data_Nb6Cl14(MeOH)4*6MeOH _publ_contact_author_name 'K\"ockerling, Martin' _publ_contact_author_address ; Universit\"at Rostock Insitut f\"ur Chemie Abt. Anorganische Chemie/Festk\"orperchemie Albert-Einstein-Str. 3a D-18059 Rostock Germany ; _publ_contact_author_email martin.koeckerling@uni-rostock.de _publ_contact_author_phone '++49 381 498 6390' _publ_contact_author_fax '++49 381 498 6382' loop_ _publ_author_name _publ_author_address 'Piedra-Garza, Luis Fernando' ; Universit\"at Rostock Institut f\"ur Chemie Abt. Anorganische Chemie/Festk\"orperchemie Albert-Einstein-Str. 3a D-18059 Rostock Germany ; 'K\"ockerling, Martin' ; Universit\"at Rostock Institut f\"ur Chemie Abt. Anorganische Chemie/Festk\"orperchemie Albert-Einstein-Str. 3a D-18059 Rostock Germany ; _audit_creation_method 'ct.exe (M. K\"ockerling, 1996)' _chemical_formula_moiety 'C4 H16 Nb6 Cl14, 6 C H4 O' _chemical_formula_sum 'C10 H40 Cl14 Nb6 O10' _chemical_formula_weight 1374.18 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' '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9648(8) _cell_length_b 10.0443(9) _cell_length_c 12.0320(11) _cell_angle_alpha 67.530(7) _cell_angle_beta 89.104(7) _cell_angle_gamma 65.392(6) _cell_volume 996.91(15) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 19272 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 29.25 _exptl_crystal_description irregular _exptl_crystal_colour green _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.22 _exptl_crystal_density_diffrn 2.289 _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 2.642 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3564 _exptl_absorpt_correction_T_max 0.4309 _exptl_absorpt_process_details ; r.h. blessing, acta cryst. (1995), a51, 33-38 ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS II' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 19219 _diffrn_reflns_av_R_equivalents 0.0523 _diffrn_reflns_av_sigmaI/netI 0.0486 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 29.22 _reflns_number_total 5358 _reflns_number_gt 4192 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie GmbH)' _computing_cell_refinement 'X-AREA (Stoe & Cie GmbH)' _computing_data_reduction 'STOE XRED32 1.28b (Stoe & Cie GmbH)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+6.2247P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0003(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5358 _refine_ls_number_parameters 202 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0654 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.1103 _refine_ls_wR_factor_gt 0.1065 _refine_ls_goodness_of_fit_ref 1.161 _refine_ls_restrained_S_all 1.161 _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 0.61692(6) 0.62522(6) 0.50452(5) 0.02372(13) Uani 1 1 d . . . Nb2 Nb 0.57122(6) 0.49190(6) 0.34076(5) 0.02404(13) Uani 1 1 d . . . Nb3 Nb 0.68857(6) 0.28394(6) 0.59954(5) 0.02402(13) Uani 1 1 d . . . Cl1 Cl 0.9214(2) 0.0163(2) 0.72189(17) 0.0406(4) Uani 1 1 d . . . Cl2 Cl 0.7219(2) 0.6404(2) 0.31612(16) 0.0344(4) Uani 1 1 d . . . Cl3 Cl 0.5548(2) 0.6565(2) 0.69508(15) 0.0342(3) Uani 1 1 d . . . Cl4 Cl 0.3652(2) 0.7417(2) 0.19485(14) 0.0356(4) Uani 1 1 d . . . Cl5 Cl 0.42043(19) 0.89903(17) 0.39087(15) 0.0322(3) Uani 1 1 d . . . Cl6 Cl 0.85721(18) 0.39854(19) 0.62001(16) 0.0347(4) Uani 1 1 d . . . Cl7 Cl 0.80318(19) 0.24082(19) 0.42629(16) 0.0333(3) Uani 1 1 d . . . O1 O 0.7433(6) 0.7611(6) 0.5127(5) 0.0411(12) Uani 1 1 d D . . H1 H 0.789(10) 0.722(11) 0.585(3) 0.062 Uiso 1 1 d D . . C1 C 0.7692(10) 0.8849(10) 0.4190(8) 0.049(2) Uani 1 1 d . . . H1A H 0.8557 0.8890 0.4486 0.074 Uiso 1 1 calc R . . H1B H 0.6834 0.9868 0.3974 0.074 Uiso 1 1 calc R . . H1C H 0.7859 0.8614 0.3483 0.074 Uiso 1 1 calc R . . O2 O 0.6500(7) 0.4879(6) 0.1636(5) 0.0410(12) Uani 1 1 d D . . H2 H 0.638(11) 0.581(5) 0.116(7) 0.061 Uiso 1 1 d D . . C2 C 0.6991(14) 0.3716(13) 0.1169(9) 0.067(3) Uani 1 1 d . . . H2A H 0.7620 0.3934 0.0582 0.101 Uiso 1 1 calc R . . H2B H 0.6142 0.3738 0.0782 0.101 Uiso 1 1 calc R . . H2C H 0.7549 0.2674 0.1821 0.101 Uiso 1 1 calc R . . O3 O 0.8594(11) 0.7285(9) 0.7180(8) 0.090(3) Uani 1 1 d D . . H3 H 0.903(14) 0.786(14) 0.715(14) 0.135 Uiso 1 1 d D . . C3 C 0.9402(13) 0.5873(13) 0.8165(10) 0.068(3) Uani 1 1 d . . . H3A H 0.9665 0.6094 0.8818 0.102 Uiso 1 1 calc R . . H3B H 1.0298 0.5238 0.7945 0.102 Uiso 1 1 calc R . . H3C H 0.8813 0.5294 0.8428 0.102 Uiso 1 1 calc R . . O4 O 0.6452(10) 0.7457(11) -0.0014(8) 0.081(2) Uani 1 1 d D . . H4 H 0.731(7) 0.743(18) 0.004(14) 0.122 Uiso 1 1 d D . . C4 C 0.5266(17) 0.8674(15) -0.0891(10) 0.087(4) Uani 1 1 d . . . H4A H 0.4357 0.8836 -0.0560 0.130 Uiso 1 1 calc R . . H4B H 0.5219 0.8399 -0.1567 0.130 Uiso 1 1 calc R . . H4C H 0.5386 0.9643 -0.1166 0.130 Uiso 1 1 calc R . . O5 O 0.8679(12) 0.8338(12) -0.0138(7) 0.096(3) Uani 1 1 d D . . H5 H 0.871(19) 0.887(17) -0.087(5) 0.145 Uiso 1 1 d D . . C5 C 0.9121(17) 0.8695(18) 0.0771(11) 0.095(4) Uani 1 1 d . . . H5AA H 0.8636 0.9837 0.0530 0.142 Uiso 1 1 calc R . . H5BA H 1.0188 0.8319 0.0882 0.142 Uiso 1 1 calc R . . H5CA H 0.8842 0.8174 0.1523 0.142 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 0.0255(3) 0.0198(2) 0.0266(3) -0.0085(2) 0.0044(2) -0.0117(2) Nb2 0.0279(3) 0.0218(2) 0.0236(3) -0.0095(2) 0.0067(2) -0.0122(2) Nb3 0.0250(3) 0.0186(2) 0.0254(3) -0.0065(2) 0.0030(2) -0.0092(2) Cl1 0.0363(9) 0.0280(8) 0.0435(10) -0.0073(7) -0.0003(7) -0.0084(7) Cl2 0.0411(9) 0.0370(8) 0.0368(8) -0.0172(7) 0.0173(7) -0.0263(7) Cl3 0.0436(9) 0.0375(8) 0.0338(8) -0.0206(7) 0.0105(7) -0.0237(7) Cl4 0.0397(9) 0.0311(8) 0.0245(7) -0.0057(6) 0.0027(6) -0.0107(7) Cl5 0.0339(8) 0.0191(6) 0.0399(8) -0.0083(6) 0.0048(7) -0.0119(6) Cl6 0.0276(8) 0.0277(7) 0.0440(9) -0.0108(7) -0.0009(7) -0.0114(6) Cl7 0.0311(8) 0.0270(7) 0.0382(8) -0.0148(6) 0.0106(7) -0.0087(6) O1 0.049(3) 0.037(3) 0.040(3) -0.009(2) 0.000(2) -0.028(3) C1 0.059(5) 0.047(4) 0.064(5) -0.032(4) 0.024(4) -0.037(4) O2 0.058(3) 0.032(3) 0.032(3) -0.011(2) 0.017(2) -0.021(3) C2 0.094(8) 0.067(6) 0.063(6) -0.045(5) 0.037(6) -0.040(6) O3 0.126(8) 0.062(5) 0.078(5) -0.005(4) -0.041(5) -0.058(5) C3 0.067(7) 0.064(6) 0.064(6) -0.025(5) -0.004(5) -0.021(5) O4 0.101(7) 0.076(5) 0.061(5) -0.004(4) 0.015(5) -0.056(5) C4 0.140(13) 0.085(8) 0.053(6) -0.023(6) 0.021(7) -0.070(9) O5 0.132(8) 0.119(8) 0.050(4) -0.011(5) 0.013(5) -0.088(7) C5 0.116(11) 0.109(10) 0.056(7) -0.009(7) -0.001(7) -0.069(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 2.235(5) . ? Nb1 Cl5 2.4478(16) . ? Nb1 Cl6 2.4482(18) . ? Nb1 Cl2 2.4597(17) . ? Nb1 Cl3 2.4662(17) . ? Nb1 Nb2 2.9013(8) 2_666 ? Nb1 Nb2 2.9044(8) . ? Nb1 Nb3 2.9256(8) . ? Nb1 Nb3 2.9325(9) 2_666 ? Nb2 O2 2.269(5) . ? Nb2 Cl7 2.4490(17) . ? Nb2 Cl4 2.4594(18) . ? Nb2 Cl3 2.4600(18) 2_666 ? Nb2 Cl2 2.4656(17) . ? Nb2 Nb1 2.9013(8) 2_666 ? Nb2 Nb3 2.9212(9) . ? Nb2 Nb3 2.9345(8) 2_666 ? Nb3 Cl7 2.4578(17) . ? Nb3 Cl6 2.4598(18) . ? Nb3 Cl4 2.4617(17) 2_666 ? Nb3 Cl5 2.4631(17) 2_666 ? Nb3 Cl1 2.5814(18) . ? Nb3 Nb1 2.9325(9) 2_666 ? Nb3 Nb2 2.9345(8) 2_666 ? Cl3 Nb2 2.4600(18) 2_666 ? Cl4 Nb3 2.4617(17) 2_666 ? Cl5 Nb3 2.4631(17) 2_666 ? O1 C1 1.439(9) . ? O2 C2 1.392(10) . ? O3 C3 1.363(12) . ? O4 C4 1.362(15) . ? O5 C5 1.401(15) . ? 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 Cl5 81.13(15) . . ? O1 Nb1 Cl6 80.73(15) . . ? Cl5 Nb1 Cl6 161.86(6) . . ? O1 Nb1 Cl2 82.09(15) . . ? Cl5 Nb1 Cl2 88.78(6) . . ? Cl6 Nb1 Cl2 88.48(6) . . ? O1 Nb1 Cl3 80.18(15) . . ? Cl5 Nb1 Cl3 88.44(6) . . ? Cl6 Nb1 Cl3 88.73(6) . . ? Cl2 Nb1 Cl3 162.27(6) . . ? O1 Nb1 Nb2 134.00(15) . 2_666 ? Cl5 Nb1 Nb2 96.01(4) . 2_666 ? Cl6 Nb1 Nb2 96.75(5) . 2_666 ? Cl2 Nb1 Nb2 143.91(5) . 2_666 ? Cl3 Nb1 Nb2 53.82(4) . 2_666 ? O1 Nb1 Nb2 136.05(15) . . ? Cl5 Nb1 Nb2 96.69(5) . . ? Cl6 Nb1 Nb2 96.16(5) . . ? Cl2 Nb1 Nb2 53.96(4) . . ? Cl3 Nb1 Nb2 143.77(5) . . ? Nb2 Nb1 Nb2 89.95(2) 2_666 . ? O1 Nb1 Nb3 134.31(14) . . ? Cl5 Nb1 Nb3 144.55(5) . . ? Cl6 Nb1 Nb3 53.59(4) . . ? Cl2 Nb1 Nb3 96.26(4) . . ? Cl3 Nb1 Nb3 96.14(4) . . ? Nb2 Nb1 Nb3 60.477(19) 2_666 . ? Nb2 Nb1 Nb3 60.14(2) . . ? O1 Nb1 Nb3 134.70(14) . 2_666 ? Cl5 Nb1 Nb3 53.57(4) . 2_666 ? Cl6 Nb1 Nb3 144.57(5) . 2_666 ? Cl2 Nb1 Nb3 96.20(5) . 2_666 ? Cl3 Nb1 Nb3 96.21(5) . 2_666 ? Nb2 Nb1 Nb3 60.10(2) 2_666 2_666 ? Nb2 Nb1 Nb3 60.36(2) . 2_666 ? Nb3 Nb1 Nb3 90.97(2) . 2_666 ? O2 Nb2 Cl7 81.38(15) . . ? O2 Nb2 Cl4 80.57(15) . . ? Cl7 Nb2 Cl4 161.95(6) . . ? O2 Nb2 Cl3 81.93(15) . 2_666 ? Cl7 Nb2 Cl3 89.15(6) . 2_666 ? Cl4 Nb2 Cl3 88.16(6) . 2_666 ? O2 Nb2 Cl2 80.23(15) . . ? Cl7 Nb2 Cl2 88.59(6) . . ? Cl4 Nb2 Cl2 88.52(6) . . ? Cl3 Nb2 Cl2 162.16(6) 2_666 . ? O2 Nb2 Nb1 135.95(15) . 2_666 ? Cl7 Nb2 Nb1 96.74(5) . 2_666 ? Cl4 Nb2 Nb1 96.09(5) . 2_666 ? Cl3 Nb2 Nb1 54.02(4) 2_666 2_666 ? Cl2 Nb2 Nb1 143.82(5) . 2_666 ? O2 Nb2 Nb1 134.00(15) . . ? Cl7 Nb2 Nb1 96.29(5) . . ? Cl4 Nb2 Nb1 96.33(5) . . ? Cl3 Nb2 Nb1 144.06(5) 2_666 . ? Cl2 Nb2 Nb1 53.77(4) . . ? Nb1 Nb2 Nb1 90.05(2) 2_666 . ? O2 Nb2 Nb3 134.98(14) . . ? Cl7 Nb2 Nb3 53.60(4) . . ? Cl4 Nb2 Nb3 144.45(5) . . ? Cl3 Nb2 Nb3 96.63(5) 2_666 . ? Cl2 Nb2 Nb3 96.24(5) . . ? Nb1 Nb2 Nb3 60.48(2) 2_666 . ? Nb1 Nb2 Nb3 60.29(2) . . ? O2 Nb2 Nb3 133.99(14) . 2_666 ? Cl7 Nb2 Nb3 144.62(5) . 2_666 ? Cl4 Nb2 Nb3 53.43(4) . 2_666 ? Cl3 Nb2 Nb3 96.05(5) 2_666 2_666 ? Cl2 Nb2 Nb3 96.02(4) . 2_666 ? Nb1 Nb2 Nb3 60.17(2) 2_666 2_666 ? Nb1 Nb2 Nb3 60.29(2) . 2_666 ? Nb3 Nb2 Nb3 91.02(2) . 2_666 ? Cl7 Nb3 Cl6 88.64(6) . . ? Cl7 Nb3 Cl4 164.34(6) . 2_666 ? Cl6 Nb3 Cl4 89.02(6) . 2_666 ? Cl7 Nb3 Cl5 88.87(6) . 2_666 ? Cl6 Nb3 Cl5 164.65(6) . 2_666 ? Cl4 Nb3 Cl5 89.30(6) 2_666 2_666 ? Cl7 Nb3 Cl1 81.87(6) . . ? Cl6 Nb3 Cl1 82.40(6) . . ? Cl4 Nb3 Cl1 82.47(6) 2_666 . ? Cl5 Nb3 Cl1 82.24(6) 2_666 . ? Cl7 Nb3 Nb2 53.33(4) . . ? Cl6 Nb3 Nb2 95.48(5) . . ? Cl4 Nb3 Nb2 142.34(5) 2_666 . ? Cl5 Nb3 Nb2 95.16(5) 2_666 . ? Cl1 Nb3 Nb2 135.20(5) . . ? Cl7 Nb3 Nb1 95.56(4) . . ? Cl6 Nb3 Nb1 53.23(4) . . ? Cl4 Nb3 Nb1 95.43(5) 2_666 . ? Cl5 Nb3 Nb1 142.12(5) 2_666 . ? Cl1 Nb3 Nb1 135.63(5) . . ? Nb2 Nb3 Nb1 59.57(2) . . ? Cl7 Nb3 Nb1 95.75(5) . 2_666 ? Cl6 Nb3 Nb1 142.25(4) . 2_666 ? Cl4 Nb3 Nb1 95.57(5) 2_666 2_666 ? Cl5 Nb3 Nb1 53.10(4) 2_666 2_666 ? Cl1 Nb3 Nb1 135.34(5) . 2_666 ? Nb2 Nb3 Nb1 59.42(2) . 2_666 ? Nb1 Nb3 Nb1 89.03(2) . 2_666 ? Cl7 Nb3 Nb2 142.31(5) . 2_666 ? Cl6 Nb3 Nb2 95.64(5) . 2_666 ? Cl4 Nb3 Nb2 53.36(4) 2_666 2_666 ? Cl5 Nb3 Nb2 95.58(4) 2_666 2_666 ? Cl1 Nb3 Nb2 135.82(5) . 2_666 ? Nb2 Nb3 Nb2 88.98(2) . 2_666 ? Nb1 Nb3 Nb2 59.353(19) . 2_666 ? Nb1 Nb3 Nb2 59.35(2) 2_666 2_666 ? Nb1 Cl2 Nb2 72.27(5) . . ? Nb2 Cl3 Nb1 72.17(5) 2_666 . ? Nb2 Cl4 Nb3 73.21(5) . 2_666 ? Nb1 Cl5 Nb3 73.33(4) . 2_666 ? Nb1 Cl6 Nb3 73.18(5) . . ? Nb2 Cl7 Nb3 73.07(5) . . ? C1 O1 Nb1 131.9(5) . . ? C2 O2 Nb2 133.5(5) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 29.22 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.124 _refine_diff_density_min -0.941 _refine_diff_density_rms 0.183