#------------------------------------------------------------------------------ #$Date: 2012-02-24 19:13:23 +0200 (Fri, 24 Feb 2012) $ #$Revision: 34330 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/32/37/4323786.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4323786 loop_ _publ_author_name 'Paramasivan Halasyamani' 'Michael J. Willis' 'Charlotte L. Stern' 'Paul M. Lundquist' 'George K. Wong' 'Kenneth R. Poeppelmeier' _publ_contact_author ; Poeppelmeier, Kenneth Department of Chemistry Northwestern University Evanston, Illinois 60208-3113 USA ; _publ_contact_author_email ' krp@nwu.edu' _publ_contact_author_fax ' (708) 491-7713' _publ_contact_author_phone '(708) 491-3505' _publ_section_title ; Composition Space of the (CuO,1/2Nb~2~O~5~)/(HF)~x~.pyridine/H~2~O System. Structure and Synthesis of [pyH^+^]~2-~[CuNb~2~(py)~4~O~2~F~10~]^2+^ and CuNb(py)~4~OF~5~ ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 1367 _journal_page_last 1371 _journal_volume 35 _journal_year 1996 _chemical_compound_source 'hydro(solvato)thermal synthesis' _chemical_formula_moiety 'C30 H32 Cu F10 N6 Nb2 O2' _chemical_formula_sum 'C30 H32 Cu F10 N6 Nb2 O2' _chemical_formula_weight 947.96 _space_group_IT_number 98 _symmetry_cell_setting tetragonal _symmetry_Int_Tables_number 98 _symmetry_space_group_name_Hall 'I 4bw 2bw' _symmetry_space_group_name_H-M 'I 41 2 2' _audit_creation_date 'Fri Apr 21 17:16:01 1995' _audit_creation_method 'from TEXRAY.INF file' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.408(3) _cell_length_b 11.408(3) _cell_length_c 30.36(1) _cell_measurement_reflns_used 25 _cell_measurement_temperature 153.2 _cell_measurement_theta_max 13.5 _cell_measurement_theta_min 12.2 _cell_volume 3951(2) _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_data_reduction teXsan _computing_publication_material teXsan _computing_structure_refinement teXsan _computing_structure_solution SHELXS-86 _diffrn_ambient_temperature 153.2 _diffrn_measurement_device CAD4 _diffrn_measurement_method 'omega/theta scans' _diffrn_orient_matrix_UB_11 0.04810 _diffrn_orient_matrix_UB_12 0.04498 _diffrn_orient_matrix_UB_13 -0.02176 _diffrn_orient_matrix_UB_21 -0.07305 _diffrn_orient_matrix_UB_22 0.03513 _diffrn_orient_matrix_UB_23 -0.01251 _diffrn_orient_matrix_UB_31 0.00617 _diffrn_orient_matrix_UB_32 0.06652 _diffrn_orient_matrix_UB_33 0.02133 _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_type MoKalpha _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 3.95 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 1962 _diffrn_reflns_theta_max 24.94 _diffrn_standards_decay_% -1.39 _diffrn_standards_interval_count 90 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.185 _exptl_absorpt_correction_T_max 0.870 _exptl_absorpt_correction_T_min 0.805 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details Tompa_analytical _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_meas 1.59(1) _exptl_crystal_density_method 'flotation pycnometry' _exptl_crystal_description prismatic _exptl_crystal_F_000 1884.00 _exptl_crystal_size_max 0.460 _exptl_crystal_size_mid 0.190 _exptl_crystal_size_min 0.110 _refine_diff_density_max 0.71 _refine_diff_density_min -0.85 _refine_ls_extinction_coef 0.31440 _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_goodness_of_fit_obs 2.424 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 110 _refine_ls_number_reflns 872 _refine_ls_number_restraints 0 _refine_ls_R_factor_obs 0.0430 _refine_ls_shift/esd_max 0.0160 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme sigma _refine_ls_wR_factor_obs 0.0440 _reflns_number_observed 872 _reflns_number_total 1094 _reflns_observed_criterion 3.00 _[local]_cod_data_source_file ic951189w_2.cif _[local]_cod_data_source_block CuNbtet _cod_database_code 4323786 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' 1/2+x,1/2+y,1/2+z ' -x, -y, +z' 1/2-x,1/2-y,1/2+z ' -x,1/2+y,1/4-z' '1/2-x, +y,3/4-z' ' +x,1/2-y,1/4-z' '1/2+x, -y,3/4-z' ' +y, +x, -z' 1/2+y,1/2+x,1/2-z ' -y, -x, -z' 1/2-y,1/2-x,1/2-z ' -y,1/2+x,1/4+z' '1/2-y, +x,3/4+z' ' +y,1/2-x,1/4+z' '1/2+y, -x,3/4+z' 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 Nb() 0.0143(3) 0.014 0.0221(5) -0.0016(5) 0.000 -0.0002(4) Cu() 0.0158(7) 0.016 0.018(1) 0.0008(9) 0.000 0.000 F(1) 0.015(3) 0.032(4) 0.040(4) 0.004(2) 0.000(3) 0.000(3) F(2) 0.026(3) 0.024(3) 0.031(3) 0.003(2) -0.013(2) -0.010(3) F(3) 0.033(4) 0.033 0.115(9) -0.023(4) 0.018 -0.018(7) O(1) 0.015(3) 0.015 0.025(5) -0.002(4) 0.003 -0.003(5) N(1) 0.005(6) 0.042(8) 0.024(6) -0.004(5) 0.000 0.000 N(2) 0.019(3) 0.019 0.025(6) 0.002(5) 0.002 0.002(7) C(1) 0.08(1) 0.09(1) 0.022(5) -0.066(8) 0.007(10) 0.005(10) C(2) 0.07(1) 0.09(1) 0.017(6) -0.057(8) -0.004(9) -0.002(9) C(3) 0.07(1) 0.02(1) 0.011(6) -0.012(8) 0.000 0.000 C(4) 0.025(5) 0.013(4) 0.09(1) -0.002(4) -0.014(7) -0.009(6) C(5) 0.018(6) 0.032(6) 0.11(1) -0.003(5) -0.005(10) -0.019(10) C(6) 0.024(5) 0.024 0.06(1) 0.019(6) -0.007 -0.007(10) C(7) 0.10(1) 0.08(1) 0.037(6) -0.073(8) 0.03(1) -0.02(1) C(8) 0.105 0.115 0.023 -0.087 0.004 -0.006 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 Nb() 0.75696(7) 0.757 0.500 0.017 Uani ? ? Cu() 0.500 0.500 0.500 0.016 Uani ? ? F(1) 0.8868(4) 0.6507(4) 0.4911(2) 0.029 Uani ? ? F(2) 0.7859(4) 0.7532(4) 0.5626(1) 0.027 Uani ? ? F(3) 0.8871(4) 0.887 0.500 0.061 Uani ? ? O(1) 0.6493(5) 0.649 0.500 0.019 Uani ? ? N(1) 0.500 0.500 0.5676(3) 0.024 Uani ? ? N(2) 0.3722(6) 0.628 0.500 0.021 Uani ? ? N(3) 0.955(1) 0.961(1) 0.4141(3) 0.031(4) iso ? ? C(1) 0.573(2) 0.564(2) 0.5904(3) 0.067 Uani ? ? C(2) 0.579(2) 0.563(2) 0.6354(3) 0.059 Uani ? ? C(3) 0.500 0.500 0.6591(3) 0.032 Uani ? ? C(4) 0.2624(9) 0.6031(7) 0.4906(5) 0.041 Uani ? ? C(5) 0.174(1) 0.685(1) 0.4916(5) 0.052 Uani ? ? C(6) 0.1997(8) 0.800 0.500 0.037 Uani ? ? C(7) 0.917(2) 0.916(2) 0.3758(4) 0.072 Uani ? ? C(8) 0.962(2) 0.954(2) 0.3372(3) 0.081 Uani ? ? C(9) 0.955 0.961 0.414 0.053 iso ? ? H(1) 0.626 0.613 0.575 0.074 equiv ? ? H(2) 0.638 0.606 0.650 0.072 equiv ? ? H(3) 0.500 0.500 0.691 0.051 equiv ? ? H(4) 0.243 0.525 0.483 0.052 equiv ? ? H(5) 0.095 0.661 0.487 0.063 equiv ? ? H(6) 0.138 0.862 0.500 0.051 equiv ? ? H(7) 0.858 0.856 0.376 0.051 equiv ? ? H(8) 0.929 0.926 0.309 0.051 equiv ? ? H(9) 0.929 0.927 0.442 0.051 equiv ? ? 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 Cu 0 4 0.320 1.265 'International Tables' Nb 0 8 -2.073 0.621 'International Tables' O 0 8 0.011 0.006 'International Tables' F 0 40 0.017 0.010 'International Tables' N 0 24 0.006 0.003 'International Tables' C 0 120 0.003 0.002 'International Tables' H 0 128 0.000 0.000 'International Tables' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? 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) Nb F(1) 168.9(3) . . . yes F(1) Nb F(2) 89.0(2) . . . yes F(1) Nb F(2) 89.8(2) . . . yes F(1) Nb F(3) 84.5(2) . . . yes F(1) Nb O(1) 95.5(2) . . . yes F(1) Nb F(2) 89.8(2) . . . yes F(1) Nb F(2) 89.0(2) . . . yes F(1) Nb F(3) 84.5(2) . . . yes F(1) Nb O(1) 95.5(2) . . . yes F(2) Nb F(2) 168.0(3) . . . yes F(2) Nb F(3) 84.0(2) . . . yes F(2) Nb O(1) 96.0(2) . . . yes F(2) Nb F(3) 84.0(2) . . . yes F(2) Nb O(1) 96.0(2) . . . yes F(3) Nb O(1) 180.0 . . . yes N(1) Cu N(1) 180.0 . . . yes N(1) Cu N(2) 90.0 . . . yes N(1) Cu N(2) 90.0 . . . yes N(1) Cu N(2) 90.0 . . . yes N(1) Cu N(2) 90.0 . . . yes N(2) Cu N(2) 180.0 . . . yes Cu N(1) C(1) 121.9(6) . . . yes Cu N(1) C(1) 121.9(6) . . . yes C(1) N(1) C(1) 116(1) . . . yes Cu N(2) C(4) 121.7(6) . . . yes Cu N(2) C(4) 121.7(6) . . . yes C(4) N(2) C(4) 116(1) . . . yes N(3) N(3) C(7) 119.2(6) . . . yes N(1) C(1) C(2) 124.4(10) . . . yes C(1) C(2) C(3) 119.5(10) . . . yes C(2) C(3) C(2) 115(1) . . . yes N(2) C(4) C(5) 123.9(10) . . . yes C(4) C(5) C(6) 118(1) . . . yes C(5) C(6) C(5) 117(1) . . . yes N(3) C(7) C(8) 120.2(10) . . . yes C(7) C(8) C(8) 119.7(8) . . . yes N(3) C(9) C(7) 119.2(6) . . . yes 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 Nb F(1) 1.933(5) . . yes Nb F(1) 1.933(5) . . yes Nb F(2) 1.930(4) . . yes Nb F(2) 1.930(4) . . yes Nb F(3) 2.101(7) . . yes Nb O(1) 1.731(8) . . yes Cu N(1) 2.056(10) . . yes Cu N(1) 2.056(10) . . yes Cu N(2) 2.06(1) . . yes Cu N(2) 2.06(1) . . yes N(1) C(1) 1.29(1) . . yes N(1) C(1) 1.29(1) . . yes N(2) C(4) 1.32(1) . . yes N(2) C(4) 1.32(1) . . yes N(3) N(3) 1.38(2) . . yes N(3) C(7) 1.35(1) . . yes C(1) C(2) 1.37(1) . . yes C(2) C(3) 1.37(1) . . yes C(4) C(5) 1.38(2) . . yes C(5) C(6) 1.37(1) . . yes C(7) C(8) 1.34(1) . . yes C(8) C(8) 1.37(2) . . yes