#------------------------------------------------------------------------------ #$Date: 2019-03-21 05:33:39 +0200 (Thu, 21 Mar 2019) $ #$Revision: 214248 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/10/83/2108391.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_2108391 loop_ _publ_author_name 'Marabello, Domenica' 'Antoniotti, Paola' 'Benzi, Paola' 'Cariati, Elena' 'Lo Presti, Leonardo' 'Canepa, Carlo' _publ_section_title ; Developing new SrI~2~ and \b-D-fructopyranose-based metal--organic frameworks with nonlinear optical properties ; _journal_coeditor_code UM5025SUP1 _journal_issue 2 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first ; ; _journal_paper_doi 10.1107/S2052520619001951 _journal_volume 75 _journal_year 2019 _chemical_formula_moiety 'C6 H18 I O9 Sr, I' _chemical_formula_sum 'C6 H18 I2 O9 Sr' _chemical_formula_weight 575.62 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _audit_creation_date 2018-06-19 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.1192(3) _cell_length_b 13.0908(5) _cell_length_c 13.5504(8) _cell_measurement_reflns_used 3777 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 24.1320 _cell_measurement_theta_min 3.4480 _cell_volume 1617.61(13) _computing_cell_refinement 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXS (Sheldrick, 2008)' _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.2890 _diffrn_detector_type Ruby _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w 1.00 51.00 1.00 5.00 -- 18.55 77.00 150.00 50 2 \w 9.00 88.00 1.00 5.00 -- 18.55 57.00 90.00 79 3 \w -43.00 12.00 1.00 5.00 -- -18.78 19.00 0.00 55 4 \w -49.00 57.00 1.00 5.00 -- -18.78 77.00 -30.00 106 5 \w -76.00 9.00 1.00 5.00 -- -18.78 -57.00-180.00 85 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0027123000 _diffrn_orient_matrix_UB_12 -0.0082928000 _diffrn_orient_matrix_UB_13 -0.0516756000 _diffrn_orient_matrix_UB_21 0.0029291000 _diffrn_orient_matrix_UB_22 0.0535189000 _diffrn_orient_matrix_UB_23 -0.0079630000 _diffrn_orient_matrix_UB_31 0.0777007000 _diffrn_orient_matrix_UB_32 -0.0017322000 _diffrn_orient_matrix_UB_33 0.0021036000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0647 _diffrn_reflns_av_unetI/netI 0.0562 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 12121 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 24.706 _diffrn_reflns_theta_max 24.706 _diffrn_reflns_theta_min 3.386 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 7.179 _exptl_absorpt_correction_T_max 0.788 _exptl_absorpt_correction_T_min 0.310 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.364 _exptl_crystal_description prismatic _exptl_crystal_F_000 1080 _exptl_crystal_size_max 0.274 _exptl_crystal_size_mid 0.108 _exptl_crystal_size_min 0.035 _refine_diff_density_max 1.224 _refine_diff_density_min -1.197 _refine_diff_density_rms 0.127 _refine_ls_abs_structure_details ; Flack x determined using 852 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.028(10) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 170 _refine_ls_number_reflns 2757 _refine_ls_number_restraints 17 _refine_ls_restrained_S_all 4.253 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0389 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0316P)^2^+1.0965P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0740 _refine_ls_wR_factor_ref 0.0800 _reflns_Friedel_coverage 0.731 _reflns_Friedel_fraction_full 0.999 _reflns_Friedel_fraction_max 0.999 _reflns_number_gt 2358 _reflns_number_total 2757 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file um5025sup1.cif _cod_data_source_block 3 _cod_original_cell_volume 1617.63(13) _cod_database_code 2108391 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_hkl_checksum 21631 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.26889(9) 0.33345(7) 0.43707(7) 0.0492(3) Uani 1 1 d . . . . Sr03 Sr 0.30922(10) 0.32713(8) 0.71049(9) 0.0311(3) Uani 1 1 d D . . . O1 O 0.1832(7) 0.0059(5) 0.8503(6) 0.0271(18) Uani 1 1 d . . . . O2 O 0.4438(8) -0.1235(5) 0.8673(6) 0.034(2) Uani 1 1 d D . . . H2 H 0.4067 -0.1631 0.9075 0.050 Uiso 1 1 d D . . . O3 O 0.6306(7) 0.0213(5) 0.8203(7) 0.034(2) Uani 1 1 d D . . . H3 H 0.6815 0.0723 0.8124 0.051 Uiso 1 1 d D . . . O4 O 0.4420(8) 0.1532(5) 0.7044(7) 0.035(2) Uani 1 1 d D . . . H4 H 0.5140 0.1365 0.6719 0.053 Uiso 1 1 calc DGR . . . O5 O 0.2242(7) 0.1813(5) 0.8339(6) 0.0286(18) Uani 1 1 d D . . . H5 H 0.1670 0.1779 0.8805 0.043 Uiso 1 1 calc DGR . . . O6 O 0.1459(9) 0.1702(6) 0.6422(7) 0.048(2) Uani 1 1 d D . . . H6 H 0.0881 0.1687 0.5958 0.072 Uiso 1 1 calc DGR . . . O1W O 0.5009(10) 0.3419(7) 0.8541(8) 0.059(3) Uani 1 1 d . . . . H1WA H 0.4834 0.3656 0.9113 0.089 Uiso 1 1 d GR . . . H1WB H 0.5902 0.3236 0.8505 0.089 Uiso 1 1 d GR . . . O2W O 0.1892(12) 0.4066(7) 0.8645(9) 0.079(4) Uani 1 1 d D . . . H2WA H 0.1430 0.3739 0.9089 0.118 Uiso 1 1 d DGR . . . H2WB H 0.1894 0.4695 0.8801 0.118 Uiso 1 1 d DGR . . . C1 C 0.2650(12) -0.0053(9) 0.9403(9) 0.034(3) Uani 1 1 d . . . . H1A H 0.2232 -0.0604 0.9791 0.041 Uiso 1 1 calc R . . . H1B H 0.2578 0.0571 0.9786 0.041 Uiso 1 1 calc R . . . C2 C 0.4253(10) -0.0283(7) 0.9195(10) 0.027(3) Uani 1 1 d D . . . H2A H 0.4805 -0.0300 0.9815 0.033 Uiso 1 1 calc R . . . C3 C 0.4886(10) 0.0532(8) 0.8515(9) 0.026(3) Uani 1 1 d D . . . H3A H 0.4963 0.1180 0.8873 0.032 Uiso 1 1 calc R . . . C4 C 0.3927(11) 0.0671(7) 0.7624(9) 0.025(3) Uani 1 1 d D . . . H4A H 0.4000 0.0055 0.7217 0.030 Uiso 1 1 calc R . . . C5 C 0.2327(10) 0.0847(7) 0.7868(9) 0.024(3) Uani 1 1 d D . . . C6 C 0.1272(13) 0.0800(7) 0.7017(9) 0.035(3) Uani 1 1 d D . . . H6A H 0.1461 0.0195 0.6623 0.042 Uiso 1 1 calc R . . . H6B H 0.0273 0.0764 0.7261 0.042 Uiso 1 1 calc R . . . O3W O 0.078(2) 0.4012(15) 0.6331(18) 0.058(7) Uiso 0.55(3) 1 d . P A 1 H3WA H 0.0075 0.3651 0.6054 0.087 Uiso 0.55(3) 1 d GR P A 1 H3WB H 0.0562 0.4667 0.6290 0.087 Uiso 0.55(3) 1 d GR P A 1 O3X O 0.041(2) 0.3700(16) 0.695(2) 0.051(8) Uiso 0.45(3) 1 d . P A 2 H3XA H -0.0046 0.4270 0.7108 0.077 Uiso 0.45(3) 1 d GR P A 2 H3XB H -0.0292 0.3303 0.6726 0.077 Uiso 0.45(3) 1 d GR P A 2 I2 I 0.35571(9) 0.27304(7) 1.09764(8) 0.0495(3) Uani 1 1 d . . . . 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 I1 0.0481(5) 0.0449(5) 0.0547(6) 0.0096(5) -0.0166(4) -0.0183(4) Sr03 0.0242(5) 0.0197(5) 0.0495(8) 0.0052(6) 0.0017(5) -0.0003(4) O1 0.027(4) 0.026(4) 0.029(5) 0.012(3) 0.004(4) -0.004(3) O2 0.035(4) 0.020(4) 0.046(6) 0.006(4) 0.007(4) 0.000(3) O3 0.022(4) 0.024(4) 0.055(6) 0.001(4) 0.000(4) 0.000(3) O4 0.028(4) 0.032(4) 0.046(6) 0.013(4) 0.015(4) 0.010(3) O5 0.033(4) 0.020(3) 0.032(5) -0.002(3) 0.009(4) -0.004(3) O6 0.048(5) 0.047(5) 0.049(6) 0.020(5) -0.020(5) -0.015(5) O1W 0.055(5) 0.058(7) 0.063(8) -0.002(6) -0.008(5) -0.008(5) O2W 0.098(8) 0.041(5) 0.098(10) -0.021(6) 0.050(7) -0.003(6) C1 0.040(7) 0.030(6) 0.033(8) 0.011(6) 0.019(7) 0.004(5) C2 0.022(5) 0.031(6) 0.029(8) 0.001(6) 0.001(5) 0.003(4) C3 0.024(5) 0.017(5) 0.037(9) 0.001(5) -0.003(6) 0.000(4) C4 0.027(6) 0.014(5) 0.034(8) -0.001(5) 0.012(5) 0.002(4) C5 0.019(5) 0.016(5) 0.038(8) -0.002(5) -0.005(6) 0.000(4) C6 0.036(6) 0.026(6) 0.043(9) 0.002(6) -0.005(7) -0.002(5) I2 0.0336(4) 0.0582(5) 0.0568(7) -0.0138(5) -0.0048(4) 0.0015(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.1412 0 -1 1 0.0426 -1 0 0 0.1331 0 1 -1 0.0508 0 -1 -2 0.0246 0 1 2 0.0099 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 O2 Sr03 I1 70.90(19) 3_656 . O2 Sr03 O3 60.6(2) 3_656 3_656 O2 Sr03 O4 78.3(2) 3_656 . O2 Sr03 O5 134.1(2) 3_656 . O2 Sr03 O6 122.3(3) 3_656 . O2 Sr03 O1W 72.6(3) 3_656 . O2 Sr03 O2W 127.1(3) 3_656 . O2 Sr03 C5 122.5(2) 3_656 . O3 Sr03 I1 80.89(19) 3_656 . O3 Sr03 O5 148.8(2) 3_656 . O3 Sr03 O6 142.6(2) 3_656 . O3 Sr03 C5 171.4(3) 3_656 . O4 Sr03 I1 92.0(2) . . O4 Sr03 O3 138.5(2) . 3_656 O4 Sr03 O5 61.5(2) . . O4 Sr03 O6 65.0(3) . . O4 Sr03 O1W 77.0(3) . . O4 Sr03 C5 44.3(2) . . O5 Sr03 I1 127.88(16) . . O5 Sr03 O6 60.5(2) . . O5 Sr03 C5 23.0(2) . . O6 Sr03 I1 67.76(18) . . O6 Sr03 C5 44.2(2) . . O1W Sr03 I1 143.4(2) . . O1W Sr03 O3 84.7(3) . 3_656 O1W Sr03 O5 77.3(3) . . O1W Sr03 O6 132.7(3) . . O1W Sr03 C5 88.8(3) . . O2W Sr03 I1 139.0(3) . . O2W Sr03 O3 80.0(3) . 3_656 O2W Sr03 O4 125.6(3) . . O2W Sr03 O5 69.9(3) . . O2W Sr03 O6 110.5(3) . . O2W Sr03 O1W 69.7(4) . . O2W Sr03 C5 92.5(3) . . C5 Sr03 I1 107.6(2) . . O3W Sr03 I1 60.0(5) . . O3W Sr03 O2 117.4(6) . 3_656 O3W Sr03 O3 74.9(5) . 3_656 O3W Sr03 O4 135.3(5) . . O3W Sr03 O5 107.0(5) . . O3W Sr03 O6 72.1(5) . . O3W Sr03 O1W 146.0(5) . . O3W Sr03 O2W 80.1(6) . . O3W Sr03 C5 108.1(5) . . O3X Sr03 I1 79.5(6) . . O3X Sr03 O2 139.6(7) . 3_656 O3X Sr03 O3 88.5(5) . 3_656 O3X Sr03 O4 130.5(5) . . O3X Sr03 O5 85.9(6) . . O3X Sr03 O6 66.8(5) . . O3X Sr03 O1W 133.8(6) . . O3X Sr03 O2W 64.2(6) . . O3X Sr03 C5 91.9(6) . . C5 O1 C1 115.1(8) . . Sr03 O2 H2 118.2 3_646 . C2 O2 Sr03 121.4(5) . 3_646 C2 O2 H2 99.9 . . Sr03 O3 H3 130.3 3_646 . C3 O3 Sr03 121.3(5) . 3_646 C3 O3 H3 108.4 . . Sr03 O4 H4 128.9 . . C4 O4 Sr03 121.7(5) . . C4 O4 H4 109.5 . . Sr03 O5 H5 135.2 . . C5 O5 Sr03 110.0(6) . . C5 O5 H5 109.5 . . Sr03 O6 H6 129.4 . . C6 O6 Sr03 119.8(6) . . C6 O6 H6 109.5 . . Sr03 O1W H1WA 125.3 . . Sr03 O1W H1WB 125.1 . . H1WA O1W H1WB 109.6 . . Sr03 O2W H2WA 125.5 . . Sr03 O2W H2WB 126.2 . . H2WA O2W H2WB 108.3 . . O1 C1 H1A 109.4 . . O1 C1 H1B 109.4 . . O1 C1 C2 111.3(10) . . H1A C1 H1B 108.0 . . C2 C1 H1A 109.4 . . C2 C1 H1B 109.4 . . O2 C2 C1 112.0(8) . . O2 C2 H2A 109.9 . . O2 C2 C3 105.3(9) . . C1 C2 H2A 109.9 . . C1 C2 C3 109.8(9) . . C3 C2 H2A 109.9 . . O3 C3 C2 108.6(8) . . O3 C3 H3A 109.6 . . O3 C3 C4 109.0(10) . . C2 C3 H3A 109.6 . . C4 C3 C2 110.5(8) . . C4 C3 H3A 109.6 . . O4 C4 C3 110.5(8) . . O4 C4 H4A 108.3 . . O4 C4 C5 107.4(8) . . C3 C4 H4A 108.3 . . C3 C4 C5 113.8(10) . . C5 C4 H4A 108.3 . . O1 C5 Sr03 157.9(7) . . O1 C5 O5 111.0(9) . . O1 C5 C4 109.2(8) . . O1 C5 C6 103.4(8) . . O5 C5 Sr03 47.0(5) . . O5 C5 C4 106.7(8) . . O5 C5 C6 110.3(8) . . C4 C5 Sr03 83.0(5) . . C6 C5 Sr03 86.3(6) . . C6 C5 C4 116.3(10) . . O6 C6 C5 108.7(9) . . O6 C6 H6A 110.0 . . O6 C6 H6B 110.0 . . C5 C6 H6A 110.0 . . C5 C6 H6B 110.0 . . H6A C6 H6B 108.3 . . Sr03 O3W H3WA 125.2 . . Sr03 O3W H3WB 125.8 . . H3WA O3W H3WB 109.0 . . Sr03 O3X H3XA 128.7 . . Sr03 O3X H3XB 127.1 . . H3XA O3X H3XB 104.2 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 I1 Sr03 3.7241(16) . Sr03 O2 2.569(7) 3_656 Sr03 O3 2.634(7) 3_656 Sr03 O4 2.581(7) . Sr03 O5 2.654(7) . Sr03 O6 2.701(8) . Sr03 O1W 2.623(9) . Sr03 O2W 2.576(10) . Sr03 C5 3.410(10) . Sr03 O3W 2.544(18) . Sr03 O3X 2.52(2) . O1 C1 1.437(14) . O1 C5 1.417(12) . O2 Sr03 2.569(7) 3_646 O2 H2 0.8248 . O2 C2 1.443(13) . O3 Sr03 2.634(7) 3_646 O3 H3 0.8199 . O3 C3 1.425(12) . O4 H4 0.8201 . O4 C4 1.446(11) . O5 H5 0.8201 . O5 C5 1.418(11) . O6 H6 0.8201 . O6 C6 1.440(12) . O1W H1WA 0.8501 . O1W H1WB 0.8500 . O2W H2WA 0.8498 . O2W H2WB 0.8501 . C1 H1A 0.9700 . C1 H1B 0.9700 . C1 C2 1.518(14) . C2 H2A 0.9800 . C2 C3 1.522(15) . C3 H3A 0.9800 . C3 C4 1.501(16) . C4 H4A 0.9800 . C4 C5 1.514(13) . C5 C6 1.504(16) . C6 H6A 0.9700 . C6 H6B 0.9700 . O3W H3WA 0.8833 . O3W H3WB 0.8832 . O3X H3XA 0.8790 . O3X H3XB 0.8780 . _cod_database_fobs_code 2108391