#------------------------------------------------------------------------------ #$Date: 2016-03-25 23:29:34 +0000 (Fri, 25 Mar 2016) $ #$Revision: 180103 $ #$URL: svn://www.crystallography.net/cod/cif/7/10/01/7100138.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7100138 loop_ _publ_author_name 'A. Carty' 'Todd Graham' 'Konstantin A. Udachin' _publ_section_title ; Reactivity of Electrophilic m2-Phosphinidene Complexes with Heterocumulenes: Formation of the First s-p-Aminophosphaimine Complexes [Mn2(CO)8{m-h1,h2-P(NiPr2)=NR}] and Diazoalkane Insertions into Metal-Phosphorus Bonds. ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/b505472a _journal_year 2005 _chemical_formula_sum 'C39 H42 Co2 N O4 P3' _chemical_formula_weight 799.51 _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _cell_angle_alpha 90.00 _cell_angle_beta 102.347(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 30.170(6) _cell_length_b 10.6655(19) _cell_length_c 23.493(4) _cell_measurement_temperature 125(2) _cell_volume 7385(2) _diffrn_ambient_temperature 125(2) _exptl_crystal_density_diffrn 1.438 _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 7100138 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.109009(9) 0.28979(2) 0.290132(11) 0.01930(7) Uani 1 1 d . . . Co2 Co 0.152107(8) 0.42996(2) 0.381818(10) 0.01760(6) Uani 1 1 d . . . P1 P 0.124814(16) 0.44036(5) 0.23274(2) 0.01809(10) Uani 1 1 d . . . P2 P 0.202337(16) 0.51068(5) 0.33718(2) 0.01714(10) Uani 1 1 d . . . P3 P 0.093242(17) 0.31652(5) 0.37354(2) 0.02010(10) Uani 1 1 d . . . O1 O 0.19735(5) 0.16889(15) 0.30423(7) 0.0361(4) Uani 1 1 d . . . O2 O 0.04980(6) 0.10350(16) 0.22196(8) 0.0454(4) Uani 1 1 d . . . O3 O 0.20487(6) 0.34855(18) 0.49401(7) 0.0407(4) Uani 1 1 d . . . O4 O 0.10308(5) 0.65895(15) 0.39366(7) 0.0327(3) Uani 1 1 d . . . N1 N 0.07507(6) 0.22425(17) 0.42121(7) 0.0274(4) Uani 1 1 d . . . C2A C 0.05230(7) 0.3701(2) 0.31501(9) 0.0231(4) Uani 1 1 d . . . H2A H 0.0502(7) 0.453(2) 0.3064(9) 0.023(6) Uiso 1 1 d . . . H2 H 0.0232(8) 0.325(2) 0.3038(10) 0.028(6) Uiso 1 1 d . . . C1 C 0.16291(7) 0.21815(19) 0.30052(8) 0.0257(4) Uani 1 1 d . . . C2 C 0.07361(8) 0.17548(19) 0.24813(9) 0.0283(4) Uani 1 1 d . . . C3 C 0.18518(7) 0.3743(2) 0.44804(9) 0.0259(4) Uani 1 1 d . . . C4 C 0.12198(7) 0.56931(19) 0.38575(8) 0.0223(4) Uani 1 1 d . . . C5 C 0.18308(6) 0.50226(19) 0.25692(8) 0.0200(4) Uani 1 1 d . . . H5B H 0.1844 0.5873 0.2405 0.024 Uiso 1 1 calc R . . H5A H 0.2042 0.4481 0.2411 0.024 Uiso 1 1 calc R . . C6 C 0.08953(6) 0.58026(18) 0.22054(8) 0.0204(4) Uani 1 1 d . . . C7 C 0.04769(7) 0.5748(2) 0.18134(10) 0.0308(5) Uani 1 1 d . . . H7 H 0.0382 0.4985 0.1615 0.037 Uiso 1 1 calc R . . C8 C 0.01995(8) 0.6790(2) 0.17100(11) 0.0364(5) Uani 1 1 d . . . H8 H -0.0081 0.6747 0.1435 0.044 Uiso 1 1 calc R . . C9 C 0.03300(7) 0.7899(2) 0.20069(10) 0.0316(5) Uani 1 1 d . . . H9 H 0.0140 0.8618 0.1934 0.038 Uiso 1 1 calc R . . C10 C 0.07374(7) 0.7955(2) 0.24090(9) 0.0277(4) Uani 1 1 d . . . H10 H 0.0824 0.8708 0.2619 0.033 Uiso 1 1 calc R . . C11 C 0.10204(7) 0.69152(18) 0.25066(8) 0.0234(4) Uani 1 1 d . . . H11 H 0.1301 0.6963 0.2781 0.028 Uiso 1 1 calc R . . C12 C 0.12882(6) 0.39326(19) 0.15870(8) 0.0218(4) Uani 1 1 d . . . C13 C 0.12931(8) 0.4796(2) 0.11448(9) 0.0307(5) Uani 1 1 d . . . H13 H 0.1243 0.5659 0.1208 0.037 Uiso 1 1 calc R . . C14 C 0.13711(8) 0.4405(2) 0.06114(9) 0.0363(5) Uani 1 1 d . . . H14 H 0.1377 0.5005 0.0314 0.044 Uiso 1 1 calc R . . C15 C 0.14400(8) 0.3160(2) 0.05084(9) 0.0361(5) Uani 1 1 d . . . H15 H 0.1488 0.2900 0.0140 0.043 Uiso 1 1 calc R . . C16 C 0.14386(8) 0.2291(2) 0.09413(9) 0.0353(5) Uani 1 1 d . . . H16 H 0.1490 0.1430 0.0874 0.042 Uiso 1 1 calc R . . C17 C 0.13620(7) 0.2676(2) 0.14777(9) 0.0286(4) Uani 1 1 d . . . H17 H 0.1360 0.2072 0.1774 0.034 Uiso 1 1 calc R . . C18 C 0.25945(6) 0.44272(18) 0.34593(8) 0.0188(4) Uani 1 1 d . . . C19 C 0.29002(7) 0.49185(19) 0.31507(9) 0.0243(4) Uani 1 1 d . . . H19 H 0.2819 0.5638 0.2913 0.029 Uiso 1 1 calc R . . C20 C 0.33220(7) 0.43712(19) 0.31858(9) 0.0269(4) Uani 1 1 d . . . H20 H 0.3526 0.4706 0.2968 0.032 Uiso 1 1 calc R . . C21 C 0.34453(7) 0.3337(2) 0.35388(9) 0.0270(4) Uani 1 1 d . . . H21 H 0.3734 0.2959 0.3564 0.032 Uiso 1 1 calc R . . C22 C 0.31483(8) 0.2856(2) 0.38544(10) 0.0343(5) Uani 1 1 d . . . H22 H 0.3235 0.2153 0.4101 0.041 Uiso 1 1 calc R . . C23 C 0.27224(7) 0.3396(2) 0.38136(9) 0.0288(5) Uani 1 1 d . . . H23 H 0.2519 0.3055 0.4030 0.035 Uiso 1 1 calc R . . C24 C 0.21601(6) 0.67515(18) 0.35519(8) 0.0199(4) Uani 1 1 d . . . C25 C 0.22510(7) 0.76597(19) 0.31657(9) 0.0258(4) Uani 1 1 d . . . H25 H 0.2241 0.7444 0.2771 0.031 Uiso 1 1 calc R . . C26 C 0.23569(7) 0.8881(2) 0.33560(10) 0.0295(5) Uani 1 1 d . . . H26 H 0.2415 0.9493 0.3088 0.035 Uiso 1 1 calc R . . C27 C 0.23780(7) 0.9216(2) 0.39276(10) 0.0305(5) Uani 1 1 d . . . H27 H 0.2453 1.0051 0.4053 0.037 Uiso 1 1 calc R . . C28 C 0.22891(8) 0.8326(2) 0.43169(10) 0.0314(5) Uani 1 1 d . . . H28 H 0.2303 0.8547 0.4712 0.038 Uiso 1 1 calc R . . C29 C 0.21798(7) 0.7109(2) 0.41295(9) 0.0261(4) Uani 1 1 d . . . H29 H 0.2117 0.6506 0.4399 0.031 Uiso 1 1 calc R . . C30 C 0.08905(8) 0.0889(2) 0.43002(10) 0.0357(5) Uani 1 1 d . . . C31 C 0.09564(10) 0.0538(3) 0.49453(11) 0.0525(8) Uani 1 1 d . . . H31B H 0.0992 -0.0383 0.4984 0.063 Uiso 1 1 calc R . . H31A H 0.1241 0.0927 0.5162 0.063 Uiso 1 1 calc R . . C32 C 0.05729(11) 0.0937(3) 0.52234(12) 0.0610(9) Uani 1 1 d . . . H32B H 0.0648 0.0731 0.5644 0.073 Uiso 1 1 calc R . . H32A H 0.0293 0.0481 0.5041 0.073 Uiso 1 1 calc R . . C33 C 0.04961(9) 0.2331(3) 0.51450(10) 0.0526(8) Uani 1 1 d . . . H33B H 0.0771 0.2777 0.5355 0.063 Uiso 1 1 calc R . . H33A H 0.0241 0.2577 0.5326 0.063 Uiso 1 1 calc R . . C34 C 0.03899(8) 0.2759(3) 0.45062(10) 0.0365(5) Uani 1 1 d . . . C35 C 0.13456(9) 0.0654(2) 0.41368(13) 0.0493(7) Uani 1 1 d . . . H35C H 0.1562 0.1306 0.4310 0.059 Uiso 1 1 calc R . . H35B H 0.1306 0.0674 0.3712 0.059 Uiso 1 1 calc R . . H35A H 0.1462 -0.0169 0.4283 0.059 Uiso 1 1 calc R . . C36 C 0.05383(9) 0.0025(2) 0.39205(12) 0.0453(6) Uani 1 1 d . . . H36C H 0.0454 0.0368 0.3525 0.054 Uiso 1 1 calc R . . H36B H 0.0268 -0.0031 0.4088 0.054 Uiso 1 1 calc R . . H36A H 0.0669 -0.0813 0.3906 0.054 Uiso 1 1 calc R . . C37 C -0.00916(8) 0.2364(3) 0.41988(11) 0.0464(7) Uani 1 1 d . . . H37C H -0.0122 0.1452 0.4225 0.056 Uiso 1 1 calc R . . H37B H -0.0147 0.2615 0.3788 0.056 Uiso 1 1 calc R . . H37A H -0.0313 0.2773 0.4387 0.056 Uiso 1 1 calc R . . C38 C 0.04042(9) 0.4194(3) 0.45148(11) 0.0434(6) Uani 1 1 d . . . H38C H 0.0292 0.4515 0.4119 0.052 Uiso 1 1 calc R . . H38B H 0.0717 0.4476 0.4659 0.052 Uiso 1 1 calc R . . H38A H 0.0213 0.4510 0.4772 0.052 Uiso 1 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 Co1 0.02279(13) 0.01691(13) 0.01800(12) 0.00057(9) 0.00389(9) 0.00106(10) Co2 0.01712(12) 0.01914(13) 0.01715(12) 0.00205(9) 0.00505(9) -0.00022(10) P1 0.0190(2) 0.0182(2) 0.0170(2) 0.00138(17) 0.00367(17) 0.00247(18) P2 0.0164(2) 0.0184(2) 0.0169(2) 0.00273(17) 0.00420(16) 0.00100(18) P3 0.0196(2) 0.0208(2) 0.0201(2) 0.00180(18) 0.00459(18) -0.00096(19) O1 0.0352(9) 0.0343(9) 0.0383(9) -0.0027(7) 0.0067(7) 0.0138(7) O2 0.0537(11) 0.0282(9) 0.0472(10) -0.0065(8) -0.0050(8) -0.0082(8) O3 0.0368(9) 0.0624(12) 0.0223(8) 0.0130(7) 0.0049(6) 0.0087(8) O4 0.0343(8) 0.0279(8) 0.0368(8) -0.0035(6) 0.0095(7) 0.0056(7) N1 0.0252(9) 0.0331(10) 0.0243(8) 0.0053(7) 0.0061(7) -0.0072(8) C2A 0.0201(9) 0.0230(10) 0.0255(10) 0.0011(8) 0.0033(7) 0.0023(8) C1 0.0341(11) 0.0217(10) 0.0208(9) 0.0013(7) 0.0049(8) 0.0032(9) C2 0.0364(12) 0.0203(10) 0.0267(10) 0.0015(8) 0.0036(9) 0.0031(9) C3 0.0233(10) 0.0321(11) 0.0240(10) 0.0041(8) 0.0092(8) 0.0007(8) C4 0.0224(9) 0.0249(10) 0.0199(9) -0.0008(7) 0.0052(7) -0.0024(8) C5 0.0182(9) 0.0254(10) 0.0166(8) 0.0026(7) 0.0042(7) 0.0001(7) C6 0.0204(9) 0.0193(9) 0.0222(9) 0.0053(7) 0.0064(7) 0.0024(7) C7 0.0250(10) 0.0264(11) 0.0374(12) 0.0009(9) -0.0011(9) 0.0021(9) C8 0.0227(11) 0.0376(13) 0.0452(13) 0.0057(10) -0.0014(9) 0.0067(9) C9 0.0295(11) 0.0273(11) 0.0394(12) 0.0091(9) 0.0104(9) 0.0105(9) C10 0.0317(11) 0.0215(10) 0.0317(11) 0.0021(8) 0.0108(9) 0.0045(9) C11 0.0235(10) 0.0233(10) 0.0241(10) 0.0022(7) 0.0064(7) 0.0026(8) C12 0.0208(9) 0.0270(10) 0.0163(8) 0.0003(7) 0.0014(7) 0.0020(8) C13 0.0355(12) 0.0295(11) 0.0276(11) 0.0033(8) 0.0077(9) -0.0011(9) C14 0.0402(13) 0.0470(15) 0.0223(10) 0.0073(9) 0.0075(9) -0.0010(11) C15 0.0358(12) 0.0541(16) 0.0190(10) -0.0051(9) 0.0067(9) -0.0001(11) C16 0.0430(13) 0.0379(13) 0.0246(11) -0.0069(9) 0.0065(9) 0.0056(11) C17 0.0346(11) 0.0312(11) 0.0196(9) -0.0003(8) 0.0046(8) 0.0065(9) C18 0.0172(8) 0.0208(9) 0.0179(8) 0.0000(7) 0.0027(7) 0.0009(7) C19 0.0240(10) 0.0194(10) 0.0309(10) 0.0039(8) 0.0091(8) 0.0011(8) C20 0.0225(10) 0.0247(10) 0.0364(11) -0.0011(8) 0.0125(8) -0.0016(8) C21 0.0217(10) 0.0343(12) 0.0249(10) -0.0027(8) 0.0044(8) 0.0086(9) C22 0.0327(11) 0.0405(13) 0.0315(11) 0.0153(10) 0.0110(9) 0.0169(10) C23 0.0278(10) 0.0346(12) 0.0268(10) 0.0129(9) 0.0119(8) 0.0101(9) C24 0.0152(8) 0.0189(9) 0.0252(9) 0.0021(7) 0.0037(7) 0.0016(7) C25 0.0290(10) 0.0236(10) 0.0284(10) 0.0030(8) 0.0144(8) 0.0034(8) C26 0.0309(11) 0.0194(10) 0.0419(12) 0.0064(9) 0.0161(9) 0.0036(9) C27 0.0279(11) 0.0213(10) 0.0412(12) -0.0013(9) 0.0045(9) -0.0019(9) C28 0.0359(12) 0.0272(11) 0.0272(11) -0.0011(8) -0.0019(9) -0.0017(9) C29 0.0271(10) 0.0257(10) 0.0229(9) 0.0038(8) 0.0000(8) -0.0032(8) C30 0.0376(12) 0.0313(12) 0.0348(12) 0.0120(9) 0.0000(9) -0.0103(10) C31 0.0577(17) 0.0516(17) 0.0399(14) 0.0240(12) -0.0079(12) -0.0240(14) C32 0.0605(18) 0.086(2) 0.0329(14) 0.0207(14) 0.0015(12) -0.0366(17) C33 0.0438(15) 0.089(2) 0.0275(12) 0.0053(13) 0.0128(11) -0.0212(15) C34 0.0269(11) 0.0566(16) 0.0282(11) 0.0002(10) 0.0110(9) -0.0108(11) C35 0.0476(15) 0.0310(13) 0.0698(19) 0.0225(13) 0.0134(13) 0.0087(12) C36 0.0513(15) 0.0346(14) 0.0455(14) 0.0055(11) 0.0003(12) -0.0133(12) C37 0.0253(12) 0.0709(19) 0.0430(14) 0.0027(13) 0.0074(10) -0.0100(12) C38 0.0411(14) 0.0557(17) 0.0394(13) -0.0104(12) 0.0224(11) -0.0022(12) 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 Co1 C1 1.766(2) . ? Co1 C2 1.775(2) . ? Co1 C2A 2.105(2) . ? Co1 P3 2.1321(6) . ? Co1 P1 2.2135(6) . ? Co1 Co2 2.7143(5) . ? Co2 C4 1.755(2) . ? Co2 C3 1.762(2) . ? Co2 P3 2.1232(6) . ? Co2 P2 2.1948(6) . ? P1 C6 1.8196(19) . ? P1 C12 1.8392(19) . ? P1 C5 1.8498(19) . ? P2 C24 1.831(2) . ? P2 C18 1.8400(19) . ? P2 C5 1.8525(18) . ? P3 N1 1.6691(17) . ? P3 C2A 1.737(2) . ? O1 C1 1.151(2) . ? O2 C2 1.138(3) . ? O3 C3 1.149(2) . ? O4 C4 1.148(2) . ? N1 C30 1.506(3) . ? N1 C34 1.512(3) . ? C6 C11 1.392(3) . ? C6 C7 1.396(3) . ? C7 C8 1.381(3) . ? C8 C9 1.387(3) . ? C9 C10 1.382(3) . ? C10 C11 1.389(3) . ? C12 C13 1.391(3) . ? C12 C17 1.391(3) . ? C13 C14 1.388(3) . ? C14 C15 1.373(4) . ? C15 C16 1.377(3) . ? C16 C17 1.391(3) . ? C18 C23 1.383(3) . ? C18 C19 1.392(3) . ? C19 C20 1.386(3) . ? C20 C21 1.382(3) . ? C21 C22 1.378(3) . ? C22 C23 1.392(3) . ? C24 C25 1.394(3) . ? C24 C29 1.398(3) . ? C25 C26 1.392(3) . ? C26 C27 1.378(3) . ? C27 C28 1.384(3) . ? C28 C29 1.387(3) . ? C30 C35 1.523(4) . ? C30 C31 1.532(3) . ? C30 C36 1.539(3) . ? C31 C32 1.507(5) . ? C32 C33 1.510(5) . ? C33 C34 1.535(3) . ? C34 C38 1.532(4) . ? C34 C37 1.536(3) . ?