#------------------------------------------------------------------------------ #$Date: 2012-02-03 19:16:24 +0200 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/32/2013239.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2013239 loop_ _publ_author_name 'Zhicheng Liu' 'Linhong Weng' 'Zhenxia Chen' 'Dongyuan Zhao' _publ_section_title ; (NH~4~)~2~ZrGe~3~O~9~: a new microporous zirconogermanate ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first i29 _journal_page_last i31 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac '(N H4)2 Zr Ge3 O9' _chemical_formula_moiety 'Ge3 N2 O9 Zr' _chemical_formula_sum 'Ge3 N2 O9 Zr' _chemical_formula_weight 481.01 _chemical_name_common FDZG-2 _chemical_name_systematic ; diammonium zirconium getmanate ; _space_group_IT_number 176 _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall '-P 6c' _symmetry_space_group_name_H-M 'P 63/m' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 2 _cell_length_a 7.117(5) _cell_length_b 7.117(5) _cell_length_c 10.542(9) _cell_measurement_reflns_used 568 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 23.02 _cell_measurement_theta_min 5.62 _cell_volume 462.4(6) _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_collection 'SMART (Bruker, 2001)' _computing_data_reduction SAINT _computing_molecular_graphics 'DS Viewerpro (Accelrys, 2002)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Nonius KappaCCDr' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0852 _diffrn_reflns_av_sigmaI/netI 0.0741 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 2333 _diffrn_reflns_theta_full 27.11 _diffrn_reflns_theta_max 27.11 _diffrn_reflns_theta_min 3.31 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 10.789 _exptl_absorpt_correction_T_max 0.6722 _exptl_absorpt_correction_T_min 0.6722 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 3.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 444 _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _refine_diff_density_max 1.460 _refine_diff_density_min -0.840 _refine_ls_extinction_coef 0.009(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 28 _refine_ls_number_reflns 367 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.126 _refine_ls_R_factor_all 0.0763 _refine_ls_R_factor_gt 0.0524 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0415P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1025 _refine_ls_wR_factor_ref 0.1098 _reflns_number_gt 280 _reflns_number_total 367 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bc1005.cif _[local]_cod_data_source_block I _cod_database_code 2013239 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Zr 1.0000 1.0000 0.0000 0.0112(6) Uani d S 1 . . Zr Ge 0.8761(2) 0.6230(2) 0.2500 0.0135(5) Uani d S 1 . . Ge O1 0.9877(12) 0.7564(12) 0.1128(6) 0.0236(17) Uani d . 1 . . O O2 0.9235(16) 0.4027(16) 0.2500 0.025(3) Uani d S 1 . . O N 0.3333 0.6667 0.0559(14) 0.025(4) Uani d S 1 . . N 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 Zr 0.0120(8) 0.0120(8) 0.0096(12) 0.0060(4) 0.000 0.000 Ge 0.0118(8) 0.0101(8) 0.0182(9) 0.0052(7) 0.000 0.000 O1 0.029(5) 0.027(4) 0.024(4) 0.020(4) 0.004(3) 0.014(3) O2 0.014(5) 0.013(5) 0.053(7) 0.011(5) 0.000 0.000 N 0.025(5) 0.025(5) 0.026(9) 0.012(3) 0.000 0.000 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Zr O1 8_565 2.068(7) no Zr O1 2_765 2.068(7) no Zr O1 9_655 2.068(7) no Zr O1 . 2.068(7) yes Zr O1 7_775 2.068(7) no Zr O1 3_675 2.068(7) no Ge O1 10_556 1.694(7) no Ge O1 . 1.694(7) yes Ge O2 2_655 1.738(10) yes Ge O2 . 1.761(9) yes O2 Ge 3_665 1.738(10) no loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 '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' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 Zr O1 8_565 2_765 180.0 no O1 Zr O1 8_565 9_655 90.2(3) no O1 Zr O1 2_765 9_655 89.8(3) no O1 Zr O1 8_565 . 89.8(3) no O1 Zr O1 2_765 . 90.2(3) no O1 Zr O1 9_655 . 89.8(3) no O1 Zr O1 8_565 7_775 90.2(3) no O1 Zr O1 2_765 7_775 89.8(3) no O1 Zr O1 9_655 7_775 90.2(3) no O1 Zr O1 . 7_775 180.0 no O1 Zr O1 8_565 3_675 89.8(3) no O1 Zr O1 2_765 3_675 90.2(3) no O1 Zr O1 9_655 3_675 180.0 no O1 Zr O1 . 3_675 90.2(3) yes O1 Zr O1 7_775 3_675 89.8(3) no O1 Ge O1 10_556 . 117.2(5) yes O1 Ge O2 10_556 2_655 110.6(3) no O1 Ge O2 . 2_655 110.6(3) yes O1 Ge O2 10_556 . 104.7(3) no O1 Ge O2 . . 104.7(3) yes O2 Ge O2 2_655 . 108.3(6) yes Ge O1 Zr . . 140.5(4) yes Ge O2 Ge 3_665 . 131.7(6) yes