#------------------------------------------------------------------------------ #$Date: 2016-03-21 00:21:50 +0100 (Mon, 21 Mar 2016) $ #$Revision: 178377 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/14/4001450.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_4001450 loop_ _publ_author_name 'Shi, Lei' 'Christensen, Kirsten E.' 'Jansson, Kjell' 'Sun, Junliang' 'Zou, Xiaodong' _publ_section_title ; Synthesis and Characterization of an Aluminogermanate SU-46 with a Zeolite Structure ; _journal_issue 24 _journal_name_full 'Chemistry of Materials' _journal_page_first 5973 _journal_paper_doi 10.1021/cm071790f _journal_volume 19 _journal_year 2007 _chemical_formula_moiety 'Al4 Ge6 O20, 4(C2 N1.5 H7.5)' _chemical_formula_sum 'C8 H30 Al4 Ge6 N6 O20' _chemical_formula_weight 1073.84 _chemical_name_systematic ; ? ; _space_group_IT_number 190 _space_group_name_Hall 'P -6c -2c' _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall 'P -6c -2c' _symmetry_space_group_name_H-M 'P -6 2 c' _atom_sites_solution_hydrogens none _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 1 _cell_length_a 7.5240(11) _cell_length_b 7.5240(11) _cell_length_c 14.746(3) _cell_measurement_reflns_used 13733 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 40.9667 _cell_measurement_theta_min 4.1441 _cell_volume 722.9(2) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 16.5467 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _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 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 24646 _diffrn_reflns_theta_full 41.02 _diffrn_reflns_theta_max 41.02 _diffrn_reflns_theta_min 4.17 _exptl_absorpt_coefficient_mu 6.373 _exptl_absorpt_correction_T_max 0.8318 _exptl_absorpt_correction_T_min 0.7010 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'XRED 1.09 (STOE & CIE, 1997a)' _exptl_crystal_colour 'light yellow' _exptl_crystal_density_diffrn 2.467 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 524 _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.711 _refine_diff_density_min -1.202 _refine_diff_density_rms 0.137 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_hydrogen_treatment none _refine_ls_matrix_type full _refine_ls_number_parameters 39 _refine_ls_number_reflns 1625 _refine_ls_number_restraints 5 _refine_ls_restrained_S_all 1.090 _refine_ls_R_factor_all 0.0315 _refine_ls_R_factor_gt 0.0251 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0414P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0636 _refine_ls_wR_factor_ref 0.0647 _reflns_number_gt 1407 _reflns_number_total 1625 _reflns_threshold_expression >2sigma(I) _cod_data_source_file cm071790f-file003.cif _cod_data_source_block p-62c _cod_database_code 4001450 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, y, -z+1/2' 'y, x, z+1/2' 'y, x, -z' 'x-y, -y, -z' 'x-y, -y, z+1/2' '-x, -x+y, z+1/2' '-x, -x+y, -z' '-y, x-y, z' '-y, x-y, -z+1/2' '-x+y, -x, -z+1/2' '-x+y, -x, z' 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 Ge1 Ge 0.83816(4) 0.22663(4) 0.2500 0.01166(7) Uani 0.688(7) 2 d SP Al1 Al 0.83816(4) 0.22663(4) 0.2500 0.01166(7) Uani 0.312(7) 2 d SP Ge2 Ge 1.0000 0.0000 0.38440(2) 0.01044(11) Uani 0.461(6) 3 d SP Al2 Al 1.0000 0.0000 0.38440(2) 0.01044(11) Uani 0.539(6) 3 d SP O1 O 0.9386(3) 0.1815(3) 0.34660(13) 0.0351(5) Uani 1 1 d . O2 O 0.5710(3) 0.0820(3) 0.2500 0.0255(5) Uani 1 2 d S O3 O 1.0000 0.0000 0.5000 0.0346(10) Uani 1 6 d S N1 N 0.3333 0.6667 0.3398(8) 0.060(3) Uiso 0.50 3 d SPD C1 C 0.3333 0.6667 0.4405(11) 0.194(8) Uiso 1 3 d SD C2 C 0.162(2) 0.640(3) 0.4740(11) 0.094(6) Uiso 0.33 1 d PD N2 N 0.0000 0.463(3) 0.5000 0.177(7) Uiso 0.67 2 d SPD 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 Ge1 0.00875(11) 0.00904(12) 0.01834(12) 0.000 0.000 0.00530(10) Al1 0.00875(11) 0.00904(12) 0.01834(12) 0.000 0.000 0.00530(10) Ge2 0.01092(13) 0.01092(13) 0.00948(15) 0.000 0.000 0.00546(6) Al2 0.01092(13) 0.01092(13) 0.00948(15) 0.000 0.000 0.00546(6) O1 0.0485(11) 0.0323(8) 0.0365(9) -0.0049(6) -0.0205(8) 0.0292(8) O2 0.0101(7) 0.0131(8) 0.0548(13) 0.000 0.000 0.0068(6) O3 0.0475(15) 0.0475(15) 0.0089(10) 0.000 0.000 0.0237(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 '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' 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' 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 O1 Ge1 O1 111.42(14) . 2 O1 Ge1 O2 111.07(8) . . O1 Ge1 O2 111.07(8) 2 . O1 Ge1 O2 106.54(7) . 9_655 O1 Ge1 O2 106.54(7) 2 9_655 O2 Ge1 O2 110.00(12) . 9_655 O3 Ge2 O1 108.71(7) . 9_645 O3 Ge2 O1 108.71(7) . 12_765 O1 Ge2 O1 110.22(7) 9_645 12_765 O3 Ge2 O1 108.71(7) . . O1 Ge2 O1 110.22(7) 9_645 . O1 Ge2 O1 110.22(7) 12_765 . Ge1 O1 Ge2 137.29(11) . . Ge1 O2 Al1 130.00(12) . 11_665 Ge1 O2 Ge1 130.00(12) . 11_665 Al2 O3 Ge2 180.0 4_646 . Ge2 O3 Ge2 180.0 4_646 . C2 C1 C2 106.5(12) . 12_565 C2 C1 C2 106.5(13) . 9_665 C2 C1 C2 106.5(12) 12_565 9_665 C2 C1 N1 112.3(11) . . C2 C1 N1 112.3(11) 12_565 . C2 C1 N1 112.3(11) 9_665 . C1 C2 N2 126.8(15) . . C2 N2 C2 114(2) . 8_556 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ge1 O1 1.7241(16) . Ge1 O1 1.7241(16) 2 Ge1 O2 1.7427(18) . Ge1 O2 1.7526(18) 9_655 Ge2 O3 1.7047(5) . Ge2 O1 1.7376(15) 9_645 Ge2 O1 1.7376(15) 12_765 Ge2 O1 1.7376(15) . O2 Al1 1.7526(18) 11_665 O2 Ge1 1.7526(18) 11_665 O3 Al2 1.7047(5) 4_646 O3 Ge2 1.7047(5) 4_646 N1 C1 1.486(15) . C1 C2 1.301(13) . C1 C2 1.301(13) 12_565 C1 C2 1.301(13) 9_665 C2 N2 1.336(16) . N2 C2 1.336(16) 8_556