#------------------------------------------------------------------------------ #$Date: 2015-01-23 14:30:19 +0200 (Fri, 23 Jan 2015) $ #$Revision: 130086 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/10/16/7101642.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_7101642 loop_ _publ_author_name 'Ram\'irez, Juan' 'Stadler, Adrian-Mihail' 'Kyritsakas, Nathalie' 'Lehn, Jean-Marie' _publ_section_title ; Solvent-modulated reversible conversion of a [2 x 2]-grid into a pincer-like complex. ; _journal_issue 3 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 237 _journal_page_last 239 _journal_paper_doi 10.1039/b612222a _journal_year 2007 _chemical_formula_moiety 'C27 H27 Co N11, 2(Cl O4)' _chemical_formula_sum 'C27 H27 Cl2 Co N11 O8' _chemical_formula_weight 763.43 _chemical_name_systematic ; ? ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _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 112.93(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 15.542(4) _cell_length_b 16.699(4) _cell_length_c 13.539(3) _cell_measurement_reflns_used 4680 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 27.47 _cell_measurement_theta_min 2.3 _cell_volume 3236.2(14) _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p 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 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0738 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 3679 _diffrn_reflns_theta_full 27.47 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_theta_min 2.09 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time . _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.762 _exptl_absorpt_correction_type none _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.567 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1564 _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.626 _refine_diff_density_min -0.638 _refine_diff_density_rms 0.078 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 242 _refine_ls_number_reflns 3679 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.035 _refine_ls_R_factor_all 0.0793 _refine_ls_R_factor_gt 0.0488 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.003 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0685P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1211 _refine_ls_wR_factor_ref 0.1357 _reflns_number_gt 2528 _reflns_number_total 3679 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file b612222a.txt _[local]_cod_data_source_block st1581 _[local]_cod_cif_authors_sg_H-M C2/c _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'none' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas ; _cod_database_code 7101642 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' 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 Co Co 0.5000 0.16137(3) 0.2500 0.02427(18) Uani 1 2 d S N1 N 0.61392(16) 0.16738(12) 0.19976(18) 0.0292(5) Uani 1 1 d . C1 C 0.6740(2) 0.17579(16) 0.1736(2) 0.0344(7) Uani 1 1 d . C2 C 0.7511(3) 0.1841(2) 0.1392(4) 0.0665(12) Uani 1 1 d . N2 N 0.58253(15) 0.26031(13) 0.36348(18) 0.0274(5) Uani 1 1 d . C3 C 0.5981(2) 0.33481(16) 0.3377(2) 0.0346(7) Uani 1 1 d . C4 C 0.6412(2) 0.39348(17) 0.4132(3) 0.0441(8) Uani 1 1 d . C5 C 0.6724(2) 0.3746(2) 0.5207(3) 0.0485(9) Uani 1 1 d . C6 C 0.6622(2) 0.29721(18) 0.5492(2) 0.0411(8) Uani 1 1 d . C7 C 0.61729(18) 0.24185(17) 0.4691(2) 0.0299(6) Uani 1 1 d . C8 C 0.61273(19) 0.15819(16) 0.4951(2) 0.0304(6) Uani 1 1 d . N3 N 0.57721(15) 0.11068(12) 0.41670(17) 0.0256(5) Uani 1 1 d . N4 N 0.57510(16) 0.03041(12) 0.43210(18) 0.0284(5) Uani 1 1 d . C9 C 0.6240(2) -0.00599(17) 0.5368(2) 0.0338(7) Uani 1 1 d . N5 N 0.5000 0.03023(17) 0.2500 0.0254(7) Uani 1 2 d S C10 C 0.53533(18) -0.01297(15) 0.3393(2) 0.0267(6) Uani 1 1 d . N6 N 0.53409(16) -0.09279(12) 0.34570(19) 0.0308(6) Uani 1 1 d . C11 C 0.5000 -0.1292(2) 0.2500 0.0290(9) Uani 1 2 d S C12 C 0.5000 -0.2182(2) 0.2500 0.0330(10) Uani 1 2 d S C13 C 0.4806(2) -0.26017(17) 0.1546(3) 0.0393(8) Uani 1 1 d . C14 C 0.4811(2) -0.34324(18) 0.1547(3) 0.0476(9) Uani 1 1 d . C15 C 0.5000 -0.3841(2) 0.2500 0.0504(13) Uani 1 2 d S Cl Cl 0.77616(5) 0.91933(5) 0.33185(6) 0.0433(2) Uani 1 1 d . O1 O 0.7195(2) 0.86549(15) 0.2551(2) 0.0789(10) Uani 1 1 d . O2 O 0.7618(3) 0.9281(3) 0.4244(2) 0.1225(16) Uani 1 1 d . O3 O 0.8025(5) 0.9814(3) 0.2831(5) 0.0617(17) Uani 0.50 1 d P O4 O 0.8592(4) 0.8640(4) 0.3803(4) 0.0651(15) Uani 0.50 1 d P O5 O 0.7083(4) 0.9902(3) 0.2928(5) 0.0756(17) Uani 0.50 1 d P O6 O 0.8611(5) 0.9480(6) 0.3327(7) 0.111(3) Uani 0.50 1 d P H1 H 0.7674 0.2392 0.1406 0.085 Uiso 1 1 d . H2 H 0.8035 0.1549 0.1863 0.085 Uiso 1 1 d . H3 H 0.7331 0.1641 0.0684 0.085 Uiso 1 1 d . H4 H 0.5791 0.3480 0.2641 0.044 Uiso 1 1 d . H5 H 0.6493 0.4458 0.3911 0.058 Uiso 1 1 d . H6 H 0.6995 0.4144 0.5735 0.064 Uiso 1 1 d . H7 H 0.6852 0.2818 0.6222 0.052 Uiso 1 1 d . H8 H 0.6363 0.1397 0.5677 0.039 Uiso 1 1 d . H9 H 0.6142 -0.0622 0.5309 0.045 Uiso 1 1 d . H10 H 0.6887 0.0052 0.5602 0.045 Uiso 1 1 d . H11 H 0.6004 0.0155 0.5859 0.045 Uiso 1 1 d . H12 H 0.4663 -0.2318 0.0894 0.052 Uiso 1 1 d . H13 H 0.4695 -0.3721 0.0904 0.063 Uiso 1 1 d . H14 H 0.5000 -0.4410 0.2500 0.065 Uiso 1 2 d S 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 Co 0.0272(3) 0.0251(3) 0.0207(3) 0.000 0.0097(2) 0.000 N1 0.0304(12) 0.0304(12) 0.0275(13) -0.0043(10) 0.0121(10) -0.0017(10) C1 0.0333(16) 0.0349(15) 0.0373(18) -0.0133(13) 0.0164(14) -0.0056(12) C2 0.056(2) 0.075(2) 0.092(3) -0.040(2) 0.055(2) -0.028(2) N2 0.0263(12) 0.0320(12) 0.0250(13) -0.0017(10) 0.0111(10) -0.0005(9) C3 0.0316(15) 0.0328(15) 0.0421(19) 0.0013(13) 0.0173(14) -0.0032(13) C4 0.0341(16) 0.0342(16) 0.062(2) -0.0050(16) 0.0165(16) -0.0068(13) C5 0.052(2) 0.0429(18) 0.050(2) -0.0207(17) 0.0189(17) -0.0130(16) C6 0.0498(19) 0.0409(17) 0.0333(18) -0.0101(14) 0.0168(15) -0.0075(15) C7 0.0278(15) 0.0382(15) 0.0243(15) -0.0062(12) 0.0107(12) -0.0023(12) C8 0.0327(15) 0.0387(15) 0.0180(14) -0.0001(12) 0.0078(12) 0.0010(13) N3 0.0266(11) 0.0271(11) 0.0231(12) 0.0003(10) 0.0098(9) 0.0026(9) N4 0.0343(13) 0.0261(11) 0.0227(12) 0.0018(10) 0.0088(10) -0.0001(10) C9 0.0356(16) 0.0388(15) 0.0225(15) 0.0102(12) 0.0062(13) 0.0048(13) N5 0.0296(17) 0.0272(15) 0.0190(16) 0.000 0.0089(14) 0.000 C10 0.0264(14) 0.0282(13) 0.0265(15) 0.0036(12) 0.0115(12) 0.0019(11) N6 0.0314(13) 0.0278(12) 0.0339(14) 0.0025(11) 0.0136(11) 0.0004(10) C11 0.0242(19) 0.0287(19) 0.036(2) 0.000 0.0142(17) 0.000 C12 0.026(2) 0.0277(19) 0.046(3) 0.000 0.0140(19) 0.000 C13 0.0381(17) 0.0320(15) 0.047(2) -0.0044(14) 0.0151(15) -0.0026(13) C14 0.0430(18) 0.0347(16) 0.065(3) -0.0086(17) 0.0214(18) -0.0029(15) C15 0.040(3) 0.027(2) 0.079(4) 0.000 0.017(3) 0.000 Cl 0.0479(5) 0.0502(5) 0.0316(5) -0.0116(3) 0.0154(4) -0.0052(4) O1 0.118(2) 0.0542(14) 0.0365(14) -0.0075(13) 0.0000(15) -0.0340(16) O2 0.120(3) 0.214(4) 0.051(2) -0.043(2) 0.051(2) -0.083(3) O3 0.087(5) 0.064(3) 0.049(4) -0.011(3) 0.042(4) -0.041(4) O4 0.059(3) 0.086(4) 0.039(3) -0.005(3) 0.006(2) 0.030(3) O5 0.082(4) 0.056(3) 0.066(4) -0.009(3) 0.004(3) 0.016(3) O6 0.063(5) 0.156(8) 0.133(8) -0.096(7) 0.061(5) -0.052(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 N1 Co N1 174.60(11) . 2_655 N1 Co N5 92.70(6) . . N1 Co N5 92.70(6) 2_655 . N1 Co N3 83.30(8) . 2_655 N1 Co N3 98.74(8) 2_655 2_655 N5 Co N3 68.08(5) . 2_655 N1 Co N3 98.74(8) . . N1 Co N3 83.30(8) 2_655 . N5 Co N3 68.08(5) . . N3 Co N3 136.15(11) 2_655 . N1 Co N2 82.05(8) . . N1 Co N2 94.01(8) 2_655 . N5 Co N2 136.43(6) . . N3 Co N2 151.87(8) 2_655 . N3 Co N2 70.07(8) . . N1 Co N2 94.01(8) . 2_655 N1 Co N2 82.06(8) 2_655 2_655 N5 Co N2 136.43(6) . 2_655 N3 Co N2 70.07(8) 2_655 2_655 N3 Co N2 151.87(8) . 2_655 N2 Co N2 87.14(11) . 2_655 C1 N1 Co 175.5(2) . . N1 C1 C2 178.3(3) . . C1 C2 H1 109.4 . . C1 C2 H2 109.6 . . H1 C2 H2 109.3 . . C1 C2 H3 109.6 . . H1 C2 H3 109.4 . . H2 C2 H3 109.7 . . C3 N2 C7 116.7(2) . . C3 N2 Co 127.5(2) . . C7 N2 Co 115.80(17) . . N2 C3 C4 123.4(3) . . N2 C3 H4 118.4 . . C4 C3 H4 118.2 . . C5 C4 C3 119.1(3) . . C5 C4 H5 120.6 . . C3 C4 H5 120.3 . . C6 C5 C4 118.6(3) . . C6 C5 H6 121.0 . . C4 C5 H6 120.4 . . C5 C6 C7 119.0(3) . . C5 C6 H7 120.7 . . C7 C6 H7 120.3 . . N2 C7 C6 123.1(3) . . N2 C7 C8 116.1(2) . . C6 C7 C8 120.6(3) . . N3 C8 C7 116.5(2) . . N3 C8 H8 121.8 . . C7 C8 H8 121.7 . . C8 N3 N4 121.2(2) . . C8 N3 Co 119.29(18) . . N4 N3 Co 119.08(16) . . N3 N4 C10 114.2(2) . . N3 N4 C9 121.8(2) . . C10 N4 C9 123.3(2) . . N4 C9 H9 109.0 . . N4 C9 H10 109.1 . . H9 C9 H10 109.8 . . N4 C9 H11 109.1 . . H9 C9 H11 109.7 . . H10 C9 H11 110.0 . . C10 N5 C10 114.3(3) 2_655 . C10 N5 Co 122.87(15) 2_655 . C10 N5 Co 122.87(15) . . N5 C10 N6 126.1(3) . . N5 C10 N4 115.2(2) . . N6 C10 N4 118.7(2) . . C10 N6 C11 113.6(2) . . N6 C11 N6 126.0(3) . 2_655 N6 C11 C12 117.00(16) . . N6 C11 C12 117.00(16) 2_655 . C13 C12 C13 119.7(3) . 2_655 C13 C12 C11 120.16(17) . . C13 C12 C11 120.16(17) 2_655 . C14 C13 C12 120.2(3) . . C14 C13 H12 119.9 . . C12 C13 H12 119.9 . . C15 C14 C13 119.4(3) . . C15 C14 H13 120.0 . . C13 C14 H13 120.6 . . C14 C15 C14 121.1(4) 2_655 . C14 C15 H14 119.5 2_655 . C14 C15 H14 119.5 . . O2 Cl O3 123.1(3) . . O2 Cl O1 118.2(2) . . O3 Cl O1 110.3(3) . . O2 Cl O6 116.6(3) . . O1 Cl O6 123.0(3) . . O2 Cl O4 94.8(3) . . O3 Cl O4 107.8(4) . . O1 Cl O4 96.5(3) . . O6 Cl O4 64.1(5) . . O2 Cl O5 84.1(3) . . O3 Cl O5 63.1(4) . . O1 Cl O5 95.2(2) . . O6 Cl O5 105.0(5) . . O4 Cl O5 167.2(3) . . O6 O3 Cl 68.9(6) . . O6 O3 O5 127.9(7) . . Cl O3 O5 63.6(3) . . Cl O4 O6 54.4(3) . . O3 O5 Cl 53.3(3) . . O3 O6 Cl 66.3(5) . . O3 O6 O4 126.3(7) . . Cl O6 O4 61.5(4) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Co N1 2.132(2) . Co N1 2.132(2) 2_655 Co N5 2.190(3) . Co N3 2.267(2) 2_655 Co N3 2.267(2) . Co N2 2.280(2) . Co N2 2.280(2) 2_655 N1 C1 1.128(4) . C1 C2 1.453(5) . C2 H1 0.9531 . C2 H2 0.9494 . C2 H3 0.9483 . N2 C3 1.339(3) . N2 C7 1.352(3) . C3 C4 1.385(4) . C3 H4 0.9492 . C4 C5 1.380(5) . C4 H5 0.9471 . C5 C6 1.376(5) . C5 H6 0.9463 . C6 C7 1.388(4) . C6 H7 0.9470 . C7 C8 1.449(4) . C8 N3 1.267(3) . C8 H8 0.9554 . N3 N4 1.359(3) . N4 C10 1.371(3) . N4 C9 1.455(3) . C9 H9 0.9495 . C9 H10 0.9466 . C9 H11 0.9474 . N5 C10 1.329(3) 2_655 N5 C10 1.329(3) . C10 N6 1.336(3) . N6 C11 1.339(3) . C11 N6 1.340(3) 2_655 C11 C12 1.486(5) . C12 C13 1.395(4) . C12 C13 1.395(4) 2_655 C13 C14 1.387(4) . C13 H12 0.9494 . C14 C15 1.386(4) . C14 H13 0.9486 . C15 C14 1.386(4) 2_655 C15 H14 0.9498 . Cl O2 1.363(3) . Cl O3 1.374(5) . Cl O1 1.397(2) . Cl O6 1.400(7) . Cl O4 1.514(5) . Cl O5 1.535(5) . O3 O6 1.056(9) . O3 O5 1.527(9) . O4 O6 1.548(11) .