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 loop_ _publ_author_name _publ_author_address 'Stefanus Otto' ; Sasol Technology Researh & Development P. O. Box 1 Sasolburg 1947 South Africa ; 'Peter N. Bunga' ; Sasol Technology Research & Development P.O. Box 1 Sasolburg 1947 South Africa and Department of Chemistry University of the Free State P.O. Box 339 Bloemfontein 9300 South Africa ; _publ_contact_author_name 'Stefanus Otto' _publ_contact_author_address ; Research & Development Sasol Technology P.O. Box 1 Sasolburg Free State 1947 SOUTH AFRICA ; _publ_contact_author_email FANIE.OTTO@SASOL.COM _publ_section_title ; Bicyclic phosphines as ligands for cobalt catalysed hydroformylation. Crystal structures of [Co(Phoban[3.3.1]-Q)(CO)3]2 (Q= C2H5, C5H11, C3H6NMe2, C6H11) ; _publ_section_exptl_refinement ; The intensity data were collected on a Bruker SMART ApexII 4K CCD diffractometer using an exposure time of 50 seconds/frame with a frame width of 0.50\%. The first 50 frames were recollected at the end of the data collection to check for decay,no decay was found. ; _publ_section_references ; Brandenburg, K. & Berndt, M. (1999). DIAMOND. Release 2.1c. Crystal Impact GbR, Bonn, Germany. Bruker (2005). Apex2 (Version 1.0-27). Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (2004). SAINT-Plus. Version 7.12 (including XPREP). Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (2004). SADABS (Version 2004/1). Bruker AXS Inc., Madison, Wisconsin, USA. Sheldrick, G.M. (1997a). SHELXS-97. Program for Crystal Structure Solution. University of G\"ottingen, Germany. Sheldrick, G.M. (1997b). SHELXL-97. Program for Crystal Structure Refinement. University of G\"ottingen, Germany. ; _journal_coden_ASTM ? _journal_coeditor_code ? _journal_coeditor_name ? _journal_coeditor_notes ? _journal_date_accepted ? _journal_date_from_coeditor ? _journal_date_printers_final ? _journal_date_printers_first ? _journal_date_proofs_in ? _journal_date_proofs_out ? #========================================================================== # 2. PROCESSING SUMMARY (Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_volume ? _journal_year ? # Attachment '637088_cif_vs2.txt' #=================================================================== # 1. SUBMISSION DETAILS _publ_contact_author ; Stefanus Otto Sasol Technology Researh & Development P.O. Box 1 Sasolburg 1947 South Africa ; _publ_contact_author_fax 'Intl-27-11-522 3218' _publ_contact_author_phone 'Intl-27-16-960 4456' _publ_contact_letter ; Please consider this CIF file as supplementary material to our paper submitted for publication in Dalton Tarnsactions. Sincerely. Stefanus Otto ; _publ_requested_coeditor_name ? #========================================================================== data_nme _database_code_depnum_ccdc_archive 'CCDC 637085' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Hexacarbony-bis(9-(3-dimethylamino-propyl)-9- phosphabicyclo[3.3.1]nonane)-dicobalt ; _chemical_name_common ; Hexacarbony-bis(9-(3-dimethylamino-propyl)-9- phosphabicyclo(3.3.1)nonane)-dicobalt ; _chemical_formula_moiety 'C32 H52 Co2 N2 O6 P2' _chemical_formula_sum 'C32 H52 Co2 N2 O6 P2' _chemical_formula_weight 740.56 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.4773(2) _cell_length_b 10.4794(2) _cell_length_c 14.4129(2) _cell_angle_alpha 90.00 _cell_angle_beta 111.4920(10) _cell_angle_gamma 90.00 _cell_volume 1753.52(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3546 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 27.84 _exptl_crystal_description Rectangle _exptl_crystal_colour Red _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'Not measured' _exptl_crystal_density_diffrn 1.403 _exptl_crystal_density_method 'Not measured' _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 1.081 _exptl_absorpt_correction_type Multi-scans _exptl_absorpt_correction_T_min 0.8634 _exptl_absorpt_correction_T_max 0.9479 _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _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 'Bruker SMART ApexII 4K CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number 'First 50 frames repeated after data collection.' __diffrn_standards_interval_count 'After collection' _diffrn_standards_interval_time 'After collection' _diffrn_standards_decay_% None _diffrn_reflns_number 18093 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 28.25 _reflns_number_total 4321 _reflns_number_gt 3188 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2004)' _computing_data_reduction 'SAINT-Plus and XPREP (Bruker, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'DIAMOND (Brandenburg & Berndt, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997b)' _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 'w=1/[\s^2^(Fo^2^)+(0.0717P)^2^+2.7044P] 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 4321 _refine_ls_number_parameters 201 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0790 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.1563 _refine_ls_wR_factor_gt 0.1412 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.96822(4) 0.00864(4) 0.40046(3) 0.03066(16) Uani 1 d . . . P P 0.94405(7) 0.02681(10) 0.24163(6) 0.0349(2) Uani 1 d . . . N N 1.3369(4) 0.0156(4) 0.2791(3) 0.0670(11) Uani 1 d . . . O1 O 0.7334(2) -0.0257(3) 0.3971(2) 0.0523(7) Uani 1 d . . . O2 O 1.1145(3) -0.2134(3) 0.4173(2) 0.0713(10) Uani 1 d . . . O3 O 1.0481(3) 0.2722(3) 0.4356(2) 0.0539(7) Uani 1 d . . . C1 C 0.8240(3) -0.0137(3) 0.3960(2) 0.0374(8) Uani 1 d . . . C2 C 1.0572(3) -0.1261(4) 0.4124(3) 0.0441(9) Uani 1 d . . . C3 C 1.0192(3) 0.1682(4) 0.4242(2) 0.0380(8) Uani 1 d . . . C11 C 0.8666(4) -0.1070(5) 0.1551(3) 0.0586(12) Uani 1 d . . . H11 H 0.9078 -0.1889 0.1811 0.070 Uiso 1 calc R . . C12 C 0.8707(4) -0.0810(6) 0.0518(3) 0.0690(15) Uani 1 d . . . H12A H 0.9521 -0.0862 0.0576 0.083 Uiso 1 calc R . . H12B H 0.8288 -0.1509 0.0069 0.083 Uiso 1 calc R . . C13 C 0.8233(5) 0.0415(6) 0.0025(4) 0.0728(15) Uani 1 d . . . H13A H 0.8475 0.0520 -0.0552 0.087 Uiso 1 calc R . . H13B H 0.7382 0.0349 -0.0242 0.087 Uiso 1 calc R . . C14 C 0.8554(4) 0.1580(5) 0.0633(3) 0.0531(11) Uani 1 d . . . H14A H 0.8049 0.2282 0.0258 0.064 Uiso 1 calc R . . H14B H 0.9353 0.1807 0.0713 0.064 Uiso 1 calc R . . C15 C 0.8485(3) 0.1522(4) 0.1676(3) 0.0401(8) Uani 1 d . . . H15 H 0.8765 0.2357 0.2014 0.048 Uiso 1 calc R . . C16 C 0.7266(3) 0.1288(4) 0.1677(3) 0.0425(8) Uani 1 d . . . H16A H 0.7309 0.1315 0.2376 0.051 Uiso 1 calc R . . H16B H 0.6768 0.2003 0.1319 0.051 Uiso 1 calc R . . C17 C 0.6683(3) 0.0044(4) 0.1212(3) 0.0493(10) Uani 1 d . . . H17A H 0.5965 -0.0044 0.1348 0.059 Uiso 1 calc R . . H17B H 0.6464 0.0105 0.0480 0.059 Uiso 1 calc R . . C18 C 0.7396(3) -0.1160(4) 0.1570(3) 0.0445(9) Uani 1 d . . . H18A H 0.6988 -0.1883 0.1145 0.053 Uiso 1 calc R . . H18B H 0.7453 -0.1345 0.2260 0.053 Uiso 1 calc R . . C21 C 1.0819(4) 0.0353(5) 0.2256(3) 0.0605(12) Uani 1 d . . . H21A H 1.1187 -0.0497 0.2415 0.073 Uiso 1 calc R . . H21B H 1.0665 0.0519 0.1543 0.073 Uiso 1 calc R . . C22 C 1.1657(4) 0.1307(6) 0.2846(4) 0.0681(14) Uani 1 d . . . H22A H 1.1860 0.1112 0.3562 0.082 Uiso 1 calc R . . H22B H 1.1284 0.2157 0.2719 0.082 Uiso 1 calc R . . C23 C 1.2766(4) 0.1381(5) 0.2632(4) 0.0594(12) Uani 1 d . . . H23A H 1.2581 0.1655 0.1933 0.071 Uiso 1 calc R . . H23B H 1.3280 0.2032 0.3072 0.071 Uiso 1 calc R . . C24 C 1.3790(7) -0.0182(7) 0.3826(6) 0.118(3) Uani 1 d . . . H24A H 1.4298 0.0494 0.4217 0.177 Uiso 1 calc R . . H24B H 1.4221 -0.0985 0.3923 0.177 Uiso 1 calc R . . H24C H 1.3139 -0.0287 0.4046 0.177 Uiso 1 calc R . . C25 C 1.4336(5) 0.0245(5) 0.2464(5) 0.0799(17) Uani 1 d . . . H25A H 1.4839 0.0949 0.2814 0.120 Uiso 1 calc R . . H25B H 1.4052 0.0402 0.1744 0.120 Uiso 1 calc R . . H25C H 1.4772 -0.0556 0.2614 0.120 Uiso 1 calc R . . 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 0.0313(2) 0.0372(3) 0.0199(2) -0.00283(18) 0.00513(17) 0.00290(19) P 0.0289(4) 0.0520(6) 0.0214(4) -0.0056(4) 0.0062(3) 0.0016(4) N 0.057(2) 0.078(3) 0.064(3) 0.002(2) 0.019(2) -0.005(2) O1 0.0408(15) 0.076(2) 0.0408(15) 0.0002(14) 0.0162(13) -0.0029(14) O2 0.095(3) 0.072(2) 0.0462(18) 0.0080(16) 0.0256(18) 0.043(2) O3 0.070(2) 0.0447(17) 0.0421(16) -0.0086(13) 0.0151(15) -0.0085(14) C1 0.0409(19) 0.045(2) 0.0226(15) -0.0009(14) 0.0070(14) 0.0039(15) C2 0.052(2) 0.052(2) 0.0266(17) 0.0004(16) 0.0120(16) 0.0124(18) C3 0.0392(19) 0.048(2) 0.0227(16) -0.0036(14) 0.0070(14) 0.0025(16) C11 0.061(3) 0.073(3) 0.032(2) -0.007(2) 0.0051(19) 0.025(2) C12 0.051(3) 0.119(5) 0.038(2) -0.021(3) 0.016(2) 0.005(3) C13 0.081(4) 0.099(4) 0.049(3) -0.007(3) 0.036(3) -0.010(3) C14 0.051(2) 0.076(3) 0.033(2) 0.0148(19) 0.0165(18) 0.010(2) C15 0.047(2) 0.042(2) 0.0316(18) 0.0009(15) 0.0151(16) -0.0020(16) C16 0.044(2) 0.047(2) 0.039(2) 0.0090(16) 0.0173(17) 0.0118(16) C17 0.0319(17) 0.064(3) 0.050(2) 0.009(2) 0.0131(17) -0.0001(18) C18 0.047(2) 0.048(2) 0.0332(19) -0.0086(16) 0.0091(17) -0.0010(17) C21 0.039(2) 0.105(4) 0.037(2) -0.001(2) 0.0141(18) -0.003(2) C22 0.053(3) 0.099(4) 0.052(3) -0.004(3) 0.019(2) -0.016(3) C23 0.041(2) 0.077(3) 0.061(3) -0.002(2) 0.020(2) -0.003(2) C24 0.111(6) 0.142(7) 0.080(5) 0.021(4) 0.009(4) 0.042(5) C25 0.053(3) 0.077(4) 0.112(5) -0.015(3) 0.032(3) -0.001(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 C2 1.765(4) . ? Co C3 1.777(4) . ? Co C1 1.792(4) . ? Co P 2.2049(9) . ? Co Co 2.6885(8) 3_756 ? P C21 1.819(4) . ? P C15 1.832(4) . ? P C11 1.891(5) . ? N C24 1.433(8) . ? N C25 1.450(6) . ? N C23 1.464(6) . ? O1 C1 1.143(4) . ? O2 C2 1.147(5) . ? O3 C3 1.141(5) . ? C11 C12 1.533(6) . ? C11 C18 1.598(6) . ? C11 H11 1.0000 . ? C12 C13 1.482(8) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.471(7) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.538(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.541(5) . ? C15 H15 1.0000 . ? C16 C17 1.523(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.520(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C21 C22 1.471(7) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.526(6) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 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 C2 Co C3 124.47(19) . . ? C2 Co C1 119.08(18) . . ? C3 Co C1 114.45(17) . . ? C2 Co P 90.70(12) . . ? C3 Co P 91.25(11) . . ? C1 Co P 102.76(11) . . ? C2 Co Co 85.01(12) . 3_756 ? C3 Co Co 85.02(11) . 3_756 ? C1 Co Co 85.91(11) . 3_756 ? P Co Co 171.33(4) . 3_756 ? C21 P C15 109.6(2) . . ? C21 P C11 103.4(2) . . ? C15 P C11 94.68(19) . . ? C21 P Co 111.08(15) . . ? C15 P Co 118.61(12) . . ? C11 P Co 117.60(15) . . ? C24 N C25 108.9(5) . . ? C24 N C23 110.6(5) . . ? C25 N C23 109.5(4) . . ? O1 C1 Co 177.1(3) . . ? O2 C2 Co 178.0(3) . . ? O3 C3 Co 177.0(3) . . ? C12 C11 C18 114.4(3) . . ? C12 C11 P 108.5(4) . . ? C18 C11 P 107.6(3) . . ? C12 C11 H11 108.7 . . ? C18 C11 H11 108.7 . . ? P C11 H11 108.7 . . ? C13 C12 C11 118.1(4) . . ? C13 C12 H12A 107.8 . . ? C11 C12 H12A 107.8 . . ? C13 C12 H12B 107.8 . . ? C11 C12 H12B 107.8 . . ? H12A C12 H12B 107.1 . . ? C14 C13 C12 117.4(4) . . ? C14 C13 H13A 108.0 . . ? C12 C13 H13A 108.0 . . ? C14 C13 H13B 108.0 . . ? C12 C13 H13B 108.0 . . ? H13A C13 H13B 107.2 . . ? C13 C14 C15 116.7(4) . . ? C13 C14 H14A 108.1 . . ? C15 C14 H14A 108.1 . . ? C13 C14 H14B 108.1 . . ? C15 C14 H14B 108.1 . . ? H14A C14 H14B 107.3 . . ? C14 C15 C16 114.6(3) . . ? C14 C15 P 109.9(3) . . ? C16 C15 P 108.5(2) . . ? C14 C15 H15 107.9 . . ? C16 C15 H15 107.9 . . ? P C15 H15 107.9 . . ? C17 C16 C15 116.6(3) . . ? C17 C16 H16A 108.1 . . ? C15 C16 H16A 108.1 . . ? C17 C16 H16B 108.1 . . ? C15 C16 H16B 108.1 . . ? H16A C16 H16B 107.3 . . ? C18 C17 C16 115.8(3) . . ? C18 C17 H17A 108.3 . . ? C16 C17 H17A 108.3 . . ? C18 C17 H17B 108.3 . . ? C16 C17 H17B 108.3 . . ? H17A C17 H17B 107.4 . . ? C17 C18 C11 113.9(3) . . ? C17 C18 H18A 108.8 . . ? C11 C18 H18A 108.8 . . ? C17 C18 H18B 108.8 . . ? C11 C18 H18B 108.8 . . ? H18A C18 H18B 107.7 . . ? C22 C21 P 117.7(4) . . ? C22 C21 H21A 107.9 . . ? P C21 H21A 107.9 . . ? C22 C21 H21B 107.9 . . ? P C21 H21B 107.9 . . ? H21A C21 H21B 107.2 . . ? C21 C22 C23 115.1(4) . . ? C21 C22 H22A 108.5 . . ? C23 C22 H22A 108.5 . . ? C21 C22 H22B 108.5 . . ? C23 C22 H22B 108.5 . . ? H22A C22 H22B 107.5 . . ? N C23 C22 112.1(4) . . ? N C23 H23A 109.2 . . ? C22 C23 H23A 109.2 . . ? N C23 H23B 109.2 . . ? C22 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? N C24 H24A 109.5 . . ? N C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N C25 H25A 109.5 . . ? N C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 28.25 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 1.068 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.089 #========================================================================== # 4. TEXT _publ_section_abstract ; See text. ; _publ_section_comment ; See text. ; _publ_section_exptl_prep ; See text. ; _publ_section_exptl_refinement ; The intensity data were collected on a Bruker X8 ApexII 4K Kappa CCD diffractometer using an exposure time of 10 seconds/frame with a frame width of 0.50\%. The first 50 frames were recollected at the end of the data collection to check for decay,no decay was found. ; _publ_section_references ; Brandenburg, K. & Berndt, M. (1999). DIAMOND. Release 2.1c. Crystal Impact GbR, Bonn, Germany. Bruker (2005). Apex2 (Version 1.0-27). Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (2004). SAINT-Plus. Version 7.12 (including XPREP). Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (2004). SADABS (Version 2004/1). Bruker AXS Inc., Madison, Wisconsin, USA. Sheldrick, G.M. (1997a). SHELXS-97. Program for Crystal Structure Solution. University of G\"ottingen, Germany. Sheldrick, G.M. (1997b). SHELXL-97. Program for Crystal Structure Refinement. University of G\"ottingen, Germany. ; _publ_section_figure_captions ; See text. ; _publ_section_acknowledgements ; See text. ; #========================================================================== data_coc2 _database_code_depnum_ccdc_archive 'CCDC 637086' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Hexacarbonyl-bis(9-ethyl-9-phosphabicyclo[3.3.1]nonane)-dicobalt ; _chemical_name_common ;Hexacarbonyl-bis(9-ethyl-9-phosphabicyclo(3.3.1)nonane)- dicobalt ; _chemical_melting_point ? _chemical_formula_moiety 'C26 H38 Co2 O6 P2' _chemical_formula_sum 'C26 H38 Co2 O6 P2' _chemical_formula_weight 626.36 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Cmca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' '-x+1/2, y+1, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' 'x+1/2, -y, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 11.403(2) _cell_length_b 14.964(3) _cell_length_c 16.632(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2838.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 923 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 25.91 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 1.322 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6769 _exptl_absorpt_correction_T_max 0.9368 _exptl_absorpt_process_details ; SADABS (Bruker, 2004) ; _exptl_special_details ; The intensity data was collected on a Bruker SMART 1K CCD diffractometer using an exposure time of 20 seconds/frame. A total of 1315 frames were collected with a frame width of 0.3\% covering up to \q = 26.36\% with 99.5% completeness accomplished. ; _diffrn_ambient_temperature 293(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 'Bruker SMART 1K CCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 512 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8301 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_sigmaI/netI 0.0235 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.31 _diffrn_reflns_theta_max 26.36 _reflns_number_total 1520 _reflns_number_gt 1342 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT (Bruker, 1998)' _computing_cell_refinement 'SAINT-Plus (Bruker, 1999)' _computing_data_reduction 'SAINT-Plus and XPREP (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg & Berndt, 1999)' _computing_publication_material Word _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^)+(0.0683P)^2^+69.4673P] 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 1520 _refine_ls_number_parameters 98 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1004 _refine_ls_R_factor_gt 0.0925 _refine_ls_wR_factor_ref 0.2145 _refine_ls_wR_factor_gt 0.2109 _refine_ls_goodness_of_fit_ref 1.199 _refine_ls_restrained_S_all 1.199 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.5000 0.42391(10) 0.54400(9) 0.0415(5) Uani 1 d S . . C2 C 0.6365(10) 0.4622(6) 0.5799(6) 0.063(2) Uani 1 d . . . O2 O 0.7275(8) 0.4809(6) 0.6039(5) 0.108(3) Uani 1 d . . . c1 C 0.5000 0.3678(8) 0.4506(8) 0.060(4) Uani 1 d S . . O1 O 0.5000 0.3329(7) 0.3880(6) 0.112(5) Uani 1 d S . . P P 0.5000 0.30863(19) 0.62602(17) 0.0445(8) Uani 1 d S . . C21 C 0.5000 0.3443(8) 0.7319(7) 0.065(4) Uani 1 d S . . H21A H 0.4349 0.3854 0.7388 0.078 Uiso 0.50 calc PR . . H21B H 0.4828 0.2920 0.7643 0.078 Uiso 0.50 calc PR . . C22 C 0.5962(19) 0.3837(14) 0.7637(11) 0.076(6) Uani 0.50 d P . . H22A H 0.6121 0.4384 0.7356 0.114 Uiso 0.50 calc PR . . H22B H 0.6622 0.3443 0.7587 0.114 Uiso 0.50 calc PR . . H22C H 0.5825 0.3964 0.8195 0.114 Uiso 0.50 calc PR . . C11 C 0.3822(12) 0.2269(7) 0.6178(6) 0.085(4) Uani 1 d . . . H11 H 0.3070 0.2583 0.6222 0.102 Uiso 1 calc R . . C12 C 0.3913(14) 0.1858(8) 0.5321(6) 0.111(6) Uani 1 d . . . H12A H 0.3269 0.1440 0.5261 0.133 Uiso 1 calc R . . H12B H 0.3784 0.2336 0.4938 0.133 Uiso 1 calc R . . C18 C 0.390(2) 0.1571(9) 0.6863(7) 0.152(9) Uani 1 d . . . H18A H 0.3813 0.1882 0.7371 0.183 Uiso 1 calc R . . H18B H 0.3243 0.1165 0.6811 0.183 Uiso 1 calc R . . C13 C 0.5000 0.1387(12) 0.5081(11) 0.148(13) Uani 1 d S . . H13A H 0.5000 0.1313 0.4501 0.177 Uiso 1 calc SR . . H13B H 0.5000 0.0796 0.5320 0.177 Uiso 1 calc SR . . C17 C 0.5000 0.1029(13) 0.6899(14) 0.22(3) Uani 1 d S . . H17A H 0.5000 0.0609 0.6455 0.269 Uiso 1 calc SR . . H17B H 0.5000 0.0686 0.7394 0.269 Uiso 1 calc SR . . 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 0.0522(9) 0.0329(7) 0.0395(8) 0.0038(6) 0.000 0.000 C2 0.077(7) 0.053(5) 0.059(5) 0.014(4) -0.009(5) -0.010(5) O2 0.095(6) 0.114(7) 0.116(6) 0.033(5) -0.047(6) -0.055(6) c1 0.099(11) 0.036(6) 0.046(7) 0.007(5) 0.000 0.000 O1 0.230(17) 0.063(7) 0.044(6) -0.003(5) 0.000 0.000 P 0.065(2) 0.0318(14) 0.0367(14) 0.0012(11) 0.000 0.000 C21 0.112(12) 0.042(7) 0.042(7) -0.003(5) 0.000 0.000 C22 0.093(15) 0.087(14) 0.048(11) -0.016(10) -0.014(11) -0.025(13) C11 0.127(10) 0.066(6) 0.061(6) -0.002(5) 0.019(7) -0.051(7) C12 0.198(17) 0.079(8) 0.056(6) -0.007(6) -0.014(8) -0.087(10) C18 0.31(3) 0.083(9) 0.064(7) -0.004(7) 0.032(12) -0.117(14) C13 0.33(4) 0.056(10) 0.053(10) -0.025(8) 0.000 0.000 C17 0.57(8) 0.040(10) 0.066(12) 0.013(10) 0.000 0.000 _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 C2 1.763(11) . ? Co C2 1.763(11) 12_655 ? Co c1 1.766(13) . ? Co P 2.199(3) . ? Co Co 2.707(3) 9_666 ? C2 O2 1.146(12) . ? c1 O1 1.165(15) . ? P C11 1.821(10) . ? P C11 1.821(10) 12_655 ? P C21 1.840(12) . ? C21 C22 1.35(2) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C11 C18 1.549(16) . ? C11 C12 1.555(14) . ? C11 H11 0.9800 . ? C12 C13 1.480(16) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C18 C17 1.49(2) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C13 C12 1.480(16) 12_655 ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C17 C18 1.49(2) 12_655 ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? 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 C2 Co C2 124.0(7) . 12_655 ? C2 Co c1 116.9(3) . . ? C2 Co c1 116.9(3) 12_655 . ? C2 Co P 92.6(3) . . ? C2 Co P 92.6(3) 12_655 . ? c1 Co P 99.9(4) . . ? C2 Co Co 84.8(3) . 9_666 ? C2 Co Co 84.8(3) 12_655 9_666 ? c1 Co Co 85.7(4) . 9_666 ? P Co Co 174.39(13) . 9_666 ? O2 C2 Co 175.1(10) . . ? O1 c1 Co 178.2(11) . . ? C11 P C11 95.0(9) . 12_655 ? C11 P C21 105.5(4) . . ? C11 P C21 105.5(4) 12_655 . ? C11 P Co 118.7(4) . . ? C11 P Co 118.7(4) 12_655 . ? C21 P Co 111.5(4) . . ? C22 C21 P 120.1(10) . . ? C22 C21 H21A 107.3 . . ? P C21 H21A 107.3 . . ? C22 C21 H21B 107.3 . . ? P C21 H21B 107.3 . . ? H21A C21 H21B 106.9 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C18 C11 C12 113.8(9) . . ? C18 C11 P 110.7(10) . . ? C12 C11 P 106.6(7) . . ? C18 C11 H11 108.5 . . ? C12 C11 H11 108.5 . . ? P C11 H11 108.5 . . ? C13 C12 C11 119.5(13) . . ? C13 C12 H12A 107.4 . . ? C11 C12 H12A 107.4 . . ? C13 C12 H12B 107.4 . . ? C11 C12 H12B 107.4 . . ? H12A C12 H12B 107.0 . . ? C17 C18 C11 116.4(16) . . ? C17 C18 H18A 108.2 . . ? C11 C18 H18A 108.2 . . ? C17 C18 H18B 108.2 . . ? C11 C18 H18B 108.2 . . ? H18A C18 H18B 107.3 . . ? C12 C13 C12 113.6(13) . 12_655 ? C12 C13 H13A 108.8 . . ? C12 C13 H13A 108.8 12_655 . ? C12 C13 H13B 108.8 . . ? C12 C13 H13B 108.8 12_655 . ? H13A C13 H13B 107.7 . . ? C18 C17 C18 114.0(16) . 12_655 ? C18 C17 H17A 108.7 . . ? C18 C17 H17A 108.7 12_655 . ? C18 C17 H17B 108.7 . . ? C18 C17 H17B 108.7 12_655 . ? H17A C17 H17B 107.6 . . ? 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 C2 Co C2 O2 130(11) 12_655 . . . ? c1 Co C2 O2 -67(12) . . . . ? P Co C2 O2 35(12) . . . . ? Co Co C2 O2 -150(12) 9_666 . . . ? C2 Co c1 O1 -81.9(4) . . . . ? C2 Co c1 O1 81.9(4) 12_655 . . . ? P Co c1 O1 180.00(8) . . . . ? Co Co c1 O1 0.00(8) 9_666 . . . ? C2 Co P C11 -175.1(6) . . . . ? C2 Co P C11 60.7(6) 12_655 . . . ? C1 Co P C11 -57.2(4) . . . . ? Co Co P C11 122.8(4) 9_666 . . . ? C2 Co P C11 -60.7(6) . . . 12_655 ? C2 Co P C11 175.1(6) 12_655 . . 12_655 ? C1 Co P C11 57.2(4) . . . 12_655 ? Co Co P C11 -122.8(4) 9_666 . . 12_655 ? C2 Co P C21 62.1(3) . . . . ? C2 Co P C21 -62.1(3) 12_655 . . . ? C1 Co P C21 180.000(2) . . . . ? Co Co P C21 0.000(5) 9_666 . . . ? C11 P C21 C22 160.4(14) . . . . ? C11 P C21 C22 60.6(15) 12_655 . . . ? Co P C21 C22 -69.5(14) . . . . ? C11 P C11 C18 59.6(11) 12_655 . . . ? C21 P C11 C18 -48.0(11) . . . . ? Co P C11 C18 -173.7(9) . . . . ? C11 P C11 C12 -64.6(10) 12_655 . . . ? C21 P C11 C12 -172.2(9) . . . . ? Co P C11 C12 62.0(10) . . . . ? C18 C11 C12 C13 -62.4(17) . . . . ? P C11 C12 C13 59.9(14) . . . . ? C12 C11 C18 C17 59.7(19) . . . . ? P C11 C18 C17 -60.3(14) . . . . ? C11 C12 C13 C12 -44(2) . . . 12_655 ? C11 C18 C17 C18 50(3) . . . 12_655 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 0.465 _refine_diff_density_max 0.714 _refine_diff_density_min -0.997 _refine_diff_density_rms 0.129 #========================================================================== # 4. TEXT _publ_section_abstract ; See text. ; _publ_section_comment ; See text. ; _publ_section_exptl_prep ; See text. ; _publ_section_exptl_refinement ; The intensity data were collected on a Bruker SMART 1K CCD diffractometer using an exposure time of 10 seconds/frame with a frame width of 0.30\%. The first 50 frames were recollected at the end of the data collection to check for decay,no decay was found. ; _publ_section_references ; Brandenburg, K. & Berndt, M. (1999). DIAMOND. Release 2.1c. Crystal Impact GbR, Bonn, Germany. Bruker (1998). SMART-NT (Version 5.050). Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (1999). SAINT+. Version 6.02 (including XPREP). Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (2004). SADABS (Version 2004/1). Bruker AXS Inc., Madison, Wisconsin, USA. Sheldrick, G.M. (1997a). SHELXS-97. Program for Crystal Structure Solution. University of G\"ottingen, Germany. Sheldrick, G.M. (1997b). SHELXL-97. Program for Crystal Structure Refinement. University of G\"ottingen, Germany. ; _publ_section_figure_captions ; See text. ; _publ_section_acknowledgements ; See text. ; #========================================================================== data_coc5 _database_code_depnum_ccdc_archive 'CCDC 637087' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Hexacarbony-bis(9-pentyl-9-phosphabicyclo[3.3.1]nonane)-dicobalt ; _chemical_name_common ;Hexacarbony-bis(9-pentyl-9-phosphabicyclo(3.3.1)nonane)- dicobalt ; _chemical_formula_moiety 'C32 H50 Co2 O6 P2' _chemical_formula_sum 'C32 H50 Co2 O6 P2' _chemical_formula_weight 710.52 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2166(18) _cell_length_b 9.3388(19) _cell_length_c 11.667(2) _cell_angle_alpha 92.67(3) _cell_angle_beta 109.75(3) _cell_angle_gamma 109.15(3) _cell_volume 878.7(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 725 _cell_measurement_theta_min 2.74 _cell_measurement_theta_max 27.25 _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'Not measured' _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_method 'Not measured' _exptl_crystal_F_000 374 _exptl_absorpt_coefficient_mu 1.074 _exptl_absorpt_correction_type Multi-scans _exptl_absorpt_correction_T_min 0.616 _exptl_absorpt_correction_T_max 0.856 _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Bruker SMART 1K CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number 'First 50 frames repeated after data collection.' _diffrn_standards_interval_count 'After collection' _diffrn_standards_interval_time 'After collection' _diffrn_standards_decay_% None _diffrn_reflns_number 6128 _diffrn_reflns_av_R_equivalents 0.0210 _diffrn_reflns_av_sigmaI/netI 0.0462 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 28.30 _reflns_number_total 4248 _reflns_number_gt 2976 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT (Bruker, 1998)' _computing_cell_refinement 'SAINT+ (Bruker, 1999)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'DIAMOND (Brandenburg & Berndt, 1999)' _computing_publication_material Word _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 'w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+0.0792P] 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 4248 _refine_ls_number_parameters 220 _refine_ls_number_restraints 51 _refine_ls_R_factor_all 0.0671 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.1048 _refine_ls_wR_factor_gt 0.0927 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.035 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.45527(4) 0.58823(4) 0.56538(3) 0.04429(13) Uani 1 d . . . P P 0.40422(8) 0.71952(7) 0.69956(6) 0.04279(16) Uani 1 d . . . C1 C 0.3176(4) 0.6022(3) 0.4196(3) 0.0601(7) Uani 1 d . . . C2 C 0.3892(4) 0.4216(3) 0.6282(3) 0.0613(7) Uani 1 d . . . C3 C 0.6616(4) 0.7219(3) 0.6127(3) 0.0537(6) Uani 1 d . . . O1 O 0.2317(3) 0.6087(3) 0.3246(2) 0.0988(8) Uani 1 d . . . O2 O 0.3414(4) 0.3180(3) 0.6721(2) 0.0950(8) Uani 1 d . . . O3 O 0.7926(3) 0.8135(3) 0.6445(2) 0.0749(6) Uani 1 d . . . C11 C 0.1885(3) 0.6750(3) 0.6845(2) 0.0516(6) Uani 1 d . . . H11 H 0.1399 0.5644 0.6837 0.062 Uiso 1 calc R . . C12 C 0.1787(4) 0.7612(4) 0.7952(3) 0.0678(8) Uani 1 d . . . H12A H 0.0628 0.7347 0.7827 0.081 Uiso 1 calc R . . H12B H 0.2292 0.7238 0.8689 0.081 Uiso 1 calc R . . C13 C 0.2601(4) 0.9355(4) 0.8196(3) 0.0751(9) Uani 1 d . . . H13A H 0.2702 0.9738 0.9018 0.090 Uiso 1 calc R . . H13B H 0.1864 0.9753 0.7611 0.090 Uiso 1 calc R . . C14 C 0.4305(4) 1.0023(3) 0.8112(3) 0.0695(8) Uani 1 d . . . H14A H 0.5121 0.9948 0.8869 0.083 Uiso 1 calc R . . H14B H 0.4554 1.1109 0.8075 0.083 Uiso 1 calc R . . C15 C 0.4515(3) 0.9261(3) 0.7004(2) 0.0533(6) Uani 1 d . . . H15 H 0.5679 0.9733 0.7100 0.064 Uiso 1 calc R . . C16 C 0.3455(4) 0.9451(3) 0.5741(3) 0.0605(7) Uani 1 d . . . H16A H 0.3754 0.9022 0.5120 0.073 Uiso 1 calc R . . H16B H 0.3741 1.0544 0.5724 0.073 Uiso 1 calc R . . C17 C 0.1572(4) 0.8714(4) 0.5360(3) 0.0674(8) Uani 1 d . . . H17A H 0.1222 0.9355 0.5803 0.081 Uiso 1 calc R . . H17B H 0.1055 0.8711 0.4484 0.081 Uiso 1 calc R . . C18 C 0.0932(3) 0.7078(3) 0.5595(3) 0.0592(7) Uani 1 d . . . H18A H 0.0929 0.6386 0.4948 0.071 Uiso 1 calc R . . H18B H -0.0209 0.6826 0.5518 0.071 Uiso 1 calc R . . C21 C 0.5050(4) 0.6921(4) 0.8574(3) 0.0624(7) Uani 1 d . . . H21A H 0.4878 0.7589 0.9136 0.075 Uiso 1 calc R . . H21B H 0.4480 0.5869 0.8637 0.075 Uiso 1 calc R . . C22 C 0.6871(4) 0.7211(4) 0.9029(3) 0.0744(9) Uani 1 d D . . H22A H 0.7056 0.6492 0.8519 0.089 Uiso 1 calc R A 1 H22B H 0.7457 0.8244 0.8936 0.089 Uiso 1 calc R A 1 C231 C 0.7564(18) 0.705(3) 1.0348(14) 0.086(7) Uani 0.304(14) d PDU B 1 H23A H 0.7006 0.7436 1.0787 0.103 Uiso 0.304(14) calc PR B 1 H23B H 0.7268 0.5957 1.0375 0.103 Uiso 0.304(14) calc PR B 1 C241 C 0.9375(16) 0.781(2) 1.1050(13) 0.120(6) Uani 0.304(14) d PDU B 1 H24A H 0.9645 0.8915 1.1155 0.144 Uiso 0.304(14) calc PR B 1 H24B H 0.9623 0.7539 1.1868 0.144 Uiso 0.304(14) calc PR B 1 C251 C 1.046(3) 0.746(3) 1.052(2) 0.136(10) Uani 0.304(14) d PDU B 1 H25A H 1.0115 0.6363 1.0306 0.204 Uiso 0.304(14) calc PR B 1 H25B H 1.1575 0.7866 1.1120 0.204 Uiso 0.304(14) calc PR B 1 H25C H 1.0407 0.7915 0.9798 0.204 Uiso 0.304(14) calc PR B 1 C232 C 0.7494(9) 0.6631(15) 1.0234(7) 0.082(3) Uani 0.696(14) d PDU B 2 H23C H 0.7389 0.7234 1.0880 0.098 Uiso 0.696(14) calc PR B 2 H23D H 0.6766 0.5574 1.0136 0.098 Uiso 0.696(14) calc PR B 2 C242 C 0.9230(8) 0.6679(10) 1.0668(7) 0.108(3) Uani 0.696(14) d PDU B 2 H24C H 0.9412 0.6133 1.1359 0.129 Uiso 0.696(14) calc PR B 2 H24D H 0.9371 0.6140 1.0007 0.129 Uiso 0.696(14) calc PR B 2 C252 C 1.0481(12) 0.8232(12) 1.1053(13) 0.156(5) Uani 0.696(14) d PDU B 2 H25D H 1.0295 0.8792 1.0382 0.233 Uiso 0.696(14) calc PR B 2 H25E H 1.1561 0.8177 1.1279 0.233 Uiso 0.696(14) calc PR B 2 H25F H 1.0408 0.8750 1.1750 0.233 Uiso 0.696(14) calc PR B 2 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 0.0470(2) 0.0443(2) 0.0522(2) 0.00585(15) 0.02308(16) 0.02554(16) P 0.0424(3) 0.0429(3) 0.0488(4) 0.0037(3) 0.0190(3) 0.0214(3) C1 0.0671(19) 0.0685(18) 0.0623(18) 0.0069(14) 0.0285(15) 0.0430(16) C2 0.077(2) 0.0513(16) 0.0699(19) 0.0048(14) 0.0366(16) 0.0325(15) C3 0.0540(17) 0.0582(17) 0.0625(17) 0.0086(13) 0.0285(14) 0.0308(14) O1 0.108(2) 0.149(2) 0.0602(14) 0.0156(14) 0.0170(13) 0.0882(19) O2 0.156(2) 0.0580(14) 0.1132(19) 0.0335(13) 0.0885(18) 0.0493(15) O3 0.0526(13) 0.0768(15) 0.0914(16) 0.0026(12) 0.0316(12) 0.0156(11) C11 0.0476(15) 0.0501(15) 0.0638(16) 0.0039(12) 0.0290(13) 0.0188(12) C12 0.0627(19) 0.090(2) 0.0671(19) 0.0049(16) 0.0345(16) 0.0386(17) C13 0.080(2) 0.086(2) 0.070(2) -0.0117(16) 0.0273(17) 0.0474(19) C14 0.078(2) 0.0568(18) 0.0680(19) -0.0121(14) 0.0157(16) 0.0321(16) C15 0.0472(15) 0.0424(14) 0.0703(18) -0.0004(12) 0.0225(13) 0.0174(12) C16 0.076(2) 0.0467(15) 0.0717(19) 0.0163(13) 0.0340(16) 0.0308(15) C17 0.072(2) 0.078(2) 0.0636(19) 0.0089(15) 0.0182(15) 0.0485(18) C18 0.0371(14) 0.0724(19) 0.0651(17) -0.0040(14) 0.0159(13) 0.0220(13) C21 0.0658(18) 0.0726(19) 0.0568(17) 0.0109(14) 0.0217(14) 0.0365(16) C22 0.0652(19) 0.103(3) 0.065(2) 0.0258(18) 0.0226(16) 0.0428(19) C231 0.076(8) 0.088(13) 0.098(13) 0.001(9) 0.020(9) 0.052(8) C241 0.078(8) 0.099(15) 0.184(16) 0.008(12) 0.048(10) 0.036(10) C251 0.090(14) 0.21(3) 0.126(18) 0.048(18) 0.060(13) 0.053(19) C232 0.072(4) 0.100(7) 0.070(5) 0.044(4) 0.016(3) 0.033(3) C242 0.086(4) 0.122(6) 0.100(5) 0.036(4) 0.005(4) 0.047(4) C252 0.091(7) 0.134(8) 0.189(14) 0.017(7) 0.016(8) 0.016(6) _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 C2 1.765(3) . ? Co C3 1.774(3) . ? Co C1 1.786(3) . ? Co P 2.2074(9) . ? Co Co 2.6888(9) 2_666 ? P C15 1.832(3) . ? P C21 1.834(3) . ? P C11 1.836(3) . ? C1 O1 1.142(3) . ? C2 O2 1.146(3) . ? C3 O3 1.148(3) . ? C11 C18 1.531(4) . ? C11 C12 1.534(4) . ? C11 H11 0.9800 . ? C12 C13 1.519(5) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.527(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.546(4) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.524(4) . ? C15 H15 0.9800 . ? C16 C17 1.533(4) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.522(4) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C21 C22 1.503(4) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C231 1.490(14) . ? C22 C232 1.527(7) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C231 C241 1.485(14) . ? C231 H23A 0.9700 . ? C231 H23B 0.9700 . ? C241 C251 1.447(14) . ? C241 H24A 0.9700 . ? C241 H24B 0.9700 . ? C251 H25A 0.9600 . ? C251 H25B 0.9600 . ? C251 H25C 0.9600 . ? C232 C242 1.491(8) . ? C232 H23C 0.9700 . ? C232 H23D 0.9700 . ? C242 C252 1.458(10) . ? C242 H24C 0.9700 . ? C242 H24D 0.9700 . ? C252 H25D 0.9600 . ? C252 H25E 0.9600 . ? C252 H25F 0.9600 . ? 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 C2 Co C3 125.90(14) . . ? C2 Co C1 117.62(15) . . ? C3 Co C1 114.72(14) . . ? C2 Co P 89.41(9) . . ? C3 Co P 91.65(9) . . ? C1 Co P 103.00(9) . . ? C2 Co Co 84.39(9) . 2_666 ? C3 Co Co 86.20(9) . 2_666 ? C1 Co Co 86.29(8) . 2_666 ? P Co Co 170.49(3) . 2_666 ? C15 P C21 108.44(14) . . ? C15 P C11 95.19(13) . . ? C21 P C11 103.37(13) . . ? C15 P Co 118.47(9) . . ? C21 P Co 110.73(10) . . ? C11 P Co 118.76(9) . . ? O1 C1 Co 177.9(2) . . ? O2 C2 Co 175.7(2) . . ? O3 C3 Co 176.9(2) . . ? C18 C11 C12 113.6(2) . . ? C18 C11 P 108.65(17) . . ? C12 C11 P 111.34(19) . . ? C18 C11 H11 107.7 . . ? C12 C11 H11 107.7 . . ? P C11 H11 107.7 . . ? C13 C12 C11 116.3(2) . . ? C13 C12 H12A 108.2 . . ? C11 C12 H12A 108.2 . . ? C13 C12 H12B 108.2 . . ? C11 C12 H12B 108.2 . . ? H12A C12 H12B 107.4 . . ? C12 C13 C14 116.9(2) . . ? C12 C13 H13A 108.1 . . ? C14 C13 H13A 108.1 . . ? C12 C13 H13B 108.1 . . ? C14 C13 H13B 108.1 . . ? H13A C13 H13B 107.3 . . ? C13 C14 C15 116.1(2) . . ? C13 C14 H14A 108.3 . . ? C15 C14 H14A 108.3 . . ? C13 C14 H14B 108.3 . . ? C15 C14 H14B 108.3 . . ? H14A C14 H14B 107.4 . . ? C16 C15 C14 114.6(2) . . ? C16 C15 P 107.67(18) . . ? C14 C15 P 111.02(19) . . ? C16 C15 H15 107.8 . . ? C14 C15 H15 107.8 . . ? P C15 H15 107.8 . . ? C15 C16 C17 116.8(2) . . ? C15 C16 H16A 108.1 . . ? C17 C16 H16A 108.1 . . ? C15 C16 H16B 108.1 . . ? C17 C16 H16B 108.1 . . ? H16A C16 H16B 107.3 . . ? C18 C17 C16 115.4(2) . . ? C18 C17 H17A 108.4 . . ? C16 C17 H17A 108.4 . . ? C18 C17 H17B 108.4 . . ? C16 C17 H17B 108.4 . . ? H17A C17 H17B 107.5 . . ? C17 C18 C11 116.7(2) . . ? C17 C18 H18A 108.1 . . ? C11 C18 H18A 108.1 . . ? C17 C18 H18B 108.1 . . ? C11 C18 H18B 108.1 . . ? H18A C18 H18B 107.3 . . ? C22 C21 P 118.1(2) . . ? C22 C21 H21A 107.8 . . ? P C21 H21A 107.8 . . ? C22 C21 H21B 107.8 . . ? P C21 H21B 107.8 . . ? H21A C21 H21B 107.1 . . ? C231 C22 C21 112.9(7) . . ? C231 C22 C232 14.5(15) . . ? C21 C22 C232 113.3(4) . . ? C231 C22 H22A 109.0 . . ? C21 C22 H22A 109.0 . . ? C232 C22 H22A 95.9 . . ? C231 C22 H22B 109.0 . . ? C21 C22 H22B 109.0 . . ? C232 C22 H22B 120.5 . . ? H22A C22 H22B 107.8 . . ? C241 C231 C22 118.7(13) . . ? C241 C231 H23A 107.6 . . ? C22 C231 H23A 107.6 . . ? C241 C231 H23B 107.6 . . ? C22 C231 H23B 107.6 . . ? H23A C231 H23B 107.1 . . ? C251 C241 C231 117.2(14) . . ? C251 C241 H24A 108.0 . . ? C231 C241 H24A 108.0 . . ? C251 C241 H24B 108.0 . . ? C231 C241 H24B 108.0 . . ? H24A C241 H24B 107.3 . . ? C242 C232 C22 117.1(6) . . ? C242 C232 H23C 108.0 . . ? C22 C232 H23C 108.0 . . ? C242 C232 H23D 108.0 . . ? C22 C232 H23D 108.0 . . ? H23C C232 H23D 107.3 . . ? C252 C242 C232 114.0(9) . . ? C252 C242 H24C 108.8 . . ? C232 C242 H24C 108.8 . . ? C252 C242 H24D 108.8 . . ? C232 C242 H24D 108.8 . . ? H24C C242 H24D 107.7 . . ? C242 C252 H25D 109.5 . . ? C242 C252 H25E 109.5 . . ? H25D C252 H25E 109.5 . . ? C242 C252 H25F 109.5 . . ? H25D C252 H25F 109.5 . . ? H25E C252 H25F 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 C2 Co P C15 177.65(14) . . . . ? C3 Co P C15 51.75(14) . . . . ? C1 Co P C15 -64.09(15) . . . . ? Co Co P C15 128.46(18) 2_666 . . . ? C2 Co P C21 51.50(15) . . . . ? C3 Co P C21 -74.40(14) . . . . ? C1 Co P C21 169.76(14) . . . . ? Co Co P C21 2.3(2) 2_666 . . . ? C2 Co P C11 -67.83(15) . . . . ? C3 Co P C11 166.27(13) . . . . ? C1 Co P C11 50.43(15) . . . . ? Co Co P C11 -117.02(19) 2_666 . . . ? C2 Co C1 O1 -87(8) . . . . ? C3 Co C1 O1 78(8) . . . . ? P Co C1 O1 176(8) . . . . ? Co Co C1 O1 -6(8) 2_666 . . . ? C3 Co C2 O2 110(4) . . . . ? C1 Co C2 O2 -86(4) . . . . ? P Co C2 O2 18(4) . . . . ? Co Co C2 O2 -169(4) 2_666 . . . ? C2 Co C3 O3 -121(5) . . . . ? C1 Co C3 O3 74(5) . . . . ? P Co C3 O3 -31(5) . . . . ? Co Co C3 O3 159(5) 2_666 . . . ? C15 P C11 C18 64.6(2) . . . . ? C21 P C11 C18 174.97(19) . . . . ? Co P C11 C18 -62.0(2) . . . . ? C15 P C11 C12 -61.3(2) . . . . ? C21 P C11 C12 49.1(2) . . . . ? Co P C11 C12 172.14(16) . . . . ? C18 C11 C12 C13 -65.5(3) . . . . ? P C11 C12 C13 57.6(3) . . . . ? C11 C12 C13 C14 -43.8(4) . . . . ? C12 C13 C14 C15 43.7(4) . . . . ? C13 C14 C15 C16 64.9(3) . . . . ? C13 C14 C15 P -57.4(3) . . . . ? C21 P C15 C16 -171.21(18) . . . . ? C11 P C15 C16 -65.2(2) . . . . ? Co P C15 C16 61.5(2) . . . . ? C21 P C15 C14 -45.0(2) . . . . ? C11 P C15 C14 61.0(2) . . . . ? Co P C15 C14 -172.22(16) . . . . ? C14 C15 C16 C17 -63.3(3) . . . . ? P C15 C16 C17 60.8(3) . . . . ? C15 C16 C17 C18 -45.4(3) . . . . ? C16 C17 C18 C11 44.0(3) . . . . ? C12 C11 C18 C17 65.8(3) . . . . ? P C11 C18 C17 -58.7(3) . . . . ? C15 P C21 C22 -79.0(3) . . . . ? C11 P C21 C22 -179.3(2) . . . . ? Co P C21 C22 52.5(3) . . . . ? P C21 C22 C231 176.3(12) . . . . ? P C21 C22 C232 -168.0(6) . . . . ? C21 C22 C231 C241 -158.7(15) . . . . ? C232 C22 C231 C241 107(4) . . . . ? C22 C231 C241 C251 -54(3) . . . . ? C231 C22 C232 C242 -96(3) . . . . ? C21 C22 C232 C242 172.1(7) . . . . ? C22 C232 C242 C252 67.6(13) . . . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.348 _refine_diff_density_min -0.280 _refine_diff_density_rms 0.053 #========================================================================== # 4. TEXT _publ_section_abstract ; See text. ; _publ_section_comment ; See text. ; _publ_section_exptl_prep ; See text. ; _publ_section_exptl_refinement ; The intensity data were collected on a Bruker X8 ApexII 4K Kappa CCD diffractometer using an exposure time of 10 seconds/frame with a frame width of 0.50\%. The first 50 frames were recollected at the end of the data collection to check for decay,no decay was found. ; _publ_section_references ; Brandenburg, K. & Berndt, M. (1999). DIAMOND. Release 2.1c. Crystal Impact GbR, Bonn, Germany. Bruker (2005). Apex2 (Version 1.0-27). Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (2004). SAINT-Plus. Version 7.12 (including XPREP). Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (2004). SADABS (Version 2004/1). Bruker AXS Inc., Madison, Wisconsin, USA. Sheldrick, G.M. (1997a). SHELXS-97. Program for Crystal Structure Solution. University of G\"ottingen, Germany. Sheldrick, G.M. (1997b). SHELXL-97. Program for Crystal Structure Refinement. University of G\"ottingen, Germany. ; _publ_section_figure_captions ; See text. ; _publ_section_acknowledgements ; See text. ; #========================================================================== data_pcy2 _database_code_depnum_ccdc_archive 'CCDC 637088' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Hexacarbony-bis(9-cyclohexyl-9-phosphabicyclo[3.3.1]nonane)-dicobalt ; _chemical_name_common ;Hexacarbony-bis(9-cyclohexyl-9-phosphabicyclo(3.3.1)nonane)- dicobalt ; _chemical_formula_moiety 'C34 H50 Co2 O6 P2' _chemical_formula_sum 'C34 H50 Co2 O6 P2' _chemical_formula_weight 734.54 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.058(5) _cell_length_b 10.035(5) _cell_length_c 15.622(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 98.695(5) _cell_angle_gamma 90.000(5) _cell_volume 1713.6(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8058 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 28.29 _exptl_crystal_description Plate _exptl_crystal_colour Red _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'Not measured' _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method 'Not measured' _exptl_crystal_F_000 772 _exptl_absorpt_coefficient_mu 1.104 _exptl_absorpt_correction_type Multi-scans _exptl_absorpt_correction_T_min 0.726 _exptl_absorpt_correction_T_max 0.957 _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker X8 ApexII 4K Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number 'First 50 frames repeated after data collection.' __diffrn_standards_interval_count 'After collection' _diffrn_standards_interval_time 'After collection' _diffrn_standards_decay_% None _diffrn_reflns_number 19586 _diffrn_reflns_av_R_equivalents 0.0328 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 28.31 _reflns_number_total 4256 _reflns_number_gt 3760 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2004)' _computing_data_reduction 'SAINT-Plus and XPREP (Bruker, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'DIAMOND (Brandenburg & Berndt, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997b)' _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 'w=1/[\s^2^(Fo^2^)+(0.0336P)^2^+0.4850P] 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 4256 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0310 _refine_ls_R_factor_gt 0.0253 _refine_ls_wR_factor_ref 0.0655 _refine_ls_wR_factor_gt 0.0626 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.405688(16) 0.083136(17) 0.488854(11) 0.01314(6) Uani 1 d . . . P P 0.25829(3) 0.23084(3) 0.48432(2) 0.01306(8) Uani 1 d . . . O1 O 0.46108(10) 0.08494(10) 0.31102(6) 0.0211(2) Uani 1 d . . . O2 O 0.24776(11) -0.14038(11) 0.52114(8) 0.0316(3) Uani 1 d . . . O3 O 0.56841(9) 0.26318(11) 0.59921(7) 0.0253(2) Uani 1 d . . . C1 C 0.43695(12) 0.08494(13) 0.37992(9) 0.0164(3) Uani 1 d . . . C2 C 0.31049(13) -0.05244(14) 0.51139(9) 0.0203(3) Uani 1 d . . . C3 C 0.50465(13) 0.18843(14) 0.55901(9) 0.0179(3) Uani 1 d . . . C11 C 0.29774(13) 0.39984(13) 0.45141(9) 0.0182(3) Uani 1 d . . . H11 H 0.3693 0.4299 0.4915 0.022 Uiso 1 calc R . . C12 C 0.19312(15) 0.49913(15) 0.45687(10) 0.0249(3) Uani 1 d . . . H12A H 0.1815 0.5069 0.5170 0.030 Uiso 1 calc R . . H12B H 0.2179 0.5859 0.4384 0.030 Uiso 1 calc R . . C13 C 0.06993(15) 0.46300(17) 0.40274(10) 0.0292(4) Uani 1 d . . . H13A H 0.0078 0.5209 0.4202 0.035 Uiso 1 calc R . . H13B H 0.0748 0.4826 0.3426 0.035 Uiso 1 calc R . . C14 C 0.02696(13) 0.31855(17) 0.40840(10) 0.0256(3) Uani 1 d . . . H14A H -0.0418 0.3042 0.3629 0.031 Uiso 1 calc R . . H14B H -0.0025 0.3069 0.4633 0.031 Uiso 1 calc R . . C15 C 0.12354(13) 0.21025(15) 0.40064(9) 0.0195(3) Uani 1 d . . . H15 H 0.0867 0.1236 0.4098 0.023 Uiso 1 calc R . . C16 C 0.16774(14) 0.20649(16) 0.31173(9) 0.0234(3) Uani 1 d . . . H16A H 0.2182 0.1278 0.3097 0.028 Uiso 1 calc R . . H16B H 0.0967 0.1963 0.2675 0.028 Uiso 1 calc R . . C17 C 0.24089(14) 0.32806(16) 0.28823(9) 0.0255(3) Uani 1 d . . . H17A H 0.1830 0.3973 0.2666 0.031 Uiso 1 calc R . . H17B H 0.2836 0.3026 0.2409 0.031 Uiso 1 calc R . . C18 C 0.33529(14) 0.38925(14) 0.36018(10) 0.0221(3) Uani 1 d . . . H18A H 0.3550 0.4780 0.3420 0.027 Uiso 1 calc R . . H18B H 0.4095 0.3366 0.3649 0.027 Uiso 1 calc R . . C21 C 0.19540(12) 0.25038(13) 0.58719(8) 0.0156(3) Uani 1 d . . . H21 H 0.1352 0.3226 0.5782 0.019 Uiso 1 calc R . . C22 C 0.29229(13) 0.29212(15) 0.66333(9) 0.0192(3) Uani 1 d . . . H22A H 0.3540 0.2230 0.6746 0.023 Uiso 1 calc R . . H22B H 0.3322 0.3733 0.6486 0.023 Uiso 1 calc R . . C23 C 0.23325(14) 0.31538(15) 0.74465(9) 0.0224(3) Uani 1 d . . . H23A H 0.2960 0.3393 0.7925 0.027 Uiso 1 calc R . . H23B H 0.1760 0.3890 0.7346 0.027 Uiso 1 calc R . . C24 C 0.16623(15) 0.19132(15) 0.76835(9) 0.0248(3) Uani 1 d . . . H24A H 0.2244 0.1195 0.7829 0.030 Uiso 1 calc R . . H24B H 0.1273 0.2096 0.8187 0.030 Uiso 1 calc R . . C25 C 0.06987(15) 0.14882(16) 0.69319(10) 0.0269(3) Uani 1 d . . . H25A H 0.0075 0.2173 0.6823 0.032 Uiso 1 calc R . . H25B H 0.0309 0.0673 0.7083 0.032 Uiso 1 calc R . . C26 C 0.12735(14) 0.12593(15) 0.61100(10) 0.0225(3) Uani 1 d . . . H26A H 0.1840 0.0517 0.6201 0.027 Uiso 1 calc R . . H26B H 0.0637 0.1032 0.5635 0.027 Uiso 1 calc R . . 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 0.01551(10) 0.01220(10) 0.01215(9) -0.00049(6) 0.00350(7) 0.00359(7) P 0.01513(17) 0.01215(16) 0.01229(16) 0.00017(12) 0.00328(12) 0.00290(12) O1 0.0268(5) 0.0213(5) 0.0163(5) -0.0017(4) 0.0073(4) -0.0002(4) O2 0.0366(7) 0.0190(6) 0.0444(7) -0.0046(5) 0.0231(6) -0.0032(5) O3 0.0232(5) 0.0276(6) 0.0245(5) -0.0091(4) 0.0018(4) 0.0010(4) C1 0.0171(6) 0.0134(6) 0.0186(7) -0.0014(5) 0.0018(5) 0.0011(5) C2 0.0244(7) 0.0176(7) 0.0208(7) -0.0012(5) 0.0093(6) 0.0067(6) C3 0.0192(7) 0.0189(7) 0.0165(6) -0.0007(5) 0.0053(5) 0.0071(5) C11 0.0229(7) 0.0132(6) 0.0198(7) 0.0021(5) 0.0075(5) 0.0030(5) C12 0.0344(8) 0.0166(7) 0.0269(8) 0.0051(6) 0.0151(7) 0.0094(6) C13 0.0323(9) 0.0328(9) 0.0242(8) 0.0086(7) 0.0102(6) 0.0203(7) C14 0.0182(7) 0.0386(9) 0.0192(7) 0.0001(6) 0.0000(5) 0.0102(6) C15 0.0169(6) 0.0250(7) 0.0160(6) -0.0004(5) 0.0009(5) 0.0016(5) C16 0.0223(7) 0.0320(8) 0.0150(7) -0.0024(6) 0.0001(5) 0.0065(6) C17 0.0315(8) 0.0309(8) 0.0157(7) 0.0055(6) 0.0088(6) 0.0118(7) C18 0.0294(8) 0.0161(7) 0.0236(7) 0.0055(6) 0.0129(6) 0.0046(6) C21 0.0172(6) 0.0152(6) 0.0156(6) -0.0003(5) 0.0066(5) 0.0043(5) C22 0.0214(7) 0.0207(7) 0.0165(7) -0.0030(5) 0.0058(5) 0.0020(6) C23 0.0283(8) 0.0230(7) 0.0168(7) -0.0043(6) 0.0060(6) 0.0031(6) C24 0.0370(9) 0.0212(7) 0.0189(7) 0.0005(6) 0.0130(6) 0.0060(6) C25 0.0341(9) 0.0233(8) 0.0273(8) -0.0023(6) 0.0172(7) -0.0040(6) C26 0.0300(8) 0.0193(7) 0.0203(7) -0.0019(6) 0.0108(6) -0.0031(6) _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 C3 1.7755(15) . ? Co C1 1.7871(15) . ? Co C2 1.7875(16) . ? Co P 2.1963(8) . ? Co Co 2.6526(10) 3_656 ? P C15 1.8393(15) . ? P C11 1.8435(16) . ? P C21 1.8556(14) . ? O1 C1 1.1474(17) . ? O2 C2 1.1467(19) . ? O3 C3 1.1490(18) . ? C11 C12 1.539(2) . ? C11 C18 1.5472(19) . ? C11 H11 0.9800 . ? C12 C13 1.534(2) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.532(3) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.541(2) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.541(2) . ? C15 H15 0.9800 . ? C16 C17 1.539(2) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.541(2) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C21 C26 1.533(2) . ? C21 C22 1.534(2) . ? C21 H21 0.9800 . ? C22 C23 1.5314(19) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.523(2) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.522(2) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.534(2) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? 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 C3 Co C1 113.07(6) . . ? C3 Co C2 131.13(7) . . ? C1 Co C2 113.56(6) . . ? C3 Co P 90.20(5) . . ? C1 Co P 102.23(4) . . ? C2 Co P 93.66(6) . . ? C3 Co Co 83.93(5) . 3_656 ? C1 Co Co 82.53(4) . 3_656 ? C2 Co Co 88.29(6) . 3_656 ? P Co Co 173.581(15) . 3_656 ? C15 P C11 96.06(7) . . ? C15 P C21 104.95(7) . . ? C11 P C21 106.24(6) . . ? C15 P Co 117.69(5) . . ? C11 P Co 115.09(5) . . ? C21 P Co 114.64(5) . . ? O1 C1 Co 177.67(12) . . ? O2 C2 Co 176.32(13) . . ? O3 C3 Co 174.78(13) . . ? C12 C11 C18 113.83(12) . . ? C12 C11 P 111.63(10) . . ? C18 C11 P 107.54(9) . . ? C12 C11 H11 107.9 . . ? C18 C11 H11 107.9 . . ? P C11 H11 107.9 . . ? C13 C12 C11 115.39(13) . . ? C13 C12 H12A 108.4 . . ? C11 C12 H12A 108.4 . . ? C13 C12 H12B 108.4 . . ? C11 C12 H12B 108.4 . . ? H12A C12 H12B 107.5 . . ? C14 C13 C12 116.68(12) . . ? C14 C13 H13A 108.1 . . ? C12 C13 H13A 108.1 . . ? C14 C13 H13B 108.1 . . ? C12 C13 H13B 108.1 . . ? H13A C13 H13B 107.3 . . ? C13 C14 C15 115.97(13) . . ? C13 C14 H14A 108.3 . . ? C15 C14 H14A 108.3 . . ? C13 C14 H14B 108.3 . . ? C15 C14 H14B 108.3 . . ? H14A C14 H14B 107.4 . . ? C16 C15 C14 113.95(12) . . ? C16 C15 P 108.06(10) . . ? C14 C15 P 111.19(10) . . ? C16 C15 H15 107.8 . . ? C14 C15 H15 107.8 . . ? P C15 H15 107.8 . . ? C17 C16 C15 116.46(12) . . ? C17 C16 H16A 108.2 . . ? C15 C16 H16A 108.2 . . ? C17 C16 H16B 108.2 . . ? C15 C16 H16B 108.2 . . ? H16A C16 H16B 107.3 . . ? C16 C17 C18 117.67(12) . . ? C16 C17 H17A 107.9 . . ? C18 C17 H17A 107.9 . . ? C16 C17 H17B 107.9 . . ? C18 C17 H17B 107.9 . . ? H17A C17 H17B 107.2 . . ? C17 C18 C11 116.92(12) . . ? C17 C18 H18A 108.1 . . ? C11 C18 H18A 108.1 . . ? C17 C18 H18B 108.1 . . ? C11 C18 H18B 108.1 . . ? H18A C18 H18B 107.3 . . ? C26 C21 C22 110.20(11) . . ? C26 C21 P 112.71(9) . . ? C22 C21 P 113.03(9) . . ? C26 C21 H21 106.8 . . ? C22 C21 H21 106.8 . . ? P C21 H21 106.8 . . ? C23 C22 C21 110.46(12) . . ? C23 C22 H22A 109.6 . . ? C21 C22 H22A 109.6 . . ? C23 C22 H22B 109.6 . . ? C21 C22 H22B 109.6 . . ? H22A C22 H22B 108.1 . . ? C24 C23 C22 111.18(12) . . ? C24 C23 H23A 109.4 . . ? C22 C23 H23A 109.4 . . ? C24 C23 H23B 109.4 . . ? C22 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? C25 C24 C23 110.55(12) . . ? C25 C24 H24A 109.5 . . ? C23 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 108.1 . . ? C24 C25 C26 110.93(13) . . ? C24 C25 H25A 109.5 . . ? C26 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 108.0 . . ? C21 C26 C25 111.22(12) . . ? C21 C26 H26A 109.4 . . ? C25 C26 H26A 109.4 . . ? C21 C26 H26B 109.4 . . ? C25 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 0.444 _refine_diff_density_min -0.228 _refine_diff_density_rms 0.057