#------------------------------------------------------------------------------ #$Date: 2013-08-29 18:37:19 +0300 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/21/60/2216059.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2216059 loop_ _publ_author_name 'Yu, Fengli' 'Zhou, Jin' 'Li, Xiaoyan' _publ_section_title ;Bis(2-hydroxybenzonitrile-\kN)dimethylbis(trimethylphosphine-\kP)cobalt(III) iodide ; _journal_coeditor_code LX2017 _journal_issue 11 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m2787 _journal_page_last m2787 _journal_volume 63 _journal_year 2007 _chemical_formula_iupac '[Co (C H3)2 (C7 H5 N O)2 (C3 H9 P)2] I' _chemical_formula_moiety ' C22 H34 Co N2 O2 P2 +, I -' _chemical_formula_sum 'C22 H34 Co I N2 O2 P2' _chemical_formula_weight 606.28 _chemical_name_systematic ; Bis(2-hydroxybenzonitrile-\kN)dimethylbis(trimethylphosphine-\kP)cobalt(III) iodide ; _space_group_IT_number 62 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_space_group_name_H-M 'P n m a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 13.749(6) _cell_length_b 13.817(6) _cell_length_c 14.771(7) _cell_measurement_reflns_used 2687 _cell_measurement_temperature 294(2) _cell_measurement_theta_max 22.08 _cell_measurement_theta_min 2.50 _cell_volume 2806(2) _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_collection 'SMART (Bruker, 1997)' _computing_data_reduction 'SAINT (Bruker, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 2001)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 294(2) _diffrn_detector_area_resol_mean 10 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'Bruker SMART CCD area-detector' _diffrn_measurement_method '\f and \w' _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 0.0674 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 15120 _diffrn_reflns_theta_full 26.36 _diffrn_reflns_theta_max 26.36 _diffrn_reflns_theta_min 2.02 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.844 _exptl_absorpt_correction_T_max 0.7568 _exptl_absorpt_correction_T_min 0.6871 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour Yellow _exptl_crystal_density_diffrn 1.435 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1224 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _refine_diff_density_max 0.732 _refine_diff_density_min -0.458 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 149 _refine_ls_number_reflns 2980 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.987 _refine_ls_R_factor_all 0.0962 _refine_ls_R_factor_gt 0.0389 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+2.8161P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0796 _refine_ls_wR_factor_ref 0.1015 _reflns_number_gt 1677 _reflns_number_total 2980 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file lx2017.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_Hall -p_2ac_2n _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2216059 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy Co Co 0.51637(6) 0.7500 0.12124(5) 0.0395(2) Uani d S 1 I I 0.35233(4) 0.2500 0.38891(3) 0.0675(2) Uani d S 1 P P1 0.52454(12) 0.7500 -0.02964(11) 0.0497(4) Uani d S 1 P P2 0.53498(15) 0.7500 0.27142(12) 0.0614(5) Uani d S 1 N N 0.4156(3) 0.6501(3) 0.1238(2) 0.0441(9) Uani d . 1 O O 0.3357(3) 0.4629(3) 0.2627(3) 0.0831(13) Uani d . 1 H H1 0.338(3) 0.412(4) 0.298(3) 0.071(17) Uiso d . 1 C C1 0.3565(3) 0.5930(3) 0.1243(3) 0.0451(10) Uani d . 1 C C2 0.2783(3) 0.5229(3) 0.1237(3) 0.0484(11) Uani d . 1 C C3 0.2679(4) 0.4589(3) 0.1967(4) 0.0570(13) Uani d . 1 C C4 0.1891(4) 0.3960(4) 0.1970(4) 0.0737(16) Uani d . 1 H H4 0.1798 0.3543 0.2456 0.088 Uiso calc R 1 C C5 0.1248(4) 0.3953(4) 0.1259(5) 0.087(2) Uani d . 1 H H5 0.0723 0.3528 0.1269 0.104 Uiso calc R 1 C C6 0.1366(4) 0.4564(4) 0.0530(5) 0.0834(18) Uani d . 1 H H6 0.0932 0.4541 0.0049 0.100 Uiso calc R 1 C C7 0.2130(4) 0.5209(4) 0.0517(4) 0.0692(15) Uani d . 1 H H7 0.2210 0.5628 0.0030 0.083 Uiso calc R 1 C C8 0.6466(5) 0.7500 -0.0769(5) 0.076(2) Uani d S 1 H H8A 0.6775 0.8109 -0.0643 0.115 Uiso calc PR 0.50 H H8B 0.6431 0.7405 -0.1412 0.115 Uiso calc PR 0.50 H H8C 0.6838 0.6986 -0.0501 0.115 Uiso calc PR 0.50 C C9 0.4688(4) 0.8524(4) -0.0866(3) 0.0831(18) Uani d . 1 H H9A 0.4841 0.8501 -0.1500 0.125 Uiso calc R 1 H H9B 0.4933 0.9115 -0.0611 0.125 Uiso calc R 1 H H9C 0.3995 0.8497 -0.0788 0.125 Uiso calc R 1 C C10 0.6603(6) 0.7500 0.3117(5) 0.093(3) Uani d S 1 H H10A 0.6612 0.7633 0.3754 0.139 Uiso calc PR 0.50 H H10B 0.6966 0.7989 0.2802 0.139 Uiso calc PR 0.50 H H10C 0.6890 0.6878 0.3006 0.139 Uiso calc PR 0.50 C C11 0.4839(5) 0.8528(5) 0.3307(4) 0.111(2) Uani d . 1 H H11A 0.4142 0.8492 0.3289 0.166 Uiso calc R 1 H H11B 0.5049 0.9115 0.3021 0.166 Uiso calc R 1 H H11C 0.5054 0.8522 0.3925 0.166 Uiso calc R 1 C C12 0.6168(3) 0.8572(3) 0.1187(3) 0.0610(13) Uani d . 1 H H12A 0.6079 0.8957 0.0652 0.091 Uiso calc R 1 H H12B 0.6808 0.8295 0.1184 0.091 Uiso calc R 1 H H12C 0.6092 0.8974 0.1713 0.091 Uiso calc R 1 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 0.0443(5) 0.0331(4) 0.0411(5) 0.000 -0.0009(4) 0.000 I 0.0849(4) 0.0531(3) 0.0645(3) 0.000 -0.0021(3) 0.000 P1 0.0541(11) 0.0531(11) 0.0420(10) 0.000 0.0048(8) 0.000 P2 0.0831(15) 0.0558(12) 0.0452(11) 0.000 -0.0119(10) 0.000 N 0.054(2) 0.0358(19) 0.043(2) -0.0006(18) -0.0003(18) 0.0010(16) O 0.102(3) 0.073(3) 0.075(3) -0.031(2) -0.010(2) 0.025(2) C1 0.053(3) 0.034(2) 0.048(3) 0.002(2) 0.001(2) 0.003(2) C2 0.045(3) 0.036(2) 0.065(3) -0.003(2) 0.004(2) -0.005(2) C3 0.056(3) 0.042(3) 0.073(4) -0.005(3) 0.015(3) -0.001(2) C4 0.066(4) 0.050(3) 0.105(5) -0.015(3) 0.028(4) 0.002(3) C5 0.048(3) 0.051(3) 0.162(7) -0.013(3) 0.007(4) -0.010(4) C6 0.064(4) 0.059(4) 0.127(5) -0.005(3) -0.026(4) -0.014(4) C7 0.070(4) 0.055(3) 0.082(4) -0.001(3) -0.020(3) 0.002(3) C8 0.070(5) 0.086(6) 0.074(5) 0.000 0.025(4) 0.000 C9 0.102(4) 0.095(4) 0.052(3) 0.030(4) 0.006(3) 0.017(3) C10 0.113(7) 0.081(6) 0.084(6) 0.000 -0.048(5) 0.000 C11 0.160(6) 0.118(6) 0.054(4) 0.040(5) -0.006(4) -0.030(4) C12 0.059(3) 0.051(3) 0.073(3) -0.016(2) -0.004(3) -0.007(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle N Co N . 8_575 89.8(2) N Co C12 . . 177.90(17) N Co C12 8_575 . 88.08(18) N Co C12 8_575 8_575 177.90(17) C12 Co C12 . 8_575 94.0(3) N Co P1 . . 93.14(10) C12 Co P1 . . 86.96(14) N Co P2 . . 93.57(10) C12 Co P2 . . 86.59(14) P1 Co P2 . . 170.53(8) N Co C1 8_575 . 89.53(13) C12 Co C1 . . 177.60(16) C12 Co C1 8_575 . 88.36(16) P1 Co C1 . . 92.88(8) P2 Co C1 . . 93.85(9) C9 P1 C9 8_575 . 102.4(4) C9 P1 C8 . . 102.2(2) C9 P1 Co . . 116.20(17) C8 P1 Co . . 115.5(3) C11 P2 C11 8_575 . 103.3(5) C11 P2 C10 . . 102.1(3) C11 P2 Co . . 115.8(2) C10 P2 Co . . 115.6(3) C1 N Co . . 179.0(4) C3 O H1 . . 114(3) N C1 C2 . . 177.7(5) C2 C1 Co . . 177.1(3) C7 C2 C3 . . 120.6(4) C7 C2 C1 . . 119.8(4) C3 C2 C1 . . 119.5(4) O C3 C4 . . 124.2(5) O C3 C2 . . 117.3(4) C4 C3 C2 . . 118.4(5) C5 C4 C3 . . 120.3(5) C5 C4 H4 . . 119.8 C3 C4 H4 . . 119.8 C4 C5 C6 . . 121.1(5) C4 C5 H5 . . 119.4 C6 C5 H5 . . 119.4 C7 C6 C5 . . 119.9(6) C7 C6 H6 . . 120.1 C5 C6 H6 . . 120.1 C6 C7 C2 . . 119.6(5) C6 C7 H7 . . 120.2 C2 C7 H7 . . 120.2 P1 C8 H8A . . 109.5 P1 C8 H8B . . 109.5 H8A C8 H8B . . 109.5 P1 C8 H8C . . 109.5 H8A C8 H8C . . 109.5 H8B C8 H8C . . 109.5 P1 C9 H9A . . 109.5 P1 C9 H9B . . 109.5 H9A C9 H9B . . 109.5 P1 C9 H9C . . 109.5 H9A C9 H9C . . 109.5 H9B C9 H9C . . 109.5 P2 C10 H10A . . 109.5 P2 C10 H10B . . 109.5 H10A C10 H10B . . 109.5 P2 C10 H10C . . 109.5 H10A C10 H10C . . 109.5 H10B C10 H10C . . 109.5 P2 C11 H11A . . 109.5 P2 C11 H11B . . 109.5 H11A C11 H11B . . 109.5 P2 C11 H11C . . 109.5 H11A C11 H11C . . 109.5 H11B C11 H11C . . 109.5 Co C12 H12A . . 109.5 Co C12 H12B . . 109.5 H12A C12 H12B . . 109.5 Co C12 H12C . . 109.5 H12A C12 H12C . . 109.5 H12B C12 H12C . . 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance Co N . 1.956(4) Co N 8_575 1.956(4) Co C12 . 2.026(4) Co C12 8_575 2.026(4) Co P1 . 2.232(2) Co P2 . 2.233(2) Co C1 . 3.089(5) P1 C9 8_575 1.816(5) P1 C9 . 1.816(5) P1 C8 . 1.818(7) P2 C11 8_575 1.810(6) P2 C11 . 1.810(6) P2 C10 . 1.822(7) N C1 . 1.133(5) O C3 . 1.350(6) O H1 . 0.88(5) C1 C2 . 1.447(6) C2 C7 . 1.391(6) C2 C3 . 1.402(6) C3 C4 . 1.389(6) C4 C5 . 1.372(7) C4 H4 . 0.9300 C5 C6 . 1.378(8) C5 H5 . 0.9300 C6 C7 . 1.377(7) C6 H6 . 0.9300 C7 H7 . 0.9300 C8 H8A . 0.9600 C8 H8B . 0.9600 C8 H8C . 0.9600 C9 H9A . 0.9600 C9 H9B . 0.9600 C9 H9C . 0.9600 C10 H10A . 0.9600 C10 H10B . 0.9600 C10 H10C . 0.9600 C11 H11A . 0.9600 C11 H11B . 0.9600 C11 H11C . 0.9600 C12 H12A . 0.9600 C12 H12B . 0.9600 C12 H12C . 0.9600 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA O H1 I 0.88(5) 2.62(5) 3.490(4) 175(4) loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_4 _geom_torsion N Co P1 C9 . 8_575 -15.3(2) N Co P1 C9 8_575 8_575 -105.3(3) C12 Co P1 C9 . 8_575 166.8(3) C12 Co P1 C9 8_575 8_575 72.6(3) C1 Co P1 C9 . 8_575 -15.6(2) N Co P1 C9 . . 105.3(3) N Co P1 C9 8_575 . 15.3(2) C12 Co P1 C9 . . -72.6(3) C12 Co P1 C9 8_575 . -166.8(3) C1 Co P1 C9 . . 105.0(2) N Co P1 C8 . . -135.01(10) N Co P1 C8 8_575 . 135.01(10) C12 Co P1 C8 . . 47.10(14) C12 Co P1 C8 8_575 . -47.10(14) C1 Co P1 C8 . . -135.30(8) N Co P2 C11 . 8_575 15.6(3) N Co P2 C11 8_575 8_575 105.7(3) C12 Co P2 C11 . 8_575 -166.5(3) C12 Co P2 C11 8_575 8_575 -72.2(3) C1 Co P2 C11 . 8_575 15.9(3) N Co P2 C11 . . -105.7(3) N Co P2 C11 8_575 . -15.6(3) C12 Co P2 C11 . . 72.2(3) C12 Co P2 C11 8_575 . 166.5(3) C1 Co P2 C11 . . -105.4(3) N Co P2 C10 . . 134.98(10) N Co P2 C10 8_575 . -134.98(10) C12 Co P2 C10 . . -47.12(14) C12 Co P2 C10 8_575 . 47.12(14) C1 Co P2 C10 . . 135.24(8) C7 C2 C3 O . . 177.9(4) C1 C2 C3 O . . -3.4(6) C7 C2 C3 C4 . . -2.3(7) C1 C2 C3 C4 . . 176.4(4) O C3 C4 C5 . . -178.4(5) C2 C3 C4 C5 . . 1.8(7) C3 C4 C5 C6 . . -0.1(9) C4 C5 C6 C7 . . -1.2(9) C5 C6 C7 C2 . . 0.7(8) C3 C2 C7 C6 . . 1.1(7) C1 C2 C7 C6 . . -177.6(5) _cod_database_fobs_code 2216059