Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Hanai, Hiroshi' 'Kaizaki, Sumio' 'Komorita, Takashi' 'Suzuki, Takayoshi' 'Yagi, Takashi' _publ_contact_author_name 'Prof Sumio Kaizaki' _publ_contact_author_address ; Prof Sumio Kaizaki Department of Chemistry, Graduate School of Science Osaka University Toyonaka 560-0043 JAPAN ; _publ_contact_author_email 'KAIZAKI@CHEM.SCI.OSAKA-U.AC.JP' _publ_section_title ; Structural and spectroscopic comparisions of the square planar four coordinate (o-phenylenebis(biuretato)cobaltate(III) complex and the five coordinate mono and six coordinate dicyano adducts. ; data_[K(crypt)][Co(bbphen)] _database_code_CSD 169288 #------------------------------------------------------------------------------ _audit_creation_date 'Wed Mar 3 12:48:11 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'SHELXS86' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics 'ORTEP in teXsan' #------------------------------------------------------------------------------ _chemical_compound_source ; Prepared from K[Co(bbphen)] and cryptand[2,2,2] in water,recrystallized from a mixture of dimethylsulfoxide and water. ; _chemical_name_systematic ; 4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8,8,8]hexacosane pottassium (o-phenylenebis(biuretato))cobaltate(III) ; _chemical_name_common '[K(crypt)][Co(bbphen)]' _chemical_formula_weight 750.73 _chemical_formula_analytical 'C28 H44 Co K N8 O10' _chemical_formula_sum 'C28 H44 Co K N8 O10' _chemical_formula_moiety 'C18 H36 K N2 O6 1+, C10 H8 N6 O4 Co 1-' _chemical_formula_structural '(K (C18 H36 N2 O6)), (Co (C10 H8 N6 O4))' _chemical_melting_point 476 #------------------------------------------------------------------------------ _cell_length_a 13.540(2) _cell_length_b 16.692(4) _cell_length_c 15.317(2) _cell_angle_alpha 90 _cell_angle_beta 93.92(1) _cell_angle_gamma 90 _cell_volume 3453(1) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.9 _cell_measurement_theta_max 15.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'red-purple' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.360 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576.00 _exptl_absorpt_coefficient_mu 0.683 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details Coppens_numerical _exptl_absorpt_correction_T_min 0.790 _exptl_absorpt_correction_T_max 0.877 _exptl_special_details 'none' #------------------------------------------------------------------------------ _diffrn_special_details ; \q scan width (1.680 + 0.35tan\q)\%, \w scan rate 16\% per min. Background counts for 25% time on each side every scan. ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method '\w-2\q' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -3.49 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 3 -3 1 1 -3 0 2 -4 _diffrn_reflns_number 10456 _reflns_number_total 10074 _reflns_number_gt 5910 _reflns_observed_expression 'F^2^ > 2.0 \s(F^2^)' _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_av_sigmaI/netI 0.087 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 30.01 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.03951 _diffrn_orient_matrix_UB_12 0.03291 _diffrn_orient_matrix_UB_13 -0.04435 _diffrn_orient_matrix_UB_21 -0.06258 _diffrn_orient_matrix_UB_22 -0.02195 _diffrn_orient_matrix_UB_23 0.02161 _diffrn_orient_matrix_UB_31 -0.00159 _diffrn_orient_matrix_UB_32 0.04499 _diffrn_orient_matrix_UB_33 0.04300 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'Co' 'Co' 0.349 0.972 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'K' 'K' 0.200 0.250 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'C' 'C' 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.31801(2) 0.10104(2) 0.11966(2) 0.02963(7) Uani 1.00 d . . . K K 0.75894(4) 0.12814(4) 0.46827(4) 0.0495(2) Uani 1.00 d . . . O(1) O 0.5967(1) 0.0260(1) 0.0863(1) 0.0527(5) Uani 1.00 d . . . O(2) O 0.5209(1) 0.1819(1) 0.3053(1) 0.0707(7) Uani 1.00 d . . . O(3) O 0.0391(1) 0.1296(1) 0.1930(1) 0.0574(6) Uani 1.00 d . . . O(4) O 0.1147(1) -0.0113(1) -0.0411(1) 0.0589(6) Uani 1.00 d . . . O(5) O 0.9508(1) 0.2033(1) 0.4901(1) 0.0708(7) Uani 1.00 d . . . O(6) O 0.8979(1) 0.0889(1) 0.6139(1) 0.0717(7) Uani 1.00 d . . . O(7) O 0.6425(1) 0.2643(1) 0.4894(1) 0.0619(6) Uani 1.00 d . . . O(8) O 0.5856(2) 0.1156(1) 0.5638(1) 0.0663(7) Uani 1.00 d . . . O(9) O 0.7566(1) 0.1136(1) 0.2806(1) 0.0563(6) Uani 1.00 d . . . O(10) O 0.7641(2) -0.0236(1) 0.3935(2) 0.0736(7) Uani 1.00 d . . . N(1) N 0.4322(1) 0.0579(1) 0.0819(1) 0.0387(5) Uani 1.00 d . . . N(2) N 0.5444(1) 0.1050(1) 0.1918(1) 0.0401(5) Uani 1.00 d . . . N(3) N 0.3864(1) 0.1615(1) 0.2067(1) 0.0322(5) Uani 1.00 d . . . N(4) N 0.2033(1) 0.1430(1) 0.1631(1) 0.0334(5) Uani 1.00 d . . . N(5) N 0.0896(1) 0.0623(1) 0.0786(1) 0.0424(5) Uani 1.00 d . . . N(6) N 0.2490(1) 0.0447(1) 0.0332(1) 0.0357(5) Uani 1.00 d . . . N(7) N 0.7998(2) 0.2721(2) 0.3651(2) 0.0616(8) Uani 1.00 d . . . N(8) N 0.7275(2) -0.0172(2) 0.5793(2) 0.0727(9) Uani 1.00 d . . . C(1) C 0.5253(2) 0.0606(1) 0.1165(1) 0.0363(6) Uani 1.00 d . . . C(2) C 0.4833(2) 0.1526(1) 0.2385(1) 0.0390(6) Uani 1.00 d . . . C(3) C 0.3243(2) 0.2133(1) 0.2517(1) 0.0351(6) Uani 1.00 d . . . C(4) C 0.3548(2) 0.2731(2) 0.3113(2) 0.0471(7) Uani 1.00 d . . . C(5) C 0.2846(2) 0.3187(2) 0.3510(2) 0.0562(8) Uani 1.00 d . . . C(6) C 0.1856(2) 0.3066(2) 0.3302(2) 0.0571(9) Uani 1.00 d . . . C(7) C 0.1536(2) 0.2493(2) 0.2693(2) 0.0484(7) Uani 1.00 d . . . C(8) C 0.2228(2) 0.2022(1) 0.2286(1) 0.0359(6) Uani 1.00 d . . . C(9) C 0.1080(2) 0.1134(1) 0.1481(2) 0.0385(6) Uani 1.00 d . . . C(10) C 0.1514(2) 0.0303(1) 0.0197(1) 0.0385(6) Uani 1.00 d . . . C(11) C 0.9072(3) 0.2891(3) 0.3713(2) 0.092(1) Uani 1.00 d . . . C(12) C 0.9534(2) 0.2841(2) 0.4627(2) 0.083(1) Uani 1.00 d . . . C(13) C 0.9989(2) 0.1968(2) 0.5749(2) 0.078(1) Uani 1.00 d . . . C(14) C 0.9974(2) 0.1127(2) 0.6045(3) 0.086(1) Uani 1.00 d . . . C(15) C 0.8964(3) 0.0109(2) 0.6478(3) 0.087(1) Uani 1.00 d . . . C(16) C 0.7912(3) -0.0130(2) 0.6600(3) 0.092(1) Uani 1.00 d . . . C(17) C 0.7460(3) 0.3397(2) 0.3997(2) 0.079(1) Uani 1.00 d . . . C(18) C 0.6417(3) 0.3208(2) 0.4198(2) 0.072(1) Uani 1.00 d . . . C(19) C 0.5448(2) 0.2453(2) 0.5117(2) 0.0645(9) Uani 1.00 d . . . C(20) C 0.5502(2) 0.1923(2) 0.5885(2) 0.073(1) Uani 1.00 d . . . C(21) C 0.5864(3) 0.0584(3) 0.6318(3) 0.100(2) Uani 1.00 d . . . C(22) C 0.6234(3) -0.0190(3) 0.6002(3) 0.096(1) Uani 1.00 d . . . C(23) C 0.7642(2) 0.2566(2) 0.2731(2) 0.0661(10) Uani 1.00 d . . . C(24) C 0.7987(2) 0.1788(3) 0.2368(2) 0.073(1) Uani 1.00 d . . . C(25) C 0.7980(3) 0.0377(3) 0.2582(2) 0.083(1) Uani 1.00 d . . . C(26) C 0.7453(3) -0.0267(2) 0.3006(3) 0.093(1) Uani 1.00 d . . . C(27) C 0.7155(3) -0.0865(2) 0.4363(3) 0.103(2) Uani 1.00 d . . . C(28) C 0.7505(3) -0.0895(2) 0.5304(3) 0.094(1) Uani 1.00 d . . . H(1) H 0.4321 0.0205 0.0360 0.0618 Uiso 1.00 d . . . H(2) H 0.6100 0.1091 0.2142 0.0618 Uiso 1.00 d . . . H(3) H 0.4262 0.2786 0.3311 0.0618 Uiso 1.00 d . . . H(4) H 0.3061 0.3590 0.3928 0.0618 Uiso 1.00 d . . . H(5) H 0.1356 0.3462 0.3584 0.0618 Uiso 1.00 d . . . H(6) H 0.0822 0.2368 0.2600 0.0618 Uiso 1.00 d . . . H(7) H 0.0221 0.0506 0.0702 0.0618 Uiso 1.00 d . . . H(8) H 0.2850 0.0145 -0.0089 0.0618 Uiso 1.00 d . . . H(9) H 0.9274 0.3357 0.3448 0.0618 Uiso 1.00 d . . . H(10) H 0.9411 0.2432 0.3305 0.0618 Uiso 1.00 d . . . H(11) H 0.9162 0.3284 0.5111 0.0618 Uiso 1.00 d . . . H(12) H 1.0285 0.2981 0.4629 0.0618 Uiso 1.00 d . . . H(13) H 1.0705 0.2096 0.5795 0.0618 Uiso 1.00 d . . . H(14) H 0.9607 0.2399 0.6221 0.0618 Uiso 1.00 d . . . H(15) H 1.0356 0.1174 0.6658 0.0618 Uiso 1.00 d . . . H(16) H 1.0273 0.0769 0.5492 0.0618 Uiso 1.00 d . . . H(17) H 0.9407 -0.0021 0.7074 0.0618 Uiso 1.00 d . . . H(18) H 0.9118 -0.0354 0.5962 0.0618 Uiso 1.00 d . . . H(19) H 0.7886 -0.0620 0.6940 0.1152 Uiso 1.00 d . . . H(20) H 0.7637 0.0284 0.6998 0.1152 Uiso 1.00 d . . . H(21) H 0.7527 0.3904 0.3573 0.0618 Uiso 1.00 d . . . H(22) H 0.7820 0.3633 0.4549 0.0618 Uiso 1.00 d . . . H(23) H 0.6166 0.3822 0.4364 0.0618 Uiso 1.00 d . . . H(24) H 0.5958 0.3005 0.3647 0.0618 Uiso 1.00 d . . . H(25) H 0.5038 0.2990 0.5244 0.0618 Uiso 1.00 d . . . H(26) H 0.5066 0.2185 0.4586 0.0618 Uiso 1.00 d . . . H(27) H 0.5948 0.2064 0.6450 0.0618 Uiso 1.00 d . . . H(28) H 0.4785 0.1885 0.6127 0.0618 Uiso 1.00 d . . . H(29) H 0.6312 0.0765 0.6816 0.1152 Uiso 1.00 d . . . H(30) H 0.5223 0.0535 0.6550 0.1152 Uiso 1.00 d . . . H(31) H 0.5749 -0.0381 0.5445 0.0618 Uiso 1.00 d . . . H(32) H 0.6131 -0.0699 0.6444 0.0618 Uiso 1.00 d . . . H(33) H 0.7943 0.3016 0.2311 0.0618 Uiso 1.00 d . . . H(34) H 0.6847 0.2571 0.2682 0.0618 Uiso 1.00 d . . . H(35) H 0.8703 0.1812 0.2468 0.0618 Uiso 1.00 d . . . H(36) H 0.7822 0.1831 0.1721 0.0618 Uiso 1.00 d . . . H(37) H 0.8717 0.0359 0.2842 0.0618 Uiso 1.00 d . . . H(38) H 0.7837 0.0239 0.1921 0.0618 Uiso 1.00 d . . . H(39) H 0.7539 -0.0850 0.2879 0.0618 Uiso 1.00 d . . . H(40) H 0.6649 -0.0199 0.2888 0.0618 Uiso 1.00 d . . . H(41) H 0.7190 -0.1341 0.3991 0.0618 Uiso 1.00 d . . . H(42) H 0.6387 -0.0893 0.4383 0.0618 Uiso 1.00 d . . . H(43) H 0.7295 -0.1393 0.5762 0.0618 Uiso 1.00 d . . . H(44) H 0.8308 -0.0953 0.5414 0.0618 Uiso 1.00 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co 0.0222(1) 0.0368(2) 0.0298(1) -0.0018(1) 0.00091(9) -0.0031(1) K 0.0464(3) 0.0524(3) 0.0499(3) -0.0041(2) 0.0049(2) 0.0017(3) O(1) 0.0277(8) 0.078(1) 0.051(1) 0.0105(8) -0.0028(7) -0.0257(9) O(2) 0.0361(10) 0.110(2) 0.064(1) 0.006(1) -0.0095(9) -0.049(1) O(3) 0.0300(8) 0.079(1) 0.064(1) -0.0010(9) 0.0146(8) -0.019(1) O(4) 0.0294(8) 0.090(1) 0.057(1) -0.0107(9) -0.0018(8) -0.029(1) O(5) 0.057(1) 0.088(2) 0.065(1) -0.025(1) -0.0119(10) 0.003(1) O(6) 0.053(1) 0.083(2) 0.077(1) -0.004(1) -0.015(1) 0.022(1) O(7) 0.055(1) 0.059(1) 0.071(1) 0.0013(10) -0.0043(10) -0.009(1) O(8) 0.060(1) 0.087(2) 0.053(1) -0.001(1) 0.0106(9) 0.009(1) O(9) 0.0393(9) 0.082(1) 0.048(1) 0.0107(9) 0.0049(8) -0.0109(10) O(10) 0.074(1) 0.058(1) 0.085(2) 0.005(1) -0.023(1) -0.011(1) N(1) 0.0244(9) 0.052(1) 0.040(1) 0.0005(8) -0.0001(7) -0.0154(9) N(2) 0.0252(8) 0.056(1) 0.039(1) 0.0007(8) -0.0032(7) -0.0136(9) N(3) 0.0277(8) 0.0384(10) 0.0303(9) -0.0008(7) 0.0006(7) -0.0073(8) N(4) 0.0254(8) 0.041(1) 0.0341(9) 0.0009(7) 0.0036(7) -0.0033(8) N(5) 0.0215(8) 0.059(1) 0.046(1) -0.0026(8) 0.0007(8) -0.0100(10) N(6) 0.0233(8) 0.047(1) 0.0366(10) -0.0031(8) 0.0005(7) -0.0071(8) N(7) 0.055(1) 0.071(2) 0.058(1) -0.023(1) -0.006(1) 0.012(1) N(8) 0.061(2) 0.070(2) 0.085(2) -0.010(1) -0.011(1) 0.035(2) C(1) 0.029(1) 0.045(1) 0.035(1) -0.0005(9) 0.0005(9) -0.0079(10) C(2) 0.028(1) 0.050(1) 0.039(1) -0.0047(10) 0.0008(9) -0.011(1) C(3) 0.035(1) 0.037(1) 0.033(1) 0.0011(9) 0.0009(9) -0.0025(9) C(4) 0.049(1) 0.045(1) 0.046(1) 0.003(1) -0.005(1) -0.011(1) C(5) 0.068(2) 0.050(2) 0.050(2) 0.011(1) -0.003(1) -0.017(1) C(6) 0.063(2) 0.055(2) 0.054(2) 0.015(1) 0.012(1) -0.014(1) C(7) 0.040(1) 0.053(2) 0.053(2) 0.010(1) 0.009(1) -0.008(1) C(8) 0.036(1) 0.038(1) 0.034(1) 0.0028(9) 0.0032(9) 0.0002(9) C(9) 0.0260(10) 0.047(1) 0.042(1) 0.0024(9) 0.0014(9) -0.001(1) C(10) 0.027(1) 0.049(1) 0.039(1) -0.0040(10) -0.0009(9) -0.001(1) C(11) 0.066(2) 0.127(3) 0.082(2) -0.051(2) -0.008(2) 0.036(2) C(12) 0.066(2) 0.101(3) 0.078(2) -0.045(2) -0.017(2) 0.014(2) C(13) 0.052(2) 0.096(3) 0.083(2) -0.014(2) -0.023(2) 0.003(2) C(14) 0.052(2) 0.097(3) 0.105(3) -0.007(2) -0.027(2) 0.004(2) C(15) 0.074(2) 0.083(3) 0.099(3) 0.001(2) -0.025(2) 0.030(2) C(16) 0.078(2) 0.104(3) 0.092(3) -0.012(2) -0.018(2) 0.053(2) C(17) 0.101(3) 0.048(2) 0.084(2) -0.023(2) -0.015(2) 0.003(2) C(18) 0.084(2) 0.048(2) 0.082(2) 0.007(2) -0.009(2) -0.009(2) C(19) 0.050(2) 0.074(2) 0.068(2) 0.010(1) -0.006(1) -0.028(2) C(20) 0.051(2) 0.116(3) 0.051(2) 0.000(2) 0.004(1) -0.025(2) C(21) 0.059(2) 0.164(4) 0.080(3) -0.003(2) 0.014(2) 0.056(3) C(22) 0.063(2) 0.103(3) 0.122(3) -0.026(2) -0.005(2) 0.066(3) C(23) 0.058(2) 0.087(2) 0.053(2) -0.017(2) -0.003(1) 0.019(2) C(24) 0.047(2) 0.129(3) 0.046(2) -0.006(2) 0.011(1) 0.008(2) C(25) 0.076(2) 0.115(3) 0.057(2) 0.049(2) -0.010(2) -0.032(2) C(26) 0.102(3) 0.067(2) 0.103(3) 0.028(2) -0.036(2) -0.032(2) C(27) 0.099(3) 0.056(2) 0.147(4) -0.021(2) -0.025(3) -0.011(2) C(28) 0.093(3) 0.063(2) 0.121(3) -0.010(2) -0.025(2) 0.032(2) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F^2^ against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^, conventional R-factors (R) are calculated on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. R-factors based on F^2^ are statistically about twice as large as those based on F, and R-factor based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + 0.00090(Fo^2^)^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details Centrosymmetric _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 10074 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.1069 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.1099 _refine_ls_wR_factor_gt 0.0962 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.270 _refine_ls_shift/su_max 0.0010 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.91 _refine_diff_density_max 0.51 #------------------------------------------------------------------------------ loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co N(1) 1.835(2) 1_555 1_555 yes Co N(3) 1.867(2) 1_555 1_555 yes Co N(4) 1.867(2) 1_555 1_555 yes Co N(6) 1.829(2) 1_555 1_555 yes K O(5) 2.884(2) 1_555 1_555 yes K O(6) 2.893(2) 1_555 1_555 yes K O(7) 2.798(2) 1_555 1_555 yes K O(8) 2.857(2) 1_555 1_555 yes K O(9) 2.883(2) 1_555 1_555 yes K O(10) 2.783(2) 1_555 1_555 yes K N(7) 2.949(2) 1_555 1_555 yes K N(8) 3.010(3) 1_555 1_555 yes O(1) C(1) 1.242(3) 1_555 1_555 yes O(2) C(2) 1.215(3) 1_555 1_555 yes O(3) C(9) 1.225(3) 1_555 1_555 yes O(4) C(10) 1.237(3) 1_555 1_555 yes O(5) C(12) 1.414(4) 1_555 1_555 yes O(5) C(13) 1.416(4) 1_555 1_555 yes O(6) C(14) 1.421(4) 1_555 1_555 yes O(6) C(15) 1.403(4) 1_555 1_555 yes O(7) C(18) 1.422(4) 1_555 1_555 yes O(7) C(19) 1.424(4) 1_555 1_555 yes O(8) C(20) 1.426(4) 1_555 1_555 yes O(8) C(21) 1.412(4) 1_555 1_555 yes O(9) C(24) 1.418(4) 1_555 1_555 yes O(9) C(25) 1.436(4) 1_555 1_555 yes O(10) C(26) 1.430(4) 1_555 1_555 yes O(10) C(27) 1.422(4) 1_555 1_555 yes N(1) C(1) 1.335(3) 1_555 1_555 yes N(2) C(1) 1.381(3) 1_555 1_555 yes N(2) C(2) 1.380(3) 1_555 1_555 yes N(3) C(2) 1.376(3) 1_555 1_555 yes N(3) C(3) 1.418(3) 1_555 1_555 yes N(4) C(8) 1.420(3) 1_555 1_555 yes N(4) C(9) 1.386(3) 1_555 1_555 yes N(5) C(9) 1.374(3) 1_555 1_555 yes N(5) C(10) 1.380(3) 1_555 1_555 yes N(6) C(10) 1.345(3) 1_555 1_555 yes N(7) C(11) 1.477(4) 1_555 1_555 yes N(7) C(17) 1.462(4) 1_555 1_555 yes N(7) C(23) 1.482(4) 1_555 1_555 yes N(8) C(16) 1.461(4) 1_555 1_555 yes N(8) C(22) 1.467(4) 1_555 1_555 yes N(8) C(28) 1.464(5) 1_555 1_555 yes C(3) C(4) 1.396(3) 1_555 1_555 yes C(3) C(8) 1.408(3) 1_555 1_555 yes C(4) C(5) 1.389(4) 1_555 1_555 yes C(5) C(6) 1.371(4) 1_555 1_555 yes C(6) C(7) 1.385(4) 1_555 1_555 yes C(7) C(8) 1.402(3) 1_555 1_555 yes C(11) C(12) 1.497(5) 1_555 1_555 yes C(13) C(14) 1.476(5) 1_555 1_555 yes C(15) C(16) 1.503(5) 1_555 1_555 yes C(17) C(18) 1.498(5) 1_555 1_555 yes C(19) C(20) 1.470(5) 1_555 1_555 yes C(21) C(22) 1.479(6) 1_555 1_555 yes C(23) C(24) 1.500(5) 1_555 1_555 yes C(25) C(26) 1.467(6) 1_555 1_555 yes C(27) C(28) 1.486(6) 1_555 1_555 yes N(1) H(1) 0.939 1_555 1_555 no N(2) H(2) 0.933 1_555 1_555 no N(5) H(7) 0.935 1_555 1_555 no N(6) H(8) 0.975 1_555 1_555 no C(4) H(3) 0.998 1_555 1_555 no C(5) H(4) 0.960 1_555 1_555 no C(6) H(5) 1.058 1_555 1_555 no C(7) H(6) 0.989 1_555 1_555 no C(11) H(9) 0.927 1_555 1_555 no C(11) H(10) 1.109 1_555 1_555 no C(12) H(11) 1.184 1_555 1_555 no C(12) H(12) 1.044 1_555 1_555 no C(13) H(13) 0.990 1_555 1_555 no C(13) H(14) 1.166 1_555 1_555 no C(14) H(15) 1.043 1_555 1_555 no C(14) H(16) 1.133 1_555 1_555 no C(15) H(17) 1.080 1_555 1_555 no C(15) H(18) 1.134 1_555 1_555 no C(16) H(19) 0.973 1_555 1_555 no C(16) H(20) 1.010 1_555 1_555 no C(17) H(21) 1.075 1_555 1_555 no C(17) H(22) 1.026 1_555 1_555 no C(18) H(23) 1.114 1_555 1_555 no C(18) H(24) 1.070 1_555 1_555 no C(19) H(25) 1.080 1_555 1_555 no C(19) H(26) 1.036 1_555 1_555 no C(20) H(27) 1.047 1_555 1_555 no C(20) H(28) 1.065 1_555 1_555 no C(21) H(29) 0.989 1_555 1_555 no C(21) H(30) 0.963 1_555 1_555 no C(22) H(31) 1.088 1_555 1_555 no C(22) H(32) 1.102 1_555 1_555 no C(23) H(33) 1.086 1_555 1_555 no C(23) H(34) 1.074 1_555 1_555 no C(24) H(35) 0.971 1_555 1_555 no C(24) H(36) 1.004 1_555 1_555 no C(25) H(37) 1.050 1_555 1_555 no C(25) H(38) 1.044 1_555 1_555 no C(26) H(39) 1.001 1_555 1_555 no C(26) H(40) 1.098 1_555 1_555 no C(27) H(41) 0.982 1_555 1_555 no C(27) H(42) 1.043 1_555 1_555 no C(28) H(43) 1.137 1_555 1_555 no C(28) H(44) 1.093 1_555 1_555 no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Co N(3) 92.88(8) 1_555 1_555 1_555 yes N(1) Co N(4) 177.43(8) 1_555 1_555 1_555 yes N(1) Co N(6) 88.23(8) 1_555 1_555 1_555 yes N(3) Co N(4) 85.81(8) 1_555 1_555 1_555 yes N(3) Co N(6) 178.22(8) 1_555 1_555 1_555 yes N(4) Co N(6) 93.13(8) 1_555 1_555 1_555 yes O(5) K O(6) 58.37(6) 1_555 1_555 1_555 yes O(5) K O(7) 98.26(6) 1_555 1_555 1_555 yes O(5) K O(8) 137.51(7) 1_555 1_555 1_555 yes O(5) K O(9) 95.79(6) 1_555 1_555 1_555 yes O(5) K O(10) 113.32(7) 1_555 1_555 1_555 yes O(5) K N(7) 60.47(6) 1_555 1_555 1_555 yes O(5) K N(8) 116.50(7) 1_555 1_555 1_555 yes O(6) K O(7) 115.88(7) 1_555 1_555 1_555 yes O(6) K O(8) 95.86(6) 1_555 1_555 1_555 yes O(6) K O(9) 135.39(6) 1_555 1_555 1_555 yes O(6) K O(10) 94.48(7) 1_555 1_555 1_555 yes O(6) K N(7) 117.47(6) 1_555 1_555 1_555 yes O(6) K N(8) 59.46(7) 1_555 1_555 1_555 yes O(7) K O(8) 60.72(6) 1_555 1_555 1_555 yes O(7) K O(9) 102.48(6) 1_555 1_555 1_555 yes O(7) K O(10) 144.82(6) 1_555 1_555 1_555 yes O(7) K N(7) 61.84(7) 1_555 1_555 1_555 yes O(7) K N(8) 119.14(8) 1_555 1_555 1_555 yes O(8) K O(9) 123.46(6) 1_555 1_555 1_555 yes O(8) K O(10) 100.89(7) 1_555 1_555 1_555 yes O(8) K N(7) 121.67(7) 1_555 1_555 1_555 yes O(8) K N(8) 59.91(7) 1_555 1_555 1_555 yes O(9) K O(10) 60.77(7) 1_555 1_555 1_555 yes O(9) K N(7) 61.59(7) 1_555 1_555 1_555 yes O(9) K N(8) 120.19(8) 1_555 1_555 1_555 yes O(10) K N(7) 120.69(8) 1_555 1_555 1_555 yes O(10) K N(8) 60.47(8) 1_555 1_555 1_555 yes N(7) K N(8) 176.92(7) 1_555 1_555 1_555 yes K O(5) C(12) 114.9(2) 1_555 1_555 1_555 yes K O(5) C(13) 115.3(2) 1_555 1_555 1_555 yes C(12) O(5) C(13) 109.0(3) 1_555 1_555 1_555 yes K O(6) C(14) 115.5(2) 1_555 1_555 1_555 yes K O(6) C(15) 118.1(2) 1_555 1_555 1_555 yes C(14) O(6) C(15) 109.5(3) 1_555 1_555 1_555 yes K O(7) C(18) 115.2(2) 1_555 1_555 1_555 yes K O(7) C(19) 112.7(2) 1_555 1_555 1_555 yes C(18) O(7) C(19) 111.6(2) 1_555 1_555 1_555 yes K O(8) C(20) 111.9(2) 1_555 1_555 1_555 yes K O(8) C(21) 117.5(2) 1_555 1_555 1_555 yes C(20) O(8) C(21) 113.4(3) 1_555 1_555 1_555 yes K O(9) C(24) 115.4(2) 1_555 1_555 1_555 yes K O(9) C(25) 109.6(2) 1_555 1_555 1_555 yes C(24) O(9) C(25) 112.8(3) 1_555 1_555 1_555 yes K O(10) C(26) 115.8(2) 1_555 1_555 1_555 yes K O(10) C(27) 117.1(2) 1_555 1_555 1_555 yes C(26) O(10) C(27) 112.1(3) 1_555 1_555 1_555 yes Co N(1) C(1) 130.9(2) 1_555 1_555 1_555 yes C(1) N(2) C(2) 131.1(2) 1_555 1_555 1_555 yes Co N(3) C(2) 127.5(1) 1_555 1_555 1_555 yes Co N(3) C(3) 113.3(1) 1_555 1_555 1_555 yes C(2) N(3) C(3) 118.5(2) 1_555 1_555 1_555 yes Co N(4) C(8) 113.2(1) 1_555 1_555 1_555 yes Co N(4) C(9) 126.6(2) 1_555 1_555 1_555 yes C(8) N(4) C(9) 119.4(2) 1_555 1_555 1_555 yes C(9) N(5) C(10) 131.5(2) 1_555 1_555 1_555 yes Co N(6) C(10) 130.6(2) 1_555 1_555 1_555 yes K N(7) C(11) 110.0(2) 1_555 1_555 1_555 yes K N(7) C(17) 108.5(2) 1_555 1_555 1_555 yes K N(7) C(23) 107.8(2) 1_555 1_555 1_555 yes C(11) N(7) C(17) 110.0(3) 1_555 1_555 1_555 yes C(11) N(7) C(23) 110.4(2) 1_555 1_555 1_555 yes C(17) N(7) C(23) 110.0(3) 1_555 1_555 1_555 yes K N(8) C(16) 109.9(2) 1_555 1_555 1_555 yes K N(8) C(22) 108.3(2) 1_555 1_555 1_555 yes K N(8) C(28) 109.4(2) 1_555 1_555 1_555 yes C(16) N(8) C(22) 109.7(3) 1_555 1_555 1_555 yes C(16) N(8) C(28) 109.8(3) 1_555 1_555 1_555 yes C(22) N(8) C(28) 109.6(3) 1_555 1_555 1_555 yes O(1) C(1) N(1) 125.0(2) 1_555 1_555 1_555 yes O(1) C(1) N(2) 117.1(2) 1_555 1_555 1_555 yes N(1) C(1) N(2) 117.9(2) 1_555 1_555 1_555 yes O(2) C(2) N(2) 115.9(2) 1_555 1_555 1_555 yes O(2) C(2) N(3) 126.1(2) 1_555 1_555 1_555 yes N(2) C(2) N(3) 118.0(2) 1_555 1_555 1_555 yes N(3) C(3) C(4) 126.6(2) 1_555 1_555 1_555 yes N(3) C(3) C(8) 113.5(2) 1_555 1_555 1_555 yes C(4) C(3) C(8) 119.9(2) 1_555 1_555 1_555 yes C(3) C(4) C(5) 119.8(2) 1_555 1_555 1_555 yes C(4) C(5) C(6) 120.3(2) 1_555 1_555 1_555 yes C(5) C(6) C(7) 120.9(2) 1_555 1_555 1_555 yes C(6) C(7) C(8) 119.9(2) 1_555 1_555 1_555 yes N(4) C(8) C(3) 113.6(2) 1_555 1_555 1_555 yes N(4) C(8) C(7) 127.4(2) 1_555 1_555 1_555 yes C(3) C(8) C(7) 119.0(2) 1_555 1_555 1_555 yes O(3) C(9) N(4) 124.4(2) 1_555 1_555 1_555 yes O(3) C(9) N(5) 117.8(2) 1_555 1_555 1_555 yes N(4) C(9) N(5) 117.8(2) 1_555 1_555 1_555 yes O(4) C(10) N(5) 118.7(2) 1_555 1_555 1_555 yes O(4) C(10) N(6) 123.8(2) 1_555 1_555 1_555 yes N(5) C(10) N(6) 117.6(2) 1_555 1_555 1_555 yes N(7) C(11) C(12) 113.3(3) 1_555 1_555 1_555 yes O(5) C(12) C(11) 108.3(3) 1_555 1_555 1_555 yes O(5) C(13) C(14) 109.8(3) 1_555 1_555 1_555 yes O(6) C(14) C(13) 109.3(3) 1_555 1_555 1_555 yes O(6) C(15) C(16) 109.3(3) 1_555 1_555 1_555 yes N(8) C(16) C(15) 114.7(3) 1_555 1_555 1_555 yes N(7) C(17) C(18) 114.4(2) 1_555 1_555 1_555 yes O(7) C(18) C(17) 109.6(3) 1_555 1_555 1_555 yes O(7) C(19) C(20) 109.3(2) 1_555 1_555 1_555 yes O(8) C(20) C(19) 109.1(2) 1_555 1_555 1_555 yes O(8) C(21) C(22) 109.6(3) 1_555 1_555 1_555 yes N(8) C(22) C(21) 114.0(3) 1_555 1_555 1_555 yes N(7) C(23) C(24) 114.5(3) 1_555 1_555 1_555 yes O(9) C(24) C(23) 110.1(2) 1_555 1_555 1_555 yes O(9) C(25) C(26) 109.4(3) 1_555 1_555 1_555 yes O(10) C(26) C(25) 110.8(3) 1_555 1_555 1_555 yes O(10) C(27) C(28) 110.2(3) 1_555 1_555 1_555 yes N(8) C(28) C(27) 113.8(3) 1_555 1_555 1_555 yes Co N(1) H(1) 122.6 1_555 1_555 1_555 no C(1) N(1) H(1) 105.8 1_555 1_555 1_555 no C(1) N(2) H(2) 117.7 1_555 1_555 1_555 no C(2) N(2) H(2) 111.0 1_555 1_555 1_555 no C(9) N(5) H(7) 111.1 1_555 1_555 1_555 no C(10) N(5) H(7) 117.3 1_555 1_555 1_555 no Co N(6) H(8) 119.5 1_555 1_555 1_555 no C(10) N(6) H(8) 109.6 1_555 1_555 1_555 no C(3) C(4) H(3) 120.1 1_555 1_555 1_555 no C(5) C(4) H(3) 119.7 1_555 1_555 1_555 no C(4) C(5) H(4) 119.4 1_555 1_555 1_555 no C(6) C(5) H(4) 120.3 1_555 1_555 1_555 no C(5) C(6) H(5) 117.1 1_555 1_555 1_555 no C(7) C(6) H(5) 121.7 1_555 1_555 1_555 no C(6) C(7) H(6) 120.1 1_555 1_555 1_555 no C(8) C(7) H(6) 119.5 1_555 1_555 1_555 no N(7) C(11) H(9) 116.9 1_555 1_555 1_555 no N(7) C(11) H(10) 105.9 1_555 1_555 1_555 no C(12) C(11) H(9) 109.8 1_555 1_555 1_555 no C(12) C(11) H(10) 109.1 1_555 1_555 1_555 no H(9) C(11) H(10) 100.8 1_555 1_555 1_555 no O(5) C(12) H(11) 113.0 1_555 1_555 1_555 no O(5) C(12) H(12) 104.8 1_555 1_555 1_555 no C(11) C(12) H(11) 112.5 1_555 1_555 1_555 no C(11) C(12) H(12) 109.6 1_555 1_555 1_555 no H(11) C(12) H(12) 108.3 1_555 1_555 1_555 no O(5) C(13) H(13) 115.8 1_555 1_555 1_555 no O(5) C(13) H(14) 109.0 1_555 1_555 1_555 no C(14) C(13) H(13) 102.5 1_555 1_555 1_555 no C(14) C(13) H(14) 112.3 1_555 1_555 1_555 no H(13) C(13) H(14) 107.3 1_555 1_555 1_555 no O(6) C(14) H(15) 110.2 1_555 1_555 1_555 no O(6) C(14) H(16) 108.6 1_555 1_555 1_555 no C(13) C(14) H(15) 100.9 1_555 1_555 1_555 no C(13) C(14) H(16) 105.0 1_555 1_555 1_555 no H(15) C(14) H(16) 122.1 1_555 1_555 1_555 no O(6) C(15) H(17) 118.6 1_555 1_555 1_555 no O(6) C(15) H(18) 111.5 1_555 1_555 1_555 no C(16) C(15) H(17) 108.5 1_555 1_555 1_555 no C(16) C(15) H(18) 97.3 1_555 1_555 1_555 no H(17) C(15) H(18) 109.5 1_555 1_555 1_555 no N(8) C(16) H(19) 111.8 1_555 1_555 1_555 no N(8) C(16) H(20) 108.9 1_555 1_555 1_555 no C(15) C(16) H(19) 111.1 1_555 1_555 1_555 no C(15) C(16) H(20) 106.6 1_555 1_555 1_555 no H(19) C(16) H(20) 102.9 1_555 1_555 1_555 no N(7) C(17) H(21) 108.9 1_555 1_555 1_555 no N(7) C(17) H(22) 112.0 1_555 1_555 1_555 no C(18) C(17) H(21) 114.2 1_555 1_555 1_555 no C(18) C(17) H(22) 108.2 1_555 1_555 1_555 no H(21) C(17) H(22) 98.0 1_555 1_555 1_555 no O(7) C(18) H(23) 115.1 1_555 1_555 1_555 no O(7) C(18) H(24) 110.9 1_555 1_555 1_555 no C(17) C(18) H(23) 99.2 1_555 1_555 1_555 no C(17) C(18) H(24) 114.1 1_555 1_555 1_555 no H(23) C(18) H(24) 107.5 1_555 1_555 1_555 no O(7) C(19) H(25) 110.8 1_555 1_555 1_555 no O(7) C(19) H(26) 109.3 1_555 1_555 1_555 no C(20) C(19) H(25) 110.7 1_555 1_555 1_555 no C(20) C(19) H(26) 111.3 1_555 1_555 1_555 no H(25) C(19) H(26) 105.3 1_555 1_555 1_555 no O(8) C(20) H(27) 103.6 1_555 1_555 1_555 no O(8) C(20) H(28) 111.7 1_555 1_555 1_555 no C(19) C(20) H(27) 121.3 1_555 1_555 1_555 no C(19) C(20) H(28) 108.5 1_555 1_555 1_555 no H(27) C(20) H(28) 102.4 1_555 1_555 1_555 no O(8) C(21) H(29) 109.6 1_555 1_555 1_555 no O(8) C(21) H(30) 111.6 1_555 1_555 1_555 no C(22) C(21) H(29) 108.4 1_555 1_555 1_555 no C(22) C(21) H(30) 112.3 1_555 1_555 1_555 no H(29) C(21) H(30) 105.2 1_555 1_555 1_555 no N(8) C(22) H(31) 111.9 1_555 1_555 1_555 no N(8) C(22) H(32) 108.3 1_555 1_555 1_555 no C(21) C(22) H(31) 108.3 1_555 1_555 1_555 no C(21) C(22) H(32) 114.4 1_555 1_555 1_555 no H(31) C(22) H(32) 99.2 1_555 1_555 1_555 no N(7) C(23) H(33) 109.3 1_555 1_555 1_555 no N(7) C(23) H(34) 108.9 1_555 1_555 1_555 no C(24) C(23) H(33) 104.0 1_555 1_555 1_555 no C(24) C(23) H(34) 108.5 1_555 1_555 1_555 no H(33) C(23) H(34) 111.5 1_555 1_555 1_555 no O(9) C(24) H(35) 112.7 1_555 1_555 1_555 no O(9) C(24) H(36) 116.9 1_555 1_555 1_555 no C(23) C(24) H(35) 103.8 1_555 1_555 1_555 no C(23) C(24) H(36) 104.4 1_555 1_555 1_555 no H(35) C(24) H(36) 107.7 1_555 1_555 1_555 no O(9) C(25) H(37) 108.2 1_555 1_555 1_555 no O(9) C(25) H(38) 112.2 1_555 1_555 1_555 no C(26) C(25) H(37) 106.8 1_555 1_555 1_555 no C(26) C(25) H(38) 101.7 1_555 1_555 1_555 no H(37) C(25) H(38) 118.0 1_555 1_555 1_555 no O(10) C(26) H(39) 102.3 1_555 1_555 1_555 no O(10) C(26) H(40) 105.5 1_555 1_555 1_555 no C(25) C(26) H(39) 124.2 1_555 1_555 1_555 no C(25) C(26) H(40) 111.0 1_555 1_555 1_555 no H(39) C(26) H(40) 101.3 1_555 1_555 1_555 no O(10) C(27) H(41) 106.7 1_555 1_555 1_555 no O(10) C(27) H(42) 122.7 1_555 1_555 1_555 no C(28) C(27) H(41) 120.7 1_555 1_555 1_555 no C(28) C(27) H(42) 102.9 1_555 1_555 1_555 no H(41) C(27) H(42) 93.8 1_555 1_555 1_555 no N(8) C(28) H(43) 102.5 1_555 1_555 1_555 no N(8) C(28) H(44) 103.7 1_555 1_555 1_555 no C(27) C(28) H(43) 123.2 1_555 1_555 1_555 no C(27) C(28) H(44) 113.6 1_555 1_555 1_555 no H(43) C(28) H(44) 97.3 1_555 1_555 1_555 no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) N(1) 2.934(2) 1_555 3_655 ? O(1) N(6) 3.103(2) 1_555 3_655 ? O(4) N(5) 2.915(2) 1_555 3_555 ? O(9) N(2) 3.097(3) 1_555 1_555 ? #------------------------------------------------------------------------------ #===END data_[PPh4]2[Co(bbphen)(CN)] _database_code_CSD 169289 #------------------------------------------------------------------------------ _audit_creation_date 'Sat Feb 20 14:20:32 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'SHELXS86' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics 'ORTEP in teXsan' #------------------------------------------------------------------------------ _chemical_compound_source ; Prepared from PPh~4~[Co(bbphen)], PPh~4~Cl, and excess of KCN in refluxing chloroform, recrystallized from acetonitrile. ; _chemical_name_systematic ; Tetraphenylphosphonium Cyano(o-phenylenebis(biuretato))cobaltate(III) Diacetonitrile Unihydrate Solvate ; _chemical_name_common '(PPh~4~)~2~[Co(bbphen)(CN)].2CH~3~CN.H~2~O' _chemical_formula_weight 1140.07 _chemical_formula_analytical 'C63 H56 Co N9 O5 P2 ' _chemical_formula_sum 'C63 H56 Co N9 O5 P2 ' _chemical_formula_moiety '2(C24 H20 P 1+) C11 H8 N7 O4 Co 2-,2(C2 H3 N),H2 O' _chemical_formula_structural '2(P(C6 H5)4),(Co (C10 H8 N6 O4)(C N)),2(C2 H3 N),(H2 O)' _chemical_melting_point 485 #------------------------------------------------------------------------------ _cell_length_a 13.579(3) _cell_length_b 16.696(5) _cell_length_c 13.047(4) _cell_angle_alpha 96.82(3) _cell_angle_beta 101.26(2) _cell_angle_gamma 101.25(2) _cell_volume 2807(1) _cell_formula_units_Z 2 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.0 _cell_measurement_theta_max 12.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1188.00 _exptl_absorpt_coefficient_mu 0.422 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.930 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details 'none' #------------------------------------------------------------------------------ _diffrn_special_details ; \q scan width (0.945 + 0.350tan\q)\%, \w scan rate 8\% per min. Background counts for 25% time on each side every scan. ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.10 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 -4 0 -3 0 -1 0 -1 -3 _diffrn_reflns_number 10812 _reflns_number_total 10442 _reflns_number_gt 4352 _reflns_observed_expression 'F^2^ 2 \s(F^2^)' _diffrn_reflns_av_R_equivalents 0.134 _diffrn_reflns_av_sigmaI/netI 0.234 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.04280 _diffrn_orient_matrix_UB_12 -0.02581 _diffrn_orient_matrix_UB_13 -0.07206 _diffrn_orient_matrix_UB_21 0.04937 _diffrn_orient_matrix_UB_22 -0.03629 _diffrn_orient_matrix_UB_23 -0.00845 _diffrn_orient_matrix_UB_31 -0.04083 _diffrn_orient_matrix_UB_32 -0.04299 _diffrn_orient_matrix_UB_33 0.03179 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'Co' 'Co' 0.349 0.972 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'C' 'C' 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'P' 'P' 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.26266(6) 0.25913(5) 0.05275(7) 0.0287(2) Uani 1.00 d . . . P(1) P 0.1221(1) 0.6826(1) 0.5647(1) 0.0410(6) Uani 1.00 d . . . P(2) P 0.3233(1) 0.1989(1) 0.6348(1) 0.0434(6) Uani 1.00 d . . . O(1) O 0.5119(3) 0.4010(2) -0.0154(3) 0.041(1) Uani 1.00 d . . . O(2) O 0.2362(4) 0.4962(3) 0.0287(5) 0.070(2) Uani 1.00 d . . . O(3) O -0.0140(3) 0.0964(2) -0.0063(4) 0.062(2) Uani 1.00 d . . . O(4) O 0.2864(3) 0.0187(3) 0.0538(4) 0.057(2) Uani 1.00 d . . . O(5) O 0.7986(4) 0.1191(3) 0.8646(4) 0.067(2) Uani 1.00 d . . . N(1) N 0.3839(4) 0.3011(3) 0.0094(4) 0.036(2) Uani 1.00 d . . . N(2) N 0.3675(4) 0.4371(3) 0.0135(4) 0.036(2) Uani 1.00 d . . . N(3) N 0.2115(4) 0.3564(3) 0.0368(4) 0.031(2) Uani 1.00 d . . . N(4) N 0.1246(3) 0.2082(3) 0.0495(4) 0.029(1) Uani 1.00 d . . . N(5) N 0.1424(4) 0.0701(3) 0.0284(4) 0.037(2) Uani 1.00 d . . . N(6) N 0.3025(4) 0.1577(3) 0.0495(4) 0.037(2) Uani 1.00 d . . . N(7) N 0.3546(4) 0.3206(4) 0.2820(5) 0.052(2) Uani 1.00 d . . . N(8) N 0.5855(6) 0.2038(5) 0.0880(6) 0.093(3) Uani 1.00 d . . . N(9) N 0.5997(7) 0.1173(6) 0.4586(8) 0.120(4) Uani 1.00 d . . . C(1) C 0.4244(5) 0.3784(4) 0.0024(5) 0.032(2) Uani 1.00 d . . . C(2) C 0.2676(5) 0.4319(4) 0.0267(5) 0.041(2) Uani 1.00 d . . . C(3) C 0.1096(4) 0.3471(3) 0.0480(5) 0.030(2) Uani 1.00 d . . . C(4) C 0.0519(5) 0.4086(4) 0.0509(5) 0.039(2) Uani 1.00 d . . . C(5) C -0.0470(5) 0.3895(4) 0.0665(5) 0.044(2) Uani 1.00 d . . . C(6) C -0.0906(5) 0.3106(4) 0.0796(5) 0.041(2) Uani 1.00 d . . . C(7) C -0.0371(5) 0.2494(4) 0.0742(5) 0.037(2) Uani 1.00 d . . . C(8) C 0.0627(5) 0.2654(4) 0.0560(5) 0.030(2) Uani 1.00 d . . . C(9) C 0.0811(5) 0.1261(4) 0.0229(5) 0.035(2) Uani 1.00 d . . . C(10) C 0.2495(5) 0.0817(4) 0.0459(5) 0.035(2) Uani 1.00 d . . . C(11) C 0.3180(5) 0.2944(4) 0.1935(6) 0.035(2) Uani 1.00 d . . . C(12) C 0.2722(5) 0.1413(4) 0.5061(5) 0.047(2) Uani 1.00 d . . . C(13) C 0.2807(6) 0.0602(4) 0.4801(6) 0.054(3) Uani 1.00 d . . . C(14) C 0.2366(6) 0.0163(4) 0.3813(7) 0.065(3) Uani 1.00 d . . . C(15) C 0.1832(7) 0.0518(5) 0.3037(6) 0.070(3) Uani 1.00 d . . . C(16) C 0.1746(6) 0.1324(5) 0.3281(6) 0.068(3) Uani 1.00 d . . . C(17) C 0.2158(6) 0.1761(4) 0.4273(6) 0.058(2) Uani 1.00 d . . . C(18) C 0.4103(5) 0.2947(4) 0.6354(5) 0.046(2) Uani 1.00 d . . . C(19) C 0.4289(5) 0.3216(4) 0.5416(5) 0.051(2) Uani 1.00 d . . . C(20) C 0.5004(6) 0.3955(5) 0.5486(6) 0.061(3) Uani 1.00 d . . . C(21) C 0.5510(6) 0.4402(5) 0.6456(7) 0.070(3) Uani 1.00 d . . . C(22) C 0.5352(6) 0.4136(5) 0.7400(6) 0.068(3) Uani 1.00 d . . . C(23) C 0.4639(6) 0.3399(4) 0.7327(5) 0.052(2) Uani 1.00 d . . . C(24) C 0.2171(5) 0.2180(4) 0.6900(5) 0.044(2) Uani 1.00 d . . . C(25) C 0.2130(6) 0.2933(5) 0.7411(6) 0.057(3) Uani 1.00 d . . . C(26) C 0.1300(8) 0.3030(6) 0.7840(7) 0.078(4) Uani 1.00 d . . . C(27) C 0.0511(7) 0.2363(8) 0.7772(7) 0.082(4) Uani 1.00 d . . . C(28) C 0.0511(7) 0.1602(7) 0.7239(8) 0.089(4) Uani 1.00 d . . . C(29) C 0.1342(6) 0.1513(5) 0.6793(7) 0.071(3) Uani 1.00 d . . . C(30) C 0.3946(5) 0.1411(4) 0.7151(5) 0.038(2) Uani 1.00 d . . . C(31) C 0.3653(5) 0.1149(4) 0.8047(5) 0.047(2) Uani 1.00 d . . . C(32) C 0.4259(6) 0.0705(5) 0.8643(6) 0.058(3) Uani 1.00 d . . . C(33) C 0.5118(6) 0.0538(5) 0.8353(7) 0.068(3) Uani 1.00 d . . . C(34) C 0.5415(6) 0.0789(5) 0.7471(6) 0.066(3) Uani 1.00 d . . . C(35) C 0.4831(6) 0.1237(5) 0.6864(6) 0.055(3) Uani 1.00 d . . . C(36) C 0.2075(5) 0.6310(4) 0.6424(5) 0.042(2) Uani 1.00 d . . . C(37) C 0.1759(5) 0.5874(4) 0.7195(5) 0.050(2) Uani 1.00 d . . . C(38) C 0.2473(6) 0.5562(5) 0.7864(5) 0.057(3) Uani 1.00 d . . . C(39) C 0.3482(6) 0.5697(5) 0.7740(6) 0.065(3) Uani 1.00 d . . . C(40) C 0.3789(5) 0.6121(5) 0.6984(7) 0.062(3) Uani 1.00 d . . . C(41) C 0.3083(5) 0.6430(4) 0.6336(6) 0.057(3) Uani 1.00 d . . . C(42) C 0.1466(5) 0.6722(4) 0.4352(5) 0.045(2) Uani 1.00 d . . . C(43) C 0.1313(6) 0.5930(4) 0.3789(6) 0.057(3) Uani 1.00 d . . . C(44) C 0.1511(7) 0.5824(5) 0.2794(6) 0.069(3) Uani 1.00 d . . . C(45) C 0.1868(7) 0.6485(6) 0.2350(7) 0.082(3) Uani 1.00 d . . . C(46) C 0.2045(7) 0.7285(6) 0.2896(7) 0.075(3) Uani 1.00 d . . . C(47) C 0.1846(6) 0.7417(5) 0.3912(6) 0.061(3) Uani 1.00 d . . . C(48) C 0.1435(5) 0.7862(4) 0.6275(6) 0.047(2) Uani 1.00 d . . . C(49) C 0.0786(6) 0.8365(5) 0.5868(7) 0.069(3) Uani 1.00 d . . . C(50) C 0.0841(7) 0.9133(5) 0.6454(10) 0.092(4) Uani 1.00 d . . . C(51) C 0.1505(8) 0.9396(5) 0.7414(9) 0.091(4) Uani 1.00 d . . . C(52) C 0.2143(7) 0.8926(5) 0.7800(7) 0.080(3) Uani 1.00 d . . . C(53) C 0.2126(6) 0.8159(4) 0.7237(6) 0.060(3) Uani 1.00 d . . . C(54) C -0.0120(5) 0.6407(4) 0.5588(5) 0.039(2) Uani 1.00 d . . . C(55) C -0.0823(5) 0.6042(4) 0.4661(5) 0.044(2) Uani 1.00 d . . . C(56) C -0.1850(5) 0.5811(4) 0.4679(6) 0.049(2) Uani 1.00 d . . . C(57) C -0.2170(5) 0.5913(4) 0.5604(7) 0.054(3) Uani 1.00 d . . . C(58) C -0.1479(6) 0.6267(5) 0.6539(6) 0.052(3) Uani 1.00 d . . . C(59) C -0.0459(5) 0.6522(4) 0.6526(5) 0.046(2) Uani 1.00 d . . . C(60) C 0.6522(6) 0.2729(6) -0.0581(6) 0.079(3) Uani 1.00 d . . . C(61) C 0.6159(6) 0.2329(6) 0.0208(8) 0.076(3) Uani 1.00 d . . . C(62) C 0.4725(7) 0.1480(5) 0.2991(7) 0.083(3) Uani 1.00 d . . . C(63) C 0.5416(8) 0.1336(6) 0.3872(9) 0.089(4) Uani 1.00 d . . . H(1) H 0.4223 0.2608 -0.0119 0.0442 Uiso 1.00 calc . . . H(2) H 0.4040 0.4928 0.0106 0.0433 Uiso 1.00 calc . . . H(3) H 0.0849 0.4719 0.0482 0.0629 Uiso 1.00 calc . . . H(4) H -0.0868 0.4326 0.0670 0.0517 Uiso 1.00 calc . . . H(5) H -0.1593 0.2992 0.0940 0.0495 Uiso 1.00 calc . . . H(6) H -0.0694 0.1934 0.0822 0.0458 Uiso 1.00 calc . . . H(7) H 0.1064 0.0128 0.0187 0.0432 Uiso 1.00 calc . . . H(8) H 0.3758 0.1611 0.0515 0.0459 Uiso 1.00 calc . . . H(9) H 0.3148 0.0266 0.5514 0.0629 Uiso 1.00 calc . . . H(10) H 0.2426 -0.0418 0.3651 0.0802 Uiso 1.00 calc . . . H(11) H 0.1526 0.0201 0.2318 0.0836 Uiso 1.00 calc . . . H(12) H 0.1378 0.1588 0.2728 0.0793 Uiso 1.00 calc . . . H(13) H 0.2077 0.2332 0.4437 0.0718 Uiso 1.00 calc . . . H(14) H 0.3924 0.2888 0.4716 0.0613 Uiso 1.00 calc . . . H(15) H 0.5078 0.4103 0.4741 0.0629 Uiso 1.00 calc . . . H(16) H 0.6006 0.4931 0.6499 0.0804 Uiso 1.00 calc . . . H(17) H 0.5565 0.4663 0.8169 0.0629 Uiso 1.00 calc . . . H(18) H 0.4644 0.3173 0.8036 0.0629 Uiso 1.00 calc . . . H(19) H 0.2705 0.3419 0.7470 0.0723 Uiso 1.00 calc . . . H(20) H 0.1259 0.3582 0.8198 0.0951 Uiso 1.00 calc . . . H(21) H -0.0059 0.2434 0.8109 0.0979 Uiso 1.00 calc . . . H(22) H -0.0061 0.1137 0.7183 0.1069 Uiso 1.00 calc . . . H(23) H 0.1339 0.0970 0.6404 0.0913 Uiso 1.00 calc . . . H(24) H 0.2897 0.1268 0.8246 0.0629 Uiso 1.00 calc . . . H(25) H 0.4059 0.0519 0.9277 0.0685 Uiso 1.00 calc . . . H(26) H 0.5539 0.0230 0.8774 0.0808 Uiso 1.00 calc . . . H(27) H 0.6040 0.0666 0.7275 0.0766 Uiso 1.00 calc . . . H(28) H 0.5046 0.1428 0.6227 0.0658 Uiso 1.00 calc . . . H(29) H 0.1043 0.5793 0.7277 0.0636 Uiso 1.00 calc . . . H(30) H 0.2202 0.5242 0.8456 0.0629 Uiso 1.00 calc . . . H(31) H 0.3992 0.5467 0.8191 0.0762 Uiso 1.00 calc . . . H(32) H 0.4503 0.6202 0.6902 0.0762 Uiso 1.00 calc . . . H(33) H 0.3299 0.6752 0.5801 0.0668 Uiso 1.00 calc . . . H(34) H 0.1068 0.5444 0.4105 0.0668 Uiso 1.00 calc . . . H(35) H 0.1376 0.5263 0.2372 0.0818 Uiso 1.00 calc . . . H(36) H 0.2038 0.6409 0.1652 0.0961 Uiso 1.00 calc . . . H(37) H 0.2307 0.7761 0.2570 0.0879 Uiso 1.00 calc . . . H(38) H 0.1966 0.7986 0.4317 0.0774 Uiso 1.00 calc . . . H(39) H 0.0293 0.8160 0.5169 0.0835 Uiso 1.00 calc . . . H(40) H 0.0381 0.9488 0.6151 0.1056 Uiso 1.00 calc . . . H(41) H 0.1495 0.9917 0.7828 0.1112 Uiso 1.00 calc . . . H(42) H 0.2637 0.9138 0.8490 0.0948 Uiso 1.00 calc . . . H(43) H 0.2606 0.7820 0.7517 0.0753 Uiso 1.00 calc . . . H(44) H -0.0593 0.5937 0.3997 0.0546 Uiso 1.00 calc . . . H(45) H -0.2356 0.5573 0.4016 0.0607 Uiso 1.00 calc . . . H(46) H -0.2986 0.5749 0.5495 0.0629 Uiso 1.00 calc . . . H(47) H -0.1721 0.6337 0.7205 0.0647 Uiso 1.00 calc . . . H(48) H 0.0050 0.6790 0.7191 0.0574 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co 0.0262(5) 0.0251(5) 0.0371(6) 0.0038(4) 0.0085(4) 0.0148(4) P(1) 0.040(1) 0.045(1) 0.040(1) 0.0103(9) 0.0081(9) 0.0150(9) P(2) 0.046(1) 0.044(1) 0.041(1) 0.0101(9) 0.0051(9) 0.0169(9) O(1) 0.036(3) 0.035(3) 0.057(3) 0.002(2) 0.024(2) 0.017(2) O(2) 0.056(3) 0.030(3) 0.139(5) 0.017(3) 0.037(3) 0.037(3) O(3) 0.027(3) 0.027(3) 0.119(5) -0.001(2) -0.004(3) 0.013(3) O(4) 0.037(3) 0.035(3) 0.112(4) 0.016(2) 0.027(3) 0.035(3) O(5) 0.062(3) 0.061(3) 0.077(4) 0.006(3) 0.001(3) 0.041(3) N(1) 0.031(3) 0.029(3) 0.056(4) 0.010(2) 0.022(3) 0.018(3) N(2) 0.036(3) 0.027(3) 0.052(4) 0.004(2) 0.018(3) 0.019(3) N(3) 0.028(3) 0.024(3) 0.046(3) 0.007(2) 0.014(3) 0.014(2) N(4) 0.023(3) 0.024(3) 0.040(3) 0.003(2) 0.006(2) 0.009(2) N(5) 0.028(3) 0.026(3) 0.059(4) 0.004(2) 0.008(3) 0.016(3) N(6) 0.030(3) 0.023(3) 0.063(4) 0.002(2) 0.024(3) 0.013(3) N(7) 0.049(4) 0.073(4) 0.036(4) 0.017(3) 0.009(3) 0.015(3) N(8) 0.069(6) 0.128(7) 0.085(6) 0.027(5) 0.015(5) 0.026(5) N(9) 0.102(8) 0.130(8) 0.110(8) 0.002(6) -0.002(6) 0.036(6) C(1) 0.028(4) 0.036(4) 0.034(4) 0.002(3) 0.009(3) 0.011(3) C(2) 0.037(4) 0.033(4) 0.053(5) 0.002(3) 0.009(3) 0.017(3) C(3) 0.029(4) 0.028(3) 0.031(4) 0.007(3) 0.004(3) 0.009(3) C(4) 0.048(4) 0.030(4) 0.045(4) 0.014(3) 0.012(3) 0.016(3) C(5) 0.038(4) 0.056(5) 0.049(5) 0.024(4) 0.012(4) 0.022(4) C(6) 0.026(4) 0.051(4) 0.051(5) 0.014(3) 0.013(3) 0.008(4) C(7) 0.032(4) 0.034(4) 0.044(4) 0.001(3) 0.013(3) 0.009(3) C(8) 0.032(4) 0.035(4) 0.029(4) 0.013(3) 0.008(3) 0.012(3) C(9) 0.033(4) 0.028(4) 0.042(4) 0.003(3) 0.006(3) 0.012(3) C(10) 0.026(4) 0.036(4) 0.040(4) 0.004(3) -0.001(3) 0.020(3) C(11) 0.035(4) 0.040(4) 0.041(5) 0.017(3) 0.017(3) 0.018(3) C(12) 0.050(5) 0.039(4) 0.046(5) 0.003(3) 0.003(4) 0.010(4) C(13) 0.068(6) 0.047(5) 0.045(5) 0.009(4) 0.013(4) 0.010(4) C(14) 0.079(6) 0.046(5) 0.068(6) 0.008(4) 0.016(5) 0.006(5) C(15) 0.088(7) 0.067(6) 0.039(5) -0.014(5) 0.013(5) -0.002(5) C(16) 0.071(6) 0.081(6) 0.037(5) 0.004(5) -0.012(4) 0.014(5) C(17) 0.063(5) 0.049(5) 0.049(5) 0.004(4) -0.014(4) 0.013(4) C(18) 0.054(5) 0.043(4) 0.038(4) 0.007(3) 0.007(4) 0.013(4) C(19) 0.052(5) 0.059(5) 0.045(5) 0.015(4) 0.009(4) 0.018(4) C(20) 0.064(5) 0.077(6) 0.042(5) 0.004(4) 0.011(4) 0.026(4) C(21) 0.075(6) 0.060(5) 0.066(6) -0.016(4) 0.021(5) 0.016(5) C(22) 0.086(6) 0.057(5) 0.049(5) -0.001(5) 0.002(5) 0.009(4) C(23) 0.063(5) 0.053(5) 0.032(4) 0.006(4) -0.001(4) 0.010(4) C(24) 0.043(4) 0.054(5) 0.037(4) 0.014(4) 0.001(3) 0.026(4) C(25) 0.070(6) 0.070(6) 0.035(5) 0.030(5) 0.004(4) 0.011(4) C(26) 0.086(7) 0.109(8) 0.053(6) 0.052(6) 0.008(5) 0.024(5) C(27) 0.069(7) 0.142(10) 0.051(6) 0.048(7) 0.018(5) 0.032(6) C(28) 0.052(6) 0.112(8) 0.109(9) 0.011(6) 0.029(6) 0.043(7) C(29) 0.048(5) 0.073(6) 0.095(7) 0.017(5) 0.011(5) 0.027(5) C(30) 0.036(4) 0.043(4) 0.035(4) 0.011(3) 0.002(3) 0.012(3) C(31) 0.035(4) 0.061(5) 0.047(5) 0.015(4) 0.004(4) 0.023(4) C(32) 0.048(5) 0.070(5) 0.059(5) 0.019(4) 0.003(4) 0.030(4) C(33) 0.062(6) 0.068(6) 0.073(6) 0.029(5) -0.005(5) 0.025(5) C(34) 0.057(5) 0.095(6) 0.058(6) 0.035(5) 0.020(4) 0.020(5) C(35) 0.050(5) 0.068(5) 0.049(5) 0.016(4) 0.012(4) 0.019(4) C(36) 0.044(4) 0.045(4) 0.040(4) 0.014(3) 0.008(3) 0.014(3) C(37) 0.047(5) 0.061(5) 0.048(5) 0.021(4) 0.011(4) 0.014(4) C(38) 0.072(6) 0.071(5) 0.038(5) 0.033(4) 0.010(4) 0.024(4) C(39) 0.059(6) 0.085(6) 0.053(5) 0.041(5) -0.008(4) 0.009(5) C(40) 0.039(5) 0.077(6) 0.069(6) 0.019(4) 0.008(4) 0.008(5) C(41) 0.041(5) 0.068(5) 0.066(5) 0.011(4) 0.009(4) 0.028(4) C(42) 0.041(4) 0.059(5) 0.039(4) 0.013(4) 0.010(3) 0.018(4) C(43) 0.072(6) 0.054(5) 0.044(5) 0.010(4) 0.014(4) 0.018(4) C(44) 0.093(7) 0.071(6) 0.052(6) 0.021(5) 0.033(5) 0.017(4) C(45) 0.088(7) 0.113(8) 0.053(6) 0.019(6) 0.030(5) 0.031(6) C(46) 0.081(6) 0.097(7) 0.055(6) 0.010(5) 0.026(5) 0.044(5) C(47) 0.062(5) 0.061(5) 0.063(6) 0.010(4) 0.016(4) 0.028(4) C(48) 0.041(4) 0.048(4) 0.053(5) 0.010(4) 0.015(4) 0.011(4) C(49) 0.060(6) 0.050(5) 0.094(7) 0.013(4) 0.009(5) 0.015(5) C(50) 0.070(7) 0.039(5) 0.16(1) 0.014(5) 0.013(7) 0.009(6) C(51) 0.094(8) 0.047(6) 0.124(10) -0.003(5) 0.035(7) -0.001(6) C(52) 0.093(7) 0.052(6) 0.079(7) -0.007(5) 0.007(6) 0.006(5) C(53) 0.063(5) 0.043(5) 0.067(6) 0.000(4) 0.015(5) 0.005(4) C(54) 0.043(4) 0.044(4) 0.034(4) 0.011(3) 0.010(3) 0.015(3) C(55) 0.042(4) 0.053(4) 0.034(4) 0.004(3) 0.004(4) 0.014(3) C(56) 0.041(4) 0.056(5) 0.045(5) 0.007(4) -0.003(4) 0.016(4) C(57) 0.040(5) 0.058(5) 0.070(6) 0.016(4) 0.012(4) 0.028(4) C(58) 0.051(5) 0.071(5) 0.047(5) 0.027(4) 0.020(4) 0.023(4) C(59) 0.046(5) 0.058(5) 0.040(4) 0.023(4) 0.008(4) 0.012(4) C(60) 0.068(6) 0.127(8) 0.054(6) 0.026(5) 0.021(5) 0.041(5) C(61) 0.041(5) 0.099(8) 0.080(7) 0.018(5) 0.000(5) 0.008(6) C(62) 0.086(7) 0.095(7) 0.073(7) 0.033(6) 0.002(5) 0.038(6) C(63) 0.086(8) 0.084(7) 0.092(9) -0.007(6) 0.040(7) 0.009(6) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F^2^ against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^, conventional R-factors (R) are calculated on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. R-factors based on F^2^ are statistically about twice as large as those based on F, and R-factor based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + 0.00040(Fo^2^)^2^]' _refine_ls_hydrogen_treatment 'noref except for Hatoms of solvated molecules which were not included' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details centrosymmetric _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 10442 _refine_ls_number_parameters 721 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.2415 _refine_ls_R_factor_gt 0.0689 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.1585 _refine_ls_wR_factor_gt 0.1264 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.148 _refine_ls_shift/su_max 0.0070 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.86 _refine_diff_density_max 0.82 #------------------------------------------------------------------------------ loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co N(1) 1.878(5) 1_555 1_555 yes Co N(3) 1.905(4) 1_555 1_555 yes Co N(4) 1.891(4) 1_555 1_555 yes Co N(6) 1.874(5) 1_555 1_555 yes Co C(11) 1.821(7) 1_555 1_555 yes P(1) C(36) 1.803(6) 1_555 1_555 yes P(1) C(42) 1.780(7) 1_555 1_555 yes P(1) C(48) 1.767(7) 1_555 1_555 yes P(1) C(54) 1.802(7) 1_555 1_555 yes P(2) C(12) 1.768(7) 1_555 1_555 yes P(2) C(18) 1.793(6) 1_555 1_555 yes P(2) C(24) 1.797(7) 1_555 1_555 yes P(2) C(30) 1.782(6) 1_555 1_555 yes O(1) C(1) 1.250(6) 1_555 1_555 yes O(2) C(2) 1.229(7) 1_555 1_555 yes O(3) C(9) 1.253(7) 1_555 1_555 yes O(4) C(10) 1.258(7) 1_555 1_555 yes N(1) C(1) 1.321(7) 1_555 1_555 yes N(2) C(1) 1.373(7) 1_555 1_555 yes N(2) C(2) 1.388(8) 1_555 1_555 yes N(3) C(2) 1.375(7) 1_555 1_555 yes N(3) C(3) 1.401(7) 1_555 1_555 yes N(4) C(8) 1.396(7) 1_555 1_555 yes N(4) C(9) 1.357(7) 1_555 1_555 yes N(5) C(9) 1.367(7) 1_555 1_555 yes N(5) C(10) 1.398(7) 1_555 1_555 yes N(6) C(10) 1.321(7) 1_555 1_555 yes N(7) C(11) 1.158(7) 1_555 1_555 yes N(8) C(61) 1.16(1) 1_555 1_555 yes N(9) C(63) 1.19(1) 1_555 1_555 yes C(3) C(4) 1.408(8) 1_555 1_555 yes C(3) C(8) 1.414(8) 1_555 1_555 yes C(4) C(5) 1.380(8) 1_555 1_555 yes C(5) C(6) 1.378(8) 1_555 1_555 yes C(6) C(7) 1.369(8) 1_555 1_555 yes C(7) C(8) 1.401(8) 1_555 1_555 yes C(12) C(13) 1.389(9) 1_555 1_555 yes C(12) C(17) 1.410(9) 1_555 1_555 yes C(13) C(14) 1.364(10) 1_555 1_555 yes C(14) C(15) 1.39(1) 1_555 1_555 yes C(15) C(16) 1.38(1) 1_555 1_555 yes C(16) C(17) 1.362(10) 1_555 1_555 yes C(18) C(19) 1.403(9) 1_555 1_555 yes C(18) C(23) 1.382(9) 1_555 1_555 yes C(19) C(20) 1.396(9) 1_555 1_555 yes C(20) C(21) 1.366(10) 1_555 1_555 yes C(21) C(22) 1.399(10) 1_555 1_555 yes C(22) C(23) 1.390(9) 1_555 1_555 yes C(24) C(25) 1.369(9) 1_555 1_555 yes C(24) C(29) 1.393(9) 1_555 1_555 yes C(25) C(26) 1.38(1) 1_555 1_555 yes C(26) C(27) 1.37(1) 1_555 1_555 yes C(27) C(28) 1.37(1) 1_555 1_555 yes C(28) C(29) 1.39(1) 1_555 1_555 yes C(30) C(31) 1.396(8) 1_555 1_555 yes C(30) C(35) 1.397(9) 1_555 1_555 yes C(31) C(32) 1.398(9) 1_555 1_555 yes C(32) C(33) 1.36(1) 1_555 1_555 yes C(33) C(34) 1.38(1) 1_555 1_555 yes C(34) C(35) 1.395(10) 1_555 1_555 yes C(36) C(37) 1.395(9) 1_555 1_555 yes C(36) C(41) 1.374(9) 1_555 1_555 yes C(37) C(38) 1.396(9) 1_555 1_555 yes C(38) C(39) 1.39(1) 1_555 1_555 yes C(39) C(40) 1.36(1) 1_555 1_555 yes C(40) C(41) 1.372(9) 1_555 1_555 yes C(42) C(43) 1.390(9) 1_555 1_555 yes C(42) C(47) 1.407(9) 1_555 1_555 yes C(43) C(44) 1.375(10) 1_555 1_555 yes C(44) C(45) 1.36(1) 1_555 1_555 yes C(45) C(46) 1.39(1) 1_555 1_555 yes C(46) C(47) 1.41(1) 1_555 1_555 yes C(48) C(49) 1.407(9) 1_555 1_555 yes C(48) C(53) 1.383(9) 1_555 1_555 yes C(49) C(50) 1.39(1) 1_555 1_555 yes C(50) C(51) 1.36(1) 1_555 1_555 yes C(51) C(52) 1.35(1) 1_555 1_555 yes C(52) C(53) 1.39(1) 1_555 1_555 yes C(54) C(55) 1.376(8) 1_555 1_555 yes C(54) C(59) 1.394(9) 1_555 1_555 yes C(55) C(56) 1.378(9) 1_555 1_555 yes C(56) C(57) 1.363(9) 1_555 1_555 yes C(57) C(58) 1.373(9) 1_555 1_555 yes C(58) C(59) 1.371(9) 1_555 1_555 yes C(60) C(61) 1.41(1) 1_555 1_555 yes C(62) C(63) 1.41(1) 1_555 1_555 yes N(1) H(1) 0.975 1_555 1_555 no N(2) H(2) 0.973 1_555 1_555 no N(5) H(7) 0.966 1_555 1_555 no N(6) H(8) 0.980 1_555 1_555 no C(4) H(3) 1.072 1_555 1_555 no C(5) H(4) 0.981 1_555 1_555 no C(6) H(5) 0.974 1_555 1_555 no C(7) H(6) 0.978 1_555 1_555 no C(13) H(9) 1.205 1_555 1_555 no C(14) H(10) 0.990 1_555 1_555 no C(15) H(11) 0.988 1_555 1_555 no C(16) H(12) 0.993 1_555 1_555 no C(17) H(13) 0.985 1_555 1_555 no C(19) H(14) 0.989 1_555 1_555 no C(20) H(15) 1.049 1_555 1_555 no C(21) H(16) 0.989 1_555 1_555 no C(22) H(17) 1.201 1_555 1_555 no C(23) H(18) 1.039 1_555 1_555 no C(25) H(19) 0.994 1_555 1_555 no C(26) H(20) 1.000 1_555 1_555 no C(27) H(21) 0.982 1_555 1_555 no C(28) H(22) 0.970 1_555 1_555 no C(29) H(23) 0.984 1_555 1_555 no C(31) H(24) 1.155 1_555 1_555 no C(32) H(25) 0.985 1_555 1_555 no C(33) H(26) 0.976 1_555 1_555 no C(34) H(27) 0.984 1_555 1_555 no C(35) H(28) 0.999 1_555 1_555 no C(37) H(29) 0.983 1_555 1_555 no C(38) H(30) 1.073 1_555 1_555 no C(39) H(31) 0.985 1_555 1_555 no C(40) H(32) 0.980 1_555 1_555 no C(41) H(33) 0.985 1_555 1_555 no C(43) H(34) 0.983 1_555 1_555 no C(44) H(35) 0.992 1_555 1_555 no C(45) H(36) 0.982 1_555 1_555 no C(46) H(37) 0.984 1_555 1_555 no C(47) H(38) 0.998 1_555 1_555 no C(49) H(39) 0.997 1_555 1_555 no C(50) H(40) 1.001 1_555 1_555 no C(51) H(41) 0.972 1_555 1_555 no C(52) H(42) 0.990 1_555 1_555 no C(53) H(43) 0.989 1_555 1_555 no C(55) H(44) 0.985 1_555 1_555 no C(56) H(45) 0.978 1_555 1_555 no C(57) H(46) 1.064 1_555 1_555 no C(58) H(47) 0.988 1_555 1_555 no C(59) H(48) 0.991 1_555 1_555 no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Co N(3) 93.1(2) 1_555 1_555 1_555 yes N(1) Co N(4) 161.8(2) 1_555 1_555 1_555 yes N(1) Co N(6) 87.4(2) 1_555 1_555 1_555 yes N(1) Co C(11) 95.0(2) 1_555 1_555 1_555 yes N(3) Co N(4) 85.0(2) 1_555 1_555 1_555 yes N(3) Co N(6) 172.2(2) 1_555 1_555 1_555 yes N(3) Co C(11) 92.7(2) 1_555 1_555 1_555 yes N(4) Co N(6) 92.0(2) 1_555 1_555 1_555 yes N(4) Co C(11) 103.1(2) 1_555 1_555 1_555 yes N(6) Co C(11) 95.0(2) 1_555 1_555 1_555 yes C(36) P(1) C(42) 106.6(3) 1_555 1_555 1_555 yes C(36) P(1) C(48) 108.9(3) 1_555 1_555 1_555 yes C(36) P(1) C(54) 113.2(3) 1_555 1_555 1_555 yes C(42) P(1) C(48) 114.1(3) 1_555 1_555 1_555 yes C(42) P(1) C(54) 110.2(3) 1_555 1_555 1_555 yes C(48) P(1) C(54) 103.9(3) 1_555 1_555 1_555 yes C(12) P(2) C(18) 112.8(3) 1_555 1_555 1_555 yes C(12) P(2) C(24) 107.8(3) 1_555 1_555 1_555 yes C(12) P(2) C(30) 109.8(3) 1_555 1_555 1_555 yes C(18) P(2) C(24) 110.2(3) 1_555 1_555 1_555 yes C(18) P(2) C(30) 106.6(3) 1_555 1_555 1_555 yes C(24) P(2) C(30) 109.7(3) 1_555 1_555 1_555 yes Co N(1) C(1) 128.8(4) 1_555 1_555 1_555 yes C(1) N(2) C(2) 132.2(5) 1_555 1_555 1_555 yes Co N(3) C(2) 126.2(4) 1_555 1_555 1_555 yes Co N(3) C(3) 112.6(3) 1_555 1_555 1_555 yes C(2) N(3) C(3) 120.9(5) 1_555 1_555 1_555 yes Co N(4) C(8) 112.4(4) 1_555 1_555 1_555 yes Co N(4) C(9) 126.2(4) 1_555 1_555 1_555 yes C(8) N(4) C(9) 120.2(5) 1_555 1_555 1_555 yes C(9) N(5) C(10) 130.6(5) 1_555 1_555 1_555 yes Co N(6) C(10) 131.5(4) 1_555 1_555 1_555 yes O(1) C(1) N(1) 123.3(6) 1_555 1_555 1_555 yes O(1) C(1) N(2) 117.8(5) 1_555 1_555 1_555 yes N(1) C(1) N(2) 118.9(5) 1_555 1_555 1_555 yes O(2) C(2) N(2) 116.7(5) 1_555 1_555 1_555 yes O(2) C(2) N(3) 124.9(6) 1_555 1_555 1_555 yes N(2) C(2) N(3) 118.4(6) 1_555 1_555 1_555 yes N(3) C(3) C(4) 127.4(5) 1_555 1_555 1_555 yes N(3) C(3) C(8) 113.6(5) 1_555 1_555 1_555 yes C(4) C(3) C(8) 119.0(6) 1_555 1_555 1_555 yes C(3) C(4) C(5) 119.9(6) 1_555 1_555 1_555 yes C(4) C(5) C(6) 120.8(6) 1_555 1_555 1_555 yes C(5) C(6) C(7) 120.2(6) 1_555 1_555 1_555 yes C(6) C(7) C(8) 120.9(6) 1_555 1_555 1_555 yes N(4) C(8) C(3) 115.0(5) 1_555 1_555 1_555 yes N(4) C(8) C(7) 126.0(5) 1_555 1_555 1_555 yes C(3) C(8) C(7) 118.9(6) 1_555 1_555 1_555 yes O(3) C(9) N(4) 124.3(6) 1_555 1_555 1_555 yes O(3) C(9) N(5) 116.0(5) 1_555 1_555 1_555 yes N(4) C(9) N(5) 119.7(5) 1_555 1_555 1_555 yes O(4) C(10) N(5) 117.2(5) 1_555 1_555 1_555 yes O(4) C(10) N(6) 125.9(6) 1_555 1_555 1_555 yes N(5) C(10) N(6) 116.9(5) 1_555 1_555 1_555 yes Co C(11) N(7) 176.8(6) 1_555 1_555 1_555 yes P(2) C(12) C(13) 122.3(5) 1_555 1_555 1_555 yes P(2) C(12) C(17) 119.9(5) 1_555 1_555 1_555 yes C(13) C(12) C(17) 117.7(6) 1_555 1_555 1_555 yes C(12) C(13) C(14) 120.9(7) 1_555 1_555 1_555 yes C(13) C(14) C(15) 120.8(7) 1_555 1_555 1_555 yes C(14) C(15) C(16) 119.0(7) 1_555 1_555 1_555 yes C(15) C(16) C(17) 120.7(7) 1_555 1_555 1_555 yes C(12) C(17) C(16) 120.8(7) 1_555 1_555 1_555 yes P(2) C(18) C(19) 122.1(5) 1_555 1_555 1_555 yes P(2) C(18) C(23) 117.4(5) 1_555 1_555 1_555 yes C(19) C(18) C(23) 120.4(6) 1_555 1_555 1_555 yes C(18) C(19) C(20) 118.8(6) 1_555 1_555 1_555 yes C(19) C(20) C(21) 119.9(7) 1_555 1_555 1_555 yes C(20) C(21) C(22) 122.2(7) 1_555 1_555 1_555 yes C(21) C(22) C(23) 117.8(7) 1_555 1_555 1_555 yes C(18) C(23) C(22) 121.0(6) 1_555 1_555 1_555 yes P(2) C(24) C(25) 124.2(6) 1_555 1_555 1_555 yes P(2) C(24) C(29) 117.2(6) 1_555 1_555 1_555 yes C(25) C(24) C(29) 118.6(7) 1_555 1_555 1_555 yes C(24) C(25) C(26) 121.1(8) 1_555 1_555 1_555 yes C(25) C(26) C(27) 119.9(9) 1_555 1_555 1_555 yes C(26) C(27) C(28) 120.7(9) 1_555 1_555 1_555 yes C(27) C(28) C(29) 119.0(9) 1_555 1_555 1_555 yes C(24) C(29) C(28) 120.6(8) 1_555 1_555 1_555 yes P(2) C(30) C(31) 122.0(5) 1_555 1_555 1_555 yes P(2) C(30) C(35) 117.5(5) 1_555 1_555 1_555 yes C(31) C(30) C(35) 120.5(6) 1_555 1_555 1_555 yes C(30) C(31) C(32) 118.6(6) 1_555 1_555 1_555 yes C(31) C(32) C(33) 120.3(7) 1_555 1_555 1_555 yes C(32) C(33) C(34) 121.8(7) 1_555 1_555 1_555 yes C(33) C(34) C(35) 119.2(7) 1_555 1_555 1_555 yes C(30) C(35) C(34) 119.5(7) 1_555 1_555 1_555 yes P(1) C(36) C(37) 120.9(5) 1_555 1_555 1_555 yes P(1) C(36) C(41) 119.0(5) 1_555 1_555 1_555 yes C(37) C(36) C(41) 119.7(6) 1_555 1_555 1_555 yes C(36) C(37) C(38) 119.4(7) 1_555 1_555 1_555 yes C(37) C(38) C(39) 118.7(7) 1_555 1_555 1_555 yes C(38) C(39) C(40) 121.9(7) 1_555 1_555 1_555 yes C(39) C(40) C(41) 119.0(7) 1_555 1_555 1_555 yes C(36) C(41) C(40) 121.4(7) 1_555 1_555 1_555 yes P(1) C(42) C(43) 118.4(5) 1_555 1_555 1_555 yes P(1) C(42) C(47) 121.5(6) 1_555 1_555 1_555 yes C(43) C(42) C(47) 120.0(6) 1_555 1_555 1_555 yes C(42) C(43) C(44) 120.2(7) 1_555 1_555 1_555 yes C(43) C(44) C(45) 120.8(8) 1_555 1_555 1_555 yes C(44) C(45) C(46) 120.6(8) 1_555 1_555 1_555 yes C(45) C(46) C(47) 120.0(7) 1_555 1_555 1_555 yes C(42) C(47) C(46) 118.3(7) 1_555 1_555 1_555 yes P(1) C(48) C(49) 119.2(6) 1_555 1_555 1_555 yes P(1) C(48) C(53) 121.8(6) 1_555 1_555 1_555 yes C(49) C(48) C(53) 118.4(7) 1_555 1_555 1_555 yes C(48) C(49) C(50) 119.2(8) 1_555 1_555 1_555 yes C(49) C(50) C(51) 121.0(9) 1_555 1_555 1_555 yes C(50) C(51) C(52) 120.2(9) 1_555 1_555 1_555 yes C(51) C(52) C(53) 121.0(9) 1_555 1_555 1_555 yes C(48) C(53) C(52) 120.2(8) 1_555 1_555 1_555 yes P(1) C(54) C(55) 123.2(5) 1_555 1_555 1_555 yes P(1) C(54) C(59) 117.2(5) 1_555 1_555 1_555 yes C(55) C(54) C(59) 119.4(6) 1_555 1_555 1_555 yes C(54) C(55) C(56) 119.1(6) 1_555 1_555 1_555 yes C(55) C(56) C(57) 121.0(6) 1_555 1_555 1_555 yes C(56) C(57) C(58) 120.8(7) 1_555 1_555 1_555 yes C(57) C(58) C(59) 118.7(7) 1_555 1_555 1_555 yes C(54) C(59) C(58) 121.0(6) 1_555 1_555 1_555 yes N(8) C(61) C(60) 176(1) 1_555 1_555 1_555 yes N(9) C(63) C(62) 176(1) 1_555 1_555 1_555 yes Co N(1) H(1) 116.4 1_555 1_555 1_555 no C(1) N(1) H(1) 114.8 1_555 1_555 1_555 no C(1) N(2) H(2) 113.8 1_555 1_555 1_555 no C(2) N(2) H(2) 114.0 1_555 1_555 1_555 no C(9) N(5) H(7) 115.4 1_555 1_555 1_555 no C(10) N(5) H(7) 114.0 1_555 1_555 1_555 no Co N(6) H(8) 114.9 1_555 1_555 1_555 no C(10) N(6) H(8) 113.6 1_555 1_555 1_555 no C(3) C(4) H(3) 121.8 1_555 1_555 1_555 no C(5) C(4) H(3) 118.0 1_555 1_555 1_555 no C(4) C(5) H(4) 119.1 1_555 1_555 1_555 no C(6) C(5) H(4) 120.1 1_555 1_555 1_555 no C(5) C(6) H(5) 119.4 1_555 1_555 1_555 no C(7) C(6) H(5) 120.3 1_555 1_555 1_555 no C(6) C(7) H(6) 119.4 1_555 1_555 1_555 no C(8) C(7) H(6) 119.6 1_555 1_555 1_555 no C(12) C(13) H(9) 117.4 1_555 1_555 1_555 no C(14) C(13) H(9) 120.8 1_555 1_555 1_555 no C(13) C(14) H(10) 119.4 1_555 1_555 1_555 no C(15) C(14) H(10) 119.8 1_555 1_555 1_555 no C(14) C(15) H(11) 120.6 1_555 1_555 1_555 no C(16) C(15) H(11) 120.5 1_555 1_555 1_555 no C(15) C(16) H(12) 119.6 1_555 1_555 1_555 no C(17) C(16) H(12) 119.7 1_555 1_555 1_555 no C(12) C(17) H(13) 119.6 1_555 1_555 1_555 no C(16) C(17) H(13) 119.5 1_555 1_555 1_555 no C(18) C(19) H(14) 120.9 1_555 1_555 1_555 no C(20) C(19) H(14) 120.2 1_555 1_555 1_555 no C(19) C(20) H(15) 112.7 1_555 1_555 1_555 no C(21) C(20) H(15) 127.4 1_555 1_555 1_555 no C(20) C(21) H(16) 119.4 1_555 1_555 1_555 no C(22) C(21) H(16) 118.4 1_555 1_555 1_555 no C(21) C(22) H(17) 116.2 1_555 1_555 1_555 no C(23) C(22) H(17) 121.4 1_555 1_555 1_555 no C(18) C(23) H(18) 123.3 1_555 1_555 1_555 no C(22) C(23) H(18) 114.9 1_555 1_555 1_555 no C(24) C(25) H(19) 119.4 1_555 1_555 1_555 no C(26) C(25) H(19) 119.6 1_555 1_555 1_555 no C(25) C(26) H(20) 121 1_555 1_555 1_555 no C(27) C(26) H(20) 118 1_555 1_555 1_555 no C(26) C(27) H(21) 119 1_555 1_555 1_555 no C(28) C(27) H(21) 120 1_555 1_555 1_555 no C(27) C(28) H(22) 119 1_555 1_555 1_555 no C(29) C(28) H(22) 121 1_555 1_555 1_555 no C(24) C(29) H(23) 120.3 1_555 1_555 1_555 no C(28) C(29) H(23) 119.1 1_555 1_555 1_555 no C(30) C(31) H(24) 119.5 1_555 1_555 1_555 no C(32) C(31) H(24) 121.8 1_555 1_555 1_555 no C(31) C(32) H(25) 119.2 1_555 1_555 1_555 no C(33) C(32) H(25) 120.5 1_555 1_555 1_555 no C(32) C(33) H(26) 119.9 1_555 1_555 1_555 no C(34) C(33) H(26) 118.2 1_555 1_555 1_555 no C(33) C(34) H(27) 120.8 1_555 1_555 1_555 no C(35) C(34) H(27) 120.0 1_555 1_555 1_555 no C(30) C(35) H(28) 120.7 1_555 1_555 1_555 no C(34) C(35) H(28) 119.8 1_555 1_555 1_555 no C(36) C(37) H(29) 120.6 1_555 1_555 1_555 no C(38) C(37) H(29) 120.0 1_555 1_555 1_555 no C(37) C(38) H(30) 116.9 1_555 1_555 1_555 no C(39) C(38) H(30) 124.4 1_555 1_555 1_555 no C(38) C(39) H(31) 119.7 1_555 1_555 1_555 no C(40) C(39) H(31) 118.3 1_555 1_555 1_555 no C(39) C(40) H(32) 120.6 1_555 1_555 1_555 no C(41) C(40) H(32) 120.4 1_555 1_555 1_555 no C(36) C(41) H(33) 118.8 1_555 1_555 1_555 no C(40) C(41) H(33) 119.8 1_555 1_555 1_555 no C(42) C(43) H(34) 120.0 1_555 1_555 1_555 no C(44) C(43) H(34) 119.8 1_555 1_555 1_555 no C(43) C(44) H(35) 120.9 1_555 1_555 1_555 no C(45) C(44) H(35) 118.3 1_555 1_555 1_555 no C(44) C(45) H(36) 120 1_555 1_555 1_555 no C(46) C(45) H(36) 118.4 1_555 1_555 1_555 no C(45) C(46) H(37) 120.1 1_555 1_555 1_555 no C(47) C(46) H(37) 119.8 1_555 1_555 1_555 no C(42) C(47) H(38) 120.3 1_555 1_555 1_555 no C(46) C(47) H(38) 121.4 1_555 1_555 1_555 no C(48) C(49) H(39) 119.0 1_555 1_555 1_555 no C(50) C(49) H(39) 121.8 1_555 1_555 1_555 no C(49) C(50) H(40) 118 1_555 1_555 1_555 no C(51) C(50) H(40) 120.6 1_555 1_555 1_555 no C(50) C(51) H(41) 119 1_555 1_555 1_555 no C(52) C(51) H(41) 120 1_555 1_555 1_555 no C(51) C(52) H(42) 118.9 1_555 1_555 1_555 no C(53) C(52) H(42) 120.2 1_555 1_555 1_555 no C(48) C(53) H(43) 119.2 1_555 1_555 1_555 no C(52) C(53) H(43) 120.7 1_555 1_555 1_555 no C(54) C(55) H(44) 120.4 1_555 1_555 1_555 no C(56) C(55) H(44) 120.5 1_555 1_555 1_555 no C(55) C(56) H(45) 119.3 1_555 1_555 1_555 no C(57) C(56) H(45) 119.7 1_555 1_555 1_555 no C(56) C(57) H(46) 113.0 1_555 1_555 1_555 no C(58) C(57) H(46) 125.9 1_555 1_555 1_555 no C(57) C(58) H(47) 120.0 1_555 1_555 1_555 no C(59) C(58) H(47) 121.3 1_555 1_555 1_555 no C(54) C(59) H(48) 119.0 1_555 1_555 1_555 no C(58) C(59) H(48) 120.0 1_555 1_555 1_555 no #------------------------------------------------------------------------------ #===END data_K3[Co(bbphen)(CN)2] _database_code_CSD 169290 #------------------------------------------------------------------------------ _audit_creation_date 'Mon Feb 22 11:25:41 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'SHELXS86' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics 'ORTEP in teXsan' #------------------------------------------------------------------------------ _chemical_compound_source ; Prepared from K[Co(bbphen)] and KCN in refluxing water, recrystallized from aqueous ethanol. ; _chemical_name_common 'K~3~[Co(bbphen)(CN)~2~].5.5H~2~O' _chemical_formula_weight 603.56 _chemical_formula_analytical 'C12 H19 Co K3 N8 O9.50 ' _chemical_formula_sum 'C12 H19 Co K3 N8 O9.50 ' _chemical_formula_moiety '3(K +), C12 H6 N8 O4 Co 3-, 5.5(H2 O)' _chemical_formula_structural 'K3, (Co (C10 H8 N6 O4) 2(C N), 5.5(H2 O)' _chemical_melting_point 527 #------------------------------------------------------------------------------ _cell_length_a 11.126(3) _cell_length_b 12.813(2) _cell_length_c 9.737(2) _cell_angle_alpha 112.19(1) _cell_angle_beta 114.59(2) _cell_angle_gamma 79.37(2) _cell_volume 1168.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 23 _cell_measurement_theta_min 11.1 _cell_measurement_theta_max 11.8 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.716 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 614.00 _exptl_absorpt_coefficient_mu 1.332 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details Coppens_numerical _exptl_absorpt_correction_T_min 0.683 _exptl_absorpt_correction_T_max 0.881 _exptl_special_details 'none' #------------------------------------------------------------------------------ _diffrn_special_details ; \q scan width (1.050 + 0.350tan\q)\%, \w scan rate 8\% per min. Background counts for 25% time on each side every scan. ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -4.07 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 -3 0 2 -3 1 1 -2 1 _diffrn_reflns_number 5151 _reflns_number_total 4873 _reflns_number_gt 4024 _reflns_observed_expression 'F^2^ 2 \s(F^2^)' _diffrn_reflns_av_R_equivalents 0.014 _diffrn_reflns_av_sigmaI/netI 0.000 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 0.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.00858 _diffrn_orient_matrix_UB_12 -0.08328 _diffrn_orient_matrix_UB_13 -0.03489 _diffrn_orient_matrix_UB_21 -0.04338 _diffrn_orient_matrix_UB_22 -0.00342 _diffrn_orient_matrix_UB_23 -0.11444 _diffrn_orient_matrix_UB_31 0.08845 _diffrn_orient_matrix_UB_32 -0.01282 _diffrn_orient_matrix_UB_33 -0.00847 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'Co' 'Co' 0.349 0.972 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'K' 'K' 0.200 0.250 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'C' 'C' 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #------------------------------------------------------------------------------ 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_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.30360(6) 0.16735(5) 0.04203(7) 0.0173(2) Uani 1.00 d . . . K(1) K 0.2692(1) 0.0249(1) 0.3937(2) 0.0373(4) Uani 1.00 d . . . K(2) K 0.5835(2) 0.3557(1) 0.7200(2) 0.0568(5) Uani 1.00 d . . . K(3a) K 0.8455(2) 0.4374(2) 0.5013(2) 0.0208(5) Uani 0.50 d P . . K(3b) K 0.9074(2) 0.4723(2) 0.2517(3) 0.0316(6) Uani 0.50 d P . . O(1) O 0.6579(4) 0.3150(4) 0.2227(5) 0.036(1) Uani 1.00 d . . . O(2) O 0.3703(4) 0.4312(3) 0.4648(4) 0.033(1) Uani 1.00 d . . . O(3) O -0.0963(3) 0.1410(3) -0.1755(4) 0.033(1) Uani 1.00 d . . . O(4) O 0.1739(4) -0.0286(3) -0.4305(4) 0.032(1) Uani 1.00 d . . . O(5) O 0.7507(4) 0.2990(4) 0.9853(5) 0.043(1) Uani 1.00 d . . . O(6) O 0.4220(5) 0.1908(4) 0.6922(6) 0.055(2) Uani 1.00 d . . . O(7) O 0.6094(6) 0.1585(5) 0.4825(6) 0.069(2) Uani 1.00 d . . . O(8) O 0.8423(7) 0.3488(6) 0.7309(9) 0.096(3) Uani 1.00 d . . . O(9) O 0.4031(9) 0.4801(5) 0.841(1) 0.113(3) Uani 1.00 d . . . O(10) O 0.033(1) 0.451(1) 0.048(2) 0.090(5) Uani 0.50 d P . . N(1) N 0.4848(4) 0.1954(4) 0.1017(5) 0.025(1) Uani 1.00 d . . . N(2) N 0.4872(4) 0.3667(4) 0.3082(5) 0.027(1) Uani 1.00 d . . . N(3) N 0.3035(4) 0.2689(3) 0.2457(4) 0.0194(10) Uani 1.00 d . . . N(4) N 0.1237(4) 0.1468(3) -0.0036(5) 0.0209(10) Uani 1.00 d . . . N(5) N 0.0598(4) 0.0832(4) -0.2811(5) 0.027(1) Uani 1.00 d . . . N(6) N 0.2880(4) 0.0612(4) -0.1648(5) 0.022(1) Uani 1.00 d . . . N(7) N 0.3990(6) -0.0288(4) 0.1763(6) 0.043(2) Uani 1.00 d . . . N(8) N 0.2283(8) 0.3554(5) -0.1040(8) 0.072(2) Uani 1.00 d . . . C(1) C 0.5472(5) 0.2877(5) 0.2056(6) 0.026(1) Uani 1.00 d . . . C(2) C 0.3824(5) 0.3556(4) 0.3422(6) 0.022(1) Uani 1.00 d . . . C(3) C 0.1969(5) 0.2498(4) 0.2764(6) 0.019(1) Uani 1.00 d . . . C(4) C 0.1864(5) 0.2832(4) 0.4252(6) 0.024(1) Uani 1.00 d . . . C(5) C 0.0821(6) 0.2502(5) 0.4395(6) 0.029(1) Uani 1.00 d . . . C(6) C -0.0157(5) 0.1818(4) 0.3029(7) 0.029(1) Uani 1.00 d . . . C(7) C -0.0059(5) 0.1479(4) 0.1548(6) 0.025(1) Uani 1.00 d . . . C(8) C 0.0983(5) 0.1815(4) 0.1392(6) 0.020(1) Uani 1.00 d . . . C(9) C 0.0262(5) 0.1251(4) -0.1479(6) 0.023(1) Uani 1.00 d . . . C(10) C 0.1801(5) 0.0368(4) -0.2902(5) 0.021(1) Uani 1.00 d . . . C(11) C 0.3609(5) 0.0447(4) 0.1257(6) 0.026(1) Uani 1.00 d . . . C(12) C 0.2527(6) 0.2882(5) -0.0469(7) 0.034(2) Uani 1.00 d . . . H(1) H 0.5228 0.1343 0.0036 0.0863 Uiso 1.00 d . . . H(2) H 0.5158 0.4477 0.3824 0.0405 Uiso 1.00 d . . . H(3) H 0.2605 0.3200 0.5071 0.0226 Uiso 1.00 d . . . H(4) H 0.0668 0.2640 0.5253 0.0070 Uiso 1.00 d . . . H(5) H -0.0796 0.1249 0.3048 0.0789 Uiso 1.00 d . . . H(6) H -0.0531 0.0865 0.0480 0.0535 Uiso 1.00 d . . . H(7) H -0.0200 0.0153 -0.3971 0.0502 Uiso 1.00 d . . . H(8) H 0.3417 0.0080 -0.1955 0.0202 Uiso 1.00 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co 0.0155(3) 0.0192(3) 0.0147(3) -0.0035(2) 0.0046(2) 0.0027(2) K(1) 0.0428(8) 0.0380(7) 0.0363(7) -0.0062(6) 0.0186(6) 0.0113(6) K(2) 0.0523(10) 0.066(1) 0.0475(9) 0.0115(8) 0.0140(7) 0.0249(8) K(3a) 0.0081(9) 0.025(1) 0.0222(10) 0.0005(8) 0.0031(8) 0.0031(8) K(3b) 0.025(1) 0.039(1) 0.031(1) -0.006(1) 0.0058(10) 0.014(1) O(1) 0.025(2) 0.050(3) 0.032(2) -0.018(2) 0.015(2) -0.001(2) O(2) 0.032(2) 0.028(2) 0.031(2) -0.012(2) 0.017(2) -0.010(2) O(3) 0.014(2) 0.046(2) 0.027(2) 0.000(2) 0.004(1) 0.004(2) O(4) 0.027(2) 0.046(2) 0.015(2) -0.004(2) 0.007(2) 0.001(2) O(5) 0.042(3) 0.046(3) 0.043(2) 0.005(2) 0.018(2) 0.018(2) O(6) 0.050(3) 0.063(3) 0.058(3) 0.002(2) 0.012(2) 0.035(3) O(7) 0.078(4) 0.066(4) 0.045(3) 0.021(3) 0.017(3) 0.015(3) O(8) 0.077(5) 0.104(6) 0.111(6) 0.001(4) 0.024(4) 0.052(5) O(9) 0.190(8) 0.052(4) 0.164(7) 0.018(4) 0.147(7) 0.027(4) O(10) 0.09(1) 0.088(10) 0.09(1) 0.009(8) 0.058(9) 0.016(8) N(1) 0.020(2) 0.026(2) 0.022(2) -0.009(2) 0.009(2) -0.004(2) N(2) 0.028(2) 0.025(2) 0.026(2) -0.009(2) 0.014(2) -0.003(2) N(3) 0.016(2) 0.020(2) 0.018(2) -0.004(2) 0.006(2) 0.000(2) N(4) 0.012(2) 0.026(2) 0.017(2) -0.004(2) 0.003(2) 0.000(2) N(5) 0.024(2) 0.034(3) 0.018(2) -0.001(2) 0.006(2) 0.005(2) N(6) 0.017(2) 0.027(2) 0.015(2) -0.003(2) 0.005(2) -0.001(2) N(7) 0.057(3) 0.039(3) 0.044(3) 0.017(3) 0.028(3) 0.024(2) N(8) 0.100(6) 0.049(4) 0.064(4) -0.005(4) 0.013(4) 0.034(3) C(1) 0.027(3) 0.032(3) 0.018(2) -0.008(2) 0.008(2) 0.004(2) C(2) 0.019(3) 0.021(2) 0.020(2) -0.002(2) 0.005(2) 0.003(2) C(3) 0.018(2) 0.017(2) 0.022(2) 0.001(2) 0.008(2) 0.005(2) C(4) 0.024(3) 0.023(3) 0.021(2) -0.001(2) 0.008(2) 0.001(2) C(5) 0.036(3) 0.027(3) 0.026(3) 0.002(2) 0.018(2) 0.006(2) C(6) 0.030(3) 0.027(3) 0.037(3) -0.001(2) 0.018(2) 0.012(2) C(7) 0.023(3) 0.023(3) 0.027(3) -0.004(2) 0.011(2) 0.004(2) C(8) 0.019(2) 0.018(2) 0.021(2) 0.002(2) 0.008(2) 0.005(2) C(9) 0.021(3) 0.022(2) 0.020(2) 0.001(2) 0.008(2) 0.003(2) C(10) 0.020(2) 0.025(2) 0.018(2) -0.006(2) 0.007(2) 0.004(2) C(11) 0.025(3) 0.031(3) 0.020(2) 0.002(2) 0.012(2) 0.004(2) C(12) 0.038(3) 0.029(3) 0.030(3) -0.007(3) 0.004(2) 0.012(2) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F^2^ against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^, conventional R-factors (R) are calculated on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. R-factors based on F^2^ are statistically about twice as large as those based on F, and R-factor based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + 0.00040(Fo^2^)^2^]' _refine_ls_hydrogen_treatment 'noref except for Hatoms of solvated molecules which were not included' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details centrosymmetric _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4873 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0810 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.1801 _refine_ls_wR_factor_gt 0.1756 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 2.716 _refine_ls_shift/su_max 0.0020 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -1.02 _refine_diff_density_max 2.05 #------------------------------------------------------------------------------ loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co N(1) 1.915(4) 1_555 1_555 yes Co N(3) 1.918(4) 1_555 1_555 yes Co N(4) 1.908(4) 1_555 1_555 yes Co N(6) 1.914(4) 1_555 1_555 yes Co C(11) 1.925(5) 1_555 1_555 yes Co C(12) 1.937(6) 1_555 1_555 yes K(3a) K(3b) 2.872(3) 1_555 2_766 yes O(1) C(1) 1.270(6) 1_555 1_555 yes O(2) C(2) 1.263(6) 1_555 1_555 yes O(3) C(9) 1.267(6) 1_555 1_555 yes O(4) C(10) 1.284(6) 1_555 1_555 yes O(10) O(10) 1.73(3) 1_555 2_565 yes N(1) C(1) 1.311(6) 1_555 1_555 yes N(2) C(1) 1.418(7) 1_555 1_555 yes N(2) C(2) 1.381(7) 1_555 1_555 yes N(3) C(2) 1.331(6) 1_555 1_555 yes N(3) C(3) 1.419(6) 1_555 1_555 yes N(4) C(8) 1.422(6) 1_555 1_555 yes N(4) C(9) 1.333(6) 1_555 1_555 yes N(5) C(9) 1.384(6) 1_555 1_555 yes N(5) C(10) 1.385(7) 1_555 1_555 yes N(6) C(10) 1.288(6) 1_555 1_555 yes N(7) C(11) 1.157(7) 1_555 1_555 yes N(8) C(12) 1.128(8) 1_555 1_555 yes C(3) C(4) 1.396(7) 1_555 1_555 yes C(3) C(8) 1.417(7) 1_555 1_555 yes C(4) C(5) 1.380(8) 1_555 1_555 yes C(5) C(6) 1.410(8) 1_555 1_555 yes C(6) C(7) 1.386(7) 1_555 1_555 yes C(7) C(8) 1.390(7) 1_555 1_555 yes N(1) H(1) 1.164 1_555 1_555 no N(2) H(2) 1.032 1_555 1_555 no N(5) H(7) 1.237 1_555 1_555 no N(6) H(8) 0.870 1_555 1_555 no C(4) H(3) 0.922 1_555 1_555 no C(5) H(4) 0.869 1_555 1_555 no C(6) H(5) 1.118 1_555 1_555 no C(7) H(6) 1.027 1_555 1_555 no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Co N(3) 91.8(2) 1_555 1_555 1_555 yes N(1) Co N(4) 176.1(2) 1_555 1_555 1_555 yes N(1) Co N(6) 93.5(2) 1_555 1_555 1_555 yes N(1) Co C(11) 89.3(2) 1_555 1_555 1_555 yes N(1) Co C(12) 88.6(2) 1_555 1_555 1_555 yes N(3) Co N(4) 84.3(2) 1_555 1_555 1_555 yes N(3) Co N(6) 174.6(2) 1_555 1_555 1_555 yes N(3) Co C(11) 90.4(2) 1_555 1_555 1_555 yes N(3) Co C(12) 91.6(2) 1_555 1_555 1_555 yes N(4) Co N(6) 90.4(2) 1_555 1_555 1_555 yes N(4) Co C(11) 90.9(2) 1_555 1_555 1_555 yes N(4) Co C(12) 91.4(2) 1_555 1_555 1_555 yes N(6) Co C(11) 88.5(2) 1_555 1_555 1_555 yes N(6) Co C(12) 89.6(2) 1_555 1_555 1_555 yes C(11) Co C(12) 177.1(2) 1_555 1_555 1_555 yes Co N(1) C(1) 126.3(4) 1_555 1_555 1_555 yes C(1) N(2) C(2) 130.4(4) 1_555 1_555 1_555 yes Co N(3) C(2) 126.0(3) 1_555 1_555 1_555 yes Co N(3) C(3) 111.7(3) 1_555 1_555 1_555 yes C(2) N(3) C(3) 121.9(4) 1_555 1_555 1_555 yes Co N(4) C(8) 111.6(3) 1_555 1_555 1_555 yes Co N(4) C(9) 125.2(4) 1_555 1_555 1_555 yes C(8) N(4) C(9) 121.9(4) 1_555 1_555 1_555 yes C(9) N(5) C(10) 128.3(4) 1_555 1_555 1_555 yes Co N(6) C(10) 125.9(4) 1_555 1_555 1_555 yes O(1) C(1) N(1) 126.0(5) 1_555 1_555 1_555 yes O(1) C(1) N(2) 115.6(4) 1_555 1_555 1_555 yes N(1) C(1) N(2) 118.5(5) 1_555 1_555 1_555 yes O(2) C(2) N(2) 115.5(4) 1_555 1_555 1_555 yes O(2) C(2) N(3) 125.7(5) 1_555 1_555 1_555 yes N(2) C(2) N(3) 118.8(4) 1_555 1_555 1_555 yes N(3) C(3) C(4) 127.0(4) 1_555 1_555 1_555 yes N(3) C(3) C(8) 113.8(4) 1_555 1_555 1_555 yes C(4) C(3) C(8) 119.0(5) 1_555 1_555 1_555 yes C(3) C(4) C(5) 120.9(5) 1_555 1_555 1_555 yes C(4) C(5) C(6) 120.1(5) 1_555 1_555 1_555 yes C(5) C(6) C(7) 119.5(5) 1_555 1_555 1_555 yes C(6) C(7) C(8) 120.8(5) 1_555 1_555 1_555 yes N(4) C(8) C(3) 114.0(4) 1_555 1_555 1_555 yes N(4) C(8) C(7) 126.1(4) 1_555 1_555 1_555 yes C(3) C(8) C(7) 119.8(4) 1_555 1_555 1_555 yes O(3) C(9) N(4) 125.9(5) 1_555 1_555 1_555 yes O(3) C(9) N(5) 116.1(4) 1_555 1_555 1_555 yes N(4) C(9) N(5) 118.0(4) 1_555 1_555 1_555 yes O(4) C(10) N(5) 114.9(4) 1_555 1_555 1_555 yes O(4) C(10) N(6) 124.5(5) 1_555 1_555 1_555 yes N(5) C(10) N(6) 120.5(4) 1_555 1_555 1_555 yes Co C(11) N(7) 178.0(5) 1_555 1_555 1_555 yes Co C(12) N(8) 175.6(7) 1_555 1_555 1_555 yes Co N(1) H(1) 109.8 1_555 1_555 1_555 no C(1) N(1) H(1) 120.9 1_555 1_555 1_555 no C(1) N(2) H(2) 127.5 1_555 1_555 1_555 no C(2) N(2) H(2) 102.0 1_555 1_555 1_555 no C(9) N(5) H(7) 113.0 1_555 1_555 1_555 no C(10) N(5) H(7) 102.7 1_555 1_555 1_555 no Co N(6) H(8) 131.6 1_555 1_555 1_555 no C(10) N(6) H(8) 101.2 1_555 1_555 1_555 no C(3) C(4) H(3) 111.4 1_555 1_555 1_555 no C(5) C(4) H(3) 127.3 1_555 1_555 1_555 no C(4) C(5) H(4) 128.9 1_555 1_555 1_555 no C(6) C(5) H(4) 111.0 1_555 1_555 1_555 no C(5) C(6) H(5) 125.0 1_555 1_555 1_555 no C(7) C(6) H(5) 111.4 1_555 1_555 1_555 no C(6) C(7) H(6) 131.5 1_555 1_555 1_555 no C(8) C(7) H(6) 106.5 1_555 1_555 1_555 no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag K(1) O(4) 2.682(4) 1_555 1_556 ? K(1) O(3) 2.727(4) 1_555 2_555 ? K(1) N(7) 2.849(5) 1_555 1_555 ? K(1) O(6) 2.900(5) 1_555 1_555 ? K(1) O(7) 2.901(6) 1_555 2_656 ? K(1) C(4) 3.200(5) 1_555 1_555 ? K(1) C(5) 3.232(6) 1_555 1_555 ? K(1) C(11) 3.275(5) 1_555 1_555 ? K(1) C(3) 3.335(5) 1_555 1_555 ? K(1) C(6) 3.396(6) 1_555 1_555 ? K(1) C(8) 3.494(5) 1_555 1_555 ? K(1) C(7) 3.511(5) 1_555 1_555 ? K(2) O(9) 2.708(7) 1_555 1_555 ? K(2) O(5) 2.753(4) 1_555 1_555 ? K(2) O(7) 2.772(5) 1_555 1_555 ? K(2) O(8) 2.822(8) 1_555 1_555 ? K(2) O(6) 2.886(5) 1_555 1_555 ? K(2) O(2) 2.967(4) 1_555 1_555 ? K(2) N(2) 3.589(5) 1_555 2_666 ? K(3a) O(1) 2.730(4) 1_555 1_555 ? K(3a) O(2) 2.731(4) 1_555 2_666 ? K(3a) O(8) 2.880(8) 1_555 1_555 ? K(3b) O(10) 2.77(1) 1_555 1_655 ? K(3b) O(5) 2.832(5) 1_555 1_554 ? K(3b) N(8) 2.929(7) 1_555 2_665 ? K(3b) O(9) 3.188(9) 1_555 2_666 ? K(3b) O(1) 3.581(4) 1_555 1_555 ? O(1) O(9) 2.821(8) 1_555 2_666 ? O(1) O(5) 2.828(6) 1_555 1_554 ? O(2) N(2) 2.895(5) 1_555 2_666 ? O(2) O(9) 3.345(8) 1_555 1_555 ? O(3) O(5) 2.829(6) 1_555 1_454 ? O(3) O(8) 3.004(8) 1_555 1_454 ? O(4) O(7) 2.783(7) 1_555 2_655 ? O(4) N(5) 2.872(5) 1_555 2_554 ? O(5) O(9) 3.287(7) 1_555 2_667 ? O(5) O(8) 3.333(9) 1_555 1_555 ? O(6) N(7) 2.876(7) 1_555 2_656 ? O(6) O(7) 3.357(8) 1_555 1_555 ? O(6) N(6) 3.363(6) 1_555 1_556 ? O(6) N(8) 3.429(10) 1_555 1_556 ? O(6) O(9) 3.435(8) 1_555 1_555 ? O(7) N(7) 3.316(8) 1_555 1_555 ? O(7) O(8) 3.342(9) 1_555 1_555 ? O(7) N(2) 3.464(7) 1_555 1_555 ? O(7) N(1) 3.563(7) 1_555 1_555 ? O(8) O(10) 2.79(2) 1_555 2_666 ? O(8) O(10) 2.88(2) 1_555 1_656 ? O(9) O(9) 2.85(2) 1_555 2_667 ? O(9) N(8) 3.047(10) 1_555 1_556 ? O(9) N(2) 3.460(8) 1_555 2_666 ? O(10) N(8) 2.96(1) 1_555 1_555 ? O(10) N(8) 3.54(2) 1_555 2_565 ? N(1) N(7) 3.330(7) 1_555 2_655 ? N(6) N(7) 3.475(7) 1_555 2_655 ? #------------------------------------------------------------------------------ #===END