#------------------------------------------------------------------------------ #$Date: 2018-12-05 19:51:34 +0200 (Wed, 05 Dec 2018) $ #$Revision: 212380 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/03/1550334.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_1550334 loop_ _publ_author_name 'Rui-Biao Lin' 'Libo Li' 'Hao-Long Zhou' 'Hui Wu' 'Chaohui He' 'Shun Li' 'Rajamani Krishna' 'Jinping Li' 'Wei Zhou' 'Banglin Chen' _publ_section_title ; Molecular sieving of ethylene from ethane using a rigid metal-organic framework ; _journal_name_full 'Nature Materials' _journal_page_first 1128 _journal_page_last 1133 _journal_paper_doi https://doi.org/10.1038/s41563-018-0206-2 _journal_volume 17 _journal_year 2018 _chemical_formula_moiety '[Ca(C4O4)(H2O)]' _chemical_formula_sum 'C4 H2 Ca O5' _chemical_formula_weight 170.14 _space_group_IT_number 122 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall 'I -4 2bw' _symmetry_space_group_name_H-M 'I -4 2 d' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 13.6557(2) _cell_length_b 13.6557(2) _cell_length_c 7.7174(3) _cell_measurement_reflns_used 1007 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 74.1060 _cell_measurement_theta_min 6.5580 _cell_volume 1439.13(6) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.981 _diffrn_measured_fraction_theta_max 0.981 _diffrn_measurement_device_type Atlas _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 1248 _diffrn_reflns_theta_full 74.23 _diffrn_reflns_theta_max 74.23 _diffrn_reflns_theta_min 6.59 _exptl_absorpt_coefficient_mu 7.327 _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 1.570 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Columnar _exptl_crystal_F_000 688 _refine_diff_density_max 1.045 _refine_diff_density_min -1.397 _refine_diff_density_rms 0.179 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 40 _refine_ls_number_reflns 670 _refine_ls_number_restraints 12 _refine_ls_restrained_S_all 1.113 _refine_ls_R_factor_all 0.0674 _refine_ls_R_factor_gt 0.0649 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0811P)^2^+24.1677P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1696 _refine_ls_wR_factor_ref 0.1702 _reflns_number_gt 663 _reflns_number_total 670 _reflns_threshold_expression >2sigma(I) _cod_data_source_file File-3.cif _cod_data_source_block UTSA-280_activated _cod_database_code 1550334 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y, -z+3/4' 'x+1/2, -y, -z+3/4' '-y+1/2, -x, z+3/4' 'y+1/2, x, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' '-x+1, y+1/2, -z+5/4' 'x+1, -y+1/2, -z+5/4' '-y+1, -x+1/2, z+5/4' 'y+1, x+1/2, z+5/4' 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 _atom_site_disorder_assembly _atom_site_disorder_group Ca1 Ca 0.30602(10) 0.2500 0.1250 0.0037(4) Uiso 1 2 d S . . O1 O 0.2755(3) 0.0852(3) 0.0804(6) 0.0163(11) Uani 1 1 d U A . O2 O 0.2686(4) -0.1558(3) 0.0720(6) 0.0150(11) Uani 1 1 d . . . C1 C 0.2612(5) 0.0212(4) -0.0323(8) 0.0125(13) Uiso 1 1 d . . . C2 C 0.2599(5) -0.0859(4) -0.0326(8) 0.0094(12) Uani 1 1 d U . . O3A O 0.4778(8) 0.2500 0.1250 0.001(3) Uiso 0.50 2 d SP A 1 H3AA H 0.4978 0.2415 0.2240 0.002 Uiso 0.50 1 calc PR A 1 O3B O 0.4733(13) 0.2825(14) 0.132(3) 0.006(3) Uiso 0.25 1 d P . 2 H3BA H 0.4967 0.3088 0.0461 0.009 Uiso 0.50 1 calc PR . 2 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 O1 0.0198(14) 0.0145(13) 0.0145(14) -0.0009(9) -0.0003(9) -0.0010(9) O2 0.028(3) 0.0073(18) 0.010(2) 0.0021(17) 0.002(2) 0.0002(16) C2 0.0105(15) 0.0094(14) 0.0083(15) -0.0004(10) 0.0003(9) 0.0001(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.3641 1.2855 '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 Ca1 O1 159.3(2) . 14_454 O1 Ca1 O3B 111.4(5) . . O1 Ca1 O3B 89.3(5) 14_454 . O1 Ca1 O3B 89.3(5) . 14_454 O1 Ca1 O3B 111.4(5) 14_454 14_454 O3B Ca1 O3B 22.2(10) . 14_454 O1 Ca1 O3A 100.36(11) . . O1 Ca1 O3A 100.36(11) 14_454 . O3B Ca1 O3A 11.1(5) . . O3B Ca1 O3A 11.1(5) 14_454 . O1 Ca1 O2 89.84(16) . 8_554 O1 Ca1 O2 94.62(16) 14_454 8_554 O3B Ca1 O2 77.9(5) . 8_554 O3B Ca1 O2 77.6(5) 14_454 8_554 O3A Ca1 O2 77.52(11) . 8_554 O1 Ca1 O2 94.62(16) . 11 O1 Ca1 O2 89.84(16) 14_454 11 O3B Ca1 O2 77.6(5) . 11 O3B Ca1 O2 77.9(5) 14_454 11 O3A Ca1 O2 77.52(11) . 11 O2 Ca1 O2 155.0(2) 8_554 11 O1 Ca1 O2 82.21(16) . 4 O1 Ca1 O2 81.25(16) 14_454 4 O3B Ca1 O2 141.2(5) . 4 O3B Ca1 O2 142.1(5) 14_454 4 O3A Ca1 O2 143.07(10) . 4 O2 Ca1 O2 65.61(16) 8_554 4 O2 Ca1 O2 139.33(13) 11 4 O1 Ca1 O2 81.25(16) . 15_454 O1 Ca1 O2 82.21(16) 14_454 15_454 O3B Ca1 O2 142.1(5) . 15_454 O3B Ca1 O2 141.2(5) 14_454 15_454 O3A Ca1 O2 143.07(10) . 15_454 O2 Ca1 O2 139.33(13) 8_554 15_454 O2 Ca1 O2 65.61(16) 11 15_454 O2 Ca1 O2 73.9(2) 4 15_454 O1 Ca1 C2 80.41(16) . 4 O1 Ca1 C2 79.45(17) 14_454 4 O3B Ca1 C2 162.0(5) . 4 O3B Ca1 C2 163.1(5) 14_454 4 O3A Ca1 C2 166.42(11) . 4 O2 Ca1 C2 88.95(15) 8_554 4 O2 Ca1 C2 116.02(16) 11 4 O2 Ca1 C2 23.36(15) 4 4 O2 Ca1 C2 50.51(15) 15_454 4 O1 Ca1 C2 79.45(17) . 15_454 O1 Ca1 C2 80.41(16) 14_454 15_454 O3B Ca1 C2 163.1(5) . 15_454 O3B Ca1 C2 162.0(5) 14_454 15_454 O3A Ca1 C2 166.42(11) . 15_454 O2 Ca1 C2 116.02(16) 8_554 15_454 O2 Ca1 C2 88.95(15) 11 15_454 O2 Ca1 C2 50.51(15) 4 15_454 O2 Ca1 C2 23.36(15) 15_454 15_454 C2 Ca1 C2 27.2(2) 4 15_454 O1 Ca1 Ca1 78.20(11) . 10_554 O1 Ca1 Ca1 94.12(11) 14_454 10_554 O3B Ca1 Ca1 112.6(5) . 10_554 O3B Ca1 Ca1 109.8(5) 14_454 10_554 O3A Ca1 Ca1 111.63(3) . 10_554 O2 Ca1 Ca1 34.65(10) 8_554 10_554 O2 Ca1 Ca1 169.10(12) 11 10_554 O2 Ca1 Ca1 32.27(10) 4 10_554 O2 Ca1 Ca1 104.85(11) 15_454 10_554 C2 Ca1 Ca1 55.06(11) 4 10_554 C2 Ca1 Ca1 81.73(12) 15_454 10_554 C1 O1 Ca1 144.3(4) . . C2 O2 Ca1 141.1(4) . 12_545 C2 O2 Ca1 102.6(4) . 3 Ca1 O2 Ca1 113.08(16) 12_545 3 O1 C1 C2 134.7(6) . . O1 C1 C1 135.6(3) . 5_554 C2 C1 C1 89.8(4) . 5_554 O2 C2 C2 130.5(3) . 5_554 O2 C2 C1 139.3(6) . . C2 C2 C1 90.2(4) 5_554 . O2 C2 Ca1 54.1(3) . 3 C2 C2 Ca1 76.42(11) 5_554 3 C1 C2 Ca1 166.6(4) . 3 Ca1 O3A H3AA 109.5 . . O3B O3B Ca1 78.9(5) 14_454 . O3B O3B H3BA 109.5 14_454 . Ca1 O3B H3BA 116.6 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ca1 O1 2.314(4) . Ca1 O1 2.314(4) 14_454 Ca1 O3B 2.327(18) . Ca1 O3B 2.327(18) 14_454 Ca1 O3A 2.345(12) . Ca1 O2 2.409(5) 8_554 Ca1 O2 2.409(5) 11 Ca1 O2 2.566(5) 4 Ca1 O2 2.566(5) 15_454 Ca1 C2 3.093(6) 4 Ca1 C2 3.093(6) 15_454 Ca1 Ca1 4.1510(10) 10_554 O1 C1 1.249(8) . O2 C2 1.256(7) . O2 Ca1 2.409(5) 12_545 O2 Ca1 2.566(5) 3 C1 C2 1.463(8) . C1 C1 1.463(13) 5_554 C2 C2 1.452(12) 5_554 C2 Ca1 3.093(6) 3 O3A H3AA 0.8200 . O3B O3B 0.89(4) 14_454 O3B H3BA 0.8200 . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 O1 Ca1 O1 C1 88.9(7) 14_454 . . . O3B Ca1 O1 C1 -90.7(9) . . . . O3B Ca1 O1 C1 -91.4(8) 14_454 . . . O3A Ca1 O1 C1 -91.1(7) . . . . O2 Ca1 O1 C1 -13.8(7) 8_554 . . . O2 Ca1 O1 C1 -169.2(7) 11 . . . O2 Ca1 O1 C1 51.6(7) 4 . . . O2 Ca1 O1 C1 126.4(7) 15_454 . . . C2 Ca1 O1 C1 75.2(7) 4 . . . C2 Ca1 O1 C1 102.7(7) 15_454 . . . Ca1 Ca1 O1 C1 19.1(7) 10_554 . . . Ca1 O1 C1 C2 166.7(6) . . . . Ca1 O1 C1 C1 -13.3(16) . . . 5_554 Ca1 O2 C2 C2 -153.9(7) 12_545 . . 5_554 Ca1 O2 C2 C2 2.4(11) 3 . . 5_554 Ca1 O2 C2 C1 24.1(14) 12_545 . . . Ca1 O2 C2 C1 -179.6(8) 3 . . . Ca1 O2 C2 Ca1 -156.3(8) 12_545 . . 3 O1 C1 C2 O2 2.9(16) . . . . C1 C1 C2 O2 -177.1(8) 5_554 . . . O1 C1 C2 C2 -178.7(8) . . . 5_554 C1 C1 C2 C2 1.3(8) 5_554 . . 5_554 O1 C1 C2 Ca1 -175.9(15) . . . 3 C1 C1 C2 Ca1 4(2) 5_554 . . 3 O1 Ca1 O3B O3B -2(3) . . . 14_454 O1 Ca1 O3B O3B 178(2) 14_454 . . 14_454 O3A Ca1 O3B O3B 0.000(1) . . . 14_454 O2 Ca1 O3B O3B -87(2) 8_554 . . 14_454 O2 Ca1 O3B O3B 88(2) 11 . . 14_454 O2 Ca1 O3B O3B -107(2) 4 . . 14_454 O2 Ca1 O3B O3B 102(2) 15_454 . . 14_454 C2 Ca1 O3B O3B -130.7(19) 4 . . 14_454 C2 Ca1 O3B O3B 126(2) 15_454 . . 14_454 Ca1 Ca1 O3B O3B -87(2) 10_554 . . 14_454