Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _audit_creation_date 10-03-06 _publ_contact_author_name 'Pierre Braunstein' _publ_contact_author_address ; Institut Le Bel, rue Blaise Pascal, 67000 STRASBOURG, FRANCE ; _publ_contact_author_phone 0390241308 _publ_contact_author_fax 0390241322 _publ_contact_author_email braunstein@chimie.u-strasbg.fr _publ_contact_letter ; ; _publ_requested_category FM _publ_section_title ; Mono- and dinuclear cobalt complexes with bidentate P,N phosphino- and phosphinito-oxazoline ligands. ; loop_ _publ_author_name _publ_author_address 'Jie Suyun.' ; Laboratoire de Chimie de Coordination, UMR CNRS 7177 Universit\'e Louis Pasteur 4, rue Blaise Pascal 67000 STRASBOURG, France ; M.Agostinho ; Laboratoire de Chimie de Coordination, UMR CNRS 7177 Universit\'e Louis Pasteur 4, rue Blaise Pascal 67000 STRASBOURG, France ; A.Kermagoret ; Laboratoire de Chimie de Coordination, UMR CNRS 7177 Universit\'e Louis Pasteur 4, rue Blaise Pascal 67000 STRASBOURG, France ; C.Cazin ; Laboratoire de Chimie de Coordination, UMR CNRS 7177 Universit\'e Louis Pasteur 4, rue Blaise Pascal 67000 STRASBOURG, France ; P.Braunstein ; Laboratoire de Chimie de Coordination, UMR CNRS 7177 Universit\'e Louis Pasteur 4, rue Blaise Pascal 67000 STRASBOURG, France ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. Dowty, E. (1994). ATOMS for Mac. Version 3.0. Shape Software, 521 Hidden Valley Road, Kingsport, TN 37663, E-U. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. Sheldrick, G.M. (1997). SHELXL97. Program for the refinement of crystal structures. University of Gottingen. Germany. Spek, A.L., PLATON 98, Utrecht University, The Netherland, 1998. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; data_6 _database_code_depnum_ccdc_archive 'CCDC 646279' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H40 Cl4 Co2 N2 O2 P2' _chemical_formula_sum 'C20 H40 Cl4 Co2 N2 O2 P2' _chemical_formula_weight 662.14 _chemical_absolute_configuration ? 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.4010(4) _cell_length_b 9.8100(4) _cell_length_c 14.2570(5) _cell_angle_alpha 90.00 _cell_angle_beta 122.6151(16) _cell_angle_gamma 90.00 _cell_volume 1460.92(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3012 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 29.131 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 684 _exptl_absorpt_coefficient_mu 1.631 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6273 _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_sigmaI/netI 0.0660 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 29.05 _reflns_number_total 3896 _reflns_number_gt 2586 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of 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 based 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. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors 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 'calc w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+1.1651P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3896 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0857 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1135 _refine_ls_wR_factor_gt 0.0974 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.12493(4) 0.50841(4) -0.07791(3) 0.02804(13) Uani 1 1 d . . . Cl1 Cl 0.18950(8) 0.53360(9) -0.19635(7) 0.0390(2) Uani 1 1 d . . . Cl2 Cl 0.16522(8) 0.30576(7) 0.00819(7) 0.0334(2) Uani 1 1 d . . . P P 0.24643(7) 0.65263(8) 0.08352(7) 0.0281(2) Uani 1 1 d . . . O O 0.27672(19) 0.4519(2) 0.28510(17) 0.0324(5) Uani 1 1 d . . . N N 0.0630(2) 0.4473(3) 0.1755(2) 0.0294(6) Uani 1 1 d . . . C1 C 0.1794(3) 0.6501(3) 0.1732(3) 0.0304(7) Uani 1 1 d . . . H1A H 0.2353 0.7056 0.2405 0.037 Uiso 1 1 calc . . . H1B H 0.0939 0.6937 0.1322 0.037 Uiso 1 1 calc . . . C2 C 0.1668(3) 0.5124(3) 0.2084(2) 0.0263(6) Uani 1 1 d . . . C3 C 0.2436(3) 0.3167(3) 0.3054(3) 0.0377(8) Uani 1 1 d . . . H3A H 0.2763 0.3040 0.3853 0.045 Uiso 1 1 calc . . . H3B H 0.2792 0.2443 0.2814 0.045 Uiso 1 1 calc . . . C4 C 0.0988(3) 0.3145(4) 0.2359(3) 0.0436(9) Uani 1 1 d . . . H4A H 0.0667 0.2372 0.1830 0.052 Uiso 1 1 calc . . . H4B H 0.0638 0.3072 0.2838 0.052 Uiso 1 1 calc . . . C5 C 0.2648(3) 0.8379(3) 0.0733(3) 0.0395(8) Uani 1 1 d . . . H5 H 0.3171 0.8746 0.1509 0.047 Uiso 1 1 calc . . . C6 C 0.1362(4) 0.9108(4) 0.0148(4) 0.0604(11) Uani 1 1 d . . . H6A H 0.1502 1.0096 0.0209 0.091 Uiso 1 1 calc . . . H6B H 0.0894 0.8852 0.0498 0.091 Uiso 1 1 calc . . . H6C H 0.0863 0.8845 -0.0639 0.091 Uiso 1 1 calc . . . C7 C 0.3376(5) 0.8670(4) 0.0167(4) 0.0663(13) Uani 1 1 d . . . H7A H 0.3119 0.8011 -0.0435 0.099 Uiso 1 1 calc . . . H7B H 0.4298 0.8591 0.0713 0.099 Uiso 1 1 calc . . . H7C H 0.3178 0.9595 -0.0142 0.099 Uiso 1 1 calc . . . C8 C 0.4098(3) 0.5816(3) 0.1728(3) 0.0340(7) Uani 1 1 d . . . H8 H 0.3992 0.4940 0.2028 0.041 Uiso 1 1 calc . . . C9 C 0.4671(3) 0.5427(4) 0.1046(3) 0.0472(9) Uani 1 1 d . . . H9A H 0.4788 0.6250 0.0720 0.071 Uiso 1 1 calc . . . H9B H 0.4092 0.4799 0.0450 0.071 Uiso 1 1 calc . . . H9C H 0.5502 0.4984 0.1532 0.071 Uiso 1 1 calc . . . C10 C 0.4999(3) 0.6678(4) 0.2741(3) 0.0505(10) Uani 1 1 d . . . H10A H 0.5816 0.6198 0.3200 0.076 Uiso 1 1 calc . . . H10B H 0.4615 0.6838 0.3178 0.076 Uiso 1 1 calc . . . H10C H 0.5148 0.7553 0.2498 0.076 Uiso 1 1 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.0269(2) 0.0245(2) 0.0351(3) 0.00313(18) 0.01827(19) 0.00154(18) Cl1 0.0429(5) 0.0381(5) 0.0481(5) 0.0053(4) 0.0324(4) 0.0017(4) Cl2 0.0406(4) 0.0236(4) 0.0374(4) 0.0039(3) 0.0219(4) 0.0033(3) P 0.0284(4) 0.0246(4) 0.0334(5) 0.0026(3) 0.0181(4) 0.0001(3) O 0.0274(11) 0.0327(12) 0.0337(12) 0.0054(10) 0.0141(10) 0.0001(10) N 0.0299(14) 0.0246(13) 0.0386(15) 0.0042(11) 0.0216(12) 0.0010(11) C1 0.0307(16) 0.0258(16) 0.0375(18) -0.0027(14) 0.0202(15) 0.0004(13) C2 0.0286(15) 0.0281(16) 0.0274(15) 0.0004(13) 0.0185(13) 0.0009(13) C3 0.0372(18) 0.0323(18) 0.045(2) 0.0129(15) 0.0227(17) 0.0027(15) C4 0.0318(18) 0.0383(19) 0.052(2) 0.0199(17) 0.0167(17) 0.0039(16) C5 0.053(2) 0.0275(17) 0.0377(19) 0.0000(15) 0.0238(18) -0.0068(16) C6 0.065(3) 0.0255(19) 0.072(3) 0.0115(19) 0.024(2) 0.0058(19) C7 0.106(4) 0.043(2) 0.076(3) 0.007(2) 0.066(3) -0.013(2) C8 0.0267(16) 0.0387(19) 0.0354(18) 0.0051(15) 0.0161(14) 0.0014(14) C9 0.0325(18) 0.062(2) 0.053(2) 0.002(2) 0.0275(17) 0.0041(18) C10 0.0341(18) 0.057(2) 0.045(2) -0.0040(19) 0.0108(17) -0.0062(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co N 2.015(2) 3_565 ? Co Cl1 2.2385(9) . ? Co Cl2 2.2466(8) . ? Co P 2.4147(9) . ? P C5 1.847(3) . ? P C8 1.852(3) . ? P C1 1.863(3) . ? O C2 1.341(4) . ? O C3 1.462(4) . ? N C2 1.278(4) . ? N C4 1.491(4) . ? N Co 2.015(2) 3_565 ? C1 C2 1.479(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C3 C4 1.513(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.521(5) . ? C5 C7 1.528(5) . ? C5 H5 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C10 1.520(5) . ? C8 C9 1.530(5) . ? C8 H8 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N Co Cl1 101.88(8) 3_565 . ? N Co Cl2 113.70(7) 3_565 . ? Cl1 Co Cl2 116.44(3) . . ? N Co P 115.30(8) 3_565 . ? Cl1 Co P 111.17(3) . . ? Cl2 Co P 99.03(3) . . ? C5 P C8 106.79(16) . . ? C5 P C1 100.75(15) . . ? C8 P C1 104.53(14) . . ? C5 P Co 122.78(12) . . ? C8 P Co 108.90(11) . . ? C1 P Co 111.49(10) . . ? C2 O C3 107.0(2) . . ? C2 N C4 107.3(3) . . ? C2 N Co 135.0(2) . 3_565 ? C4 N Co 117.43(19) . 3_565 ? C2 C1 P 114.4(2) . . ? C2 C1 H1A 108.7 . . ? P C1 H1A 108.7 . . ? C2 C1 H1B 108.7 . . ? P C1 H1B 108.7 . . ? H1A C1 H1B 107.6 . . ? N C2 O 117.3(3) . . ? N C2 C1 127.0(3) . . ? O C2 C1 115.7(3) . . ? O C3 C4 104.1(2) . . ? O C3 H3A 110.9 . . ? C4 C3 H3A 110.9 . . ? O C3 H3B 110.9 . . ? C4 C3 H3B 110.9 . . ? H3A C3 H3B 108.9 . . ? N C4 C3 104.2(3) . . ? N C4 H4A 110.9 . . ? C3 C4 H4A 110.9 . . ? N C4 H4B 110.9 . . ? C3 C4 H4B 110.9 . . ? H4A C4 H4B 108.9 . . ? C6 C5 C7 111.4(3) . . ? C6 C5 P 111.6(2) . . ? C7 C5 P 111.0(3) . . ? C6 C5 H5 107.5 . . ? C7 C5 H5 107.5 . . ? P C5 H5 107.5 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C10 C8 C9 112.8(3) . . ? C10 C8 P 114.5(2) . . ? C9 C8 P 111.6(2) . . ? C10 C8 H8 105.7 . . ? C9 C8 H8 105.7 . . ? P C8 H8 105.7 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N Co P C5 -62.40(16) 3_565 . . . ? Cl1 Co P C5 52.90(14) . . . . ? Cl2 Co P C5 175.92(14) . . . . ? N Co P C8 171.90(13) 3_565 . . . ? Cl1 Co P C8 -72.80(11) . . . . ? Cl2 Co P C8 50.22(11) . . . . ? N Co P C1 57.08(13) 3_565 . . . ? Cl1 Co P C1 172.37(11) . . . . ? Cl2 Co P C1 -64.61(11) . . . . ? C5 P C1 C2 -173.4(2) . . . . ? C8 P C1 C2 -62.7(3) . . . . ? Co P C1 C2 54.8(2) . . . . ? C4 N C2 O -0.6(4) . . . . ? Co N C2 O 172.6(2) 3_565 . . . ? C4 N C2 C1 -178.9(3) . . . . ? Co N C2 C1 -5.7(5) 3_565 . . . ? C3 O C2 N 3.3(4) . . . . ? C3 O C2 C1 -178.2(2) . . . . ? P C1 C2 N -109.2(3) . . . . ? P C1 C2 O 72.4(3) . . . . ? C2 O C3 C4 -4.3(3) . . . . ? C2 N C4 C3 -2.3(3) . . . . ? Co N C4 C3 -176.8(2) 3_565 . . . ? O C3 C4 N 3.9(3) . . . . ? C8 P C5 C6 -172.3(3) . . . . ? C1 P C5 C6 -63.4(3) . . . . ? Co P C5 C6 61.1(3) . . . . ? C8 P C5 C7 62.7(3) . . . . ? C1 P C5 C7 171.6(3) . . . . ? Co P C5 C7 -63.9(3) . . . . ? C5 P C8 C10 41.6(3) . . . . ? C1 P C8 C10 -64.6(3) . . . . ? Co P C8 C10 176.1(2) . . . . ? C5 P C8 C9 -88.0(3) . . . . ? C1 P C8 C9 165.7(2) . . . . ? Co P C8 C9 46.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 29.05 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.999 _refine_diff_density_min -0.777 _refine_diff_density_rms 0.099 # Attachment 'final_7.CIF' data_7 _database_code_depnum_ccdc_archive 'CCDC 646280' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H32 Cl4 Co2 N2 O2 P2' _chemical_formula_sum 'C32 H32 Cl4 Co2 N2 O2 P2' _chemical_formula_weight 798.20 _chemical_absolute_configuration ? 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.1310(4) _cell_length_b 10.0750(3) _cell_length_c 13.4300(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.3060(11) _cell_angle_gamma 90.00 _cell_volume 1748.05(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4860 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 1.378 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9091 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0581 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 29.94 _reflns_number_total 5053 _reflns_number_gt 3541 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of 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 based 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. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors 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 'calc w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+1.0270P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5053 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0795 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1255 _refine_ls_wR_factor_gt 0.1126 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.38902(3) -0.01435(4) 0.12223(3) 0.03026(12) Uani 1 1 d . . . Cl1 Cl 0.27480(6) 0.03486(8) 0.22120(6) 0.0430(2) Uani 1 1 d . . . Cl2 Cl 0.51164(5) -0.16313(8) 0.17764(6) 0.0424(2) Uani 1 1 d . . . P P 0.70512(5) 0.11819(7) 0.02891(5) 0.02930(17) Uani 1 1 d . . . O O 0.52970(14) 0.34494(19) 0.06457(17) 0.0379(5) Uani 1 1 d . . . N N 0.43738(15) 0.1647(2) 0.08727(18) 0.0290(5) Uani 1 1 d . . . C1 C 0.62773(19) 0.1530(3) 0.1284(2) 0.0325(6) Uani 1 1 d . . . H1A H 0.6150 0.0683 0.1614 0.039 Uiso 1 1 calc . . . H1B H 0.6690 0.2103 0.1804 0.039 Uiso 1 1 calc . . . C2 C 0.52647(19) 0.2184(3) 0.0918(2) 0.0290(6) Uani 1 1 d . . . C3 C 0.4220(2) 0.3871(3) 0.0314(3) 0.0456(8) Uani 1 1 d . . . H3A H 0.4073 0.4036 -0.0425 0.055 Uiso 1 1 calc . . . H3B H 0.4070 0.4688 0.0671 0.055 Uiso 1 1 calc . . . C4 C 0.3592(2) 0.2713(3) 0.0589(2) 0.0379(7) Uani 1 1 d . . . H4A H 0.3247 0.2940 0.1165 0.046 Uiso 1 1 calc . . . H4B H 0.3061 0.2440 0.0006 0.046 Uiso 1 1 calc . . . C5 C 0.81114(19) 0.0224(3) 0.1008(2) 0.0296(6) Uani 1 1 d . . . C6 C 0.7899(2) -0.0908(3) 0.1541(2) 0.0350(6) Uani 1 1 d . . . H6 H 0.7201 -0.1151 0.1547 0.042 Uiso 1 1 calc . . . C7 C 0.8697(2) -0.1680(3) 0.2061(2) 0.0399(7) Uani 1 1 d . . . H7 H 0.8545 -0.2446 0.2421 0.048 Uiso 1 1 calc . . . C8 C 0.9712(2) -0.1330(3) 0.2055(3) 0.0463(8) Uani 1 1 d . . . H8 H 1.0259 -0.1853 0.2415 0.056 Uiso 1 1 calc . . . C9 C 0.9935(2) -0.0234(4) 0.1531(3) 0.0487(8) Uani 1 1 d . . . H9 H 1.0636 -0.0007 0.1524 0.058 Uiso 1 1 calc . . . C10 C 0.9143(2) 0.0552(3) 0.1007(2) 0.0398(7) Uani 1 1 d . . . H10 H 0.9306 0.1312 0.0648 0.048 Uiso 1 1 calc . . . C11 C 0.76451(18) 0.2733(3) 0.0012(2) 0.0303(6) Uani 1 1 d . . . C12 C 0.7942(2) 0.2869(3) -0.0926(2) 0.0413(7) Uani 1 1 d . . . H12 H 0.7801 0.2177 -0.1411 0.050 Uiso 1 1 calc . . . C13 C 0.8441(3) 0.4009(4) -0.1157(2) 0.0485(8) Uani 1 1 d . . . H13 H 0.8642 0.4096 -0.1799 0.058 Uiso 1 1 calc . . . C14 C 0.8648(2) 0.5018(3) -0.0457(3) 0.0433(8) Uani 1 1 d . . . H14 H 0.8987 0.5800 -0.0618 0.052 Uiso 1 1 calc . . . C15 C 0.8363(3) 0.4893(3) 0.0473(3) 0.0457(8) Uani 1 1 d . . . H15 H 0.8509 0.5586 0.0957 0.055 Uiso 1 1 calc . . . C16 C 0.7862(2) 0.3750(3) 0.0706(2) 0.0402(7) Uani 1 1 d . . . H16 H 0.7667 0.3667 0.1351 0.048 Uiso 1 1 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.02296(19) 0.0301(2) 0.0391(2) 0.00571(16) 0.00920(14) 0.00006(14) Cl1 0.0349(4) 0.0461(5) 0.0532(5) 0.0003(4) 0.0219(3) -0.0023(3) Cl2 0.0322(4) 0.0411(4) 0.0542(5) 0.0145(3) 0.0087(3) 0.0073(3) P 0.0206(3) 0.0302(4) 0.0380(4) 0.0043(3) 0.0078(3) -0.0007(3) O 0.0266(10) 0.0289(11) 0.0587(13) 0.0092(9) 0.0090(8) -0.0011(8) N 0.0231(10) 0.0271(12) 0.0381(13) 0.0037(10) 0.0087(8) 0.0012(9) C1 0.0233(12) 0.0369(16) 0.0393(15) 0.0089(12) 0.0109(10) 0.0023(10) C2 0.0270(13) 0.0317(15) 0.0298(14) 0.0042(11) 0.0088(10) 0.0013(10) C3 0.0314(15) 0.0356(17) 0.070(2) 0.0132(16) 0.0099(14) 0.0061(12) C4 0.0254(13) 0.0284(15) 0.059(2) 0.0058(14) 0.0055(12) 0.0040(11) C5 0.0220(12) 0.0346(15) 0.0321(14) -0.0024(12) 0.0048(10) 0.0017(10) C6 0.0307(14) 0.0335(16) 0.0414(16) 0.0023(13) 0.0082(11) 0.0000(11) C7 0.0439(17) 0.0338(17) 0.0421(17) 0.0014(13) 0.0074(13) 0.0051(13) C8 0.0355(16) 0.048(2) 0.053(2) 0.0013(16) 0.0004(13) 0.0159(14) C9 0.0221(14) 0.057(2) 0.066(2) 0.0069(18) 0.0065(13) 0.0048(13) C10 0.0271(14) 0.0421(18) 0.0516(18) 0.0073(15) 0.0106(12) 0.0017(12) C11 0.0213(12) 0.0319(15) 0.0382(15) 0.0036(12) 0.0066(10) -0.0011(10) C12 0.0485(17) 0.0376(18) 0.0388(17) -0.0028(14) 0.0106(13) -0.0128(14) C13 0.060(2) 0.046(2) 0.0422(18) 0.0065(15) 0.0146(15) -0.0134(16) C14 0.0336(16) 0.0345(18) 0.061(2) 0.0077(15) 0.0073(14) -0.0068(12) C15 0.0442(18) 0.0342(17) 0.059(2) -0.0090(15) 0.0107(15) -0.0088(13) C16 0.0441(16) 0.0395(18) 0.0397(17) -0.0048(14) 0.0149(13) -0.0067(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co N 1.996(2) . ? Co Cl2 2.2281(8) . ? Co Cl1 2.2306(8) . ? Co P 2.4176(8) 3_655 ? P C11 1.815(3) . ? P C5 1.823(3) . ? P C1 1.851(3) . ? P Co 2.4176(8) 3_655 ? O C2 1.329(3) . ? O C3 1.467(3) . ? N C2 1.281(3) . ? N C4 1.487(3) . ? C1 C2 1.487(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C3 C4 1.513(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C10 1.395(4) . ? C5 C6 1.401(4) . ? C6 C7 1.389(4) . ? C6 H6 0.9500 . ? C7 C8 1.381(4) . ? C7 H7 0.9500 . ? C8 C9 1.369(5) . ? C8 H8 0.9500 . ? C9 C10 1.393(4) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C16 1.379(4) . ? C11 C12 1.391(4) . ? C12 C13 1.385(4) . ? C12 H12 0.9500 . ? C13 C14 1.378(5) . ? C13 H13 0.9500 . ? C14 C15 1.372(5) . ? C14 H14 0.9500 . ? C15 C16 1.389(4) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N Co Cl2 116.44(6) . . ? N Co Cl1 102.44(7) . . ? Cl2 Co Cl1 118.25(3) . . ? N Co P 109.27(7) . 3_655 ? Cl2 Co P 102.69(3) . 3_655 ? Cl1 Co P 107.41(3) . 3_655 ? C11 P C5 104.44(12) . . ? C11 P C1 107.23(13) . . ? C5 P C1 100.60(12) . . ? C11 P Co 112.00(9) . 3_655 ? C5 P Co 116.29(9) . 3_655 ? C1 P Co 115.07(9) . 3_655 ? C2 O C3 106.6(2) . . ? C2 N C4 106.8(2) . . ? C2 N Co 134.23(19) . . ? C4 N Co 118.61(16) . . ? C2 C1 P 114.81(19) . . ? C2 C1 H1A 108.6 . . ? P C1 H1A 108.6 . . ? C2 C1 H1B 108.6 . . ? P C1 H1B 108.6 . . ? H1A C1 H1B 107.5 . . ? N C2 O 117.8(2) . . ? N C2 C1 125.7(2) . . ? O C2 C1 116.5(2) . . ? O C3 C4 103.9(2) . . ? O C3 H3A 111.0 . . ? C4 C3 H3A 111.0 . . ? O C3 H3B 111.0 . . ? C4 C3 H3B 111.0 . . ? H3A C3 H3B 109.0 . . ? N C4 C3 103.8(2) . . ? N C4 H4A 111.0 . . ? C3 C4 H4A 111.0 . . ? N C4 H4B 111.0 . . ? C3 C4 H4B 111.0 . . ? H4A C4 H4B 109.0 . . ? C10 C5 C6 118.4(2) . . ? C10 C5 P 121.6(2) . . ? C6 C5 P 119.92(19) . . ? C7 C6 C5 120.8(3) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C8 C7 C6 119.8(3) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C9 C8 C7 120.3(3) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C10 120.6(3) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C9 C10 C5 120.2(3) . . ? C9 C10 H10 119.9 . . ? C5 C10 H10 119.9 . . ? C16 C11 C12 118.8(3) . . ? C16 C11 P 123.1(2) . . ? C12 C11 P 118.1(2) . . ? C13 C12 C11 120.3(3) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C14 C13 C12 120.1(3) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C15 C14 C13 120.1(3) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 119.8(3) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C11 C16 C15 120.8(3) . . ? C11 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl2 Co N C2 -2.3(3) . . . . ? Cl1 Co N C2 128.3(3) . . . . ? P Co N C2 -118.0(3) 3_655 . . . ? Cl2 Co N C4 -174.49(18) . . . . ? Cl1 Co N C4 -43.9(2) . . . . ? P Co N C4 69.8(2) 3_655 . . . ? C11 P C1 C2 77.9(2) . . . . ? C5 P C1 C2 -173.3(2) . . . . ? Co P C1 C2 -47.4(2) 3_655 . . . ? C4 N C2 O -4.9(3) . . . . ? Co N C2 O -177.7(2) . . . . ? C4 N C2 C1 172.9(3) . . . . ? Co N C2 C1 0.1(4) . . . . ? C3 O C2 N -2.2(3) . . . . ? C3 O C2 C1 179.8(2) . . . . ? P C1 C2 N 110.3(3) . . . . ? P C1 C2 O -71.9(3) . . . . ? C2 O C3 C4 8.0(3) . . . . ? C2 N C4 C3 9.5(3) . . . . ? Co N C4 C3 -176.4(2) . . . . ? O C3 C4 N -10.4(3) . . . . ? C11 P C5 C10 -17.2(3) . . . . ? C1 P C5 C10 -128.2(3) . . . . ? Co P C5 C10 106.8(2) 3_655 . . . ? C11 P C5 C6 165.8(2) . . . . ? C1 P C5 C6 54.7(3) . . . . ? Co P C5 C6 -70.2(2) 3_655 . . . ? C10 C5 C6 C7 0.4(4) . . . . ? P C5 C6 C7 177.5(2) . . . . ? C5 C6 C7 C8 0.0(5) . . . . ? C6 C7 C8 C9 -0.6(5) . . . . ? C7 C8 C9 C10 0.7(5) . . . . ? C8 C9 C10 C5 -0.3(5) . . . . ? C6 C5 C10 C9 -0.3(5) . . . . ? P C5 C10 C9 -177.3(3) . . . . ? C5 P C11 C16 -79.6(3) . . . . ? C1 P C11 C16 26.6(3) . . . . ? Co P C11 C16 153.7(2) 3_655 . . . ? C5 P C11 C12 97.0(2) . . . . ? C1 P C11 C12 -156.8(2) . . . . ? Co P C11 C12 -29.7(2) 3_655 . . . ? C16 C11 C12 C13 -0.3(5) . . . . ? P C11 C12 C13 -177.0(3) . . . . ? C11 C12 C13 C14 0.0(5) . . . . ? C12 C13 C14 C15 0.3(5) . . . . ? C13 C14 C15 C16 -0.3(5) . . . . ? C12 C11 C16 C15 0.3(5) . . . . ? P C11 C16 C15 176.9(2) . . . . ? C14 C15 C16 C11 0.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 29.94 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.623 _refine_diff_density_min -0.777 _refine_diff_density_rms 0.084 data_shelxl _database_code_depnum_ccdc_archive 'CCDC 646281' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H20 Cl2 Co N O P' _chemical_formula_sum 'C18 H20 Cl2 Co N O P' _chemical_formula_weight 427.15 _chemical_absolute_configuration ? 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' Cl Cl 0.1484 0.1585 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.0690(2) _cell_length_b 28.7830(6) _cell_length_c 10.8560(2) _cell_angle_alpha 90.00 _cell_angle_beta 120.5011(9) _cell_angle_gamma 90.00 _cell_volume 1903.18(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4277 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 29.131 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 876 _exptl_absorpt_coefficient_mu 1.271 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8851 _diffrn_reflns_av_R_equivalents 0.0447 _diffrn_reflns_av_sigmaI/netI 0.0868 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 29.11 _reflns_number_total 5105 _reflns_number_gt 3092 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of 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 based 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. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors 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 'calc w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5105 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0997 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1162 _refine_ls_wR_factor_gt 0.0957 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 1.18629(6) 0.163388(11) 0.96839(4) 0.02338(12) Uani 1 1 d . . . Cl1 Cl 1.24866(13) 0.14005(2) 1.18119(7) 0.03176(19) Uani 1 1 d . . . Cl2 Cl 1.48755(14) 0.16986(3) 0.95451(9) 0.0439(2) Uani 1 1 d . . . P P 0.91529(13) 0.11690(2) 0.77642(8) 0.02361(18) Uani 1 1 d . . . O O 0.6187(3) 0.23880(6) 0.7331(2) 0.0310(5) Uani 1 1 d . . . N N 0.9591(4) 0.21359(7) 0.8852(2) 0.0229(5) Uani 1 1 d . . . C1 C 0.6838(5) 0.15865(8) 0.7107(3) 0.0256(6) Uani 1 1 d . . . H1A H 0.6142 0.1623 0.6058 0.031 Uiso 1 1 calc . . . H1B H 0.5719 0.1466 0.7316 0.031 Uiso 1 1 calc . . . C2 C 0.7657(5) 0.20464(9) 0.7817(3) 0.0240(6) Uani 1 1 d . . . C3 C 0.7315(6) 0.28010(10) 0.8186(4) 0.0430(9) Uani 1 1 d . . . H3A H 0.6533 0.2927 0.8655 0.052 Uiso 1 1 calc . . . H3B H 0.7407 0.3046 0.7580 0.052 Uiso 1 1 calc . . . C4 C 0.9612(5) 0.26295(9) 0.9303(3) 0.0255(6) Uani 1 1 d . . . C5 C 1.1414(6) 0.28975(9) 0.9258(3) 0.0353(8) Uani 1 1 d . . . H5A H 1.2832 0.2749 0.9891 0.053 Uiso 1 1 calc . . . H5B H 1.1441 0.3217 0.9577 0.053 Uiso 1 1 calc . . . H5C H 1.1139 0.2900 0.8278 0.053 Uiso 1 1 calc . . . C6 C 0.9984(6) 0.26257(10) 1.0805(3) 0.0370(8) Uani 1 1 d . . . H6A H 0.8833 0.2441 1.0823 0.056 Uiso 1 1 calc . . . H6B H 0.9938 0.2945 1.1104 0.056 Uiso 1 1 calc . . . H6C H 1.1422 0.2489 1.1460 0.056 Uiso 1 1 calc . . . C7 C 0.9467(5) 0.10321(8) 0.6243(3) 0.0259(6) Uani 1 1 d . . . C8 C 1.1492(5) 0.08581(10) 0.6534(3) 0.0330(7) Uani 1 1 d . . . H8 H 1.2655 0.0828 0.7496 0.040 Uiso 1 1 calc . . . C9 C 1.1819(5) 0.07285(11) 0.5422(4) 0.0427(9) Uani 1 1 d . . . H9 H 1.3193 0.0604 0.5627 0.051 Uiso 1 1 calc . . . C10 C 1.0154(6) 0.07809(10) 0.4021(4) 0.0404(8) Uani 1 1 d . . . H10 H 1.0391 0.0698 0.3263 0.048 Uiso 1 1 calc . . . C11 C 0.8144(6) 0.09543(10) 0.3720(3) 0.0358(8) Uani 1 1 d . . . H11 H 0.6996 0.0989 0.2755 0.043 Uiso 1 1 calc . . . C12 C 0.7799(5) 0.10782(9) 0.4830(3) 0.0277(7) Uani 1 1 d . . . H12 H 0.6409 0.1195 0.4619 0.033 Uiso 1 1 calc . . . C13 C 0.8098(5) 0.06408(9) 0.8113(3) 0.0252(6) Uani 1 1 d . . . C14 C 0.7552(5) 0.02460(9) 0.7252(3) 0.0332(7) Uani 1 1 d . . . H14 H 0.7682 0.0249 0.6423 0.040 Uiso 1 1 calc . . . C15 C 0.6823(6) -0.01504(9) 0.7606(4) 0.0403(8) Uani 1 1 d . . . H15 H 0.6436 -0.0418 0.7012 0.048 Uiso 1 1 calc . . . C16 C 0.6656(6) -0.01587(10) 0.8817(4) 0.0415(8) Uani 1 1 d . . . H16 H 0.6169 -0.0432 0.9062 0.050 Uiso 1 1 calc . . . C17 C 0.7191(6) 0.02284(11) 0.9670(4) 0.0391(8) Uani 1 1 d . . . H17 H 0.7063 0.0222 1.0500 0.047 Uiso 1 1 calc . . . C18 C 0.7917(5) 0.06281(10) 0.9327(3) 0.0337(7) Uani 1 1 d . . . H18 H 0.8292 0.0894 0.9925 0.040 Uiso 1 1 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.0218(2) 0.0231(2) 0.0230(2) -0.00030(15) 0.00970(18) 0.00184(16) Cl1 0.0366(5) 0.0286(4) 0.0258(4) 0.0038(3) 0.0127(3) 0.0029(3) Cl2 0.0317(5) 0.0588(5) 0.0482(5) -0.0156(4) 0.0255(4) -0.0085(4) P 0.0223(4) 0.0203(3) 0.0257(4) -0.0015(3) 0.0103(3) 0.0002(3) O 0.0250(12) 0.0228(10) 0.0338(12) -0.0023(8) 0.0067(10) 0.0041(8) N 0.0262(14) 0.0203(11) 0.0206(12) -0.0004(9) 0.0108(11) 0.0012(10) C1 0.0227(16) 0.0213(13) 0.0281(16) -0.0021(11) 0.0096(13) 0.0009(11) C2 0.0258(17) 0.0230(14) 0.0239(15) 0.0040(11) 0.0132(14) 0.0053(12) C3 0.038(2) 0.0237(15) 0.043(2) -0.0108(13) 0.0026(17) 0.0035(14) C4 0.0304(18) 0.0185(13) 0.0225(15) -0.0026(10) 0.0097(13) 0.0004(12) C5 0.044(2) 0.0241(14) 0.0376(18) -0.0037(13) 0.0211(17) -0.0057(14) C6 0.054(2) 0.0297(15) 0.0337(18) -0.0046(13) 0.0267(17) 0.0019(15) C7 0.0260(17) 0.0184(13) 0.0301(16) -0.0016(11) 0.0119(14) -0.0003(12) C8 0.0246(18) 0.0397(16) 0.0316(17) -0.0026(13) 0.0119(15) 0.0072(14) C9 0.031(2) 0.049(2) 0.049(2) -0.0073(16) 0.0202(18) 0.0103(15) C10 0.045(2) 0.0443(18) 0.038(2) -0.0120(15) 0.0254(18) -0.0017(16) C11 0.042(2) 0.0341(16) 0.0267(17) -0.0056(13) 0.0145(16) -0.0001(15) C12 0.0259(17) 0.0257(14) 0.0296(16) -0.0042(12) 0.0126(14) 0.0000(12) C13 0.0178(15) 0.0236(14) 0.0311(16) 0.0026(11) 0.0103(13) 0.0018(11) C14 0.0341(19) 0.0250(15) 0.0406(19) -0.0007(13) 0.0191(16) 0.0020(13) C15 0.042(2) 0.0214(15) 0.056(2) -0.0014(14) 0.0244(19) 0.0000(14) C16 0.035(2) 0.0293(16) 0.061(2) 0.0091(15) 0.0252(19) -0.0042(14) C17 0.040(2) 0.0400(18) 0.044(2) 0.0055(14) 0.0253(18) 0.0007(15) C18 0.0286(18) 0.0313(15) 0.0390(19) -0.0006(13) 0.0155(16) -0.0052(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co N 2.003(2) . ? Co Cl2 2.2177(9) . ? Co Cl1 2.2245(8) . ? Co P 2.3981(8) . ? P C13 1.816(3) . ? P C7 1.818(3) . ? P C1 1.856(3) . ? O C2 1.330(3) . ? O C3 1.470(3) . ? N C2 1.280(3) . ? N C4 1.500(3) . ? C1 C2 1.493(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C3 C4 1.534(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.511(4) . ? C4 C6 1.514(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C12 1.387(4) . ? C7 C8 1.393(4) . ? C8 C9 1.391(4) . ? C8 H8 0.9500 . ? C9 C10 1.380(4) . ? C9 H9 0.9500 . ? C10 C11 1.379(5) . ? C10 H10 0.9500 . ? C11 C12 1.392(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.388(4) . ? C13 C14 1.396(4) . ? C14 C15 1.384(4) . ? C14 H14 0.9500 . ? C15 C16 1.379(5) . ? C15 H15 0.9500 . ? C16 C17 1.373(4) . ? C16 H16 0.9500 . ? C17 C18 1.385(4) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N Co Cl2 119.13(7) . . ? N Co Cl1 112.15(7) . . ? Cl2 Co Cl1 113.88(4) . . ? N Co P 84.65(7) . . ? Cl2 Co P 111.04(3) . . ? Cl1 Co P 112.57(3) . . ? C13 P C7 105.09(12) . . ? C13 P C1 104.31(13) . . ? C7 P C1 106.34(13) . . ? C13 P Co 121.16(10) . . ? C7 P Co 119.89(10) . . ? C1 P Co 97.61(9) . . ? C2 O C3 106.4(2) . . ? C2 N C4 107.8(2) . . ? C2 N Co 120.36(18) . . ? C4 N Co 131.54(18) . . ? C2 C1 P 109.9(2) . . ? C2 C1 H1A 109.7 . . ? P C1 H1A 109.7 . . ? C2 C1 H1B 109.7 . . ? P C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? N C2 O 118.1(2) . . ? N C2 C1 126.4(2) . . ? O C2 C1 115.5(2) . . ? O C3 C4 104.8(2) . . ? O C3 H3A 110.8 . . ? C4 C3 H3A 110.8 . . ? O C3 H3B 110.8 . . ? C4 C3 H3B 110.8 . . ? H3A C3 H3B 108.9 . . ? N C4 C5 110.0(2) . . ? N C4 C6 108.2(2) . . ? C5 C4 C6 110.5(2) . . ? N C4 C3 102.5(2) . . ? C5 C4 C3 112.5(2) . . ? C6 C4 C3 112.9(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C12 C7 C8 119.0(3) . . ? C12 C7 P 123.8(2) . . ? C8 C7 P 117.2(2) . . ? C9 C8 C7 120.3(3) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C10 C9 C8 120.2(3) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C11 C10 C9 120.0(3) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.0(3) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C7 C12 C11 120.6(3) . . ? C7 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C18 C13 C14 119.1(3) . . ? C18 C13 P 117.7(2) . . ? C14 C13 P 123.1(2) . . ? C15 C14 C13 120.1(3) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C16 C15 C14 120.2(3) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C17 C16 C15 120.1(3) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C16 C17 C18 120.4(3) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C17 C18 C13 120.2(3) . . ? C17 C18 H18 119.9 . . ? C13 C18 H18 119.9 . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N Co P C13 -120.02(12) . . . . ? Cl2 Co P C13 120.79(11) . . . . ? Cl1 Co P C13 -8.24(11) . . . . ? N Co P C7 105.67(12) . . . . ? Cl2 Co P C7 -13.52(11) . . . . ? Cl1 Co P C7 -142.55(10) . . . . ? N Co P C1 -8.17(11) . . . . ? Cl2 Co P C1 -127.36(10) . . . . ? Cl1 Co P C1 103.61(9) . . . . ? Cl2 Co N C2 117.3(2) . . . . ? Cl1 Co N C2 -106.0(2) . . . . ? P Co N C2 6.2(2) . . . . ? Cl2 Co N C4 -69.3(2) . . . . ? Cl1 Co N C4 67.4(2) . . . . ? P Co N C4 179.6(2) . . . . ? C13 P C1 C2 134.9(2) . . . . ? C7 P C1 C2 -114.3(2) . . . . ? Co P C1 C2 10.0(2) . . . . ? C4 N C2 O 3.1(3) . . . . ? Co N C2 O 177.96(17) . . . . ? C4 N C2 C1 -175.1(3) . . . . ? Co N C2 C1 -0.2(4) . . . . ? C3 O C2 N 0.5(3) . . . . ? C3 O C2 C1 178.9(2) . . . . ? P C1 C2 N -8.1(4) . . . . ? P C1 C2 O 173.68(19) . . . . ? C2 O C3 C4 -3.8(3) . . . . ? C2 N C4 C5 -124.9(3) . . . . ? Co N C4 C5 61.1(3) . . . . ? C2 N C4 C6 114.3(3) . . . . ? Co N C4 C6 -59.7(3) . . . . ? C2 N C4 C3 -5.1(3) . . . . ? Co N C4 C3 -179.2(2) . . . . ? O C3 C4 N 5.3(3) . . . . ? O C3 C4 C5 123.3(3) . . . . ? O C3 C4 C6 -110.8(3) . . . . ? C13 P C7 C12 86.9(2) . . . . ? C1 P C7 C12 -23.3(2) . . . . ? Co P C7 C12 -132.4(2) . . . . ? C13 P C7 C8 -91.1(2) . . . . ? C1 P C7 C8 158.7(2) . . . . ? Co P C7 C8 49.6(2) . . . . ? C12 C7 C8 C9 -0.7(4) . . . . ? P C7 C8 C9 177.4(2) . . . . ? C7 C8 C9 C10 1.4(5) . . . . ? C8 C9 C10 C11 -1.2(5) . . . . ? C9 C10 C11 C12 0.3(5) . . . . ? C8 C7 C12 C11 -0.3(4) . . . . ? P C7 C12 C11 -178.2(2) . . . . ? C10 C11 C12 C7 0.5(4) . . . . ? C7 P C13 C18 173.2(2) . . . . ? C1 P C13 C18 -75.1(3) . . . . ? Co P C13 C18 33.2(3) . . . . ? C7 P C13 C14 -4.1(3) . . . . ? C1 P C13 C14 107.5(3) . . . . ? Co P C13 C14 -144.2(2) . . . . ? C18 C13 C14 C15 0.6(5) . . . . ? P C13 C14 C15 177.9(2) . . . . ? C13 C14 C15 C16 -0.7(5) . . . . ? C14 C15 C16 C17 0.7(5) . . . . ? C15 C16 C17 C18 -0.5(5) . . . . ? C16 C17 C18 C13 0.3(5) . . . . ? C14 C13 C18 C17 -0.4(5) . . . . ? P C13 C18 C17 -177.9(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 29.11 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.587 _refine_diff_density_min -0.707 _refine_diff_density_rms 0.100 # Attachment 'final_9.CIF' data_9 _database_code_depnum_ccdc_archive 'CCDC 646282' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H20 Cl2 Co N O2 P' _chemical_formula_sum 'C18 H20 Cl2 Co N O2 P' _chemical_formula_weight 443.15 _chemical_absolute_configuration ? 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.3700(3) _cell_length_b 18.1880(5) _cell_length_c 9.7290(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.4760(11) _cell_angle_gamma 90.00 _cell_volume 2002.75(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4184 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 29.131 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.470 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 908 _exptl_absorpt_coefficient_mu 1.214 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8643 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0680 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 29.10 _reflns_number_total 5357 _reflns_number_gt 3417 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of 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 based 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. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors 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 'calc w=1/[\s^2^(Fo^2^)+(0.0459P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5357 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0850 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.1036 _refine_ls_wR_factor_gt 0.0872 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.29173(3) -0.005443(17) 0.16681(3) 0.02710(11) Uani 1 1 d . . . Cl1 Cl 0.16647(6) -0.07265(4) 0.27631(7) 0.04619(19) Uani 1 1 d . . . Cl2 Cl 0.47794(5) -0.04083(4) 0.20937(6) 0.03865(17) Uani 1 1 d . . . P P 0.28525(5) 0.12144(3) 0.21864(6) 0.02657(15) Uani 1 1 d . . . O1 O 0.23363(15) 0.06888(9) -0.23798(15) 0.0366(4) Uani 1 1 d . . . O2 O 0.25940(13) 0.16567(9) 0.07318(14) 0.0300(4) Uani 1 1 d . . . N N 0.24428(17) 0.01053(11) -0.03503(18) 0.0279(4) Uani 1 1 d . . . C1 C 0.3146(2) 0.13980(14) -0.0451(2) 0.0337(6) Uani 1 1 d . . . H1A H 0.3999 0.1322 -0.0186 0.040 Uiso 1 1 calc . . . H1B H 0.3064 0.1778 -0.1183 0.040 Uiso 1 1 calc . . . C2 C 0.2612(2) 0.06924(13) -0.1013(2) 0.0285(5) Uani 1 1 d . . . C3 C 0.1987(3) -0.00619(16) -0.2744(3) 0.0581(9) Uani 1 1 d . . . H3A H 0.2557 -0.0289 -0.3326 0.070 Uiso 1 1 calc . . . H3B H 0.1192 -0.0071 -0.3255 0.070 Uiso 1 1 calc . . . C4 C 0.1984(2) -0.04738(14) -0.1364(2) 0.0336(6) Uani 1 1 d . . . C5 C 0.2842(3) -0.11051(16) -0.1277(3) 0.0529(8) Uani 1 1 d . . . H5A H 0.3623 -0.0928 -0.1475 0.079 Uiso 1 1 calc . . . H5B H 0.2568 -0.1482 -0.1954 0.079 Uiso 1 1 calc . . . H5C H 0.2895 -0.1317 -0.0347 0.079 Uiso 1 1 calc . . . C6 C 0.0766(3) -0.07142(18) -0.1076(3) 0.0584(9) Uani 1 1 d . . . H6A H 0.0789 -0.0902 -0.0129 0.088 Uiso 1 1 calc . . . H6B H 0.0489 -0.1103 -0.1726 0.088 Uiso 1 1 calc . . . H6C H 0.0225 -0.0294 -0.1183 0.088 Uiso 1 1 calc . . . C7 C 0.41942(19) 0.16147(13) 0.3007(2) 0.0273(5) Uani 1 1 d . . . C8 C 0.4671(2) 0.22692(14) 0.2560(2) 0.0320(6) Uani 1 1 d . . . H8 H 0.4288 0.2526 0.1793 0.038 Uiso 1 1 calc . . . C9 C 0.5704(2) 0.25426(14) 0.3237(3) 0.0394(6) Uani 1 1 d . . . H9 H 0.6033 0.2988 0.2935 0.047 Uiso 1 1 calc . . . C10 C 0.6255(2) 0.21673(16) 0.4351(3) 0.0417(7) Uani 1 1 d . . . H10 H 0.6962 0.2359 0.4816 0.050 Uiso 1 1 calc . . . C11 C 0.5794(2) 0.15195(15) 0.4798(2) 0.0405(6) Uani 1 1 d . . . H11 H 0.6181 0.1267 0.5568 0.049 Uiso 1 1 calc . . . C12 C 0.4771(2) 0.12382(14) 0.4126(2) 0.0351(6) Uani 1 1 d . . . H12 H 0.4458 0.0788 0.4425 0.042 Uiso 1 1 calc . . . C13 C 0.16794(19) 0.15979(14) 0.3096(2) 0.0300(5) Uani 1 1 d . . . C14 C 0.1185(2) 0.22749(15) 0.2742(2) 0.0396(6) Uani 1 1 d . . . H14 H 0.1475 0.2557 0.2026 0.048 Uiso 1 1 calc . . . C15 C 0.0262(2) 0.25398(18) 0.3439(3) 0.0516(8) Uani 1 1 d . . . H15 H -0.0086 0.3003 0.3199 0.062 Uiso 1 1 calc . . . C16 C -0.0147(2) 0.2125(2) 0.4485(3) 0.0566(9) Uani 1 1 d . . . H16 H -0.0780 0.2305 0.4962 0.068 Uiso 1 1 calc . . . C17 C 0.0350(3) 0.14581(19) 0.4840(3) 0.0553(8) Uani 1 1 d . . . H17 H 0.0067 0.1180 0.5566 0.066 Uiso 1 1 calc . . . C18 C 0.1260(2) 0.11896(16) 0.4145(3) 0.0427(7) Uani 1 1 d . . . H18 H 0.1600 0.0724 0.4387 0.051 Uiso 1 1 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.02549(18) 0.0298(2) 0.02589(18) 0.00361(13) 0.00180(12) -0.00065(14) Cl1 0.0380(4) 0.0524(4) 0.0484(4) 0.0156(3) 0.0056(3) -0.0119(3) Cl2 0.0280(3) 0.0402(4) 0.0477(4) -0.0001(3) 0.0036(3) 0.0050(3) P 0.0251(3) 0.0282(3) 0.0263(3) 0.0032(3) 0.0016(2) 0.0002(3) O1 0.0466(11) 0.0382(11) 0.0242(8) 0.0037(8) -0.0002(7) 0.0022(8) O2 0.0330(9) 0.0307(9) 0.0266(8) 0.0037(7) 0.0038(6) 0.0062(7) N 0.0279(11) 0.0318(11) 0.0238(10) -0.0001(9) 0.0008(8) 0.0025(9) C1 0.0382(15) 0.0343(14) 0.0296(12) 0.0016(11) 0.0092(10) -0.0002(11) C2 0.0271(12) 0.0348(14) 0.0240(11) 0.0000(11) 0.0037(9) 0.0057(11) C3 0.094(3) 0.0452(19) 0.0325(15) -0.0032(13) -0.0088(15) -0.0063(17) C4 0.0392(15) 0.0345(15) 0.0265(12) -0.0061(11) -0.0005(10) 0.0005(12) C5 0.060(2) 0.0430(18) 0.0535(17) -0.0137(14) -0.0041(14) 0.0166(15) C6 0.0405(17) 0.077(2) 0.0562(18) -0.0192(17) -0.0016(14) -0.0165(16) C7 0.0255(12) 0.0291(13) 0.0279(12) -0.0024(10) 0.0056(9) 0.0014(10) C8 0.0308(14) 0.0303(14) 0.0352(13) 0.0011(11) 0.0040(10) 0.0032(11) C9 0.0340(14) 0.0330(14) 0.0520(15) -0.0075(13) 0.0088(12) -0.0050(12) C10 0.0291(14) 0.0457(17) 0.0494(15) -0.0180(14) -0.0013(11) -0.0024(12) C11 0.0402(16) 0.0451(17) 0.0342(14) -0.0027(12) -0.0073(11) 0.0028(13) C12 0.0348(14) 0.0377(15) 0.0325(13) 0.0035(12) 0.0015(10) -0.0025(12) C13 0.0224(12) 0.0390(15) 0.0278(12) -0.0046(11) -0.0006(9) -0.0018(11) C14 0.0338(15) 0.0467(17) 0.0380(13) -0.0041(12) 0.0013(11) 0.0061(12) C15 0.0410(17) 0.062(2) 0.0509(16) -0.0142(16) 0.0000(13) 0.0208(15) C16 0.0284(15) 0.092(3) 0.0496(16) -0.0291(19) 0.0064(12) 0.0072(16) C17 0.0490(19) 0.075(2) 0.0441(17) -0.0070(16) 0.0190(14) -0.0060(17) C18 0.0375(16) 0.0527(18) 0.0392(14) 0.0020(13) 0.0095(12) -0.0015(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co N 2.0073(18) . ? Co Cl2 2.2139(7) . ? Co Cl1 2.2242(7) . ? Co P 2.3648(7) . ? P O2 1.6300(15) . ? P C7 1.806(2) . ? P C13 1.810(2) . ? O1 C2 1.337(3) . ? O1 C3 1.456(3) . ? O2 C1 1.441(3) . ? N C2 1.272(3) . ? N C4 1.502(3) . ? C1 C2 1.500(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C3 C4 1.538(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.504(4) . ? C4 C6 1.504(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.395(3) . ? C7 C12 1.396(3) . ? C8 C9 1.383(3) . ? C8 H8 0.9500 . ? C9 C10 1.380(4) . ? C9 H9 0.9500 . ? C10 C11 1.377(4) . ? C10 H10 0.9500 . ? C11 C12 1.378(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.383(3) . ? C13 C14 1.384(3) . ? C14 C15 1.389(3) . ? C14 H14 0.9500 . ? C15 C16 1.382(4) . ? C15 H15 0.9500 . ? C16 C17 1.369(5) . ? C16 H16 0.9500 . ? C17 C18 1.378(4) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N Co Cl2 112.83(6) . . ? N Co Cl1 115.06(6) . . ? Cl2 Co Cl1 113.28(3) . . ? N Co P 93.24(6) . . ? Cl2 Co P 107.01(3) . . ? Cl1 Co P 113.57(3) . . ? O2 P C7 105.04(9) . . ? O2 P C13 98.87(10) . . ? C7 P C13 105.03(10) . . ? O2 P Co 107.65(6) . . ? C7 P Co 116.46(8) . . ? C13 P Co 121.32(8) . . ? C2 O1 C3 106.20(19) . . ? C1 O2 P 118.43(14) . . ? C2 N C4 108.41(18) . . ? C2 N Co 125.32(16) . . ? C4 N Co 125.80(15) . . ? O2 C1 C2 112.24(19) . . ? O2 C1 H1A 109.2 . . ? C2 C1 H1A 109.2 . . ? O2 C1 H1B 109.2 . . ? C2 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? N C2 O1 117.9(2) . . ? N C2 C1 127.53(19) . . ? O1 C2 C1 114.51(19) . . ? O1 C3 C4 105.5(2) . . ? O1 C3 H3A 110.6 . . ? C4 C3 H3A 110.6 . . ? O1 C3 H3B 110.6 . . ? C4 C3 H3B 110.6 . . ? H3A C3 H3B 108.8 . . ? N C4 C5 108.4(2) . . ? N C4 C6 110.5(2) . . ? C5 C4 C6 111.8(3) . . ? N C4 C3 101.7(2) . . ? C5 C4 C3 111.4(2) . . ? C6 C4 C3 112.5(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C12 119.6(2) . . ? C8 C7 P 122.91(17) . . ? C12 C7 P 117.47(18) . . ? C9 C8 C7 119.7(2) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C10 C9 C8 119.8(2) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C11 C10 C9 120.9(2) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C10 C11 C12 119.8(2) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C11 C12 C7 120.1(2) . . ? C11 C12 H12 120.0 . . ? C7 C12 H12 120.0 . . ? C18 C13 C14 120.1(2) . . ? C18 C13 P 118.4(2) . . ? C14 C13 P 121.51(19) . . ? C13 C14 C15 119.7(3) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C16 C15 C14 119.6(3) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C17 C16 C15 120.6(3) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C18 120.1(3) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C17 C18 C13 120.0(3) . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N Co P O2 -5.37(8) . . . . ? Cl2 Co P O2 109.70(6) . . . . ? Cl1 Co P O2 -124.54(6) . . . . ? N Co P C7 -122.92(10) . . . . ? Cl2 Co P C7 -7.85(9) . . . . ? Cl1 Co P C7 117.91(8) . . . . ? N Co P C13 107.15(10) . . . . ? Cl2 Co P C13 -137.78(9) . . . . ? Cl1 Co P C13 -12.02(9) . . . . ? C7 P O2 C1 86.45(17) . . . . ? C13 P O2 C1 -165.27(17) . . . . ? Co P O2 C1 -38.27(17) . . . . ? Cl2 Co N C2 -84.39(19) . . . . ? Cl1 Co N C2 143.53(17) . . . . ? P Co N C2 25.59(19) . . . . ? Cl2 Co N C4 86.78(18) . . . . ? Cl1 Co N C4 -45.31(19) . . . . ? P Co N C4 -163.24(17) . . . . ? P O2 C1 C2 71.9(2) . . . . ? C4 N C2 O1 1.8(3) . . . . ? Co N C2 O1 174.27(15) . . . . ? C4 N C2 C1 -175.2(2) . . . . ? Co N C2 C1 -2.7(3) . . . . ? C3 O1 C2 N -4.8(3) . . . . ? C3 O1 C2 C1 172.5(2) . . . . ? O2 C1 C2 N -51.2(3) . . . . ? O2 C1 C2 O1 131.71(19) . . . . ? C2 O1 C3 C4 5.5(3) . . . . ? C2 N C4 C5 119.3(2) . . . . ? Co N C4 C5 -53.1(3) . . . . ? C2 N C4 C6 -117.8(2) . . . . ? Co N C4 C6 69.8(3) . . . . ? C2 N C4 C3 1.8(3) . . . . ? Co N C4 C3 -170.57(19) . . . . ? O1 C3 C4 N -4.4(3) . . . . ? O1 C3 C4 C5 -119.7(3) . . . . ? O1 C3 C4 C6 113.8(3) . . . . ? O2 P C7 C8 13.1(2) . . . . ? C13 P C7 C8 -90.7(2) . . . . ? Co P C7 C8 132.03(17) . . . . ? O2 P C7 C12 -166.18(18) . . . . ? C13 P C7 C12 90.1(2) . . . . ? Co P C7 C12 -47.2(2) . . . . ? C12 C7 C8 C9 -0.6(3) . . . . ? P C7 C8 C9 -179.85(18) . . . . ? C7 C8 C9 C10 -0.1(4) . . . . ? C8 C9 C10 C11 0.3(4) . . . . ? C9 C10 C11 C12 0.2(4) . . . . ? C10 C11 C12 C7 -0.9(4) . . . . ? C8 C7 C12 C11 1.1(4) . . . . ? P C7 C12 C11 -179.60(19) . . . . ? O2 P C13 C18 154.77(19) . . . . ? C7 P C13 C18 -96.9(2) . . . . ? Co P C13 C18 37.8(2) . . . . ? O2 P C13 C14 -23.7(2) . . . . ? C7 P C13 C14 84.6(2) . . . . ? Co P C13 C14 -140.74(18) . . . . ? C18 C13 C14 C15 -0.4(4) . . . . ? P C13 C14 C15 178.1(2) . . . . ? C13 C14 C15 C16 0.4(4) . . . . ? C14 C15 C16 C17 0.1(4) . . . . ? C15 C16 C17 C18 -0.6(5) . . . . ? C16 C17 C18 C13 0.6(4) . . . . ? C14 C13 C18 C17 -0.1(4) . . . . ? P C13 C18 C17 -178.6(2) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 29.10 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.619 _refine_diff_density_min -0.631 _refine_diff_density_rms 0.080 # Attachment 'final_10.CIF' data_10 _database_code_depnum_ccdc_archive 'CCDC 646283' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H24 Cl2 Co N O2 P' _chemical_formula_sum 'C20 H24 Cl2 Co N O2 P' _chemical_formula_weight 471.20 _chemical_absolute_configuration ? 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.9970(2) _cell_length_b 14.5140(4) _cell_length_c 16.7880(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.2150(15) _cell_angle_gamma 90.00 _cell_volume 2188.77(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5783 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 29.131 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 972 _exptl_absorpt_coefficient_mu 1.116 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10203 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0721 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 29.11 _reflns_number_total 5883 _reflns_number_gt 3834 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of 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 based 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. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors 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 'calc w=1/[\s^2^(Fo^2^)+(0.0602P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5883 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0881 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1234 _refine_ls_wR_factor_gt 0.1063 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.63651(4) 0.37441(3) 0.809488(18) 0.02424(12) Uani 1 1 d . . . Cl1 Cl 0.64492(8) 0.22596(5) 0.84460(4) 0.03245(17) Uani 1 1 d . . . Cl2 Cl 0.78154(8) 0.47154(5) 0.88059(4) 0.03647(19) Uani 1 1 d . . . P P 0.69372(7) 0.39283(5) 0.67690(4) 0.02321(16) Uani 1 1 d . . . O1 O 0.2037(2) 0.42282(15) 0.71833(11) 0.0400(5) Uani 1 1 d . . . O2 O 0.54009(19) 0.40372(13) 0.62161(9) 0.0278(4) Uani 1 1 d . . . N N 0.4253(2) 0.41356(16) 0.78401(11) 0.0258(5) Uani 1 1 d . . . C1 C 0.3985(3) 0.3629(2) 0.63962(15) 0.0306(6) Uani 1 1 d . . . C2 C 0.3485(3) 0.40156(19) 0.71865(16) 0.0281(6) Uani 1 1 d . . . C3 C 0.1731(3) 0.4471(2) 0.80090(18) 0.0460(8) Uani 1 1 d . . . H3A H 0.1177 0.3972 0.8264 0.055 Uiso 1 1 calc . . . H3B H 0.1146 0.5048 0.8026 0.055 Uiso 1 1 calc . . . C4 C 0.3278(3) 0.4597(2) 0.84228(15) 0.0319(6) Uani 1 1 d . . . C5 C 0.3434(4) 0.4130(2) 0.92308(17) 0.0443(8) Uani 1 1 d . . . H5A H 0.3249 0.3468 0.9167 0.067 Uiso 1 1 calc . . . H5B H 0.2711 0.4393 0.9582 0.067 Uiso 1 1 calc . . . H5C H 0.4444 0.4227 0.9466 0.067 Uiso 1 1 calc . . . C6 C 0.3745(4) 0.5605(2) 0.84802(19) 0.0443(8) Uani 1 1 d . . . H6A H 0.4794 0.5644 0.8670 0.066 Uiso 1 1 calc . . . H6B H 0.3128 0.5926 0.8855 0.066 Uiso 1 1 calc . . . H6C H 0.3614 0.5893 0.7953 0.066 Uiso 1 1 calc . . . C7 C 0.4108(3) 0.2590(2) 0.64554(17) 0.0371(7) Uani 1 1 d . . . H7A H 0.4405 0.2340 0.5946 0.056 Uiso 1 1 calc . . . H7B H 0.3143 0.2331 0.6580 0.056 Uiso 1 1 calc . . . H7C H 0.4857 0.2426 0.6878 0.056 Uiso 1 1 calc . . . C8 C 0.2925(3) 0.3925(3) 0.57003(17) 0.0463(9) Uani 1 1 d . . . H8A H 0.2823 0.4598 0.5701 0.069 Uiso 1 1 calc . . . H8B H 0.1947 0.3642 0.5757 0.069 Uiso 1 1 calc . . . H8C H 0.3323 0.3726 0.5197 0.069 Uiso 1 1 calc . . . C9 C 0.7778(3) 0.50194(19) 0.65349(14) 0.0252(6) Uani 1 1 d . . . C10 C 0.7013(3) 0.5819(2) 0.67063(16) 0.0375(7) Uani 1 1 d . . . H10 H 0.6057 0.5777 0.6916 0.045 Uiso 1 1 calc . . . C11 C 0.7626(4) 0.6674(2) 0.65755(16) 0.0398(7) Uani 1 1 d . . . H11 H 0.7087 0.7218 0.6687 0.048 Uiso 1 1 calc . . . C12 C 0.9026(4) 0.6735(2) 0.62811(17) 0.0394(7) Uani 1 1 d . . . H12 H 0.9457 0.7321 0.6197 0.047 Uiso 1 1 calc . . . C13 C 0.9796(3) 0.5949(2) 0.61096(19) 0.0427(8) Uani 1 1 d . . . H13 H 1.0754 0.5995 0.5903 0.051 Uiso 1 1 calc . . . C14 C 0.9185(3) 0.5089(2) 0.62359(17) 0.0345(7) Uani 1 1 d . . . H14 H 0.9725 0.4548 0.6119 0.041 Uiso 1 1 calc . . . C15 C 0.8032(3) 0.30516(18) 0.63136(14) 0.0227(5) Uani 1 1 d . . . C16 C 0.9048(3) 0.25651(19) 0.68047(14) 0.0280(6) Uani 1 1 d . . . H16 H 0.9146 0.2700 0.7359 0.034 Uiso 1 1 calc . . . C17 C 0.9925(3) 0.1880(2) 0.64878(15) 0.0300(6) Uani 1 1 d . . . H17 H 1.0632 0.1554 0.6822 0.036 Uiso 1 1 calc . . . C18 C 0.9756(3) 0.1678(2) 0.56833(16) 0.0328(6) Uani 1 1 d . . . H18 H 1.0348 0.1209 0.5465 0.039 Uiso 1 1 calc . . . C19 C 0.8729(3) 0.2153(2) 0.51932(14) 0.0314(6) Uani 1 1 d . . . H19 H 0.8613 0.2004 0.4642 0.038 Uiso 1 1 calc . . . C20 C 0.7871(3) 0.28436(19) 0.55033(14) 0.0286(6) Uani 1 1 d . . . H20 H 0.7177 0.3174 0.5165 0.034 Uiso 1 1 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.0259(2) 0.0252(2) 0.02158(19) -0.00073(14) 0.00055(13) -0.00010(15) Cl1 0.0392(4) 0.0265(4) 0.0311(3) 0.0035(3) -0.0032(3) -0.0021(3) Cl2 0.0434(4) 0.0349(4) 0.0305(3) -0.0045(3) -0.0033(3) -0.0114(3) P 0.0239(4) 0.0248(4) 0.0210(3) 0.0003(3) 0.0018(2) 0.0022(3) O1 0.0237(11) 0.0507(14) 0.0457(11) -0.0126(10) 0.0020(8) 0.0066(10) O2 0.0250(10) 0.0341(12) 0.0241(9) 0.0031(8) -0.0005(7) 0.0029(8) N 0.0254(12) 0.0261(13) 0.0261(11) -0.0016(9) 0.0039(9) 0.0018(10) C1 0.0202(14) 0.0407(18) 0.0304(14) -0.0041(12) -0.0023(10) 0.0021(12) C2 0.0224(14) 0.0267(15) 0.0354(14) -0.0003(12) 0.0023(11) 0.0011(11) C3 0.0338(17) 0.055(2) 0.0508(19) -0.0139(16) 0.0162(14) 0.0032(16) C4 0.0312(16) 0.0303(17) 0.0353(15) -0.0071(12) 0.0102(12) 0.0016(12) C5 0.058(2) 0.043(2) 0.0344(15) -0.0067(14) 0.0181(14) -0.0049(16) C6 0.0438(19) 0.0308(18) 0.0593(19) -0.0105(15) 0.0131(15) 0.0011(15) C7 0.0318(16) 0.0379(19) 0.0417(16) -0.0128(14) 0.0036(12) -0.0057(14) C8 0.0321(18) 0.072(3) 0.0339(16) -0.0049(15) -0.0093(12) 0.0103(16) C9 0.0288(14) 0.0256(15) 0.0209(12) -0.0004(10) 0.0002(10) 0.0015(12) C10 0.0441(18) 0.0310(18) 0.0390(15) 0.0019(13) 0.0159(13) 0.0020(14) C11 0.058(2) 0.0263(17) 0.0366(15) 0.0027(13) 0.0138(14) 0.0038(15) C12 0.0508(19) 0.0290(18) 0.0383(16) 0.0035(13) 0.0025(13) -0.0086(15) C13 0.0293(17) 0.038(2) 0.062(2) 0.0031(15) 0.0046(14) -0.0037(14) C14 0.0240(15) 0.0301(17) 0.0491(17) 0.0022(13) 0.0007(12) 0.0046(12) C15 0.0224(13) 0.0214(14) 0.0247(12) 0.0010(10) 0.0031(10) 0.0003(11) C16 0.0256(14) 0.0303(16) 0.0280(13) -0.0009(11) 0.0004(10) -0.0010(12) C17 0.0256(15) 0.0286(16) 0.0358(14) 0.0030(12) 0.0024(11) 0.0036(12) C18 0.0322(16) 0.0274(16) 0.0397(15) -0.0048(12) 0.0107(12) 0.0021(13) C19 0.0350(16) 0.0352(18) 0.0244(13) -0.0027(12) 0.0068(11) 0.0008(13) C20 0.0305(15) 0.0309(16) 0.0247(13) 0.0017(11) 0.0043(11) 0.0004(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co N 2.006(2) . ? Co Cl2 2.2227(7) . ? Co Cl1 2.2340(8) . ? Co P 2.3281(7) . ? P O2 1.6288(18) . ? P C15 1.805(3) . ? P C9 1.808(3) . ? O1 C2 1.339(3) . ? O1 C3 1.471(3) . ? O2 C1 1.452(3) . ? N C2 1.275(3) . ? N C4 1.507(3) . ? C1 C7 1.515(4) . ? C1 C8 1.528(4) . ? C1 C2 1.531(4) . ? C3 C4 1.531(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.516(4) . ? C4 C6 1.524(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.388(4) . ? C9 C14 1.391(4) . ? C10 C11 1.381(4) . ? C10 H10 0.9500 . ? C11 C12 1.381(4) . ? C11 H11 0.9500 . ? C12 C13 1.373(4) . ? C12 H12 0.9500 . ? C13 C14 1.384(4) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.389(4) . ? C15 C20 1.393(3) . ? C16 C17 1.393(4) . ? C16 H16 0.9500 . ? C17 C18 1.382(4) . ? C17 H17 0.9500 . ? C18 C19 1.386(4) . ? C18 H18 0.9500 . ? C19 C20 1.384(4) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N Co Cl2 117.09(7) . . ? N Co Cl1 110.31(7) . . ? Cl2 Co Cl1 117.38(3) . . ? N Co P 91.21(6) . . ? Cl2 Co P 106.62(3) . . ? Cl1 Co P 110.92(3) . . ? O2 P C15 107.04(11) . . ? O2 P C9 98.24(11) . . ? C15 P C9 106.28(12) . . ? O2 P Co 109.26(7) . . ? C15 P Co 118.63(8) . . ? C9 P Co 115.22(8) . . ? C2 O1 C3 106.5(2) . . ? C1 O2 P 124.62(15) . . ? C2 N C4 108.2(2) . . ? C2 N Co 127.28(18) . . ? C4 N Co 124.50(16) . . ? O2 C1 C7 111.0(2) . . ? O2 C1 C8 104.1(2) . . ? C7 C1 C8 111.7(2) . . ? O2 C1 C2 109.6(2) . . ? C7 C1 C2 109.4(2) . . ? C8 C1 C2 111.0(2) . . ? N C2 O1 116.9(2) . . ? N C2 C1 128.6(2) . . ? O1 C2 C1 114.5(2) . . ? O1 C3 C4 104.1(2) . . ? O1 C3 H3A 110.9 . . ? C4 C3 H3A 110.9 . . ? O1 C3 H3B 110.9 . . ? C4 C3 H3B 110.9 . . ? H3A C3 H3B 109.0 . . ? N C4 C5 110.7(2) . . ? N C4 C6 107.4(2) . . ? C5 C4 C6 111.2(3) . . ? N C4 C3 101.5(2) . . ? C5 C4 C3 112.9(3) . . ? C6 C4 C3 112.6(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C1 C7 H7A 109.5 . . ? C1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C1 C8 H8A 109.5 . . ? C1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C14 119.1(3) . . ? C10 C9 P 118.0(2) . . ? C14 C9 P 122.9(2) . . ? C11 C10 C9 120.8(3) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 C12 119.6(3) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C13 C12 C11 120.2(3) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C14 120.4(3) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C13 C14 C9 119.9(3) . . ? C13 C14 H14 120.1 . . ? C9 C14 H14 120.1 . . ? C16 C15 C20 119.9(2) . . ? C16 C15 P 117.62(18) . . ? C20 C15 P 122.47(19) . . ? C15 C16 C17 120.3(2) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C18 C17 C16 119.4(2) . . ? C18 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? C17 C18 C19 120.5(2) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C20 C19 C18 120.3(2) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C15 119.6(2) . . ? C19 C20 H20 120.2 . . ? C15 C20 H20 120.2 . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N Co P O2 -13.10(10) . . . . ? Cl2 Co P O2 -131.89(8) . . . . ? Cl1 Co P O2 99.22(8) . . . . ? N Co P C15 -136.08(12) . . . . ? Cl2 Co P C15 105.13(10) . . . . ? Cl1 Co P C15 -23.77(10) . . . . ? N Co P C9 96.32(12) . . . . ? Cl2 Co P C9 -22.47(10) . . . . ? Cl1 Co P C9 -151.36(10) . . . . ? C15 P O2 C1 100.3(2) . . . . ? C9 P O2 C1 -149.8(2) . . . . ? Co P O2 C1 -29.4(2) . . . . ? Cl2 Co N C2 140.5(2) . . . . ? Cl1 Co N C2 -81.8(2) . . . . ? P Co N C2 31.1(2) . . . . ? Cl2 Co N C4 -42.3(2) . . . . ? Cl1 Co N C4 95.4(2) . . . . ? P Co N C4 -151.7(2) . . . . ? P O2 C1 C7 -59.2(3) . . . . ? P O2 C1 C8 -179.50(18) . . . . ? P O2 C1 C2 61.7(3) . . . . ? C4 N C2 O1 -6.0(3) . . . . ? Co N C2 O1 171.65(18) . . . . ? C4 N C2 C1 176.0(3) . . . . ? Co N C2 C1 -6.4(4) . . . . ? C3 O1 C2 N -5.4(3) . . . . ? C3 O1 C2 C1 173.0(2) . . . . ? O2 C1 C2 N -44.5(4) . . . . ? C7 C1 C2 N 77.3(4) . . . . ? C8 C1 C2 N -158.9(3) . . . . ? O2 C1 C2 O1 137.4(2) . . . . ? C7 C1 C2 O1 -100.7(3) . . . . ? C8 C1 C2 O1 23.0(4) . . . . ? C2 O1 C3 C4 13.8(3) . . . . ? C2 N C4 C5 134.0(3) . . . . ? Co N C4 C5 -43.7(3) . . . . ? C2 N C4 C6 -104.5(3) . . . . ? Co N C4 C6 77.9(3) . . . . ? C2 N C4 C3 13.9(3) . . . . ? Co N C4 C3 -163.83(19) . . . . ? O1 C3 C4 N -16.1(3) . . . . ? O1 C3 C4 C5 -134.7(3) . . . . ? O1 C3 C4 C6 98.4(3) . . . . ? O2 P C9 C10 59.4(2) . . . . ? C15 P C9 C10 169.9(2) . . . . ? Co P C9 C10 -56.5(2) . . . . ? O2 P C9 C14 -124.4(2) . . . . ? C15 P C9 C14 -13.9(2) . . . . ? Co P C9 C14 119.7(2) . . . . ? C14 C9 C10 C11 0.7(4) . . . . ? P C9 C10 C11 177.0(2) . . . . ? C9 C10 C11 C12 -0.9(4) . . . . ? C10 C11 C12 C13 0.9(4) . . . . ? C11 C12 C13 C14 -0.6(5) . . . . ? C12 C13 C14 C9 0.3(4) . . . . ? C10 C9 C14 C13 -0.4(4) . . . . ? P C9 C14 C13 -176.6(2) . . . . ? O2 P C15 C16 -153.9(2) . . . . ? C9 P C15 C16 101.9(2) . . . . ? Co P C15 C16 -29.8(2) . . . . ? O2 P C15 C20 25.0(2) . . . . ? C9 P C15 C20 -79.3(2) . . . . ? Co P C15 C20 149.05(19) . . . . ? C20 C15 C16 C17 1.0(4) . . . . ? P C15 C16 C17 180.0(2) . . . . ? C15 C16 C17 C18 -1.1(4) . . . . ? C16 C17 C18 C19 0.2(4) . . . . ? C17 C18 C19 C20 0.7(4) . . . . ? C18 C19 C20 C15 -0.8(4) . . . . ? C16 C15 C20 C19 -0.1(4) . . . . ? P C15 C20 C19 -179.0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 29.11 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.656 _refine_diff_density_min -0.840 _refine_diff_density_rms 0.252 data_sj_1_openring _database_code_depnum_ccdc_archive 'CCDC 646284' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H23 Cl3 Co N O2 P' _chemical_formula_sum 'C18 H23 Cl3 Co N O2 P' _chemical_formula_weight 481.62 _chemical_absolute_configuration . 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' Cl Cl 0.1484 0.1585 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.2380(6) _cell_length_b 12.8960(6) _cell_length_c 13.1040(9) _cell_angle_alpha 90.00 _cell_angle_beta 111.8260(16) _cell_angle_gamma 90.00 _cell_volume 2233.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4355 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.432 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 988 _exptl_absorpt_coefficient_mu 1.211 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8922 _diffrn_reflns_av_R_equivalents 0.1023 _diffrn_reflns_av_sigmaI/netI 0.1857 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5086 _reflns_number_gt 2468 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of 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 based 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. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors 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 'calc w=1/[\s^2^(Fo^2^)+(0.0574P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5086 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1905 _refine_ls_R_factor_gt 0.0746 _refine_ls_wR_factor_ref 0.1490 _refine_ls_wR_factor_gt 0.1186 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.956 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.20155(5) 0.39623(4) 0.52874(5) 0.0356(2) Uani 1 1 d . . . Cl1 Cl 0.06137(10) 0.33910(10) 0.55310(10) 0.0478(4) Uani 1 1 d . . . Cl2 Cl 0.15927(10) 0.50596(9) 0.38593(11) 0.0529(4) Uani 1 1 d . . . Cl3 Cl 0.30498(10) 0.46030(9) 0.69139(10) 0.0477(4) Uani 1 1 d . . . P P 0.28745(11) 0.26447(9) 0.46930(11) 0.0391(4) Uani 1 1 d . . . O1 O 0.0415(3) 0.2642(2) 0.2941(3) 0.0430(9) Uani 1 1 d . . . O2 O 0.0918(3) 0.0991(3) 0.3275(3) 0.0482(10) Uani 1 1 d . . . N N -0.0866(3) 0.4166(3) 0.3081(3) 0.0446(11) Uani 1 1 d . . . C1 C 0.2113(4) 0.2282(4) 0.3268(4) 0.0401(13) Uani 1 1 d . . . H1A H 0.2025 0.2896 0.2787 0.048 Uiso 1 1 calc . . . H1B H 0.2476 0.1744 0.3019 0.048 Uiso 1 1 calc . . . C2 C 0.1106(4) 0.1882(4) 0.3162(4) 0.0405(13) Uani 1 1 d . . . C3 C -0.0584(4) 0.2321(3) 0.2870(5) 0.0488(15) Uani 1 1 d . . . H3A H -0.0577 0.2149 0.3609 0.059 Uiso 1 1 calc . . . H3B H -0.0806 0.1701 0.2395 0.059 Uiso 1 1 calc . . . C4 C -0.1291(4) 0.3224(3) 0.2382(5) 0.0516(16) Uani 1 1 d . . . C5 C -0.1373(6) 0.3481(4) 0.1231(5) 0.094(3) Uani 1 1 d . . . H5A H -0.0813 0.3937 0.1260 0.140 Uiso 1 1 calc . . . H5B H -0.2018 0.3833 0.0841 0.140 Uiso 1 1 calc . . . H5C H -0.1343 0.2841 0.0842 0.140 Uiso 1 1 calc . . . C6 C -0.2309(5) 0.2955(4) 0.2480(7) 0.094(3) Uani 1 1 d . . . H6A H -0.2644 0.2403 0.1958 0.140 Uiso 1 1 calc . . . H6B H -0.2742 0.3572 0.2316 0.140 Uiso 1 1 calc . . . H6C H -0.2188 0.2720 0.3230 0.140 Uiso 1 1 calc . . . C7 C 0.3134(4) 0.1423(4) 0.5418(4) 0.0412(13) Uani 1 1 d . . . C8 C 0.2478(4) 0.1068(4) 0.5900(4) 0.0509(15) Uani 1 1 d . . . H8 H 0.1913 0.1481 0.5862 0.061 Uiso 1 1 calc . . . C9 C 0.2631(5) 0.0119(4) 0.6439(5) 0.0616(17) Uani 1 1 d . . . H9 H 0.2171 -0.0116 0.6760 0.074 Uiso 1 1 calc . . . C10 C 0.3448(6) -0.0475(4) 0.6505(5) 0.0683(19) Uani 1 1 d . . . H10 H 0.3547 -0.1131 0.6859 0.082 Uiso 1 1 calc . . . C11 C 0.4125(6) -0.0125(5) 0.6061(6) 0.084(2) Uani 1 1 d . . . H11 H 0.4698 -0.0534 0.6118 0.101 Uiso 1 1 calc . . . C12 C 0.3969(5) 0.0829(4) 0.5528(6) 0.0731(19) Uani 1 1 d . . . H12 H 0.4446 0.1074 0.5236 0.088 Uiso 1 1 calc . . . C13 C 0.4066(4) 0.3047(3) 0.4616(4) 0.0403(13) Uani 1 1 d . . . C14 C 0.4761(4) 0.3550(4) 0.5518(4) 0.0493(14) Uani 1 1 d . . . H14 H 0.4599 0.3681 0.6146 0.059 Uiso 1 1 calc . . . C15 C 0.5683(4) 0.3860(4) 0.5511(5) 0.0533(15) Uani 1 1 d . . . H15 H 0.6153 0.4200 0.6136 0.064 Uiso 1 1 calc . . . C16 C 0.5932(4) 0.3683(4) 0.4606(5) 0.0540(16) Uani 1 1 d . . . H16 H 0.6572 0.3894 0.4609 0.065 Uiso 1 1 calc . . . C17 C 0.5254(5) 0.3200(4) 0.3703(5) 0.0621(17) Uani 1 1 d . . . H17 H 0.5422 0.3081 0.3076 0.074 Uiso 1 1 calc . . . C18 C 0.4318(5) 0.2884(4) 0.3701(5) 0.0554(16) Uani 1 1 d . . . H18 H 0.3849 0.2554 0.3069 0.066 Uiso 1 1 calc . . . H1 H -0.0728 0.4182 0.3648 0.050 Uiso 1 1 d . . . H2 H -0.1261 0.4720 0.3008 0.050 Uiso 1 1 d . . . H3 H -0.0236 0.4516 0.3014 0.050 Uiso 1 1 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.0420(5) 0.0357(4) 0.0293(4) 0.0014(3) 0.0133(3) 0.0024(3) Cl1 0.0484(9) 0.0608(8) 0.0348(8) 0.0024(6) 0.0163(7) -0.0058(7) Cl2 0.0506(9) 0.0508(8) 0.0515(9) 0.0206(6) 0.0122(7) 0.0046(6) Cl3 0.0522(9) 0.0550(8) 0.0353(8) -0.0061(6) 0.0156(7) -0.0108(6) P 0.0452(9) 0.0420(7) 0.0291(8) 0.0005(6) 0.0125(7) 0.0026(6) O1 0.048(2) 0.0326(18) 0.046(2) -0.0068(15) 0.0150(18) 0.0015(17) O2 0.060(3) 0.036(2) 0.041(2) 0.0025(16) 0.0107(19) 0.0033(18) N 0.047(3) 0.030(2) 0.048(3) -0.0058(19) 0.007(2) 0.0020(19) C1 0.045(4) 0.047(3) 0.030(3) -0.004(2) 0.016(3) 0.004(2) C2 0.052(4) 0.042(3) 0.023(3) -0.007(2) 0.008(3) 0.000(3) C3 0.039(4) 0.038(3) 0.065(4) -0.014(3) 0.015(3) -0.005(2) C4 0.054(4) 0.032(3) 0.051(4) -0.015(3) -0.001(3) -0.002(3) C5 0.131(7) 0.059(4) 0.050(5) -0.017(3) -0.014(4) 0.012(4) C6 0.047(4) 0.055(4) 0.161(8) -0.033(4) 0.017(5) -0.015(3) C7 0.040(3) 0.049(3) 0.033(3) 0.001(2) 0.012(3) 0.006(3) C8 0.066(4) 0.052(3) 0.039(3) -0.006(3) 0.023(3) 0.003(3) C9 0.092(5) 0.056(4) 0.043(4) 0.008(3) 0.031(4) -0.001(4) C10 0.087(6) 0.062(4) 0.048(4) 0.017(3) 0.016(4) 0.010(4) C11 0.086(6) 0.073(4) 0.101(6) 0.025(4) 0.046(5) 0.037(4) C12 0.088(5) 0.061(4) 0.083(5) 0.019(3) 0.047(4) 0.011(4) C13 0.043(3) 0.041(3) 0.036(3) 0.004(2) 0.014(3) 0.006(2) C14 0.045(4) 0.065(3) 0.037(3) 0.001(3) 0.013(3) 0.007(3) C15 0.036(4) 0.063(4) 0.048(4) -0.003(3) 0.002(3) 0.002(3) C16 0.039(4) 0.048(3) 0.073(5) 0.005(3) 0.018(3) 0.001(3) C17 0.070(5) 0.066(4) 0.063(4) -0.002(3) 0.040(4) -0.010(3) C18 0.056(4) 0.066(4) 0.050(4) -0.006(3) 0.026(3) -0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co Cl2 2.2427(14) . ? Co Cl3 2.2495(14) . ? Co Cl1 2.2587(15) . ? Co P 2.3870(15) . ? P C7 1.806(5) . ? P C13 1.813(5) . ? P C1 1.837(5) . ? O1 C2 1.343(6) . ? O1 C3 1.450(6) . ? O2 C2 1.201(5) . ? N C4 1.507(6) . ? N H1 0.6948 . ? N H2 0.8920 . ? N H3 1.0365 . ? C1 C2 1.481(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C3 C4 1.516(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.506(9) . ? C4 C6 1.542(9) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C12 1.376(8) . ? C7 C8 1.386(7) . ? C8 C9 1.389(7) . ? C8 H8 0.9500 . ? C9 C10 1.368(8) . ? C9 H9 0.9500 . ? C10 C11 1.375(9) . ? C10 H10 0.9500 . ? C11 C12 1.391(8) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.388(7) . ? C13 C18 1.390(7) . ? C14 C15 1.376(7) . ? C14 H14 0.9500 . ? C15 C16 1.377(8) . ? C15 H15 0.9500 . ? C16 C17 1.367(8) . ? C16 H16 0.9500 . ? C17 C18 1.392(8) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl2 Co Cl3 115.91(5) . . ? Cl2 Co Cl1 110.28(6) . . ? Cl3 Co Cl1 106.71(6) . . ? Cl2 Co P 100.83(5) . . ? Cl3 Co P 109.65(5) . . ? Cl1 Co P 113.63(5) . . ? C7 P C13 105.5(2) . . ? C7 P C1 103.9(2) . . ? C13 P C1 103.1(2) . . ? C7 P Co 118.62(19) . . ? C13 P Co 114.71(16) . . ? C1 P Co 109.41(16) . . ? C2 O1 C3 115.3(4) . . ? C4 N H1 124.3 . . ? C4 N H2 119.1 . . ? H1 N H2 90.4 . . ? C4 N H3 117.7 . . ? H1 N H3 99.7 . . ? H2 N H3 100.0 . . ? C2 C1 P 111.6(3) . . ? C2 C1 H1A 109.3 . . ? P C1 H1A 109.3 . . ? C2 C1 H1B 109.3 . . ? P C1 H1B 109.3 . . ? H1A C1 H1B 108.0 . . ? O2 C2 O1 123.1(5) . . ? O2 C2 C1 125.0(5) . . ? O1 C2 C1 111.8(4) . . ? O1 C3 C4 106.8(4) . . ? O1 C3 H3A 110.4 . . ? C4 C3 H3A 110.4 . . ? O1 C3 H3B 110.4 . . ? C4 C3 H3B 110.4 . . ? H3A C3 H3B 108.6 . . ? C5 C4 N 107.2(4) . . ? C5 C4 C3 112.6(5) . . ? N C4 C3 108.0(4) . . ? C5 C4 C6 114.1(5) . . ? N C4 C6 107.9(5) . . ? C3 C4 C6 106.9(5) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C12 C7 C8 118.1(5) . . ? C12 C7 P 122.8(4) . . ? C8 C7 P 119.1(4) . . ? C7 C8 C9 121.1(5) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C10 C9 C8 119.7(6) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C9 C10 C11 120.2(5) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C10 C11 C12 119.7(6) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C7 C12 C11 121.1(6) . . ? C7 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C14 C13 C18 118.3(5) . . ? C14 C13 P 118.2(4) . . ? C18 C13 P 123.5(4) . . ? C15 C14 C13 120.7(5) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 120.6(5) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C17 C16 C15 119.7(5) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C18 120.2(6) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C13 C18 C17 120.5(5) . . ? C13 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl2 Co P C7 -166.5(2) . . . . ? Cl3 Co P C7 70.7(2) . . . . ? Cl1 Co P C7 -48.6(2) . . . . ? Cl2 Co P C13 67.65(19) . . . . ? Cl3 Co P C13 -55.08(19) . . . . ? Cl1 Co P C13 -174.39(18) . . . . ? Cl2 Co P C1 -47.65(18) . . . . ? Cl3 Co P C1 -170.39(18) . . . . ? Cl1 Co P C1 70.31(18) . . . . ? C7 P C1 C2 67.7(4) . . . . ? C13 P C1 C2 177.6(3) . . . . ? Co P C1 C2 -59.9(4) . . . . ? C3 O1 C2 O2 1.3(7) . . . . ? C3 O1 C2 C1 -177.6(4) . . . . ? P C1 C2 O2 -88.6(5) . . . . ? P C1 C2 O1 90.3(4) . . . . ? C2 O1 C3 C4 -168.1(4) . . . . ? O1 C3 C4 C5 63.1(5) . . . . ? O1 C3 C4 N -55.0(6) . . . . ? O1 C3 C4 C6 -170.9(4) . . . . ? C13 P C7 C12 -18.5(6) . . . . ? C1 P C7 C12 89.7(5) . . . . ? Co P C7 C12 -148.6(5) . . . . ? C13 P C7 C8 160.6(4) . . . . ? C1 P C7 C8 -91.3(4) . . . . ? Co P C7 C8 30.4(5) . . . . ? C12 C7 C8 C9 -2.8(8) . . . . ? P C7 C8 C9 178.1(4) . . . . ? C7 C8 C9 C10 0.6(9) . . . . ? C8 C9 C10 C11 1.4(10) . . . . ? C9 C10 C11 C12 -1.0(11) . . . . ? C8 C7 C12 C11 3.1(10) . . . . ? P C7 C12 C11 -177.8(5) . . . . ? C10 C11 C12 C7 -1.3(11) . . . . ? C7 P C13 C14 -82.7(4) . . . . ? C1 P C13 C14 168.6(4) . . . . ? Co P C13 C14 49.7(4) . . . . ? C7 P C13 C18 97.6(5) . . . . ? C1 P C13 C18 -11.1(5) . . . . ? Co P C13 C18 -130.0(4) . . . . ? C18 C13 C14 C15 -1.2(8) . . . . ? P C13 C14 C15 179.1(4) . . . . ? C13 C14 C15 C16 0.4(8) . . . . ? C14 C15 C16 C17 0.5(8) . . . . ? C15 C16 C17 C18 -0.4(9) . . . . ? C14 C13 C18 C17 1.3(8) . . . . ? P C13 C18 C17 -179.1(4) . . . . ? C16 C17 C18 C13 -0.5(9) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.392 _refine_diff_density_min -0.358 _refine_diff_density_rms 0.082 # Attachment 'final_12.cif' data_jie1 _database_code_depnum_ccdc_archive 'CCDC 646285' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H40 Cl4 Co2 N2 O4 P2' _chemical_formula_sum 'C36 H40 Cl4 Co2 N2 O4 P2' _chemical_formula_weight 886.36 _chemical_absolute_configuration ? 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.6150(10) _cell_length_b 18.264(3) _cell_length_c 12.580(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.325(5) _cell_angle_gamma 90.00 _cell_volume 1917.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 17232 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 908 _exptl_absorpt_coefficient_mu 1.268 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17961 _diffrn_reflns_av_R_equivalents 0.0676 _diffrn_reflns_av_sigmaI/netI 0.0765 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 30.02 _reflns_number_total 5587 _reflns_number_gt 3656 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of 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 based 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. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors 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 'calc w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+6.3914P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5587 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1192 _refine_ls_R_factor_gt 0.0731 _refine_ls_wR_factor_ref 0.1785 _refine_ls_wR_factor_gt 0.1594 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co -0.18471(7) 0.06094(3) 0.60039(5) 0.03225(17) Uani 1 1 d . . . Cl1 Cl -0.24435(15) 0.14076(6) 0.71978(9) 0.0418(3) Uani 1 1 d . . . Cl2 Cl -0.28867(18) -0.04954(6) 0.62504(10) 0.0513(3) Uani 1 1 d . . . P P 0.18304(18) 0.06389(6) 0.69573(9) 0.0420(3) Uani 1 1 d . . . O1 O -0.3591(4) 0.09786(17) 0.2612(2) 0.0445(8) Uani 1 1 d . . . O2 O 0.0384(4) 0.0409(2) 0.6208(3) 0.0548(9) Uani 1 1 d . . . N2 N -0.2636(4) 0.09862(18) 0.4442(3) 0.0289(7) Uani 1 1 d . . . C1 C 0.3435(7) 0.0193(2) 0.6518(4) 0.0484(13) Uani 1 1 d . . . H1A H 0.3490 0.0391 0.5795 0.058 Uiso 1 1 calc . . . H1B H 0.4466 0.0301 0.7049 0.058 Uiso 1 1 calc . . . C2 C -0.3202(6) 0.0611(2) 0.3569(4) 0.0358(9) Uani 1 1 d . . . C3 C -0.2985(5) 0.1713(2) 0.2853(3) 0.0347(9) Uani 1 1 d . . . H3A H -0.3786 0.2080 0.2486 0.042 Uiso 1 1 calc . . . H3B H -0.1986 0.1786 0.2611 0.042 Uiso 1 1 calc . . . C4 C -0.2663(5) 0.1777(2) 0.4110(3) 0.0285(8) Uani 1 1 d . . . C5 C -0.4035(6) 0.2162(3) 0.4442(4) 0.0398(10) Uani 1 1 d . . . H5A H -0.5046 0.1918 0.4094 0.060 Uiso 1 1 calc . . . H5B H -0.4080 0.2674 0.4206 0.060 Uiso 1 1 calc . . . H5C H -0.3863 0.2141 0.5241 0.060 Uiso 1 1 calc . . . C6 C -0.1075(6) 0.2139(3) 0.4617(4) 0.0410(11) Uani 1 1 d . . . H6A H -0.0960 0.2204 0.5406 0.062 Uiso 1 1 calc . . . H6B H -0.1034 0.2618 0.4274 0.062 Uiso 1 1 calc . . . H6C H -0.0202 0.1831 0.4499 0.062 Uiso 1 1 calc . . . C7 C 0.2915(5) 0.1904(2) 0.6167(3) 0.0342(9) Uani 1 1 d . . . H7 H 0.3336 0.1593 0.5701 0.041 Uiso 1 1 calc . . . C8 C 0.3018(5) 0.2658(2) 0.6074(4) 0.0367(10) Uani 1 1 d . . . H8 H 0.3501 0.2862 0.5540 0.044 Uiso 1 1 calc . . . C9 C 0.2417(5) 0.3114(2) 0.6758(4) 0.0363(10) Uani 1 1 d . . . H9 H 0.2495 0.3630 0.6696 0.044 Uiso 1 1 calc . . . C10 C 0.1703(5) 0.2815(2) 0.7533(4) 0.0368(10) Uani 1 1 d . . . H10 H 0.1290 0.3128 0.8001 0.044 Uiso 1 1 calc . . . C11 C 0.1590(5) 0.2070(2) 0.7627(4) 0.0359(10) Uani 1 1 d . . . H11 H 0.1099 0.1869 0.8160 0.043 Uiso 1 1 calc . . . C12 C 0.2192(5) 0.1603(2) 0.6945(3) 0.0324(9) Uani 1 1 d . . . C13 C 0.1994(6) 0.0353(2) 0.8345(3) 0.0349(9) Uani 1 1 d . . . C14 C 0.3186(6) 0.0650(3) 0.9197(4) 0.0438(11) Uani 1 1 d . . . H14 H 0.3837 0.1043 0.9063 0.053 Uiso 1 1 calc . . . C15 C 0.3400(7) 0.0360(3) 1.0243(4) 0.0530(14) Uani 1 1 d . . . H15 H 0.4198 0.0561 1.0831 0.064 Uiso 1 1 calc . . . C16 C 0.2496(7) -0.0201(4) 1.0441(4) 0.0604(17) Uani 1 1 d . . . H16 H 0.2661 -0.0388 1.1165 0.072 Uiso 1 1 calc . . . C17 C 0.1333(7) -0.0507(3) 0.9603(5) 0.0590(15) Uani 1 1 d . . . H17 H 0.0719 -0.0911 0.9746 0.071 Uiso 1 1 calc . . . C18 C 0.1064(6) -0.0223(3) 0.8549(4) 0.0441(11) Uani 1 1 d . . . H18 H 0.0247 -0.0423 0.7972 0.053 Uiso 1 1 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.0462(4) 0.0251(3) 0.0258(3) 0.0038(2) 0.0096(2) 0.0011(2) Cl1 0.0592(7) 0.0378(6) 0.0310(5) -0.0027(4) 0.0161(5) 0.0034(5) Cl2 0.0810(9) 0.0320(6) 0.0382(6) 0.0079(5) 0.0094(6) -0.0113(6) P 0.0788(9) 0.0253(6) 0.0221(5) -0.0019(4) 0.0129(5) -0.0079(6) O1 0.077(2) 0.0327(17) 0.0225(15) 0.0000(12) 0.0109(15) -0.0076(16) O2 0.054(2) 0.055(2) 0.055(2) 0.0000(18) 0.0130(17) -0.0005(18) N2 0.0399(19) 0.0243(17) 0.0229(16) 0.0014(13) 0.0085(14) 0.0004(14) C1 0.098(4) 0.024(2) 0.029(2) -0.0025(18) 0.027(2) -0.008(2) C2 0.055(3) 0.026(2) 0.029(2) 0.0016(17) 0.0148(19) 0.0016(19) C3 0.045(2) 0.029(2) 0.029(2) 0.0047(16) 0.0077(18) -0.0026(18) C4 0.035(2) 0.0247(19) 0.0243(19) 0.0037(15) 0.0046(15) 0.0003(16) C5 0.043(3) 0.039(3) 0.038(2) 0.0046(19) 0.0116(19) 0.010(2) C6 0.041(2) 0.043(3) 0.036(2) 0.005(2) 0.0034(19) -0.008(2) C7 0.044(2) 0.030(2) 0.031(2) -0.0018(17) 0.0129(18) 0.0034(18) C8 0.042(2) 0.031(2) 0.041(2) 0.0015(19) 0.0165(19) -0.0010(19) C9 0.039(2) 0.024(2) 0.046(3) -0.0024(18) 0.0124(19) -0.0032(18) C10 0.038(2) 0.034(2) 0.040(2) -0.0096(19) 0.0141(19) -0.0031(19) C11 0.045(3) 0.034(2) 0.030(2) -0.0063(18) 0.0141(18) -0.0075(19) C12 0.044(2) 0.027(2) 0.0258(19) -0.0026(15) 0.0060(17) -0.0015(17) C13 0.051(3) 0.033(2) 0.0221(19) 0.0007(16) 0.0105(18) 0.0044(19) C14 0.057(3) 0.044(3) 0.031(2) -0.008(2) 0.009(2) 0.003(2) C15 0.055(3) 0.074(4) 0.026(2) -0.007(2) 0.002(2) 0.026(3) C16 0.068(4) 0.084(4) 0.037(3) 0.027(3) 0.027(3) 0.033(3) C17 0.061(3) 0.064(4) 0.061(4) 0.030(3) 0.032(3) 0.012(3) C18 0.047(3) 0.046(3) 0.039(3) 0.009(2) 0.011(2) 0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co O2 1.910(4) . ? Co N2 2.033(3) . ? Co Cl1 2.2421(12) . ? Co Cl2 2.2599(13) . ? P O2 1.427(4) . ? P C12 1.789(4) . ? P C13 1.794(4) . ? P C1 1.805(6) . ? O1 C2 1.346(5) . ? O1 C3 1.445(5) . ? N2 C2 1.284(5) . ? N2 C4 1.502(5) . ? C1 C2 1.483(6) 3_556 ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C1 1.483(6) 3_556 ? C3 C4 1.541(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C6 1.511(6) . ? C4 C5 1.519(6) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.386(6) . ? C7 C12 1.396(6) . ? C7 H7 0.9500 . ? C8 C9 1.387(6) . ? C8 H8 0.9500 . ? C9 C10 1.386(6) . ? C9 H9 0.9500 . ? C10 C11 1.373(6) . ? C10 H10 0.9500 . ? C11 C12 1.398(6) . ? C11 H11 0.9500 . ? C13 C18 1.385(7) . ? C13 C14 1.398(6) . ? C14 C15 1.388(7) . ? C14 H14 0.9500 . ? C15 C16 1.347(9) . ? C15 H15 0.9500 . ? C16 C17 1.381(9) . ? C16 H16 0.9500 . ? C17 C18 1.389(7) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Co N2 106.24(15) . . ? O2 Co Cl1 115.09(12) . . ? N2 Co Cl1 110.48(10) . . ? O2 Co Cl2 103.31(12) . . ? N2 Co Cl2 112.68(10) . . ? Cl1 Co Cl2 108.93(5) . . ? O2 P C12 114.2(2) . . ? O2 P C13 113.7(2) . . ? C12 P C13 108.8(2) . . ? O2 P C1 106.0(2) . . ? C12 P C1 107.0(2) . . ? C13 P C1 106.6(2) . . ? C2 O1 C3 106.2(3) . . ? P O2 Co 135.9(3) . . ? C2 N2 C4 107.4(3) . . ? C2 N2 Co 127.7(3) . . ? C4 N2 Co 124.9(2) . . ? C2 C1 P 111.7(4) 3_556 . ? C2 C1 H1A 109.3 3_556 . ? P C1 H1A 109.3 . . ? C2 C1 H1B 109.3 3_556 . ? P C1 H1B 109.3 . . ? H1A C1 H1B 107.9 . . ? N2 C2 O1 117.2(4) . . ? N2 C2 C1 127.4(4) . 3_556 ? O1 C2 C1 115.4(4) . 3_556 ? O1 C3 C4 104.4(3) . . ? O1 C3 H3A 110.9 . . ? C4 C3 H3A 110.9 . . ? O1 C3 H3B 110.9 . . ? C4 C3 H3B 110.9 . . ? H3A C3 H3B 108.9 . . ? N2 C4 C6 110.7(3) . . ? N2 C4 C5 109.1(3) . . ? C6 C4 C5 111.5(4) . . ? N2 C4 C3 101.5(3) . . ? C6 C4 C3 112.3(3) . . ? C5 C4 C3 111.2(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C12 120.0(4) . . ? C8 C7 H7 120.0 . . ? C12 C7 H7 120.0 . . ? C7 C8 C9 120.2(4) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C10 C9 C8 119.9(4) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C11 C10 C9 120.3(4) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 120.5(4) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C7 C12 C11 119.2(4) . . ? C7 C12 P 120.2(3) . . ? C11 C12 P 120.2(3) . . ? C18 C13 C14 120.1(4) . . ? C18 C13 P 119.5(3) . . ? C14 C13 P 119.9(4) . . ? C15 C14 C13 118.6(5) . . ? C15 C14 H14 120.7 . . ? C13 C14 H14 120.7 . . ? C16 C15 C14 121.2(5) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C15 C16 C17 120.7(5) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C16 C17 C18 119.7(5) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C13 C18 C17 119.6(5) . . ? C13 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C12 P O2 Co -60.6(4) . . . . ? C13 P O2 Co 65.1(4) . . . . ? C1 P O2 Co -178.1(3) . . . . ? N2 Co O2 P 123.2(3) . . . . ? Cl1 Co O2 P 0.6(4) . . . . ? Cl2 Co O2 P -118.0(3) . . . . ? O2 Co N2 C2 89.9(4) . . . . ? Cl1 Co N2 C2 -144.6(4) . . . . ? Cl2 Co N2 C2 -22.5(4) . . . . ? O2 Co N2 C4 -90.5(3) . . . . ? Cl1 Co N2 C4 35.0(3) . . . . ? Cl2 Co N2 C4 157.1(3) . . . . ? O2 P C1 C2 -54.2(4) . . . 3_556 ? C12 P C1 C2 -176.5(3) . . . 3_556 ? C13 P C1 C2 67.2(4) . . . 3_556 ? C4 N2 C2 O1 3.0(5) . . . . ? Co N2 C2 O1 -177.3(3) . . . . ? C4 N2 C2 C1 -179.1(5) . . . 3_556 ? Co N2 C2 C1 0.5(7) . . . 3_556 ? C3 O1 C2 N2 9.2(6) . . . . ? C3 O1 C2 C1 -168.9(4) . . . 3_556 ? C2 O1 C3 C4 -16.6(4) . . . . ? C2 N2 C4 C6 -132.3(4) . . . . ? Co N2 C4 C6 48.0(4) . . . . ? C2 N2 C4 C5 104.6(4) . . . . ? Co N2 C4 C5 -75.1(4) . . . . ? C2 N2 C4 C3 -12.9(4) . . . . ? Co N2 C4 C3 167.4(3) . . . . ? O1 C3 C4 N2 17.6(4) . . . . ? O1 C3 C4 C6 135.9(4) . . . . ? O1 C3 C4 C5 -98.4(4) . . . . ? C12 C7 C8 C9 0.6(7) . . . . ? C7 C8 C9 C10 -0.4(7) . . . . ? C8 C9 C10 C11 0.1(7) . . . . ? C9 C10 C11 C12 0.0(7) . . . . ? C8 C7 C12 C11 -0.4(7) . . . . ? C8 C7 C12 P 172.2(4) . . . . ? C10 C11 C12 C7 0.1(7) . . . . ? C10 C11 C12 P -172.5(4) . . . . ? O2 P C12 C7 -83.8(4) . . . . ? C13 P C12 C7 147.9(4) . . . . ? C1 P C12 C7 33.1(4) . . . . ? O2 P C12 C11 88.7(4) . . . . ? C13 P C12 C11 -39.5(4) . . . . ? C1 P C12 C11 -154.3(4) . . . . ? O2 P C13 C18 19.8(5) . . . . ? C12 P C13 C18 148.3(4) . . . . ? C1 P C13 C18 -96.6(4) . . . . ? O2 P C13 C14 -167.9(4) . . . . ? C12 P C13 C14 -39.5(4) . . . . ? C1 P C13 C14 75.7(4) . . . . ? C18 C13 C14 C15 -0.6(7) . . . . ? P C13 C14 C15 -172.8(4) . . . . ? C13 C14 C15 C16 0.7(8) . . . . ? C14 C15 C16 C17 0.4(8) . . . . ? C15 C16 C17 C18 -1.5(9) . . . . ? C14 C13 C18 C17 -0.5(7) . . . . ? P C13 C18 C17 171.7(4) . . . . ? C16 C17 C18 C13 1.6(8) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.930 _refine_diff_density_min -1.477 _refine_diff_density_rms 0.102