data_S72-IC971224U # ic971224u.cif #--------------------------------------------------------------------------- --- _audit_creation_date 'Fri Jul 18 09:48:59 1997' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #--------------------------------------------------------------------------- --- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #--------------------------------------------------------------------------- --- _cell_length_a 12.993(1) _cell_length_b 10.733(1) _cell_length_c 16.878(3) _cell_angle_alpha 90 _cell_angle_beta 97.11(1) _cell_angle_gamma 90 _cell_volume 2335.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 153.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.0 _cell_measurement_theta_max 11.9 #--------------------------------------------------------------------------- --- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' +x, +y, +z' ' -x, +y,1/2-z' ' -x, +y,1/2-z' ' -x, -y, -z' ' -x, -y, -z' ' +x, -y,1/2+z' ' +x, -y,1/2+z' #--------------------------------------------------------------------------- --- _exptl_crystal_description 'platey' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.230 _exptl_crystal_size_min 0.140 _exptl_crystal_density_diffrn 1.799 _exptl_crystal_density_meas 1.78(2) _exptl_crystal_density_method 'flotation pycnometry' _chemical_formula_weight 632.71 _chemical_formula_analytical ? _chemical_formula_sum 'C20 H20 Cd F5 N4 Nb O ' _chemical_formula_moiety 'C20 H20 Cd F5 N4 Nb O ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1240.00 _exptl_absorpt_coefficient_mu 1.461 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details Tompa_analytical _exptl_absorpt_correction_T_max 0.832 _exptl_absorpt_correction_T_min 0.729 #--------------------------------------------------------------------------- --- _diffrn_special_details none _diffrn_ambient_temperature 153.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'CAD4' _diffrn_measurement_method 'omega/theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 90 _diffrn_standards_decay_% -2.09 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -4 4 6 4 4 4 3 3 -8 _diffrn_reflns_number 4534 _reflns_number_total 2163 _reflns_number_observed 3685 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents .0228 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 24.97 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.02130 _diffrn_orient_matrix_UB_12 0.08924 _diffrn_orient_matrix_UB_13 -0.00705 _diffrn_orient_matrix_UB_21 -0.01784 _diffrn_orient_matrix_UB_22 -0.01408 _diffrn_orient_matrix_UB_23 -0.05866 _diffrn_orient_matrix_UB_31 -0.07242 _diffrn_orient_matrix_UB_32 -0.02275 _diffrn_orient_matrix_UB_33 0.00861 #--------------------------------------------------------------------------- --- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Nb 0 4 -2.073 0.621 'International Tables' F 0 20 0.017 0.010 'International Tables' O 0 4 0.011 0.006 'International Tables' C 0 80 0.003 0.002 'International Tables' N 0 16 0.006 0.003 'International Tables' H 0 80 0.000 0.000 'International Tables' Cd 0 4 -0.807 1.202 'International Tables' #--------------------------------------------------------------------------- --- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Cd(1) 0.250 0.250 0.500 0.02290(6) Uij ? ? Nb(1) 0.000 0.000 0.500 0.03077(8) Uij ? ? F(1) 0.111 0.118 0.498 0.029 Uij ? ? F(2) -0.0957(1) 0.1209(1) 0.45287(9) 0.0429(4) Uij ? ? F(3) -0.0223(1) 0.0573(1) 0.60492(8) 0.0388(4) Uij ? ? O(1) 0.1110(1) 0.1182(1) 0.49781(7) 0.0294(4) Uij ? ? N(1) 0.2464(1) 0.2222(2) 0.3614(1) 0.0258(5) Uij ? ? N(2) 0.3593(2) 0.0832(2) 0.5401(1) 0.0324(5) Uij ? ? C(1) 0.1761(2) 0.1488(2) 0.3194(1) 0.0320(6) Uij ? ? C(2) 0.1584(2) 0.1499(2) 0.2373(1) 0.0357(7) Uij ? ? C(3) 0.2163(2) 0.2293(2) 0.1959(1) 0.0399(7) Uij ? ? C(4) 0.2898(2) 0.3039(2) 0.2383(1) 0.0393(7) Uij ? ? C(5) 0.3016(2) 0.2990(2) 0.3205(1) 0.0303(6) Uij ? ? C(6) 0.4470(2) 0.1008(2) 0.5888(2) 0.0431(8) Uij ? ? C(7) 0.5030(2) 0.0049(3) 0.6256(2) 0.062(1) Uij ? ? C(8) 0.4690(3) -0.1160(3) 0.6096(2) 0.071(1) Uij ? ? C(9) 0.3807(3) -0.1355(3) 0.5586(2) 0.065(1) Uij ? ? C(10) 0.3280(2) -0.0338(2) 0.5255(2) 0.0449(8) Uij ? ? H(1) 0.137 0.093 0.348 0.038 Uij ? ? H(2) 0.107 0.097 0.209 0.043 Uij ? ? H(3) 0.206 0.232 0.139 0.048 Uij ? ? H(4) 0.332 0.358 0.211 0.047 Uij ? ? H(5) 0.351 0.352 0.349 0.036 Uij ? ? H(6) 0.471 0.184 0.598 0.052 Uij ? ? H(7) 0.564 0.021 0.662 0.075 Uij ? ? H(8) 0.507 -0.185 0.634 0.085 Uij ? ? H(9) 0.356 -0.217 0.546 0.079 Uij ? ? H(10) 0.266 -0.047 0.490 0.053 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cd(1) 0.0288(1) 0.0196(1) 0.0196(1) -0.0104(1) 0.00015(9) 0.00082(9) Nb(1) 0.0425(2) 0.0287(2) 0.0189(1) 0.0053(1) -0.0049(1) 0.0032(1) F(1) 0.033 0.027 0.027 -0.014 0.000 0.002 F(2) 0.0387(8) 0.0339(8) 0.0527(9) 0.0002(7) -0.0079(7) 0.0184(7) F(3) 0.0539(9) 0.0368(8) 0.0268(7) -0.0207(7) 0.0087(6) -0.0061(6) O(1) 0.0330(8) 0.0275(8) 0.0266(7) -0.0143(7) -0.0005(6) 0.0020(6) N(1) 0.030(1) 0.0228(10) 0.0234(9) -0.0031(8) 0.0001(8) -0.0014(8) N(2) 0.036(1) 0.027(1) 0.036(1) -0.0024(9) 0.0116(9) 0.0006(9) C(1) 0.037(1) 0.030(1) 0.030(1) -0.012(1) 0.008(1) -0.003(1) C(2) 0.039(1) 0.037(1) 0.030(1) -0.012(1) 0.001(1) -0.010(1) C(3) 0.049(2) 0.047(2) 0.024(1) -0.008(1) 0.003(1) -0.004(1) C(4) 0.047(2) 0.043(1) 0.028(1) -0.017(1) 0.007(1) 0.001(1) C(5) 0.031(1) 0.030(1) 0.029(1) -0.008(1) 0.000(1) -0.003(1) C(6) 0.039(2) 0.039(2) 0.052(2) 0.003(1) 0.009(1) 0.007(1) C(7) 0.039(2) 0.073(2) 0.075(2) 0.016(2) 0.008(2) 0.019(2) C(8) 0.052(2) 0.052(2) 0.116(3) 0.025(2) 0.041(2) 0.040(2) C(9) 0.056(2) 0.029(2) 0.121(3) 0.007(1) 0.050(2) 0.007(2) C(10) 0.046(2) 0.027(1) 0.065(2) -0.001(1) 0.024(1) -0.006(1) #--------------------------------------------------------------------------- --- _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_extinction_coef 2.19778 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3685 _refine_ls_number_parameters 148 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0258 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0306 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.093 _refine_ls_shift/esd_max 0.0035 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.63 _refine_diff_density_max 1.18 #--------------------------------------------------------------------------- --- _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd(1) F(1) 2.2909(1) ? ? yes Cd(1) F(1) 2.2909(1) ? ? yes Cd(1) N(1) 2.354(2) ? ? yes Cd(1) N(1) 2.354(2) ? ? yes Cd(1) N(2) 2.333(2) ? ? yes Cd(1) N(2) 2.333(2) ? ? yes Nb(1) F(1) 1.9245(1) ? ? yes Nb(1) F(1) 1.9245(1) ? ? yes Nb(1) F(2) 1.902(1) ? ? yes Nb(1) F(2) 1.902(1) ? ? yes Nb(1) F(3) 1.930(1) ? ? yes Nb(1) F(3) 1.930(1) ? ? yes N(1) C(1) 1.340(3) ? ? yes N(1) C(5) 1.339(3) ? ? yes N(2) C(6) 1.333(3) ? ? yes N(2) C(10) 1.333(3) ? ? yes C(1) C(2) 1.377(3) ? ? yes C(2) C(3) 1.382(4) ? ? yes C(3) C(4) 1.377(4) ? ? yes C(4) C(5) 1.377(3) ? ? yes C(6) C(7) 1.365(4) ? ? yes C(7) C(8) 1.387(5) ? ? yes C(8) C(9) 1.363(5) ? ? yes C(9) C(10) 1.370(4) ? ? yes #--------------------------------------------------------------------------- --- 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F(1) Cd(1) F(1) 180.0 ? ? ? yes F(1) Cd(1) N(1) 89.25(4) ? ? ? yes F(1) Cd(1) N(1) 90.75(4) ? ? ? yes F(1) Cd(1) N(2) 88.93(5) ? ? ? yes F(1) Cd(1) N(2) 91.07(5) ? ? ? yes F(1) Cd(1) N(1) 90.75(4) ? ? ? yes F(1) Cd(1) N(1) 89.25(4) ? ? ? yes F(1) Cd(1) N(2) 91.07(5) ? ? ? yes F(1) Cd(1) N(2) 88.93(5) ? ? ? yes N(1) Cd(1) N(1) 180.0 ? ? ? yes N(1) Cd(1) N(2) 97.33(7) ? ? ? yes N(1) Cd(1) N(2) 82.67(7) ? ? ? yes N(1) Cd(1) N(2) 82.67(7) ? ? ? yes N(1) Cd(1) N(2) 97.33(7) ? ? ? yes N(2) Cd(1) N(2) 180.0 ? ? ? yes F(1) Nb(1) F(1) 180.0 ? ? ? yes F(1) Nb(1) F(2) 89.71(4) ? ? ? yes F(1) Nb(1) F(2) 90.29(4) ? ? ? yes F(1) Nb(1) F(3) 90.33(4) ? ? ? yes F(1) Nb(1) F(3) 89.67(4) ? ? ? yes F(1) Nb(1) F(2) 90.29(4) ? ? ? yes F(1) Nb(1) F(2) 89.71(4) ? ? ? yes F(1) Nb(1) F(3) 89.67(4) ? ? ? yes F(1) Nb(1) F(3) 90.33(4) ? ? ? yes F(2) Nb(1) F(2) 180.0 ? ? ? yes F(2) Nb(1) F(3) 90.08(7) ? ? ? yes F(2) Nb(1) F(3) 89.92(7) ? ? ? yes F(2) Nb(1) F(3) 89.92(7) ? ? ? yes F(2) Nb(1) F(3) 90.08(7) ? ? ? yes F(3) Nb(1) F(3) 180.0 ? ? ? yes Cd(1) F(1) Nb(1) 176.3021(1) ? ? ? yes Cd(1) O(1) Nb(1) 176.30(7) ? ? ? yes Cd(1) N(1) C(1) 121.9(1) ? ? ? yes Cd(1) N(1) C(5) 119.2(1) ? ? ? yes C(1) N(1) C(5) 117.6(2) ? ? ? yes Cd(1) N(2) C(6) 120.8(2) ? ? ? yes Cd(1) N(2) C(10) 120.5(2) ? ? ? yes C(6) N(2) C(10) 117.8(2) ? ? ? yes N(1) C(1) C(2) 123.0(2) ? ? ? yes C(1) C(2) C(3) 118.7(2) ? ? ? yes C(2) C(3) C(4) 118.7(2) ? ? ? yes C(3) C(4) C(5) 119.1(2) ? ? ? yes N(1) C(5) C(4) 122.8(2) ? ? ? yes N(2) C(6) C(7) 122.7(3) ? ? ? yes C(6) C(7) C(8) 118.6(3) ? ? ? yes C(7) C(8) C(9) 119.3(3) ? ? ? yes C(8) C(9) C(10) 118.3(3) ? ? ? yes N(2) C(10) C(9) 123.3(3) ? ? ? yes #--------------------------------------------------------------------------- --- _publ_requested_journal 'Inorganic Chemistry' _publ_contact_author ; Poeppelmeier, Kenneth R. Department of Chemistry Northwestern University Evanston, Illinois 60208-3113 ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone '(847) 491-3505' _publ_contact_author_fax '(847) 491-7713' _publ_contact_author_email 'krp@nwu.edu' loop_ _publ_author_name _publ_author_address 'Halasyamani, Paramasivan' ; Department of Chemistry Northwestern University Evanston, Illinois 60208-3113 ; 'Heier, Kevin R.' ; Department of Chemistry Northwestern University Evanston, Illinois 60208-3113 ; 'Norquist, Alexander J.' ; Department of Chemistry Northwestern University Evanston, Illinois 60208-3113 ; 'Stern, Charlotte L.' ; Department of Chemistry Northwestern University Evanston, Illinois 60208-3113 ; 'Poeppelmeier^*^, Kenneth R.' ; Department of Chemistry Northwestern University Evanston, Illinois 60208-3113 ; _publ_section_title ; Composition Space of the (CdO, 1/2 Nb2O5)/(HF)x.pyridine/H2O System. Structure and Synthesis of CdNb(py)4OF5 ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ;