#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2011884.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_2011884 loop_ _publ_author_name 'Tripathi, Akhilesh' 'Parise, John B.' 'Kim, Sun Jin' 'Lee, Yongjae' 'Uh, Young Sun' _publ_section_title ; K~5.76~Ga~5.76~Si~10.24~O~32~·3.4H~2~O, a gallosilicate with the zeolite gismondine topology ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 344 _journal_page_last 346 _journal_volume 57 _journal_year 2001 _chemical_formula_moiety 'K5.76 Ga5.76 Si10.24 O32 , 3.4H2 O' _chemical_formula_sum 'Ga5.76 H6.8 K5.76 O35.36 Si10.24' _chemical_formula_weight 1484.3994 _chemical_name_common Gismondine _space_group_IT_number 88 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall '-I 4ad' _symmetry_space_group_name_H-M 'I 41/a :2' _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 1 _cell_length_a 9.9639(6) _cell_length_b 9.9639(6) _cell_length_c 9.3806(9) _cell_measurement_reflns_used 5045 _cell_measurement_temperature 298(5) _cell_measurement_theta_max 30.62 _cell_measurement_theta_min 2.62 _cell_volume 931.30(12) _computing_cell_refinement SMART _computing_data_collection 'SMART (Bruker AXS, 1996)' _computing_data_reduction 'SAINT (Bruker AXS, 1996)' _computing_molecular_graphics 'Crystalmaker (Palmer, 2000)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 0.70 _diffrn_measured_fraction_theta_full .864 _diffrn_measured_fraction_theta_max .864 _diffrn_measurement_device_type 'Bruker SMART CCD area detector diffractometer' _diffrn_measurement_method '\f scans' _diffrn_radiation_monochromator Si(111) _diffrn_radiation_source Synchrotron _diffrn_radiation_type Synchrotron _diffrn_radiation_wavelength .6430 _diffrn_reflns_av_R_equivalents .0935 _diffrn_reflns_av_sigmaI/netI .0643 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 5111 _diffrn_reflns_theta_full 30.62 _diffrn_reflns_theta_max 30.62 _diffrn_reflns_theta_min 2.62 _exptl_absorpt_coefficient_mu 5.196 _exptl_absorpt_correction_T_max .959 _exptl_absorpt_correction_T_min .949 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.647 _exptl_crystal_density_meas 'not measured' _exptl_crystal_description octahedral _exptl_crystal_F_000 715 _exptl_crystal_size_max .010 _exptl_crystal_size_mid .008 _exptl_crystal_size_min .008 _refine_diff_density_max 1.189 _refine_diff_density_min -.974 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_hydrogen_treatment none _refine_ls_matrix_type full _refine_ls_number_parameters 47 _refine_ls_number_reflns 939 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.131 _refine_ls_R_factor_all .0844 _refine_ls_R_factor_gt .0671 _refine_ls_shift/su_max <0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0460P)^2^+15.7958P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .1558 _reflns_number_gt 749 _reflns_number_total 939 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file iz1009.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M ' I 41/a ' _[local]_cod_cif_authors_sg_Hall ' -I 4ad ' _[local]_cod_chemical_formula_sum_orig 'Ga5.76 H6.8 K5.76 O35.36 Si10.24 ' _cod_original_cell_volume 931.30(10) _cod_database_code 2011884 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' 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_type_symbol Ga1 .32466(8) .62521(8) .08729(8) .0117(2) Uani d P .36 Ga Si1 .32466(8) .62521(8) .08729(8) .0117(2) Uani d P .64 Si O1 .3199(6) .7937(5) .0689(5) .0363(10) Uani d . 1 O O2 .3218(5) .5660(4) -.0810(5) .0327(10) Uani d . 1 O K1 .1712(12) .7056(7) -.2649(6) .099(3) Uani d P .36 K OW1 .057(3) .731(3) -.215(3) .057(8) Uani d P .21 O 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 Ga1 .0121(4) .0124(4) .0107(3) -.0002(3) .0028(3) -.0017(3) Si1 .0121(4) .0124(4) .0107(3) -.0002(3) .0028(3) -.0017(3) O1 .052(3) .023(2) .034(2) .0019(19) -.006(2) -.0013(18) O2 .049(3) .023(2) .0257(19) .0059(18) .009(2) -.0019(16) K1 .210(11) .054(4) .033(3) .057(5) -.002(4) .017(3) OW1 .09(2) .023(12) .053(15) .000(13) .026(15) -.003(11) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si .0817 .0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K .2009 .2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga .2307 1.6083 '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 Ga1 O2 12_766 3 108.0(2) yes O1 Ga1 O2 12_766 . 113.0(3) yes O2 Ga1 O2 3 . 107.5(3) yes O1 Ga1 O1 12_766 . 113.8(4) yes O2 Ga1 O1 3 . 109.7(3) yes O2 Ga1 O1 . . 104.6(2) yes O1 Ga1 K1 12_766 13_564 127.6(3) ? O2 Ga1 K1 3 13_564 124.1(3) ? O2 Ga1 K1 . 13_564 49.66(19) ? O1 Ga1 K1 . 13_564 55.0(2) ? O1 Ga1 K1 12_766 2_565 58.9(3) ? O2 Ga1 K1 3 2_565 62.7(2) ? O2 Ga1 K1 . 2_565 92.32(18) ? O1 Ga1 K1 . 2_565 163.05(19) ? K1 Ga1 K1 13_564 2_565 141.93(13) ? O1 Ga1 K1 12_766 3 124.4(3) ? O2 Ga1 K1 3 3 45.1(2) ? O2 Ga1 K1 . 3 62.4(2) ? O1 Ga1 K1 . 3 121.0(3) ? K1 Ga1 K1 13_564 3 93.0(3) ? K1 Ga1 K1 2_565 3 65.79(2) ? O1 Ga1 K1 12_766 . 149.2(2) ? O2 Ga1 K1 3 . 97.5(2) ? O2 Ga1 K1 . . 40.35(19) ? O1 Ga1 K1 . . 71.6(2) ? K1 Ga1 K1 13_564 . 29.1(4) ? K1 Ga1 K1 2_565 . 123.11(12) ? K1 Ga1 K1 3 . 64.22(11) ? O1 Ga1 K1 12_766 11_565 145.0(2) ? O2 Ga1 K1 3 11_565 39.71(19) ? O2 Ga1 K1 . 11_565 76.8(2) ? O1 Ga1 K1 . 11_565 94.4(3) ? K1 Ga1 K1 13_564 11_565 85.08(14) ? K1 Ga1 K1 2_565 11_565 88.2(4) ? K1 Ga1 K1 3 11_565 28.6(4) ? K1 Ga1 K1 . 11_565 57.8(3) ? O1 Ga1 K1 12_766 4_455 38.0(2) ? O2 Ga1 K1 3 4_455 79.02(18) ? O2 Ga1 K1 . 4_455 147.5(2) ? O1 Ga1 K1 . 4_455 102.8(2) ? K1 Ga1 K1 13_564 4_455 150.6(3) ? K1 Ga1 K1 2_565 4_455 61.69(11) ? K1 Ga1 K1 3 4_455 116.13(11) ? K1 Ga1 K1 . 4_455 172.1(2) ? K1 Ga1 K1 11_565 4_455 118.32(13) ? Si1 O1 Ga1 15_565 . 135.8(3) yes Si1 O1 K1 15_565 13_564 120.9(3) ? Ga1 O1 K1 . 13_564 96.0(2) ? Si1 O1 K1 15_565 16_665 93.3(3) ? Ga1 O1 K1 . 16_665 117.0(3) ? K1 O1 K1 13_564 16_665 82.1(2) ? Si1 O2 Ga1 4_454 . 135.4(3) yes Si1 O2 K1 4_454 . 108.5(3) ? Ga1 O2 K1 . . 115.6(3) ? Si1 O2 K1 4_454 13_564 116.8(3) ? Ga1 O2 K1 . 13_564 101.9(2) ? K1 O2 K1 . 13_564 39.7(5) ? Si1 O2 K1 4_454 3 89.2(3) ? Ga1 O2 K1 . 3 89.5(2) ? K1 O2 K1 . 3 82.78(17) ? K1 O2 K1 13_564 3 120.7(5) ? OW1 K1 K1 . 13_564 128.5(16) ? OW1 K1 OW1 . 6_464 11.3(10) ? K1 K1 OW1 13_564 6_464 131.2(8) ? OW1 K1 O2 . . 112.0(14) ? K1 K1 O2 13_564 . 70.8(4) ? OW1 K1 O2 6_464 . 123.0(7) ? OW1 K1 O2 . 13_564 92.9(13) ? K1 K1 O2 13_564 13_564 69.5(4) ? OW1 K1 O2 6_464 13_564 84.5(7) ? O2 K1 O2 . 13_564 140.3(5) ? OW1 K1 OW1 . 13_564 148.9(12) ? K1 K1 OW1 13_564 13_564 20.4(6) ? OW1 K1 OW1 6_464 13_564 150.6(11) ? O2 K1 OW1 . 13_564 67.4(6) ? O2 K1 OW1 13_564 13_564 75.3(6) ? OW1 K1 OW1 . 16_665 32.8(19) ? K1 K1 OW1 13_564 16_665 99.4(8) ? OW1 K1 OW1 6_464 16_665 42.0(10) ? O2 K1 OW1 . 16_665 89.8(7) ? O2 K1 OW1 13_564 16_665 96.6(8) ? OW1 K1 OW1 13_564 16_665 118.8(10) ? OW1 K1 O1 . 13_564 113.5(16) ? K1 K1 O1 13_564 13_564 97.2(5) ? OW1 K1 O1 6_464 13_564 102.5(7) ? O2 K1 O1 . 13_564 128.9(3) ? O2 K1 O1 13_564 13_564 57.43(17) ? OW1 K1 O1 13_564 13_564 84.6(7) ? OW1 K1 O1 16_665 13_564 141.2(7) ? OW1 K1 OW1 . 11_565 30.2(17) ? K1 K1 OW1 13_564 11_565 118.4(7) ? OW1 K1 OW1 6_464 11_565 41.4(9) ? O2 K1 OW1 . 11_565 81.8(6) ? O2 K1 OW1 13_564 11_565 117.6(7) ? OW1 K1 OW1 13_564 11_565 134.3(11) ? OW1 K1 OW1 16_665 11_565 25.1(14) ? O1 K1 OW1 13_564 11_565 140.5(7) ? OW1 K1 O1 . 11_565 82.5(15) ? K1 K1 O1 13_564 11_565 144.7(6) ? OW1 K1 O1 6_464 11_565 82.7(7) ? O2 K1 O1 . 11_565 82.7(2) ? O2 K1 O1 13_564 11_565 132.7(3) ? OW1 K1 O1 13_564 11_565 126.7(6) ? OW1 K1 O1 16_665 11_565 103.4(7) ? O1 K1 O1 13_564 11_565 81.4(2) ? OW1 K1 O1 11_565 11_565 78.8(7) ? OW1 K1 O2 . 4_454 131.4(14) ? K1 K1 O2 13_564 4_454 93.5(5) ? OW1 K1 O2 6_464 4_454 133.9(7) ? O2 K1 O2 . 4_454 54.51(13) ? O2 K1 O2 13_564 4_454 128.1(3) ? OW1 K1 O2 13_564 4_454 75.3(6) ? OW1 K1 O2 16_665 4_454 135.0(8) ? O1 K1 O2 13_564 4_454 78.1(2) ? OW1 K1 O2 11_565 4_454 113.6(7) ? O1 K1 O2 11_565 4_454 51.52(16) ? OW1 K1 Ga1 . 13_564 103.6(14) ? K1 K1 Ga1 13_564 13_564 83.6(4) ? OW1 K1 Ga1 6_464 13_564 92.8(7) ? O2 K1 Ga1 . 13_564 144.0(4) ? O2 K1 Ga1 13_564 13_564 28.46(11) ? OW1 K1 Ga1 13_564 13_564 79.7(7) ? OW1 K1 Ga1 16_665 13_564 119.7(8) ? O1 K1 Ga1 13_564 13_564 29.01(11) ? OW1 K1 Ga1 11_565 13_564 133.6(6) ? O1 K1 Ga1 11_565 13_564 107.3(2) ? O2 K1 Ga1 4_454 13_564 104.3(2) ? K1 OW1 OW1 . 6_464 157.6(16) ? K1 OW1 K1 . 6_464 147(2) ? OW1 OW1 K1 6_464 6_464 11.1(8) ? K1 OW1 K1 . 13_564 31.1(12) ? OW1 OW1 K1 6_464 13_564 149(3) ? K1 OW1 K1 6_464 13_564 148.0(12) ? K1 OW1 K1 . 11_565 120.3(17) ? OW1 OW1 K1 6_464 11_565 79.5(19) ? K1 OW1 K1 6_464 11_565 86.4(9) ? K1 OW1 K1 13_564 11_565 121.7(12) ? K1 OW1 K1 . 16_665 117(2) ? OW1 OW1 K1 6_464 16_665 75.4(15) ? K1 OW1 K1 6_464 16_665 85.4(8) ? K1 OW1 K1 13_564 16_665 87.0(10) ? K1 OW1 K1 11_565 16_665 75.9(7) ? 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 Ga1 O1 12_766 1.673(5) yes Ga1 O2 3 1.684(4) yes Ga1 O2 . 1.686(5) yes Ga1 O1 . 1.688(5) yes Ga1 K1 13_564 3.462(5) ? Ga1 K1 2_565 3.576(7) ? Ga1 K1 3 3.584(7) ? Ga1 K1 . 3.728(6) ? Ga1 K1 11_565 3.768(6) ? Ga1 K1 4_455 3.979(7) ? K1 O2 . 2.676(8) yes K1 OW1 . 1.23(3) ? K1 K1 13_564 1.82(2) ? K1 OW1 6_464 2.43(4) ? K1 O2 13_564 2.697(7) yes K1 OW1 13_564 2.76(4) yes K1 OW1 16_665 2.84(3) yes K1 O1 13_564 2.852(8) yes K1 OW1 11_565 2.89(3) yes K1 O1 11_565 3.066(11) yes K1 O2 4_454 3.178(8) yes K1 Ga1 13_564 3.462(5) ? OW1 OW1 6_464 1.25(7) ?