cell_angle_gamma 97.324(2) _cell_volume 2186.3(7) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8711 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 34.8 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.724 _exptl_crystal_F_000 1140 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.040 _exptl_crystal_size_mid 0.030 _exptl_crystal_size_min 0.030 _exptl_absorpt_coefficient_mu 1.191 _shelx_estimated_absorpt_T_min 0.954 _shelx_estimated_absorpt_T_max 0.965 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.925 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ; Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_source_power 2.475 _diffrn_source_voltage 45.0 _diffrn_source_current 55.0 _diffrn_source 'Rotating Anode' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_collimation 'Confocal mirrors, VHF Varimax ' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean 28.5714 _diffrn_measurement_device 'four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 (Right)' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_measurement_specimen_support 'MiTeGen MicroMesh' _diffrn_reflns_number 22109 _diffrn_reflns_av_unetI/netI 0.0396 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.065 _diffrn_reflns_theta_max 27.483 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_point_group_measured_fraction_full 0.995 _reflns_number_total 9978 _reflns_number_gt 8802 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ; CrystalClear-SM Expert 3.1 (Rigaku, 2013) ; _computing_cell_refinement ; CrystalClear-SM Expert 3.1 (Rigaku, 2013) ; _computing_data_reduction ; CrystalClear-SM Expert 3.1 (Rigaku, 2013) ; _computing_structure_solution 'SHELXS-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics ; Images generated using CrystalMaker: a crystal and molecular structures program for Mac and Windows. CrystalMaker Software Ltd, Oxford, England (www.crystalmaker.com) ; _computing_publication_material 'WINGX (Farrugia, 2013)' _refine_special_details ; Molecule 3 (NB3) was refined with a whole molecule disorder model (PART 1 & PART 2). The occupancy for PART1 refined to ca. 0.49 and the occupancies for both parts were subsequently fixed at 0.5. Geometry restraints were applied (SAME with default esd) to restrain the geometry of the 2 parts to be similar to molecule 1 (NB1). The ADPs for the carbon atoms were constrained to be equal for atoms pairs A & B, and SIMU & DELU restraints with default esd were applied to the whole model. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0417P)^2^+2.0239P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 9978 _refine_ls_number_parameters 556 _refine_ls_number_restraints 752 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.0880 _refine_ls_wR_factor_gt 0.0847 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.172 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 1.05898(3) 0.14528(2) 0.23827(2) 0.01946(7) Uani 1 1 d D U . . . F1 F 1.0113(3) 0.04587(14) 0.28616(10) 0.0347(5) Uani 1 1 d D U . . . F2 F 1.2628(2) 0.20321(15) 0.30376(10) 0.0341(5) Uani 1 1 d D U . . . F3 F 1.0576(3) 0.25366(13) 0.19841(9) 0.0290(4) Uani 1 1 d D U . . . O1 O 1.1540(3) 0.07530(16) 0.17555(11) 0.0251(5) Uani 1 1 d D U . . . O2 O 0.8063(2) 0.09487(15) 0.17689(10) 0.0191(4) Uani 1 1 d D U . . . O3 O 0.9116(2) 0.22108(15) 0.31007(10) 0.0191(4) Uani 1 1 d D U . . . P1 P 0.61626(9) 0.10148(5) 0.17962(4) 0.01508(14) Uani 1 1 d D U . . . C1 C 0.4806(4) 0.0392(2) 0.09772(15) 0.0228(6) Uani 1 1 d D U . . . H1A H 0.5104 0.0696 0.0612 0.034 Uiso 1 1 calc R U . . . H1B H 0.3579 0.0411 0.1001 0.034 Uiso 1 1 calc R U . . . H1C H 0.4987 -0.0272 0.0868 0.034 Uiso 1 1 calc R U . . . C2 C 0.5798(4) 0.2218(2) 0.19378(17) 0.0241(6) Uani 1 1 d D U . . . H2A H 0.6561 0.2599 0.2374 0.036 Uiso 1 1 calc R U . . . H2B H 0.4576 0.2236 0.1969 0.036 Uiso 1 1 calc R U . . . H2C H 0.6056 0.2480 0.1548 0.036 Uiso 1 1 calc R U . . . C3 C 0.5502(4) 0.0488(2) 0.24542(16) 0.0230(6) Uani 1 1 d D U . . . H3A H 0.5462 -0.0203 0.2317 0.035 Uiso 1 1 calc R U . . . H3B H 0.4341 0.0620 0.2511 0.035 Uiso 1 1 calc R U . . . H3C H 0.6339 0.0756 0.2897 0.035 Uiso 1 1 calc R U . . . P2 P 0.92456(10) 0.26345(5) 0.38763(4) 0.01752(15) Uani 1 1 d D U . . . C4 C 0.7447(4) 0.3239(2) 0.40043(17) 0.0259(7) Uani 1 1 d D U . . . H4A H 0.7499 0.3775 0.3782 0.039 Uiso 1 1 calc R U . . . H4B H 0.7507 0.3478 0.4505 0.039 Uiso 1 1 calc R U . . . H4C H 0.6348 0.2795 0.3796 0.039 Uiso 1 1 calc R U . . . C5 C 1.1208(4) 0.3476(2) 0.42481(16) 0.0236(6) Uani 1 1 d D U . . . H5A H 1.2218 0.3158 0.4197 0.035 Uiso 1 1 calc R U . . . H5B H 1.1243 0.3738 0.4744 0.035 Uiso 1 1 calc R U . . . H5C H 1.1241 0.3993 0.4007 0.035 Uiso 1 1 calc R U . . . C6 C 0.9183(4) 0.1723(2) 0.43468(16) 0.0253(6) Uani 1 1 d D U . . . H6A H 0.8049 0.1299 0.4187 0.038 Uiso 1 1 calc R U . . . H6B H 0.9350 0.2016 0.4847 0.038 Uiso 1 1 calc R U . . . H6C H 1.0114 0.1354 0.4264 0.038 Uiso 1 1 calc R U . . . Nb2 Nb 0.97841(3) -0.37610(2) 0.36522(2) 0.01947(7) Uani 1 1 d . U . . . F4 F 1.1926(2) -0.30535(14) 0.42821(10) 0.0318(4) Uani 1 1 d . U . . . F5 F 0.9462(3) -0.45901(16) 0.42208(13) 0.0481(6) Uani 1 1 d . U . . . F6 F 0.8042(2) -0.45376(17) 0.28866(12) 0.0468(6) Uani 1 1 d . U . . . O4 O 0.8431(2) -0.29534(14) 0.39758(11) 0.0186(4) Uani 1 1 d . U . . . O5 O 1.1545(2) -0.46533(14) 0.32130(10) 0.0185(4) Uani 1 1 d . U . . . O6 O 1.0468(3) -0.29150(17) 0.29784(13) 0.0339(6) Uani 1 1 d . U . . . P3 P 1.34830(9) -0.46125(5) 0.32188(4) 0.01557(14) Uani 1 1 d . U . . . C7 C 1.3859(4) -0.5698(2) 0.27127(17) 0.0240(6) Uani 1 1 d . U . . . H7A H 1.3446 -0.6226 0.2907 0.036 Uiso 1 1 calc R U . . . H7B H 1.5112 -0.5664 0.2722 0.036 Uiso 1 1 calc R U . . . H7C H 1.3228 -0.5803 0.2230 0.036 Uiso 1 1 calc R U . . . C8 C 1.4715(4) -0.4464(2) 0.40834(16) 0.0230(6) Uani 1 1 d . U . . . H8A H 1.4538 -0.3874 0.4385 0.034 Uiso 1 1 calc R U . . . H8B H 1.5957 -0.4431 0.4071 0.034 Uiso 1 1 calc R U . . . H8C H 1.4323 -0.5006 0.4268 0.034 Uiso 1 1 calc R U . . . C9 C 1.4324(4) -0.3660(2) 0.28720(16) 0.0209(6) Uani 1 1 d . U . . . H9A H 1.3674 -0.3737 0.2395 0.031 Uiso 1 1 calc R U . . . H9B H 1.5562 -0.3669 0.2866 0.031 Uiso 1 1 calc R U . . . H9C H 1.4199 -0.3050 0.3164 0.031 Uiso 1 1 calc R U . . . P4 P 1.03397(11) -0.18923(6) 0.29247(5) 0.02625(18) Uani 1 1 d . U . . . C10 C 1.0933(5) -0.1050(3) 0.37584(18) 0.0333(8) Uani 1 1 d . U . . . H10A H 1.0143 -0.1216 0.4058 0.050 Uiso 1 1 calc R U . . . H10B H 1.0844 -0.0409 0.3696 0.050 Uiso 1 1 calc R U . . . H10C H 1.2135 -0.1067 0.3976 0.050 Uiso 1 1 calc R U . . . C11 C 0.8159(4) -0.1793(3) 0.25568(19) 0.0332(8) Uani 1 1 d . U . . . H11A H 0.7755 -0.2263 0.2108 0.050 Uiso 1 1 calc R U . . . H11B H 0.8139 -0.1151 0.2486 0.050 Uiso 1 1 calc R U . . . H11C H 0.7389 -0.1913 0.2875 0.050 Uiso 1 1 calc R U . . . C12 C 1.1758(5) -0.1544(3) 0.2390(2) 0.0380(9) Uani 1 1 d . U . . . H12A H 1.2972 -0.1515 0.2618 0.057 Uiso 1 1 calc R U . . . H12B H 1.1591 -0.0915 0.2318 0.057 Uiso 1 1 calc R U . . . H12C H 1.1494 -0.2010 0.1937 0.057 Uiso 1 1 calc R U . . . Nb3A Nb 0.6379(6) 0.2805(4) 0.9408(3) 0.0283(9) Uani 0.5 1 d D U P A 1 F7A F 0.7354(12) 0.3487(5) 0.8775(4) 0.0227(14) Uani 0.5 1 d D U P A 1 F8A F 0.6015(7) 0.1687(3) 0.8859(2) 0.0375(10) Uani 0.5 1 d D U P A 1 F9A F 0.5784(5) 0.1857(3) 0.9983(2) 0.0242(7) Uani 0.5 1 d D U P A 1 O7A O 0.4317(8) 0.3157(5) 0.9237(3) 0.0314(14) Uani 0.5 1 d D U P A 1 O8A O 0.9142(6) 0.2672(4) 0.9727(3) 0.0267(10) Uani 0.5 1 d D U P A 1 O9A O 0.7830(6) 0.3620(3) 1.0388(2) 0.0276(9) Uani 0.5 1 d D U P A 1 P5A P 1.0268(16) 0.1971(9) 0.9908(7) 0.0168(14) Uani 0.5 1 d D U P A 1 C13A C 1.105(2) 0.1337(15) 0.9199(8) 0.022(2) Uani 0.5 1 d D U P A 1 H13A H 1.0064 0.1009 0.8820 0.034 Uiso 0.5 1 calc R U P A 1 H13B H 1.1710 0.0867 0.9352 0.034 Uiso 0.5 1 calc R U P A 1 H13C H 1.1817 0.1783 0.9033 0.034 Uiso 0.5 1 calc R U P A 1 C14A C 0.923(4) 0.109(2) 1.0276(17) 0.0247(16) Uani 0.5 1 d D U P A 1 H14A H 0.8413 0.1369 1.0547 0.037 Uiso 0.5 1 calc R U P A 1 H14B H 1.0113 0.0874 1.0583 0.037 Uiso 0.5 1 calc R U P A 1 H14C H 0.8586 0.0548 0.9900 0.037 Uiso 0.5 1 calc R U P A 1 C15A C 1.2180(9) 0.2561(5) 1.0564(4) 0.0222(11) Uani 0.5 1 d D U P A 1 H15A H 1.2746 0.3108 1.0425 0.033 Uiso 0.5 1 calc R U P A 1 H15B H 1.2996 0.2114 1.0611 0.033 Uiso 0.5 1 calc R U P A 1 H15C H 1.1839 0.2781 1.1011 0.033 Uiso 0.5 1 calc R U P A 1 P6A P 0.7971(16) 0.4616(8) 1.0882(6) 0.0210(14) Uani 0.5 1 d D U P A 1 C16A C 0.603(3) 0.474(2) 1.1193(14) 0.0296(12) Uani 0.5 1 d D U P A 1 H16A H 0.5071 0.4694 1.0800 0.044 Uiso 0.5 1 calc R U P A 1 H16B H 0.6187 0.5365 1.1522 0.044 Uiso 0.5 1 calc R U P A 1 H16C H 0.5763 0.4237 1.1430 0.044 Uiso 0.5 1 calc R U P A 1 C17A C 0.8429(8) 0.5486(4) 1.0395(3) 0.0268(9) Uani 0.5 1 d D U P A 1 H17A H 0.9533 0.5421 1.0242 0.040 Uiso 0.5 1 calc R U P A 1 H17B H 0.8522 0.6127 1.0692 0.040 Uiso 0.5 1 calc R U P A 1 H17C H 0.7484 0.5383 0.9986 0.040 Uiso 0.5 1 calc R U P A 1 C18A C 0.9814(9) 0.4791(5) 1.1571(3) 0.0306(10) Uani 0.5 1 d D U P A 1 H18A H 0.9732 0.4255 1.1792 0.046 Uiso 0.5 1 calc R U P A 1 H18B H 0.9845 0.5384 1.1918 0.046 Uiso 0.5 1 calc R U P A 1 H18C H 1.0882 0.4831 1.1383 0.046 Uiso 0.5 1 calc R U P A 1 Nb3B Nb 0.6332(6) 0.2880(4) 0.9453(3) 0.0210(5) Uani 0.5 1 d . U P B 2 F7B F 0.7186(12) 0.3698(5) 0.8960(4) 0.0255(14) Uani 0.5 1 d . U P B 2 F8B F 0.5241(6) 0.1861(3) 0.8609(2) 0.0334(9) Uani 0.5 1 d . U P B 2 F9B F 0.6157(5) 0.2476(3) 1.02635(19) 0.0249(8) Uani 0.5 1 d . U P B 2 O7B O 0.4442(7) 0.3344(4) 0.9571(3) 0.0211(11) Uani 0.5 1 d . U P B 2 O8B O 0.8730(6) 0.2238(4) 0.9393(2) 0.0188(9) Uani 0.5 1 d . U P B 2 O9B O 0.7490(6) 0.4265(3) 1.0147(2) 0.0260(9) Uani 0.5 1 d . U P B 2 P5B P 1.0157(16) 0.1887(10) 0.9848(7) 0.0178(15) Uani 0.5 1 d . U P B 2 C13B C 1.141(3) 0.1246(15) 0.9288(8) 0.022(2) Uani 0.5 1 d . U P B 2 H13D H 1.0649 0.0693 0.8959 0.034 Uiso 0.5 1 calc R U P B 2 H13E H 1.2347 0.1031 0.9573 0.034 Uiso 0.5 1 calc R U P B 2 H13F H 1.1928 0.1668 0.9029 0.034 Uiso 0.5 1 calc R U P B 2 C14B C 0.919(4) 0.115(2) 1.0321(17) 0.0247(16) Uani 0.5 1 d . U P B 2 H14D H 0.8933 0.1550 1.0741 0.037 Uiso 0.5 1 calc R U P B 2 H14E H 0.9991 0.0733 1.0457 0.037 Uiso 0.5 1 calc R U P B 2 H14F H 0.8100 0.0765 1.0029 0.037 Uiso 0.5 1 calc R U P B 2 C15B C 1.1622(9) 0.2821(5) 1.0466(4) 0.0222(11) Uani 0.5 1 d . U P B 2 H15D H 1.2000 0.3318 1.0237 0.033 Uiso 0.5 1 calc R U P B 2 H15E H 1.2640 0.2574 1.0664 0.033 Uiso 0.5 1 calc R U P B 2 H15F H 1.1039 0.3091 1.0839 0.033 Uiso 0.5 1 calc R U P B 2 P6B P 0.7830(17) 0.4714(9) 1.0912(6) 0.0227(15) Uani 0.5 1 d . U P B 2 C16B C 0.584(3) 0.473(2) 1.1235(14) 0.0296(12) Uani 0.5 1 d . U P B 2 H16D H 0.5203 0.5191 1.1063 0.044 Uiso 0.5 1 calc R U P B 2 H16E H 0.6121 0.4905 1.1747 0.044 Uiso 0.5 1 calc R U P B 2 H16F H 0.5122 0.4091 1.1072 0.044 Uiso 0.5 1 calc R U P B 2 C17B C 0.8875(8) 0.5920(4) 1.1137(3) 0.0268(9) Uani 0.5 1 d . U P B 2 H17D H 0.9937 0.5970 1.0946 0.040 Uiso 0.5 1 calc R U P B 2 H17E H 0.9182 0.6150 1.1647 0.040 Uiso 0.5 1 calc R U P B 2 H17F H 0.8084 0.6307 1.0944 0.040 Uiso 0.5 1 calc R U P B 2 C18B C 0.9186(9) 0.4112(5) 1.1426(3) 0.0306(10) Uani 0.5 1 d . U P B 2 H18D H 0.8673 0.3435 1.1317 0.046 Uiso 0.5 1 calc R U P B 2 H18E H 0.9269 0.4396 1.1923 0.046 Uiso 0.5 1 calc R U P B 2 H18F H 1.0355 0.4177 1.1318 0.046 Uiso 0.5 1 calc R U P B 2 Cl1 Cl 0.37885(17) 0.07140(9) 0.56960(7) 0.0612(3) Uani 1 1 d . U . . . Cl2 Cl 0.39367(12) 0.14664(8) 0.44601(5) 0.0444(2) Uani 1 1 d . U . . . C19 C 0.4283(5) 0.1727(3) 0.5371(2) 0.0371(8) Uani 1 1 d . U . . . H19A H 0.3552 0.2200 0.5532 0.045 Uiso 1 1 calc R U . . . H19B H 0.5520 0.2020 0.5568 0.045 Uiso 1 1 calc R U . . . 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 Nb1 0.01307(12) 0.02402(15) 0.02548(14) 0.00937(11) 0.00817(10) 0.00711(10) F1 0.0482(12) 0.0267(10) 0.0337(11) 0.0139(9) 0.0082(9) 0.0117(9) F2 0.0192(9) 0.0478(13) 0.0262(10) -0.0053(9) -0.0009(7) 0.0044(8) F3 0.0392(11) 0.0231(10) 0.0236(9) 0.0082(8) 0.0075(8) -0.0047(8) O1 0.0114(9) 0.0373(13) 0.0206(10) -0.0071(9) 0.0007(8) 0.0097(9) O2 0.0115(9) 0.0233(11) 0.0188(10) -0.0016(8) 0.0028(7) 0.0018(8) O3 0.0176(10) 0.0249(11) 0.0136(9) 0.0008(8) 0.0041(7) 0.0041(8) P1 0.0111(3) 0.0160(3) 0.0164(3) 0.0007(3) 0.0021(3) 0.0023(3) C1 0.0141(13) 0.0269(16) 0.0217(14) -0.0039(12) 0.0014(11) 0.0025(12) C2 0.0226(15) 0.0173(14) 0.0295(16) 0.0033(12) -0.0002(12) 0.0050(12) C3 0.0168(14) 0.0287(17) 0.0251(15) 0.0084(13) 0.0055(11) 0.0039(12) P2 0.0185(3) 0.0188(4) 0.0154(3) 0.0027(3) 0.0054(3) 0.0039(3) C4 0.0256(15) 0.0283(17) 0.0249(16) 0.0030(13) 0.0086(12) 0.0096(13) C5 0.0248(15) 0.0213(15) 0.0212(15) 0.0013(12) 0.0036(12) -0.0004(12) C6 0.0324(17) 0.0215(16) 0.0220(15) 0.0071(12) 0.0057(13) 0.0014(13) Nb2 0.01278(12) 0.02505(15) 0.01794(13) 0.00061(10) 0.00488(9) -0.00086(10) F4 0.0205(9) 0.0336(11) 0.0312(10) -0.0086(8) -0.0021(8) 0.0064(8) F5 0.0703(16) 0.0347(12) 0.0609(15) 0.0267(11) 0.0425(13) 0.0232(11) F6 0.0182(9) 0.0514(14) 0.0492(13) -0.0250(11) -0.0044(9) 0.0061(9) O4 0.0158(9) 0.0165(10) 0.0247(10) 0.0019(8) 0.0088(8) 0.0057(8) O5 0.0131(9) 0.0176(10) 0.0225(10) -0.0005(8) 0.0040(8) 0.0027(8) O6 0.0503(15) 0.0333(13) 0.0311(13) 0.0162(11) 0.0230(11) 0.0212(11) P3 0.0116(3) 0.0150(3) 0.0196(3) 0.0023(3) 0.0039(3) 0.0026(3) C7 0.0176(14) 0.0181(15) 0.0354(17) -0.0004(13) 0.0098(12) 0.0055(11) C8 0.0181(14) 0.0291(17) 0.0219(14) 0.0084(13) 0.0025(11) 0.0029(12) C9 0.0145(13) 0.0212(15) 0.0280(15) 0.0085(12) 0.0040(11) 0.0025(11) P4 0.0309(4) 0.0288(4) 0.0272(4) 0.0137(4) 0.0138(3) 0.0128(3) C10 0.043(2) 0.0312(18) 0.0278(17) 0.0121(14) 0.0048(15) 0.0080(15) C11 0.0277(17) 0.038(2) 0.0377(19) 0.0167(16) 0.0068(14) 0.0068(15) C12 0.0363(19) 0.045(2) 0.046(2) 0.0243(18) 0.0253(17) 0.0122(17) Nb3A 0.0277(11) 0.0434(17) 0.0192(12) 0.0143(13) 0.0067(7) 0.0122(9) F7A 0.033(3) 0.020(3) 0.017(3) 0.003(2) 0.006(2) 0.010(2) F8A 0.049(3) 0.025(2) 0.032(2) -0.0012(18) 0.006(2) 0.000(2) F9A 0.0246(18) 0.025(2) 0.0271(19) 0.0132(17) 0.0097(15) 0.0029(16) O7A 0.019(2) 0.037(4) 0.042(4) 0.014(3) 0.006(3) 0.013(2) O8A 0.017(2) 0.028(3) 0.041(3) 0.022(2) 0.005(2) 0.0045(19) O9A 0.029(2) 0.028(2) 0.021(2) -0.0025(18) 0.0007(17) 0.0067(18) P5A 0.017(3) 0.015(2) 0.021(2) 0.010(2) 0.0047(18) 0.0007(15) C13A 0.037(7) 0.022(3) 0.012(3) 0.009(3) 0.002(4) 0.013(3) C14A 0.0253(18) 0.025(3) 0.022(3) 0.010(2) 0.000(2) -0.002(2) C15A 0.013(3) 0.031(3) 0.020(2) 0.002(2) 0.003(2) 0.0032(19) P6A 0.021(2) 0.0141(19) 0.027(2) 0.0064(15) 0.0043(14) -0.0014(19) C16A 0.029(3) 0.031(2) 0.029(2) 0.005(2) 0.010(2) 0.007(2) C17A 0.026(2) 0.023(2) 0.030(2) 0.0040(19) 0.0066(18) -0.0016(18) C18A 0.031(3) 0.031(2) 0.024(2) -0.003(2) -0.0007(19) 0.012(2) Nb3B 0.0166(8) 0.0323(8) 0.0130(7) 0.0010(5) -0.0006(6) 0.0127(6) F7B 0.022(2) 0.017(3) 0.039(4) 0.010(3) 0.005(3) 0.006(2) F8B 0.027(2) 0.034(2) 0.033(2) -0.0002(18) -0.0006(18) 0.0034(18) F9B 0.0275(19) 0.029(2) 0.0213(18) 0.0093(17) 0.0113(15) 0.0034(17) O7B 0.015(2) 0.021(3) 0.032(3) 0.007(3) 0.012(2) 0.0116(19) O8B 0.019(2) 0.026(3) 0.016(2) 0.0074(18) 0.0072(17) 0.0086(19) O9B 0.036(2) 0.021(2) 0.020(2) 0.0023(17) 0.0119(18) 0.0013(18) P5B 0.0090(17) 0.018(3) 0.025(3) 0.0044(15) 0.0016(14) 0.0032(17) C13B 0.037(7) 0.022(3) 0.012(3) 0.009(3) 0.002(4) 0.013(3) C14B 0.0253(18) 0.025(3) 0.022(3) 0.010(2) 0.000(2) -0.002(2) C15B 0.013(3) 0.031(3) 0.020(2) 0.002(2) 0.003(2) 0.0032(19) P6B 0.023(2) 0.022(3) 0.0197(19) 0.0040(15) -0.0029(17) 0.0038(15) C16B 0.029(3) 0.031(2) 0.029(2) 0.005(2) 0.010(2) 0.007(2) C17B 0.026(2) 0.023(2) 0.030(2) 0.0040(19) 0.0066(18) -0.0016(18) C18B 0.031(3) 0.031(2) 0.024(2) -0.003(2) -0.0007(19) 0.012(2) Cl1 0.0758(8) 0.0523(7) 0.0751(8) 0.0316(6) 0.0404(7) 0.0218(6) Cl2 0.0364(5) 0.0500(6) 0.0487(6) 0.0144(5) 0.0095(4) 0.0094(4) C19 0.0289(18) 0.0284(19) 0.053(2) 0.0043(17) 0.0115(16) 0.0069(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 O1 1.773(2) . ? Nb1 F2 1.8649(18) . ? Nb1 F3 1.9197(18) . ? Nb1 F1 1.9367(18) . ? Nb1 O2 2.1043(19) . ? Nb1 O3 2.2034(19) . ? O2 P1 1.524(2) . ? O3 P2 1.524(2) . ? P1 C3 1.781(3) . ? P1 C1 1.782(3) . ? P1 C2 1.784(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? P2 C5 1.785(3) . ? P2 C6 1.790(3) . ? P2 C4 1.790(3) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? Nb2 O4 1.7813(19) . ? Nb2 F5 1.856(2) . ? Nb2 F6 1.913(2) . ? Nb2 F4 1.9438(18) . ? Nb2 O6 2.106(2) . ? Nb2 O5 2.1864(19) . ? O5 P3 1.520(2) . ? O6 P4 1.533(2) . ? P3 C7 1.775(3) . ? P3 C9 1.788(3) . ? P3 C8 1.790(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? P4 C12 1.778(3) . ? P4 C11 1.789(3) . ? P4 C10 1.794(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? Nb3A F8A 1.717(7) . ? Nb3A O7A 1.768(8) . ? Nb3A F7A 1.969(9) . ? Nb3A F9A 2.042(6) . ? Nb3A O9A 2.112(7) . ? Nb3A O8A 2.211(7) . ? O8A P5A 1.499(11) . ? O9A P6A 1.550(13) . ? P5A C13A 1.771(15) . ? P5A C14A 1.793(17) . ? P5A C15A 1.802(14) . ? C13A H13A 0.9800 . ? C13A H13B 0.9800 . ? C13A H13C 0.9800 . ? C14A H14A 0.9800 . ? C14A H14B 0.9800 . ? C14A H14C 0.9800 . ? C15A H15A 0.9800 . ? C15A H15B 0.9800 . ? C15A H15C 0.9800 . ? P6A C16A 1.763(15) . ? P6A C18A 1.777(12) . ? P6A C17A 1.797(12) . ? C16A H16A 0.9800 . ? C16A H16B 0.9800 . ? C16A H16C 0.9800 . ? C17A H17A 0.9800 . ? C17A H17B 0.9800 . ? C17A H17C 0.9800 . ? C18A H18A 0.9800 . ? C18A H18B 0.9800 . ? C18A H18C 0.9800 . ? Nb3B O7B 1.745(8) . ? Nb3B F7B 1.839(10) . ? Nb3B F9B 1.865(6) . ? Nb3B F8B 1.976(7) . ? Nb3B O9B 2.176(7) . ? Nb3B O8B 2.225(7) . ? O8B P5B 1.537(12) . ? O9B P6B 1.494(12) . ? P5B C14B 1.762(19) . ? P5B C15B 1.762(16) . ? P5B C13B 1.811(16) . ? C13B H13D 0.9800 . ? C13B H13E 0.9800 . ? C13B H13F 0.9800 . ? C14B H14D 0.9800 . ? C14B H14E 0.9800 . ? C14B H14F 0.9800 . ? C15B H15D 0.9800 . ? C15B H15E 0.9800 . ? C15B H15F 0.9800 . ? P6B C17B 1.771(13) . ? P6B C16B 1.795(17) . ? P6B C18B 1.798(14) . ? C16B H16D 0.9800 . ? C16B H16E 0.9800 . ? C16B H16F 0.9800 . ? C17B H17D 0.9800 . ? C17B H17E 0.9800 . ? C17B H17F 0.9800 . ? C18B H18D 0.9800 . ? C18B H18E 0.9800 . ? C18B H18F 0.9800 . ? Cl1 C19 1.765(4) . ? Cl2 C19 1.749(4) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Nb1 F2 98.39(9) . . ? O1 Nb1 F3 97.02(10) . . ? F2 Nb1 F3 92.17(9) . . ? O1 Nb1 F1 95.09(10) . . ? F2 Nb1 F1 92.76(9) . . ? F3 Nb1 F1 166.12(9) . . ? O1 Nb1 O2 91.96(9) . . ? F2 Nb1 O2 169.65(8) . . ? F3 Nb1 O2 86.26(8) . . ? F1 Nb1 O2 86.57(9) . . ? O1 Nb1 O3 173.25(9) . . ? F2 Nb1 O3 88.04(8) . . ? F3 Nb1 O3 84.72(8) . . ? F1 Nb1 O3 82.49(8) . . ? O2 Nb1 O3 81.63(7) . . ? P1 O2 Nb1 140.47(12) . . ? P2 O3 Nb1 140.64(12) . . ? O2 P1 C3 110.75(13) . . ? O2 P1 C1 109.43(13) . . ? C3 P1 C1 108.26(15) . . ? O2 P1 C2 111.66(13) . . ? C3 P1 C2 110.25(16) . . ? C1 P1 C2 106.34(15) . . ? P1 C1 H1A 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? P1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? P1 C3 H3A 109.5 . . ? P1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? P1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O3 P2 C5 111.62(13) . . ? O3 P2 C6 111.03(14) . . ? C5 P2 C6 108.51(15) . . ? O3 P2 C4 110.13(13) . . ? C5 P2 C4 107.76(15) . . ? C6 P2 C4 107.64(15) . . ? P2 C4 H4A 109.5 . . ? P2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? P2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? P2 C5 H5A 109.5 . . ? P2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? P2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? P2 C6 H6A 109.5 . . ? P2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? P2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O4 Nb2 F5 97.39(9) . . ? O4 Nb2 F6 96.53(9) . . ? F5 Nb2 F6 93.25(12) . . ? O4 Nb2 F4 95.06(9) . . ? F5 Nb2 F4 92.24(11) . . ? F6 Nb2 F4 166.42(8) . . ? O4 Nb2 O6 90.70(9) . . ? F5 Nb2 O6 171.58(9) . . ? F6 Nb2 O6 88.13(11) . . ? F4 Nb2 O6 84.69(10) . . ? O4 Nb2 O5 174.84(8) . . ? F5 Nb2 O5 87.57(9) . . ? F6 Nb2 O5 84.55(8) . . ? F4 Nb2 O5 83.29(8) . . ? O6 Nb2 O5 84.29(8) . . ? P3 O5 Nb2 139.31(12) . . ? P4 O6 Nb2 135.30(14) . . ? O5 P3 C7 110.27(13) . . ? O5 P3 C9 111.55(13) . . ? C7 P3 C9 108.36(15) . . ? O5 P3 C8 111.40(13) . . ? C7 P3 C8 106.51(15) . . ? C9 P3 C8 108.57(14) . . ? P3 C7 H7A 109.5 . . ? P3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? P3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? P3 C8 H8A 109.5 . . ? P3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? P3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? P3 C9 H9A 109.5 . . ? P3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? P3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O6 P4 C12 109.58(16) . . ? O6 P4 C11 111.26(16) . . ? C12 P4 C11 108.88(17) . . ? O6 P4 C10 112.61(15) . . ? C12 P4 C10 107.94(19) . . ? C11 P4 C10 106.42(18) . . ? P4 C10 H10A 109.5 . . ? P4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? P4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? P4 C11 H11A 109.5 . . ? P4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? P4 C12 H12A 109.5 . . ? P4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? P4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? F8A Nb3A O7A 102.0(4) . . ? F8A Nb3A F7A 96.4(4) . . ? O7A Nb3A F7A 93.9(4) . . ? F8A Nb3A F9A 73.1(3) . . ? O7A Nb3A F9A 98.6(4) . . ? F7A Nb3A F9A 165.1(4) . . ? F8A Nb3A O9A 142.1(4) . . ? O7A Nb3A O9A 109.9(4) . . ? F7A Nb3A O9A 101.0(4) . . ? F9A Nb3A O9A 82.3(3) . . ? F8A Nb3A O8A 89.2(4) . . ? O7A Nb3A O8A 168.4(5) . . ? F7A Nb3A O8A 81.9(4) . . ? F9A Nb3A O8A 87.2(2) . . ? O9A Nb3A O8A 60.7(2) . . ? P5A O8A Nb3A 141.6(6) . . ? P6A O9A Nb3A 139.0(6) . . ? O8A P5A C13A 114.5(8) . . ? O8A P5A C14A 114.0(14) . . ? C13A P5A C14A 106.3(14) . . ? O8A P5A C15A 111.0(9) . . ? C13A P5A C15A 105.7(9) . . ? C14A P5A C15A 104.6(12) . . ? P5A C13A H13A 109.5 . . ? P5A C13A H13B 109.5 . . ? H13A C13A H13B 109.5 . . ? P5A C13A H13C 109.5 . . ? H13A C13A H13C 109.5 . . ? H13B C13A H13C 109.5 . . ? P5A C14A H14A 109.5 . . ? P5A C14A H14B 109.5 . . ? H14A C14A H14B 109.5 . . ? P5A C14A H14C 109.5 . . ? H14A C14A H14C 109.5 . . ? H14B C14A H14C 109.5 . . ? P5A C15A H15A 109.5 . . ? P5A C15A H15B 109.5 . . ? H15A C15A H15B 109.5 . . ? P5A C15A H15C 109.5 . . ? H15A C15A H15C 109.5 . . ? H15B C15A H15C 109.5 . . ? O9A P6A C16A 111.6(11) . . ? O9A P6A C18A 108.4(8) . . ? C16A P6A C18A 112.2(11) . . ? O9A P6A C17A 107.2(7) . . ? C16A P6A C17A 110.6(12) . . ? C18A P6A C17A 106.6(6) . . ? P6A C16A H16A 109.5 . . ? P6A C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? P6A C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? P6A C17A H17A 109.5 . . ? P6A C17A H17B 109.5 . . ? H17A C17A H17B 109.5 . . ? P6A C17A H17C 109.5 . . ? H17A C17A H17C 109.5 . . ? H17B C17A H17C 109.5 . . ? P6A C18A H18A 109.5 . . ? P6A C18A H18B 109.5 . . ? H18A C18A H18B 109.5 . . ? P6A C18A H18C 109.5 . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 109.5 . . ? O7B Nb3B F7B 98.2(4) . . ? O7B Nb3B F9B 84.7(3) . . ? F7B Nb3B F9B 154.0(4) . . ? O7B Nb3B F8B 96.7(3) . . ? F7B Nb3B F8B 94.0(4) . . ? F9B Nb3B F8B 111.4(3) . . ? O7B Nb3B O9B 80.1(3) . . ? F7B Nb3B O9B 69.5(3) . . ? F9B Nb3B O9B 85.8(3) . . ? F8B Nb3B O9B 162.3(3) . . ? O7B Nb3B O8B 174.5(4) . . ? F7B Nb3B O8B 86.7(4) . . ? F9B Nb3B O8B 89.9(3) . . ? F8B Nb3B O8B 85.2(3) . . ? O9B Nb3B O8B 99.6(2) . . ? P5B O8B Nb3B 141.0(6) . . ? P6B O9B Nb3B 137.3(5) . . ? O8B P5B C14B 109.7(14) . . ? O8B P5B C15B 113.1(8) . . ? C14B P5B C15B 106.8(13) . . ? O8B P5B C13B 108.6(8) . . ? C14B P5B C13B 111.2(14) . . ? C15B P5B C13B 107.4(10) . . ? P5B C13B H13D 109.5 . . ? P5B C13B H13E 109.5 . . ? H13D C13B H13E 109.5 . . ? P5B C13B H13F 109.5 . . ? H13D C13B H13F 109.5 . . ? H13E C13B H13F 109.5 . . ? P5B C14B H14D 109.5 . . ? P5B C14B H14E 109.5 . . ? H14D C14B H14E 109.5 . . ? P5B C14B H14F 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? P5B C15B H15D 109.5 . . ? P5B C15B H15E 109.5 . . ? H15D C15B H15E 109.5 . . ? P5B C15B H15F 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? O9B P6B C17B 113.5(7) . . ? O9B P6B C16B 111.8(11) . . ? C17B P6B C16B 105.3(12) . . ? O9B P6B C18B 113.0(9) . . ? C17B P6B C18B 106.0(6) . . ? C16B P6B C18B 106.7(11) . . ? P6B C16B H16D 109.5 . . ? P6B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? P6B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? P6B C17B H17D 109.5 . . ? P6B C17B H17E 109.5 . . ? H17D C17B H17E 109.5 . . ? P6B C17B H17F 109.5 . . ? H17D C17B H17F 109.5 . . ? H17E C17B H17F 109.5 . . ? P6B C18B H18D 109.5 . . ? P6B C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? P6B C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? Cl2 C19 Cl1 113.1(2) . . ? Cl2 C19 H19A 109.0 . . ? Cl1 C19 H19A 109.0 . . ? Cl2 C19 H19B 109.0 . . ? Cl1 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? 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 Nb1 O2 P1 C3 -65.0(2) . . . . ? Nb1 O2 P1 C1 175.76(19) . . . . ? Nb1 O2 P1 C2 58.3(2) . . . . ? Nb1 O3 P2 C5 55.3(2) . . . . ? Nb1 O3 P2 C6 -65.9(2) . . . . ? Nb1 O3 P2 C4 174.93(19) . . . . ? Nb2 O5 P3 C7 179.03(18) . . . . ? Nb2 O5 P3 C9 -60.5(2) . . . . ? Nb2 O5 P3 C8 61.0(2) . . . . ? Nb2 O6 P4 C12 162.5(2) . . . . ? Nb2 O6 P4 C11 -77.1(3) . . . . ? Nb2 O6 P4 C10 42.3(3) . . . . ? Nb3A O8A P5A C13A 93.9(13) . . . . ? Nb3A O8A P5A C14A -28.7(19) . . . . ? Nb3A O8A P5A C15A -146.5(7) . . . . ? Nb3A O9A P6A C16A 64.3(14) . . . . ? Nb3A O9A P6A C18A -171.7(5) . . . . ? Nb3A O9A P6A C17A -57.0(11) . . . . ? Nb3B O8B P5B C14B 47.4(18) . . . . ? Nb3B O8B P5B C15B -71.7(12) . . . . ? Nb3B O8B P5B C13B 169.1(10) . . . . ? Nb3B O9B P6B C17B 179.7(5) . . . . ? Nb3B O9B P6B C16B -61.4(15) . . . . ? Nb3B O9B P6B C18B 59.0(12) . . . . ? _refine_diff_density_max 2.066 _refine_diff_density_min -0.845 _refine_diff_density_rms 0.092 _shelxl_version_number 2013-3 _iucr_refine_instruction_details ; Add final .res file here for Acta Cryst publications or if required. ; #===END OF CIF ============================================================== _database_code_depnum_ccdc_archive 'CCDC 973571' ####################################################################### # # 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_13rwz704 _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2013-11-06 # yyyy-mm-dd _chemical_name_systematic ; trichloro(ethane-1,2-diylbis(diphenylphosphane) dioxide)oxidoniobium(V) acetonitrile solvate ; # Ph2P(O)CH2CH2P(O)Ph2 = C26H24O2P2 = dppeO2 # ethane-1,2-diylbis(diphenylphosphine) dioxide (iLab defaults) # ethane-1,2-diylbis(diphenylphosphane) dioxide (iLab selected options) # ethane-1,2-diylbis(diphenylphosphane) dioxide (chemspider) # 2-(diphenylphosphoryl)ethyl(diphenyl)phosphine oxide (chemspider synonym) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H24 Cl3 Nb O3 P2, 0.5(C2 H3 N)' _chemical_formula_sum 'C27 H25.50 Cl3 N0.50 Nb O3 P2' _chemical_formula_weight 666.18 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 21/n' _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.752(2) _cell_length_b 14.367(3) _cell_length_c 18.048(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.519(8) _cell_angle_gamma 90.00 _cell_volume 2785.1(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9536 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 34.9 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.589 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1348 _exptl_absorpt_coefficient_mu 0.864 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.681 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, VHF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ Superbright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14141 _diffrn_reflns_av_R_equivalents 0.0555 # _diffrn_reflns_av_sigmaI/netI 0.0842 _diffrn_reflns_av_unetI/netI 0.0842 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5451 _reflns_number_gt 4692 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1997)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Shelxl-97 restraints: DFIX on N1 C27 AND C27 C28 (2). Disordered acetonitrile ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0224P)^2^+2.9589P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5451 _refine_ls_number_parameters 338 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0721 _refine_ls_R_factor_gt 0.0591 _refine_ls_wR_factor_ref 0.0968 _refine_ls_wR_factor_gt 0.0921 _refine_ls_goodness_of_fit_ref 1.160 _refine_ls_restrained_S_all 1.160 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 0.93124(3) 0.70023(3) 0.20301(2) 0.00821(11) Uani 1 1 d . . . Cl1 Cl 1.13879(10) 0.65664(7) 0.18315(7) 0.0171(3) Uani 1 1 d . . . Cl2 Cl 0.93921(10) 0.64003(7) 0.32841(6) 0.0136(2) Uani 1 1 d . . . Cl3 Cl 0.91930(10) 0.79580(7) 0.09293(6) 0.0163(2) Uani 1 1 d . . . P1 P 0.68016(10) 0.84732(7) 0.22703(6) 0.0085(2) Uani 1 1 d . . . P2 P 1.00867(10) 0.92664(7) 0.28364(6) 0.0084(2) Uani 1 1 d . . . O1 O 0.8603(3) 0.60447(19) 0.16509(16) 0.0127(7) Uani 1 1 d . . . O2 O 0.7636(2) 0.76113(18) 0.22931(15) 0.0086(6) Uani 1 1 d . . . O3 O 1.0091(2) 0.82660(18) 0.25847(16) 0.0114(7) Uani 1 1 d . . . C1 C 0.6001(4) 0.8504(3) 0.3116(2) 0.0092(9) Uani 1 1 d . . . C2 C 0.6429(4) 0.7956(3) 0.3714(2) 0.0122(9) Uani 1 1 d . . . H2 H 0.7088 0.7525 0.3654 0.015 Uiso 1 1 calc R . . C3 C 0.5894(4) 0.8042(3) 0.4394(2) 0.0149(10) Uani 1 1 d . . . H3 H 0.6176 0.7663 0.4799 0.018 Uiso 1 1 calc R . . C4 C 0.4950(4) 0.8678(3) 0.4484(3) 0.0163(10) Uani 1 1 d . . . H4A H 0.4595 0.8742 0.4954 0.020 Uiso 1 1 calc R . . C5 C 0.4515(4) 0.9225(3) 0.3893(3) 0.0153(10) Uani 1 1 d . . . H5A H 0.3858 0.9655 0.3958 0.018 Uiso 1 1 calc R . . C6 C 0.5036(4) 0.9144(3) 0.3209(2) 0.0119(10) Uani 1 1 d . . . H6A H 0.4743 0.9520 0.2805 0.014 Uiso 1 1 calc R . . C7 C 0.5702(4) 0.8444(3) 0.1490(2) 0.0101(9) Uani 1 1 d . . . C8 C 0.4596(4) 0.7944(3) 0.1535(2) 0.0106(9) Uani 1 1 d . . . H8A H 0.4396 0.7655 0.1988 0.013 Uiso 1 1 calc R . . C9 C 0.3788(4) 0.7871(3) 0.0916(3) 0.0163(10) Uani 1 1 d . . . H9A H 0.3032 0.7533 0.0947 0.020 Uiso 1 1 calc R . . C10 C 0.4080(4) 0.8285(3) 0.0259(3) 0.0147(10) Uani 1 1 d . . . H10A H 0.3527 0.8225 -0.0164 0.018 Uiso 1 1 calc R . . C11 C 0.5170(4) 0.8790(3) 0.0205(3) 0.0157(10) Uani 1 1 d . . . H11A H 0.5360 0.9079 -0.0249 0.019 Uiso 1 1 calc R . . C12 C 0.5983(4) 0.8870(3) 0.0823(2) 0.0123(10) Uani 1 1 d . . . H12A H 0.6733 0.9215 0.0790 0.015 Uiso 1 1 calc R . . C13 C 0.7673(4) 0.9542(3) 0.2225(2) 0.0096(9) Uani 1 1 d . . . H13A H 0.8183 0.9528 0.1782 0.011 Uiso 1 1 calc R . . H13B H 0.7085 1.0070 0.2169 0.011 Uiso 1 1 calc R . . C14 C 0.8529(4) 0.9700(3) 0.2918(2) 0.0105(9) Uani 1 1 d . . . H14A H 0.8156 0.9393 0.3347 0.013 Uiso 1 1 calc R . . H14B H 0.8571 1.0376 0.3024 0.013 Uiso 1 1 calc R . . C15 C 1.0889(4) 0.9998(3) 0.2210(2) 0.0079(9) Uani 1 1 d . . . C16 C 1.0546(4) 1.0924(3) 0.2056(3) 0.0142(10) Uani 1 1 d . . . H16A H 0.9825 1.1180 0.2264 0.017 Uiso 1 1 calc R . . C17 C 1.1257(4) 1.1462(3) 0.1601(3) 0.0189(11) Uani 1 1 d . . . H17A H 1.1024 1.2088 0.1496 0.023 Uiso 1 1 calc R . . C18 C 1.2305(4) 1.1092(3) 0.1300(3) 0.0174(11) Uani 1 1 d . . . H18A H 1.2799 1.1468 0.0994 0.021 Uiso 1 1 calc R . . C19 C 1.2642(4) 1.0182(3) 0.1439(3) 0.0215(12) Uani 1 1 d . . . H19A H 1.3357 0.9929 0.1221 0.026 Uiso 1 1 calc R . . C20 C 1.1943(4) 0.9633(3) 0.1894(3) 0.0180(11) Uani 1 1 d . . . H20A H 1.2182 0.9007 0.1991 0.022 Uiso 1 1 calc R . . C21 C 1.0825(4) 0.9370(3) 0.3742(3) 0.0128(10) Uani 1 1 d . . . C22 C 1.1080(4) 0.8569(3) 0.4152(3) 0.0151(10) Uani 1 1 d . . . H22A H 1.0870 0.7975 0.3952 0.018 Uiso 1 1 calc R . . C23 C 1.1646(4) 0.8646(3) 0.4859(3) 0.0188(11) Uani 1 1 d . . . H23A H 1.1820 0.8103 0.5145 0.023 Uiso 1 1 calc R . . C24 C 1.1956(4) 0.9514(3) 0.5144(3) 0.0171(11) Uani 1 1 d . . . H24A H 1.2361 0.9561 0.5621 0.020 Uiso 1 1 calc R . . C25 C 1.1683(4) 1.0314(3) 0.4742(3) 0.0181(11) Uani 1 1 d . . . H25A H 1.1879 1.0908 0.4948 0.022 Uiso 1 1 calc R . . C26 C 1.1122(4) 1.0248(3) 0.4037(3) 0.0137(10) Uani 1 1 d . . . H26A H 1.0940 1.0794 0.3757 0.016 Uiso 1 1 calc R . . N1 N 0.8435(9) 0.0555(6) 0.0492(5) 0.033(2) Uani 0.50 1 d PD . . C27 C 0.9242(19) 0.0220(19) 0.0238(19) 0.030(4) Uani 0.50 1 d PD . . C28 C 1.0337(18) -0.0195(19) -0.0105(18) 0.030(4) Uani 0.50 1 d PD . . H28A H 1.0606 0.0211 -0.0503 0.046 Uiso 0.50 1 calc PR . . H28B H 1.0114 -0.0808 -0.0309 0.046 Uiso 0.50 1 calc PR . . H28C H 1.1016 -0.0264 0.0272 0.046 Uiso 0.50 1 calc PR . . 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 Nb1 0.0097(2) 0.00781(18) 0.0072(2) -0.00087(16) 0.00080(15) -0.00069(16) Cl1 0.0131(6) 0.0169(5) 0.0217(7) -0.0027(5) 0.0042(5) 0.0015(5) Cl2 0.0168(6) 0.0139(5) 0.0096(6) 0.0015(4) -0.0032(5) -0.0025(5) Cl3 0.0232(6) 0.0156(5) 0.0102(6) 0.0019(5) 0.0033(5) 0.0022(5) P1 0.0079(5) 0.0108(5) 0.0068(6) 0.0006(5) 0.0012(5) 0.0004(5) P2 0.0087(5) 0.0089(5) 0.0075(6) -0.0013(5) -0.0005(5) -0.0013(5) O1 0.0131(16) 0.0125(15) 0.0123(18) -0.0013(13) -0.0018(13) -0.0019(13) O2 0.0110(15) 0.0097(14) 0.0052(16) 0.0008(12) 0.0015(12) 0.0018(12) O3 0.0085(15) 0.0093(14) 0.0166(18) -0.0037(13) 0.0012(13) -0.0014(12) C1 0.008(2) 0.008(2) 0.011(2) 0.0010(18) 0.0023(18) -0.0047(17) C2 0.005(2) 0.015(2) 0.017(3) 0.000(2) 0.0007(18) 0.0008(19) C3 0.015(2) 0.021(2) 0.008(2) 0.002(2) 0.0002(19) 0.000(2) C4 0.021(3) 0.020(2) 0.009(3) -0.002(2) 0.008(2) -0.007(2) C5 0.016(2) 0.013(2) 0.017(3) -0.002(2) 0.009(2) 0.003(2) C6 0.014(2) 0.014(2) 0.008(2) 0.0028(19) 0.0001(18) -0.0013(19) C7 0.010(2) 0.009(2) 0.011(2) -0.0037(18) 0.0003(18) 0.0030(18) C8 0.012(2) 0.011(2) 0.009(2) -0.0001(19) 0.0020(18) -0.0018(19) C9 0.012(2) 0.014(2) 0.022(3) -0.001(2) -0.003(2) -0.002(2) C10 0.017(2) 0.017(2) 0.010(3) -0.0029(19) -0.0027(19) -0.001(2) C11 0.021(2) 0.015(2) 0.012(3) -0.001(2) -0.001(2) 0.003(2) C12 0.015(2) 0.013(2) 0.010(3) 0.0018(19) 0.0021(19) -0.0014(19) C13 0.007(2) 0.008(2) 0.014(2) 0.0047(18) 0.0010(18) -0.0002(17) C14 0.008(2) 0.008(2) 0.016(3) -0.0006(19) 0.0049(18) -0.0020(18) C15 0.007(2) 0.012(2) 0.004(2) 0.0003(17) -0.0025(17) -0.0031(18) C16 0.014(2) 0.014(2) 0.015(3) 0.0014(19) 0.0003(19) 0.0003(19) C17 0.020(3) 0.016(2) 0.020(3) 0.006(2) -0.002(2) -0.001(2) C18 0.020(3) 0.018(2) 0.014(3) 0.001(2) 0.003(2) -0.008(2) C19 0.020(3) 0.020(2) 0.026(3) 0.000(2) 0.017(2) 0.001(2) C20 0.021(3) 0.010(2) 0.023(3) 0.000(2) 0.004(2) -0.001(2) C21 0.007(2) 0.017(2) 0.015(3) -0.004(2) 0.0048(18) 0.0023(19) C22 0.015(2) 0.013(2) 0.017(3) -0.002(2) -0.004(2) 0.0019(19) C23 0.023(3) 0.020(2) 0.013(3) 0.003(2) -0.002(2) 0.005(2) C24 0.013(2) 0.031(3) 0.007(3) -0.003(2) -0.0033(19) 0.005(2) C25 0.018(3) 0.020(2) 0.016(3) -0.008(2) 0.001(2) -0.004(2) C26 0.014(2) 0.015(2) 0.012(3) 0.000(2) -0.0022(19) 0.0011(19) N1 0.039(6) 0.030(5) 0.029(6) 0.013(4) -0.008(5) -0.008(5) C27 0.027(15) 0.029(5) 0.035(12) 0.022(6) -0.011(10) -0.021(8) C28 0.027(15) 0.029(5) 0.035(12) 0.022(6) -0.011(10) -0.021(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 O1 1.702(3) . ? Nb1 O2 2.077(3) . ? Nb1 O3 2.219(3) . ? Nb1 Cl1 2.3602(12) . ? Nb1 Cl3 2.4136(12) . ? Nb1 Cl2 2.4210(13) . ? P1 O2 1.528(3) . ? P1 C1 1.786(4) . ? P1 C7 1.799(4) . ? P1 C13 1.802(4) . ? P2 O3 1.507(3) . ? P2 C21 1.792(5) . ? P2 C15 1.793(4) . ? P2 C14 1.799(4) . ? C1 C2 1.397(6) . ? C1 C6 1.402(6) . ? C2 C3 1.383(6) . ? C2 H2 0.9500 . ? C3 C4 1.381(6) . ? C3 H3 0.9500 . ? C4 C5 1.390(6) . ? C4 H4A 0.9500 . ? C5 C6 1.382(6) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C8 1.394(5) . ? C7 C12 1.396(6) . ? C8 C9 1.388(6) . ? C8 H8A 0.9500 . ? C9 C10 1.376(6) . ? C9 H9A 0.9500 . ? C10 C11 1.385(6) . ? C10 H10A 0.9500 . ? C11 C12 1.390(6) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C14 1.538(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C20 1.394(6) . ? C15 C16 1.404(6) . ? C16 C17 1.383(6) . ? C16 H16A 0.9500 . ? C17 C18 1.379(6) . ? C17 H17A 0.9500 . ? C18 C19 1.377(6) . ? C18 H18A 0.9500 . ? C19 C20 1.384(6) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C21 C22 1.388(6) . ? C21 C26 1.400(6) . ? C22 C23 1.394(6) . ? C22 H22A 0.9500 . ? C23 C24 1.384(6) . ? C23 H23A 0.9500 . ? C24 C25 1.384(6) . ? C24 H24A 0.9500 . ? C25 C26 1.387(6) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? N1 C27 1.108(18) . ? C27 C28 1.479(12) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? 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 O1 Nb1 O2 93.09(12) . . ? O1 Nb1 O3 174.91(12) . . ? O2 Nb1 O3 82.31(10) . . ? O1 Nb1 Cl1 97.74(10) . . ? O2 Nb1 Cl1 169.16(8) . . ? O3 Nb1 Cl1 86.86(8) . . ? O1 Nb1 Cl3 97.02(10) . . ? O2 Nb1 Cl3 86.17(8) . . ? O3 Nb1 Cl3 84.91(8) . . ? Cl1 Nb1 Cl3 92.43(4) . . ? O1 Nb1 Cl2 94.82(10) . . ? O2 Nb1 Cl2 86.11(8) . . ? O3 Nb1 Cl2 82.73(8) . . ? Cl1 Nb1 Cl2 93.00(4) . . ? Cl3 Nb1 Cl2 166.19(4) . . ? O2 P1 C1 107.54(18) . . ? O2 P1 C7 111.54(17) . . ? C1 P1 C7 110.2(2) . . ? O2 P1 C13 112.70(18) . . ? C1 P1 C13 106.8(2) . . ? C7 P1 C13 108.01(19) . . ? O3 P2 C21 110.32(18) . . ? O3 P2 C15 111.18(19) . . ? C21 P2 C15 108.68(19) . . ? O3 P2 C14 111.72(17) . . ? C21 P2 C14 105.8(2) . . ? C15 P2 C14 108.93(19) . . ? P1 O2 Nb1 148.11(17) . . ? P2 O3 Nb1 155.49(17) . . ? C2 C1 C6 119.9(4) . . ? C2 C1 P1 119.4(3) . . ? C6 C1 P1 120.4(3) . . ? C3 C2 C1 119.9(4) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C4 C3 C2 120.0(4) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 120.5(4) . . ? C3 C4 H4A 119.7 . . ? C5 C4 H4A 119.7 . . ? C6 C5 C4 120.1(4) . . ? C6 C5 H5A 119.9 . . ? C4 C5 H5A 119.9 . . ? C5 C6 C1 119.5(4) . . ? C5 C6 H6A 120.2 . . ? C1 C6 H6A 120.2 . . ? C8 C7 C12 119.5(4) . . ? C8 C7 P1 120.0(3) . . ? C12 C7 P1 120.4(3) . . ? C9 C8 C7 119.8(4) . . ? C9 C8 H8A 120.1 . . ? C7 C8 H8A 120.1 . . ? C10 C9 C8 120.1(4) . . ? C10 C9 H9A 119.9 . . ? C8 C9 H9A 119.9 . . ? C9 C10 C11 120.8(4) . . ? C9 C10 H10A 119.6 . . ? C11 C10 H10A 119.6 . . ? C10 C11 C12 119.5(4) . . ? C10 C11 H11A 120.3 . . ? C12 C11 H11A 120.3 . . ? C11 C12 C7 120.2(4) . . ? C11 C12 H12A 119.9 . . ? C7 C12 H12A 119.9 . . ? C14 C13 P1 112.5(3) . . ? C14 C13 H13A 109.1 . . ? P1 C13 H13A 109.1 . . ? C14 C13 H13B 109.1 . . ? P1 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? C13 C14 P2 114.1(3) . . ? C13 C14 H14A 108.7 . . ? P2 C14 H14A 108.7 . . ? C13 C14 H14B 108.7 . . ? P2 C14 H14B 108.7 . . ? H14A C14 H14B 107.6 . . ? C20 C15 C16 119.1(4) . . ? C20 C15 P2 117.4(3) . . ? C16 C15 P2 123.4(3) . . ? C17 C16 C15 120.0(4) . . ? C17 C16 H16A 120.0 . . ? C15 C16 H16A 120.0 . . ? C18 C17 C16 120.1(4) . . ? C18 C17 H17A 120.0 . . ? C16 C17 H17A 120.0 . . ? C19 C18 C17 120.5(4) . . ? C19 C18 H18A 119.8 . . ? C17 C18 H18A 119.8 . . ? C18 C19 C20 120.2(4) . . ? C18 C19 H19A 119.9 . . ? C20 C19 H19A 119.9 . . ? C19 C20 C15 120.1(4) . . ? C19 C20 H20A 120.0 . . ? C15 C20 H20A 120.0 . . ? C22 C21 C26 120.5(4) . . ? C22 C21 P2 119.1(3) . . ? C26 C21 P2 120.4(3) . . ? C21 C22 C23 119.3(4) . . ? C21 C22 H22A 120.3 . . ? C23 C22 H22A 120.3 . . ? C24 C23 C22 120.0(4) . . ? C24 C23 H23A 120.0 . . ? C22 C23 H23A 120.0 . . ? C25 C24 C23 120.8(4) . . ? C25 C24 H24A 119.6 . . ? C23 C24 H24A 119.6 . . ? C24 C25 C26 119.8(4) . . ? C24 C25 H25A 120.1 . . ? C26 C25 H25A 120.1 . . ? C25 C26 C21 119.6(4) . . ? C25 C26 H26A 120.2 . . ? C21 C26 H26A 120.2 . . ? N1 C27 C28 178.1(15) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? 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 P1 C13 C14 P2 92.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.528 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.109 _iucr_refine_instruction_details ; Add final .res file here for Acta Cryst publications or if required. ; _database_code_depnum_ccdc_archive 'CCDC 973572' ####################################################################### # # 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_13rwz131b _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2013-11-08 # yyyy-mm-dd _chemical_name_systematic ; trichloro(methanediylbis(diphenylphosphane) dioxide)oxidoniobium(V) acetonitrile solvate ; # Ph2P(O)CH2P(O)Ph2 = C25H22O2P2 = dppmO2 # methylenebis(diphenylphosphine) dioxide (iLab defaults) # methanediylbis(diphenylphosphane) dioxide (iLab selected options) # methanediylbis(diphenylphosphane) dioxide (chemspider) # [(Diphenylphosphoryl)methyl](diphenyl)phosphine oxide (chemspider synonym) # bis(diphenylphosphino)methane dioxide (mw) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H22 Cl3 Nb O3 P2, 0.3(C2 H3 N)' _chemical_formula_sum 'C25.60 H22.90 Cl3 N0.30 Nb O3 P2' _chemical_formula_weight 643.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 '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' _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 21/n' _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.694(3) _cell_length_b 15.640(4) _cell_length_c 17.181(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.721(6) _cell_angle_gamma 90.00 _cell_volume 2766.0(13) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4753 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.546 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1298.4 # lst file gives 1298.4, cif 1298 _exptl_absorpt_coefficient_mu 0.867 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.879 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, VHF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ Superbright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11311 _diffrn_reflns_av_R_equivalents 0.0386 # _diffrn_reflns_av_sigmaI/netI 0.0744 _diffrn_reflns_av_unetI/netI 0.0744 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5388 _reflns_number_gt 4213 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1997)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. SHELXL-97 DFIX on N1-C26, C26-C27. All 3 atoms isotropic. sof estimated refining a common FVAR2 and then fixing (to 2 dec points) ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0373P)^2^+0.8179P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5388 _refine_ls_number_parameters 320 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0742 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.1045 _refine_ls_wR_factor_gt 0.0946 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 0.57383(4) 0.00896(2) 0.22894(2) 0.01947(11) Uani 1 1 d . . . Cl1 Cl 0.40324(10) 0.01616(7) 0.10677(8) 0.0358(3) Uani 1 1 d . . . Cl2 Cl 0.74675(11) 0.03804(7) 0.34981(6) 0.0314(3) Uani 1 1 d . . . Cl3 Cl 0.43373(13) -0.04186(8) 0.30260(9) 0.0480(4) Uani 1 1 d . . . P1 P 0.55543(10) 0.23173(7) 0.25941(6) 0.0158(2) Uani 1 1 d . . . P2 P 0.74633(10) 0.16993(7) 0.17249(6) 0.0157(2) Uani 1 1 d . . . O1 O 0.5058(2) 0.14143(16) 0.25199(16) 0.0186(6) Uani 1 1 d . . . O2 O 0.6843(2) 0.08223(17) 0.16987(15) 0.0175(6) Uani 1 1 d . . . O3 O 0.6385(3) -0.08621(17) 0.21066(17) 0.0246(7) Uani 1 1 d . . . C1 C 0.5515(4) 0.2811(3) 0.3529(2) 0.0185(9) Uani 1 1 d . . . C2 C 0.4559(5) 0.2541(3) 0.3881(3) 0.0375(12) Uani 1 1 d . . . H2B H 0.3997 0.2084 0.3648 0.045 Uiso 1 1 calc R . . C3 C 0.4425(5) 0.2940(4) 0.4577(3) 0.0480(15) Uani 1 1 d . . . H3A H 0.3777 0.2754 0.4823 0.058 Uiso 1 1 calc R . . C4 C 0.5236(5) 0.3608(4) 0.4909(3) 0.0410(13) Uani 1 1 d . . . H4A H 0.5126 0.3892 0.5375 0.049 Uiso 1 1 calc R . . C5 C 0.6208(5) 0.3868(3) 0.4572(3) 0.0322(11) Uani 1 1 d . . . H5A H 0.6775 0.4321 0.4811 0.039 Uiso 1 1 calc R . . C6 C 0.6351(4) 0.3464(3) 0.3880(2) 0.0236(9) Uani 1 1 d . . . H6A H 0.7024 0.3636 0.3648 0.028 Uiso 1 1 calc R . . C7 C 0.4607(4) 0.2968(3) 0.1795(2) 0.0184(9) Uani 1 1 d . . . C8 C 0.4779(5) 0.3851(3) 0.1823(3) 0.0463(15) Uani 1 1 d . . . H8A H 0.5404 0.4107 0.2262 0.056 Uiso 1 1 calc R . . C9 C 0.4037(6) 0.4355(3) 0.1207(3) 0.0512(16) Uani 1 1 d . . . H9A H 0.4144 0.4958 0.1229 0.061 Uiso 1 1 calc R . . C10 C 0.3143(5) 0.3986(3) 0.0566(3) 0.0360(12) Uani 1 1 d . . . H10A H 0.2630 0.4334 0.0146 0.043 Uiso 1 1 calc R . . C11 C 0.2993(5) 0.3113(3) 0.0531(3) 0.0354(12) Uani 1 1 d . . . H11A H 0.2387 0.2859 0.0083 0.043 Uiso 1 1 calc R . . C12 C 0.3723(4) 0.2601(3) 0.1148(2) 0.0256(10) Uani 1 1 d . . . H12A H 0.3613 0.1998 0.1122 0.031 Uiso 1 1 calc R . . C13 C 0.7224(4) 0.2342(2) 0.2549(2) 0.0181(9) Uani 1 1 d . . . H13A H 0.7794 0.2128 0.3066 0.022 Uiso 1 1 calc R . . H13B H 0.7476 0.2941 0.2479 0.022 Uiso 1 1 calc R . . C14 C 0.6787(4) 0.2248(3) 0.0792(2) 0.0177(9) Uani 1 1 d . . . C15 C 0.6925(5) 0.3127(3) 0.0729(3) 0.0313(11) Uani 1 1 d . . . H15A H 0.7378 0.3450 0.1187 0.038 Uiso 1 1 calc R . . C16 C 0.6400(5) 0.3528(3) -0.0004(3) 0.0418(13) Uani 1 1 d . . . H16A H 0.6473 0.4130 -0.0045 0.050 Uiso 1 1 calc R . . C17 C 0.5766(5) 0.3053(3) -0.0681(3) 0.0395(13) Uani 1 1 d . . . H17A H 0.5426 0.3328 -0.1188 0.047 Uiso 1 1 calc R . . C18 C 0.5634(4) 0.2189(3) -0.0612(3) 0.0303(11) Uani 1 1 d . . . H18A H 0.5192 0.1868 -0.1075 0.036 Uiso 1 1 calc R . . C19 C 0.6132(4) 0.1771(3) 0.0120(2) 0.0237(10) Uani 1 1 d . . . H19A H 0.6028 0.1171 0.0162 0.028 Uiso 1 1 calc R . . C20 C 0.9179(4) 0.1575(3) 0.1907(2) 0.0189(9) Uani 1 1 d . . . C21 C 0.9993(4) 0.2287(3) 0.2021(3) 0.0276(10) Uani 1 1 d . . . H21A H 0.9640 0.2847 0.2002 0.033 Uiso 1 1 calc R . . C22 C 1.1322(4) 0.2171(3) 0.2163(3) 0.0335(12) Uani 1 1 d . . . H22A H 1.1885 0.2652 0.2241 0.040 Uiso 1 1 calc R . . C23 C 1.1828(4) 0.1353(3) 0.2193(3) 0.0295(11) Uani 1 1 d . . . H23A H 1.2740 0.1277 0.2294 0.035 Uiso 1 1 calc R . . C24 C 1.1026(4) 0.0647(3) 0.2076(3) 0.0278(10) Uani 1 1 d . . . H24A H 1.1379 0.0088 0.2098 0.033 Uiso 1 1 calc R . . C25 C 0.9691(4) 0.0765(3) 0.1925(2) 0.0237(10) Uani 1 1 d . . . H25A H 0.9130 0.0283 0.1834 0.028 Uiso 1 1 calc R . . N1 N 0.0887(17) 0.5847(11) 0.0151(12) 0.067(5) Uiso 0.30 1 d PD . . C26 C 0.0354(17) 0.5226(10) 0.0004(12) 0.041(4) Uiso 0.30 1 d PD . . C27 C -0.024(2) 0.4365(13) -0.0162(16) 0.080(8) Uiso 0.30 1 d PD . . H27A H 0.0400 0.3961 -0.0257 0.120 Uiso 0.30 1 calc PR . . H27B H -0.0988 0.4391 -0.0641 0.120 Uiso 0.30 1 calc PR . . H27C H -0.0533 0.4175 0.0304 0.120 Uiso 0.30 1 calc PR . . 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 Nb1 0.0203(2) 0.01262(18) 0.0281(2) 0.00048(17) 0.01097(17) 0.00066(16) Cl1 0.0235(6) 0.0259(6) 0.0486(7) -0.0131(5) -0.0064(5) 0.0032(5) Cl2 0.0410(7) 0.0282(6) 0.0216(5) 0.0028(5) 0.0027(5) 0.0078(5) Cl3 0.0560(8) 0.0238(6) 0.0835(10) 0.0076(7) 0.0521(8) 0.0005(6) P1 0.0176(5) 0.0136(5) 0.0174(5) -0.0007(4) 0.0067(4) 0.0010(4) P2 0.0171(5) 0.0150(5) 0.0163(5) -0.0021(4) 0.0068(4) -0.0014(4) O1 0.0184(15) 0.0112(13) 0.0290(15) -0.0007(12) 0.0113(13) 0.0004(11) O2 0.0188(15) 0.0149(14) 0.0196(14) -0.0013(12) 0.0066(12) -0.0031(12) O3 0.0267(16) 0.0174(15) 0.0319(17) -0.0001(13) 0.0117(14) -0.0002(13) C1 0.021(2) 0.018(2) 0.018(2) -0.0009(17) 0.0083(18) 0.0055(17) C2 0.038(3) 0.047(3) 0.033(3) -0.011(2) 0.020(2) -0.012(2) C3 0.040(3) 0.072(4) 0.043(3) -0.016(3) 0.031(3) -0.012(3) C4 0.046(3) 0.056(4) 0.024(3) -0.016(2) 0.015(2) 0.010(3) C5 0.040(3) 0.033(3) 0.019(2) -0.010(2) 0.000(2) 0.006(2) C6 0.028(2) 0.024(2) 0.020(2) -0.0014(19) 0.0078(19) 0.0000(19) C7 0.024(2) 0.016(2) 0.0161(19) 0.0006(17) 0.0068(18) 0.0031(18) C8 0.071(4) 0.023(3) 0.029(3) -0.001(2) -0.014(3) -0.001(3) C9 0.089(4) 0.019(3) 0.032(3) 0.004(2) -0.007(3) 0.010(3) C10 0.055(3) 0.031(3) 0.019(2) 0.006(2) 0.003(2) 0.016(2) C11 0.034(3) 0.040(3) 0.025(2) 0.003(2) -0.005(2) -0.004(2) C12 0.027(2) 0.022(2) 0.024(2) 0.0007(19) 0.001(2) -0.0021(19) C13 0.019(2) 0.0148(19) 0.021(2) 0.0004(17) 0.0066(18) -0.0005(17) C14 0.019(2) 0.019(2) 0.0160(19) -0.0019(17) 0.0063(17) 0.0023(17) C15 0.050(3) 0.023(2) 0.018(2) -0.0022(19) 0.004(2) -0.007(2) C16 0.073(4) 0.022(2) 0.026(3) 0.004(2) 0.006(3) -0.004(3) C17 0.059(3) 0.036(3) 0.020(2) 0.003(2) 0.005(2) 0.000(3) C18 0.041(3) 0.029(3) 0.020(2) -0.006(2) 0.006(2) -0.005(2) C19 0.026(2) 0.024(2) 0.023(2) -0.0037(19) 0.0086(19) 0.0046(19) C20 0.020(2) 0.020(2) 0.019(2) -0.0033(18) 0.0085(18) 0.0003(18) C21 0.028(2) 0.022(2) 0.038(3) -0.003(2) 0.017(2) 0.001(2) C22 0.023(2) 0.028(3) 0.053(3) -0.011(2) 0.017(2) -0.012(2) C23 0.016(2) 0.036(3) 0.039(3) 0.002(2) 0.012(2) 0.001(2) C24 0.021(2) 0.028(2) 0.038(3) 0.002(2) 0.014(2) 0.008(2) C25 0.025(2) 0.019(2) 0.029(2) -0.0007(19) 0.009(2) -0.0043(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 O3 1.706(3) . ? Nb1 O2 2.095(3) . ? Nb1 O1 2.266(3) . ? Nb1 Cl3 2.3463(13) . ? Nb1 Cl1 2.3815(13) . ? Nb1 Cl2 2.4203(12) . ? P1 O1 1.502(3) . ? P1 C7 1.787(4) . ? P1 C1 1.793(4) . ? P1 C13 1.808(4) . ? P2 O2 1.519(3) . ? P2 C20 1.787(4) . ? P2 C14 1.789(4) . ? P2 C13 1.811(4) . ? C1 C6 1.384(6) . ? C1 C2 1.386(6) . ? C2 C3 1.391(6) . ? C2 H2B 0.9500 . ? C3 C4 1.379(7) . ? C3 H3A 0.9500 . ? C4 C5 1.381(6) . ? C4 H4A 0.9500 . ? C5 C6 1.391(5) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C12 1.375(5) . ? C7 C8 1.392(6) . ? C8 C9 1.383(6) . ? C8 H8A 0.9500 . ? C9 C10 1.375(6) . ? C9 H9A 0.9500 . ? C10 C11 1.373(6) . ? C10 H10A 0.9500 . ? C11 C12 1.387(6) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.389(6) . ? C14 C19 1.394(5) . ? C15 C16 1.382(6) . ? C15 H15A 0.9500 . ? C16 C17 1.392(6) . ? C16 H16A 0.9500 . ? C17 C18 1.367(6) . ? C17 H17A 0.9500 . ? C18 C19 1.389(6) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 C25 1.377(5) . ? C20 C21 1.395(6) . ? C21 C22 1.388(6) . ? C21 H21A 0.9500 . ? C22 C23 1.384(6) . ? C22 H22A 0.9500 . ? C23 C24 1.379(6) . ? C23 H23A 0.9500 . ? C24 C25 1.391(5) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? N1 C26 1.119(16) . ? C26 C27 1.484(17) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? 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 O3 Nb1 O2 94.47(12) . . ? O3 Nb1 O1 174.46(11) . . ? O2 Nb1 O1 80.48(10) . . ? O3 Nb1 Cl3 98.84(10) . . ? O2 Nb1 Cl3 166.64(8) . . ? O1 Nb1 Cl3 86.17(7) . . ? O3 Nb1 Cl1 97.53(10) . . ? O2 Nb1 Cl1 86.85(8) . . ? O1 Nb1 Cl1 84.56(7) . . ? Cl3 Nb1 Cl1 92.45(6) . . ? O3 Nb1 Cl2 93.91(10) . . ? O2 Nb1 Cl2 85.00(8) . . ? O1 Nb1 Cl2 83.41(7) . . ? Cl3 Nb1 Cl2 92.98(5) . . ? Cl1 Nb1 Cl2 166.43(4) . . ? O1 P1 C7 110.90(18) . . ? O1 P1 C1 112.76(18) . . ? C7 P1 C1 107.26(18) . . ? O1 P1 C13 110.33(17) . . ? C7 P1 C13 108.40(18) . . ? C1 P1 C13 106.99(18) . . ? O2 P2 C20 109.04(17) . . ? O2 P2 C14 109.85(17) . . ? C20 P2 C14 110.84(18) . . ? O2 P2 C13 111.83(17) . . ? C20 P2 C13 106.24(18) . . ? C14 P2 C13 109.01(18) . . ? P1 O1 Nb1 138.72(16) . . ? P2 O2 Nb1 141.13(16) . . ? C6 C1 C2 120.0(4) . . ? C6 C1 P1 122.6(3) . . ? C2 C1 P1 117.3(3) . . ? C1 C2 C3 119.9(5) . . ? C1 C2 H2B 120.1 . . ? C3 C2 H2B 120.1 . . ? C4 C3 C2 119.8(5) . . ? C4 C3 H3A 120.1 . . ? C2 C3 H3A 120.1 . . ? C3 C4 C5 120.6(4) . . ? C3 C4 H4A 119.7 . . ? C5 C4 H4A 119.7 . . ? C4 C5 C6 119.6(4) . . ? C4 C5 H5A 120.2 . . ? C6 C5 H5A 120.2 . . ? C1 C6 C5 120.0(4) . . ? C1 C6 H6A 120.0 . . ? C5 C6 H6A 120.0 . . ? C12 C7 C8 119.8(4) . . ? C12 C7 P1 120.4(3) . . ? C8 C7 P1 119.8(3) . . ? C9 C8 C7 119.7(4) . . ? C9 C8 H8A 120.1 . . ? C7 C8 H8A 120.1 . . ? C10 C9 C8 120.3(5) . . ? C10 C9 H9A 119.9 . . ? C8 C9 H9A 119.9 . . ? C11 C10 C9 119.9(4) . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C10 C11 C12 120.4(4) . . ? C10 C11 H11A 119.8 . . ? C12 C11 H11A 119.8 . . ? C7 C12 C11 119.9(4) . . ? C7 C12 H12A 120.1 . . ? C11 C12 H12A 120.1 . . ? P1 C13 P2 111.8(2) . . ? P1 C13 H13A 109.3 . . ? P2 C13 H13A 109.3 . . ? P1 C13 H13B 109.3 . . ? P2 C13 H13B 109.3 . . ? H13A C13 H13B 107.9 . . ? C15 C14 C19 120.3(4) . . ? C15 C14 P2 121.3(3) . . ? C19 C14 P2 118.4(3) . . ? C16 C15 C14 119.6(4) . . ? C16 C15 H15A 120.2 . . ? C14 C15 H15A 120.2 . . ? C15 C16 C17 120.3(4) . . ? C15 C16 H16A 119.8 . . ? C17 C16 H16A 119.8 . . ? C18 C17 C16 119.6(4) . . ? C18 C17 H17A 120.2 . . ? C16 C17 H17A 120.2 . . ? C17 C18 C19 121.3(4) . . ? C17 C18 H18A 119.3 . . ? C19 C18 H18A 119.3 . . ? C18 C19 C14 118.8(4) . . ? C18 C19 H19A 120.6 . . ? C14 C19 H19A 120.6 . . ? C25 C20 C21 120.2(4) . . ? C25 C20 P2 119.2(3) . . ? C21 C20 P2 120.6(3) . . ? C22 C21 C20 119.3(4) . . ? C22 C21 H21A 120.3 . . ? C20 C21 H21A 120.3 . . ? C23 C22 C21 120.0(4) . . ? C23 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C24 C23 C22 120.8(4) . . ? C24 C23 H23A 119.6 . . ? C22 C23 H23A 119.6 . . ? C23 C24 C25 119.2(4) . . ? C23 C24 H24A 120.4 . . ? C25 C24 H24A 120.4 . . ? C20 C25 C24 120.5(4) . . ? C20 C25 H25A 119.8 . . ? C24 C25 H25A 119.8 . . ? N1 C26 C27 175(2) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.515 _refine_diff_density_min -0.535 _refine_diff_density_rms 0.093 _iucr_refine_instruction_details ; Add final .res file here for Acta Cryst publications or if required. ; _database_code_depnum_ccdc_archive 'CCDC 973573' ####################################################################### # # 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_12wz1206a _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2013-11-11 # yyyy-mm-dd _chemical_name_systematic ; trichloro(N,N,N',N'-tetramethylethane-1,2-diamine)oxidoniobium(V) ; # Me2NCH2CH2NMe2 = C6H16N2 = tmeda # 1,2-bis(dimethylamino)ethane # N,N,N',N'-tetramethylethylenediamine # N,N,N',N'-tetramethyl-1,2-diamino-ethane # N,N,N',N'-tetramethylethane-1,2-diamine (from iLab naming (defaults)) # N,N,N',N'-tetramethylethane-1,2-diamine (Chemspider) # N,N,N',N'-Tetramethyl-1,2-ethanediamine (Chemspider alternative) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H16 Cl3 N2 Nb O' _chemical_formula_sum 'C6 H16 Cl3 N2 Nb O' _chemical_formula_weight 331.47 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_name_H-M_alt 'P n a 21' _space_group_IT_number 33 _space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 14.352(7) _cell_length_b 7.368(4) _cell_length_c 11.781(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1245.8(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2979 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.767 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 1.578 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.801 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, VHF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ Superbright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3500 _diffrn_reflns_av_R_equivalents 0.0196 # _diffrn_reflns_av_sigmaI/netI 0.0345 _diffrn_reflns_av_unetI/netI 0.0345 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2135 _reflns_number_gt 1874 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Shelxl-97 Used BASF/TWIN From the adp values for several C atoms of Me2N(CH2)NMe2 there appears to be some disorder. Attempts to model this with split atoms (2) were not successful. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0624P)^2^+1.2782P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.82(15) _refine_ls_number_reflns 2135 _refine_ls_number_parameters 119 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1162 _refine_ls_wR_factor_gt 0.1102 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 0.36287(4) 0.27773(7) 0.24676(8) 0.0456(2) Uani 1 1 d . . . Cl1 Cl 0.44608(17) 0.1771(3) 0.40752(17) 0.0572(5) Uani 1 1 d . . . Cl2 Cl 0.2907(3) 0.4397(4) 0.0993(3) 0.1298(18) Uani 1 1 d . . . Cl3 Cl 0.4795(2) 0.1775(4) 0.1246(2) 0.0932(11) Uani 1 1 d . . . O1 O 0.2794(3) 0.0957(6) 0.2446(8) 0.0780(17) Uani 1 1 d . . . N1 N 0.4512(4) 0.5689(7) 0.2776(5) 0.0427(14) Uani 1 1 d . . . N2 N 0.2717(5) 0.4511(11) 0.3694(9) 0.080(3) Uani 1 1 d . . . C1 C 0.5447(6) 0.5398(13) 0.3268(12) 0.106(5) Uani 1 1 d . . . H1A H 0.5398 0.4590 0.3927 0.159 Uiso 1 1 calc R . . H1B H 0.5708 0.6566 0.3507 0.159 Uiso 1 1 calc R . . H1C H 0.5854 0.4845 0.2698 0.159 Uiso 1 1 calc R . . C2 C 0.4615(10) 0.6803(16) 0.1753(11) 0.102(4) Uani 1 1 d . . . H2A H 0.4970 0.6129 0.1182 0.153 Uiso 1 1 calc R . . H2B H 0.4945 0.7926 0.1944 0.153 Uiso 1 1 calc R . . H2C H 0.3997 0.7099 0.1450 0.153 Uiso 1 1 calc R . . C3 C 0.3973(8) 0.6703(15) 0.3623(12) 0.087(3) Uani 1 1 d . . . H3A H 0.4276 0.6516 0.4369 0.104 Uiso 1 1 calc R . . H3B H 0.4032 0.8009 0.3439 0.104 Uiso 1 1 calc R . . C4 C 0.3061(11) 0.6345(17) 0.3753(16) 0.180(10) Uani 1 1 d . . . H4A H 0.2724 0.7055 0.3171 0.217 Uiso 1 1 calc R . . H4B H 0.2874 0.6839 0.4501 0.217 Uiso 1 1 calc R . . C5 C 0.2509(13) 0.361(3) 0.4699(14) 0.236(15) Uani 1 1 d D . . H5A H 0.3088 0.3204 0.5060 0.354 Uiso 1 1 calc R . . H5B H 0.2116 0.2554 0.4534 0.354 Uiso 1 1 calc R . . H5C H 0.2177 0.4432 0.5212 0.354 Uiso 1 1 calc R . . C6 C 0.1753(7) 0.477(2) 0.324(2) 0.226(14) Uani 1 1 d D . . H6A H 0.1777 0.5542 0.2559 0.339 Uiso 1 1 calc R . . H6B H 0.1361 0.5346 0.3813 0.339 Uiso 1 1 calc R . . H6C H 0.1488 0.3586 0.3033 0.339 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nb1 0.0591(3) 0.0250(3) 0.0527(4) -0.0095(4) -0.0118(5) 0.0060(2) Cl1 0.0936(14) 0.0307(9) 0.0474(10) 0.0047(9) -0.0119(11) 0.0009(9) Cl2 0.221(4) 0.0439(14) 0.124(2) -0.0119(16) -0.118(3) 0.022(2) Cl3 0.171(3) 0.0442(12) 0.0642(14) 0.0028(12) 0.0551(18) 0.0322(17) O1 0.065(3) 0.027(2) 0.142(6) 0.004(5) 0.002(5) 0.006(2) N1 0.056(3) 0.022(2) 0.050(4) 0.003(3) -0.005(3) -0.007(2) N2 0.060(4) 0.039(4) 0.141(8) 0.002(5) 0.058(5) 0.006(3) C1 0.061(5) 0.047(5) 0.209(14) 0.044(7) -0.045(6) -0.029(4) C2 0.157(12) 0.061(6) 0.089(8) 0.037(6) -0.006(8) -0.037(8) C3 0.118(8) 0.043(5) 0.101(8) -0.040(6) -0.004(7) -0.006(6) C4 0.202(14) 0.081(8) 0.26(2) -0.112(12) 0.183(15) -0.077(10) C5 0.31(2) 0.153(15) 0.25(2) 0.091(15) 0.25(2) 0.117(16) C6 0.081(8) 0.150(14) 0.45(4) 0.07(2) 0.068(15) 0.070(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 O1 1.798(5) . ? Nb1 N2 2.331(8) . ? Nb1 Cl3 2.328(3) . ? Nb1 Cl2 2.348(3) . ? Nb1 Cl1 2.358(2) . ? Nb1 N1 2.518(5) . ? N1 C2 1.466(12) . ? N1 C3 1.467(12) . ? N1 C1 1.478(10) . ? N2 C5 1.390(15) . ? N2 C4 1.441(13) . ? N2 C6 1.498(16) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.343(16) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? 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 O1 Nb1 N2 92.5(3) . . ? O1 Nb1 Cl3 103.5(2) . . ? N2 Nb1 Cl3 163.9(2) . . ? O1 Nb1 Cl2 94.3(3) . . ? N2 Nb1 Cl2 86.1(3) . . ? Cl3 Nb1 Cl2 91.21(16) . . ? O1 Nb1 Cl1 96.5(3) . . ? N2 Nb1 Cl1 87.6(3) . . ? Cl3 Nb1 Cl1 91.87(10) . . ? Cl2 Nb1 Cl1 167.70(10) . . ? O1 Nb1 N1 166.6(3) . . ? N2 Nb1 N1 74.1(2) . . ? Cl3 Nb1 N1 89.86(16) . . ? Cl2 Nb1 N1 84.00(15) . . ? Cl1 Nb1 N1 84.09(15) . . ? C2 N1 C3 109.1(8) . . ? C2 N1 C1 108.2(8) . . ? C3 N1 C1 106.6(8) . . ? C2 N1 Nb1 114.2(6) . . ? C3 N1 Nb1 105.5(5) . . ? C1 N1 Nb1 113.0(4) . . ? C5 N2 C4 118.7(14) . . ? C5 N2 C6 99.8(9) . . ? C4 N2 C6 102.5(12) . . ? C5 N2 Nb1 112.7(8) . . ? C4 N2 Nb1 110.6(6) . . ? C6 N2 Nb1 111.4(11) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 N1 119.4(8) . . ? C4 C3 H3A 107.5 . . ? N1 C3 H3A 107.5 . . ? C4 C3 H3B 107.5 . . ? N1 C3 H3B 107.5 . . ? H3A C3 H3B 107.0 . . ? C3 C4 N2 120.9(12) . . ? C3 C4 H4A 107.1 . . ? N2 C4 H4A 107.1 . . ? C3 C4 H4B 107.1 . . ? N2 C4 H4B 107.1 . . ? H4A C4 H4B 106.8 . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.596 _refine_diff_density_min -0.529 _refine_diff_density_rms 0.093 _iucr_refine_instruction_details ; Add final .res file here for Acta Cryst publications or if required. ; _database_code_depnum_ccdc_archive 'CCDC 973574' ####################################################################### # # 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_12wz1115a _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2013-11-18 # yyyy-mm-dd _chemical_name_systematic ; 2,2'-bipyridyl-trifluorooxidoniobium(V) ; # 2,2'-bipyridyl = C10H8N2 = bipy # 2,2'-bipyridyl (chemspider) # 2,2'-bipyridine (iLab defaults & selected options) # 2,2'-bipyridine (chemspider systematic name) # 2-(2-pyridyl)pyridine (chemspider) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H8 Cl3 N2 Nb O' _chemical_formula_sum 'C10 H8 Cl3 N2 Nb O' _chemical_formula_weight 371.44 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_name_H-M_alt 'F d d 2' _space_group_IT_number 43 _space_group_name_Hall 'F 2 -2d' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 12.4975(4) _cell_length_b 21.6322(9) _cell_length_c 29.090(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7864.3(7) _cell_formula_units_Z 24 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5140 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.882 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4368 _exptl_absorpt_coefficient_mu 1.512 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.714 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, VHF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ Superbright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5418 _diffrn_reflns_av_R_equivalents 0.0243 # _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_av_unetI/netI 0.0343 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 3.34 _diffrn_reflns_theta_max 27.46 _reflns_number_total 2991 _reflns_number_gt 2808 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1997)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Shelxl-97 refinement: the Nb2 atom on the 2-fold axis with a very elongated ellipsoid was moved off the mirror by a few tenths of an Angstrom (and held as isotropic) resulting a reduction of R1 from 0.08 to 0.047. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0685P)^2^+117.3700P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.06(11) _refine_ls_number_reflns 2991 _refine_ls_number_parameters 240 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0506 _refine_ls_R_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.1204 _refine_ls_wR_factor_gt 0.1169 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb -0.01056(5) 0.64247(2) 0.38079(2) 0.01954(16) Uani 1 1 d U . . Nb2 Nb 0.74379(9) 0.26592(4) 0.12012(4) 0.0144(3) Uiso 0.50 1 d P . . Cl1 Cl 0.14756(14) 0.70223(8) 0.37775(7) 0.0301(4) Uani 1 1 d . . . Cl2 Cl -0.08945(17) 0.70298(9) 0.43898(7) 0.0316(4) Uani 1 1 d . . . Cl3 Cl -0.17679(13) 0.59825(7) 0.35916(7) 0.0234(4) Uani 1 1 d . . . Cl4 Cl 0.90961(15) 0.30680(9) 0.13006(9) 0.0360(4) Uani 1 1 d . . . Cl5 Cl 0.6831(3) 0.29146(15) 0.05950(13) 0.0232(7) Uani 0.50 1 d P . . O1 O 0.0402(5) 0.5803(3) 0.4086(2) 0.0304(12) Uani 1 1 d . . . O2 O 0.8154(9) 0.1733(4) 0.0938(4) 0.024(2) Uani 0.50 1 d P . . N1 N 0.0484(5) 0.6025(3) 0.3136(2) 0.0201(12) Uani 1 1 d . . . N2 N -0.0567(5) 0.7088(2) 0.3184(2) 0.0200(12) Uani 1 1 d U . . N3 N 0.6957(5) 0.3030(3) 0.1858(3) 0.0263(15) Uani 1 1 d . . . C1 C 0.1060(6) 0.5500(3) 0.3135(3) 0.0236(15) Uani 1 1 d . . . H1 H 0.1229 0.5310 0.3421 0.028 Uiso 1 1 calc R . . C2 C 0.1416(6) 0.5226(3) 0.2734(3) 0.0278(17) Uani 1 1 d . . . H2 H 0.1832 0.4858 0.2745 0.033 Uiso 1 1 calc R . . C3 C 0.1163(7) 0.5489(4) 0.2323(4) 0.035(2) Uani 1 1 d . . . H3 H 0.1393 0.5306 0.2043 0.042 Uiso 1 1 calc R . . C4 C 0.0562(7) 0.6030(3) 0.2320(3) 0.0256(16) Uani 1 1 d . . . H4 H 0.0366 0.6214 0.2035 0.031 Uiso 1 1 calc R . . C5 C 0.0248(5) 0.6303(3) 0.2726(3) 0.0181(14) Uani 1 1 d . . . C6 C -0.0353(6) 0.6894(3) 0.2757(3) 0.0183(13) Uani 1 1 d U . . C7 C -0.0617(6) 0.7232(3) 0.2364(3) 0.0224(15) Uani 1 1 d U . . H7 H -0.0448 0.7082 0.2066 0.027 Uiso 1 1 calc R . . C8 C -0.1140(6) 0.7799(3) 0.2426(3) 0.0275(16) Uani 1 1 d U . . H8 H -0.1344 0.8040 0.2168 0.033 Uiso 1 1 calc R . . C9 C -0.1354(6) 0.8001(3) 0.2864(3) 0.0264(16) Uani 1 1 d U . . H9 H -0.1693 0.8389 0.2912 0.032 Uiso 1 1 calc R . . C10 C -0.1075(7) 0.7636(3) 0.3234(3) 0.0278(16) Uani 1 1 d U . . H10 H -0.1245 0.7775 0.3535 0.033 Uiso 1 1 calc R . . C11 C 0.6413(7) 0.3559(4) 0.1846(4) 0.044(3) Uani 1 1 d . . . H11 H 0.6232 0.3722 0.1553 0.053 Uiso 1 1 calc R . . C12 C 0.6101(7) 0.3881(4) 0.2219(5) 0.049(3) Uani 1 1 d . . . H12 H 0.5722 0.4259 0.2189 0.059 Uiso 1 1 calc R . . C13 C 0.6348(7) 0.3645(4) 0.2646(4) 0.039(2) Uani 1 1 d . . . H13 H 0.6135 0.3859 0.2916 0.047 Uiso 1 1 calc R . . C14 C 0.6899(6) 0.3102(3) 0.2679(3) 0.0258(16) Uani 1 1 d . . . H14 H 0.7069 0.2934 0.2972 0.031 Uiso 1 1 calc R . . C15 C 0.7210(6) 0.2795(3) 0.2278(3) 0.0179(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nb1 0.0188(3) 0.0245(3) 0.0153(3) -0.0006(2) 0.0002(3) -0.0031(2) Cl1 0.0248(9) 0.0419(9) 0.0237(10) -0.0043(9) 0.0017(8) -0.0138(6) Cl2 0.0344(11) 0.0371(9) 0.0234(10) -0.0110(8) 0.0095(8) -0.0061(7) Cl3 0.0150(8) 0.0259(7) 0.0294(10) -0.0037(7) 0.0011(7) -0.0053(6) Cl4 0.0185(10) 0.0605(11) 0.0290(10) 0.0131(10) 0.0027(9) -0.0003(7) Cl5 0.0190(18) 0.0321(16) 0.0184(17) 0.0092(14) -0.0016(13) -0.0031(12) O1 0.030(3) 0.043(3) 0.018(3) 0.004(2) -0.002(2) 0.000(2) O2 0.029(6) 0.019(4) 0.023(6) -0.002(4) 0.007(5) 0.001(4) N1 0.016(3) 0.028(3) 0.016(3) 0.003(2) 0.002(2) -0.003(2) N2 0.025(3) 0.018(2) 0.017(3) -0.004(2) 0.000(3) -0.002(2) N3 0.020(4) 0.036(3) 0.023(4) 0.010(3) -0.001(3) -0.010(2) C1 0.016(4) 0.025(3) 0.030(4) 0.002(3) 0.000(3) 0.001(2) C2 0.021(4) 0.029(3) 0.033(5) -0.003(3) -0.001(3) -0.001(3) C3 0.033(5) 0.032(4) 0.040(5) -0.005(4) 0.006(4) 0.001(3) C4 0.031(5) 0.027(3) 0.019(4) 0.000(3) 0.001(3) 0.000(3) C5 0.015(4) 0.020(3) 0.019(4) -0.001(3) -0.002(3) -0.005(2) C6 0.018(4) 0.015(3) 0.022(3) -0.004(2) 0.001(3) -0.002(2) C7 0.020(4) 0.025(3) 0.022(4) 0.003(3) 0.001(3) 0.002(3) C8 0.020(4) 0.031(3) 0.031(4) 0.006(3) -0.008(3) 0.004(3) C9 0.018(4) 0.022(3) 0.039(5) -0.002(3) 0.001(3) 0.004(2) C10 0.036(5) 0.023(3) 0.025(4) -0.004(3) 0.003(3) -0.002(3) C11 0.022(5) 0.046(5) 0.064(8) 0.035(5) -0.012(5) -0.006(3) C12 0.021(5) 0.026(4) 0.100(10) 0.011(5) 0.002(5) 0.001(3) C13 0.027(5) 0.028(4) 0.062(7) -0.014(4) 0.009(4) 0.000(3) C14 0.018(4) 0.034(4) 0.026(4) -0.006(3) 0.007(3) -0.001(3) C15 0.014(4) 0.026(3) 0.013(3) 0.001(3) 0.001(3) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 O1 1.694(6) . ? Nb1 N1 2.262(6) . ? Nb1 Cl2 2.356(2) . ? Nb1 Cl1 2.3630(17) . ? Nb1 Cl3 2.3722(17) . ? Nb1 N2 2.385(6) . ? Nb2 Nb2 0.7062(17) 14_655 ? Nb2 O2 1.693(10) 14_655 ? Nb2 Cl5 1.998(4) . ? Nb2 N3 2.158(8) . ? Nb2 Cl4 2.272(2) . ? Nb2 O2 2.325(9) . ? Nb2 Cl5 2.342(4) 14_655 ? Nb2 Cl4 2.497(2) 14_655 ? Nb2 N3 2.539(8) 14_655 ? Cl4 Nb2 2.497(2) 14_655 ? Cl5 O2 1.255(12) 14_655 ? Cl5 Nb2 2.342(4) 14_655 ? Cl5 Cl5 2.453(7) 14_655 ? O2 Cl5 1.255(12) 14_655 ? O2 Nb2 1.693(10) 14_655 ? N1 C1 1.346(9) . ? N1 C5 1.365(9) . ? N2 C6 1.337(10) . ? N2 C10 1.353(9) . ? N3 C11 1.331(11) . ? N3 C15 1.361(10) . ? N3 Nb2 2.539(8) 14_655 ? C1 C2 1.383(12) . ? C1 H1 0.9500 . ? C2 C3 1.361(13) . ? C2 H2 0.9500 . ? C3 C4 1.392(11) . ? C3 H3 0.9500 . ? C4 C5 1.379(10) . ? C4 H4 0.9500 . ? C5 C6 1.485(9) . ? C6 C7 1.395(10) . ? C7 C8 1.401(9) . ? C7 H7 0.9500 . ? C8 C9 1.374(12) . ? C8 H8 0.9500 . ? C9 C10 1.379(12) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.348(17) . ? C11 H11 0.9500 . ? C12 C13 1.376(18) . ? C12 H12 0.9500 . ? C13 C14 1.365(11) . ? C13 H13 0.9500 . ? C14 C15 1.398(10) . ? C14 H14 0.9500 . ? C15 C15 1.467(13) 14_655 ? 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 # Nb2 Nb2 O2 148.7(4) 14_655 14_655 ? # Nb2 Nb2 Cl5 110.69(12) 14_655 . ? # Nb2 Nb2 N3 115.09(17) 14_655 . ? # Nb2 Nb2 Cl4 100.32(19) 14_655 . ? # Nb2 Nb2 O2 22.3(3) 14_655 . ? # Nb2 Nb2 Cl5 52.93(11) 14_655 14_655 ? # O2 Nb2 Cl5 31.2(3) . 14_655 ? # Nb2 Nb2 Cl4 63.52(17) 14_655 14_655 ? # Nb2 Nb2 N3 50.32(15) 14_655 14_655 ? # Nb2 Cl4 Nb2 16.16(5) . 14_655 ? # Nb2 Cl5 Nb2 16.38(5) . 14_655 ? # Nb2 O2 Nb2 9.09(11) 14_655 . ? # Nb2 N3 Nb2 14.59(6) . 14_655 ? O1 Nb1 N1 89.3(3) . . ? O1 Nb1 Cl2 104.8(2) . . ? N1 Nb1 Cl2 165.92(16) . . ? O1 Nb1 Cl1 98.0(2) . . ? N1 Nb1 Cl1 84.50(16) . . ? Cl2 Nb1 Cl1 94.18(7) . . ? O1 Nb1 Cl3 97.7(2) . . ? N1 Nb1 Cl3 84.37(16) . . ? Cl2 Nb1 Cl3 92.76(7) . . ? Cl1 Nb1 Cl3 160.58(8) . . ? O1 Nb1 N2 158.8(3) . . ? N1 Nb1 N2 69.5(2) . . ? Cl2 Nb1 N2 96.41(15) . . ? Cl1 Nb1 N2 81.08(15) . . ? Cl3 Nb1 N2 80.13(15) . . ? O2 Nb2 Cl5 38.7(4) 14_655 . ? O2 Nb2 N3 89.5(4) 14_655 . ? Cl5 Nb2 N3 125.0(2) . . ? O2 Nb2 Cl4 98.9(4) 14_655 . ? Cl5 Nb2 Cl4 110.57(12) . . ? N3 Nb2 Cl4 89.81(19) . . ? O2 Nb2 O2 133.5(7) 14_655 . ? Cl5 Nb2 O2 95.4(3) . . ? N3 Nb2 O2 136.0(3) . . ? Cl4 Nb2 O2 91.5(3) . . ? O2 Nb2 Cl5 104.0(4) 14_655 14_655 ? Cl5 Nb2 Cl5 68.3(2) . 14_655 ? N3 Nb2 Cl5 166.5(2) . 14_655 ? Cl4 Nb2 Cl5 86.91(11) . 14_655 ? O2 Nb2 Cl4 101.9(4) 14_655 14_655 ? Cl5 Nb2 Cl4 89.12(12) . 14_655 ? N3 Nb2 Cl4 85.29(17) . 14_655 ? Cl4 Nb2 Cl4 158.60(9) . 14_655 ? O2 Nb2 Cl4 77.9(3) . 14_655 ? Cl5 Nb2 Cl4 93.04(10) 14_655 14_655 ? O2 Nb2 N3 158.0(4) 14_655 14_655 ? Cl5 Nb2 N3 160.02(18) . 14_655 ? N3 Nb2 N3 68.6(3) . 14_655 ? Cl4 Nb2 N3 82.02(15) . 14_655 ? O2 Nb2 N3 68.1(3) . 14_655 ? Cl5 Nb2 N3 97.99(18) 14_655 14_655 ? Cl4 Nb2 N3 76.79(15) 14_655 14_655 ? O2 Cl5 Nb2 57.4(5) 14_655 . ? O2 Cl5 Nb2 73.6(5) 14_655 14_655 ? O2 Cl5 Cl5 115.7(5) 14_655 14_655 ? Nb2 Cl5 Cl5 62.53(11) . 14_655 ? Nb2 Cl5 Cl5 49.18(10) 14_655 14_655 ? Cl5 O2 Nb2 83.9(5) 14_655 14_655 ? Cl5 O2 Nb2 75.2(4) 14_655 . ? C1 N1 C5 119.1(7) . . ? C1 N1 Nb1 119.9(5) . . ? C5 N1 Nb1 121.0(5) . . ? C6 N2 C10 117.9(7) . . ? C6 N2 Nb1 118.0(4) . . ? C10 N2 Nb1 124.0(5) . . ? C11 N3 C15 117.6(8) . . ? C11 N3 Nb2 116.0(7) . . ? C15 N3 Nb2 126.2(5) . . ? C11 N3 Nb2 129.6(7) . 14_655 ? C15 N3 Nb2 112.8(5) . 14_655 ? N1 C1 C2 122.3(8) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C3 C2 C1 119.2(8) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C2 C3 C4 118.9(8) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C5 C4 C3 120.5(8) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? N1 C5 C4 119.9(6) . . ? N1 C5 C6 115.8(7) . . ? C4 C5 C6 124.2(7) . . ? N2 C6 C7 123.2(6) . . ? N2 C6 C5 115.3(7) . . ? C7 C6 C5 121.4(7) . . ? C6 C7 C8 117.7(7) . . ? C6 C7 H7 121.2 . . ? C8 C7 H7 121.2 . . ? C9 C8 C7 119.2(8) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C8 C9 C10 119.4(7) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? N2 C10 C9 122.5(8) . . ? N2 C10 H10 118.8 . . ? C9 C10 H10 118.8 . . ? N3 C11 C12 124.8(10) . . ? N3 C11 H11 117.6 . . ? C12 C11 H11 117.6 . . ? C11 C12 C13 118.0(8) . . ? C11 C12 H12 121.0 . . ? C13 C12 H12 121.0 . . ? C14 C13 C12 119.8(10) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C13 C14 C15 119.3(9) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? N3 C15 C14 120.5(7) . . ? N3 C15 C15 116.1(4) . 14_655 ? C14 C15 C15 123.4(4) . 14_655 ? 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 C5 C6 N2 1.4(9) . . . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 3.979 _refine_diff_density_min -0.979 _refine_diff_density_rms 0.142 _iucr_refine_instruction_details ; Add final .res file here for Acta Cryst publications or if required. ; _database_code_depnum_ccdc_archive 'CCDC 973575' ####################################################################### # # 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_13rwz1017 _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2013-11-15 # yyyy-mm-dd _chemical_name_systematic ; trifluoro-(bis(diphenylphosphino)methane dioxide)-oxidoniobium(V) ; # Ph2P(O)CH2P(O)Ph2 = C25H22O2P2 = dppmO2 # methylenebis(diphenylphosphine) dioxide (iLab defaults) seems wrong ? (mw) # methanediylbis(diphenylphosphane) dioxide (iLab selected options) # methanediylbis(diphenylphosphane) dioxide (chemspider) # [(Diphenylphosphoryl)methyl](diphenyl)phosphine oxide (chemspider synonym) # bis(diphenylphosphino)methane dioxide (mw) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H22 F3 Nb O3 P2' _chemical_formula_sum 'C25 H22 F3 Nb O3 P2' _chemical_formula_weight 582.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 21/n' _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.154(8) _cell_length_b 10.967(6) _cell_length_c 17.248(10) _cell_angle_alpha 90.00 _cell_angle_beta 97.173(19) _cell_angle_gamma 90.00 _cell_volume 2469(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7848 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 34.6 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.567 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 0.665 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.643 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, VHF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ Superbright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15969 _diffrn_reflns_av_R_equivalents 0.0915 # _diffrn_reflns_av_sigmaI/netI 0.0989 _diffrn_reflns_av_unetI/netI 0.0989 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4794 _reflns_number_gt 3837 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1997)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0790P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4794 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0982 _refine_ls_R_factor_gt 0.0770 _refine_ls_wR_factor_ref 0.1854 _refine_ls_wR_factor_gt 0.1725 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.132 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 0.98709(4) -0.01329(4) 0.81684(3) 0.0332(2) Uani 1 1 d . . . P1 P 0.91564(10) 0.22258(12) 0.68682(8) 0.0230(3) Uani 1 1 d . . . P2 P 0.86848(9) 0.25696(12) 0.85112(8) 0.0207(3) Uani 1 1 d . . . F1 F 1.0141(3) -0.1431(3) 0.7540(2) 0.0507(10) Uani 1 1 d . . . F2 F 1.1234(2) 0.0506(3) 0.8275(2) 0.0373(8) Uani 1 1 d . . . F3 F 0.8372(2) -0.0267(3) 0.7923(2) 0.0357(8) Uani 1 1 d . . . O1 O 0.9651(3) 0.1007(3) 0.7070(2) 0.0272(8) Uani 1 1 d . . . O2 O 0.9500(3) 0.1602(3) 0.8670(2) 0.0231(8) Uani 1 1 d . . . O3 O 0.9935(3) -0.0862(3) 0.9097(2) 0.0338(9) Uani 1 1 d . . . C1 C 0.8558(4) 0.2216(5) 0.5870(3) 0.0259(12) Uani 1 1 d . . . C2 C 0.8780(4) 0.1245(6) 0.5398(3) 0.0345(14) Uani 1 1 d . . . H2 H 0.9206 0.0595 0.5607 0.041 Uiso 1 1 calc R . . C3 C 0.8365(5) 0.1243(7) 0.4604(4) 0.0470(18) Uani 1 1 d . . . H3 H 0.8508 0.0588 0.4274 0.056 Uiso 1 1 calc R . . C4 C 0.7749(5) 0.2195(8) 0.4310(4) 0.052(2) Uani 1 1 d . . . H4 H 0.7487 0.2202 0.3771 0.063 Uiso 1 1 calc R . . C5 C 0.7507(5) 0.3140(6) 0.4784(4) 0.0447(17) Uani 1 1 d . . . H5 H 0.7059 0.3772 0.4577 0.054 Uiso 1 1 calc R . . C6 C 0.7919(4) 0.3160(6) 0.5560(4) 0.0370(15) Uani 1 1 d . . . H6 H 0.7767 0.3818 0.5885 0.044 Uiso 1 1 calc R . . C7 C 1.0087(4) 0.3434(5) 0.6990(3) 0.0229(11) Uani 1 1 d . . . C8 C 1.1122(4) 0.3111(5) 0.7149(3) 0.0284(12) Uani 1 1 d . . . H8 H 1.1317 0.2276 0.7179 0.034 Uiso 1 1 calc R . . C9 C 1.1867(4) 0.4022(5) 0.7264(3) 0.0296(13) Uani 1 1 d . . . H9 H 1.2570 0.3809 0.7370 0.036 Uiso 1 1 calc R . . C10 C 1.1577(4) 0.5237(5) 0.7222(3) 0.0347(14) Uani 1 1 d . . . H10 H 1.2088 0.5853 0.7298 0.042 Uiso 1 1 calc R . . C11 C 1.0557(4) 0.5569(5) 0.7071(3) 0.0321(13) Uani 1 1 d . . . H11 H 1.0367 0.6405 0.7049 0.039 Uiso 1 1 calc R . . C12 C 0.9809(4) 0.4661(5) 0.6950(3) 0.0290(13) Uani 1 1 d . . . H12 H 0.9108 0.4881 0.6839 0.035 Uiso 1 1 calc R . . C13 C 0.8170(3) 0.2567(4) 0.7487(3) 0.0187(10) Uani 1 1 d . . . H13A H 0.7868 0.3376 0.7344 0.022 Uiso 1 1 calc R . . H13B H 0.7618 0.1951 0.7397 0.022 Uiso 1 1 calc R . . C14 C 0.7636(4) 0.2306(5) 0.9062(3) 0.0260(12) Uani 1 1 d . . . C15 C 0.6653(4) 0.2801(5) 0.8833(3) 0.0304(13) Uani 1 1 d . . . H15 H 0.6527 0.3274 0.8370 0.037 Uiso 1 1 calc R . . C16 C 0.5878(5) 0.2595(6) 0.9285(4) 0.0429(16) Uani 1 1 d . . . H16 H 0.5217 0.2933 0.9138 0.052 Uiso 1 1 calc R . . C17 C 0.6067(5) 0.1888(6) 0.9959(4) 0.0446(16) Uani 1 1 d . . . H17 H 0.5533 0.1753 1.0272 0.054 Uiso 1 1 calc R . . C18 C 0.7022(5) 0.1379(6) 1.0179(4) 0.0423(16) Uani 1 1 d . . . H18 H 0.7135 0.0893 1.0637 0.051 Uiso 1 1 calc R . . C19 C 0.7813(4) 0.1576(5) 0.9735(3) 0.0295(12) Uani 1 1 d . . . H19 H 0.8468 0.1222 0.9883 0.035 Uiso 1 1 calc R . . C20 C 0.9234(4) 0.4036(5) 0.8752(3) 0.0214(11) Uani 1 1 d . . . C21 C 0.8652(4) 0.5110(5) 0.8676(3) 0.0263(12) Uani 1 1 d . . . H21 H 0.7936 0.5074 0.8512 0.032 Uiso 1 1 calc R . . C22 C 0.9130(4) 0.6225(5) 0.8841(3) 0.0291(13) Uani 1 1 d . . . H22 H 0.8739 0.6955 0.8781 0.035 Uiso 1 1 calc R . . C23 C 1.0179(4) 0.6284(5) 0.9094(3) 0.0285(12) Uani 1 1 d . . . H23 H 1.0502 0.7051 0.9202 0.034 Uiso 1 1 calc R . . C24 C 1.0747(4) 0.5219(5) 0.9186(3) 0.0264(12) Uani 1 1 d . . . H24 H 1.1457 0.5258 0.9369 0.032 Uiso 1 1 calc R . . C25 C 1.0289(4) 0.4095(5) 0.9014(3) 0.0269(12) Uani 1 1 d . . . H25 H 1.0686 0.3370 0.9072 0.032 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nb1 0.0243(3) 0.0230(3) 0.0475(4) 0.0007(2) -0.0140(2) 0.0012(2) P1 0.0207(7) 0.0272(7) 0.0199(8) -0.0016(5) -0.0020(5) -0.0026(6) P2 0.0181(6) 0.0243(7) 0.0181(8) -0.0003(5) -0.0040(5) 0.0006(5) F1 0.062(2) 0.038(2) 0.046(3) -0.0113(16) -0.0156(19) 0.0095(18) F2 0.0216(16) 0.0446(19) 0.043(2) -0.0118(16) -0.0060(14) 0.0056(15) F3 0.0279(17) 0.0381(19) 0.038(2) 0.0048(14) -0.0067(15) -0.0080(14) O1 0.028(2) 0.0280(19) 0.024(2) -0.0020(16) -0.0007(16) 0.0027(16) O2 0.0240(18) 0.0205(18) 0.023(2) -0.0028(14) -0.0041(15) 0.0025(15) O3 0.047(2) 0.024(2) 0.026(2) 0.0027(16) -0.0109(18) 0.0053(18) C1 0.022(3) 0.037(3) 0.017(3) -0.003(2) -0.004(2) -0.009(2) C2 0.025(3) 0.047(4) 0.031(4) -0.011(3) 0.004(2) -0.015(3) C3 0.036(4) 0.068(5) 0.037(4) -0.024(3) 0.005(3) -0.018(3) C4 0.038(4) 0.097(6) 0.020(4) -0.005(4) -0.007(3) -0.030(4) C5 0.049(4) 0.051(4) 0.030(4) 0.011(3) -0.015(3) -0.019(3) C6 0.038(3) 0.041(3) 0.029(4) 0.005(3) -0.012(3) -0.011(3) C7 0.019(3) 0.038(3) 0.011(3) -0.004(2) -0.001(2) -0.004(2) C8 0.024(3) 0.037(3) 0.024(3) -0.003(2) 0.003(2) -0.001(2) C9 0.017(3) 0.049(4) 0.022(3) -0.001(3) -0.001(2) -0.003(2) C10 0.029(3) 0.048(4) 0.026(3) 0.001(3) 0.001(3) -0.012(3) C11 0.038(3) 0.028(3) 0.029(3) 0.003(2) 0.000(3) -0.006(3) C12 0.025(3) 0.038(3) 0.024(3) 0.001(2) 0.000(2) 0.000(2) C13 0.017(2) 0.022(2) 0.015(3) 0.004(2) -0.0052(19) -0.002(2) C14 0.029(3) 0.025(3) 0.024(3) -0.001(2) -0.001(2) 0.001(2) C15 0.021(3) 0.039(3) 0.031(4) -0.001(2) 0.000(2) -0.001(2) C16 0.032(3) 0.060(4) 0.038(4) -0.009(3) 0.008(3) -0.001(3) C17 0.044(4) 0.059(4) 0.035(4) -0.007(3) 0.020(3) -0.008(3) C18 0.056(4) 0.042(4) 0.030(4) 0.002(3) 0.009(3) -0.001(3) C19 0.032(3) 0.033(3) 0.021(3) 0.001(2) -0.004(2) 0.003(2) C20 0.020(3) 0.026(3) 0.016(3) 0.000(2) -0.005(2) 0.003(2) C21 0.024(3) 0.032(3) 0.022(3) -0.001(2) -0.005(2) 0.004(2) C22 0.028(3) 0.030(3) 0.028(3) -0.006(2) -0.003(2) 0.004(2) C23 0.029(3) 0.031(3) 0.024(3) -0.005(2) -0.003(2) -0.002(2) C24 0.018(3) 0.032(3) 0.027(3) 0.000(2) -0.005(2) -0.001(2) C25 0.022(3) 0.030(3) 0.026(3) 0.000(2) -0.007(2) 0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 O3 1.782(4) . ? Nb1 F1 1.850(3) . ? Nb1 F2 1.912(3) . ? Nb1 F3 1.970(3) . ? Nb1 O2 2.171(3) . ? Nb1 O1 2.257(4) . ? P1 O1 1.508(4) . ? P1 C7 1.798(5) . ? P1 C1 1.801(6) . ? P1 C13 1.819(5) . ? P2 O2 1.509(3) . ? P2 C20 1.791(5) . ? P2 C14 1.793(5) . ? P2 C13 1.811(5) . ? C1 C2 1.394(8) . ? C1 C6 1.397(8) . ? C2 C3 1.408(9) . ? C2 H2 0.9500 . ? C3 C4 1.379(10) . ? C3 H3 0.9500 . ? C4 C5 1.382(10) . ? C4 H4 0.9500 . ? C5 C6 1.380(8) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.394(8) . ? C7 C8 1.401(7) . ? C8 C9 1.396(7) . ? C8 H8 0.9500 . ? C9 C10 1.386(8) . ? C9 H9 0.9500 . ? C10 C11 1.383(8) . ? C10 H10 0.9500 . ? C11 C12 1.396(8) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C19 1.405(7) . ? C14 C15 1.413(7) . ? C15 C16 1.377(8) . ? C15 H15 0.9500 . ? C16 C17 1.393(9) . ? C16 H16 0.9500 . ? C17 C18 1.383(9) . ? C17 H17 0.9500 . ? C18 C19 1.384(8) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.401(7) . ? C20 C25 1.406(7) . ? C21 C22 1.388(7) . ? C21 H21 0.9500 . ? C22 C23 1.396(7) . ? C22 H22 0.9500 . ? C23 C24 1.385(7) . ? C23 H23 0.9500 . ? C24 C25 1.387(7) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? 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 O3 Nb1 F1 100.96(17) . . ? O3 Nb1 F2 98.04(16) . . ? F1 Nb1 F2 95.28(15) . . ? O3 Nb1 F3 95.34(16) . . ? F1 Nb1 F3 94.41(15) . . ? F2 Nb1 F3 161.67(13) . . ? O3 Nb1 O2 91.31(15) . . ? F1 Nb1 O2 167.68(15) . . ? F2 Nb1 O2 83.99(13) . . ? F3 Nb1 O2 83.24(13) . . ? O3 Nb1 O1 171.44(15) . . ? F1 Nb1 O1 87.03(15) . . ? F2 Nb1 O1 84.16(14) . . ? F3 Nb1 O1 80.84(13) . . ? O2 Nb1 O1 80.66(13) . . ? O1 P1 C7 111.0(2) . . ? O1 P1 C1 109.9(2) . . ? C7 P1 C1 109.0(2) . . ? O1 P1 C13 111.4(2) . . ? C7 P1 C13 107.8(2) . . ? C1 P1 C13 107.7(2) . . ? O2 P2 C20 109.4(2) . . ? O2 P2 C14 111.5(2) . . ? C20 P2 C14 109.7(2) . . ? O2 P2 C13 110.3(2) . . ? C20 P2 C13 108.6(2) . . ? C14 P2 C13 107.3(2) . . ? P1 O1 Nb1 133.7(2) . . ? P2 O2 Nb1 137.2(2) . . ? C2 C1 C6 120.2(5) . . ? C2 C1 P1 117.7(4) . . ? C6 C1 P1 122.1(4) . . ? C1 C2 C3 119.0(6) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C4 C3 C2 119.7(6) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 121.2(6) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C6 C5 C4 119.7(7) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C5 C6 C1 120.2(6) . . ? C5 C6 H6 119.9 . . ? C1 C6 H6 119.9 . . ? C12 C7 C8 119.7(5) . . ? C12 C7 P1 122.4(4) . . ? C8 C7 P1 117.9(4) . . ? C9 C8 C7 119.7(5) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C10 C9 C8 119.8(5) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C11 C10 C9 121.1(5) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C10 C11 C12 119.3(6) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C7 C12 C11 120.4(5) . . ? C7 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? P2 C13 P1 111.4(2) . . ? P2 C13 H13A 109.3 . . ? P1 C13 H13A 109.3 . . ? P2 C13 H13B 109.3 . . ? P1 C13 H13B 109.3 . . ? H13A C13 H13B 108.0 . . ? C19 C14 C15 120.0(5) . . ? C19 C14 P2 118.1(4) . . ? C15 C14 P2 121.9(4) . . ? C16 C15 C14 119.7(6) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 119.7(6) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C18 C17 C16 121.0(6) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C17 C18 C19 120.3(6) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C18 C19 C14 119.2(5) . . ? C18 C19 H19 120.4 . . ? C14 C19 H19 120.4 . . ? C21 C20 C25 119.8(5) . . ? C21 C20 P2 122.2(4) . . ? C25 C20 P2 118.0(4) . . ? C22 C21 C20 119.5(5) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C21 C22 C23 120.6(5) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C24 C23 C22 119.6(5) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C23 C24 C25 120.8(5) . . ? C23 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? C24 C25 C20 119.6(5) . . ? C24 C25 H25 120.2 . . ? C20 C25 H25 120.2 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.230 _refine_diff_density_min -0.913 _refine_diff_density_rms 0.134 _iucr_refine_instruction_details ; Add final .res file here for Acta Cryst publications or if required. ; _database_code_depnum_ccdc_archive 'CCDC 973576' ####################################################################### # # 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_12wz1206c _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2013-11-20 # yyyy-mm-dd _chemical_name_systematic ; bis(1,4,7-trimethyl-1-azonia-4,7-diazacyclononane) pentachlorooxidoniobate(V) ; # 1,4,7-trimethyl-1-azonia-4,7-diazacyclononane (from ccdc examples) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C9 H22 N3 1+), Cl5 Nb O 2-' _chemical_formula_sum 'C18 H44 Cl5 N6 Nb O' _chemical_formula_weight 630.75 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 21/c' _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.9479(15) _cell_length_b 16.788(2) _cell_length_c 16.968(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.576(3) _cell_angle_gamma 90.00 _cell_volume 2820.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8174 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 0.923 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.663 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, VHF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ Superbright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11185 _diffrn_reflns_av_R_equivalents 0.0295 # _diffrn_reflns_av_sigmaI/netI 0.0657 _diffrn_reflns_av_unetI/netI 0.0657 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5494 _reflns_number_gt 4158 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1997)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Shelxl-97 --------- H1 & H2 located in dif e/d map. Refined with common Uiso, refxyz and with DFIX on the N-H distance (although barely required). C-H: solution geom; treatment constr. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0295P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed # geom (C-H) difmap (N-H) _refine_ls_hydrogen_treatment mixed # constr (c-H) refxyz (N-H) _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5494 _refine_ls_number_parameters 293 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.0739 _refine_ls_wR_factor_gt 0.0701 _refine_ls_goodness_of_fit_ref 0.946 _refine_ls_restrained_S_all 0.946 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 0.75397(3) 0.005147(14) 0.245866(14) 0.01318(8) Uani 1 1 d . . . Cl1 Cl 0.55984(7) 0.08135(4) 0.27884(4) 0.01799(16) Uani 1 1 d . . . Cl2 Cl 0.90141(7) 0.09265(4) 0.32991(4) 0.01697(16) Uani 1 1 d . . . Cl3 Cl 0.94494(7) -0.08200(4) 0.23485(4) 0.01945(17) Uani 1 1 d . . . Cl4 Cl 0.60978(7) -0.09553(4) 0.18229(4) 0.01714(16) Uani 1 1 d . . . Cl5 Cl 0.72965(7) -0.07386(4) 0.37960(4) 0.01764(17) Uani 1 1 d . . . O1 O 0.77506(19) 0.05830(11) 0.16001(11) 0.0202(5) Uani 1 1 d . . . N1 N 0.8992(3) -0.28135(13) 0.47505(13) 0.0192(6) Uani 1 1 d . . . N2 N 0.8363(2) -0.32663(13) 0.32185(13) 0.0148(5) Uani 1 1 d D . . N3 N 0.7599(2) -0.42679(13) 0.43486(13) 0.0158(5) Uani 1 1 d . . . N4 N 0.6896(2) 0.17276(13) 0.69212(13) 0.0173(6) Uani 1 1 d . . . N5 N 0.6269(3) 0.23721(14) 0.53463(14) 0.0222(6) Uani 1 1 d . . . N6 N 0.7357(3) 0.08841(14) 0.56087(13) 0.0173(5) Uani 1 1 d D . . C1 C 0.8616(3) -0.22361(18) 0.53281(17) 0.0315(8) Uani 1 1 d . . . H1A H 0.7940 -0.2471 0.5642 0.047 Uiso 1 1 calc R . . H1B H 0.8239 -0.1761 0.5053 0.047 Uiso 1 1 calc R . . H1C H 0.9418 -0.2087 0.5679 0.047 Uiso 1 1 calc R . . C2 C 0.9843(3) -0.24822(17) 0.41708(17) 0.0252(7) Uani 1 1 d . . . H2A H 1.0786 -0.2436 0.4413 0.030 Uiso 1 1 calc R . . H2B H 0.9519 -0.1943 0.4012 0.030 Uiso 1 1 calc R . . C3 C 0.9793(3) -0.30174(17) 0.34467(17) 0.0203(7) Uani 1 1 d . . . H3A H 1.0147 -0.2728 0.3002 0.024 Uiso 1 1 calc R . . H3B H 1.0364 -0.3494 0.3566 0.024 Uiso 1 1 calc R . . C4 C 0.7674(3) -0.27314(17) 0.26147(16) 0.0219(7) Uani 1 1 d . . . H4A H 0.8129 -0.2758 0.2129 0.033 Uiso 1 1 calc R . . H4B H 0.7704 -0.2183 0.2815 0.033 Uiso 1 1 calc R . . H4C H 0.6731 -0.2898 0.2501 0.033 Uiso 1 1 calc R . . C5 C 0.8188(3) -0.41282(15) 0.29964(16) 0.0198(7) Uani 1 1 d . . . H5A H 0.8855 -0.4283 0.2628 0.024 Uiso 1 1 calc R . . H5B H 0.7271 -0.4219 0.2730 0.024 Uiso 1 1 calc R . . C6 C 0.8395(3) -0.46236(16) 0.37515(15) 0.0194(7) Uani 1 1 d . . . H6A H 0.8099 -0.5179 0.3641 0.023 Uiso 1 1 calc R . . H6B H 0.9364 -0.4631 0.3951 0.023 Uiso 1 1 calc R . . C7 C 0.6311(3) -0.46673(17) 0.43977(18) 0.0262(7) Uani 1 1 d . . . H7A H 0.5796 -0.4666 0.3875 0.039 Uiso 1 1 calc R . . H7B H 0.5799 -0.4387 0.4777 0.039 Uiso 1 1 calc R . . H7C H 0.6473 -0.5218 0.4573 0.039 Uiso 1 1 calc R . . C8 C 0.8359(3) -0.41687(17) 0.51257(16) 0.0225(7) Uani 1 1 d . . . H8A H 0.8742 -0.4689 0.5306 0.027 Uiso 1 1 calc R . . H8B H 0.7736 -0.3992 0.5512 0.027 Uiso 1 1 calc R . . C9 C 0.9504(3) -0.35637(17) 0.51101(17) 0.0230(7) Uani 1 1 d . . . H9A H 0.9910 -0.3462 0.5657 0.028 Uiso 1 1 calc R . . H9B H 1.0215 -0.3782 0.4802 0.028 Uiso 1 1 calc R . . C10 C 0.7515(3) 0.20702(18) 0.76545(16) 0.0254(8) Uani 1 1 d . . . H10A H 0.7561 0.2651 0.7601 0.038 Uiso 1 1 calc R . . H10B H 0.8429 0.1855 0.7770 0.038 Uiso 1 1 calc R . . H10C H 0.6973 0.1936 0.8088 0.038 Uiso 1 1 calc R . . C11 C 0.5585(3) 0.20931(19) 0.66874(17) 0.0291(8) Uani 1 1 d . . . H11A H 0.5265 0.2363 0.7153 0.035 Uiso 1 1 calc R . . H11B H 0.4927 0.1669 0.6520 0.035 Uiso 1 1 calc R . . C12 C 0.5614(4) 0.2671(2) 0.6044(2) 0.0409(10) Uani 1 1 d . . . H12A H 0.6101 0.3153 0.6251 0.049 Uiso 1 1 calc R . . H12B H 0.4675 0.2830 0.5865 0.049 Uiso 1 1 calc R . . C13 C 0.6602(3) 0.30328(17) 0.48448(17) 0.0276(8) Uani 1 1 d . . . H13A H 0.7199 0.2844 0.4458 0.041 Uiso 1 1 calc R . . H13B H 0.7060 0.3451 0.5173 0.041 Uiso 1 1 calc R . . H13C H 0.5772 0.3248 0.4566 0.041 Uiso 1 1 calc R . . C14 C 0.5559(4) 0.1732(2) 0.4929(2) 0.0399(9) Uani 1 1 d . . . H14A H 0.5183 0.1918 0.4399 0.048 Uiso 1 1 calc R . . H14B H 0.4800 0.1557 0.5223 0.048 Uiso 1 1 calc R . . C15 C 0.6510(3) 0.1041(2) 0.48419(17) 0.0328(9) Uani 1 1 d . . . H15A H 0.5981 0.0558 0.4681 0.039 Uiso 1 1 calc R . . H15B H 0.7105 0.1163 0.4423 0.039 Uiso 1 1 calc R . . C16 C 0.8658(3) 0.04994(17) 0.54903(17) 0.0249(7) Uani 1 1 d . . . H16A H 0.9192 0.0435 0.6003 0.037 Uiso 1 1 calc R . . H16B H 0.9157 0.0832 0.5144 0.037 Uiso 1 1 calc R . . H16C H 0.8490 -0.0025 0.5246 0.037 Uiso 1 1 calc R . . C17 C 0.6575(4) 0.04710(18) 0.62023(18) 0.0348(9) Uani 1 1 d . . . H17A H 0.5598 0.0493 0.6024 0.042 Uiso 1 1 calc R . . H17B H 0.6847 -0.0096 0.6244 0.042 Uiso 1 1 calc R . . C18 C 0.6829(4) 0.08549(17) 0.69819(17) 0.0302(8) Uani 1 1 d . . . H18A H 0.6099 0.0708 0.7312 0.036 Uiso 1 1 calc R . . H18B H 0.7691 0.0654 0.7249 0.036 Uiso 1 1 calc R . . H1 H 0.798(3) -0.3211(16) 0.3676(13) 0.028(6) Uiso 1 1 d D . . H2 H 0.754(3) 0.1359(12) 0.5849(15) 0.028(6) Uiso 1 1 d 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 Nb1 0.01066(13) 0.01354(14) 0.01519(13) 0.00016(11) 0.00052(9) -0.00037(11) Cl1 0.0134(4) 0.0179(4) 0.0226(4) 0.0003(3) 0.0012(3) 0.0027(3) Cl2 0.0148(4) 0.0165(4) 0.0195(4) -0.0006(3) 0.0012(3) -0.0044(3) Cl3 0.0126(4) 0.0197(4) 0.0262(4) -0.0018(3) 0.0029(3) 0.0011(3) Cl4 0.0152(4) 0.0188(4) 0.0172(4) -0.0008(3) -0.0001(3) -0.0033(3) Cl5 0.0180(4) 0.0167(4) 0.0178(4) 0.0025(3) -0.0001(3) -0.0024(3) O1 0.0190(12) 0.0192(11) 0.0230(11) -0.0023(9) 0.0059(9) -0.0043(9) N1 0.0291(16) 0.0145(13) 0.0135(12) -0.0029(11) -0.0001(11) -0.0041(11) N2 0.0143(14) 0.0170(13) 0.0140(13) 0.0012(11) 0.0049(10) -0.0007(11) N3 0.0132(13) 0.0154(13) 0.0191(13) 0.0002(11) 0.0030(10) -0.0028(11) N4 0.0157(14) 0.0175(13) 0.0193(13) -0.0042(11) 0.0049(11) -0.0013(11) N5 0.0234(15) 0.0188(13) 0.0239(14) 0.0032(12) -0.0007(12) 0.0011(12) N6 0.0241(15) 0.0129(13) 0.0155(13) -0.0042(11) 0.0052(11) -0.0013(11) C1 0.044(2) 0.0284(19) 0.0212(17) 0.0010(15) -0.0011(16) -0.0023(16) C2 0.0185(18) 0.0236(17) 0.0324(18) -0.0004(15) -0.0027(14) -0.0061(14) C3 0.0122(16) 0.0213(17) 0.0277(17) 0.0066(14) 0.0035(13) -0.0032(13) C4 0.0205(18) 0.0225(17) 0.0219(17) 0.0052(14) -0.0020(14) 0.0016(14) C5 0.0227(18) 0.0156(15) 0.0220(16) -0.0051(13) 0.0063(13) 0.0005(13) C6 0.0206(18) 0.0156(15) 0.0224(16) 0.0014(13) 0.0041(13) 0.0006(13) C7 0.0217(19) 0.0212(17) 0.0363(19) 0.0041(15) 0.0047(15) -0.0077(14) C8 0.0238(18) 0.0238(17) 0.0197(16) 0.0057(14) 0.0012(13) 0.0004(14) C9 0.0277(19) 0.0242(18) 0.0160(15) 0.0024(13) -0.0033(13) 0.0000(14) C10 0.0253(19) 0.0297(18) 0.0214(17) -0.0060(14) 0.0038(14) 0.0026(15) C11 0.026(2) 0.040(2) 0.0216(17) -0.0101(16) 0.0049(14) 0.0054(16) C12 0.029(2) 0.043(2) 0.053(2) 0.014(2) 0.0144(18) 0.0148(18) C13 0.029(2) 0.0308(19) 0.0232(17) 0.0112(15) 0.0052(15) 0.0043(16) C14 0.045(2) 0.034(2) 0.036(2) 0.0008(17) -0.0172(18) 0.0011(18) C15 0.0190(19) 0.054(2) 0.0241(17) -0.0225(17) -0.0060(14) 0.0071(17) C16 0.0218(19) 0.0219(17) 0.0298(18) -0.0063(15) -0.0035(14) 0.0078(14) C17 0.052(3) 0.0200(18) 0.036(2) -0.0020(16) 0.0207(18) -0.0041(17) C18 0.045(2) 0.0200(17) 0.0281(18) 0.0004(15) 0.0135(16) -0.0108(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 O1 1.7385(18) . ? Nb1 Cl4 2.4036(7) . ? Nb1 Cl3 2.4194(8) . ? Nb1 Cl1 2.4267(7) . ? Nb1 Cl2 2.4364(7) . ? Nb1 Cl5 2.6596(8) . ? N1 C1 1.453(3) . ? N1 C2 1.468(3) . ? N1 C9 1.469(3) . ? N2 C4 1.480(3) . ? N2 C3 1.497(3) . ? N2 C5 1.501(3) . ? N2 H1 0.903(16) . ? N3 C7 1.455(3) . ? N3 C8 1.465(3) . ? N3 C6 1.472(3) . ? N4 C10 1.453(3) . ? N4 C11 1.461(4) . ? N4 C18 1.471(3) . ? N5 C14 1.434(4) . ? N5 C13 1.456(3) . ? N5 C12 1.492(4) . ? N6 C16 1.478(3) . ? N6 C17 1.501(3) . ? N6 C15 1.503(4) . ? N6 H2 0.906(17) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.519(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.525(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.528(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.464(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.513(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.471(4) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Nb1 Cl4 95.75(6) . . ? O1 Nb1 Cl3 94.94(6) . . ? Cl4 Nb1 Cl3 88.79(3) . . ? O1 Nb1 Cl1 94.94(6) . . ? Cl4 Nb1 Cl1 91.18(3) . . ? Cl3 Nb1 Cl1 170.08(2) . . ? O1 Nb1 Cl2 93.79(6) . . ? Cl4 Nb1 Cl2 170.30(2) . . ? Cl3 Nb1 Cl2 88.70(3) . . ? Cl1 Nb1 Cl2 89.69(3) . . ? O1 Nb1 Cl5 177.98(7) . . ? Cl4 Nb1 Cl5 86.13(2) . . ? Cl3 Nb1 Cl5 84.35(2) . . ? Cl1 Nb1 Cl5 85.75(2) . . ? Cl2 Nb1 Cl5 84.31(2) . . ? C1 N1 C2 113.7(2) . . ? C1 N1 C9 113.2(2) . . ? C2 N1 C9 113.8(2) . . ? C4 N2 C3 112.0(2) . . ? C4 N2 C5 112.1(2) . . ? C3 N2 C5 114.7(2) . . ? C4 N2 H1 109.0(19) . . ? C3 N2 H1 103(2) . . ? C5 N2 H1 105.5(18) . . ? C7 N3 C8 112.4(2) . . ? C7 N3 C6 112.8(2) . . ? C8 N3 C6 113.6(2) . . ? C10 N4 C11 111.1(2) . . ? C10 N4 C18 110.7(2) . . ? C11 N4 C18 113.1(3) . . ? C14 N5 C13 114.3(3) . . ? C14 N5 C12 114.3(3) . . ? C13 N5 C12 110.4(2) . . ? C16 N6 C17 114.0(2) . . ? C16 N6 C15 112.6(2) . . ? C17 N6 C15 112.2(3) . . ? C16 N6 H2 108(2) . . ? C17 N6 H2 101.4(18) . . ? C15 N6 H2 107.9(19) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 110.0(2) . . ? N1 C2 H2A 109.7 . . ? C3 C2 H2A 109.7 . . ? N1 C2 H2B 109.7 . . ? C3 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? N2 C3 C2 109.3(2) . . ? N2 C3 H3A 109.8 . . ? C2 C3 H3A 109.8 . . ? N2 C3 H3B 109.8 . . ? C2 C3 H3B 109.8 . . ? H3A C3 H3B 108.3 . . ? N2 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 C6 108.2(2) . . ? N2 C5 H5A 110.1 . . ? C6 C5 H5A 110.1 . . ? N2 C5 H5B 110.1 . . ? C6 C5 H5B 110.1 . . ? H5A C5 H5B 108.4 . . ? N3 C6 C5 108.6(2) . . ? N3 C6 H6A 110.0 . . ? C5 C6 H6A 110.0 . . ? N3 C6 H6B 110.0 . . ? C5 C6 H6B 110.0 . . ? H6A C6 H6B 108.3 . . ? N3 C7 H7A 109.5 . . ? N3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 C9 112.4(2) . . ? N3 C8 H8A 109.1 . . ? C9 C8 H8A 109.1 . . ? N3 C8 H8B 109.1 . . ? C9 C8 H8B 109.1 . . ? H8A C8 H8B 107.9 . . ? N1 C9 C8 110.4(2) . . ? N1 C9 H9A 109.6 . . ? C8 C9 H9A 109.6 . . ? N1 C9 H9B 109.6 . . ? C8 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? N4 C10 H10A 109.5 . . ? N4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N4 C11 C12 113.5(3) . . ? N4 C11 H11A 108.9 . . ? C12 C11 H11A 108.9 . . ? N4 C11 H11B 108.9 . . ? C12 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? C11 C12 N5 114.2(3) . . ? C11 C12 H12A 108.7 . . ? N5 C12 H12A 108.7 . . ? C11 C12 H12B 108.7 . . ? N5 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? N5 C13 H13A 109.5 . . ? N5 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N5 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N5 C14 C15 109.9(3) . . ? N5 C14 H14A 109.7 . . ? C15 C14 H14A 109.7 . . ? N5 C14 H14B 109.7 . . ? C15 C14 H14B 109.7 . . ? H14A C14 H14B 108.2 . . ? N6 C15 C14 110.6(2) . . ? N6 C15 H15A 109.5 . . ? C14 C15 H15A 109.5 . . ? N6 C15 H15B 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? N6 C16 H16A 109.5 . . ? N6 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N6 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 N6 110.2(3) . . ? C18 C17 H17A 109.6 . . ? N6 C17 H17A 109.6 . . ? C18 C17 H17B 109.6 . . ? N6 C17 H17B 109.6 . . ? H17A C17 H17B 108.1 . . ? N4 C18 C17 112.2(2) . . ? N4 C18 H18A 109.2 . . ? C17 C18 H18A 109.2 . . ? N4 C18 H18B 109.2 . . ? C17 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? 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 C1 N1 C2 C3 -160.8(3) . . . . ? C9 N1 C2 C3 67.7(3) . . . . ? C4 N2 C3 C2 93.5(3) . . . . ? C5 N2 C3 C2 -137.2(2) . . . . ? N1 C2 C3 N2 43.8(3) . . . . ? C4 N2 C5 C6 -157.1(2) . . . . ? C3 N2 C5 C6 73.6(3) . . . . ? C7 N3 C6 C5 98.4(3) . . . . ? C8 N3 C6 C5 -132.1(2) . . . . ? N2 C5 C6 N3 47.7(3) . . . . ? C7 N3 C8 C9 -164.5(2) . . . . ? C6 N3 C8 C9 65.9(3) . . . . ? C1 N1 C9 C8 93.6(3) . . . . ? C2 N1 C9 C8 -134.6(2) . . . . ? N3 C8 C9 N1 51.7(3) . . . . ? C10 N4 C11 C12 103.2(3) . . . . ? C18 N4 C11 C12 -131.6(3) . . . . ? N4 C11 C12 N5 50.0(4) . . . . ? C14 N5 C12 C11 65.7(4) . . . . ? C13 N5 C12 C11 -163.7(3) . . . . ? C13 N5 C14 C15 104.0(3) . . . . ? C12 N5 C14 C15 -127.4(3) . . . . ? C16 N6 C15 C14 -154.1(3) . . . . ? C17 N6 C15 C14 75.7(3) . . . . ? N5 C14 C15 N6 44.9(4) . . . . ? C16 N6 C17 C18 96.5(3) . . . . ? C15 N6 C17 C18 -134.0(3) . . . . ? C10 N4 C18 C17 -163.8(3) . . . . ? C11 N4 C18 C17 70.9(3) . . . . ? N6 C17 C18 N4 39.7(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H1 N1 0.903(16) 2.10(3) 2.722(3) 125(2) . N2 H1 N3 0.903(16) 2.16(3) 2.714(3) 119(2) . N6 H2 N4 0.906(17) 2.08(2) 2.715(3) 126(2) . N6 H2 N5 0.906(17) 2.24(3) 2.742(3) 115(2) . _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.136 _refine_diff_density_min -0.552 _refine_diff_density_rms 0.085 _iucr_refine_instruction_details ; Add final .res file here for Acta Cryst publications or if required. ; _vrf_PLAT112_12wz1206c ; PROBLEM: ADDSYM Detects Additional (Pseudo) Symm. Elem... B RESPONSE: ... It is pseudosymmetry and not genuine. ; #===END OF CIF ========== #===END OF FILE ========= _database_code_depnum_ccdc_archive 'CCDC 973577'