# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Duncan Wass' _publ_contact_author_email DUNCAN.WASS@BRISTOL.AC.UK _publ_section_title ; Ligand effects in chromium diphosphine catalysed olefin co-trimerisation and diene trimerisation ; loop_ _publ_author_name 'Duncan Wass' 'Lucy E Bowen' 'Manutsavin Charernsuk' 'Thomas Hey' 'Claire L McMullin' 'A Orpen' # Attachment '9.cif' data_twh39 _database_code_depnum_ccdc_archive 'CCDC 739221' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H27 Cr N O4 P2, 0.5(C H3 O)' _chemical_formula_sum 'C31.5 H28.5 Cr N O4.5 P2' _chemical_formula_weight 607.02 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' Cr Cr 0.3209 0.6236 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.9443(4) _cell_length_b 15.8753(7) _cell_length_c 38.8284(15) _cell_angle_alpha 90.00 _cell_angle_beta 101.4160(10) _cell_angle_gamma 90.00 _cell_volume 6008.5(4) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 57913 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.342 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2516 _exptl_absorpt_coefficient_mu 0.525 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.838 _exptl_absorpt_correction_T_max 0.872 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Bruker-Nonius Roper CCD camera on \k-goniostat ; _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_reflns_number 51936 _diffrn_reflns_av_R_equivalents 0.0897 _diffrn_reflns_av_sigmaI/netI 0.0930 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -51 _diffrn_reflns_limit_l_max 50 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 28.63 _reflns_number_total 13757 _reflns_number_gt 9189 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement ; DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' Although determined using DirAx, the cell is refined in the HKL package during data reduction ; _computing_data_reduction ;DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; The co-crystallised methanol solvent molecule was modelled to have 50% static disorder over two positions. The EADP command was used on C32a and C32b so their thermal parameters were the same as O5a and O5b respectively. The bond lengths between the O5 and C32 atoms were fixed to be 1.43 angstroms using the DFIX command. The hydrogen attached to the oxygen of the disordered methanol's were left out of the model. 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^)+(0.0914P)^2^+7.9923P] 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 13757 _refine_ls_number_parameters 735 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1147 _refine_ls_R_factor_gt 0.0694 _refine_ls_wR_factor_ref 0.1882 _refine_ls_wR_factor_gt 0.1654 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.004 _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 Cr1A Cr 1.04801(6) 0.68098(4) 0.820718(15) 0.01991(15) Uani 1 1 d . . . P1A P 0.81000(10) 0.71182(6) 0.81241(2) 0.0198(2) Uani 1 1 d . . . P2A P 0.91234(9) 0.57134(6) 0.79230(2) 0.0185(2) Uani 1 1 d . . . O1A O 1.0879(3) 0.78839(19) 0.75877(8) 0.0374(7) Uani 1 1 d . . . O2A O 1.1624(3) 0.82717(18) 0.86706(8) 0.0367(7) Uani 1 1 d . . . O3A O 1.3121(3) 0.59611(19) 0.81359(9) 0.0423(8) Uani 1 1 d . . . O4A O 1.0662(4) 0.5865(2) 0.88935(8) 0.0519(10) Uani 1 1 d . . . N1A N 0.7610(3) 0.61223(19) 0.79882(8) 0.0207(7) Uani 1 1 d . . . C1A C 0.6259(4) 0.5717(3) 0.79098(11) 0.0259(8) Uani 1 1 d . . . H1 H 0.5800 0.5857 0.7669 0.039 Uiso 1 1 calc R . . H2 H 0.5703 0.5918 0.8075 0.039 Uiso 1 1 calc R . . H3 H 0.6371 0.5105 0.7933 0.039 Uiso 1 1 calc R . . C2A C 0.7138(4) 0.7375(2) 0.84699(10) 0.0252(8) Uani 1 1 d . . . C3A C 0.7916(5) 0.7355(3) 0.88122(11) 0.0360(10) Uani 1 1 d . . . H3A H 0.8863 0.7219 0.8848 0.043 Uiso 1 1 calc R . . C4A C 0.7334(6) 0.7531(3) 0.90993(13) 0.0484(13) Uani 1 1 d . . . H4A H 0.7878 0.7514 0.9330 0.058 Uiso 1 1 calc R . . C5A C 0.5956(6) 0.7733(3) 0.90489(14) 0.0526(15) Uani 1 1 d . . . H5A H 0.5546 0.7850 0.9245 0.063 Uiso 1 1 calc R . . C6A C 0.5174(5) 0.7763(3) 0.87118(14) 0.0420(12) Uani 1 1 d . . . H6A H 0.4229 0.7901 0.8681 0.050 Uiso 1 1 calc R . . C7A C 0.5733(4) 0.7596(3) 0.84126(12) 0.0312(9) Uani 1 1 d . . . C8A C 0.4815(5) 0.7713(3) 0.80612(13) 0.0377(11) Uani 1 1 d . . . H4 H 0.3856 0.7714 0.8088 0.056 Uiso 1 1 calc R . . H5 H 0.4961 0.7251 0.7905 0.056 Uiso 1 1 calc R . . H6 H 0.5028 0.8251 0.7960 0.056 Uiso 1 1 calc R . . C9A C 0.7439(4) 0.7838(2) 0.77624(10) 0.0212(8) Uani 1 1 d . . . C10A C 0.6813(4) 0.7526(3) 0.74341(10) 0.0254(8) Uani 1 1 d . . . H10A H 0.6719 0.6934 0.7402 0.031 Uiso 1 1 calc R . . C11A C 0.6325(4) 0.8057(3) 0.71532(11) 0.0292(9) Uani 1 1 d . . . H11A H 0.5888 0.7835 0.6932 0.035 Uiso 1 1 calc R . . C12A C 0.6487(4) 0.8925(3) 0.72017(11) 0.0318(10) Uani 1 1 d . . . H12A H 0.6140 0.9300 0.7015 0.038 Uiso 1 1 calc R . . C13A C 0.7150(4) 0.9237(3) 0.75204(11) 0.0287(9) Uani 1 1 d . . . H13A H 0.7273 0.9828 0.7547 0.034 Uiso 1 1 calc R . . C14A C 0.7645(4) 0.8716(2) 0.78046(10) 0.0239(8) Uani 1 1 d . . . C15A C 0.8420(4) 0.9089(2) 0.81464(11) 0.0293(9) Uani 1 1 d . . . H15A H 0.9363 0.8874 0.8195 0.044 Uiso 1 1 calc R . . H15B H 0.7964 0.8930 0.8339 0.044 Uiso 1 1 calc R . . H15C H 0.8435 0.9704 0.8127 0.044 Uiso 1 1 calc R . . C16A C 0.8862(4) 0.5440(2) 0.74588(10) 0.0214(8) Uani 1 1 d . . . C17A C 0.9441(4) 0.5952(2) 0.72311(10) 0.0257(8) Uani 1 1 d . . . H17A H 1.0041 0.6399 0.7323 0.031 Uiso 1 1 calc R . . C18A C 0.9138(5) 0.5807(3) 0.68722(11) 0.0304(9) Uani 1 1 d . . . H18A H 0.9516 0.6161 0.6718 0.036 Uiso 1 1 calc R . . C19A C 0.8287(4) 0.5148(3) 0.67377(11) 0.0309(9) Uani 1 1 d . . . H19A H 0.8088 0.5047 0.6492 0.037 Uiso 1 1 calc R . . C20A C 0.7723(4) 0.4634(3) 0.69590(10) 0.0288(9) Uani 1 1 d . . . H20A H 0.7139 0.4182 0.6865 0.035 Uiso 1 1 calc R . . C21A C 0.8008(4) 0.4776(2) 0.73194(10) 0.0248(8) Uani 1 1 d . . . H21A H 0.7620 0.4421 0.7471 0.030 Uiso 1 1 calc R . . C22A C 0.9324(4) 0.4702(2) 0.81454(9) 0.0192(7) Uani 1 1 d . . . C23A C 1.0242(4) 0.4112(2) 0.80570(10) 0.0250(8) Uani 1 1 d . . . H23A H 1.0591 0.4185 0.7848 0.030 Uiso 1 1 calc R . . C24A C 1.0648(4) 0.3421(3) 0.82718(11) 0.0290(9) Uani 1 1 d . . . H24A H 1.1262 0.3017 0.8209 0.035 Uiso 1 1 calc R . . C25A C 1.0146(4) 0.3324(3) 0.85803(11) 0.0310(9) Uani 1 1 d . . . H25A H 1.0442 0.2861 0.8731 0.037 Uiso 1 1 calc R . . C26A C 0.9231(4) 0.3892(3) 0.86678(11) 0.0295(9) Uani 1 1 d . . . H26A H 0.8884 0.3815 0.8877 0.035 Uiso 1 1 calc R . . C27A C 0.8807(4) 0.4581(2) 0.84517(10) 0.0253(8) Uani 1 1 d . . . H27A H 0.8165 0.4970 0.8512 0.030 Uiso 1 1 calc R . . C28A C 1.0664(4) 0.7470(2) 0.78157(10) 0.0250(8) Uani 1 1 d . . . C29A C 1.1193(4) 0.7722(3) 0.84893(10) 0.0260(8) Uani 1 1 d . . . C30A C 1.2117(4) 0.6301(2) 0.81692(11) 0.0284(9) Uani 1 1 d . . . C31A C 1.0542(4) 0.6214(3) 0.86286(11) 0.0315(9) Uani 1 1 d . . . Cr1B Cr 0.44125(6) 0.15231(4) 0.932635(15) 0.01969(15) Uani 1 1 d . . . P1B P 0.66062(9) 0.12746(6) 0.91913(2) 0.0186(2) Uani 1 1 d . . . P2B P 0.58784(9) 0.26813(6) 0.94673(2) 0.0192(2) Uani 1 1 d . . . O1B O 0.3256(3) 0.19684(18) 0.85643(8) 0.0342(7) Uani 1 1 d . . . O2B O 0.3178(3) -0.02136(19) 0.91935(8) 0.0348(7) Uani 1 1 d . . . O3B O 0.1874(3) 0.2324(2) 0.94942(9) 0.0467(9) Uani 1 1 d . . . O4B O 0.5077(3) 0.10227(19) 1.00962(8) 0.0359(7) Uani 1 1 d . . . N1B N 0.7296(3) 0.21814(19) 0.93887(8) 0.0193(6) Uani 1 1 d . . . C1B C 0.8741(4) 0.2445(2) 0.94721(10) 0.0234(8) Uani 1 1 d . . . H7 H 0.8997 0.2689 0.9262 0.035 Uiso 1 1 calc R . . H8 H 0.9322 0.1955 0.9549 0.035 Uiso 1 1 calc R . . H9 H 0.8867 0.2866 0.9660 0.035 Uiso 1 1 calc R . . C2B C 0.7817(4) 0.0430(2) 0.93650(10) 0.0212(8) Uani 1 1 d . . . C3B C 0.7410(4) -0.0065(2) 0.96244(10) 0.0259(9) Uani 1 1 d . . . H3B H 0.6556 0.0049 0.9689 0.031 Uiso 1 1 calc R . . C4B C 0.8218(4) -0.0715(3) 0.97889(12) 0.0345(10) Uani 1 1 d . . . H4B H 0.7925 -0.1042 0.9965 0.041 Uiso 1 1 calc R . . C5B C 0.9468(4) -0.0884(3) 0.96920(12) 0.0372(11) Uani 1 1 d . . . H5B H 1.0040 -0.1323 0.9805 0.045 Uiso 1 1 calc R . . C6B C 0.9867(4) -0.0414(3) 0.94334(11) 0.0309(9) Uani 1 1 d . . . H6B H 1.0711 -0.0546 0.9366 0.037 Uiso 1 1 calc R . . C7B C 0.9076(4) 0.0257(2) 0.92638(10) 0.0236(8) Uani 1 1 d . . . C8B C 0.9612(4) 0.0723(3) 0.89783(11) 0.0321(10) Uani 1 1 d . . . H10 H 1.0606 0.0642 0.9011 0.048 Uiso 1 1 calc R . . H11 H 0.9410 0.1325 0.8991 0.048 Uiso 1 1 calc R . . H12 H 0.9166 0.0504 0.8748 0.048 Uiso 1 1 calc R . . C9B C 0.6655(4) 0.1368(2) 0.87243(10) 0.0210(8) Uani 1 1 d . . . C10B C 0.7027(4) 0.2136(2) 0.85937(10) 0.0247(8) Uani 1 1 d . . . H10B H 0.7302 0.2592 0.8750 0.030 Uiso 1 1 calc R . . C11B C 0.6997(4) 0.2241(3) 0.82351(11) 0.0311(9) Uani 1 1 d . . . H11B H 0.7272 0.2760 0.8149 0.037 Uiso 1 1 calc R . . C12B C 0.6561(4) 0.1580(3) 0.80058(11) 0.0343(10) Uani 1 1 d . . . H12B H 0.6546 0.1642 0.7762 0.041 Uiso 1 1 calc R . . C13B C 0.6153(4) 0.0835(3) 0.81332(11) 0.0328(10) Uani 1 1 d . . . H13B H 0.5829 0.0394 0.7973 0.039 Uiso 1 1 calc R . . C14B C 0.6197(4) 0.0704(3) 0.84893(10) 0.0258(8) Uani 1 1 d . . . C15B C 0.5773(5) -0.0132(3) 0.86162(12) 0.0346(10) Uani 1 1 d . . . H15D H 0.5400 -0.0489 0.8414 0.052 Uiso 1 1 calc R . . H15E H 0.5070 -0.0043 0.8757 0.052 Uiso 1 1 calc R . . H15F H 0.6572 -0.0409 0.8760 0.052 Uiso 1 1 calc R . . C16B C 0.5719(4) 0.3687(2) 0.92317(10) 0.0247(8) Uani 1 1 d . . . C17B C 0.6781(4) 0.4282(3) 0.92904(11) 0.0305(9) Uani 1 1 d . . . H17B H 0.7595 0.4169 0.9458 0.037 Uiso 1 1 calc R . . C18B C 0.6654(5) 0.5035(3) 0.91051(12) 0.0390(11) Uani 1 1 d . . . H18B H 0.7384 0.5432 0.9144 0.047 Uiso 1 1 calc R . . C19B C 0.5466(6) 0.5206(3) 0.88648(12) 0.0404(12) Uani 1 1 d . . . H19B H 0.5382 0.5720 0.8737 0.048 Uiso 1 1 calc R . . C20B C 0.4402(5) 0.4637(3) 0.88092(11) 0.0414(12) Uani 1 1 d . . . H20B H 0.3582 0.4762 0.8646 0.050 Uiso 1 1 calc R . . C21B C 0.4526(5) 0.3873(3) 0.89932(11) 0.0330(10) Uani 1 1 d . . . H21B H 0.3789 0.3482 0.8954 0.040 Uiso 1 1 calc R . . C22B C 0.6295(4) 0.3028(2) 0.99240(10) 0.0232(8) Uani 1 1 d . . . C23B C 0.5604(4) 0.3716(3) 1.00313(11) 0.0322(10) Uani 1 1 d . . . H23B H 0.5020 0.4051 0.9862 0.039 Uiso 1 1 calc R . . C24B C 0.5769(5) 0.3910(3) 1.03855(12) 0.0431(12) Uani 1 1 d . . . H24B H 0.5301 0.4379 1.0458 0.052 Uiso 1 1 calc R . . C25B C 0.6613(5) 0.3421(4) 1.06329(12) 0.0447(12) Uani 1 1 d . . . H25B H 0.6713 0.3552 1.0875 0.054 Uiso 1 1 calc R . . C26B C 0.7312(5) 0.2743(3) 1.05300(11) 0.0436(12) Uani 1 1 d . . . H26B H 0.7904 0.2416 1.0701 0.052 Uiso 1 1 calc R . . C27B C 0.7146(4) 0.2538(3) 1.01726(10) 0.0312(9) Uani 1 1 d . . . H27B H 0.7613 0.2067 1.0101 0.037 Uiso 1 1 calc R . . C28B C 0.3731(4) 0.1807(2) 0.88509(10) 0.0242(8) Uani 1 1 d . . . C29B C 0.3653(4) 0.0448(3) 0.92420(10) 0.0242(8) Uani 1 1 d . . . C30B C 0.2857(4) 0.2011(3) 0.94280(11) 0.0293(9) Uani 1 1 d . . . C31B C 0.4883(4) 0.1210(2) 0.98042(10) 0.0245(8) Uani 1 1 d . . . O5A O 0.1405(8) 0.4368(4) 0.9545(2) 0.0572(17) Uani 0.50 1 d PD A 1 C32A C 0.1611(12) 0.4197(7) 0.9915(3) 0.0572(17) Uani 0.50 1 d PD A 1 H32A H 0.1905 0.3612 0.9960 0.069 Uiso 0.50 1 calc PR A 1 H32B H 0.0750 0.4289 0.9997 0.069 Uiso 0.50 1 calc PR A 1 H32C H 0.2318 0.4575 1.0042 0.069 Uiso 0.50 1 calc PR A 1 O5B O -0.0526(6) 0.6073(5) 0.98193(17) 0.0501(15) Uani 0.50 1 d PD B 2 C32B C 0.0405(9) 0.5361(7) 0.9755(2) 0.0501(15) Uani 0.50 1 d PD B 2 H32D H 0.0453 0.4938 0.9941 0.075 Uiso 0.50 1 calc PR B 2 H32E H 0.1326 0.5582 0.9756 0.075 Uiso 0.50 1 calc PR B 2 H32F H 0.0039 0.5102 0.9527 0.075 Uiso 0.50 1 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 Cr1A 0.0173(3) 0.0203(3) 0.0209(3) 0.0020(2) 0.0009(2) -0.0026(2) P1A 0.0191(5) 0.0188(5) 0.0220(5) -0.0033(4) 0.0050(4) -0.0015(4) P2A 0.0166(5) 0.0186(5) 0.0205(5) -0.0004(4) 0.0044(4) -0.0007(4) O1A 0.052(2) 0.0333(17) 0.0266(16) 0.0046(13) 0.0074(14) -0.0077(15) O2A 0.0448(19) 0.0299(17) 0.0303(16) -0.0018(13) -0.0052(14) -0.0107(14) O3A 0.0230(16) 0.0322(18) 0.071(2) 0.0056(16) 0.0087(15) 0.0068(13) O4A 0.074(3) 0.046(2) 0.0280(18) 0.0110(15) -0.0071(16) -0.0231(18) N1A 0.0172(15) 0.0178(16) 0.0278(17) -0.0034(12) 0.0060(13) -0.0027(12) C1A 0.0171(18) 0.026(2) 0.034(2) -0.0061(17) 0.0054(16) -0.0058(16) C2A 0.031(2) 0.019(2) 0.028(2) -0.0044(15) 0.0123(17) -0.0040(16) C3A 0.047(3) 0.035(3) 0.028(2) -0.0057(18) 0.013(2) -0.004(2) C4A 0.069(4) 0.047(3) 0.033(3) -0.011(2) 0.019(3) -0.016(3) C5A 0.085(4) 0.038(3) 0.048(3) -0.015(2) 0.046(3) -0.015(3) C6A 0.046(3) 0.026(2) 0.063(3) -0.007(2) 0.035(3) -0.006(2) C7A 0.033(2) 0.021(2) 0.044(3) -0.0018(18) 0.018(2) -0.0016(17) C8A 0.032(2) 0.031(2) 0.055(3) -0.004(2) 0.019(2) 0.0001(19) C9A 0.0145(17) 0.024(2) 0.0257(19) -0.0024(15) 0.0056(15) 0.0016(15) C10A 0.0201(19) 0.028(2) 0.027(2) -0.0041(16) 0.0039(16) -0.0011(16) C11A 0.023(2) 0.039(3) 0.026(2) -0.0004(17) 0.0074(16) 0.0013(18) C12A 0.029(2) 0.040(3) 0.030(2) 0.0108(18) 0.0139(18) 0.0070(19) C13A 0.025(2) 0.026(2) 0.038(2) 0.0026(17) 0.0136(18) 0.0044(17) C14A 0.0182(18) 0.024(2) 0.032(2) -0.0024(16) 0.0094(16) -0.0001(15) C15A 0.028(2) 0.020(2) 0.039(2) -0.0052(17) 0.0054(18) -0.0015(16) C16A 0.0194(18) 0.023(2) 0.0219(19) -0.0025(15) 0.0049(15) 0.0025(15) C17A 0.029(2) 0.023(2) 0.026(2) 0.0005(16) 0.0070(16) -0.0015(16) C18A 0.044(3) 0.022(2) 0.028(2) 0.0033(16) 0.0151(19) 0.0042(18) C19A 0.036(2) 0.035(2) 0.020(2) 0.0001(17) 0.0019(17) 0.0079(19) C20A 0.028(2) 0.029(2) 0.027(2) -0.0050(17) -0.0010(17) -0.0018(17) C21A 0.026(2) 0.023(2) 0.025(2) 0.0006(15) 0.0042(16) 0.0014(16) C22A 0.0194(18) 0.0174(18) 0.0215(18) -0.0001(14) 0.0055(14) -0.0026(14) C23A 0.0212(19) 0.030(2) 0.025(2) 0.0024(16) 0.0072(16) 0.0023(16) C24A 0.028(2) 0.025(2) 0.036(2) 0.0034(17) 0.0087(18) 0.0050(17) C25A 0.036(2) 0.024(2) 0.032(2) 0.0089(17) 0.0049(18) -0.0005(18) C26A 0.037(2) 0.027(2) 0.028(2) 0.0064(17) 0.0149(18) -0.0018(18) C27A 0.026(2) 0.025(2) 0.029(2) -0.0014(16) 0.0129(17) -0.0022(16) C28A 0.0223(19) 0.024(2) 0.027(2) -0.0030(16) -0.0007(16) -0.0024(16) C29A 0.024(2) 0.026(2) 0.026(2) 0.0074(16) 0.0002(16) -0.0008(16) C30A 0.024(2) 0.022(2) 0.038(2) 0.0073(17) 0.0013(17) -0.0056(17) C31A 0.035(2) 0.028(2) 0.028(2) 0.0013(18) -0.0035(18) -0.0111(18) Cr1B 0.0130(3) 0.0242(3) 0.0218(3) 0.0033(2) 0.0032(2) -0.0008(2) P1B 0.0149(4) 0.0206(5) 0.0204(5) 0.0022(4) 0.0037(4) -0.0010(4) P2B 0.0166(5) 0.0221(5) 0.0190(5) 0.0014(4) 0.0036(4) 0.0002(4) O1B 0.0344(16) 0.0338(17) 0.0298(16) 0.0065(13) -0.0052(13) -0.0010(13) O2B 0.0303(16) 0.0347(18) 0.0375(17) 0.0046(13) 0.0016(13) -0.0090(14) O3B 0.0209(16) 0.058(2) 0.064(2) -0.0001(18) 0.0163(15) 0.0075(15) O4B 0.0360(17) 0.0460(19) 0.0267(16) 0.0097(13) 0.0086(13) -0.0051(14) N1B 0.0152(15) 0.0213(16) 0.0220(16) 0.0003(12) 0.0051(12) -0.0028(12) C1B 0.0186(19) 0.025(2) 0.026(2) 0.0015(15) 0.0032(15) -0.0048(15) C2B 0.0146(17) 0.024(2) 0.0242(19) 0.0024(15) 0.0017(14) -0.0002(15) C3B 0.022(2) 0.027(2) 0.030(2) 0.0077(16) 0.0097(16) -0.0019(16) C4B 0.031(2) 0.037(2) 0.038(2) 0.0141(19) 0.0109(19) 0.0047(19) C5B 0.027(2) 0.037(3) 0.046(3) 0.016(2) 0.004(2) 0.0090(19) C6B 0.020(2) 0.036(2) 0.038(2) 0.0032(18) 0.0094(17) 0.0047(17) C7B 0.0179(18) 0.027(2) 0.026(2) -0.0005(16) 0.0055(15) 0.0024(15) C8B 0.022(2) 0.045(3) 0.031(2) 0.0065(19) 0.0089(17) 0.0028(18) C9B 0.0150(17) 0.025(2) 0.0223(18) 0.0030(15) 0.0027(14) 0.0035(15) C10B 0.023(2) 0.025(2) 0.025(2) 0.0015(16) 0.0035(16) 0.0016(16) C11B 0.028(2) 0.040(3) 0.026(2) 0.0089(18) 0.0069(17) 0.0029(19) C12B 0.033(2) 0.047(3) 0.022(2) 0.0017(19) 0.0030(17) 0.006(2) C13B 0.028(2) 0.039(3) 0.029(2) -0.0075(18) -0.0009(17) 0.0093(19) C14B 0.0198(19) 0.032(2) 0.026(2) -0.0024(16) 0.0032(16) 0.0069(16) C15B 0.034(2) 0.030(2) 0.038(2) -0.0073(19) 0.0041(19) -0.0050(19) C16B 0.030(2) 0.025(2) 0.0214(19) 0.0018(15) 0.0105(16) 0.0043(16) C17B 0.029(2) 0.027(2) 0.038(2) 0.0022(18) 0.0127(18) 0.0009(17) C18B 0.055(3) 0.026(2) 0.044(3) -0.0018(19) 0.029(2) 0.002(2) C19B 0.070(3) 0.026(2) 0.031(2) 0.0047(18) 0.024(2) 0.010(2) C20B 0.059(3) 0.037(3) 0.025(2) -0.0002(19) 0.000(2) 0.013(2) C21B 0.042(3) 0.028(2) 0.026(2) 0.0012(17) -0.0016(19) 0.0059(19) C22B 0.0185(18) 0.031(2) 0.0203(18) 0.0005(15) 0.0051(14) -0.0043(16) C23B 0.037(2) 0.039(3) 0.023(2) -0.0043(17) 0.0118(18) -0.0007(19) C24B 0.044(3) 0.056(3) 0.033(3) -0.012(2) 0.018(2) -0.003(2) C25B 0.038(3) 0.075(4) 0.023(2) -0.011(2) 0.010(2) -0.013(3) C26B 0.033(2) 0.072(4) 0.024(2) 0.004(2) 0.0000(19) -0.005(2) C27B 0.026(2) 0.043(3) 0.023(2) 0.0008(18) 0.0019(17) -0.0022(19) C28B 0.0180(18) 0.027(2) 0.027(2) 0.0019(16) 0.0037(16) -0.0014(16) C29B 0.0159(18) 0.030(2) 0.025(2) 0.0048(16) 0.0018(15) -0.0027(16) C30B 0.024(2) 0.032(2) 0.031(2) 0.0014(17) 0.0035(17) -0.0042(17) C31B 0.0167(18) 0.028(2) 0.029(2) 0.0008(16) 0.0048(16) -0.0037(15) O5A 0.064(4) 0.037(3) 0.078(5) -0.016(3) 0.034(4) -0.010(3) C32A 0.064(4) 0.037(3) 0.078(5) -0.016(3) 0.034(4) -0.010(3) O5B 0.035(3) 0.074(4) 0.033(3) -0.011(3) -0.013(2) -0.032(3) C32B 0.035(3) 0.074(4) 0.033(3) -0.011(3) -0.013(2) -0.032(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1A C30A 1.849(4) . ? Cr1A C29A 1.868(4) . ? Cr1A C31A 1.881(4) . ? Cr1A C28A 1.885(4) . ? Cr1A P2A 2.3405(11) . ? Cr1A P1A 2.3756(11) . ? P1A N1A 1.707(3) . ? P1A C9A 1.829(4) . ? P1A C2A 1.842(4) . ? P1A P2A 2.6332(13) . ? P2A N1A 1.704(3) . ? P2A C22A 1.815(4) . ? P2A C16A 1.822(4) . ? O1A C28A 1.156(5) . ? O2A C29A 1.150(5) . ? O3A C30A 1.164(5) . ? O4A C31A 1.154(5) . ? N1A C1A 1.466(5) . ? C1A H1 0.9800 . ? C1A H2 0.9800 . ? C1A H3 0.9800 . ? C2A C3A 1.399(6) . ? C2A C7A 1.416(6) . ? C3A C4A 1.382(6) . ? C3A H3A 0.9500 . ? C4A C5A 1.384(8) . ? C4A H4A 0.9500 . ? C5A C6A 1.384(8) . ? C5A H5A 0.9500 . ? C6A C7A 1.408(6) . ? C6A H6A 0.9500 . ? C7A C8A 1.495(6) . ? C8A H4 0.9800 . ? C8A H5 0.9800 . ? C8A H6 0.9800 . ? C9A C10A 1.395(5) . ? C9A C14A 1.413(5) . ? C10A C11A 1.389(6) . ? C10A H10A 0.9500 . ? C11A C12A 1.396(6) . ? C11A H11A 0.9500 . ? C12A C13A 1.373(6) . ? C12A H12A 0.9500 . ? C13A C14A 1.389(6) . ? C13A H13A 0.9500 . ? C14A C15A 1.518(5) . ? C15A H15A 0.9800 . ? C15A H15B 0.9800 . ? C15A H15C 0.9800 . ? C16A C21A 1.394(5) . ? C16A C17A 1.406(5) . ? C17A C18A 1.385(5) . ? C17A H17A 0.9500 . ? C18A C19A 1.382(6) . ? C18A H18A 0.9500 . ? C19A C20A 1.381(6) . ? C19A H19A 0.9500 . ? C20A C21A 1.390(5) . ? C20A H20A 0.9500 . ? C21A H21A 0.9500 . ? C22A C23A 1.397(5) . ? C22A C27A 1.399(5) . ? C23A C24A 1.390(5) . ? C23A H23A 0.9500 . ? C24A C25A 1.394(6) . ? C24A H24A 0.9500 . ? C25A C26A 1.371(6) . ? C25A H25A 0.9500 . ? C26A C27A 1.392(5) . ? C26A H26A 0.9500 . ? C27A H27A 0.9500 . ? Cr1B C30B 1.842(4) . ? Cr1B C29B 1.869(4) . ? Cr1B C31B 1.888(4) . ? Cr1B C28B 1.891(4) . ? Cr1B P2B 2.3429(11) . ? Cr1B P1B 2.3753(11) . ? P1B N1B 1.709(3) . ? P1B C9B 1.830(4) . ? P1B C2B 1.839(4) . ? P1B P2B 2.6394(14) . ? P2B N1B 1.697(3) . ? P2B C22B 1.825(4) . ? P2B C16B 1.831(4) . ? O1B C28B 1.148(5) . ? O2B C29B 1.152(5) . ? O3B C30B 1.169(5) . ? O4B C31B 1.151(5) . ? N1B C1B 1.470(5) . ? C1B H7 0.9800 . ? C1B H8 0.9800 . ? C1B H9 0.9800 . ? C2B C3B 1.398(5) . ? C2B C7B 1.412(5) . ? C3B C4B 1.384(6) . ? C3B H3B 0.9500 . ? C4B C5B 1.394(6) . ? C4B H4B 0.9500 . ? C5B C6B 1.372(6) . ? C5B H5B 0.9500 . ? C6B C7B 1.408(6) . ? C6B H6B 0.9500 . ? C7B C8B 1.514(5) . ? C8B H10 0.9800 . ? C8B H11 0.9800 . ? C8B H12 0.9800 . ? C9B C10B 1.398(5) . ? C9B C14B 1.410(5) . ? C10B C11B 1.397(5) . ? C10B H10B 0.9500 . ? C11B C12B 1.389(6) . ? C11B H11B 0.9500 . ? C12B C13B 1.374(6) . ? C12B H12B 0.9500 . ? C13B C14B 1.390(6) . ? C13B H13B 0.9500 . ? C14B C15B 1.505(6) . ? C15B H15D 0.9800 . ? C15B H15E 0.9800 . ? C15B H15F 0.9800 . ? C16B C21B 1.385(6) . ? C16B C17B 1.402(6) . ? C17B C18B 1.388(6) . ? C17B H17B 0.9500 . ? C18B C19B 1.380(7) . ? C18B H18B 0.9500 . ? C19B C20B 1.376(7) . ? C19B H19B 0.9500 . ? C20B C21B 1.400(6) . ? C20B H20B 0.9500 . ? C21B H21B 0.9500 . ? C22B C27B 1.390(6) . ? C22B C23B 1.397(6) . ? C23B C24B 1.387(6) . ? C23B H23B 0.9500 . ? C24B C25B 1.382(7) . ? C24B H24B 0.9500 . ? C25B C26B 1.384(7) . ? C25B H25B 0.9500 . ? C26B C27B 1.402(6) . ? C26B H26B 0.9500 . ? C27B H27B 0.9500 . ? O5A C32A 1.436(11) . ? C32A H32A 0.9800 . ? C32A H32B 0.9800 . ? C32A H32C 0.9800 . ? O5B C32B 1.513(11) . ? C32B H32D 0.9800 . ? C32B H32E 0.9800 . ? C32B H32F 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 C30A Cr1A C29A 98.47(18) . . ? C30A Cr1A C31A 88.39(19) . . ? C29A Cr1A C31A 86.35(17) . . ? C30A Cr1A C28A 87.18(18) . . ? C29A Cr1A C28A 87.48(17) . . ? C31A Cr1A C28A 171.80(18) . . ? C30A Cr1A P2A 94.14(13) . . ? C29A Cr1A P2A 165.69(13) . . ? C31A Cr1A P2A 87.29(13) . . ? C28A Cr1A P2A 99.92(12) . . ? C30A Cr1A P1A 161.52(13) . . ? C29A Cr1A P1A 99.90(13) . . ? C31A Cr1A P1A 94.72(14) . . ? C28A Cr1A P1A 91.66(12) . . ? P2A Cr1A P1A 67.88(4) . . ? N1A P1A C9A 107.72(17) . . ? N1A P1A C2A 105.80(16) . . ? C9A P1A C2A 105.20(17) . . ? N1A P1A Cr1A 93.84(11) . . ? C9A P1A Cr1A 115.46(12) . . ? C2A P1A Cr1A 126.42(14) . . ? C9A P1A P2A 113.76(12) . . ? C2A P1A P2A 133.66(13) . . ? Cr1A P1A P2A 55.43(3) . . ? N1A P2A C22A 106.48(16) . . ? N1A P2A C16A 106.29(16) . . ? C22A P2A C16A 103.94(17) . . ? N1A P2A Cr1A 95.18(11) . . ? C22A P2A Cr1A 115.76(12) . . ? C16A P2A Cr1A 126.83(13) . . ? C22A P2A P1A 128.36(12) . . ? C16A P2A P1A 120.47(13) . . ? Cr1A P2A P1A 56.70(3) . . ? C1A N1A P2A 127.0(3) . . ? C1A N1A P1A 131.7(3) . . ? P2A N1A P1A 101.08(16) . . ? N1A C1A H1 109.5 . . ? N1A C1A H2 109.5 . . ? H1 C1A H2 109.5 . . ? N1A C1A H3 109.5 . . ? H1 C1A H3 109.5 . . ? H2 C1A H3 109.5 . . ? C3A C2A C7A 119.8(4) . . ? C3A C2A P1A 114.8(3) . . ? C7A C2A P1A 125.4(3) . . ? C4A C3A C2A 121.4(5) . . ? C4A C3A H3A 119.3 . . ? C2A C3A H3A 119.3 . . ? C3A C4A C5A 119.6(5) . . ? C3A C4A H4A 120.2 . . ? C5A C4A H4A 120.2 . . ? C4A C5A C6A 119.8(4) . . ? C4A C5A H5A 120.1 . . ? C6A C5A H5A 120.1 . . ? C5A C6A C7A 122.3(5) . . ? C5A C6A H6A 118.8 . . ? C7A C6A H6A 118.8 . . ? C6A C7A C2A 117.1(4) . . ? C6A C7A C8A 117.4(4) . . ? C2A C7A C8A 125.4(4) . . ? C7A C8A H4 109.5 . . ? C7A C8A H5 109.5 . . ? H4 C8A H5 109.5 . . ? C7A C8A H6 109.5 . . ? H4 C8A H6 109.5 . . ? H5 C8A H6 109.5 . . ? C10A C9A C14A 119.0(4) . . ? C10A C9A P1A 120.4(3) . . ? C14A C9A P1A 120.4(3) . . ? C11A C10A C9A 121.7(4) . . ? C11A C10A H10A 119.2 . . ? C9A C10A H10A 119.2 . . ? C10A C11A C12A 118.7(4) . . ? C10A C11A H11A 120.6 . . ? C12A C11A H11A 120.6 . . ? C13A C12A C11A 119.9(4) . . ? C13A C12A H12A 120.0 . . ? C11A C12A H12A 120.0 . . ? C12A C13A C14A 122.2(4) . . ? C12A C13A H13A 118.9 . . ? C14A C13A H13A 118.9 . . ? C13A C14A C9A 118.3(4) . . ? C13A C14A C15A 120.1(4) . . ? C9A C14A C15A 121.6(4) . . ? C14A C15A H15A 109.5 . . ? C14A C15A H15B 109.5 . . ? H15A C15A H15B 109.5 . . ? C14A C15A H15C 109.5 . . ? H15A C15A H15C 109.5 . . ? H15B C15A H15C 109.5 . . ? C21A C16A C17A 119.1(3) . . ? C21A C16A P2A 121.4(3) . . ? C17A C16A P2A 119.3(3) . . ? C18A C17A C16A 120.1(4) . . ? C18A C17A H17A 119.9 . . ? C16A C17A H17A 119.9 . . ? C19A C18A C17A 120.1(4) . . ? C19A C18A H18A 120.0 . . ? C17A C18A H18A 120.0 . . ? C20A C19A C18A 120.4(4) . . ? C20A C19A H19A 119.8 . . ? C18A C19A H19A 119.8 . . ? C19A C20A C21A 120.2(4) . . ? C19A C20A H20A 119.9 . . ? C21A C20A H20A 119.9 . . ? C20A C21A C16A 120.0(4) . . ? C20A C21A H21A 120.0 . . ? C16A C21A H21A 120.0 . . ? C23A C22A C27A 119.0(3) . . ? C23A C22A P2A 119.4(3) . . ? C27A C22A P2A 120.1(3) . . ? C24A C23A C22A 120.5(4) . . ? C24A C23A H23A 119.7 . . ? C22A C23A H23A 119.7 . . ? C23A C24A C25A 119.5(4) . . ? C23A C24A H24A 120.3 . . ? C25A C24A H24A 120.3 . . ? C26A C25A C24A 120.6(4) . . ? C26A C25A H25A 119.7 . . ? C24A C25A H25A 119.7 . . ? C25A C26A C27A 120.3(4) . . ? C25A C26A H26A 119.9 . . ? C27A C26A H26A 119.9 . . ? C26A C27A C22A 120.1(4) . . ? C26A C27A H27A 120.0 . . ? C22A C27A H27A 120.0 . . ? O1A C28A Cr1A 174.8(4) . . ? O2A C29A Cr1A 178.2(4) . . ? O3A C30A Cr1A 177.5(4) . . ? O4A C31A Cr1A 175.9(4) . . ? C30B Cr1B C29B 95.40(18) . . ? C30B Cr1B C31B 87.43(17) . . ? C29B Cr1B C31B 86.85(17) . . ? C30B Cr1B C28B 87.40(17) . . ? C29B Cr1B C28B 89.58(17) . . ? C31B Cr1B C28B 173.42(16) . . ? C30B Cr1B P2B 97.48(13) . . ? C29B Cr1B P2B 165.65(12) . . ? C31B Cr1B P2B 87.43(12) . . ? C28B Cr1B P2B 97.29(12) . . ? C30B Cr1B P1B 164.67(13) . . ? C29B Cr1B P1B 99.59(12) . . ? C31B Cr1B P1B 96.52(12) . . ? C28B Cr1B P1B 89.52(12) . . ? P2B Cr1B P1B 68.03(4) . . ? N1B P1B C9B 106.79(16) . . ? N1B P1B C2B 105.93(16) . . ? C9B P1B C2B 106.20(17) . . ? N1B P1B Cr1B 93.76(11) . . ? C9B P1B Cr1B 114.27(12) . . ? C2B P1B Cr1B 127.10(12) . . ? C9B P1B P2B 113.37(13) . . ? C2B P1B P2B 132.88(13) . . ? Cr1B P1B P2B 55.40(3) . . ? N1B P2B C22B 106.21(16) . . ? N1B P2B C16B 108.12(16) . . ? C22B P2B C16B 101.69(18) . . ? N1B P2B Cr1B 95.25(11) . . ? C22B P2B Cr1B 118.36(13) . . ? C16B P2B Cr1B 125.39(14) . . ? C22B P2B P1B 128.49(13) . . ? C16B P2B P1B 122.59(12) . . ? Cr1B P2B P1B 56.57(3) . . ? C1B N1B P2B 129.7(3) . . ? C1B N1B P1B 128.8(3) . . ? P2B N1B P1B 101.58(15) . . ? N1B C1B H7 109.5 . . ? N1B C1B H8 109.5 . . ? H7 C1B H8 109.5 . . ? N1B C1B H9 109.5 . . ? H7 C1B H9 109.5 . . ? H8 C1B H9 109.5 . . ? C3B C2B C7B 119.4(3) . . ? C3B C2B P1B 114.3(3) . . ? C7B C2B P1B 126.3(3) . . ? C4B C3B C2B 121.8(4) . . ? C4B C3B H3B 119.1 . . ? C2B C3B H3B 119.1 . . ? C3B C4B C5B 119.1(4) . . ? C3B C4B H4B 120.5 . . ? C5B C4B H4B 120.5 . . ? C6B C5B C4B 119.7(4) . . ? C6B C5B H5B 120.1 . . ? C4B C5B H5B 120.1 . . ? C5B C6B C7B 122.6(4) . . ? C5B C6B H6B 118.7 . . ? C7B C6B H6B 118.7 . . ? C6B C7B C2B 117.4(3) . . ? C6B C7B C8B 117.9(3) . . ? C2B C7B C8B 124.7(3) . . ? C7B C8B H10 109.5 . . ? C7B C8B H11 109.5 . . ? H10 C8B H11 109.5 . . ? C7B C8B H12 109.5 . . ? H10 C8B H12 109.5 . . ? H11 C8B H12 109.5 . . ? C10B C9B C14B 119.5(4) . . ? C10B C9B P1B 119.4(3) . . ? C14B C9B P1B 120.8(3) . . ? C11B C10B C9B 120.7(4) . . ? C11B C10B H10B 119.6 . . ? C9B C10B H10B 119.6 . . ? C12B C11B C10B 119.4(4) . . ? C12B C11B H11B 120.3 . . ? C10B C11B H11B 120.3 . . ? C13B C12B C11B 119.8(4) . . ? C13B C12B H12B 120.1 . . ? C11B C12B H12B 120.1 . . ? C12B C13B C14B 122.2(4) . . ? C12B C13B H13B 118.9 . . ? C14B C13B H13B 118.9 . . ? C13B C14B C9B 118.3(4) . . ? C13B C14B C15B 120.1(4) . . ? C9B C14B C15B 121.6(4) . . ? C14B C15B H15D 109.5 . . ? C14B C15B H15E 109.5 . . ? H15D C15B H15E 109.5 . . ? C14B C15B H15F 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? C21B C16B C17B 118.9(4) . . ? C21B C16B P2B 119.9(3) . . ? C17B C16B P2B 121.2(3) . . ? C18B C17B C16B 120.5(4) . . ? C18B C17B H17B 119.8 . . ? C16B C17B H17B 119.8 . . ? C19B C18B C17B 119.9(5) . . ? C19B C18B H18B 120.1 . . ? C17B C18B H18B 120.1 . . ? C20B C19B C18B 120.4(4) . . ? C20B C19B H19B 119.8 . . ? C18B C19B H19B 119.8 . . ? C19B C20B C21B 120.1(4) . . ? C19B C20B H20B 119.9 . . ? C21B C20B H20B 119.9 . . ? C16B C21B C20B 120.2(4) . . ? C16B C21B H21B 119.9 . . ? C20B C21B H21B 119.9 . . ? C27B C22B C23B 119.9(4) . . ? C27B C22B P2B 119.7(3) . . ? C23B C22B P2B 119.7(3) . . ? C24B C23B C22B 120.0(4) . . ? C24B C23B H23B 120.0 . . ? C22B C23B H23B 120.0 . . ? C25B C24B C23B 120.1(5) . . ? C25B C24B H24B 120.0 . . ? C23B C24B H24B 120.0 . . ? C24B C25B C26B 120.5(4) . . ? C24B C25B H25B 119.8 . . ? C26B C25B H25B 119.8 . . ? C25B C26B C27B 119.9(4) . . ? C25B C26B H26B 120.0 . . ? C27B C26B H26B 120.0 . . ? C22B C27B C26B 119.6(4) . . ? C22B C27B H27B 120.2 . . ? C26B C27B H27B 120.2 . . ? O1B C28B Cr1B 176.7(3) . . ? O2B C29B Cr1B 179.2(4) . . ? O3B C30B Cr1B 179.5(4) . . ? O4B C31B Cr1B 175.4(3) . . ? O5B C32B H32D 109.5 . . ? O5B C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? O5B C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 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 C30A Cr1A P1A N1A 23.3(4) . . . . ? C29A Cr1A P1A N1A -162.88(16) . . . . ? C31A Cr1A P1A N1A -75.77(17) . . . . ? C28A Cr1A P1A N1A 109.39(16) . . . . ? P2A Cr1A P1A N1A 9.36(11) . . . . ? C30A Cr1A P1A C9A -88.4(4) . . . . ? C29A Cr1A P1A C9A 85.41(18) . . . . ? C31A Cr1A P1A C9A 172.52(19) . . . . ? C28A Cr1A P1A C9A -2.32(18) . . . . ? P2A Cr1A P1A C9A -102.35(14) . . . . ? C30A Cr1A P1A C2A 136.2(4) . . . . ? C29A Cr1A P1A C2A -50.0(2) . . . . ? C31A Cr1A P1A C2A 37.1(2) . . . . ? C28A Cr1A P1A C2A -137.73(19) . . . . ? P2A Cr1A P1A C2A 122.24(16) . . . . ? C30A Cr1A P1A P2A 14.0(4) . . . . ? C29A Cr1A P1A P2A -172.24(12) . . . . ? C31A Cr1A P1A P2A -85.13(13) . . . . ? C28A Cr1A P1A P2A 100.03(12) . . . . ? C30A Cr1A P2A N1A 175.00(17) . . . . ? C29A Cr1A P2A N1A 23.2(5) . . . . ? C31A Cr1A P2A N1A 86.81(18) . . . . ? C28A Cr1A P2A N1A -97.14(16) . . . . ? P1A Cr1A P2A N1A -9.40(11) . . . . ? C30A Cr1A P2A C22A 63.89(18) . . . . ? C29A Cr1A P2A C22A -87.9(5) . . . . ? C31A Cr1A P2A C22A -24.3(2) . . . . ? C28A Cr1A P2A C22A 151.75(18) . . . . ? P1A Cr1A P2A C22A -120.50(13) . . . . ? C30A Cr1A P2A C16A -70.2(2) . . . . ? C29A Cr1A P2A C16A 138.0(5) . . . . ? C31A Cr1A P2A C16A -158.4(2) . . . . ? C28A Cr1A P2A C16A 17.7(2) . . . . ? P1A Cr1A P2A C16A 105.42(16) . . . . ? C30A Cr1A P2A P1A -175.60(13) . . . . ? C29A Cr1A P2A P1A 32.6(5) . . . . ? C31A Cr1A P2A P1A 96.21(14) . . . . ? C28A Cr1A P2A P1A -87.75(13) . . . . ? C9A P1A P2A N1A -89.3(2) . . . . ? C2A P1A P2A N1A 55.4(2) . . . . ? Cr1A P1A P2A N1A 165.19(17) . . . . ? N1A P1A P2A C22A -67.0(2) . . . . ? C9A P1A P2A C22A -156.3(2) . . . . ? C2A P1A P2A C22A -11.6(3) . . . . ? Cr1A P1A P2A C22A 98.23(16) . . . . ? N1A P1A P2A C16A 78.3(2) . . . . ? C9A P1A P2A C16A -11.0(2) . . . . ? C2A P1A P2A C16A 133.7(2) . . . . ? Cr1A P1A P2A C16A -116.47(15) . . . . ? N1A P1A P2A Cr1A -165.19(17) . . . . ? C9A P1A P2A Cr1A 105.49(13) . . . . ? C2A P1A P2A Cr1A -109.82(19) . . . . ? C22A P2A N1A C1A -54.0(4) . . . . ? C16A P2A N1A C1A 56.4(4) . . . . ? Cr1A P2A N1A C1A -172.8(3) . . . . ? P1A P2A N1A C1A 174.8(4) . . . . ? C22A P2A N1A P1A 131.20(17) . . . . ? C16A P2A N1A P1A -118.42(18) . . . . ? Cr1A P2A N1A P1A 12.39(15) . . . . ? C9A P1A N1A C1A -68.3(4) . . . . ? C2A P1A N1A C1A 43.8(4) . . . . ? Cr1A P1A N1A C1A 173.4(3) . . . . ? P2A P1A N1A C1A -174.5(4) . . . . ? C9A P1A N1A P2A 106.10(18) . . . . ? C2A P1A N1A P2A -141.78(18) . . . . ? Cr1A P1A N1A P2A -12.18(14) . . . . ? N1A P1A C2A C3A 105.2(3) . . . . ? C9A P1A C2A C3A -140.9(3) . . . . ? Cr1A P1A C2A C3A -1.9(4) . . . . ? P2A P1A C2A C3A 72.4(4) . . . . ? N1A P1A C2A C7A -76.0(4) . . . . ? C9A P1A C2A C7A 37.8(4) . . . . ? Cr1A P1A C2A C7A 176.8(3) . . . . ? P2A P1A C2A C7A -108.9(3) . . . . ? C7A C2A C3A C4A 1.4(6) . . . . ? P1A C2A C3A C4A -179.8(4) . . . . ? C2A C3A C4A C5A -0.1(7) . . . . ? C3A C4A C5A C6A -0.5(7) . . . . ? C4A C5A C6A C7A -0.1(7) . . . . ? C5A C6A C7A C2A 1.4(6) . . . . ? C5A C6A C7A C8A -175.4(4) . . . . ? C3A C2A C7A C6A -2.0(6) . . . . ? P1A C2A C7A C6A 179.4(3) . . . . ? C3A C2A C7A C8A 174.5(4) . . . . ? P1A C2A C7A C8A -4.2(6) . . . . ? N1A P1A C9A C10A -7.0(3) . . . . ? C2A P1A C9A C10A -119.5(3) . . . . ? Cr1A P1A C9A C10A 96.3(3) . . . . ? P2A P1A C9A C10A 34.8(3) . . . . ? N1A P1A C9A C14A 177.6(3) . . . . ? C2A P1A C9A C14A 65.1(3) . . . . ? Cr1A P1A C9A C14A -79.1(3) . . . . ? P2A P1A C9A C14A -140.6(3) . . . . ? C14A C9A C10A C11A -3.4(6) . . . . ? P1A C9A C10A C11A -178.8(3) . . . . ? C9A C10A C11A C12A 1.0(6) . . . . ? C10A C11A C12A C13A 1.5(6) . . . . ? C11A C12A C13A C14A -1.6(6) . . . . ? C12A C13A C14A C9A -0.8(6) . . . . ? C12A C13A C14A C15A 177.5(4) . . . . ? C10A C9A C14A C13A 3.2(5) . . . . ? P1A C9A C14A C13A 178.7(3) . . . . ? C10A C9A C14A C15A -175.0(3) . . . . ? P1A C9A C14A C15A 0.4(5) . . . . ? N1A P2A C16A C21A -69.4(3) . . . . ? C22A P2A C16A C21A 42.8(3) . . . . ? Cr1A P2A C16A C21A -179.0(2) . . . . ? P1A P2A C16A C21A -109.9(3) . . . . ? N1A P2A C16A C17A 105.2(3) . . . . ? C22A P2A C16A C17A -142.6(3) . . . . ? Cr1A P2A C16A C17A -4.4(4) . . . . ? P1A P2A C16A C17A 64.8(3) . . . . ? C21A C16A C17A C18A 1.4(6) . . . . ? P2A C16A C17A C18A -173.3(3) . . . . ? C16A C17A C18A C19A -1.3(6) . . . . ? C17A C18A C19A C20A 0.6(6) . . . . ? C18A C19A C20A C21A 0.0(6) . . . . ? C19A C20A C21A C16A 0.1(6) . . . . ? C17A C16A C21A C20A -0.8(6) . . . . ? P2A C16A C21A C20A 173.8(3) . . . . ? N1A P2A C22A C23A 161.5(3) . . . . ? C16A P2A C22A C23A 49.5(3) . . . . ? Cr1A P2A C22A C23A -94.2(3) . . . . ? P1A P2A C22A C23A -160.9(2) . . . . ? N1A P2A C22A C27A -32.4(3) . . . . ? C16A P2A C22A C27A -144.4(3) . . . . ? Cr1A P2A C22A C27A 71.9(3) . . . . ? P1A P2A C22A C27A 5.2(4) . . . . ? C27A C22A C23A C24A -0.7(6) . . . . ? P2A C22A C23A C24A 165.5(3) . . . . ? C22A C23A C24A C25A -0.9(6) . . . . ? C23A C24A C25A C26A 1.8(6) . . . . ? C24A C25A C26A C27A -1.0(7) . . . . ? C25A C26A C27A C22A -0.6(6) . . . . ? C23A C22A C27A C26A 1.5(6) . . . . ? P2A C22A C27A C26A -164.7(3) . . . . ? C30B Cr1B P1B N1B 27.5(5) . . . . ? C29B Cr1B P1B N1B -164.70(16) . . . . ? C31B Cr1B P1B N1B -76.81(16) . . . . ? C28B Cr1B P1B N1B 105.81(16) . . . . ? P2B Cr1B P1B N1B 7.74(10) . . . . ? C30B Cr1B P1B C9B -82.8(5) . . . . ? C29B Cr1B P1B C9B 84.98(18) . . . . ? C31B Cr1B P1B C9B 172.87(18) . . . . ? C28B Cr1B P1B C9B -4.51(18) . . . . ? P2B Cr1B P1B C9B -102.57(14) . . . . ? C30B Cr1B P1B C2B 140.7(5) . . . . ? C29B Cr1B P1B C2B -51.5(2) . . . . ? C31B Cr1B P1B C2B 36.4(2) . . . . ? C28B Cr1B P1B C2B -141.0(2) . . . . ? P2B Cr1B P1B C2B 120.98(16) . . . . ? C30B Cr1B P1B P2B 19.7(5) . . . . ? C29B Cr1B P1B P2B -172.45(12) . . . . ? C31B Cr1B P1B P2B -84.56(12) . . . . ? C28B Cr1B P1B P2B 98.06(12) . . . . ? C30B Cr1B P2B N1B 177.35(17) . . . . ? C29B Cr1B P2B N1B 23.7(5) . . . . ? C31B Cr1B P2B N1B 90.27(16) . . . . ? C28B Cr1B P2B N1B -94.33(16) . . . . ? P1B Cr1B P2B N1B -7.82(11) . . . . ? C30B Cr1B P2B C22B 65.7(2) . . . . ? C29B Cr1B P2B C22B -87.9(5) . . . . ? C31B Cr1B P2B C22B -21.32(19) . . . . ? C28B Cr1B P2B C22B 154.07(19) . . . . ? P1B Cr1B P2B C22B -119.42(15) . . . . ? C30B Cr1B P2B C16B -66.0(2) . . . . ? C29B Cr1B P2B C16B 140.4(5) . . . . ? C31B Cr1B P2B C16B -153.08(19) . . . . ? C28B Cr1B P2B C16B 22.31(19) . . . . ? P1B Cr1B P2B C16B 108.82(15) . . . . ? C30B Cr1B P2B P1B -174.84(13) . . . . ? C29B Cr1B P2B P1B 31.5(5) . . . . ? C31B Cr1B P2B P1B 98.09(12) . . . . ? C28B Cr1B P2B P1B -86.51(12) . . . . ? C9B P1B P2B N1B -88.1(2) . . . . ? C2B P1B P2B N1B 56.6(2) . . . . ? Cr1B P1B P2B N1B 167.67(17) . . . . ? N1B P1B P2B C22B -66.0(2) . . . . ? C9B P1B P2B C22B -154.1(2) . . . . ? C2B P1B P2B C22B -9.4(2) . . . . ? Cr1B P1B P2B C22B 101.67(16) . . . . ? N1B P1B P2B C16B 78.6(2) . . . . ? C9B P1B P2B C16B -9.5(2) . . . . ? C2B P1B P2B C16B 135.2(2) . . . . ? Cr1B P1B P2B C16B -113.68(16) . . . . ? N1B P1B P2B Cr1B -167.67(16) . . . . ? C9B P1B P2B Cr1B 104.23(13) . . . . ? C2B P1B P2B Cr1B -111.07(17) . . . . ? C22B P2B N1B C1B -47.2(4) . . . . ? C16B P2B N1B C1B 61.2(4) . . . . ? Cr1B P2B N1B C1B -168.8(3) . . . . ? P1B P2B N1B C1B -179.1(4) . . . . ? C22B P2B N1B P1B 131.87(17) . . . . ? C16B P2B N1B P1B -119.64(18) . . . . ? Cr1B P2B N1B P1B 10.31(14) . . . . ? C9B P1B N1B C1B -74.3(3) . . . . ? C2B P1B N1B C1B 38.6(3) . . . . ? Cr1B P1B N1B C1B 169.0(3) . . . . ? P2B P1B N1B C1B 179.1(4) . . . . ? C9B P1B N1B P2B 106.60(17) . . . . ? C2B P1B N1B P2B -140.49(16) . . . . ? Cr1B P1B N1B P2B -10.14(14) . . . . ? N1B P1B C2B C3B 102.1(3) . . . . ? C9B P1B C2B C3B -144.6(3) . . . . ? Cr1B P1B C2B C3B -5.4(4) . . . . ? P2B P1B C2B C3B 69.0(3) . . . . ? N1B P1B C2B C7B -77.1(4) . . . . ? C9B P1B C2B C7B 36.3(4) . . . . ? Cr1B P1B C2B C7B 175.4(3) . . . . ? P2B P1B C2B C7B -110.2(3) . . . . ? C7B C2B C3B C4B 0.8(6) . . . . ? P1B C2B C3B C4B -178.4(3) . . . . ? C2B C3B C4B C5B -0.3(7) . . . . ? C3B C4B C5B C6B -0.8(7) . . . . ? C4B C5B C6B C7B 1.6(7) . . . . ? C5B C6B C7B C2B -1.1(6) . . . . ? C5B C6B C7B C8B -179.1(4) . . . . ? C3B C2B C7B C6B -0.1(6) . . . . ? P1B C2B C7B C6B 179.0(3) . . . . ? C3B C2B C7B C8B 177.8(4) . . . . ? P1B C2B C7B C8B -3.1(6) . . . . ? N1B P1B C9B C10B -8.3(3) . . . . ? C2B P1B C9B C10B -121.0(3) . . . . ? Cr1B P1B C9B C10B 93.9(3) . . . . ? P2B P1B C9B C10B 32.8(3) . . . . ? N1B P1B C9B C14B 177.8(3) . . . . ? C2B P1B C9B C14B 65.1(3) . . . . ? Cr1B P1B C9B C14B -80.0(3) . . . . ? P2B P1B C9B C14B -141.1(3) . . . . ? C14B C9B C10B C11B -2.4(6) . . . . ? P1B C9B C10B C11B -176.3(3) . . . . ? C9B C10B C11B C12B 1.6(6) . . . . ? C10B C11B C12B C13B 0.6(6) . . . . ? C11B C12B C13B C14B -2.0(6) . . . . ? C12B C13B C14B C9B 1.2(6) . . . . ? C12B C13B C14B C15B -178.4(4) . . . . ? C10B C9B C14B C13B 1.0(5) . . . . ? P1B C9B C14B C13B 174.8(3) . . . . ? C10B C9B C14B C15B -179.4(4) . . . . ? P1B C9B C14B C15B -5.6(5) . . . . ? N1B P2B C16B C21B 123.7(3) . . . . ? C22B P2B C16B C21B -124.8(3) . . . . ? Cr1B P2B C16B C21B 13.1(4) . . . . ? P1B P2B C16B C21B 82.8(3) . . . . ? N1B P2B C16B C17B -57.0(4) . . . . ? C22B P2B C16B C17B 54.6(3) . . . . ? Cr1B P2B C16B C17B -167.5(3) . . . . ? P1B P2B C16B C17B -97.8(3) . . . . ? C21B C16B C17B C18B -1.8(6) . . . . ? P2B C16B C17B C18B 178.8(3) . . . . ? C16B C17B C18B C19B 0.9(6) . . . . ? C17B C18B C19B C20B 0.4(6) . . . . ? C18B C19B C20B C21B -0.8(7) . . . . ? C17B C16B C21B C20B 1.3(6) . . . . ? P2B C16B C21B C20B -179.3(3) . . . . ? C19B C20B C21B C16B 0.0(7) . . . . ? N1B P2B C22B C27B -34.3(4) . . . . ? C16B P2B C22B C27B -147.3(3) . . . . ? Cr1B P2B C22B C27B 71.1(3) . . . . ? P1B P2B C22B C27B 2.8(4) . . . . ? N1B P2B C22B C23B 155.0(3) . . . . ? C16B P2B C22B C23B 42.0(4) . . . . ? Cr1B P2B C22B C23B -99.6(3) . . . . ? P1B P2B C22B C23B -167.8(3) . . . . ? C27B C22B C23B C24B 0.1(6) . . . . ? P2B C22B C23B C24B 170.8(3) . . . . ? C22B C23B C24B C25B -0.3(7) . . . . ? C23B C24B C25B C26B 0.8(7) . . . . ? C24B C25B C26B C27B -1.2(7) . . . . ? C23B C22B C27B C26B -0.5(6) . . . . ? P2B C22B C27B C26B -171.1(3) . . . . ? C25B C26B C27B C22B 1.0(7) . . . . ? _diffrn_measured_fraction_theta_max 0.891 _diffrn_reflns_theta_full 28.63 _diffrn_measured_fraction_theta_full 0.891 _refine_diff_density_max 1.494 _refine_diff_density_min -1.139 _refine_diff_density_rms 0.107 # Attachment '10.cif' data_twh80_0m _database_code_depnum_ccdc_archive 'CCDC 739222' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H34 Cr N2 O4 P2, 0.75(C H2 Cl2)' _chemical_formula_sum 'C34.75 H35.5 Cl1.5 Cr N2 O4 P2' _chemical_formula_weight 712.27 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' 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.8254(7) _cell_length_b 16.6151(9) _cell_length_c 20.6833(9) _cell_angle_alpha 90.00 _cell_angle_beta 121.267(3) _cell_angle_gamma 90.00 _cell_volume 3473.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 30278 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.94 _exptl_crystal_size_mid 0.85 _exptl_crystal_size_min 0.45 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.362 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1478 _exptl_absorpt_coefficient_mu 0.577 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.587 _exptl_absorpt_correction_T_max 0.771 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.366 _diffrn_detector_type 'Bruker-AXS SMART APEX' _diffrn_measurement_details 'frames, 0.3\% width' _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Bruker-AXS Kappa' _diffrn_measurement_method '\w & \f scans' _diffrn_measurement_specimen_support ; glass fibre ; _diffrn_radiation_collimation '0.5 mm double pinhole' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe X-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71074 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 40 _diffrn_source_power 2 _diffrn_source_size '0.4 x 8 mm fine focus' _diffrn_source_target Mo _diffrn_source_type 'Bruker-AXS KFF Mo 2K 90\% Ceramic' _diffrn_source_voltage 50 _diffrn_reflns_number 29582 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0274 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.52 _reflns_number_total 7919 _reflns_number_gt 6957 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'Apex II (Bruker-AXS, 2007)' _computing_data_reduction ; SAINT v7.34A (Bruker-AXS, 2007) & XPREP v2005/4 (Bruker-AXS, 2005) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Ten low angle disagreeable reflections omitted: 0 1 1, -1 1 1, 1 0 0, -1 0 2, 0 1 2, 1 1 0, 0 2 0, -1 1 2, 0 0 2 and 0 2 8. Have not modelled disorder present in CH2CH2 co-crystallised solvent as did not signficantly improve the model of the crystal structure. Instead the occupancy of this solvent molecule has been set to 75% within the asymmetric unit, this was the value given after refining the solution with a free variable. 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^)+(0.0463P)^2^+3.8846P] 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 7919 _refine_ls_number_parameters 421 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0431 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.1037 _refine_ls_wR_factor_gt 0.1004 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.006 _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 0.70125(3) 0.723508(17) 0.684910(15) 0.01270(8) Uani 1 1 d . . . P1 P 0.51166(5) 0.80355(3) 0.60444(3) 0.01368(10) Uani 1 1 d . . . P2 P 0.77300(5) 0.85095(3) 0.74704(3) 0.01407(11) Uani 1 1 d . . . O1 O 0.57554(16) 0.66790(10) 0.77386(9) 0.0319(4) Uani 1 1 d . . . O2 O 0.58727(15) 0.58071(9) 0.58157(9) 0.0284(3) Uani 1 1 d . . . O3 O 0.92930(16) 0.61844(10) 0.79178(9) 0.0333(4) Uani 1 1 d . . . O4 O 0.86960(14) 0.74327(10) 0.61507(8) 0.0268(3) Uani 1 1 d . . . N1 N 0.55116(15) 0.90043(9) 0.63770(9) 0.0158(3) Uani 1 1 d . . . N2 N 0.68849(15) 0.92301(10) 0.67754(8) 0.0153(3) Uani 1 1 d . . . C1 C 0.4651(2) 0.96921(12) 0.59986(11) 0.0219(4) Uani 1 1 d . . . H1A H 0.5015 1.0171 0.6319 0.033 Uiso 1 1 calc R . . H1B H 0.3766 0.9581 0.5908 0.033 Uiso 1 1 calc R . . H1C H 0.4593 0.9787 0.5515 0.033 Uiso 1 1 calc R . . C2 C 0.73859(19) 0.93753(12) 0.62642(11) 0.0191(4) Uani 1 1 d . . . H2A H 0.7304 0.8881 0.5984 0.029 Uiso 1 1 calc R . . H2B H 0.8318 0.9536 0.6562 0.029 Uiso 1 1 calc R . . H2C H 0.6869 0.9805 0.5907 0.029 Uiso 1 1 calc R . . C3 C 0.44013(18) 0.80991(11) 0.50119(10) 0.0161(4) Uani 1 1 d . . . C4 C 0.5256(2) 0.78477(12) 0.47700(11) 0.0200(4) Uani 1 1 d . . . H4 H 0.6072 0.7602 0.5126 0.024 Uiso 1 1 calc R . . C5 C 0.4950(2) 0.79453(13) 0.40309(11) 0.0216(4) Uani 1 1 d . . . H5 H 0.5546 0.7766 0.3883 0.026 Uiso 1 1 calc R . . C6 C 0.3768(2) 0.83070(12) 0.35124(11) 0.0215(4) Uani 1 1 d . . . H6 H 0.3561 0.8399 0.3009 0.026 Uiso 1 1 calc R . . C7 C 0.2891(2) 0.85332(12) 0.37301(11) 0.0197(4) Uani 1 1 d . . . H7 H 0.2070 0.8766 0.3364 0.024 Uiso 1 1 calc R . . C8 C 0.31671(19) 0.84316(11) 0.44737(11) 0.0171(4) Uani 1 1 d . . . C9 C 0.20793(19) 0.86654(13) 0.46121(11) 0.0216(4) Uani 1 1 d . . . H9A H 0.1748 0.9202 0.4401 0.032 Uiso 1 1 calc R . . H9B H 0.2426 0.8673 0.5157 0.032 Uiso 1 1 calc R . . H9C H 0.1356 0.8274 0.4368 0.032 Uiso 1 1 calc R . . C10 C 0.37558(18) 0.78125(12) 0.61996(10) 0.0178(4) Uani 1 1 d . . . C11 C 0.3683(2) 0.82708(14) 0.67445(11) 0.0232(4) Uani 1 1 d . . . H11 H 0.4275 0.8709 0.6979 0.028 Uiso 1 1 calc R . . C12 C 0.2763(2) 0.80978(16) 0.69470(12) 0.0300(5) Uani 1 1 d . . . H12 H 0.2721 0.8418 0.7314 0.036 Uiso 1 1 calc R . . C13 C 0.1906(2) 0.74567(16) 0.66133(13) 0.0323(5) Uani 1 1 d . . . H13 H 0.1272 0.7334 0.6749 0.039 Uiso 1 1 calc R . . C14 C 0.1981(2) 0.69970(14) 0.60822(12) 0.0276(5) Uani 1 1 d . . . H14 H 0.1391 0.6556 0.5858 0.033 Uiso 1 1 calc R . . C15 C 0.28928(19) 0.71568(12) 0.58614(11) 0.0208(4) Uani 1 1 d . . . C16 C 0.2872(2) 0.66295(13) 0.52665(12) 0.0252(4) Uani 1 1 d . . . H16A H 0.2541 0.6095 0.5286 0.038 Uiso 1 1 calc R . . H16B H 0.3770 0.6581 0.5359 0.038 Uiso 1 1 calc R . . H16C H 0.2292 0.6868 0.4767 0.038 Uiso 1 1 calc R . . C24 C 0.73281(19) 0.88005(12) 0.81851(10) 0.0188(4) Uani 1 1 d . . . C25 C 0.6429(2) 0.94197(13) 0.80430(11) 0.0228(4) Uani 1 1 d . . . H25 H 0.6044 0.9702 0.7576 0.027 Uiso 1 1 calc R . . C26 C 0.6084(2) 0.96331(15) 0.85677(13) 0.0314(5) Uani 1 1 d . . . H26 H 0.5463 1.0052 0.8458 0.038 Uiso 1 1 calc R . . C27 C 0.6657(3) 0.92289(17) 0.92521(14) 0.0379(6) Uani 1 1 d . . . H27 H 0.6422 0.9365 0.9614 0.045 Uiso 1 1 calc R . . C28 C 0.7569(3) 0.86272(15) 0.94071(12) 0.0331(5) Uani 1 1 d . . . H28 H 0.7967 0.8361 0.9882 0.040 Uiso 1 1 calc R . . C29 C 0.7924(2) 0.83970(13) 0.88844(11) 0.0241(4) Uani 1 1 d . . . C30 C 0.8941(2) 0.77460(14) 0.90974(12) 0.0293(5) Uani 1 1 d . . . H30A H 0.9292 0.7586 0.9624 0.044 Uiso 1 1 calc R . . H30B H 0.9664 0.7948 0.9041 0.044 Uiso 1 1 calc R . . H30C H 0.8530 0.7280 0.8766 0.044 Uiso 1 1 calc R . . C17 C 0.94511(18) 0.88495(11) 0.78915(10) 0.0161(4) Uani 1 1 d . . . C18 C 1.03678(19) 0.82809(12) 0.79498(11) 0.0182(4) Uani 1 1 d . . . H18 H 1.0072 0.7752 0.7762 0.022 Uiso 1 1 calc R . . C19 C 1.1699(2) 0.84654(12) 0.82740(11) 0.0207(4) Uani 1 1 d . . . H19 H 1.2305 0.8067 0.8310 0.025 Uiso 1 1 calc R . . C20 C 1.2133(2) 0.92337(13) 0.85435(12) 0.0232(4) Uani 1 1 d . . . H20 H 1.3039 0.9370 0.8761 0.028 Uiso 1 1 calc R . . C21 C 1.1242(2) 0.98028(12) 0.84947(11) 0.0222(4) Uani 1 1 d . . . H21 H 1.1553 1.0329 0.8684 0.027 Uiso 1 1 calc R . . C22 C 0.98992(19) 0.96326(12) 0.81772(11) 0.0185(4) Uani 1 1 d . . . C23 C 0.9029(2) 1.02975(12) 0.81732(13) 0.0248(4) Uani 1 1 d . . . H23A H 0.8860 1.0210 0.8584 0.037 Uiso 1 1 calc R . . H23B H 0.8188 1.0298 0.7688 0.037 Uiso 1 1 calc R . . H23C H 0.9472 1.0816 0.8245 0.037 Uiso 1 1 calc R . . C34 C 0.6193(2) 0.69240(12) 0.73980(11) 0.0211(4) Uani 1 1 d . . . C32 C 0.62804(19) 0.63585(12) 0.62102(11) 0.0195(4) Uani 1 1 d . . . C33 C 0.8426(2) 0.66050(12) 0.75272(11) 0.0219(4) Uani 1 1 d . . . C31 C 0.80185(19) 0.74086(12) 0.63984(10) 0.0184(4) Uani 1 1 d . . . Cl1 Cl 0.81118(8) 0.90529(5) 0.47882(4) 0.03644(18) Uani 0.75 1 d P . . Cl2 Cl 1.04362(8) 0.96702(5) 0.61391(5) 0.03872(19) Uani 0.75 1 d P . . C35 C 0.9804(3) 0.8972(2) 0.54050(19) 0.0369(7) Uani 0.75 1 d P . . H35A H 1.0253 0.9044 0.5117 0.044 Uiso 0.75 1 calc PR . . H35B H 1.0009 0.8424 0.5623 0.044 Uiso 0.75 1 calc PR . . 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 0.01107(14) 0.01417(15) 0.01100(14) 0.00079(10) 0.00442(11) 0.00061(10) P1 0.0122(2) 0.0165(2) 0.0121(2) 0.00101(17) 0.00611(18) 0.00053(17) P2 0.0131(2) 0.0155(2) 0.0125(2) 0.00027(17) 0.00584(18) 0.00007(17) O1 0.0337(9) 0.0402(9) 0.0283(8) 0.0082(7) 0.0207(7) 0.0008(7) O2 0.0233(8) 0.0224(8) 0.0322(8) -0.0069(6) 0.0091(7) 0.0003(6) O3 0.0254(8) 0.0288(8) 0.0296(8) 0.0057(7) 0.0029(7) 0.0072(7) O4 0.0188(7) 0.0393(9) 0.0243(7) -0.0037(6) 0.0126(6) -0.0002(6) N1 0.0121(7) 0.0166(8) 0.0157(7) 0.0003(6) 0.0052(6) 0.0011(6) N2 0.0127(7) 0.0176(8) 0.0143(7) 0.0015(6) 0.0061(6) -0.0002(6) C1 0.0183(9) 0.0190(10) 0.0233(10) 0.0014(8) 0.0073(8) 0.0045(7) C2 0.0207(9) 0.0202(9) 0.0183(9) 0.0028(7) 0.0115(8) 0.0001(7) C3 0.0164(9) 0.0171(9) 0.0138(8) -0.0002(7) 0.0071(7) -0.0025(7) C4 0.0173(9) 0.0240(10) 0.0165(9) 0.0001(7) 0.0073(8) 0.0009(8) C5 0.0230(10) 0.0264(10) 0.0185(9) -0.0030(8) 0.0129(8) -0.0032(8) C6 0.0269(10) 0.0204(10) 0.0152(9) -0.0008(7) 0.0096(8) -0.0053(8) C7 0.0196(9) 0.0171(9) 0.0159(9) 0.0011(7) 0.0046(8) -0.0020(7) C8 0.0164(9) 0.0151(9) 0.0179(9) 0.0000(7) 0.0074(7) -0.0025(7) C9 0.0168(9) 0.0248(10) 0.0196(9) 0.0033(8) 0.0069(8) 0.0018(8) C10 0.0132(9) 0.0241(10) 0.0158(9) 0.0055(7) 0.0072(7) 0.0019(7) C11 0.0176(9) 0.0336(11) 0.0187(9) 0.0011(8) 0.0096(8) 0.0006(8) C12 0.0223(11) 0.0484(14) 0.0234(10) 0.0038(10) 0.0147(9) 0.0037(10) C13 0.0195(10) 0.0530(15) 0.0278(11) 0.0120(10) 0.0147(9) -0.0006(10) C14 0.0174(10) 0.0342(12) 0.0260(11) 0.0112(9) 0.0076(9) -0.0042(9) C15 0.0149(9) 0.0247(10) 0.0183(9) 0.0082(8) 0.0053(8) 0.0010(8) C16 0.0216(10) 0.0219(10) 0.0279(11) 0.0010(8) 0.0097(9) -0.0039(8) C24 0.0189(9) 0.0222(9) 0.0156(9) -0.0043(7) 0.0092(8) -0.0060(8) C25 0.0209(10) 0.0274(10) 0.0204(9) -0.0051(8) 0.0109(8) -0.0021(8) C26 0.0323(12) 0.0366(13) 0.0329(12) -0.0108(10) 0.0222(10) -0.0029(10) C27 0.0465(15) 0.0492(15) 0.0319(12) -0.0129(11) 0.0302(12) -0.0113(12) C28 0.0421(14) 0.0410(13) 0.0188(10) -0.0026(9) 0.0176(10) -0.0106(11) C29 0.0256(10) 0.0273(11) 0.0169(9) -0.0024(8) 0.0091(8) -0.0083(8) C30 0.0308(12) 0.0326(12) 0.0175(10) 0.0063(8) 0.0075(9) 0.0001(9) C17 0.0143(8) 0.0179(9) 0.0138(8) 0.0010(7) 0.0057(7) -0.0003(7) C18 0.0181(9) 0.0175(9) 0.0176(9) 0.0000(7) 0.0083(8) -0.0003(7) C19 0.0179(9) 0.0218(10) 0.0230(10) 0.0023(8) 0.0110(8) 0.0023(8) C20 0.0159(9) 0.0249(10) 0.0265(10) 0.0010(8) 0.0094(8) -0.0030(8) C21 0.0201(10) 0.0198(10) 0.0244(10) -0.0019(8) 0.0098(8) -0.0049(8) C22 0.0176(9) 0.0182(9) 0.0183(9) 0.0004(7) 0.0082(8) 0.0000(7) C23 0.0221(10) 0.0182(10) 0.0318(11) -0.0041(8) 0.0124(9) -0.0002(8) C34 0.0197(9) 0.0223(10) 0.0178(9) 0.0009(7) 0.0071(8) 0.0017(8) C32 0.0151(9) 0.0216(10) 0.0202(9) 0.0034(8) 0.0080(8) 0.0033(7) C33 0.0212(10) 0.0215(10) 0.0188(9) -0.0015(8) 0.0075(8) -0.0027(8) C31 0.0146(9) 0.0199(9) 0.0156(9) -0.0014(7) 0.0042(7) 0.0005(7) Cl1 0.0344(4) 0.0409(4) 0.0333(4) 0.0010(3) 0.0171(3) 0.0126(3) Cl2 0.0334(4) 0.0310(4) 0.0481(5) -0.0059(3) 0.0186(4) 0.0027(3) C35 0.0303(16) 0.0395(18) 0.0374(17) -0.0033(14) 0.0151(14) 0.0055(14) _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 C33 1.850(2) . ? Cr1 C32 1.852(2) . ? Cr1 C31 1.876(2) . ? Cr1 C34 1.907(2) . ? Cr1 P1 2.3858(5) . ? Cr1 P2 2.3924(6) . ? P1 N1 1.7171(16) . ? P1 C10 1.835(2) . ? P1 C3 1.8472(19) . ? P2 N2 1.7342(16) . ? P2 C24 1.837(2) . ? P2 C17 1.8385(19) . ? O1 C34 1.144(3) . ? O2 C32 1.153(2) . ? O3 C33 1.154(3) . ? O4 C31 1.154(2) . ? N1 N2 1.438(2) . ? N1 C1 1.459(2) . ? N2 C2 1.475(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.404(3) . ? C3 C8 1.410(3) . ? C4 C5 1.386(3) . ? C4 H4 0.9500 . ? C5 C6 1.382(3) . ? C5 H5 0.9500 . ? C6 C7 1.381(3) . ? C6 H6 0.9500 . ? C7 C8 1.407(3) . ? C7 H7 0.9500 . ? C8 C9 1.507(3) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.399(3) . ? C10 C15 1.406(3) . ? C11 C12 1.383(3) . ? C11 H11 0.9500 . ? C12 C13 1.383(4) . ? C12 H12 0.9500 . ? C13 C14 1.378(4) . ? C13 H13 0.9500 . ? C14 C15 1.398(3) . ? C14 H14 0.9500 . ? C15 C16 1.500(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C24 C25 1.397(3) . ? C24 C29 1.407(3) . ? C25 C26 1.389(3) . ? C25 H25 0.9500 . ? C26 C27 1.385(4) . ? C26 H26 0.9500 . ? C27 C28 1.381(4) . ? C27 H27 0.9500 . ? C28 C29 1.401(3) . ? C28 H28 0.9500 . ? C29 C30 1.503(3) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C17 C18 1.395(3) . ? C17 C22 1.414(3) . ? C18 C19 1.387(3) . ? C18 H18 0.9500 . ? C19 C20 1.381(3) . ? C19 H19 0.9500 . ? C20 C21 1.380(3) . ? C20 H20 0.9500 . ? C21 C22 1.396(3) . ? C21 H21 0.9500 . ? C22 C23 1.507(3) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? Cl1 C35 1.732(3) . ? Cl2 C35 1.741(3) . ? C35 H35A 0.9900 . ? C35 H35B 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 C33 Cr1 C32 89.98(9) . . ? C33 Cr1 C31 84.69(9) . . ? C32 Cr1 C31 87.05(8) . . ? C33 Cr1 C34 86.19(9) . . ? C32 Cr1 C34 91.02(9) . . ? C31 Cr1 C34 170.67(8) . . ? C33 Cr1 P1 175.09(7) . . ? C32 Cr1 P1 91.07(6) . . ? C31 Cr1 P1 100.16(6) . . ? C34 Cr1 P1 88.99(6) . . ? C33 Cr1 P2 99.48(6) . . ? C32 Cr1 P2 169.59(6) . . ? C31 Cr1 P2 89.51(6) . . ? C34 Cr1 P2 93.91(6) . . ? P1 Cr1 P2 79.873(18) . . ? N1 P1 C10 101.55(9) . . ? N1 P1 C3 106.00(8) . . ? C10 P1 C3 107.27(9) . . ? N1 P1 Cr1 106.34(5) . . ? C10 P1 Cr1 110.94(6) . . ? C3 P1 Cr1 122.62(6) . . ? N2 P2 C24 101.95(8) . . ? N2 P2 C17 101.57(8) . . ? C24 P2 C17 102.89(9) . . ? N2 P2 Cr1 105.94(6) . . ? C24 P2 Cr1 119.83(6) . . ? C17 P2 Cr1 121.54(6) . . ? N2 N1 C1 111.66(15) . . ? N2 N1 P1 117.75(12) . . ? C1 N1 P1 123.40(13) . . ? N1 N2 C2 112.71(14) . . ? N1 N2 P2 106.76(11) . . ? C2 N2 P2 115.72(12) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N2 C2 H2A 109.5 . . ? N2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 C8 118.47(17) . . ? C4 C3 P1 114.37(14) . . ? C8 C3 P1 126.90(15) . . ? C5 C4 C3 122.34(18) . . ? C5 C4 H4 118.8 . . ? C3 C4 H4 118.8 . . ? C6 C5 C4 119.09(19) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? C7 C6 C5 119.62(18) . . ? C7 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C6 C7 C8 122.44(18) . . ? C6 C7 H7 118.8 . . ? C8 C7 H7 118.8 . . ? C7 C8 C3 117.91(18) . . ? C7 C8 C9 116.10(17) . . ? C3 C8 C9 125.94(17) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C15 119.34(18) . . ? C11 C10 P1 117.21(15) . . ? C15 C10 P1 123.06(15) . . ? C12 C11 C10 121.2(2) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C13 C12 C11 119.8(2) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C14 C13 C12 119.5(2) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C13 C14 C15 122.3(2) . . ? C13 C14 H14 118.8 . . ? C15 C14 H14 118.8 . . ? C14 C15 C10 117.9(2) . . ? C14 C15 C16 118.05(19) . . ? C10 C15 C16 123.99(18) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C25 C24 C29 119.20(18) . . ? C25 C24 P2 120.74(15) . . ? C29 C24 P2 120.06(16) . . ? C26 C25 C24 121.6(2) . . ? C26 C25 H25 119.2 . . ? C24 C25 H25 119.2 . . ? C27 C26 C25 119.3(2) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C28 C27 C26 119.8(2) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C27 C28 C29 122.0(2) . . ? C27 C28 H28 119.0 . . ? C29 C28 H28 119.0 . . ? C28 C29 C24 118.2(2) . . ? C28 C29 C30 119.0(2) . . ? C24 C29 C30 122.81(19) . . ? 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 . . ? C18 C17 C22 118.78(17) . . ? C18 C17 P2 116.89(14) . . ? C22 C17 P2 124.30(14) . . ? C19 C18 C17 121.85(18) . . ? C19 C18 H18 119.1 . . ? C17 C18 H18 119.1 . . ? C20 C19 C18 119.34(19) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C21 C20 C19 119.63(19) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C20 C21 C22 122.29(19) . . ? C20 C21 H21 118.9 . . ? C22 C21 H21 118.9 . . ? C21 C22 C17 118.10(18) . . ? C21 C22 C23 117.44(18) . . ? C17 C22 C23 124.45(17) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O1 C34 Cr1 174.39(18) . . ? O2 C32 Cr1 177.29(17) . . ? O3 C33 Cr1 176.26(19) . . ? O4 C31 Cr1 172.47(18) . . ? Cl1 C35 Cl2 113.59(19) . . ? Cl1 C35 H35A 108.8 . . ? Cl2 C35 H35A 108.8 . . ? Cl1 C35 H35B 108.8 . . ? Cl2 C35 H35B 108.8 . . ? H35A C35 H35B 107.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C32 Cr1 P1 N1 -170.78(8) . . . . ? C31 Cr1 P1 N1 -83.59(8) . . . . ? C34 Cr1 P1 N1 98.22(8) . . . . ? P2 Cr1 P1 N1 4.06(6) . . . . ? C32 Cr1 P1 C10 79.61(9) . . . . ? C31 Cr1 P1 C10 166.80(9) . . . . ? C34 Cr1 P1 C10 -11.39(9) . . . . ? P2 Cr1 P1 C10 -105.54(7) . . . . ? C32 Cr1 P1 C3 -48.87(10) . . . . ? C31 Cr1 P1 C3 38.33(9) . . . . ? C34 Cr1 P1 C3 -139.87(9) . . . . ? P2 Cr1 P1 C3 125.98(7) . . . . ? C33 Cr1 P2 N2 157.94(9) . . . . ? C32 Cr1 P2 N2 2.8(4) . . . . ? C31 Cr1 P2 N2 73.41(8) . . . . ? C34 Cr1 P2 N2 -115.27(8) . . . . ? P1 Cr1 P2 N2 -27.00(6) . . . . ? C33 Cr1 P2 C24 -87.73(10) . . . . ? C32 Cr1 P2 C24 117.1(4) . . . . ? C31 Cr1 P2 C24 -172.26(9) . . . . ? C34 Cr1 P2 C24 -0.95(10) . . . . ? P1 Cr1 P2 C24 87.33(8) . . . . ? C33 Cr1 P2 C17 43.11(10) . . . . ? C32 Cr1 P2 C17 -112.0(4) . . . . ? C31 Cr1 P2 C17 -41.42(9) . . . . ? C34 Cr1 P2 C17 129.89(9) . . . . ? P1 Cr1 P2 C17 -141.84(7) . . . . ? C10 P1 N1 N2 142.89(13) . . . . ? C3 P1 N1 N2 -105.16(13) . . . . ? Cr1 P1 N1 N2 26.78(13) . . . . ? C10 P1 N1 C1 -69.28(17) . . . . ? C3 P1 N1 C1 42.67(17) . . . . ? Cr1 P1 N1 C1 174.61(14) . . . . ? C1 N1 N2 C2 -74.63(19) . . . . ? P1 N1 N2 C2 76.79(17) . . . . ? C1 N1 N2 P2 157.23(13) . . . . ? P1 N1 N2 P2 -51.34(14) . . . . ? C24 P2 N2 N1 -76.61(12) . . . . ? C17 P2 N2 N1 177.36(11) . . . . ? Cr1 P2 N2 N1 49.49(11) . . . . ? C24 P2 N2 C2 157.04(13) . . . . ? C17 P2 N2 C2 51.01(15) . . . . ? Cr1 P2 N2 C2 -76.86(13) . . . . ? N1 P1 C3 C4 103.98(15) . . . . ? C10 P1 C3 C4 -148.13(15) . . . . ? Cr1 P1 C3 C4 -18.10(17) . . . . ? N1 P1 C3 C8 -70.10(18) . . . . ? C10 P1 C3 C8 37.79(19) . . . . ? Cr1 P1 C3 C8 167.83(14) . . . . ? C8 C3 C4 C5 2.7(3) . . . . ? P1 C3 C4 C5 -171.92(16) . . . . ? C3 C4 C5 C6 0.4(3) . . . . ? C4 C5 C6 C7 -2.7(3) . . . . ? C5 C6 C7 C8 1.9(3) . . . . ? C6 C7 C8 C3 1.2(3) . . . . ? C6 C7 C8 C9 -176.70(18) . . . . ? C4 C3 C8 C7 -3.4(3) . . . . ? P1 C3 C8 C7 170.46(14) . . . . ? C4 C3 C8 C9 174.27(18) . . . . ? P1 C3 C8 C9 -11.9(3) . . . . ? N1 P1 C10 C11 -22.23(17) . . . . ? C3 P1 C10 C11 -133.22(15) . . . . ? Cr1 P1 C10 C11 90.45(15) . . . . ? N1 P1 C10 C15 164.90(16) . . . . ? C3 P1 C10 C15 53.91(18) . . . . ? Cr1 P1 C10 C15 -82.42(16) . . . . ? C15 C10 C11 C12 -1.0(3) . . . . ? P1 C10 C11 C12 -174.18(16) . . . . ? C10 C11 C12 C13 0.7(3) . . . . ? C11 C12 C13 C14 0.0(3) . . . . ? C12 C13 C14 C15 -0.4(3) . . . . ? C13 C14 C15 C10 0.0(3) . . . . ? C13 C14 C15 C16 -178.8(2) . . . . ? C11 C10 C15 C14 0.7(3) . . . . ? P1 C10 C15 C14 173.43(15) . . . . ? C11 C10 C15 C16 179.36(18) . . . . ? P1 C10 C15 C16 -7.9(3) . . . . ? N2 P2 C24 C25 5.55(18) . . . . ? C17 P2 C24 C25 110.55(17) . . . . ? Cr1 P2 C24 C25 -110.87(16) . . . . ? N2 P2 C24 C29 -174.65(16) . . . . ? C17 P2 C24 C29 -69.65(17) . . . . ? Cr1 P2 C24 C29 68.93(17) . . . . ? C29 C24 C25 C26 -1.6(3) . . . . ? P2 C24 C25 C26 178.16(17) . . . . ? C24 C25 C26 C27 0.8(3) . . . . ? C25 C26 C27 C28 0.7(4) . . . . ? C26 C27 C28 C29 -1.2(4) . . . . ? C27 C28 C29 C24 0.3(3) . . . . ? C27 C28 C29 C30 179.0(2) . . . . ? C25 C24 C29 C28 1.1(3) . . . . ? P2 C24 C29 C28 -178.69(16) . . . . ? C25 C24 C29 C30 -177.6(2) . . . . ? P2 C24 C29 C30 2.6(3) . . . . ? N2 P2 C17 C18 -127.84(15) . . . . ? C24 P2 C17 C18 126.87(15) . . . . ? Cr1 P2 C17 C18 -10.80(17) . . . . ? N2 P2 C17 C22 54.31(17) . . . . ? C24 P2 C17 C22 -50.98(18) . . . . ? Cr1 P2 C17 C22 171.34(13) . . . . ? C22 C17 C18 C19 -0.5(3) . . . . ? P2 C17 C18 C19 -178.48(15) . . . . ? C17 C18 C19 C20 -0.4(3) . . . . ? C18 C19 C20 C21 0.8(3) . . . . ? C19 C20 C21 C22 -0.2(3) . . . . ? C20 C21 C22 C17 -0.7(3) . . . . ? C20 C21 C22 C23 178.51(19) . . . . ? C18 C17 C22 C21 1.0(3) . . . . ? P2 C17 C22 C21 178.82(15) . . . . ? C18 C17 C22 C23 -178.10(19) . . . . ? P2 C17 C22 C23 -0.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.256 _refine_diff_density_min -0.369 _refine_diff_density_rms 0.069 # Attachment '11.cif' data_twh63b2 _database_code_depnum_ccdc_archive 'CCDC 739223' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H34 Cr N2 O8 P2' _chemical_formula_sum 'C34 H34 Cr N2 O8 P2' _chemical_formula_weight 712.57 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.7079(4) _cell_length_b 10.7776(2) _cell_length_c 15.9097(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.3430(10) _cell_angle_gamma 90.00 _cell_volume 3329.28(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 36912 _cell_measurement_theta_min 27.46 _cell_measurement_theta_max 2.75 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 0.494 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.931 _exptl_absorpt_correction_T_max 0.952 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.366 _diffrn_detector_type 'Bruker-AXS SMART APEX' _diffrn_measurement_details 'frames, 0.3\% width' _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Bruker-AXS Kappa' _diffrn_measurement_method '\w & \f scans' _diffrn_measurement_specimen_support ; glass fibre ; _diffrn_radiation_collimation '0.5 mm double pinhole' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe X-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71074 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 40 _diffrn_source_power 2 _diffrn_source_size '0.4 x 8 mm fine focus' _diffrn_source_target Mo _diffrn_source_type 'Bruker-AXS KFF Mo 2K 90\% Ceramic' _diffrn_source_voltage 50 _diffrn_reflns_number 34901 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0251 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 27.46 _reflns_number_total 7573 _reflns_number_gt 6443 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'Apex II (Bruker-AXS, 2007)' _computing_data_reduction ; SAINT v7.34A (Bruker-AXS, 2007) & XPREP v2005/4 (Bruker-AXS, 2005) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Ten low angle disagreeable reflections were omitted: -1 0 2, 1 1 0, 2 0 0, -1 1 1, 0 1 1, -2 1 1, 2 1 0, -2 0 2, 1 1 1, 0 0 2. 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^)+(0.0376P)^2^+1.4947P] 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 7573 _refine_ls_number_parameters 430 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0382 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0793 _refine_ls_wR_factor_gt 0.0744 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 0.276254(11) 0.90381(2) 0.084991(14) 0.01238(7) Uani 1 1 d . . . P1 P 0.313141(19) 0.72085(3) 0.17097(2) 0.01397(8) Uani 1 1 d . . . P2 P 0.192901(19) 0.89502(3) 0.15452(2) 0.01299(8) Uani 1 1 d . . . N1 N 0.25436(6) 0.69456(11) 0.22321(8) 0.0150(2) Uani 1 1 d . . . N2 N 0.22562(6) 0.80343(11) 0.24962(8) 0.0151(2) Uani 1 1 d . . . O1 O 0.40671(6) 0.62925(11) 0.08533(8) 0.0260(3) Uani 1 1 d . . . O2 O 0.38730(6) 0.49521(10) 0.27999(8) 0.0277(3) Uani 1 1 d . . . O4 O 0.08939(5) 0.97146(10) -0.01201(7) 0.0199(2) Uani 1 1 d . . . O3 O 0.10525(6) 0.92190(10) 0.26993(7) 0.0209(2) Uani 1 1 d . . . C1 C 0.25637(9) 0.59086(14) 0.28358(10) 0.0212(3) Uani 1 1 d . . . H1A H 0.2919 0.6064 0.3421 0.032 Uiso 1 1 calc R . . H1B H 0.2671 0.5140 0.2582 0.032 Uiso 1 1 calc R . . H1C H 0.2115 0.5827 0.2908 0.032 Uiso 1 1 calc R . . C2 C 0.27393(8) 0.86575(14) 0.32898(9) 0.0184(3) Uani 1 1 d . . . H2A H 0.2929 0.8050 0.3771 0.028 Uiso 1 1 calc R . . H2B H 0.2496 0.9307 0.3492 0.028 Uiso 1 1 calc R . . H2C H 0.3115 0.9031 0.3135 0.028 Uiso 1 1 calc R . . C3 C 0.30137(8) 0.58223(13) 0.10086(9) 0.0161(3) Uani 1 1 d . . . C4 C 0.24097(8) 0.51256(14) 0.07643(10) 0.0191(3) Uani 1 1 d . . . H4 H 0.2059 0.5342 0.0995 0.023 Uiso 1 1 calc R . . C5 C 0.23136(9) 0.41178(15) 0.01882(10) 0.0238(3) Uani 1 1 d . . . H5 H 0.1904 0.3639 0.0037 0.029 Uiso 1 1 calc R . . C6 C 0.28183(9) 0.38147(15) -0.01637(10) 0.0254(4) Uani 1 1 d . . . H6 H 0.2754 0.3122 -0.0554 0.031 Uiso 1 1 calc R . . C7 C 0.34149(9) 0.45131(15) 0.00484(10) 0.0226(3) Uani 1 1 d . . . H7 H 0.3758 0.4304 -0.0197 0.027 Uiso 1 1 calc R . . C8 C 0.35093(8) 0.55247(15) 0.06243(10) 0.0193(3) Uani 1 1 d . . . C9 C 0.45459(10) 0.61565(19) 0.03921(13) 0.0339(4) Uani 1 1 d . . . H9A H 0.4762 0.5336 0.0521 0.051 Uiso 1 1 calc R . . H9B H 0.4901 0.6800 0.0594 0.051 Uiso 1 1 calc R . . H9C H 0.4302 0.6240 -0.0255 0.051 Uiso 1 1 calc R . . C10 C 0.40108(8) 0.70692(14) 0.25305(10) 0.0185(3) Uani 1 1 d . . . C11 C 0.44416(8) 0.81010(16) 0.26775(10) 0.0226(3) Uani 1 1 d . . . H11 H 0.4272 0.8840 0.2349 0.027 Uiso 1 1 calc R . . C12 C 0.51116(9) 0.80842(18) 0.32902(11) 0.0295(4) Uani 1 1 d . . . H12 H 0.5397 0.8797 0.3373 0.035 Uiso 1 1 calc R . . C13 C 0.53550(9) 0.70150(19) 0.37763(12) 0.0329(4) Uani 1 1 d . . . H13 H 0.5808 0.7001 0.4207 0.040 Uiso 1 1 calc R . . C14 C 0.49474(9) 0.59656(18) 0.36430(11) 0.0299(4) Uani 1 1 d . . . H14 H 0.5119 0.5237 0.3983 0.036 Uiso 1 1 calc R . . C15 C 0.42833(8) 0.59782(15) 0.30078(10) 0.0227(3) Uani 1 1 d . . . C16 C 0.40830(11) 0.38818(17) 0.33598(12) 0.0352(4) Uani 1 1 d . . . H16A H 0.4506 0.3543 0.3306 0.053 Uiso 1 1 calc R . . H16B H 0.3719 0.3253 0.3173 0.053 Uiso 1 1 calc R . . H16C H 0.4168 0.4115 0.3985 0.053 Uiso 1 1 calc R . . C17 C 0.16624(7) 1.03686(14) 0.19687(9) 0.0170(3) Uani 1 1 d . . . C18 C 0.18622(8) 1.15124(14) 0.17330(10) 0.0191(3) Uani 1 1 d . . . H18 H 0.2133 1.1535 0.1359 0.023 Uiso 1 1 calc R . . C19 C 0.16751(8) 1.26198(15) 0.20313(10) 0.0235(3) Uani 1 1 d . . . H19 H 0.1817 1.3391 0.1863 0.028 Uiso 1 1 calc R . . C20 C 0.12803(9) 1.25877(15) 0.25759(10) 0.0244(3) Uani 1 1 d . . . H20 H 0.1158 1.3343 0.2790 0.029 Uiso 1 1 calc R . . C21 C 0.10609(8) 1.14680(15) 0.28140(10) 0.0219(3) Uani 1 1 d . . . H21 H 0.0785 1.1458 0.3182 0.026 Uiso 1 1 calc R . . C22 C 0.12469(8) 1.03574(14) 0.25102(9) 0.0180(3) Uani 1 1 d . . . C23 C 0.06272(9) 0.91453(16) 0.32365(11) 0.0254(4) Uani 1 1 d . . . H23A H 0.0874 0.9493 0.3831 0.038 Uiso 1 1 calc R . . H23B H 0.0513 0.8275 0.3298 0.038 Uiso 1 1 calc R . . H23C H 0.0202 0.9616 0.2950 0.038 Uiso 1 1 calc R . . C24 C 0.11156(7) 0.81571(14) 0.09638(9) 0.0152(3) Uani 1 1 d . . . C25 C 0.09214(8) 0.70758(15) 0.12875(10) 0.0206(3) Uani 1 1 d . . . H25 H 0.1203 0.6758 0.1853 0.025 Uiso 1 1 calc R . . C26 C 0.03223(8) 0.64532(16) 0.07960(11) 0.0255(4) Uani 1 1 d . . . H26 H 0.0200 0.5707 0.1021 0.031 Uiso 1 1 calc R . . C27 C -0.00960(8) 0.69221(16) -0.00223(11) 0.0248(3) Uani 1 1 d . . . H27 H -0.0505 0.6493 -0.0358 0.030 Uiso 1 1 calc R . . C28 C 0.00765(8) 0.80108(15) -0.03550(10) 0.0208(3) Uani 1 1 d . . . H28 H -0.0216 0.8338 -0.0912 0.025 Uiso 1 1 calc R . . C29 C 0.06833(8) 0.86219(14) 0.01352(9) 0.0166(3) Uani 1 1 d . . . C30 C 0.05403(9) 1.01431(16) -0.10102(10) 0.0246(3) Uani 1 1 d . . . H30A H 0.0577 0.9520 -0.1440 0.037 Uiso 1 1 calc R . . H30B H 0.0747 1.0923 -0.1108 0.037 Uiso 1 1 calc R . . H30C H 0.0054 1.0281 -0.1094 0.037 Uiso 1 1 calc R . . C31 C 0.32587(8) 1.02076(15) 0.17240(10) 0.0199(3) Uani 1 1 d . . . C32 C 0.34752(8) 0.89358(14) 0.03955(10) 0.0198(3) Uani 1 1 d . . . C33 C 0.23764(8) 1.03305(15) 0.00734(10) 0.0203(3) Uani 1 1 d . . . C34 C 0.21745(8) 0.80535(14) -0.00871(10) 0.0170(3) Uani 1 1 d . . . O5 O 0.35451(6) 1.09745(11) 0.22176(8) 0.0292(3) Uani 1 1 d . . . O6 O 0.39052(6) 0.89165(11) 0.00881(8) 0.0279(3) Uani 1 1 d . . . O7 O 0.21336(7) 1.10971(11) -0.04514(8) 0.0308(3) Uani 1 1 d . . . O8 O 0.17918(6) 0.75479(11) -0.06919(7) 0.0247(3) 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 0.01259(12) 0.01346(12) 0.01115(11) -0.00188(8) 0.00422(9) -0.00252(9) P1 0.01264(18) 0.01608(19) 0.01299(17) -0.00229(13) 0.00419(14) 0.00007(14) P2 0.01307(18) 0.01385(18) 0.01206(17) -0.00093(13) 0.00436(14) 0.00014(14) N1 0.0165(6) 0.0145(6) 0.0150(6) 0.0006(4) 0.0069(5) 0.0015(5) N2 0.0164(6) 0.0168(6) 0.0125(6) -0.0012(4) 0.0055(5) 0.0031(5) O1 0.0209(6) 0.0330(6) 0.0294(6) -0.0128(5) 0.0156(5) -0.0033(5) O2 0.0269(6) 0.0215(6) 0.0296(6) 0.0034(5) 0.0035(5) 0.0066(5) O4 0.0196(6) 0.0201(6) 0.0167(5) 0.0036(4) 0.0023(4) -0.0001(4) O3 0.0246(6) 0.0218(6) 0.0215(5) 0.0040(4) 0.0147(5) 0.0051(5) C1 0.0257(8) 0.0194(8) 0.0197(7) 0.0044(6) 0.0093(6) 0.0022(6) C2 0.0190(8) 0.0216(8) 0.0129(7) -0.0020(5) 0.0033(6) 0.0003(6) C3 0.0189(7) 0.0144(7) 0.0135(6) -0.0006(5) 0.0038(6) 0.0020(6) C4 0.0216(8) 0.0181(7) 0.0167(7) 0.0017(5) 0.0055(6) 0.0015(6) C5 0.0293(9) 0.0190(8) 0.0201(8) -0.0011(6) 0.0046(7) -0.0052(7) C6 0.0399(10) 0.0163(8) 0.0180(7) -0.0022(6) 0.0074(7) 0.0010(7) C7 0.0302(9) 0.0214(8) 0.0168(7) -0.0002(6) 0.0087(6) 0.0072(7) C8 0.0198(8) 0.0208(8) 0.0162(7) 0.0002(6) 0.0047(6) 0.0035(6) C9 0.0293(10) 0.0424(11) 0.0394(10) -0.0131(8) 0.0239(8) -0.0033(8) C10 0.0151(7) 0.0245(8) 0.0154(7) -0.0041(6) 0.0048(6) 0.0028(6) C11 0.0169(8) 0.0302(9) 0.0204(8) -0.0030(6) 0.0059(6) 0.0006(7) C12 0.0168(8) 0.0428(11) 0.0264(8) -0.0086(7) 0.0046(7) -0.0042(7) C13 0.0156(8) 0.0514(12) 0.0265(9) -0.0068(8) 0.0007(7) 0.0052(8) C14 0.0220(9) 0.0406(10) 0.0243(8) 0.0016(7) 0.0047(7) 0.0131(8) C15 0.0193(8) 0.0280(9) 0.0202(7) -0.0031(6) 0.0059(6) 0.0053(7) C16 0.0452(12) 0.0255(9) 0.0332(10) 0.0065(7) 0.0113(9) 0.0117(8) C17 0.0168(7) 0.0182(7) 0.0145(7) -0.0019(5) 0.0038(6) 0.0034(6) C18 0.0191(8) 0.0191(8) 0.0184(7) -0.0024(6) 0.0056(6) -0.0009(6) C19 0.0258(9) 0.0183(8) 0.0243(8) -0.0039(6) 0.0060(7) -0.0008(6) C20 0.0274(9) 0.0223(8) 0.0201(7) -0.0067(6) 0.0039(7) 0.0059(7) C21 0.0235(8) 0.0266(8) 0.0145(7) -0.0031(6) 0.0051(6) 0.0073(7) C22 0.0189(8) 0.0211(8) 0.0131(7) 0.0013(5) 0.0042(6) 0.0032(6) C23 0.0243(9) 0.0345(9) 0.0223(8) 0.0078(7) 0.0144(7) 0.0081(7) C24 0.0135(7) 0.0184(7) 0.0150(7) -0.0025(5) 0.0063(6) -0.0001(6) C25 0.0187(8) 0.0242(8) 0.0196(7) 0.0027(6) 0.0076(6) -0.0001(6) C26 0.0226(8) 0.0259(9) 0.0296(9) 0.0014(7) 0.0114(7) -0.0071(7) C27 0.0160(8) 0.0309(9) 0.0263(8) -0.0063(7) 0.0059(6) -0.0065(7) C28 0.0154(7) 0.0275(8) 0.0177(7) -0.0026(6) 0.0034(6) 0.0014(6) C29 0.0160(7) 0.0192(7) 0.0168(7) -0.0017(5) 0.0085(6) 0.0012(6) C30 0.0243(9) 0.0304(9) 0.0172(7) 0.0064(6) 0.0050(6) 0.0043(7) C31 0.0181(8) 0.0224(8) 0.0212(7) 0.0002(6) 0.0092(6) -0.0012(6) C32 0.0184(8) 0.0228(8) 0.0153(7) -0.0039(6) 0.0022(6) -0.0061(6) C33 0.0220(8) 0.0194(8) 0.0198(7) -0.0028(6) 0.0079(6) -0.0058(6) C34 0.0174(7) 0.0183(7) 0.0183(7) 0.0009(6) 0.0101(6) 0.0010(6) O5 0.0277(7) 0.0280(7) 0.0309(6) -0.0122(5) 0.0090(5) -0.0083(5) O6 0.0226(6) 0.0402(7) 0.0247(6) -0.0058(5) 0.0133(5) -0.0080(5) O7 0.0377(7) 0.0232(6) 0.0277(6) 0.0071(5) 0.0064(5) -0.0037(5) O8 0.0225(6) 0.0313(6) 0.0197(5) -0.0089(5) 0.0066(5) -0.0057(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 Cr1 C33 1.8490(16) . ? Cr1 C32 1.8586(16) . ? Cr1 C34 1.8892(15) . ? Cr1 C31 1.8933(16) . ? Cr1 P2 2.3536(4) . ? Cr1 P1 2.3699(4) . ? P1 N1 1.7194(12) . ? P1 C3 1.8292(15) . ? P1 C10 1.8414(15) . ? P2 N2 1.7349(12) . ? P2 C24 1.8276(15) . ? P2 C17 1.8316(15) . ? N1 N2 1.4427(16) . ? N1 C1 1.4647(18) . ? N2 C2 1.4723(18) . ? O1 C8 1.3635(19) . ? O1 C9 1.4312(19) . ? O2 C15 1.363(2) . ? O2 C16 1.430(2) . ? O4 C29 1.3658(18) . ? O4 C30 1.4262(17) . ? O3 C22 1.3572(18) . ? O3 C23 1.4269(18) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.393(2) . ? C3 C8 1.402(2) . ? C4 C5 1.390(2) . ? C4 H4 0.9500 . ? C5 C6 1.385(2) . ? C5 H5 0.9500 . ? C6 C7 1.385(2) . ? C6 H6 0.9500 . ? C7 C8 1.393(2) . ? C7 H7 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.394(2) . ? C10 C15 1.407(2) . ? C11 C12 1.391(2) . ? C11 H11 0.9500 . ? C12 C13 1.382(3) . ? C12 H12 0.9500 . ? C13 C14 1.383(3) . ? C13 H13 0.9500 . ? C14 C15 1.395(2) . ? C14 H14 0.9500 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.393(2) . ? C17 C22 1.414(2) . ? C18 C19 1.388(2) . ? C18 H18 0.9500 . ? C19 C20 1.383(2) . ? C19 H19 0.9500 . ? C20 C21 1.388(2) . ? C20 H20 0.9500 . ? C21 C22 1.394(2) . ? C21 H21 0.9500 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.389(2) . ? C24 C29 1.403(2) . ? C25 C26 1.388(2) . ? C25 H25 0.9500 . ? C26 C27 1.384(2) . ? C26 H26 0.9500 . ? C27 C28 1.384(2) . ? C27 H27 0.9500 . ? C28 C29 1.393(2) . ? C28 H28 0.9500 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 O5 1.1523(19) . ? C32 O6 1.1555(19) . ? C33 O7 1.1579(19) . ? C34 O8 1.1492(18) . ? 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 C33 Cr1 C32 90.13(7) . . ? C33 Cr1 C34 83.43(6) . . ? C32 Cr1 C34 92.34(6) . . ? C33 Cr1 C31 89.28(7) . . ? C32 Cr1 C31 91.36(6) . . ? C34 Cr1 C31 171.83(7) . . ? C33 Cr1 P2 97.29(5) . . ? C32 Cr1 P2 172.58(5) . . ? C34 Cr1 P2 88.36(4) . . ? C31 Cr1 P2 88.91(5) . . ? C33 Cr1 P1 171.97(5) . . ? C32 Cr1 P1 92.00(5) . . ? C34 Cr1 P1 88.74(5) . . ? C31 Cr1 P1 98.41(5) . . ? P2 Cr1 P1 80.627(14) . . ? N1 P1 C3 101.16(6) . . ? N1 P1 C10 109.60(6) . . ? C3 P1 C10 104.78(7) . . ? N1 P1 Cr1 106.01(4) . . ? C3 P1 Cr1 112.32(5) . . ? C10 P1 Cr1 121.20(5) . . ? N2 P2 C24 100.79(6) . . ? N2 P2 C17 103.32(6) . . ? C24 P2 C17 103.53(7) . . ? N2 P2 Cr1 107.75(4) . . ? C24 P2 Cr1 118.58(5) . . ? C17 P2 Cr1 120.23(5) . . ? N2 N1 C1 110.51(11) . . ? N2 N1 P1 116.09(9) . . ? C1 N1 P1 125.39(10) . . ? N1 N2 C2 113.25(11) . . ? N1 N2 P2 106.52(8) . . ? C2 N2 P2 115.55(10) . . ? C8 O1 C9 118.31(12) . . ? C15 O2 C16 118.32(14) . . ? C29 O4 C30 117.88(12) . . ? C22 O3 C23 118.39(12) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N2 C2 H2A 109.5 . . ? N2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 C8 118.49(13) . . ? C4 C3 P1 121.79(11) . . ? C8 C3 P1 119.35(12) . . ? C5 C4 C3 120.93(15) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C6 C5 C4 119.70(15) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C7 C6 C5 120.53(14) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C6 C7 C8 119.67(15) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? O1 C8 C7 124.24(14) . . ? O1 C8 C3 115.16(13) . . ? C7 C8 C3 120.60(15) . . ? O1 C9 H9A 109.5 . . ? O1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C15 117.58(14) . . ? C11 C10 P1 118.13(12) . . ? C15 C10 P1 124.27(12) . . ? C12 C11 C10 122.11(16) . . ? C12 C11 H11 118.9 . . ? C10 C11 H11 118.9 . . ? C13 C12 C11 118.95(17) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C12 C13 C14 120.79(16) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C13 C14 C15 119.90(17) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? O2 C15 C14 122.82(15) . . ? O2 C15 C10 116.60(14) . . ? C14 C15 C10 120.56(16) . . ? O2 C16 H16A 109.5 . . ? O2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C22 118.19(13) . . ? C18 C17 P2 118.95(11) . . ? C22 C17 P2 122.84(11) . . ? C19 C18 C17 121.65(14) . . ? C19 C18 H18 119.2 . . ? C17 C18 H18 119.2 . . ? C20 C19 C18 119.24(15) . . ? C20 C19 H19 120.4 . . ? C18 C19 H19 120.4 . . ? C19 C20 C21 120.91(14) . . ? C19 C20 H20 119.5 . . ? C21 C20 H20 119.5 . . ? C20 C21 C22 119.72(14) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? O3 C22 C21 124.08(13) . . ? O3 C22 C17 115.66(13) . . ? C21 C22 C17 120.26(14) . . ? O3 C23 H23A 109.5 . . ? O3 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O3 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C29 118.38(13) . . ? C25 C24 P2 122.65(11) . . ? C29 C24 P2 118.90(11) . . ? C26 C25 C24 120.94(14) . . ? C26 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? C27 C26 C25 119.85(15) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C28 C27 C26 120.59(15) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C28 C29 119.29(14) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? O4 C29 C28 124.09(13) . . ? O4 C29 C24 114.94(13) . . ? C28 C29 C24 120.93(14) . . ? O4 C30 H30A 109.5 . . ? O4 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O4 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O5 C31 Cr1 175.86(14) . . ? O6 C32 Cr1 176.93(14) . . ? O7 C33 Cr1 176.23(14) . . ? O8 C34 Cr1 174.12(14) . . ? 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 C32 Cr1 P1 N1 -177.80(6) . . . . ? C34 Cr1 P1 N1 -85.50(6) . . . . ? C31 Cr1 P1 N1 90.53(6) . . . . ? P2 Cr1 P1 N1 3.05(4) . . . . ? C32 Cr1 P1 C3 -68.20(7) . . . . ? C34 Cr1 P1 C3 24.10(7) . . . . ? C31 Cr1 P1 C3 -159.87(7) . . . . ? P2 Cr1 P1 C3 112.65(6) . . . . ? C32 Cr1 P1 C10 56.62(7) . . . . ? C34 Cr1 P1 C10 148.92(7) . . . . ? C31 Cr1 P1 C10 -35.05(7) . . . . ? P2 Cr1 P1 C10 -122.53(6) . . . . ? C33 Cr1 P2 N2 -166.78(6) . . . . ? C34 Cr1 P2 N2 110.06(6) . . . . ? C31 Cr1 P2 N2 -77.65(7) . . . . ? P1 Cr1 P2 N2 21.06(5) . . . . ? C33 Cr1 P2 C24 79.75(7) . . . . ? C34 Cr1 P2 C24 -3.41(7) . . . . ? C31 Cr1 P2 C24 168.89(7) . . . . ? P1 Cr1 P2 C24 -92.40(6) . . . . ? C33 Cr1 P2 C17 -48.98(7) . . . . ? C34 Cr1 P2 C17 -132.14(7) . . . . ? C31 Cr1 P2 C17 40.15(7) . . . . ? P1 Cr1 P2 C17 138.87(5) . . . . ? C3 P1 N1 N2 -151.68(9) . . . . ? C10 P1 N1 N2 98.06(10) . . . . ? Cr1 P1 N1 N2 -34.34(10) . . . . ? C3 P1 N1 C1 62.60(13) . . . . ? C10 P1 N1 C1 -47.66(14) . . . . ? Cr1 P1 N1 C1 179.94(11) . . . . ? C1 N1 N2 C2 75.98(15) . . . . ? P1 N1 N2 C2 -74.67(12) . . . . ? C1 N1 N2 P2 -155.92(10) . . . . ? P1 N1 N2 P2 53.43(11) . . . . ? C24 P2 N2 N1 78.97(9) . . . . ? C17 P2 N2 N1 -174.18(9) . . . . ? Cr1 P2 N2 N1 -45.94(9) . . . . ? C24 P2 N2 C2 -154.29(10) . . . . ? C17 P2 N2 C2 -47.44(11) . . . . ? Cr1 P2 N2 C2 80.80(10) . . . . ? N1 P1 C3 C4 21.95(13) . . . . ? C10 P1 C3 C4 135.88(12) . . . . ? Cr1 P1 C3 C4 -90.69(12) . . . . ? N1 P1 C3 C8 -165.17(12) . . . . ? C10 P1 C3 C8 -51.24(13) . . . . ? Cr1 P1 C3 C8 82.19(12) . . . . ? C8 C3 C4 C5 3.2(2) . . . . ? P1 C3 C4 C5 176.18(11) . . . . ? C3 C4 C5 C6 -1.3(2) . . . . ? C4 C5 C6 C7 -0.5(2) . . . . ? C5 C6 C7 C8 0.3(2) . . . . ? C9 O1 C8 C7 8.3(2) . . . . ? C9 O1 C8 C3 -171.32(14) . . . . ? C6 C7 C8 O1 -177.91(14) . . . . ? C6 C7 C8 C3 1.6(2) . . . . ? C4 C3 C8 O1 176.20(13) . . . . ? P1 C3 C8 O1 3.09(18) . . . . ? C4 C3 C8 C7 -3.4(2) . . . . ? P1 C3 C8 C7 -176.50(11) . . . . ? N1 P1 C10 C11 -119.70(12) . . . . ? C3 P1 C10 C11 132.46(12) . . . . ? Cr1 P1 C10 C11 4.22(14) . . . . ? N1 P1 C10 C15 61.71(14) . . . . ? C3 P1 C10 C15 -46.14(14) . . . . ? Cr1 P1 C10 C15 -174.38(11) . . . . ? C15 C10 C11 C12 -1.9(2) . . . . ? P1 C10 C11 C12 179.45(12) . . . . ? C10 C11 C12 C13 -0.8(2) . . . . ? C11 C12 C13 C14 1.6(3) . . . . ? C12 C13 C14 C15 0.3(3) . . . . ? C16 O2 C15 C14 11.0(2) . . . . ? C16 O2 C15 C10 -170.44(14) . . . . ? C13 C14 C15 O2 175.36(15) . . . . ? C13 C14 C15 C10 -3.1(2) . . . . ? C11 C10 C15 O2 -174.76(14) . . . . ? P1 C10 C15 O2 3.8(2) . . . . ? C11 C10 C15 C14 3.8(2) . . . . ? P1 C10 C15 C14 -177.61(12) . . . . ? N2 P2 C17 C18 131.52(12) . . . . ? C24 P2 C17 C18 -123.73(12) . . . . ? Cr1 P2 C17 C18 11.48(14) . . . . ? N2 P2 C17 C22 -50.01(13) . . . . ? C24 P2 C17 C22 54.75(13) . . . . ? Cr1 P2 C17 C22 -170.05(10) . . . . ? C22 C17 C18 C19 1.3(2) . . . . ? P2 C17 C18 C19 179.87(12) . . . . ? C17 C18 C19 C20 0.0(2) . . . . ? C18 C19 C20 C21 -1.1(2) . . . . ? C19 C20 C21 C22 0.8(2) . . . . ? C23 O3 C22 C21 0.5(2) . . . . ? C23 O3 C22 C17 -179.43(13) . . . . ? C20 C21 C22 O3 -179.34(14) . . . . ? C20 C21 C22 C17 0.6(2) . . . . ? C18 C17 C22 O3 178.32(13) . . . . ? P2 C17 C22 O3 -0.16(18) . . . . ? C18 C17 C22 C21 -1.6(2) . . . . ? P2 C17 C22 C21 179.92(11) . . . . ? N2 P2 C24 C25 -2.91(13) . . . . ? C17 P2 C24 C25 -109.59(13) . . . . ? Cr1 P2 C24 C25 114.29(11) . . . . ? N2 P2 C24 C29 -179.75(11) . . . . ? C17 P2 C24 C29 73.57(12) . . . . ? Cr1 P2 C24 C29 -62.55(13) . . . . ? C29 C24 C25 C26 1.4(2) . . . . ? P2 C24 C25 C26 -175.47(12) . . . . ? C24 C25 C26 C27 -1.1(2) . . . . ? C25 C26 C27 C28 -0.2(2) . . . . ? C26 C27 C28 C29 1.1(2) . . . . ? C30 O4 C29 C28 -11.6(2) . . . . ? C30 O4 C29 C24 170.62(13) . . . . ? C27 C28 C29 O4 -178.39(14) . . . . ? C27 C28 C29 C24 -0.8(2) . . . . ? C25 C24 C29 O4 177.36(13) . . . . ? P2 C24 C29 O4 -5.67(17) . . . . ? C25 C24 C29 C28 -0.5(2) . . . . ? P2 C24 C29 C28 176.52(11) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.347 _refine_diff_density_min -0.334 _refine_diff_density_rms 0.055 # Attachment '8.cif' data_twh90b_0m _database_code_depnum_ccdc_archive 'CCDC 739224' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H27 Cr N O6 P2' _chemical_formula_sum 'C31 H27 Cr N O6 P2' _chemical_formula_weight 623.48 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' Cr Cr 0.3209 0.6236 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.7120(2) _cell_length_b 13.3565(2) _cell_length_c 20.7321(3) _cell_angle_alpha 90.00 _cell_angle_beta 134.6350(10) _cell_angle_gamma 90.00 _cell_volume 2898.95(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 35109 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 27.52 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.196 _exptl_crystal_size_mid 0.156 _exptl_crystal_size_min 0.052 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.429 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 0.550 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.846 _exptl_absorpt_correction_T_max 0.970 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.366 _diffrn_detector_type 'Bruker-AXS SMART APEX' _diffrn_measurement_details 'frames, 0.3\% width' _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Bruker-AXS Kappa' _diffrn_measurement_method '\w & \f scans' _diffrn_measurement_specimen_support ; glass fibre ; _diffrn_radiation_collimation '0.5 mm double pinhole' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe X-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71074 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 40 _diffrn_source_power 2 _diffrn_source_size '0.4 x 8 mm fine focus' _diffrn_source_target Mo _diffrn_source_type 'Bruker-AXS KFF Mo 2K 90\% Ceramic' _diffrn_source_voltage 50 _diffrn_reflns_number 34312 _diffrn_reflns_av_R_equivalents 0.0636 _diffrn_reflns_av_sigmaI/netI 0.0492 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.35 _diffrn_reflns_theta_max 27.52 _reflns_number_total 6627 _reflns_number_gt 5018 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'Apex II (Bruker-AXS, 2007)' _computing_data_reduction ; SAINT v7.34A (Bruker-AXS, 2007) & XPREP v2005/4 (Bruker-AXS, 2005) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Ten low angle disagreeable reflections have been omitted : 0 0 2, 1 0 0, 0 1 1, -1 0 2, -1 1 2, 1 1 0, -2 0 2, -1 1 1, 1 1 1 and 0 2 1. 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^)+(0.0481P)^2^+1.5814P] 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 6627 _refine_ls_number_parameters 373 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0611 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.1101 _refine_ls_wR_factor_gt 0.0989 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 0.28504(3) 0.90907(3) 0.55441(2) 0.01707(10) Uani 1 1 d . . . P1 P 0.33057(5) 0.74195(4) 0.54943(4) 0.01701(13) Uani 1 1 d . . . P2 P 0.31205(5) 0.80927(4) 0.65921(4) 0.01735(14) Uani 1 1 d . . . N1 N 0.34087(17) 0.70190(13) 0.63208(13) 0.0179(4) Uani 1 1 d . . . O1 O 0.07556(16) 0.67073(13) 0.46378(12) 0.0296(4) Uani 1 1 d . . . O2 O 0.43240(15) 0.81437(12) 0.47699(11) 0.0241(4) Uani 1 1 d . . . C1 C 0.3434(2) 0.59873(16) 0.65712(18) 0.0253(5) Uani 1 1 d . . . H1A H 0.2605 0.5822 0.6350 0.038 Uiso 1 1 calc R . . H1B H 0.4105 0.5919 0.7232 0.038 Uiso 1 1 calc R . . H1C H 0.3608 0.5531 0.6299 0.038 Uiso 1 1 calc R . . C2 C 0.2256(2) 0.65544(16) 0.45471(15) 0.0198(5) Uani 1 1 d . . . C3 C 0.2608(2) 0.61541(17) 0.41257(16) 0.0213(5) Uani 1 1 d . . . H3 H 0.3428 0.6301 0.4363 0.026 Uiso 1 1 calc R . . C4 C 0.1783(2) 0.55479(18) 0.33685(17) 0.0253(5) Uani 1 1 d . . . H4 H 0.2038 0.5280 0.3091 0.030 Uiso 1 1 calc R . . C5 C 0.0590(2) 0.53345(19) 0.30196(17) 0.0296(6) Uani 1 1 d . . . H5 H 0.0023 0.4922 0.2498 0.036 Uiso 1 1 calc R . . C6 C 0.0207(2) 0.57141(19) 0.34194(18) 0.0284(6) Uani 1 1 d . . . H6 H -0.0617 0.5562 0.3172 0.034 Uiso 1 1 calc R . . C7 C 0.1035(2) 0.63191(18) 0.41845(17) 0.0240(5) Uani 1 1 d . . . C8 C -0.0494(3) 0.6534(2) 0.4275(2) 0.0428(8) Uani 1 1 d . . . H8A H -0.1137 0.6817 0.3663 0.064 Uiso 1 1 calc R . . H8B H -0.0562 0.6855 0.4665 0.064 Uiso 1 1 calc R . . H8C H -0.0636 0.5813 0.4249 0.064 Uiso 1 1 calc R . . C9 C 0.4879(2) 0.71601(16) 0.59340(15) 0.0183(5) Uani 1 1 d . . . C10 C 0.5785(2) 0.66119(17) 0.67274(16) 0.0202(5) Uani 1 1 d . . . H10 H 0.5538 0.6270 0.6986 0.024 Uiso 1 1 calc R . . C11 C 0.7046(2) 0.65561(19) 0.71483(17) 0.0264(5) Uani 1 1 d . . . H11 H 0.7653 0.6174 0.7687 0.032 Uiso 1 1 calc R . . C12 C 0.7411(2) 0.70575(19) 0.67797(18) 0.0286(6) Uani 1 1 d . . . H12 H 0.8276 0.7029 0.7074 0.034 Uiso 1 1 calc R . . C13 C 0.6534(2) 0.76025(18) 0.59866(17) 0.0252(5) Uani 1 1 d . . . H13 H 0.6793 0.7946 0.5736 0.030 Uiso 1 1 calc R . . C14 C 0.5271(2) 0.76415(16) 0.55618(16) 0.0207(5) Uani 1 1 d . . . C15 C 0.4689(2) 0.87247(19) 0.44007(18) 0.0290(6) Uani 1 1 d . . . H15A H 0.5378 0.9184 0.4865 0.043 Uiso 1 1 calc R . . H15B H 0.3952 0.9110 0.3880 0.043 Uiso 1 1 calc R . . H15C H 0.4985 0.8277 0.4205 0.043 Uiso 1 1 calc R . . C16 C 0.4492(2) 0.82938(16) 0.78048(15) 0.0180(5) Uani 1 1 d . . . C17 C 0.5704(2) 0.79549(17) 0.82425(16) 0.0222(5) Uani 1 1 d . . . H17 H 0.5813 0.7562 0.7919 0.027 Uiso 1 1 calc R . . C18 C 0.6755(2) 0.81849(18) 0.91464(17) 0.0244(5) Uani 1 1 d . . . H18 H 0.7575 0.7935 0.9442 0.029 Uiso 1 1 calc R . . C19 C 0.6614(2) 0.87796(18) 0.96201(17) 0.0246(5) Uani 1 1 d . . . H19 H 0.7335 0.8945 1.0237 0.030 Uiso 1 1 calc R . . C20 C 0.5405(2) 0.91319(18) 0.91843(17) 0.0254(5) Uani 1 1 d . . . H20 H 0.5303 0.9542 0.9504 0.031 Uiso 1 1 calc R . . C21 C 0.4354(2) 0.88881(17) 0.82888(17) 0.0233(5) Uani 1 1 d . . . H21 H 0.3532 0.9125 0.7999 0.028 Uiso 1 1 calc R . . C22 C 0.1879(2) 0.78604(16) 0.65723(16) 0.0199(5) Uani 1 1 d . . . C23 C 0.2036(2) 0.71064(18) 0.71120(18) 0.0266(5) Uani 1 1 d . . . H23 H 0.2777 0.6695 0.7470 0.032 Uiso 1 1 calc R . . C24 C 0.1119(3) 0.69540(19) 0.7128(2) 0.0323(6) Uani 1 1 d . . . H24 H 0.1226 0.6434 0.7489 0.039 Uiso 1 1 calc R . . C25 C 0.0050(2) 0.7561(2) 0.66188(18) 0.0316(6) Uani 1 1 d . . . H25 H -0.0581 0.7453 0.6626 0.038 Uiso 1 1 calc R . . C26 C -0.0100(2) 0.8321(2) 0.61009(18) 0.0308(6) Uani 1 1 d . . . H26 H -0.0826 0.8746 0.5763 0.037 Uiso 1 1 calc R . . C27 C 0.0806(2) 0.84707(18) 0.60690(17) 0.0246(5) Uani 1 1 d . . . H27 H 0.0689 0.8990 0.5703 0.029 Uiso 1 1 calc R . . C28 C 0.4620(2) 0.93401(16) 0.63621(16) 0.0200(5) Uani 1 1 d . . . C29 C 0.2628(2) 0.96253(17) 0.46184(16) 0.0215(5) Uani 1 1 d . . . C30 C 0.2619(2) 1.02682(17) 0.58865(16) 0.0218(5) Uani 1 1 d . . . C31 C 0.1068(2) 0.88971(17) 0.46074(17) 0.0238(5) Uani 1 1 d . . . O3 O 0.56931(15) 0.95026(12) 0.68334(11) 0.0265(4) Uani 1 1 d . . . O4 O 0.24329(16) 0.99581(13) 0.40136(12) 0.0300(4) Uani 1 1 d . . . O5 O 0.24681(17) 1.09909(12) 0.61100(12) 0.0311(4) Uani 1 1 d . . . O6 O -0.00117(16) 0.88619(14) 0.39891(13) 0.0383(5) 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 0.01500(18) 0.01785(18) 0.0160(2) 0.00114(14) 0.01005(17) -0.00036(13) P1 0.0151(3) 0.0187(3) 0.0160(3) -0.0004(2) 0.0105(3) -0.0012(2) P2 0.0153(3) 0.0190(3) 0.0182(3) 0.0016(2) 0.0119(3) 0.0008(2) N1 0.0175(9) 0.0187(9) 0.0185(10) 0.0025(8) 0.0131(9) 0.0014(7) O1 0.0210(9) 0.0340(9) 0.0367(11) -0.0101(8) 0.0213(9) -0.0079(7) O2 0.0234(9) 0.0292(9) 0.0223(9) 0.0017(7) 0.0170(8) -0.0023(7) C1 0.0305(13) 0.0194(11) 0.0325(15) 0.0046(10) 0.0244(13) 0.0027(9) C2 0.0157(11) 0.0204(11) 0.0169(12) 0.0009(9) 0.0092(10) -0.0023(8) C3 0.0210(12) 0.0246(11) 0.0169(12) 0.0002(9) 0.0128(11) -0.0026(9) C4 0.0290(13) 0.0270(12) 0.0212(13) -0.0026(10) 0.0181(12) -0.0045(10) C5 0.0273(13) 0.0308(13) 0.0200(14) -0.0048(10) 0.0127(12) -0.0089(10) C6 0.0192(12) 0.0326(13) 0.0265(14) -0.0035(11) 0.0136(12) -0.0073(10) C7 0.0202(12) 0.0258(12) 0.0241(13) -0.0004(10) 0.0150(11) -0.0016(9) C8 0.0256(14) 0.0519(17) 0.059(2) -0.0137(15) 0.0328(16) -0.0106(12) C9 0.0178(11) 0.0191(10) 0.0186(12) -0.0037(9) 0.0129(10) -0.0016(8) C10 0.0205(11) 0.0234(11) 0.0181(12) -0.0026(9) 0.0141(10) -0.0011(9) C11 0.0206(12) 0.0329(13) 0.0221(13) -0.0009(10) 0.0137(11) 0.0031(10) C12 0.0178(12) 0.0414(14) 0.0263(14) -0.0021(11) 0.0153(11) 0.0013(10) C13 0.0248(12) 0.0303(12) 0.0285(14) -0.0049(10) 0.0216(12) -0.0049(10) C14 0.0211(11) 0.0218(11) 0.0197(12) -0.0047(9) 0.0145(11) -0.0038(9) C15 0.0337(14) 0.0310(13) 0.0302(15) 0.0010(11) 0.0253(13) -0.0039(11) C16 0.0205(11) 0.0190(10) 0.0166(12) 0.0029(9) 0.0138(10) 0.0001(8) C17 0.0223(12) 0.0264(12) 0.0193(13) -0.0005(10) 0.0150(11) 0.0012(9) C18 0.0198(12) 0.0282(12) 0.0204(13) 0.0013(10) 0.0123(11) 0.0012(9) C19 0.0249(12) 0.0267(12) 0.0176(13) 0.0001(10) 0.0133(11) -0.0047(9) C20 0.0313(13) 0.0250(12) 0.0267(14) -0.0049(10) 0.0228(12) -0.0025(10) C21 0.0202(12) 0.0252(12) 0.0262(14) -0.0013(10) 0.0169(11) 0.0008(9) C22 0.0178(11) 0.0232(11) 0.0202(13) -0.0018(9) 0.0139(11) -0.0022(9) C23 0.0252(13) 0.0277(12) 0.0309(15) 0.0057(11) 0.0211(12) 0.0025(10) C24 0.0363(15) 0.0302(13) 0.0414(17) 0.0034(12) 0.0312(14) -0.0026(11) C25 0.0242(13) 0.0452(15) 0.0320(15) -0.0061(12) 0.0221(13) -0.0082(11) C26 0.0199(12) 0.0462(15) 0.0252(14) 0.0013(12) 0.0155(12) 0.0045(11) C27 0.0215(12) 0.0313(12) 0.0211(13) 0.0028(10) 0.0151(11) 0.0027(10) C28 0.0241(12) 0.0183(10) 0.0195(12) -0.0013(9) 0.0159(11) -0.0017(9) C29 0.0179(11) 0.0237(11) 0.0211(13) -0.0017(10) 0.0131(11) -0.0020(9) C30 0.0188(11) 0.0247(12) 0.0184(13) 0.0036(9) 0.0118(11) 0.0004(9) C31 0.0227(13) 0.0248(12) 0.0245(14) 0.0011(10) 0.0168(12) -0.0003(9) O3 0.0195(9) 0.0317(9) 0.0248(10) -0.0054(7) 0.0143(8) -0.0055(7) O4 0.0261(9) 0.0389(10) 0.0220(10) 0.0068(8) 0.0159(9) 0.0001(7) O5 0.0387(11) 0.0241(9) 0.0329(11) -0.0028(8) 0.0260(10) 0.0008(7) O6 0.0172(9) 0.0461(11) 0.0315(11) 0.0032(9) 0.0099(9) -0.0018(8) _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 C29 1.849(2) . ? Cr1 C30 1.853(2) . ? Cr1 C31 1.886(2) . ? Cr1 C28 1.887(2) . ? Cr1 P2 2.3328(7) . ? Cr1 P1 2.3535(6) . ? P1 N1 1.6972(19) . ? P1 C2 1.821(2) . ? P1 C9 1.828(2) . ? P2 N1 1.6992(19) . ? P2 C22 1.825(2) . ? P2 C16 1.827(2) . ? N1 C1 1.464(3) . ? O1 C7 1.365(3) . ? O1 C8 1.433(3) . ? O2 C14 1.368(3) . ? O2 C15 1.433(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.397(3) . ? C2 C7 1.412(3) . ? C3 C4 1.384(3) . ? C3 H3 0.9500 . ? C4 C5 1.379(3) . ? C4 H4 0.9500 . ? C5 C6 1.384(4) . ? C5 H5 0.9500 . ? C6 C7 1.392(3) . ? C6 H6 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.392(3) . ? C9 C14 1.403(3) . ? C10 C11 1.391(3) . ? C10 H10 0.9500 . ? C11 C12 1.377(3) . ? C11 H11 0.9500 . ? C12 C13 1.385(4) . ? C12 H12 0.9500 . ? C13 C14 1.390(3) . ? C13 H13 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.391(3) . ? C16 C21 1.402(3) . ? C17 C18 1.388(3) . ? C17 H17 0.9500 . ? C18 C19 1.388(3) . ? C18 H18 0.9500 . ? C19 C20 1.394(3) . ? C19 H19 0.9500 . ? C20 C21 1.382(3) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C27 1.389(3) . ? C22 C23 1.398(3) . ? C23 C24 1.389(3) . ? C23 H23 0.9500 . ? C24 C25 1.382(4) . ? C24 H24 0.9500 . ? C25 C26 1.378(4) . ? C25 H25 0.9500 . ? C26 C27 1.395(3) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 O3 1.151(3) . ? C29 O4 1.160(3) . ? C30 O5 1.158(3) . ? C31 O6 1.144(3) . ? 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 C29 Cr1 C30 97.10(10) . . ? C29 Cr1 C31 83.10(10) . . ? C30 Cr1 C31 90.82(10) . . ? C29 Cr1 C28 89.48(10) . . ? C30 Cr1 C28 90.84(10) . . ? C31 Cr1 C28 172.54(10) . . ? C29 Cr1 P2 167.86(7) . . ? C30 Cr1 P2 94.89(7) . . ? C31 Cr1 P2 94.85(8) . . ? C28 Cr1 P2 92.25(7) . . ? C29 Cr1 P1 99.73(7) . . ? C30 Cr1 P1 163.03(8) . . ? C31 Cr1 P1 93.29(7) . . ? C28 Cr1 P1 87.21(7) . . ? P2 Cr1 P1 68.37(2) . . ? N1 P1 C2 107.17(10) . . ? N1 P1 C9 104.66(10) . . ? C2 P1 C9 103.59(10) . . ? N1 P1 Cr1 94.64(7) . . ? C2 P1 Cr1 126.67(8) . . ? C9 P1 Cr1 117.23(7) . . ? N1 P2 C22 109.12(10) . . ? N1 P2 C16 106.77(10) . . ? C22 P2 C16 100.14(10) . . ? N1 P2 Cr1 95.33(7) . . ? C22 P2 Cr1 124.30(8) . . ? C16 P2 Cr1 119.91(7) . . ? C1 N1 P1 128.09(16) . . ? C1 N1 P2 128.84(15) . . ? P1 N1 P2 101.66(10) . . ? C7 O1 C8 118.2(2) . . ? C14 O2 C15 117.31(18) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C7 118.3(2) . . ? C3 C2 P1 120.72(17) . . ? C7 C2 P1 120.89(18) . . ? C4 C3 C2 121.2(2) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C5 C4 C3 119.6(2) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 120.9(2) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C7 119.8(2) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? O1 C7 C6 124.1(2) . . ? O1 C7 C2 115.8(2) . . ? C6 C7 C2 120.2(2) . . ? O1 C8 H8A 109.5 . . ? O1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C14 117.9(2) . . ? C10 C9 P1 121.01(17) . . ? C14 C9 P1 120.31(17) . . ? C11 C10 C9 121.2(2) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C12 C11 C10 119.6(2) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C11 C12 C13 120.9(2) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C12 C13 C14 119.2(2) . . ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4 . . ? O2 C14 C13 124.0(2) . . ? O2 C14 C9 114.8(2) . . ? C13 C14 C9 121.2(2) . . ? O2 C15 H15A 109.5 . . ? O2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 118.8(2) . . ? C17 C16 P2 121.34(17) . . ? C21 C16 P2 119.54(17) . . ? C18 C17 C16 120.7(2) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C17 C18 C19 120.2(2) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C18 C19 C20 119.5(2) . . ? C18 C19 H19 120.3 . . ? C20 C19 H19 120.3 . . ? C21 C20 C19 120.3(2) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C16 120.4(2) . . ? C20 C21 H21 119.8 . . ? C16 C21 H21 119.8 . . ? C27 C22 C23 119.0(2) . . ? C27 C22 P2 120.55(18) . . ? C23 C22 P2 120.26(17) . . ? C24 C23 C22 120.5(2) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C25 C24 C23 119.9(2) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C26 C25 C24 120.1(2) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C25 C26 C27 120.4(2) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C22 C27 C26 120.0(2) . . ? C22 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? O3 C28 Cr1 177.4(2) . . ? O4 C29 Cr1 177.11(19) . . ? O5 C30 Cr1 178.4(2) . . ? O6 C31 Cr1 172.4(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C29 Cr1 P1 N1 -177.31(10) . . . . ? C30 Cr1 P1 N1 10.0(3) . . . . ? C31 Cr1 P1 N1 -93.75(10) . . . . ? C28 Cr1 P1 N1 93.70(10) . . . . ? P2 Cr1 P1 N1 0.17(7) . . . . ? C29 Cr1 P1 C2 -61.86(12) . . . . ? C30 Cr1 P1 C2 125.4(3) . . . . ? C31 Cr1 P1 C2 21.69(12) . . . . ? C28 Cr1 P1 C2 -150.85(12) . . . . ? P2 Cr1 P1 C2 115.61(10) . . . . ? C29 Cr1 P1 C9 73.59(11) . . . . ? C30 Cr1 P1 C9 -99.1(3) . . . . ? C31 Cr1 P1 C9 157.14(11) . . . . ? C28 Cr1 P1 C9 -15.40(11) . . . . ? P2 Cr1 P1 C9 -108.94(9) . . . . ? C29 Cr1 P2 N1 11.8(4) . . . . ? C30 Cr1 P2 N1 -177.30(9) . . . . ? C31 Cr1 P2 N1 91.46(10) . . . . ? C28 Cr1 P2 N1 -86.26(9) . . . . ? P1 Cr1 P2 N1 -0.17(6) . . . . ? C29 Cr1 P2 C22 -105.8(4) . . . . ? C30 Cr1 P2 C22 65.19(11) . . . . ? C31 Cr1 P2 C22 -26.05(12) . . . . ? C28 Cr1 P2 C22 156.22(11) . . . . ? P1 Cr1 P2 C22 -117.68(9) . . . . ? C29 Cr1 P2 C16 124.6(3) . . . . ? C30 Cr1 P2 C16 -64.47(11) . . . . ? C31 Cr1 P2 C16 -155.72(11) . . . . ? C28 Cr1 P2 C16 26.56(11) . . . . ? P1 Cr1 P2 C16 112.66(9) . . . . ? C2 P1 N1 C1 36.3(2) . . . . ? C9 P1 N1 C1 -73.3(2) . . . . ? Cr1 P1 N1 C1 167.01(18) . . . . ? C2 P1 N1 P2 -130.93(10) . . . . ? C9 P1 N1 P2 119.50(10) . . . . ? Cr1 P1 N1 P2 -0.22(8) . . . . ? C22 P2 N1 C1 -37.7(2) . . . . ? C16 P2 N1 C1 69.7(2) . . . . ? Cr1 P2 N1 C1 -166.87(19) . . . . ? C22 P2 N1 P1 129.37(10) . . . . ? C16 P2 N1 P1 -123.23(10) . . . . ? Cr1 P2 N1 P1 0.22(8) . . . . ? N1 P1 C2 C3 -132.07(18) . . . . ? C9 P1 C2 C3 -21.8(2) . . . . ? Cr1 P1 C2 C3 118.31(17) . . . . ? N1 P1 C2 C7 51.8(2) . . . . ? C9 P1 C2 C7 162.16(19) . . . . ? Cr1 P1 C2 C7 -57.8(2) . . . . ? C7 C2 C3 C4 0.4(3) . . . . ? P1 C2 C3 C4 -175.73(18) . . . . ? C2 C3 C4 C5 0.2(4) . . . . ? C3 C4 C5 C6 -0.4(4) . . . . ? C4 C5 C6 C7 0.0(4) . . . . ? C8 O1 C7 C6 -4.0(4) . . . . ? C8 O1 C7 C2 177.0(2) . . . . ? C5 C6 C7 O1 -178.4(2) . . . . ? C5 C6 C7 C2 0.7(4) . . . . ? C3 C2 C7 O1 178.2(2) . . . . ? P1 C2 C7 O1 -5.6(3) . . . . ? C3 C2 C7 C6 -0.9(3) . . . . ? P1 C2 C7 C6 175.32(19) . . . . ? N1 P1 C9 C10 8.1(2) . . . . ? C2 P1 C9 C10 -104.04(19) . . . . ? Cr1 P1 C9 C10 111.33(17) . . . . ? N1 P1 C9 C14 -161.66(18) . . . . ? C2 P1 C9 C14 86.19(19) . . . . ? Cr1 P1 C9 C14 -58.4(2) . . . . ? C14 C9 C10 C11 1.1(3) . . . . ? P1 C9 C10 C11 -168.91(18) . . . . ? C9 C10 C11 C12 0.5(4) . . . . ? C10 C11 C12 C13 -1.1(4) . . . . ? C11 C12 C13 C14 0.1(4) . . . . ? C15 O2 C14 C13 -5.0(3) . . . . ? C15 O2 C14 C9 174.5(2) . . . . ? C12 C13 C14 O2 -178.9(2) . . . . ? C12 C13 C14 C9 1.6(3) . . . . ? C10 C9 C14 O2 178.32(19) . . . . ? P1 C9 C14 O2 -11.6(3) . . . . ? C10 C9 C14 C13 -2.2(3) . . . . ? P1 C9 C14 C13 167.93(18) . . . . ? N1 P2 C16 C17 29.4(2) . . . . ? C22 P2 C16 C17 143.07(19) . . . . ? Cr1 P2 C16 C17 -77.18(19) . . . . ? N1 P2 C16 C21 -157.19(17) . . . . ? C22 P2 C16 C21 -43.52(19) . . . . ? Cr1 P2 C16 C21 96.24(18) . . . . ? C21 C16 C17 C18 1.1(3) . . . . ? P2 C16 C17 C18 174.58(18) . . . . ? C16 C17 C18 C19 -1.6(4) . . . . ? C17 C18 C19 C20 0.9(4) . . . . ? C18 C19 C20 C21 0.3(4) . . . . ? C19 C20 C21 C16 -0.8(4) . . . . ? C17 C16 C21 C20 0.1(3) . . . . ? P2 C16 C21 C20 -173.52(18) . . . . ? N1 P2 C22 C27 -127.6(2) . . . . ? C16 P2 C22 C27 120.6(2) . . . . ? Cr1 P2 C22 C27 -16.7(2) . . . . ? N1 P2 C22 C23 56.7(2) . . . . ? C16 P2 C22 C23 -55.1(2) . . . . ? Cr1 P2 C22 C23 167.55(16) . . . . ? C27 C22 C23 C24 1.5(4) . . . . ? P2 C22 C23 C24 177.3(2) . . . . ? C22 C23 C24 C25 -1.0(4) . . . . ? C23 C24 C25 C26 -0.5(4) . . . . ? C24 C25 C26 C27 1.5(4) . . . . ? C23 C22 C27 C26 -0.5(4) . . . . ? P2 C22 C27 C26 -176.30(19) . . . . ? C25 C26 C27 C22 -1.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.413 _refine_diff_density_min -0.456 _refine_diff_density_rms 0.075