# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2009 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Pascal LeFloch' _publ_contact_author_email PASCAL.LEFLOCH@POLYTECHNIQUE.EDU _publ_section_title ; Chromium (III)-bis(iminophosphoranyl)methanido Complexes Synthesis, X-ray Crystal Structures and Catalytic Ethylene Oligomerization ; loop_ _publ_author_name 'Pascal LeFloch' 'Audrey Auffrant' 'Antoine Buchard' 'Romaric Houdard' 'Christian Klemp' 'Xavier-Frederic LeGoff' ; L.Magna ; 'Nicolas Mezailles' 'Louis Ricard' 'Lucien Saussine' # Attachment 'B904619D.cif' #=============================================================================== data_nm2546 _database_code_depnum_ccdc_archive 'CCDC 651318' #compound 3a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety C62H70Cl4Cr2N4P4,6(CH2Cl2)? _chemical_formula_sum 'C68 H82 Cl16 Cr2 N4 P4' _chemical_formula_weight 1750.46 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' 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' Cr Cr 0.3209 0.6236 '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 12.779(1) _cell_length_b 12.956(1) _cell_length_c 13.700(1) _cell_angle_alpha 77.252(1) _cell_angle_beta 69.776(1) _cell_angle_gamma 69.642(1) _cell_volume 1982.4(3) _cell_formula_units_Z 1 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 8389 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 898 _exptl_absorpt_coefficient_mu 0.936 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8205 _exptl_absorpt_correction_T_max 0.9122 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29661 _diffrn_reflns_av_R_equivalents 0.0219 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 30.03 _reflns_number_total 11583 _reflns_number_gt 9507 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0491P)^2^+0.7747P] 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 SHELXL _refine_ls_extinction_coef 0.0006(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11583 _refine_ls_number_parameters 429 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.1001 _refine_ls_wR_factor_gt 0.0936 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 Cr1 Cr 0.463152(19) 0.101604(18) 0.588555(18) 0.01533(6) Uani 1 1 d . . . Cl1 Cl 0.65709(3) 0.04758(3) 0.59769(3) 0.02034(8) Uani 1 1 d . . . Cl2 Cl 0.53236(3) 0.08776(3) 0.40301(3) 0.01830(8) Uani 1 1 d . . . P1 P 0.30270(3) 0.30016(3) 0.54677(3) 0.01650(8) Uani 1 1 d . . . P2 P 0.24444(3) 0.13183(3) 0.73126(3) 0.01744(8) Uani 1 1 d . . . N1 N 0.42884(11) 0.26962(10) 0.56283(11) 0.0187(2) Uani 1 1 d . . . N2 N 0.37156(11) 0.10617(10) 0.74338(10) 0.0197(2) Uani 1 1 d . . . C1 C 0.27487(12) 0.17219(11) 0.59589(12) 0.0169(3) Uani 1 1 d . . . H1 H 0.2762 0.1259 0.5503 0.020 Uiso 1 1 calc R . . C2 C 0.19750(13) 0.41856(11) 0.61133(12) 0.0196(3) Uani 1 1 d . . . C3 C 0.22352(14) 0.46746(13) 0.67700(14) 0.0260(3) Uani 1 1 d . . . H3 H 0.2982 0.4393 0.6882 0.031 Uiso 1 1 calc R . . C4 C 0.14046(16) 0.55781(14) 0.72659(16) 0.0320(4) Uani 1 1 d . . . H4 H 0.1591 0.5919 0.7704 0.038 Uiso 1 1 calc R . . C5 C 0.03096(16) 0.59766(14) 0.71194(15) 0.0320(4) Uani 1 1 d . . . H5 H -0.0256 0.6591 0.7458 0.038 Uiso 1 1 calc R . . C6 C 0.00374(15) 0.54842(15) 0.64844(16) 0.0326(4) Uani 1 1 d . . . H6 H -0.0720 0.5755 0.6394 0.039 Uiso 1 1 calc R . . C7 C 0.08621(14) 0.45944(14) 0.59754(15) 0.0275(3) Uani 1 1 d . . . H7 H 0.0670 0.4263 0.5533 0.033 Uiso 1 1 calc R . . C8 C 0.29498(12) 0.33984(12) 0.41321(12) 0.0195(3) Uani 1 1 d . . . C9 C 0.29761(13) 0.26691(13) 0.35082(13) 0.0226(3) Uani 1 1 d . . . H9 H 0.2974 0.1932 0.3794 0.027 Uiso 1 1 calc R . . C10 C 0.30057(15) 0.30214(14) 0.24649(14) 0.0281(3) Uani 1 1 d . . . H10 H 0.3010 0.2526 0.2045 0.034 Uiso 1 1 calc R . . C11 C 0.30290(15) 0.40927(15) 0.20335(14) 0.0312(4) Uani 1 1 d . . . H11 H 0.3060 0.4324 0.1319 0.037 Uiso 1 1 calc R . . C12 C 0.30072(16) 0.48232(15) 0.26478(15) 0.0312(4) Uani 1 1 d . . . H12 H 0.3027 0.5555 0.2354 0.037 Uiso 1 1 calc R . . C13 C 0.29560(14) 0.44829(13) 0.36914(14) 0.0253(3) Uani 1 1 d . . . H13 H 0.2925 0.4990 0.4114 0.030 Uiso 1 1 calc R . . C14 C 0.50117(14) 0.34524(13) 0.53175(15) 0.0263(3) Uani 1 1 d . . . H14 H 0.4496 0.4225 0.5212 0.032 Uiso 1 1 calc R . . C15 C 0.55230(17) 0.33970(15) 0.61862(19) 0.0382(5) Uani 1 1 d . . . H15A H 0.4889 0.3588 0.6831 0.057 Uiso 1 1 calc R . . H15B H 0.5979 0.3923 0.5981 0.057 Uiso 1 1 calc R . . H15C H 0.6031 0.2645 0.6306 0.057 Uiso 1 1 calc R . . C16 C 0.59632(17) 0.31978(16) 0.42915(18) 0.0393(5) Uani 1 1 d . . . H16A H 0.6478 0.2441 0.4375 0.059 Uiso 1 1 calc R . . H16B H 0.6419 0.3723 0.4095 0.059 Uiso 1 1 calc R . . H16C H 0.5607 0.3265 0.3743 0.059 Uiso 1 1 calc R . . C17 C 0.13149(14) 0.23097(12) 0.81638(13) 0.0228(3) Uani 1 1 d . . . C18 C 0.15752(17) 0.28194(15) 0.88025(16) 0.0343(4) Uani 1 1 d . . . H18 H 0.2363 0.2671 0.8786 0.041 Uiso 1 1 calc R . . C19 C 0.0679(2) 0.35503(17) 0.94702(18) 0.0462(5) Uani 1 1 d . . . H19 H 0.0853 0.3878 0.9928 0.055 Uiso 1 1 calc R . . C20 C -0.0460(2) 0.37962(15) 0.94655(18) 0.0455(6) Uani 1 1 d . . . H20 H -0.1067 0.4307 0.9909 0.055 Uiso 1 1 calc R . . C21 C -0.07206(17) 0.33084(16) 0.88262(17) 0.0417(5) Uani 1 1 d . . . H21 H -0.1506 0.3486 0.8824 0.050 Uiso 1 1 calc R . . C22 C 0.01576(15) 0.25552(15) 0.81795(15) 0.0315(4) Uani 1 1 d . . . H22 H -0.0031 0.2207 0.7748 0.038 Uiso 1 1 calc R . . C23 C 0.18319(13) 0.01703(12) 0.76596(13) 0.0204(3) Uani 1 1 d . . . C24 C 0.14423(16) -0.01793(14) 0.87284(14) 0.0286(3) Uani 1 1 d . . . H24 H 0.1470 0.0207 0.9229 0.034 Uiso 1 1 calc R . . C25 C 0.10149(17) -0.10869(15) 0.90635(15) 0.0327(4) Uani 1 1 d . . . H25 H 0.0761 -0.1326 0.9790 0.039 Uiso 1 1 calc R . . C26 C 0.09588(15) -0.16412(14) 0.83400(15) 0.0300(4) Uani 1 1 d . . . H26 H 0.0657 -0.2257 0.8569 0.036 Uiso 1 1 calc R . . C27 C 0.13413(15) -0.13019(14) 0.72827(15) 0.0293(4) Uani 1 1 d . . . H27 H 0.1303 -0.1688 0.6788 0.035 Uiso 1 1 calc R . . C28 C 0.17836(14) -0.03985(13) 0.69357(13) 0.0241(3) Uani 1 1 d . . . H28 H 0.2050 -0.0173 0.6207 0.029 Uiso 1 1 calc R . . C29 C 0.40225(15) 0.06039(15) 0.84185(13) 0.0270(3) Uani 1 1 d . . . H29 H 0.3281 0.0712 0.9009 0.032 Uiso 1 1 calc R . . C30 C 0.46541(18) -0.06311(16) 0.84373(15) 0.0371(4) Uani 1 1 d . . . H30A H 0.4163 -0.1015 0.8343 0.056 Uiso 1 1 calc R . . H30B H 0.4816 -0.0918 0.9111 0.056 Uiso 1 1 calc R . . H30C H 0.5391 -0.0757 0.7870 0.056 Uiso 1 1 calc R . . C31 C 0.47482(18) 0.12346(19) 0.85794(17) 0.0392(4) Uani 1 1 d . . . H31A H 0.5464 0.1170 0.7991 0.059 Uiso 1 1 calc R . . H31B H 0.4952 0.0921 0.9233 0.059 Uiso 1 1 calc R . . H31C H 0.4295 0.2017 0.8618 0.059 Uiso 1 1 calc R . . C32 C -0.09631(18) 0.19487(18) 0.50907(18) 0.0404(4) Uani 1 1 d . . . H32A H -0.1251 0.2524 0.4557 0.048 Uiso 1 1 calc R . . H32B H -0.1418 0.1413 0.5296 0.048 Uiso 1 1 calc R . . Cl3 Cl 0.05268(5) 0.12547(5) 0.45432(5) 0.04810(14) Uani 1 1 d . . . Cl4 Cl -0.11850(7) 0.25669(7) 0.61846(6) 0.0693(2) Uani 1 1 d . . . C33 C -0.18797(19) 0.0087(2) 0.79594(18) 0.0450(5) Uani 1 1 d . . . H33A H -0.1052 -0.0016 0.7542 0.054 Uiso 1 1 calc R . . H33B H -0.2359 0.0338 0.7469 0.054 Uiso 1 1 calc R . . Cl5 Cl -0.20477(6) -0.11885(6) 0.86822(6) 0.05856(16) Uani 1 1 d . . . Cl6 Cl -0.23113(6) 0.10982(6) 0.88007(5) 0.05762(16) Uani 1 1 d . . . C34 C -0.3872(2) 0.3470(2) 1.1330(2) 0.0555(6) Uani 1 1 d . . . H34A H -0.3201 0.2844 1.1457 0.067 Uiso 1 1 calc R . . H34B H -0.4584 0.3387 1.1892 0.067 Uiso 1 1 calc R . . Cl7 Cl -0.40174(6) 0.34246(6) 1.01230(5) 0.06065(17) Uani 1 1 d . . . Cl8 Cl -0.36535(7) 0.47245(7) 1.13746(7) 0.0736(2) Uani 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 Cr1 0.01437(11) 0.01418(10) 0.01665(12) -0.00217(8) -0.00474(8) -0.00286(8) Cl1 0.01663(15) 0.02111(16) 0.02387(18) -0.00344(13) -0.00832(13) -0.00342(12) Cl2 0.01951(15) 0.01615(15) 0.01796(16) -0.00206(12) -0.00484(12) -0.00437(12) P1 0.01555(16) 0.01395(16) 0.02001(18) -0.00196(13) -0.00624(14) -0.00337(12) P2 0.01658(16) 0.01710(16) 0.01761(18) -0.00290(13) -0.00381(13) -0.00442(13) N1 0.0175(5) 0.0141(5) 0.0258(7) -0.0024(5) -0.0079(5) -0.0047(4) N2 0.0182(6) 0.0231(6) 0.0171(6) -0.0040(5) -0.0049(5) -0.0048(5) C1 0.0164(6) 0.0156(6) 0.0188(7) -0.0025(5) -0.0050(5) -0.0045(5) C2 0.0189(6) 0.0154(6) 0.0227(7) -0.0017(5) -0.0058(6) -0.0036(5) C3 0.0236(7) 0.0232(7) 0.0322(9) -0.0078(6) -0.0091(6) -0.0043(6) C4 0.0339(9) 0.0250(8) 0.0373(10) -0.0139(7) -0.0088(8) -0.0044(7) C5 0.0299(8) 0.0217(7) 0.0336(10) -0.0071(7) -0.0025(7) 0.0008(6) C6 0.0216(7) 0.0329(9) 0.0362(10) -0.0073(7) -0.0075(7) 0.0016(6) C7 0.0208(7) 0.0282(8) 0.0324(9) -0.0072(7) -0.0090(6) -0.0024(6) C8 0.0167(6) 0.0193(6) 0.0215(7) -0.0016(5) -0.0062(5) -0.0039(5) C9 0.0210(7) 0.0197(7) 0.0262(8) -0.0039(6) -0.0101(6) -0.0010(5) C10 0.0257(8) 0.0300(8) 0.0262(8) -0.0081(6) -0.0112(7) 0.0012(6) C11 0.0284(8) 0.0357(9) 0.0224(8) 0.0011(7) -0.0089(7) -0.0023(7) C12 0.0346(9) 0.0276(8) 0.0286(9) 0.0061(7) -0.0101(7) -0.0106(7) C13 0.0284(8) 0.0229(7) 0.0270(8) 0.0021(6) -0.0106(6) -0.0108(6) C14 0.0204(7) 0.0189(7) 0.0418(10) -0.0035(6) -0.0095(7) -0.0081(6) C15 0.0349(9) 0.0281(8) 0.0647(14) -0.0105(9) -0.0277(10) -0.0091(7) C16 0.0289(9) 0.0316(9) 0.0505(13) -0.0011(8) 0.0009(8) -0.0155(7) C17 0.0235(7) 0.0184(6) 0.0203(7) -0.0022(5) -0.0012(6) -0.0039(5) C18 0.0364(9) 0.0292(8) 0.0362(10) -0.0133(7) -0.0047(8) -0.0085(7) C19 0.0605(14) 0.0321(10) 0.0390(12) -0.0177(8) -0.0013(10) -0.0102(9) C20 0.0475(12) 0.0233(8) 0.0387(11) -0.0065(8) 0.0121(9) -0.0008(8) C21 0.0267(9) 0.0325(9) 0.0417(12) 0.0009(8) 0.0036(8) 0.0036(7) C22 0.0243(8) 0.0311(8) 0.0297(9) -0.0020(7) -0.0044(7) -0.0014(6) C23 0.0187(6) 0.0187(6) 0.0220(7) -0.0017(5) -0.0045(6) -0.0052(5) C24 0.0371(9) 0.0266(8) 0.0219(8) -0.0006(6) -0.0062(7) -0.0129(7) C25 0.0376(9) 0.0287(8) 0.0254(9) 0.0029(7) -0.0013(7) -0.0135(7) C26 0.0274(8) 0.0237(7) 0.0358(10) 0.0000(7) -0.0041(7) -0.0113(6) C27 0.0292(8) 0.0287(8) 0.0333(9) -0.0058(7) -0.0065(7) -0.0140(7) C28 0.0250(7) 0.0262(7) 0.0225(8) -0.0023(6) -0.0054(6) -0.0112(6) C29 0.0253(7) 0.0363(9) 0.0189(7) -0.0041(6) -0.0089(6) -0.0057(6) C30 0.0411(10) 0.0361(9) 0.0258(9) 0.0023(7) -0.0146(8) -0.0004(8) C31 0.0344(9) 0.0595(13) 0.0314(10) -0.0146(9) -0.0137(8) -0.0135(9) C32 0.0379(10) 0.0461(11) 0.0400(11) -0.0063(9) -0.0149(9) -0.0114(9) Cl3 0.0366(2) 0.0503(3) 0.0557(3) -0.0114(2) -0.0104(2) -0.0107(2) Cl4 0.0684(4) 0.0837(5) 0.0560(4) -0.0319(4) -0.0286(3) 0.0022(4) C33 0.0385(10) 0.0600(13) 0.0346(11) -0.0105(10) -0.0126(9) -0.0073(10) Cl5 0.0538(3) 0.0619(4) 0.0639(4) -0.0129(3) -0.0135(3) -0.0220(3) Cl6 0.0667(4) 0.0670(4) 0.0481(3) -0.0158(3) -0.0163(3) -0.0255(3) C34 0.0364(11) 0.0657(16) 0.0560(16) -0.0037(12) -0.0159(11) -0.0047(11) Cl7 0.0627(4) 0.0667(4) 0.0492(4) -0.0171(3) -0.0046(3) -0.0206(3) Cl8 0.0667(4) 0.0914(5) 0.0737(5) -0.0279(4) -0.0252(4) -0.0210(4) _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 Cr1 N1 2.0393(12) . ? Cr1 N2 2.0405(13) . ? Cr1 C1 2.2311(14) . ? Cr1 Cl1 2.3699(5) . ? Cr1 Cl2 2.4109(5) . ? Cr1 Cl2 2.4120(4) 2_656 ? Cr1 P2 2.7542(5) . ? Cr1 P1 2.7643(4) . ? Cl2 Cr1 2.4120(4) 2_656 ? P1 N1 1.6020(13) . ? P1 C1 1.7552(14) . ? P1 C2 1.8123(15) . ? P1 C8 1.8156(16) . ? P2 N2 1.6010(13) . ? P2 C1 1.7547(15) . ? P2 C23 1.8142(15) . ? P2 C17 1.8167(16) . ? N1 C14 1.4730(19) . ? N2 C29 1.475(2) . ? C1 H1 0.9500 . ? C2 C3 1.388(2) . ? C2 C7 1.399(2) . ? C3 C4 1.395(2) . ? C3 H3 0.9500 . ? C4 C5 1.382(3) . ? C4 H4 0.9500 . ? C5 C6 1.376(3) . ? C5 H5 0.9500 . ? C6 C7 1.388(2) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.393(2) . ? C8 C13 1.403(2) . ? C9 C10 1.393(2) . ? C9 H9 0.9500 . ? C10 C11 1.390(3) . ? C10 H10 0.9500 . ? C11 C12 1.386(3) . ? C11 H11 0.9500 . ? C12 C13 1.386(2) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C16 1.519(3) . ? C14 C15 1.522(3) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.386(3) . ? C17 C22 1.394(2) . ? C18 C19 1.396(3) . ? C18 H18 0.9500 . ? C19 C20 1.380(4) . ? C19 H19 0.9500 . ? C20 C21 1.367(4) . ? C20 H20 0.9500 . ? C21 C22 1.389(3) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C28 1.388(2) . ? C23 C24 1.399(2) . ? C24 C25 1.388(2) . ? C24 H24 0.9500 . ? C25 C26 1.379(3) . ? C25 H25 0.9500 . ? C26 C27 1.382(3) . ? C26 H26 0.9500 . ? C27 C28 1.394(2) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.520(3) . ? C29 C31 1.525(3) . ? C29 H29 1.0000 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 Cl4 1.745(2) . ? C32 Cl3 1.765(2) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 Cl6 1.753(2) . ? C33 Cl5 1.771(3) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 Cl7 1.742(3) . ? C34 Cl8 1.759(3) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? 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 N1 Cr1 N2 92.28(5) . . ? N1 Cr1 C1 73.35(5) . . ? N2 Cr1 C1 73.59(5) . . ? N1 Cr1 Cl1 100.46(4) . . ? N2 Cr1 Cl1 100.73(4) . . ? C1 Cr1 Cl1 171.13(4) . . ? N1 Cr1 Cl2 91.33(4) . . ? N2 Cr1 Cl2 166.66(4) . . ? C1 Cr1 Cl2 95.20(4) . . ? Cl1 Cr1 Cl2 91.232(15) . . ? N1 Cr1 Cl2 165.72(4) . 2_656 ? N2 Cr1 Cl2 91.38(4) . 2_656 ? C1 Cr1 Cl2 94.52(4) . 2_656 ? Cl1 Cr1 Cl2 92.402(14) . 2_656 ? Cl2 Cr1 Cl2 82.142(14) . 2_656 ? N1 Cr1 P2 88.31(4) . . ? N2 Cr1 P2 35.19(4) . . ? C1 Cr1 P2 39.49(4) . . ? Cl1 Cr1 P2 135.742(16) . . ? Cl2 Cr1 P2 132.199(15) . . ? Cl2 Cr1 P2 86.749(13) 2_656 . ? N1 Cr1 P1 35.02(4) . . ? N2 Cr1 P1 88.24(4) . . ? C1 Cr1 P1 39.35(4) . . ? Cl1 Cr1 P1 135.296(15) . . ? Cl2 Cr1 P1 87.366(13) . . ? Cl2 Cr1 P1 131.428(15) 2_656 . ? P2 Cr1 P1 66.252(12) . . ? Cr1 Cl2 Cr1 97.858(14) . 2_656 ? N1 P1 C1 99.03(7) . . ? N1 P1 C2 113.26(7) . . ? C1 P1 C2 116.14(7) . . ? N1 P1 C8 116.67(7) . . ? C1 P1 C8 110.34(7) . . ? C2 P1 C8 102.09(7) . . ? N1 P1 Cr1 46.92(4) . . ? C1 P1 Cr1 53.70(5) . . ? C2 P1 Cr1 140.15(5) . . ? C8 P1 Cr1 117.66(5) . . ? N2 P2 C1 99.50(7) . . ? N2 P2 C23 116.93(7) . . ? C1 P2 C23 109.79(7) . . ? N2 P2 C17 113.33(8) . . ? C1 P2 C17 117.05(7) . . ? C23 P2 C17 101.02(7) . . ? N2 P2 Cr1 47.26(5) . . ? C1 P2 Cr1 53.96(5) . . ? C23 P2 Cr1 117.21(5) . . ? C17 P2 Cr1 141.65(5) . . ? C14 N1 P1 124.86(10) . . ? C14 N1 Cr1 134.33(10) . . ? P1 N1 Cr1 98.06(6) . . ? C29 N2 P2 124.48(11) . . ? C29 N2 Cr1 134.20(10) . . ? P2 N2 Cr1 97.55(7) . . ? P2 C1 P1 118.46(9) . . ? P2 C1 Cr1 86.55(6) . . ? P1 C1 Cr1 86.95(6) . . ? P2 C1 H1 120.8 . . ? P1 C1 H1 120.8 . . ? Cr1 C1 H1 96.4 . . ? C3 C2 C7 119.12(14) . . ? C3 C2 P1 121.48(12) . . ? C7 C2 P1 119.36(13) . . ? C2 C3 C4 120.30(16) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 119.96(17) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C6 C5 C4 120.11(16) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C7 120.43(17) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C6 C7 C2 120.06(17) . . ? C6 C7 H7 120.0 . . ? C2 C7 H7 120.0 . . ? C9 C8 C13 118.95(15) . . ? C9 C8 P1 123.78(12) . . ? C13 C8 P1 117.07(12) . . ? C8 C9 C10 119.97(15) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C11 C10 C9 120.51(17) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C12 C11 C10 119.91(17) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C13 C12 C11 119.79(16) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C8 120.85(16) . . ? C12 C13 H13 119.6 . . ? C8 C13 H13 119.6 . . ? N1 C14 C16 111.13(14) . . ? N1 C14 C15 110.22(15) . . ? C16 C14 C15 111.36(16) . . ? N1 C14 H14 108.0 . . ? C16 C14 H14 108.0 . . ? C15 C14 H14 108.0 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C22 119.33(16) . . ? C18 C17 P2 121.63(13) . . ? C22 C17 P2 119.03(14) . . ? C17 C18 C19 119.9(2) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C20 C19 C18 120.0(2) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C21 C20 C19 120.32(18) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 120.4(2) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C21 C22 C17 120.0(2) . . ? C21 C22 H22 120.0 . . ? C17 C22 H22 120.0 . . ? C28 C23 C24 119.28(14) . . ? C28 C23 P2 124.10(12) . . ? C24 C23 P2 116.54(13) . . ? C25 C24 C23 120.48(17) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C26 C25 C24 119.91(17) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C27 120.03(16) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C26 C27 C28 120.61(17) . . ? C26 C27 H27 119.7 . . ? C28 C27 H27 119.7 . . ? C23 C28 C27 119.68(16) . . ? C23 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? N2 C29 C30 111.34(14) . . ? N2 C29 C31 110.11(15) . . ? C30 C29 C31 111.35(16) . . ? N2 C29 H29 108.0 . . ? C30 C29 H29 108.0 . . ? C31 C29 H29 108.0 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Cl4 C32 Cl3 111.62(12) . . ? Cl4 C32 H32A 109.3 . . ? Cl3 C32 H32A 109.3 . . ? Cl4 C32 H32B 109.3 . . ? Cl3 C32 H32B 109.3 . . ? H32A C32 H32B 108.0 . . ? Cl6 C33 Cl5 110.64(13) . . ? Cl6 C33 H33A 109.5 . . ? Cl5 C33 H33A 109.5 . . ? Cl6 C33 H33B 109.5 . . ? Cl5 C33 H33B 109.5 . . ? H33A C33 H33B 108.1 . . ? Cl7 C34 Cl8 111.39(15) . . ? Cl7 C34 H34A 109.4 . . ? Cl8 C34 H34A 109.4 . . ? Cl7 C34 H34B 109.4 . . ? Cl8 C34 H34B 109.4 . . ? H34A C34 H34B 108.0 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.895 _refine_diff_density_min -0.783 _refine_diff_density_rms 0.064 #===END data_ckl-89-1 _database_code_depnum_ccdc_archive 'CCDC 651319' #compound 3b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H78 Cl4 Cr2 N4 P4, 2(C4 H8 O)' _chemical_formula_sum 'C74 H94 Cl4 Cr2 N4 O2 P4' _chemical_formula_weight 1441.21 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 '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' O O 0.0106 0.0060 '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 ' 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 11.078(1) _cell_length_b 22.191(1) _cell_length_c 14.487(1) _cell_angle_alpha 90.00 _cell_angle_beta 97.136(1) _cell_angle_gamma 90.00 _cell_volume 3533.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 7336 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description Block _exptl_crystal_colour 'Dark Blue' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.354 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1516 _exptl_absorpt_coefficient_mu 0.598 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8600 _exptl_absorpt_correction_T_max 0.9317 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25183 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0454 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 27.46 _reflns_number_total 8075 _reflns_number_gt 6023 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0741P)^2^+1.4343P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8075 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0670 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1337 _refine_ls_wR_factor_gt 0.1206 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 Cl1 Cl 0.63935(5) 0.48777(3) 0.51417(4) 0.02772(15) Uani 1 1 d . . . Cl2 Cl 0.50041(5) 0.49514(3) 0.71295(4) 0.02629(14) Uani 1 1 d . . . Cr1 Cr 0.52201(3) 0.562321(17) 0.58647(3) 0.02458(12) Uani 1 1 d . . . N1 N 0.68299(17) 0.60778(9) 0.63710(14) 0.0269(4) Uani 1 1 d . . . N2 N 0.40218(17) 0.63066(9) 0.61171(14) 0.0257(4) Uani 1 1 d . . . P1 P 0.70146(5) 0.63946(3) 0.54035(5) 0.02596(15) Uani 1 1 d . . . P2 P 0.43002(5) 0.67398(3) 0.52835(4) 0.02473(15) Uani 1 1 d . . . C1 C 0.5508(2) 0.63395(11) 0.48807(18) 0.0258(5) Uani 1 1 d . . . H1 H 0.538(3) 0.6238(12) 0.433(2) 0.031 Uiso 1 1 d . . . C2 C 0.7943(2) 0.60565(11) 0.45829(18) 0.0288(5) Uani 1 1 d . . . C3 C 0.9165(3) 0.59255(19) 0.4853(2) 0.0598(10) Uani 1 1 d . . . H3 H 0.9502 0.5984 0.5482 0.072 Uiso 1 1 calc R . . C4 C 0.9892(3) 0.5712(2) 0.4216(2) 0.0645(11) Uani 1 1 d . . . H4 H 1.0721 0.5621 0.4414 0.077 Uiso 1 1 calc R . . C5 C 0.9430(3) 0.56310(13) 0.3305(2) 0.0410(7) Uani 1 1 d . . . H5 H 0.9942 0.5496 0.2867 0.049 Uiso 1 1 calc R . . C6 C 0.8235(2) 0.57448(12) 0.30308(19) 0.0331(6) Uani 1 1 d . . . H6 H 0.7903 0.5677 0.2403 0.040 Uiso 1 1 calc R . . C7 C 0.7494(2) 0.59602(12) 0.36678(19) 0.0342(6) Uani 1 1 d . . . H7 H 0.6662 0.6042 0.3465 0.041 Uiso 1 1 calc R . . C8 C 0.7679(2) 0.71440(12) 0.55363(19) 0.0308(6) Uani 1 1 d . . . C9 C 0.8340(3) 0.73927(13) 0.4872(2) 0.0411(7) Uani 1 1 d . . . H9 H 0.8454 0.7170 0.4329 0.049 Uiso 1 1 calc R . . C10 C 0.8834(3) 0.79669(14) 0.5005(3) 0.0490(8) Uani 1 1 d . . . H10 H 0.9271 0.8139 0.4545 0.059 Uiso 1 1 calc R . . C11 C 0.8696(3) 0.82870(14) 0.5796(3) 0.0492(8) Uani 1 1 d . . . H11 H 0.9060 0.8673 0.5890 0.059 Uiso 1 1 calc R . . C12 C 0.8031(3) 0.80500(14) 0.6455(2) 0.0453(7) Uani 1 1 d . . . H12 H 0.7925 0.8275 0.6996 0.054 Uiso 1 1 calc R . . C13 C 0.7518(2) 0.74801(12) 0.6323(2) 0.0359(6) Uani 1 1 d . . . H13 H 0.7054 0.7319 0.6773 0.043 Uiso 1 1 calc R . . C14 C 0.7703(2) 0.59568(12) 0.72244(18) 0.0307(5) Uani 1 1 d . . . C15 C 0.7039(2) 0.60846(13) 0.80684(18) 0.0350(6) Uani 1 1 d . . . H15A H 0.6799 0.6510 0.8067 0.052 Uiso 1 1 calc R . . H15B H 0.7580 0.5995 0.8640 0.052 Uiso 1 1 calc R . . H15C H 0.6311 0.5830 0.8039 0.052 Uiso 1 1 calc R . . C16 C 0.8107(3) 0.52974(13) 0.7217(2) 0.0409(7) Uani 1 1 d . . . H16A H 0.7392 0.5035 0.7189 0.061 Uiso 1 1 calc R . . H16B H 0.8658 0.5211 0.7784 0.061 Uiso 1 1 calc R . . H16C H 0.8530 0.5225 0.6672 0.061 Uiso 1 1 calc R . . C17 C 0.8855(2) 0.63490(14) 0.7326(2) 0.0385(6) Uani 1 1 d . . . H17A H 0.9240 0.6326 0.6753 0.058 Uiso 1 1 calc R . . H17B H 0.9424 0.6203 0.7850 0.058 Uiso 1 1 calc R . . H17C H 0.8636 0.6768 0.7438 0.058 Uiso 1 1 calc R . . C18 C 0.4679(2) 0.75182(11) 0.55978(18) 0.0285(5) Uani 1 1 d . . . C19 C 0.5033(2) 0.79029(12) 0.4914(2) 0.0341(6) Uani 1 1 d . . . H19 H 0.5067 0.7756 0.4302 0.041 Uiso 1 1 calc R . . C20 C 0.5333(3) 0.84960(13) 0.5125(2) 0.0401(7) Uani 1 1 d . . . H20 H 0.5577 0.8754 0.4660 0.048 Uiso 1 1 calc R . . C21 C 0.5277(2) 0.87138(13) 0.6014(2) 0.0420(7) Uani 1 1 d . . . H21 H 0.5473 0.9123 0.6155 0.050 Uiso 1 1 calc R . . C22 C 0.4938(2) 0.83393(13) 0.6695(2) 0.0406(7) Uani 1 1 d . . . H22 H 0.4899 0.8491 0.7305 0.049 Uiso 1 1 calc R . . C23 C 0.4654(2) 0.77410(13) 0.6492(2) 0.0348(6) Uani 1 1 d . . . H23 H 0.4439 0.7482 0.6967 0.042 Uiso 1 1 calc R . . C24 C 0.3123(2) 0.68297(11) 0.42919(17) 0.0277(5) Uani 1 1 d . . . C25 C 0.2971(2) 0.63967(12) 0.35902(18) 0.0304(5) Uani 1 1 d . . . H25 H 0.3495 0.6057 0.3617 0.036 Uiso 1 1 calc R . . C26 C 0.2055(2) 0.64623(13) 0.2852(2) 0.0383(6) Uani 1 1 d . . . H26 H 0.1965 0.6169 0.2371 0.046 Uiso 1 1 calc R . . C27 C 0.1278(2) 0.69458(14) 0.2811(2) 0.0404(7) Uani 1 1 d . . . H27 H 0.0647 0.6984 0.2306 0.048 Uiso 1 1 calc R . . C28 C 0.1416(2) 0.73779(14) 0.3507(2) 0.0394(7) Uani 1 1 d . . . H28 H 0.0875 0.7711 0.3482 0.047 Uiso 1 1 calc R . . C29 C 0.2340(2) 0.73243(13) 0.42396(19) 0.0337(6) Uani 1 1 d . . . H29 H 0.2441 0.7626 0.4708 0.040 Uiso 1 1 calc R . . C30 C 0.2985(2) 0.63214(11) 0.66870(18) 0.0291(5) Uani 1 1 d . . . C31 C 0.3502(2) 0.63668(13) 0.77179(18) 0.0359(6) Uani 1 1 d . . . H31A H 0.4044 0.6025 0.7886 0.054 Uiso 1 1 calc R . . H31B H 0.2832 0.6361 0.8101 0.054 Uiso 1 1 calc R . . H31C H 0.3958 0.6744 0.7825 0.054 Uiso 1 1 calc R . . C32 C 0.2242(2) 0.57375(12) 0.6533(2) 0.0347(6) Uani 1 1 d . . . H32A H 0.1937 0.5697 0.5871 0.052 Uiso 1 1 calc R . . H32B H 0.1555 0.5751 0.6898 0.052 Uiso 1 1 calc R . . H32C H 0.2761 0.5392 0.6731 0.052 Uiso 1 1 calc R . . C33 C 0.2104(2) 0.68405(12) 0.6420(2) 0.0345(6) Uani 1 1 d . . . H33A H 0.2551 0.7222 0.6463 0.052 Uiso 1 1 calc R . . H33B H 0.1480 0.6849 0.6844 0.052 Uiso 1 1 calc R . . H33C H 0.1715 0.6783 0.5780 0.052 Uiso 1 1 calc R . . O1 O 1.0975(3) 0.91522(19) 0.4432(3) 0.1178(14) Uani 1 1 d . . . C34 C 1.1225(5) 0.9721(2) 0.4066(3) 0.0828(13) Uani 1 1 d . . . H34A H 1.0546 1.0003 0.4119 0.099 Uiso 1 1 calc R . . H34B H 1.1345 0.9685 0.3402 0.099 Uiso 1 1 calc R . . C35 C 1.2353(6) 0.9936(3) 0.4625(4) 0.1080(19) Uani 1 1 d . . . H35A H 1.3058 0.9898 0.4270 0.130 Uiso 1 1 calc R . . H35B H 1.2271 1.0363 0.4807 0.130 Uiso 1 1 calc R . . C36 C 1.2498(5) 0.9550(2) 0.5433(4) 0.114(2) Uani 1 1 d . . . H36A H 1.3366 0.9444 0.5602 0.137 Uiso 1 1 calc R . . H36B H 1.2205 0.9756 0.5970 0.137 Uiso 1 1 calc R . . C37 C 1.1816(6) 0.9038(3) 0.5200(4) 0.127(2) Uani 1 1 d . . . H37A H 1.1390 0.8914 0.5731 0.152 Uiso 1 1 calc R . . H37B H 1.2359 0.8704 0.5060 0.152 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 Cl1 0.0245(3) 0.0288(3) 0.0296(3) -0.0042(2) 0.0024(2) 0.0018(2) Cl2 0.0254(3) 0.0258(3) 0.0275(3) 0.0021(2) 0.0027(2) 0.0003(2) Cr1 0.0223(2) 0.0265(2) 0.0248(2) -0.00118(15) 0.00267(15) 0.00169(15) N1 0.0230(10) 0.0310(11) 0.0257(11) -0.0021(9) -0.0005(8) 0.0000(8) N2 0.0224(10) 0.0279(11) 0.0269(11) -0.0004(8) 0.0038(8) 0.0023(8) P1 0.0213(3) 0.0299(3) 0.0265(3) -0.0011(3) 0.0025(2) 0.0012(2) P2 0.0218(3) 0.0278(3) 0.0244(3) -0.0011(3) 0.0022(2) 0.0020(2) C1 0.0250(11) 0.0296(13) 0.0225(12) -0.0034(10) 0.0019(9) 0.0015(10) C2 0.0247(12) 0.0307(13) 0.0318(14) 0.0004(11) 0.0073(10) 0.0006(10) C3 0.0291(15) 0.115(3) 0.0339(17) -0.0115(18) -0.0014(12) 0.0182(17) C4 0.0264(14) 0.125(4) 0.0426(19) -0.013(2) 0.0051(13) 0.0210(18) C5 0.0365(14) 0.0521(18) 0.0370(16) 0.0016(13) 0.0143(12) 0.0099(13) C6 0.0366(14) 0.0332(14) 0.0309(14) -0.0014(11) 0.0091(11) 0.0016(11) C7 0.0264(12) 0.0414(16) 0.0346(15) -0.0041(12) 0.0030(11) 0.0039(11) C8 0.0229(11) 0.0308(14) 0.0375(15) 0.0016(11) -0.0019(10) -0.0005(10) C9 0.0376(15) 0.0426(17) 0.0432(17) 0.0046(13) 0.0053(13) -0.0025(13) C10 0.0428(16) 0.0407(18) 0.064(2) 0.0135(16) 0.0073(15) -0.0076(14) C11 0.0364(15) 0.0324(16) 0.075(2) 0.0019(16) -0.0071(15) -0.0059(12) C12 0.0358(15) 0.0399(16) 0.057(2) -0.0085(15) -0.0054(14) -0.0004(13) C13 0.0260(13) 0.0384(15) 0.0415(16) -0.0050(12) -0.0022(11) 0.0012(11) C14 0.0270(12) 0.0374(14) 0.0264(13) -0.0020(11) -0.0018(10) 0.0032(11) C15 0.0344(13) 0.0441(16) 0.0262(14) -0.0032(11) 0.0026(11) -0.0001(12) C16 0.0405(15) 0.0432(17) 0.0367(16) -0.0006(13) -0.0049(12) 0.0114(13) C17 0.0242(12) 0.0556(18) 0.0343(15) 0.0014(13) -0.0018(11) -0.0005(12) C18 0.0225(11) 0.0284(13) 0.0342(14) -0.0003(11) 0.0013(10) 0.0014(10) C19 0.0326(13) 0.0330(14) 0.0363(15) 0.0025(11) 0.0029(11) 0.0009(11) C20 0.0361(14) 0.0324(15) 0.0514(18) 0.0049(13) 0.0040(13) -0.0036(12) C21 0.0321(14) 0.0317(15) 0.062(2) -0.0085(14) 0.0050(13) -0.0027(11) C22 0.0330(14) 0.0431(16) 0.0467(18) -0.0160(14) 0.0092(12) -0.0022(12) C23 0.0301(13) 0.0384(15) 0.0362(15) -0.0046(12) 0.0061(11) -0.0030(11) C24 0.0234(11) 0.0339(14) 0.0255(13) 0.0018(10) 0.0020(9) -0.0005(10) C25 0.0287(12) 0.0331(14) 0.0289(13) 0.0004(11) 0.0014(10) -0.0003(10) C26 0.0380(14) 0.0434(16) 0.0315(15) 0.0002(12) -0.0037(12) -0.0076(13) C27 0.0275(13) 0.0535(18) 0.0376(16) 0.0126(14) -0.0058(11) -0.0040(12) C28 0.0283(13) 0.0454(17) 0.0437(17) 0.0122(13) 0.0017(12) 0.0069(12) C29 0.0293(13) 0.0382(15) 0.0334(14) 0.0030(11) 0.0028(11) 0.0027(11) C30 0.0271(12) 0.0317(13) 0.0297(13) -0.0038(11) 0.0083(10) 0.0008(10) C31 0.0373(14) 0.0447(16) 0.0273(14) -0.0012(12) 0.0101(11) -0.0001(12) C32 0.0296(13) 0.0351(14) 0.0409(16) -0.0026(12) 0.0107(11) -0.0025(11) C33 0.0303(13) 0.0355(14) 0.0397(16) -0.0031(12) 0.0121(11) 0.0038(11) O1 0.116(3) 0.139(3) 0.086(2) 0.035(2) -0.033(2) -0.066(2) C34 0.099(3) 0.090(3) 0.055(3) 0.008(2) -0.007(2) -0.001(3) C35 0.123(5) 0.097(4) 0.100(4) -0.001(3) -0.002(4) -0.048(3) C36 0.120(4) 0.092(4) 0.110(5) -0.028(3) -0.066(4) 0.033(3) C37 0.162(6) 0.133(5) 0.073(4) 0.041(3) -0.037(4) -0.058(5) _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 Cl1 Cr1 2.4211(7) . ? Cl1 Cr1 2.4309(7) 3_666 ? Cl2 Cr1 2.3971(7) . ? Cr1 N2 2.077(2) . ? Cr1 N1 2.100(2) . ? Cr1 C1 2.185(3) . ? Cr1 Cl1 2.4309(7) 3_666 ? Cr1 P1 2.7674(7) . ? Cr1 P2 2.7702(7) . ? N1 C14 1.496(3) . ? N1 P1 1.604(2) . ? N2 C30 1.496(3) . ? N2 P2 1.603(2) . ? P1 C1 1.750(3) . ? P1 C8 1.819(3) . ? P1 C2 1.827(2) . ? P2 C1 1.764(2) . ? P2 C18 1.822(3) . ? P2 C24 1.827(3) . ? C1 H1 0.82(3) . ? C2 C7 1.373(4) . ? C2 C3 1.392(4) . ? C3 C4 1.381(4) . ? C3 H3 0.9500 . ? C4 C5 1.367(4) . ? C4 H4 0.9500 . ? C5 C6 1.358(4) . ? C5 H5 0.9500 . ? C6 C7 1.394(4) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C13 1.391(4) . ? C8 C9 1.394(4) . ? C9 C10 1.391(4) . ? C9 H9 0.9500 . ? C10 C11 1.372(5) . ? C10 H10 0.9500 . ? C11 C12 1.380(5) . ? C11 H11 0.9500 . ? C12 C13 1.390(4) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.530(4) . ? C14 C16 1.531(4) . ? C14 C17 1.537(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C23 1.390(4) . ? C18 C19 1.400(4) . ? C19 C20 1.382(4) . ? C19 H19 0.9500 . ? C20 C21 1.384(4) . ? C20 H20 0.9500 . ? C21 C22 1.378(4) . ? C21 H21 0.9500 . ? C22 C23 1.388(4) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.394(4) . ? C24 C29 1.395(4) . ? C25 C26 1.387(4) . ? C25 H25 0.9500 . ? C26 C27 1.373(4) . ? C26 H26 0.9500 . ? C27 C28 1.386(4) . ? C27 H27 0.9500 . ? C28 C29 1.385(4) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 C33 1.529(4) . ? C30 C31 1.535(4) . ? C30 C32 1.536(4) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? O1 C37 1.384(6) . ? O1 C34 1.409(6) . ? C34 C35 1.481(7) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.444(8) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.384(7) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? 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 Cr1 Cl1 Cr1 100.23(2) . 3_666 ? N2 Cr1 N1 96.97(8) . . ? N2 Cr1 C1 74.45(8) . . ? N1 Cr1 C1 72.07(9) . . ? N2 Cr1 Cl2 101.11(6) . . ? N1 Cr1 Cl2 101.12(6) . . ? C1 Cr1 Cl2 171.02(7) . . ? N2 Cr1 Cl1 164.59(6) . . ? N1 Cr1 Cl1 90.06(6) . . ? C1 Cr1 Cl1 94.89(7) . . ? Cl2 Cr1 Cl1 90.90(2) . . ? N2 Cr1 Cl1 90.06(6) . 3_666 ? N1 Cr1 Cl1 163.41(6) . 3_666 ? C1 Cr1 Cl1 95.58(7) . 3_666 ? Cl2 Cr1 Cl1 92.19(2) . 3_666 ? Cl1 Cr1 Cl1 79.77(2) . 3_666 ? N2 Cr1 P1 94.87(6) . . ? N1 Cr1 P1 35.21(6) . . ? C1 Cr1 P1 39.21(7) . . ? Cl2 Cr1 P1 135.41(2) . . ? Cl1 Cr1 P1 82.98(2) . . ? Cl1 Cr1 P1 129.41(3) 3_666 . ? N2 Cr1 P2 35.08(6) . . ? N1 Cr1 P2 86.61(6) . . ? C1 Cr1 P2 39.54(6) . . ? Cl2 Cr1 P2 136.11(2) . . ? Cl1 Cr1 P2 132.59(2) . . ? Cl1 Cr1 P2 90.65(2) 3_666 . ? P1 Cr1 P2 67.76(2) . . ? C14 N1 P1 131.41(16) . . ? C14 N1 Cr1 129.49(16) . . ? P1 N1 Cr1 95.75(10) . . ? C30 N2 P2 129.45(17) . . ? C30 N2 Cr1 131.63(16) . . ? P2 N2 Cr1 96.79(9) . . ? N1 P1 C1 97.43(11) . . ? N1 P1 C8 113.71(12) . . ? C1 P1 C8 117.47(12) . . ? N1 P1 C2 122.14(11) . . ? C1 P1 C2 105.87(12) . . ? C8 P1 C2 101.03(12) . . ? N1 P1 Cr1 49.04(7) . . ? C1 P1 Cr1 52.12(8) . . ? C8 P1 Cr1 146.43(9) . . ? C2 P1 Cr1 112.48(8) . . ? N2 P2 C1 99.90(11) . . ? N2 P2 C18 116.12(11) . . ? C1 P2 C18 113.54(12) . . ? N2 P2 C24 118.18(11) . . ? C1 P2 C24 106.94(12) . . ? C18 P2 C24 102.29(12) . . ? N2 P2 Cr1 48.13(7) . . ? C1 P2 Cr1 52.03(8) . . ? C18 P2 Cr1 135.02(8) . . ? C24 P2 Cr1 122.43(8) . . ? P1 C1 P2 122.92(15) . . ? P1 C1 Cr1 88.68(11) . . ? P2 C1 Cr1 88.43(10) . . ? P1 C1 H1 118(2) . . ? P2 C1 H1 115(2) . . ? Cr1 C1 H1 114(2) . . ? C7 C2 C3 117.5(2) . . ? C7 C2 P1 121.78(19) . . ? C3 C2 P1 120.6(2) . . ? C4 C3 C2 120.7(3) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C5 C4 C3 120.7(3) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C6 C5 C4 119.5(3) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? C5 C6 C7 120.2(3) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C2 C7 C6 121.3(2) . . ? C2 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? C13 C8 C9 119.0(3) . . ? C13 C8 P1 119.1(2) . . ? C9 C8 P1 122.0(2) . . ? C10 C9 C8 119.9(3) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C11 C10 C9 120.5(3) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 C12 120.3(3) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C13 119.7(3) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C12 C13 C8 120.6(3) . . ? C12 C13 H13 119.7 . . ? C8 C13 H13 119.7 . . ? N1 C14 C15 107.56(19) . . ? N1 C14 C16 109.0(2) . . ? C15 C14 C16 110.7(2) . . ? N1 C14 C17 114.9(2) . . ? C15 C14 C17 107.2(2) . . ? C16 C14 C17 107.6(2) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 118.8(2) . . ? C23 C18 P2 122.6(2) . . ? C19 C18 P2 118.5(2) . . ? C20 C19 C18 120.3(3) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C21 120.1(3) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C22 C21 C20 120.2(3) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 120.0(3) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C22 C23 C18 120.5(3) . . ? C22 C23 H23 119.7 . . ? C18 C23 H23 119.7 . . ? C25 C24 C29 119.0(2) . . ? C25 C24 P2 120.52(19) . . ? C29 C24 P2 120.4(2) . . ? C26 C25 C24 120.0(2) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C27 C26 C25 120.7(3) . . ? C27 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C26 C27 C28 119.8(3) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C29 C28 C27 120.1(3) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C28 C29 C24 120.3(3) . . ? C28 C29 H29 119.9 . . ? C24 C29 H29 119.9 . . ? N2 C30 C33 112.8(2) . . ? N2 C30 C31 108.6(2) . . ? C33 C30 C31 110.3(2) . . ? N2 C30 C32 109.6(2) . . ? C33 C30 C32 106.6(2) . . ? C31 C30 C32 109.0(2) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C37 O1 C34 108.8(4) . . ? O1 C34 C35 106.0(4) . . ? O1 C34 H34A 110.5 . . ? C35 C34 H34A 110.5 . . ? O1 C34 H34B 110.5 . . ? C35 C34 H34B 110.5 . . ? H34A C34 H34B 108.7 . . ? C36 C35 C34 104.7(4) . . ? C36 C35 H35A 110.8 . . ? C34 C35 H35A 110.8 . . ? C36 C35 H35B 110.8 . . ? C34 C35 H35B 110.8 . . ? H35A C35 H35B 108.9 . . ? C37 C36 C35 106.7(4) . . ? C37 C36 H36A 110.4 . . ? C35 C36 H36A 110.4 . . ? C37 C36 H36B 110.4 . . ? C35 C36 H36B 110.4 . . ? H36A C36 H36B 108.6 . . ? C36 C37 O1 109.8(5) . . ? C36 C37 H37A 109.7 . . ? O1 C37 H37A 109.7 . . ? C36 C37 H37B 109.7 . . ? O1 C37 H37B 109.7 . . ? H37A C37 H37B 108.2 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.932 _refine_diff_density_min -0.607 _refine_diff_density_rms 0.074 #===END data_ckl-122 _database_code_depnum_ccdc_archive 'CCDC 651320' #compound 3c _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H35 Cl2 Cr N2 O2 P2, 2(C4 H8 O)' _chemical_formula_sum 'C47 H51 Cl2 Cr N2 O4 P2' _chemical_formula_weight 892.74 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' Cr Cr 0.3209 0.6236 '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' _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 9.412(1) _cell_length_b 13.128(1) _cell_length_c 18.731(1) _cell_angle_alpha 72.651(1) _cell_angle_beta 83.444(1) _cell_angle_gamma 80.124(1) _cell_volume 2171.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 5135 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description needle _exptl_crystal_colour pink _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.365 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 934 _exptl_absorpt_coefficient_mu 0.506 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8968 _exptl_absorpt_correction_T_max 0.9703 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16829 _diffrn_reflns_av_R_equivalents 0.0422 _diffrn_reflns_av_sigmaI/netI 0.0805 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.35 _reflns_number_total 7856 _reflns_number_gt 5263 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1059P)^2^+6.3290P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7856 _refine_ls_number_parameters 528 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1129 _refine_ls_R_factor_gt 0.0733 _refine_ls_wR_factor_ref 0.2261 _refine_ls_wR_factor_gt 0.2047 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 Cl1 Cl -0.16034(13) 0.30242(10) 0.91754(6) 0.0253(3) Uani 1 1 d . . . Cl2 Cl -0.28996(13) 0.37569(10) 0.66948(6) 0.0259(3) Uani 1 1 d . . . Cr1 Cr -0.20081(10) 0.33972(7) 0.78885(5) 0.0330(3) Uani 1 1 d . . . P1 P 0.08317(16) 0.45490(12) 0.75729(8) 0.0315(4) Uani 1 1 d . . . P2 P 0.12026(16) 0.22464(12) 0.76464(8) 0.0322(4) Uani 1 1 d . . . O1 O -0.3607(4) 0.4645(3) 0.8037(2) 0.0435(10) Uani 1 1 d . . . O2 O -0.3177(4) 0.2094(3) 0.8201(2) 0.0408(10) Uani 1 1 d . . . O3 O 0.3918(6) 0.2774(4) 1.0058(3) 0.0632(14) Uani 1 1 d . . . N1 N -0.0918(5) 0.4669(4) 0.7530(2) 0.0319(10) Uani 1 1 d . . . N2 N -0.0526(5) 0.2217(4) 0.7679(3) 0.0354(11) Uani 1 1 d . . . C1 C 0.1574(6) 0.3256(5) 0.7982(3) 0.0350(13) Uani 1 1 d . . . H1 H 0.164(7) 0.305(5) 0.856(4) 0.042 Uiso 1 1 d . . . C2 C 0.1703(6) 0.5017(4) 0.6647(3) 0.0329(12) Uani 1 1 d . . . C3 C 0.0951(7) 0.5192(4) 0.6005(3) 0.0357(13) Uani 1 1 d . . . H3 H -0.0038 0.5100 0.6050 0.043 Uiso 1 1 calc R . . C4 C 0.1670(7) 0.5497(5) 0.5309(3) 0.0402(14) Uani 1 1 d . . . H4 H 0.1173 0.5604 0.4873 0.048 Uiso 1 1 calc R . . C5 C 0.3099(7) 0.5650(5) 0.5236(3) 0.0405(14) Uani 1 1 d . . . H5 H 0.3572 0.5881 0.4752 0.049 Uiso 1 1 calc R . . C6 C 0.3837(7) 0.5468(5) 0.5866(3) 0.0443(15) Uani 1 1 d . . . H6 H 0.4825 0.5562 0.5818 0.053 Uiso 1 1 calc R . . C7 C 0.3138(7) 0.5146(5) 0.6572(3) 0.0388(14) Uani 1 1 d . . . H7 H 0.3653 0.5014 0.7006 0.047 Uiso 1 1 calc R . . C8 C 0.1242(6) 0.5389(5) 0.8112(3) 0.0355(13) Uani 1 1 d . . . C9 C 0.1184(7) 0.5004(5) 0.8897(3) 0.0394(14) Uani 1 1 d . . . H9 H 0.0956 0.4300 0.9141 0.047 Uiso 1 1 calc R . . C10 C 0.1460(7) 0.5646(5) 0.9314(3) 0.0429(15) Uani 1 1 d . . . H10 H 0.1445 0.5376 0.9845 0.051 Uiso 1 1 calc R . . C11 C 0.1757(7) 0.6674(5) 0.8966(3) 0.0440(15) Uani 1 1 d . . . H11 H 0.1938 0.7113 0.9258 0.053 Uiso 1 1 calc R . . C12 C 0.1795(7) 0.7070(5) 0.8203(4) 0.0423(15) Uani 1 1 d . . . H12 H 0.1994 0.7784 0.7968 0.051 Uiso 1 1 calc R . . C13 C 0.1547(6) 0.6440(5) 0.7771(3) 0.0379(14) Uani 1 1 d . . . H13 H 0.1582 0.6719 0.7241 0.045 Uiso 1 1 calc R . . C14 C -0.1856(6) 0.5656(5) 0.7308(3) 0.0348(13) Uani 1 1 d . . . C15 C -0.1477(7) 0.6637(5) 0.6859(3) 0.0368(13) Uani 1 1 d . . . H15 H -0.0496 0.6690 0.6687 0.044 Uiso 1 1 calc R . . C16 C -0.2517(7) 0.7535(5) 0.6659(3) 0.0428(15) Uani 1 1 d . . . H16 H -0.2238 0.8194 0.6344 0.051 Uiso 1 1 calc R . . C17 C -0.3949(7) 0.7496(5) 0.6908(4) 0.0455(15) Uani 1 1 d . . . H17 H -0.4647 0.8123 0.6768 0.055 Uiso 1 1 calc R . . C18 C -0.4366(7) 0.6529(5) 0.7367(4) 0.0431(15) Uani 1 1 d . . . H18 H -0.5349 0.6483 0.7538 0.052 Uiso 1 1 calc R . . C19 C -0.3313(6) 0.5638(4) 0.7568(3) 0.0339(13) Uani 1 1 d . . . C20 C -0.4838(7) 0.4623(6) 0.8586(4) 0.0557(18) Uani 1 1 d . . . H20A H -0.5008 0.5295 0.8730 0.084 Uiso 1 1 calc R . . H20B H -0.4635 0.4011 0.9031 0.084 Uiso 1 1 calc R . . H20C H -0.5699 0.4548 0.8368 0.084 Uiso 1 1 calc R . . C21 C 0.1981(6) 0.2396(4) 0.6703(3) 0.0356(13) Uani 1 1 d . . . C22 C 0.1115(7) 0.2517(5) 0.6120(3) 0.0432(15) Uani 1 1 d . . . H22 H 0.0104 0.2507 0.6219 0.052 Uiso 1 1 calc R . . C23 C 0.1733(8) 0.2651(5) 0.5390(3) 0.0472(16) Uani 1 1 d . . . H23 H 0.1143 0.2730 0.4993 0.057 Uiso 1 1 calc R . . C24 C 0.3181(9) 0.2671(5) 0.5248(4) 0.0521(18) Uani 1 1 d . . . H24 H 0.3595 0.2764 0.4749 0.063 Uiso 1 1 calc R . . C25 C 0.4049(8) 0.2556(5) 0.5816(4) 0.0512(18) Uani 1 1 d . . . H25 H 0.5060 0.2562 0.5709 0.061 Uiso 1 1 calc R . . C26 C 0.3462(7) 0.2432(5) 0.6546(4) 0.0437(15) Uani 1 1 d . . . H26 H 0.4061 0.2373 0.6936 0.052 Uiso 1 1 calc R . . C27 C 0.1989(6) 0.0966(5) 0.8240(3) 0.0374(14) Uani 1 1 d . . . C28 C 0.1512(7) 0.0717(5) 0.8995(3) 0.0437(15) Uani 1 1 d . . . H28 H 0.0825 0.1218 0.9176 0.052 Uiso 1 1 calc R . . C29 C 0.2043(8) -0.0266(5) 0.9483(4) 0.0516(17) Uani 1 1 d . . . H29 H 0.1702 -0.0441 0.9996 0.062 Uiso 1 1 calc R . . C30 C 0.3068(7) -0.0994(5) 0.9226(4) 0.0488(17) Uani 1 1 d . . . H30 H 0.3456 -0.1652 0.9566 0.059 Uiso 1 1 calc R . . C31 C 0.3525(7) -0.0756(5) 0.8468(4) 0.0457(16) Uani 1 1 d . . . H31 H 0.4210 -0.1258 0.8287 0.055 Uiso 1 1 calc R . . C32 C 0.2980(7) 0.0212(5) 0.7981(4) 0.0403(14) Uani 1 1 d . . . H32 H 0.3281 0.0367 0.7463 0.048 Uiso 1 1 calc R . . C33 C -0.1131(7) 0.1344(4) 0.7597(3) 0.0357(13) Uani 1 1 d . . . C34 C -0.2584(7) 0.1292(5) 0.7859(3) 0.0376(14) Uani 1 1 d . . . C35 C -0.3332(7) 0.0520(5) 0.7792(4) 0.0481(16) Uani 1 1 d . . . H35 H -0.4319 0.0517 0.7968 0.058 Uiso 1 1 calc R . . C36 C -0.2619(8) -0.0254(5) 0.7463(4) 0.0528(18) Uani 1 1 d . . . H36 H -0.3124 -0.0792 0.7409 0.063 Uiso 1 1 calc R . . C37 C -0.1178(8) -0.0257(5) 0.7210(4) 0.0478(16) Uani 1 1 d . . . H37 H -0.0692 -0.0799 0.6991 0.057 Uiso 1 1 calc R . . C38 C -0.0443(7) 0.0547(5) 0.7278(3) 0.0419(15) Uani 1 1 d . . . H38 H 0.0545 0.0546 0.7103 0.050 Uiso 1 1 calc R . . C39 C -0.4469(8) 0.1921(6) 0.8688(4) 0.0566(19) Uani 1 1 d . . . H39A H -0.5315 0.2139 0.8388 0.085 Uiso 1 1 calc R . . H39B H -0.4557 0.2352 0.9042 0.085 Uiso 1 1 calc R . . H39C H -0.4414 0.1155 0.8966 0.085 Uiso 1 1 calc R . . C40 C 0.3664(9) 0.3288(7) 1.0647(4) 0.065(2) Uani 1 1 d . . . H40A H 0.3560 0.4082 1.0434 0.078 Uiso 1 1 calc R . . H40B H 0.4479 0.3053 1.0977 0.078 Uiso 1 1 calc R . . C41 C 0.2274(10) 0.2952(7) 1.1084(4) 0.074(2) Uani 1 1 d . . . H41A H 0.2455 0.2558 1.1613 0.088 Uiso 1 1 calc R . . H41B H 0.1536 0.3592 1.1073 0.088 Uiso 1 1 calc R . . C42 C 0.1772(9) 0.2226(8) 1.0696(4) 0.074(2) Uani 1 1 d . . . H42A H 0.1394 0.1602 1.1064 0.088 Uiso 1 1 calc R . . H42B H 0.1017 0.2628 1.0348 0.088 Uiso 1 1 calc R . . C43 C 0.3143(8) 0.1874(7) 1.0279(4) 0.064(2) Uani 1 1 d . . . H43A H 0.3715 0.1238 1.0607 0.077 Uiso 1 1 calc R . . H43B H 0.2920 0.1685 0.9834 0.077 Uiso 1 1 calc R . . O4 O 0.188(2) 0.8682(9) 0.6123(7) 0.217(8) Uani 1 1 d . . . C44 C 0.1407(18) 0.8330(10) 0.5605(11) 0.143(6) Uani 1 1 d . . . H44A H 0.0337 0.8451 0.5623 0.172 Uiso 1 1 calc R . . H44B H 0.1749 0.7550 0.5685 0.172 Uiso 1 1 calc R . . C45 C 0.2023(19) 0.8972(14) 0.4872(7) 0.152(7) Uani 1 1 d . . . H45A H 0.1278 0.9511 0.4579 0.182 Uiso 1 1 calc R . . H45B H 0.2548 0.8510 0.4567 0.182 Uiso 1 1 calc R . . C46 C 0.305(2) 0.9499(15) 0.5190(15) 0.196(10) Uani 1 1 d . . . H46A H 0.4018 0.9055 0.5228 0.236 Uiso 1 1 calc R . . H46B H 0.3158 1.0224 0.4847 0.236 Uiso 1 1 calc R . . C47 C 0.255(3) 0.9583(17) 0.5843(11) 0.187(9) Uani 1 1 d . . . H47A H 0.1850 1.0250 0.5805 0.225 Uiso 1 1 calc R . . H47B H 0.3333 0.9572 0.6156 0.225 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 Cl1 0.0256(7) 0.0326(7) 0.0176(6) -0.0053(5) 0.0010(5) -0.0090(5) Cl2 0.0251(7) 0.0325(7) 0.0195(6) -0.0067(5) -0.0079(5) 0.0002(5) Cr1 0.0291(5) 0.0384(5) 0.0321(5) -0.0103(4) 0.0012(4) -0.0084(4) P1 0.0285(8) 0.0354(8) 0.0304(7) -0.0084(6) 0.0006(6) -0.0075(6) P2 0.0285(8) 0.0336(8) 0.0335(8) -0.0077(6) -0.0020(6) -0.0051(6) O1 0.033(2) 0.043(2) 0.051(3) -0.011(2) 0.0117(19) -0.0068(19) O2 0.035(2) 0.044(2) 0.047(2) -0.0174(19) 0.0105(19) -0.0150(19) O3 0.067(4) 0.075(3) 0.053(3) -0.026(3) 0.016(3) -0.024(3) N1 0.025(2) 0.036(3) 0.034(2) -0.011(2) -0.004(2) -0.003(2) N2 0.032(3) 0.042(3) 0.033(3) -0.010(2) 0.000(2) -0.011(2) C1 0.032(3) 0.036(3) 0.040(3) -0.015(3) -0.006(3) -0.004(3) C2 0.029(3) 0.036(3) 0.035(3) -0.010(2) -0.004(2) -0.006(2) C3 0.036(3) 0.037(3) 0.034(3) -0.011(2) 0.000(3) -0.007(3) C4 0.047(4) 0.042(3) 0.031(3) -0.012(3) -0.002(3) -0.003(3) C5 0.046(4) 0.044(3) 0.029(3) -0.007(3) 0.006(3) -0.009(3) C6 0.036(4) 0.055(4) 0.040(4) -0.010(3) 0.010(3) -0.016(3) C7 0.037(3) 0.043(3) 0.036(3) -0.011(3) 0.000(3) -0.007(3) C8 0.032(3) 0.039(3) 0.037(3) -0.012(3) -0.001(3) -0.006(3) C9 0.042(4) 0.041(3) 0.038(3) -0.016(3) 0.002(3) -0.007(3) C10 0.045(4) 0.054(4) 0.035(3) -0.019(3) 0.000(3) -0.009(3) C11 0.042(4) 0.053(4) 0.043(4) -0.023(3) 0.000(3) -0.007(3) C12 0.041(4) 0.040(3) 0.050(4) -0.016(3) 0.000(3) -0.011(3) C13 0.030(3) 0.047(3) 0.037(3) -0.011(3) 0.000(3) -0.010(3) C14 0.035(3) 0.040(3) 0.029(3) -0.011(2) -0.002(2) -0.003(3) C15 0.037(3) 0.038(3) 0.035(3) -0.008(3) -0.003(3) -0.009(3) C16 0.051(4) 0.035(3) 0.042(3) -0.010(3) -0.004(3) -0.005(3) C17 0.038(4) 0.039(3) 0.058(4) -0.016(3) -0.006(3) 0.003(3) C18 0.030(3) 0.049(4) 0.053(4) -0.022(3) -0.001(3) -0.001(3) C19 0.032(3) 0.035(3) 0.035(3) -0.011(3) -0.003(2) -0.002(3) C20 0.036(4) 0.068(5) 0.060(4) -0.023(4) 0.020(3) -0.006(3) C21 0.036(3) 0.032(3) 0.038(3) -0.009(2) 0.003(3) -0.007(3) C22 0.044(4) 0.042(3) 0.043(4) -0.013(3) 0.000(3) -0.005(3) C23 0.059(5) 0.051(4) 0.032(3) -0.014(3) 0.003(3) -0.007(3) C24 0.072(5) 0.050(4) 0.036(4) -0.016(3) 0.015(3) -0.019(4) C25 0.044(4) 0.056(4) 0.053(4) -0.020(3) 0.021(3) -0.012(3) C26 0.037(4) 0.047(4) 0.048(4) -0.013(3) 0.001(3) -0.011(3) C27 0.029(3) 0.041(3) 0.044(3) -0.011(3) -0.005(3) -0.011(3) C28 0.045(4) 0.043(3) 0.040(3) -0.005(3) -0.004(3) -0.008(3) C29 0.053(4) 0.049(4) 0.046(4) -0.003(3) -0.004(3) -0.008(3) C30 0.048(4) 0.036(3) 0.060(4) -0.001(3) -0.017(3) -0.013(3) C31 0.037(4) 0.038(3) 0.060(4) -0.008(3) -0.005(3) -0.008(3) C32 0.038(4) 0.039(3) 0.044(3) -0.010(3) -0.002(3) -0.010(3) C33 0.039(3) 0.034(3) 0.034(3) -0.009(2) -0.004(3) -0.006(3) C34 0.035(3) 0.040(3) 0.039(3) -0.013(3) -0.003(3) -0.007(3) C35 0.039(4) 0.057(4) 0.051(4) -0.016(3) 0.006(3) -0.018(3) C36 0.058(5) 0.045(4) 0.064(4) -0.024(3) 0.002(4) -0.020(3) C37 0.048(4) 0.042(4) 0.058(4) -0.019(3) -0.005(3) -0.009(3) C38 0.039(4) 0.045(3) 0.043(3) -0.011(3) -0.001(3) -0.010(3) C39 0.042(4) 0.077(5) 0.061(4) -0.033(4) 0.022(3) -0.028(4) C40 0.062(5) 0.067(5) 0.066(5) -0.023(4) -0.019(4) 0.010(4) C41 0.084(6) 0.076(5) 0.050(4) -0.019(4) 0.011(4) 0.010(5) C42 0.056(5) 0.100(6) 0.054(5) -0.014(4) 0.002(4) 0.000(5) C43 0.051(5) 0.084(6) 0.064(5) -0.031(4) 0.003(4) -0.014(4) O4 0.39(2) 0.086(7) 0.120(9) -0.008(6) 0.085(11) -0.004(10) C44 0.158(14) 0.081(8) 0.194(17) -0.041(10) 0.037(12) -0.056(9) C45 0.170(15) 0.193(15) 0.068(7) -0.046(9) -0.022(8) 0.063(13) C46 0.147(16) 0.163(16) 0.31(3) -0.117(17) 0.095(18) -0.080(13) C47 0.24(2) 0.171(18) 0.140(15) -0.072(14) -0.040(15) 0.064(17) _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 Cl1 Cr1 2.3742(15) . ? Cl2 Cr1 2.3641(15) . ? Cr1 N2 1.999(5) . ? Cr1 N1 2.013(4) . ? Cr1 O1 2.087(4) . ? Cr1 O2 2.094(4) . ? P1 N1 1.636(5) . ? P1 C1 1.702(6) . ? P1 C2 1.808(6) . ? P1 C8 1.813(6) . ? P2 N2 1.628(5) . ? P2 C1 1.726(6) . ? P2 C21 1.802(6) . ? P2 C27 1.804(6) . ? O1 C19 1.389(7) . ? O1 C20 1.457(7) . ? O2 C34 1.396(7) . ? O2 C39 1.443(7) . ? O3 C43 1.426(9) . ? O3 C40 1.434(9) . ? N1 C14 1.415(7) . ? N2 C33 1.418(7) . ? C1 H1 1.04(6) . ? C2 C7 1.376(8) . ? C2 C3 1.406(8) . ? C3 C4 1.377(8) . ? C3 H3 0.9500 . ? C4 C5 1.379(9) . ? C4 H4 0.9500 . ? C5 C6 1.378(9) . ? C5 H5 0.9500 . ? C6 C7 1.386(8) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C13 1.400(8) . ? C8 C9 1.402(8) . ? C9 C10 1.381(8) . ? C9 H9 0.9500 . ? C10 C11 1.374(9) . ? C10 H10 0.9500 . ? C11 C12 1.366(9) . ? C11 H11 0.9500 . ? C12 C13 1.378(8) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.391(8) . ? C14 C19 1.404(8) . ? C15 C16 1.383(9) . ? C15 H15 0.9500 . ? C16 C17 1.380(9) . ? C16 H16 0.9500 . ? C17 C18 1.396(9) . ? C17 H17 0.9500 . ? C18 C19 1.384(8) . ? C18 H18 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.391(9) . ? C21 C26 1.397(8) . ? C22 C23 1.396(8) . ? C22 H22 0.9500 . ? C23 C24 1.362(10) . ? C23 H23 0.9500 . ? C24 C25 1.373(10) . ? C24 H24 0.9500 . ? C25 C26 1.389(9) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.391(8) . ? C27 C32 1.397(9) . ? C28 C29 1.390(9) . ? C28 H28 0.9500 . ? C29 C30 1.388(10) . ? C29 H29 0.9500 . ? C30 C31 1.394(9) . ? C30 H30 0.9500 . ? C31 C32 1.379(9) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C38 1.387(8) . ? C33 C34 1.405(8) . ? C34 C35 1.372(8) . ? C35 C36 1.381(9) . ? C35 H35 0.9500 . ? C36 C37 1.385(10) . ? C36 H36 0.9500 . ? C37 C38 1.399(8) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.522(12) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.518(12) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.507(11) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? O4 C44 1.34(2) . ? O4 C47 1.37(2) . ? C44 C45 1.492(19) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.54(2) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.29(2) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? 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 N2 Cr1 N1 101.55(19) . . ? N2 Cr1 O1 176.14(19) . . ? N1 Cr1 O1 78.71(17) . . ? N2 Cr1 O2 78.38(17) . . ? N1 Cr1 O2 176.84(18) . . ? O1 Cr1 O2 101.14(16) . . ? N2 Cr1 Cl2 90.35(14) . . ? N1 Cr1 Cl2 91.63(14) . . ? O1 Cr1 Cl2 85.79(13) . . ? O2 Cr1 Cl2 85.21(12) . . ? N2 Cr1 Cl1 96.83(14) . . ? N1 Cr1 Cl1 95.64(14) . . ? O1 Cr1 Cl1 86.96(13) . . ? O2 Cr1 Cl1 87.51(12) . . ? Cl2 Cr1 Cl1 168.55(6) . . ? N1 P1 C1 112.3(3) . . ? N1 P1 C2 110.7(3) . . ? C1 P1 C2 109.2(3) . . ? N1 P1 C8 110.0(3) . . ? C1 P1 C8 108.0(3) . . ? C2 P1 C8 106.4(3) . . ? N2 P2 C1 112.0(3) . . ? N2 P2 C21 110.1(3) . . ? C1 P2 C21 110.6(3) . . ? N2 P2 C27 106.9(3) . . ? C1 P2 C27 108.3(3) . . ? C21 P2 C27 108.8(3) . . ? C19 O1 C20 118.5(5) . . ? C19 O1 Cr1 111.3(3) . . ? C20 O1 Cr1 129.9(4) . . ? C34 O2 C39 117.3(4) . . ? C34 O2 Cr1 112.3(3) . . ? C39 O2 Cr1 130.4(4) . . ? C43 O3 C40 107.4(6) . . ? C14 N1 P1 125.3(4) . . ? C14 N1 Cr1 112.0(4) . . ? P1 N1 Cr1 122.5(3) . . ? C33 N2 P2 124.0(4) . . ? C33 N2 Cr1 113.4(4) . . ? P2 N2 Cr1 122.6(3) . . ? P1 C1 P2 118.5(4) . . ? P1 C1 H1 116(3) . . ? P2 C1 H1 115(3) . . ? C7 C2 C3 119.8(5) . . ? C7 C2 P1 119.6(4) . . ? C3 C2 P1 120.5(4) . . ? C4 C3 C2 119.0(6) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 121.1(6) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C6 C5 C4 119.8(5) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C7 120.0(6) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C2 C7 C6 120.4(6) . . ? C2 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C13 C8 C9 118.5(5) . . ? C13 C8 P1 121.9(4) . . ? C9 C8 P1 119.5(4) . . ? C10 C9 C8 120.0(6) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C11 C10 C9 120.3(6) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C12 C11 C10 120.5(6) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C13 120.4(6) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C12 C13 C8 120.2(6) . . ? C12 C13 H13 119.9 . . ? C8 C13 H13 119.9 . . ? C15 C14 C19 117.1(5) . . ? C15 C14 N1 126.5(5) . . ? C19 C14 N1 116.4(5) . . ? C16 C15 C14 120.6(6) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C17 C16 C15 121.4(6) . . ? C17 C16 H16 119.3 . . ? C15 C16 H16 119.3 . . ? C16 C17 C18 119.5(6) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C19 C18 C17 118.5(6) . . ? C19 C18 H18 120.8 . . ? C17 C18 H18 120.8 . . ? C18 C19 O1 123.1(5) . . ? C18 C19 C14 122.8(5) . . ? O1 C19 C14 114.1(5) . . ? O1 C20 H20A 109.5 . . ? O1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C26 119.4(5) . . ? C22 C21 P2 120.7(5) . . ? C26 C21 P2 119.8(5) . . ? C21 C22 C23 119.9(6) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C24 C23 C22 120.1(7) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C25 120.7(6) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C24 C25 C26 120.5(6) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C25 C26 C21 119.4(6) . . ? C25 C26 H26 120.3 . . ? C21 C26 H26 120.3 . . ? C28 C27 C32 119.3(6) . . ? C28 C27 P2 116.6(5) . . ? C32 C27 P2 124.1(5) . . ? C29 C28 C27 119.8(6) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C30 C29 C28 120.5(6) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C29 C30 C31 119.7(6) . . ? C29 C30 H30 120.1 . . ? C31 C30 H30 120.1 . . ? C32 C31 C30 119.7(6) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C31 C32 C27 120.8(6) . . ? C31 C32 H32 119.6 . . ? C27 C32 H32 119.6 . . ? C38 C33 C34 116.9(5) . . ? C38 C33 N2 126.8(5) . . ? C34 C33 N2 116.3(5) . . ? C35 C34 O2 123.6(5) . . ? C35 C34 C33 123.0(6) . . ? O2 C34 C33 113.3(5) . . ? C34 C35 C36 118.6(6) . . ? C34 C35 H35 120.7 . . ? C36 C35 H35 120.7 . . ? C35 C36 C37 120.9(6) . . ? C35 C36 H36 119.6 . . ? C37 C36 H36 119.6 . . ? C36 C37 C38 119.5(6) . . ? C36 C37 H37 120.3 . . ? C38 C37 H37 120.3 . . ? C33 C38 C37 121.2(6) . . ? C33 C38 H38 119.4 . . ? C37 C38 H38 119.4 . . ? O2 C39 H39A 109.5 . . ? O2 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? O2 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O3 C40 C41 106.4(7) . . ? O3 C40 H40A 110.4 . . ? C41 C40 H40A 110.4 . . ? O3 C40 H40B 110.4 . . ? C41 C40 H40B 110.4 . . ? H40A C40 H40B 108.6 . . ? C42 C41 C40 105.6(6) . . ? C42 C41 H41A 110.6 . . ? C40 C41 H41A 110.6 . . ? C42 C41 H41B 110.6 . . ? C40 C41 H41B 110.6 . . ? H41A C41 H41B 108.8 . . ? C43 C42 C41 102.2(7) . . ? C43 C42 H42A 111.3 . . ? C41 C42 H42A 111.3 . . ? C43 C42 H42B 111.3 . . ? C41 C42 H42B 111.3 . . ? H42A C42 H42B 109.2 . . ? O3 C43 C42 105.5(7) . . ? O3 C43 H43A 110.6 . . ? C42 C43 H43A 110.6 . . ? O3 C43 H43B 110.6 . . ? C42 C43 H43B 110.6 . . ? H43A C43 H43B 108.8 . . ? C44 O4 C47 114.8(13) . . ? O4 C44 C45 105.2(12) . . ? O4 C44 H44A 110.7 . . ? C45 C44 H44A 110.7 . . ? O4 C44 H44B 110.7 . . ? C45 C44 H44B 110.7 . . ? H44A C44 H44B 108.8 . . ? C44 C45 C46 97.3(12) . . ? C44 C45 H45A 112.3 . . ? C46 C45 H45A 112.3 . . ? C44 C45 H45B 112.3 . . ? C46 C45 H45B 112.3 . . ? H45A C45 H45B 109.9 . . ? C47 C46 C45 110.0(16) . . ? C47 C46 H46A 109.7 . . ? C45 C46 H46A 109.7 . . ? C47 C46 H46B 109.7 . . ? C45 C46 H46B 109.7 . . ? H46A C46 H46B 108.2 . . ? C46 C47 O4 101.9(16) . . ? C46 C47 H47A 111.4 . . ? O4 C47 H47A 111.4 . . ? C46 C47 H47B 111.4 . . ? O4 C47 H47B 111.4 . . ? H47A C47 H47B 109.3 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.032 _refine_diff_density_min -0.726 _refine_diff_density_rms 0.100 #===END