#------------------------------------------------------------------------------ #$Date: 2014-06-01 04:28:04 +0300 (Sun, 01 Jun 2014) $ #$Revision: 115013 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/21/62/7216233.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_7216233 loop_ _publ_author_name 'Zou, Jiyong' 'Shi, Wei' 'Zhang, Jing-Ya' 'He, Yan-Fei' 'Gao, Hong-Ling' 'Cui, Jian-Zhong' 'Cheng, Peng' _publ_section_title ; Alkaline cations directed structural diversity of cubic-cage-based cobalt(II) metal-organic frameworks: from pcu to bct net ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/c4ce00597j _journal_year 2014 _chemical_formula_sum 'C48 H12 Co9 Li3 N36 O54' _chemical_formula_weight 2508.13 _chemical_name_systematic ; ? ; _space_group_IT_number 167 _symmetry_cell_setting trigonal _symmetry_space_group_name_Hall '-R 3 2"c' _symmetry_space_group_name_H-M 'R -3 c :H' _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 6 _cell_length_a 17.6972(11) _cell_length_b 17.6972(11) _cell_length_c 76.397(5) _cell_measurement_reflns_used 4228 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 29.1686 _cell_measurement_theta_min 2.4318 _cell_volume 20721(2) _computing_cell_refinement CRYSALISPRO _computing_data_collection CRYSALISPRO _computing_data_reduction CRYSALISPRO _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'SuperNova (Mo) X-ray Source' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0782 _diffrn_reflns_av_sigmaI/netI 0.0723 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 90 _diffrn_reflns_limit_l_min -62 _diffrn_reflns_number 24160 _diffrn_reflns_theta_full 25.01 _diffrn_reflns_theta_max 25.01 _diffrn_reflns_theta_min 2.44 _exptl_absorpt_coefficient_mu 1.133 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.95666 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details CrysAlisPro _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.206 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 7416 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.08 _platon_squeeze_details ; ; _refine_diff_density_max 0.401 _refine_diff_density_min -0.699 _refine_diff_density_rms 0.072 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.903 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 228 _refine_ls_number_reflns 4069 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 0.906 _refine_ls_R_factor_all 0.1139 _refine_ls_R_factor_gt 0.0553 _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^)+(0.0726P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1475 _refine_ls_wR_factor_ref 0.1680 _reflns_number_gt 1990 _reflns_number_total 4069 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file c4ce00597j2.cif _[local]_cod_data_source_block p110616f1 _[local]_cod_cif_authors_sg_H-M R-3c _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' according to /usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. Automatic conversion script Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius ; _cod_database_code 7216233 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'y, x, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'y+2/3, x+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' 'y+1/3, x+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-y, -x, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-y+2/3, -x+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' '-y+1/3, -x+2/3, z+1/6' 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 C1 C 0.8611(5) 0.8353(4) 0.42061(6) 0.0616(15) Uani 1 1 d . C2 C 0.8299(3) 0.8589(3) 0.43692(5) 0.0500(13) Uani 1 1 d . C3 C 0.7563(4) 0.8219(3) 0.44737(5) 0.0512(13) Uani 1 1 d . C4 C 0.6686(4) 0.7404(4) 0.44818(7) 0.0652(16) Uani 1 1 d . C5 C 0.5694(4) 0.7395(5) 0.50545(9) 0.0809(19) Uani 1 1 d . C6 C 0.6511(4) 0.7329(3) 0.50676(7) 0.0622(15) Uani 1 1 d . C7 C 0.6884(3) 0.6963(4) 0.51686(7) 0.0631(15) Uani 1 1 d . C8 C 0.6638(5) 0.6377(4) 0.53263(8) 0.0815(19) Uani 1 1 d . Co1 Co 1.0000 1.0000 0.431197(12) 0.0460(3) Uani 1 3 d S Co2 Co 0.67204(5) 0.83991(5) 0.477172(7) 0.0571(3) Uani 1 1 d U Co3 Co 0.0000 0.0000 0.5000 0.0464(4) Uani 1 6 d S Li1 Li 0.7012(11) 0.6667 0.4167 0.107(6) Uani 1 2 d S N1 N 0.8841(3) 0.9364(3) 0.44389(5) 0.0484(10) Uani 1 1 d . N2 N 0.8494(3) 0.9515(3) 0.45789(5) 0.0544(12) Uani 1 1 d . N3 N 0.7717(3) 0.8823(3) 0.45981(4) 0.0491(10) Uani 1 1 d . N4 N 0.7113(3) 0.7766(3) 0.49366(5) 0.0566(11) Uani 1 1 d U N5 N 0.7791(3) 0.7663(3) 0.49552(6) 0.0667(13) Uani 1 1 d . N6 N 0.7664(3) 0.7191(3) 0.50938(6) 0.0636(13) Uani 1 1 d . O1 O 0.9375(3) 0.8930(2) 0.41612(4) 0.0615(10) Uani 1 1 d . O2 O 0.8144(3) 0.7661(3) 0.41309(5) 0.0952(15) Uani 1 1 d . O3 O 0.6470(3) 0.6822(3) 0.43692(5) 0.0907(14) Uani 1 1 d . O4 O 0.6207(2) 0.7366(2) 0.46083(4) 0.0641(10) Uani 1 1 d . O5 O 0.5662(2) 0.7817(3) 0.49250(5) 0.0793(12) Uani 1 1 d . O6 O 0.5126(3) 0.7038(4) 0.51642(6) 0.129(2) Uani 1 1 d . O7 O 0.5938(3) 0.6133(4) 0.53997(5) 0.128(2) Uani 1 1 d . O8 O 0.7215(3) 0.6186(3) 0.53710(5) 0.0776(12) Uani 1 1 d . O9 O 0.10991(19) 0.0516(2) 0.48445(3) 0.0469(8) Uani 1 1 d . H9A H 0.1566 0.0913 0.4901 0.070 Uiso 1 1 d R H9B H 0.1040 0.0774 0.4751 0.070 Uiso 1 1 d R 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 C1 0.086(5) 0.067(4) 0.040(3) -0.016(3) -0.016(3) 0.044(4) C2 0.058(4) 0.052(3) 0.037(3) -0.009(2) -0.020(3) 0.025(3) C3 0.073(4) 0.059(4) 0.027(2) -0.007(2) -0.011(2) 0.037(3) C4 0.072(4) 0.057(4) 0.066(4) -0.019(3) -0.024(3) 0.032(4) C5 0.057(5) 0.081(5) 0.089(5) -0.010(4) 0.020(4) 0.022(4) C6 0.043(4) 0.051(4) 0.068(3) -0.004(3) 0.018(3) 0.004(3) C7 0.040(4) 0.062(4) 0.064(3) -0.015(3) 0.008(3) 0.008(3) C8 0.068(5) 0.076(5) 0.073(4) 0.005(3) 0.024(4) 0.016(4) Co1 0.0504(5) 0.0504(5) 0.0371(6) 0.000 0.000 0.0252(2) Co2 0.0552(5) 0.0631(6) 0.0566(5) -0.0006(4) 0.0077(3) 0.0322(4) Co3 0.0470(6) 0.0470(6) 0.0453(8) 0.000 0.000 0.0235(3) Li1 0.119(11) 0.085(12) 0.106(11) -0.058(9) -0.029(5) 0.043(6) N1 0.062(3) 0.047(3) 0.045(2) -0.0071(19) -0.0207(19) 0.033(2) N2 0.072(3) 0.047(3) 0.045(2) -0.0143(19) -0.017(2) 0.030(3) N3 0.072(3) 0.061(3) 0.0300(19) -0.004(2) -0.0083(18) 0.045(3) N4 0.045(3) 0.042(3) 0.061(3) -0.009(2) 0.010(2) 0.006(2) N5 0.041(3) 0.057(3) 0.084(3) -0.014(3) 0.011(2) 0.011(3) N6 0.038(3) 0.059(3) 0.073(3) -0.021(3) 0.005(2) 0.008(2) O1 0.076(3) 0.065(2) 0.0376(18) -0.0164(16) 0.0039(18) 0.031(2) O2 0.102(4) 0.080(3) 0.081(3) -0.039(2) -0.006(2) 0.029(3) O3 0.099(3) 0.068(3) 0.077(2) -0.032(2) -0.003(2) 0.020(3) O4 0.053(2) 0.064(3) 0.055(2) -0.0186(17) -0.0023(18) 0.014(2) O5 0.048(2) 0.084(3) 0.093(3) -0.004(3) 0.017(2) 0.023(2) O6 0.081(4) 0.161(5) 0.141(4) 0.030(4) 0.066(3) 0.058(4) O7 0.080(4) 0.161(5) 0.111(3) 0.037(3) 0.053(3) 0.036(3) O8 0.069(3) 0.066(3) 0.078(3) 0.015(2) 0.018(2) 0.019(3) O9 0.0470(19) 0.053(2) 0.0413(16) 0.0091(15) 0.0018(13) 0.0249(18) 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 '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' O O 0.0106 0.0060 '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 O2 C1 O1 126.3(5) . . O2 C1 C2 120.6(6) . . O1 C1 C2 113.1(5) . . N1 C2 C3 106.3(4) . . N1 C2 C1 116.2(5) . . C3 C2 C1 137.5(5) . . N3 C3 C2 105.1(5) . . N3 C3 C4 115.7(5) . . C2 C3 C4 139.1(5) . . O3 C4 O4 124.3(6) . . O3 C4 C3 120.6(6) . . O4 C4 C3 115.1(5) . . O6 C5 O5 125.4(7) . . O6 C5 C6 119.3(7) . . O5 C5 C6 115.3(6) . . C7 C6 N4 104.8(5) . . C7 C6 C5 141.2(5) . . N4 C6 C5 114.0(5) . . N6 C7 C6 106.3(5) . . N6 C7 C8 116.4(6) . . C6 C7 C8 137.3(6) . . O7 C8 O8 126.0(6) . . O7 C8 C7 120.2(7) . . O8 C8 C7 113.8(6) . . O1 Co1 O1 90.40(14) . 3_675 O1 Co1 O1 90.40(14) . 2_765 O1 Co1 O1 90.40(14) 3_675 2_765 O1 Co1 N1 170.21(15) . 3_675 O1 Co1 N1 79.87(15) 3_675 3_675 O1 Co1 N1 90.78(14) 2_765 3_675 O1 Co1 N1 90.78(14) . 2_765 O1 Co1 N1 170.20(16) 3_675 2_765 O1 Co1 N1 79.87(15) 2_765 2_765 N1 Co1 N1 99.00(13) 3_675 2_765 O1 Co1 N1 79.87(15) . . O1 Co1 N1 90.78(14) 3_675 . O1 Co1 N1 170.20(15) 2_765 . N1 Co1 N1 99.00(13) 3_675 . N1 Co1 N1 99.00(13) 2_765 . O5 Co2 O4 90.83(16) . . O5 Co2 O8 91.23(18) . 20_566 O4 Co2 O8 90.50(17) . 20_566 O5 Co2 N6 91.63(16) . 20_566 O4 Co2 N6 171.21(17) . 20_566 O8 Co2 N6 81.01(19) 20_566 20_566 O5 Co2 N4 80.96(18) . . O4 Co2 N4 90.41(15) . . O8 Co2 N4 172.16(16) 20_566 . N6 Co2 N4 98.31(17) 20_566 . O5 Co2 N3 171.79(17) . . O4 Co2 N3 81.05(15) . . O8 Co2 N3 90.02(15) 20_566 . N6 Co2 N3 96.58(17) 20_566 . N4 Co2 N3 97.82(16) . . O9 Co3 O9 89.88(11) . 21_556 O9 Co3 O9 90.12(11) . 3 O9 Co3 O9 180.00(17) 21_556 3 O9 Co3 O9 90.12(11) . 2 O9 Co3 O9 89.88(11) 21_556 2 O9 Co3 O9 90.12(11) 3 2 O9 Co3 O9 89.88(11) . 20_556 O9 Co3 O9 90.12(11) 21_556 20_556 O9 Co3 O9 89.88(11) 3 20_556 O9 Co3 O9 180.00(12) 2 20_556 O9 Co3 O9 179.996(1) . 19_556 O9 Co3 O9 90.12(11) 21_556 19_556 O9 Co3 O9 89.88(11) 3 19_556 O9 Co3 O9 89.88(11) 2 19_556 O9 Co3 O9 90.12(11) 20_556 19_556 O3 Li1 O3 110.0(10) . 10_565 O3 Li1 O2 110.69(17) . . O3 Li1 O2 108.69(18) 10_565 . O3 Li1 O2 108.69(18) . 10_565 O3 Li1 O2 110.70(17) 10_565 10_565 O2 Li1 O2 108.1(10) . 10_565 N2 N1 C2 111.3(4) . . N2 N1 Co1 135.8(3) . . C2 N1 Co1 112.9(3) . . N3 N2 N1 106.0(4) . . N2 N3 C3 111.3(4) . . N2 N3 Co2 136.8(3) . . C3 N3 Co2 111.9(4) . . N5 N4 C6 110.3(5) . . N5 N4 Co2 137.4(4) . . C6 N4 Co2 112.3(4) . . N6 N5 N4 107.5(4) . . N5 N6 C7 111.1(5) . . N5 N6 Co2 137.0(4) . 21_656 C7 N6 Co2 111.9(4) . 21_656 C1 O1 Co1 117.8(3) . . C1 O2 Li1 136.5(5) . . C4 O3 Li1 135.2(5) . . C4 O4 Co2 116.1(3) . . C5 O5 Co2 117.2(4) . . C8 O8 Co2 116.8(4) . 21_656 Co3 O9 H9A 111.8 . . Co3 O9 H9B 111.5 . . H9A O9 H9B 106.9 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 C1 O2 1.225(6) . C1 O1 1.269(7) . C1 C2 1.503(7) . C2 N1 1.331(6) . C2 C3 1.382(7) . C3 N3 1.352(5) . C3 C4 1.501(7) . C4 O3 1.246(6) . C4 O4 1.266(6) . C5 O6 1.215(7) . C5 O5 1.258(7) . C5 C6 1.512(8) . C6 C7 1.369(7) . C6 N4 1.382(6) . C7 N6 1.355(6) . C7 C8 1.505(8) . C8 O7 1.225(7) . C8 O8 1.273(8) . Co1 O1 2.010(3) . Co1 O1 2.010(3) 3_675 Co1 O1 2.010(3) 2_765 Co1 N1 2.026(4) 3_675 Co1 N1 2.026(4) 2_765 Co1 N1 2.026(4) . Co2 O5 2.002(4) . Co2 O4 2.016(3) . Co2 O8 2.016(4) 20_566 Co2 N6 2.019(5) 20_566 Co2 N4 2.025(5) . Co2 N3 2.028(4) . Co3 O9 2.062(3) . Co3 O9 2.062(3) 21_556 Co3 O9 2.062(3) 3 Co3 O9 2.062(3) 2 Co3 O9 2.062(3) 20_556 Co3 O9 2.062(3) 19_556 Li1 O3 1.911(11) . Li1 O3 1.911(11) 10_565 Li1 O2 1.913(12) . Li1 O2 1.913(11) 10_565 N1 N2 1.325(5) . N2 N3 1.315(5) . N4 N5 1.309(6) . N5 N6 1.297(6) . N6 Co2 2.019(5) 21_656 O8 Co2 2.016(4) 21_656 O9 H9A 0.8831 . O9 H9B 0.8850 . loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.007 0.491 0.002 10737 3256 ' '