#------------------------------------------------------------------------------ #$Date: 2016-03-20 23:21:50 +0000 (Sun, 20 Mar 2016) $ #$Revision: 178377 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/17/4001756.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_4001756 loop_ _publ_author_name 'Jeong, Seok' 'Kim, Dongwook' 'Song, Xiaokai' 'Choi, Min' 'Park, Noejung' 'Lah, Myoung Soo' _publ_section_title ; Postsynthetic Exchanges of the Pillaring Ligand in Three-Dimensional Metal--Organic Frameworks ; _journal_issue 7 _journal_name_full 'Chemistry of Materials' _journal_page_first 1047 _journal_paper_doi 10.1021/cm303624p _journal_volume 25 _journal_year 2013 _chemical_formula_sum 'C15 H16 N2 Ni O6' _chemical_formula_weight 379.01 _chemical_name_systematic ; ? ; _space_group_IT_number 189 _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall 'P -6 -2' _symmetry_space_group_name_H-M 'P -6 2 m' _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 3 _cell_length_a 16.666(2) _cell_length_b 16.666(2) _cell_length_c 7.0012(14) _cell_measurement_reflns_used 1418 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 52.78 _cell_measurement_theta_min 7.47 _cell_volume 1684.1(4) _computing_cell_refinement 'Rigaku Rapid Auto' _computing_data_collection 'Rigaku Rapid Auto' _computing_data_reduction 'Rigaku Rapid Auto' _computing_molecular_graphics 'Diamond 3.2h,ORTEP3' _computing_publication_material WinGX _computing_structure_refinement 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'imaging plate' _diffrn_measurement_method 'omega scans' _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 0.1531 _diffrn_reflns_av_sigmaI/netI 0.0510 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 16600 _diffrn_reflns_theta_full 27.48 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_min 3.23 _exptl_absorpt_coefficient_mu 0.888 _exptl_absorpt_correction_T_max 0.9569 _exptl_absorpt_correction_T_min 0.8285 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Rigaku Rapid Auto' _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.121 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 588 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.05 _platon_squeeze_details ; ; _refine_diff_density_max 1.914 _refine_diff_density_min -0.750 _refine_diff_density_rms 0.144 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.50(5) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 75 _refine_ls_number_reflns 1476 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.081 _refine_ls_R_factor_all 0.0975 _refine_ls_R_factor_gt 0.0866 _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^)+(0.1666P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2182 _refine_ls_wR_factor_ref 0.2362 _reflns_number_gt 1261 _reflns_number_total 1476 _reflns_threshold_expression >2sigma(I) _cod_data_source_file cm303624p_si_002.cif _cod_data_source_block l12_025 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. '_exptl_absorpt_correction_type' value 'Multi-scan' changed to 'multi-scan' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. Automatic conversion script Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius ; _cod_original_cell_volume 1684.1(5) _cod_original_sg_symbol_H-M P-62m _cod_database_code 4001756 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x-y, -y, -z' '-x, -x+y, -z' 'y, x, -z' 'y, x, z' '-x, -x+y, z' 'x-y, -y, z' 'x, y, -z' '-x+y, -x, -z' '-y, x-y, -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 Ni1 Ni 0.67827(7) 1.0000 0.5000 0.0312(4) Uani 1 4 d S O1 O 0.8274(4) 1.0777(4) 0.5000 0.0412(14) Uani 1 2 d S O2 O 0.5510(4) 0.8853(4) 0.5000 0.0410(16) Uani 1 2 d S O3 O 0.4363(5) 0.9185(5) 0.5000 0.0561(18) Uani 1 2 d S C1 C 0.8253(8) 1.0000 0.5000 0.032(2) Uani 1 4 d S C2 C 0.9161(7) 1.0000 0.5000 0.034(2) Uani 1 4 d S C3 C 1.0000 1.0828(6) 0.5000 0.033(2) Uani 1 4 d S H3 H 1.0000 1.1398 0.5000 0.039 Uiso 1 4 calc SR C4 C 0.4664(7) 0.8614(5) 0.5000 0.045(2) Uani 1 2 d S C5 C 0.3984(6) 0.7612(6) 0.5000 0.0405(19) Uani 1 2 d S C6 C 0.4270(6) 0.6962(6) 0.5000 0.0393(19) Uani 1 2 d S H6 H 0.4914 0.7164 0.5000 0.047 Uiso 1 2 calc SR N1 N 0.6760(3) 1.0000 0.1857(9) 0.0311(12) Uani 1 2 d S C11 C 0.7546(6) 1.0815(5) 0.1076(11) 0.062(2) Uani 1 1 d . H11A H 0.8123 1.0848 0.1540 0.075 Uiso 1 1 calc R H11B H 0.7540 1.1372 0.1540 0.075 Uiso 1 1 calc R C12 C 0.5934(5) 1.0000 0.1080(13) 0.062(3) Uani 1 2 d S H12A H 0.5923 1.0555 0.1548 0.075 Uiso 0.50 1 calc PR H12B H 0.5368 0.9445 0.1548 0.075 Uiso 0.50 1 calc PR 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 Ni1 0.0279(5) 0.0253(7) 0.0394(7) 0.000 0.000 0.0127(3) O1 0.032(3) 0.040(4) 0.060(3) 0.000 0.000 0.024(3) O2 0.026(3) 0.037(3) 0.065(4) 0.000 0.000 0.019(3) O3 0.042(4) 0.033(3) 0.102(5) 0.000 0.000 0.026(3) C1 0.041(4) 0.031(6) 0.020(4) 0.000 0.000 0.016(3) C2 0.037(4) 0.043(6) 0.024(4) 0.000 0.000 0.021(3) C3 0.053(7) 0.032(4) 0.021(4) 0.000 0.000 0.026(3) C4 0.043(6) 0.028(4) 0.060(5) 0.000 0.000 0.014(4) C5 0.032(4) 0.033(4) 0.051(5) 0.000 0.000 0.012(3) C6 0.030(4) 0.034(4) 0.060(5) 0.000 0.000 0.020(3) N1 0.0255(18) 0.024(3) 0.043(3) 0.000 -0.0007(17) 0.0122(13) C11 0.061(4) 0.051(4) 0.037(4) -0.002(3) 0.001(3) 0.000(3) C12 0.057(4) 0.118(10) 0.033(4) 0.000 -0.001(3) 0.059(5) 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' 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' Ni Ni 0.3393 1.1124 '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 Ni1 O2 109.7(3) . 4_676 O2 Ni1 O1 156.5(2) . . O2 Ni1 O1 93.8(2) 4_676 . O2 Ni1 O1 93.8(2) . 4_676 O2 Ni1 O1 156.5(2) 4_676 4_676 O1 Ni1 O1 62.8(3) . 4_676 O2 Ni1 N1 89.44(7) . . O2 Ni1 N1 89.44(7) 4_676 . O1 Ni1 N1 90.84(11) . . O1 Ni1 N1 90.84(11) 4_676 . O2 Ni1 N1 89.44(7) . 4_676 O2 Ni1 N1 89.44(7) 4_676 4_676 O1 Ni1 N1 90.84(11) . 4_676 O1 Ni1 N1 90.83(11) 4_676 4_676 N1 Ni1 N1 178.0(3) . 4_676 O2 Ni1 C1 125.14(15) . . O2 Ni1 C1 125.14(15) 4_676 . O1 Ni1 C1 31.39(16) . . O1 Ni1 C1 31.38(16) 4_676 . N1 Ni1 C1 90.98(13) . . N1 Ni1 C1 90.98(13) 4_676 . C1 O1 Ni1 87.2(6) . . C4 O2 Ni1 141.0(5) . . O1 C1 O1 122.7(11) 4_676 . O1 C1 C2 118.6(6) 4_676 . O1 C1 C2 118.6(6) . . O1 C1 Ni1 61.4(6) 4_676 . O1 C1 Ni1 61.4(6) . . C2 C1 Ni1 180.000(1) . . C3 C2 C3 118.7(12) 2_765 . C3 C2 C1 120.6(6) 2_765 . C3 C2 C1 120.6(6) . . C2 C3 C2 121.3(12) . 3_675 O2 C4 O3 124.0(8) . . O2 C4 C5 117.5(8) . . O3 C4 C5 118.5(9) . . C6 C5 C6 119.1(8) . 2_665 C6 C5 C4 121.0(9) . . C6 C5 C4 119.9(9) 2_665 . C5 C6 C5 120.9(8) . 3_565 C11 N1 C11 109.2(8) . 9_675 C11 N1 C12 105.6(5) . . C11 N1 C12 105.6(5) 9_675 . C11 N1 Ni1 111.8(4) . . C11 N1 Ni1 111.8(4) 9_675 . C12 N1 Ni1 112.5(5) . . N1 C11 C11 112.3(4) . 10 N1 C12 C12 111.5(4) . 4_675 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ni1 O2 2.025(7) . Ni1 O2 2.025(7) 4_676 Ni1 O1 2.153(5) . Ni1 O1 2.153(5) 4_676 Ni1 N1 2.201(7) . Ni1 N1 2.201(7) 4_676 Ni1 C1 2.450(13) . O1 C1 1.277(8) . O2 C4 1.258(11) . O3 C4 1.278(11) . C1 O1 1.277(8) 4_676 C1 C2 1.514(16) . C2 C3 1.389(7) 2_765 C2 C3 1.389(7) . C3 C2 1.389(7) 3_675 C4 C5 1.478(12) . C5 C6 1.383(13) . C5 C6 1.395(12) 2_665 C6 C5 1.395(12) 3_565 N1 C11 1.442(8) . N1 C11 1.442(8) 9_675 N1 C12 1.480(10) . C11 C11 1.507(16) 10 C12 C12 1.513(18) 4_675 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 1 -0.016 0.618 -0.355 743.6 18.1