Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Andy Hor' _publ_contact_author_address ; Department of Chemistry National University of Singapore 10 Kent Ridge, Crescent 117543 SINGAPORE ; _publ_contact_author_email ANDYHOR@NUS.EDU.SG _publ_section_title ; Chromium(III) catalysed ethylene tetramerization promoted by bis(phosphino)amines with an N-functionalised pendant ; loop_ _publ_author_name 'Hor Andy' 'Shihui Teo.' 'Weng Zhiqiang.' data_6192a _database_code_depnum_ccdc_archive 'CCDC 637514' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H29 N P2 S' _chemical_formula_weight 473.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.2813(10) _cell_length_b 9.8308(8) _cell_length_c 27.659(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2523.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 755 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 25.16 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.246 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 0.271 _exptl_absorpt_correction_type 'Sadabs, (Sheldrick 2001)' _exptl_absorpt_correction_T_min 0.9328 _exptl_absorpt_correction_T_max 0.9839 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6731 _diffrn_reflns_av_R_equivalents 0.0731 _diffrn_reflns_av_sigmaI/netI 0.1150 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3723 _reflns_number_gt 2779 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.The disordered parts C1-C2 and C1x-C2x were refined with the ratio as free-variable and the final ratio is 65/35. The bond lengths involving these disordered atoms were also restraints to avoid too much deviations of the bond lengths and thermal parameters from normal values. ; _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^)+(0.0572P)^2^+2.0786P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(2) _refine_ls_number_reflns 3723 _refine_ls_number_parameters 299 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1113 _refine_ls_R_factor_gt 0.0838 _refine_ls_wR_factor_ref 0.1758 _refine_ls_wR_factor_gt 0.1564 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.7553(6) -0.0189(6) 0.8941(2) 0.0385(16) Uani 1 1 d D . . P1 P 0.87532(19) 0.01402(19) 0.93970(6) 0.0277(5) Uani 1 1 d . A . P2 P 0.83749(19) -0.1058(2) 0.84765(6) 0.0309(5) Uani 1 1 d . A . S3 S 0.2866(3) 0.2034(3) 0.84004(9) 0.0758(9) Uani 1 1 d . A . C1 C 0.5973(9) -0.0097(11) 0.9016(4) 0.038(4) Uani 0.664(15) 1 d PD A 1 H1A H 0.5770 0.0091 0.9357 0.046 Uiso 0.664(15) 1 calc PR A 1 H1B H 0.5522 -0.0966 0.8931 0.046 Uiso 0.664(15) 1 calc PR A 1 C2 C 0.5341(10) 0.1040(11) 0.8701(4) 0.042(4) Uani 0.664(15) 1 d PD A 1 H2A H 0.5359 0.0780 0.8359 0.051 Uiso 0.664(15) 1 calc PR A 1 H2B H 0.5891 0.1883 0.8741 0.051 Uiso 0.664(15) 1 calc PR A 1 C1X C 0.6290(16) 0.0711(19) 0.8810(7) 0.033(7) Uiso 0.336(15) 1 d PD A 2 H1X1 H 0.6167 0.0716 0.8458 0.040 Uiso 0.336(15) 1 calc PR A 2 H1X2 H 0.6490 0.1645 0.8914 0.040 Uiso 0.336(15) 1 calc PR A 2 C2X C 0.4893(17) 0.021(2) 0.9049(9) 0.052(9) Uiso 0.336(15) 1 d PD A 2 H2X1 H 0.4654 -0.0711 0.8943 0.062 Uiso 0.336(15) 1 calc PR A 2 H2X2 H 0.4980 0.0220 0.9402 0.062 Uiso 0.336(15) 1 calc PR A 2 C3 C 0.3749(9) 0.1232(9) 0.8880(3) 0.068(3) Uani 1 1 d D . . H3A H 0.3719 0.1797 0.9171 0.082 Uiso 0.664(15) 1 calc PR A 1 H3B H 0.3304 0.0351 0.8952 0.082 Uiso 0.664(15) 1 calc PR A 1 H3A' H 0.4052 0.2033 0.9064 0.082 Uiso 0.336(15) 1 calc PR A 2 H3B' H 0.2914 0.0886 0.9058 0.082 Uiso 0.336(15) 1 calc PR A 2 C4 C 0.2321(10) 0.0610(9) 0.8048(4) 0.076(3) Uani 1 1 d . . . H4A H 0.3155 0.0220 0.7889 0.114 Uiso 1 1 calc R A . H4B H 0.1627 0.0901 0.7807 0.114 Uiso 1 1 calc R . . H4C H 0.1883 -0.0067 0.8257 0.114 Uiso 1 1 calc R . . C1A C 0.8529(7) 0.1948(7) 0.9518(2) 0.0270(17) Uani 1 1 d . . . C2A C 0.7466(8) 0.2537(8) 0.9800(3) 0.039(2) Uani 1 1 d . A . H2A1 H 0.6759 0.1982 0.9942 0.046 Uiso 1 1 calc R . . C3A C 0.7424(9) 0.3922(9) 0.9876(3) 0.047(2) Uani 1 1 d . . . H3A1 H 0.6682 0.4303 1.0063 0.057 Uiso 1 1 calc R A . C4A C 0.8446(9) 0.4733(8) 0.9681(3) 0.048(2) Uani 1 1 d . A . H4A1 H 0.8423 0.5674 0.9743 0.057 Uiso 1 1 calc R . . C5A C 0.9517(9) 0.4208(7) 0.9395(3) 0.039(2) Uani 1 1 d . . . H5A H 1.0218 0.4782 0.9259 0.047 Uiso 1 1 calc R A . C6A C 0.9551(7) 0.2801(7) 0.9308(2) 0.0292(17) Uani 1 1 d . A . H6A H 1.0269 0.2433 0.9107 0.035 Uiso 1 1 calc R . . C1B C 0.7985(7) -0.0638(6) 0.9940(2) 0.0276(18) Uani 1 1 d . . . C2B C 0.7022(9) -0.1725(7) 0.9903(3) 0.045(2) Uani 1 1 d . A . H2B1 H 0.6641 -0.1984 0.9602 0.054 Uiso 1 1 calc R . . C3B C 0.6640(11) -0.2415(8) 1.0322(3) 0.062(3) Uani 1 1 d . . . H3B1 H 0.5980 -0.3136 1.0298 0.075 Uiso 1 1 calc R A . C4B C 0.7179(12) -0.2094(12) 1.0768(3) 0.077(3) Uani 1 1 d . A . H4B1 H 0.6909 -0.2581 1.1046 0.092 Uiso 1 1 calc R . . C5B C 0.8111(12) -0.1051(11) 1.0790(3) 0.072(3) Uani 1 1 d . . . H5B H 0.8510 -0.0823 1.1091 0.086 Uiso 1 1 calc R A . C6B C 0.8519(9) -0.0286(9) 1.0386(3) 0.051(2) Uani 1 1 d . A . H6B H 0.9148 0.0457 1.0420 0.061 Uiso 1 1 calc R . . C1C C 0.8321(7) 0.0102(7) 0.7963(2) 0.0303(16) Uani 1 1 d . . . C2C C 0.8441(8) 0.1506(7) 0.8041(3) 0.0379(19) Uani 1 1 d . A . H2C H 0.8353 0.1866 0.8354 0.046 Uiso 1 1 calc R . . C3C C 0.8690(9) 0.2358(9) 0.7651(3) 0.051(2) Uani 1 1 d . . . H3C H 0.8775 0.3298 0.7707 0.061 Uiso 1 1 calc R A . C4C C 0.8818(9) 0.1877(10) 0.7188(3) 0.054(2) Uani 1 1 d . A . H4C1 H 0.8994 0.2471 0.6928 0.065 Uiso 1 1 calc R . . C5C C 0.8682(9) 0.0506(9) 0.7116(3) 0.050(2) Uani 1 1 d . . . H5C H 0.8769 0.0160 0.6800 0.060 Uiso 1 1 calc R A . C6C C 0.8417(7) -0.0394(8) 0.7496(2) 0.0363(19) Uani 1 1 d . A . H6C H 0.8306 -0.1329 0.7435 0.044 Uiso 1 1 calc R . . C1D C 0.7102(8) -0.2384(7) 0.8308(2) 0.0311(18) Uani 1 1 d . . . C2D C 0.5927(8) -0.2277(10) 0.8005(3) 0.046(2) Uani 1 1 d . A . H2D H 0.5701 -0.1426 0.7870 0.055 Uiso 1 1 calc R . . C3D C 0.5074(9) -0.3386(11) 0.7896(3) 0.057(3) Uani 1 1 d . . . H3D H 0.4288 -0.3285 0.7684 0.069 Uiso 1 1 calc R A . C4D C 0.5371(11) -0.4647(11) 0.8097(3) 0.067(3) Uani 1 1 d . A . H4D H 0.4791 -0.5404 0.8025 0.080 Uiso 1 1 calc R . . C5D C 0.6512(11) -0.4770(10) 0.8400(3) 0.068(3) Uani 1 1 d . . . H5D H 0.6715 -0.5621 0.8539 0.082 Uiso 1 1 calc R A . C6D C 0.7381(10) -0.3676(8) 0.8507(3) 0.052(2) Uani 1 1 d . A . H6D H 0.8169 -0.3792 0.8716 0.062 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.025(3) 0.050(4) 0.041(4) -0.019(3) -0.002(3) 0.001(3) P1 0.0290(10) 0.0307(11) 0.0235(9) -0.0010(8) 0.0015(8) -0.0012(10) P2 0.0266(10) 0.0436(12) 0.0224(9) -0.0037(9) -0.0015(8) 0.0011(10) S3 0.090(2) 0.0827(19) 0.0546(15) 0.0113(14) -0.0099(14) -0.0286(16) C1 0.045(8) 0.046(8) 0.024(6) -0.001(6) 0.008(5) 0.005(7) C2 0.041(8) 0.041(8) 0.045(7) -0.008(6) -0.002(6) 0.026(7) C3 0.069(7) 0.067(7) 0.069(6) -0.004(5) -0.013(5) 0.034(6) C4 0.063(6) 0.074(7) 0.092(7) -0.007(6) -0.015(6) -0.017(6) C1A 0.023(4) 0.033(4) 0.025(4) -0.007(3) -0.007(3) -0.001(4) C2A 0.035(5) 0.032(5) 0.049(5) -0.007(4) 0.001(4) -0.005(4) C3A 0.046(5) 0.052(6) 0.044(5) -0.005(4) 0.001(4) 0.012(5) C4A 0.054(5) 0.030(5) 0.060(5) -0.004(4) -0.008(5) 0.001(5) C5A 0.048(5) 0.019(5) 0.051(5) 0.006(4) -0.002(4) -0.010(4) C6A 0.024(4) 0.036(5) 0.028(4) -0.004(3) -0.008(3) 0.005(4) C1B 0.030(4) 0.020(4) 0.033(4) 0.006(3) 0.008(3) -0.005(3) C2B 0.053(5) 0.027(5) 0.055(5) 0.009(4) 0.032(4) -0.002(4) C3B 0.082(7) 0.012(5) 0.092(7) 0.007(4) 0.051(6) 0.007(5) C4B 0.091(9) 0.082(8) 0.058(7) 0.025(6) 0.043(6) 0.015(7) C5B 0.083(8) 0.093(8) 0.038(5) 0.009(5) 0.006(5) 0.017(7) C6B 0.054(5) 0.065(6) 0.033(4) 0.004(4) -0.001(4) -0.004(5) C1C 0.027(4) 0.027(4) 0.037(4) 0.000(3) 0.002(3) -0.007(4) C2C 0.036(5) 0.034(5) 0.044(5) -0.002(4) -0.001(4) -0.005(4) C3C 0.040(5) 0.042(6) 0.072(6) 0.003(4) -0.013(5) -0.002(5) C4C 0.038(5) 0.071(7) 0.053(6) 0.018(5) 0.008(4) -0.011(5) C5C 0.051(5) 0.064(6) 0.034(5) -0.002(4) 0.005(4) -0.005(5) C6C 0.028(4) 0.044(5) 0.037(4) -0.004(4) 0.002(4) -0.008(4) C1D 0.035(4) 0.034(5) 0.024(4) -0.017(3) 0.002(3) -0.003(4) C2D 0.033(5) 0.066(6) 0.038(5) 0.003(4) 0.002(4) -0.006(5) C3D 0.044(5) 0.090(9) 0.038(5) -0.015(5) 0.005(4) -0.027(6) C4D 0.086(8) 0.061(7) 0.054(6) -0.015(5) 0.021(6) -0.045(6) C5D 0.081(7) 0.059(6) 0.065(6) -0.004(5) 0.001(6) -0.029(6) C6D 0.061(6) 0.048(6) 0.047(5) 0.002(4) -0.008(5) -0.009(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 N1 C1 1.483(8) . ? N1 C1X 1.512(10) . ? N1 P1 1.714(6) . ? N1 P2 1.721(5) . ? P1 C1A 1.820(7) . ? P1 C1B 1.829(6) . ? P2 C1D 1.820(7) . ? P2 C1C 1.821(7) . ? S3 C3 1.747(8) . ? S3 C4 1.779(9) . ? C1 C2 1.534(9) . ? C2 C3 1.569(8) . ? C1X C2X 1.537(10) . ? C2X C3 1.533(10) . ? C1A C2A 1.384(9) . ? C1A C6A 1.393(9) . ? C2A C3A 1.378(10) . ? C3A C4A 1.352(10) . ? C4A C5A 1.371(11) . ? C5A C6A 1.404(10) . ? C1B C6B 1.376(9) . ? C1B C2B 1.396(9) . ? C2B C3B 1.388(10) . ? C3B C4B 1.368(12) . ? C4B C5B 1.343(13) . ? C5B C6B 1.397(11) . ? C1C C6C 1.385(9) . ? C1C C2C 1.401(9) . ? C2C C3C 1.383(10) . ? C3C C4C 1.371(10) . ? C4C C5C 1.368(11) . ? C5C C6C 1.396(10) . ? C1D C2D 1.378(10) . ? C1D C6D 1.409(10) . ? C2D C3D 1.381(11) . ? C3D C4D 1.387(13) . ? C4D C5D 1.355(13) . ? C5D C6D 1.377(11) . ? 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 C1 N1 C1X 39.9(8) . . ? C1 N1 P1 121.9(6) . . ? C1X N1 P1 124.7(9) . . ? C1 N1 P2 124.9(6) . . ? C1X N1 P2 117.1(9) . . ? P1 N1 P2 110.8(3) . . ? N1 P1 C1A 104.2(3) . . ? N1 P1 C1B 105.8(3) . . ? C1A P1 C1B 102.3(3) . . ? N1 P2 C1D 105.0(3) . . ? N1 P2 C1C 105.0(3) . . ? C1D P2 C1C 103.3(3) . . ? C3 S3 C4 101.2(5) . . ? N1 C1 C2 110.1(7) . . ? C1 C2 C3 105.6(7) . . ? N1 C1X C2X 111.3(11) . . ? C3 C2X C1X 104.1(10) . . ? C2X C3 C2 50.7(8) . . ? C2X C3 S3 148.4(11) . . ? C2 C3 S3 104.9(6) . . ? C2A C1A C6A 117.9(6) . . ? C2A C1A P1 126.4(6) . . ? C6A C1A P1 115.7(5) . . ? C3A C2A C1A 121.3(7) . . ? C4A C3A C2A 120.1(8) . . ? C3A C4A C5A 121.1(7) . . ? C4A C5A C6A 119.1(7) . . ? C1A C6A C5A 120.4(7) . . ? C6B C1B C2B 119.2(7) . . ? C6B C1B P1 119.4(6) . . ? C2B C1B P1 120.7(5) . . ? C3B C2B C1B 118.5(8) . . ? C4B C3B C2B 123.1(9) . . ? C5B C4B C3B 116.8(9) . . ? C4B C5B C6B 123.4(9) . . ? C1B C6B C5B 118.9(8) . . ? C6C C1C C2C 119.0(7) . . ? C6C C1C P2 120.4(6) . . ? C2C C1C P2 119.7(5) . . ? C3C C2C C1C 119.4(7) . . ? C4C C3C C2C 122.2(8) . . ? C5C C4C C3C 117.9(8) . . ? C4C C5C C6C 122.1(8) . . ? C1C C6C C5C 119.4(7) . . ? C2D C1D C6D 116.8(7) . . ? C2D C1D P2 127.9(6) . . ? C6D C1D P2 115.2(6) . . ? C1D C2D C3D 121.8(8) . . ? C2D C3D C4D 120.3(9) . . ? C5D C4D C3D 118.9(9) . . ? C4D C5D C6D 121.4(9) . . ? C5D C6D C1D 120.8(8) . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 0.447 _refine_diff_density_min -0.382 _refine_diff_density_rms 0.078 # Attachment 'compound_3a.cif' data_6150 _database_code_depnum_ccdc_archive 'CCDC 637515' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H32 Cl3 Cr N2 P2 S' _chemical_formula_weight 672.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.3331(13) _cell_length_b 16.3009(19) _cell_length_c 17.286(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.248(4) _cell_angle_gamma 90.00 _cell_volume 3151.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 618 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 16.79 _exptl_crystal_description Block _exptl_crystal_colour 'gray Blue' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.418 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1388 _exptl_absorpt_coefficient_mu 0.808 _exptl_absorpt_correction_type 'Sadabs, (Sheldrick 2001)' _exptl_absorpt_correction_T_min 0.9235 _exptl_absorpt_correction_T_max 0.9840 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18076 _diffrn_reflns_av_R_equivalents 0.1524 _diffrn_reflns_av_sigmaI/netI 0.1569 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5559 _reflns_number_gt 3140 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The Cl/acetonitrile disordered pair occupancy ratio was refined as a free variable. Restraints were also applied to the bond lengths and thermalparameters of the acetonitrile as these did not behave well during refinement. ; _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^)+(0.0468P)^2^+15.4173P] 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 5559 _refine_ls_number_parameters 377 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.1918 _refine_ls_R_factor_gt 0.1172 _refine_ls_wR_factor_ref 0.2264 _refine_ls_wR_factor_gt 0.1964 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N3 N 0.604(4) 1.036(4) 0.884(3) 0.06(3) Uiso 0.386(11) 1 d PD A -2 C3N C 0.695(2) 1.0516(16) 0.9211(14) 0.041(7) Uiso 0.386(11) 1 d PD A -2 C4N C 0.804(2) 1.074(2) 0.9774(18) 0.068(10) Uiso 0.386(11) 1 d PD A -2 H4N1 H 0.8575 1.1057 0.9507 0.101 Uiso 0.386(11) 1 calc PR A -2 H4N2 H 0.8441 1.0243 0.9986 0.101 Uiso 0.386(11) 1 calc PR A -2 H4N3 H 0.7810 1.1061 1.0197 0.101 Uiso 0.386(11) 1 calc PR A -2 C2N C 0.1717(15) 0.9577(14) 0.9567(11) 0.064(6) Uani 0.614(11) 1 d PDU A -1 H2N1 H 0.1875 0.9877 1.0057 0.097 Uiso 0.614(11) 1 calc PR A -1 H2N2 H 0.1705 0.8994 0.9674 0.097 Uiso 0.614(11) 1 calc PR A -1 H2N3 H 0.0949 0.9743 0.9278 0.097 Uiso 0.614(11) 1 calc PR A -1 C1N C 0.2668(12) 0.9756(9) 0.9095(8) 0.029(4) Uani 0.614(11) 1 d PDU A -1 N2 N 0.341(2) 0.9922(14) 0.8723(11) 0.029(6) Uani 0.614(11) 1 d PDU A -1 Cl2 Cl 0.6093(7) 1.0235(8) 0.8975(7) 0.047(2) Uani 0.614(11) 1 d P A -1 Cl2A Cl 0.3513(11) 1.0130(8) 0.8953(7) 0.047(3) Uani 0.386(11) 1 d P A 2 Cr1 Cr 0.46030(14) 1.00817(9) 0.79634(9) 0.0309(4) Uani 1 1 d . . . P1 P 0.2967(2) 0.94411(15) 0.70361(15) 0.0301(6) Uani 1 1 d . A . Cl1 Cl 0.5900(2) 1.00543(16) 0.70731(14) 0.0419(7) Uani 1 1 d . A . P2 P 0.4695(2) 0.85610(15) 0.79447(15) 0.0317(6) Uani 1 1 d . A . Cl3 Cl 0.4011(3) 1.14059(16) 0.76539(17) 0.0544(8) Uani 1 1 d . A . S1 S 0.3941(4) 0.6785(3) 0.4639(2) 0.0985(14) Uani 1 1 d . . . C1B C 0.2636(8) 0.9643(5) 0.5987(6) 0.033(2) Uani 1 1 d . . . N1 N 0.3569(7) 0.8491(4) 0.7177(4) 0.0323(19) Uani 1 1 d . . . C2A C 0.0973(9) 1.0206(7) 0.7350(6) 0.049(3) Uani 1 1 d . A . H2A H 0.1376 1.0675 0.7214 0.059 Uiso 1 1 calc R . . C1C C 0.4309(9) 0.8026(6) 0.8795(6) 0.036(2) Uani 1 1 d . . . C4B C 0.2202(10) 0.9915(7) 0.4373(6) 0.048(3) Uani 1 1 d . A . H4B H 0.2076 0.9995 0.3827 0.058 Uiso 1 1 calc R . . C3C C 0.4754(12) 0.7827(7) 1.0191(7) 0.065(4) Uani 1 1 d . . . H3C H 0.5147 0.7992 1.0687 0.078 Uiso 1 1 calc R A . C1D C 0.5902(8) 0.7951(6) 0.7675(6) 0.034(2) Uani 1 1 d . . . C6C C 0.3551(10) 0.7368(6) 0.8758(6) 0.045(3) Uani 1 1 d . A . H6C H 0.3124 0.7201 0.8271 0.054 Uiso 1 1 calc R . . C1 C 0.3186(11) 0.7720(7) 0.6726(6) 0.051(3) Uani 1 1 d . A . H1A H 0.2329 0.7640 0.6725 0.061 Uiso 1 1 calc R . . H1B H 0.3605 0.7255 0.7006 0.061 Uiso 1 1 calc R . . C1A C 0.1498(8) 0.9444(6) 0.7325(5) 0.032(2) Uani 1 1 d . . . C2B C 0.1565(9) 0.9405(7) 0.5544(6) 0.050(3) Uani 1 1 d . A . H2B H 0.0984 0.9144 0.5790 0.060 Uiso 1 1 calc R . . C6B C 0.3481(9) 1.0040(6) 0.5610(5) 0.040(3) Uani 1 1 d . A . H6B H 0.4209 1.0222 0.5897 0.049 Uiso 1 1 calc R . . C2D C 0.6526(10) 0.7390(7) 0.8175(7) 0.055(3) Uani 1 1 d . A . H2D H 0.6330 0.7326 0.8679 0.066 Uiso 1 1 calc R . . C6D C 0.6221(10) 0.8049(6) 0.6930(7) 0.050(3) Uani 1 1 d . A . H6D H 0.5827 0.8438 0.6578 0.060 Uiso 1 1 calc R . . C6A C 0.0917(10) 0.8772(7) 0.7525(7) 0.058(3) Uani 1 1 d . A . H6A H 0.1281 0.8254 0.7520 0.070 Uiso 1 1 calc R . . C2C C 0.4916(10) 0.8276(7) 0.9528(6) 0.047(3) Uani 1 1 d . A . H2C H 0.5423 0.8736 0.9572 0.056 Uiso 1 1 calc R . . C5B C 0.3230(10) 1.0156(7) 0.4831(6) 0.050(3) Uani 1 1 d . . . H5B H 0.3807 1.0422 0.4587 0.060 Uiso 1 1 calc R A . C4C C 0.4032(12) 0.7151(7) 1.0126(7) 0.060(4) Uani 1 1 d . A . H4C H 0.3971 0.6830 1.0570 0.072 Uiso 1 1 calc R . . C3B C 0.1339(11) 0.9544(7) 0.4751(6) 0.054(3) Uani 1 1 d . . . H3B H 0.0600 0.9389 0.4460 0.065 Uiso 1 1 calc R A . C3A C -0.0161(10) 1.0285(8) 0.7577(7) 0.061(3) Uani 1 1 d . . . H3A H -0.0519 1.0802 0.7599 0.073 Uiso 1 1 calc R A . C5A C -0.0213(11) 0.8836(9) 0.7737(8) 0.077(4) Uani 1 1 d . . . H5A H -0.0617 0.8363 0.7860 0.093 Uiso 1 1 calc R A . C3D C 0.7422(11) 0.6922(7) 0.7964(8) 0.059(3) Uani 1 1 d . . . H3D H 0.7839 0.6547 0.8321 0.071 Uiso 1 1 calc R A . C5D C 0.7114(10) 0.7571(8) 0.6719(8) 0.065(4) Uani 1 1 d . . . H5D H 0.7324 0.7632 0.6217 0.078 Uiso 1 1 calc R A . C5C C 0.3412(11) 0.6950(8) 0.9429(8) 0.065(4) Uani 1 1 d . . . H5C H 0.2868 0.6511 0.9395 0.077 Uiso 1 1 calc R A . C4D C 0.7708(10) 0.7002(8) 0.7230(9) 0.069(4) Uani 1 1 d . A . H4D H 0.8307 0.6671 0.7074 0.083 Uiso 1 1 calc R . . C4A C -0.0730(10) 0.9583(10) 0.7765(6) 0.063(4) Uani 1 1 d . A . H4A H -0.1489 0.9623 0.7915 0.075 Uiso 1 1 calc R . . C2 C 0.3411(13) 0.7699(7) 0.5884(7) 0.070(4) Uani 1 1 d . . . H2E H 0.2686 0.7879 0.5539 0.084 Uiso 1 1 calc R A . H2F H 0.4050 0.8089 0.5826 0.084 Uiso 1 1 calc R . . C4 C 0.4984(15) 0.7602(11) 0.4541(9) 0.128(7) Uani 1 1 d . . . H4E H 0.4696 0.8109 0.4738 0.192 Uiso 1 1 calc R . . H4F H 0.5055 0.7668 0.3993 0.192 Uiso 1 1 calc R . . H4G H 0.5759 0.7467 0.4839 0.192 Uiso 1 1 calc R . . C3 C 0.3755(16) 0.6869(9) 0.5631(7) 0.099(5) Uani 1 1 d . A . H3E H 0.3140 0.6477 0.5728 0.119 Uiso 1 1 calc R . . H3F H 0.4505 0.6708 0.5960 0.119 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C2N 0.045(10) 0.101(14) 0.051(11) 0.006(10) 0.018(9) -0.014(10) C1N 0.026(7) 0.040(7) 0.023(7) 0.003(6) 0.008(6) -0.013(6) N2 0.039(8) 0.028(9) 0.019(9) -0.001(7) 0.003(7) -0.008(6) Cl2 0.045(4) 0.051(4) 0.039(4) -0.006(4) -0.014(3) -0.009(3) Cl2A 0.045(6) 0.066(8) 0.035(6) -0.010(5) 0.017(5) 0.000(5) Cr1 0.0304(9) 0.0325(9) 0.0296(9) -0.0008(8) 0.0044(7) 0.0025(8) P1 0.0276(14) 0.0303(14) 0.0339(14) 0.0038(12) 0.0093(11) 0.0017(12) Cl1 0.0380(14) 0.0486(16) 0.0423(15) 0.0011(13) 0.0162(12) -0.0063(13) P2 0.0285(14) 0.0340(14) 0.0324(14) 0.0008(12) 0.0047(11) 0.0006(12) Cl3 0.0555(18) 0.0361(15) 0.0655(19) -0.0056(14) -0.0087(15) 0.0103(14) S1 0.112(4) 0.107(3) 0.081(3) -0.026(2) 0.028(3) 0.010(3) C1B 0.030(5) 0.024(5) 0.043(6) 0.006(4) 0.005(5) 0.009(4) N1 0.040(5) 0.028(4) 0.030(4) 0.004(4) 0.009(4) -0.002(4) C2A 0.039(7) 0.048(7) 0.062(8) 0.008(6) 0.015(6) 0.001(6) C1C 0.048(7) 0.028(6) 0.037(6) 0.003(5) 0.018(5) 0.007(5) C4B 0.052(7) 0.068(8) 0.024(5) 0.005(6) 0.006(5) 0.000(6) C3C 0.103(11) 0.051(8) 0.044(8) 0.007(6) 0.019(7) 0.021(8) C1D 0.030(6) 0.025(5) 0.047(6) -0.001(5) 0.005(5) 0.003(4) C6C 0.056(7) 0.044(7) 0.036(6) 0.009(5) 0.010(6) -0.001(6) C1 0.066(8) 0.049(7) 0.040(7) -0.005(5) 0.018(6) -0.011(6) C1A 0.036(6) 0.042(6) 0.018(5) 0.010(4) 0.004(4) 0.000(5) C2B 0.034(6) 0.089(9) 0.028(6) 0.008(6) 0.007(5) 0.002(6) C6B 0.040(6) 0.054(7) 0.029(6) 0.003(5) 0.013(5) 0.003(5) C2D 0.040(7) 0.053(7) 0.070(9) -0.008(6) 0.003(6) 0.020(6) C6D 0.051(7) 0.040(7) 0.062(8) 0.003(6) 0.016(6) 0.005(6) C6A 0.053(8) 0.069(9) 0.057(8) 0.027(7) 0.023(6) 0.009(7) C2C 0.060(8) 0.042(7) 0.041(7) 0.002(5) 0.013(6) 0.004(6) C5B 0.043(7) 0.076(9) 0.033(6) 0.011(6) 0.013(5) 0.007(6) C4C 0.092(11) 0.045(8) 0.047(8) 0.024(6) 0.021(7) 0.026(7) C3B 0.054(8) 0.073(8) 0.032(6) 0.000(6) -0.005(6) 0.013(7) C3A 0.044(7) 0.086(10) 0.056(8) 0.005(7) 0.017(6) 0.027(7) C5A 0.051(8) 0.092(11) 0.100(12) 0.025(9) 0.044(8) -0.005(8) C3D 0.060(8) 0.047(7) 0.067(9) 0.001(6) 0.001(7) 0.009(6) C5D 0.053(8) 0.079(9) 0.075(9) -0.019(8) 0.048(7) 0.010(7) C5C 0.066(9) 0.063(8) 0.072(9) 0.022(7) 0.031(8) -0.009(7) C4D 0.038(7) 0.063(9) 0.109(12) -0.004(8) 0.017(8) 0.023(7) C4A 0.027(6) 0.127(12) 0.038(7) 0.011(8) 0.014(5) 0.006(8) C2 0.101(11) 0.050(8) 0.061(9) -0.016(7) 0.015(8) 0.008(7) C4 0.123(15) 0.182(19) 0.083(12) -0.056(12) 0.023(11) -0.031(14) C3 0.164(17) 0.082(11) 0.055(9) -0.011(8) 0.025(10) -0.015(11) _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 N3 C3N 1.15(2) . ? N3 Cr1 2.09(3) . ? C3N C4N 1.485(19) . ? C2N C1N 1.480(15) . ? C1N N2 1.168(17) . ? N2 Cr1 2.049(18) . ? Cl2 Cr1 2.242(7) . ? Cl2A Cr1 2.267(11) . ? Cr1 Cl1 2.293(3) . ? Cr1 Cl3 2.298(3) . ? Cr1 P1 2.478(3) . ? Cr1 P2 2.482(3) . ? P1 N1 1.694(8) . ? P1 C1A 1.814(10) . ? P1 C1B 1.822(10) . ? P2 N1 1.690(8) . ? P2 C1D 1.812(10) . ? P2 C1C 1.822(10) . ? S1 C3 1.765(13) . ? S1 C4 1.806(17) . ? C1B C2B 1.382(13) . ? C1B C6B 1.400(13) . ? N1 C1 1.506(12) . ? C2A C1A 1.381(13) . ? C2A C3A 1.408(14) . ? C1C C6C 1.369(13) . ? C1C C2C 1.401(14) . ? C4B C5B 1.357(14) . ? C4B C3B 1.398(15) . ? C3C C4C 1.367(16) . ? C3C C2C 1.397(14) . ? C1D C2D 1.373(13) . ? C1D C6D 1.402(14) . ? C6C C5C 1.376(14) . ? C1 C2 1.517(14) . ? C1A C6A 1.351(14) . ? C2B C3B 1.373(13) . ? C6B C5B 1.344(12) . ? C2D C3D 1.366(15) . ? C6D C5D 1.372(14) . ? C6A C5A 1.392(15) . ? C4C C5C 1.335(16) . ? C3A C4A 1.377(16) . ? C5A C4A 1.355(17) . ? C3D C4D 1.365(16) . ? C5D C4D 1.379(16) . ? C2 C3 1.493(16) . ? 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 C3N N3 Cr1 167(6) . . ? N3 C3N C4N 172(5) . . ? N2 C1N C2N 178(2) . . ? C1N N2 Cr1 171.8(17) . . ? N2 Cr1 N3 94.7(19) . . ? N2 Cr1 Cl2 90.4(7) . . ? N3 Cr1 Cl2 7(2) . . ? N2 Cr1 Cl2A 12.6(6) . . ? N3 Cr1 Cl2A 84.4(19) . . ? Cl2 Cr1 Cl2A 80.9(4) . . ? N2 Cr1 Cl1 171.4(6) . . ? N3 Cr1 Cl1 88.9(19) . . ? Cl2 Cr1 Cl1 92.4(3) . . ? Cl2A Cr1 Cl1 173.3(3) . . ? N2 Cr1 Cl3 94.0(7) . . ? N3 Cr1 Cl3 97.4(19) . . ? Cl2 Cr1 Cl3 103.5(4) . . ? Cl2A Cr1 Cl3 88.2(4) . . ? Cl1 Cr1 Cl3 93.26(12) . . ? N2 Cr1 P1 81.8(6) . . ? N3 Cr1 P1 167.4(19) . . ? Cl2 Cr1 P1 160.6(4) . . ? Cl2A Cr1 P1 93.5(3) . . ? Cl1 Cr1 P1 92.94(10) . . ? Cl3 Cr1 P1 94.88(10) . . ? N2 Cr1 P2 85.1(6) . . ? N3 Cr1 P2 101.4(19) . . ? Cl2 Cr1 P2 95.3(4) . . ? Cl2A Cr1 P2 94.2(4) . . ? Cl1 Cr1 P2 86.50(10) . . ? Cl3 Cr1 P2 161.19(12) . . ? P1 Cr1 P2 66.38(9) . . ? N1 P1 C1A 109.2(4) . . ? N1 P1 C1B 108.8(4) . . ? C1A P1 C1B 102.8(4) . . ? N1 P1 Cr1 92.9(3) . . ? C1A P1 Cr1 116.5(3) . . ? C1B P1 Cr1 125.5(3) . . ? N1 P2 C1D 105.5(4) . . ? N1 P2 C1C 110.6(4) . . ? C1D P2 C1C 103.5(4) . . ? N1 P2 Cr1 92.8(3) . . ? C1D P2 Cr1 125.9(3) . . ? C1C P2 Cr1 116.8(3) . . ? C3 S1 C4 102.5(7) . . ? C2B C1B C6B 118.5(9) . . ? C2B C1B P1 121.5(8) . . ? C6B C1B P1 120.0(7) . . ? C1 N1 P2 125.5(7) . . ? C1 N1 P1 127.8(7) . . ? P2 N1 P1 106.7(4) . . ? C1A C2A C3A 120.5(10) . . ? C6C C1C C2C 118.9(10) . . ? C6C C1C P2 124.5(8) . . ? C2C C1C P2 116.3(8) . . ? C5B C4B C3B 116.8(10) . . ? C4C C3C C2C 120.7(12) . . ? C2D C1D C6D 118.1(10) . . ? C2D C1D P2 122.5(8) . . ? C6D C1D P2 119.4(8) . . ? C1C C6C C5C 120.3(11) . . ? N1 C1 C2 115.8(9) . . ? C6A C1A C2A 119.5(10) . . ? C6A C1A P1 125.1(8) . . ? C2A C1A P1 115.4(7) . . ? C3B C2B C1B 120.8(10) . . ? C5B C6B C1B 118.7(10) . . ? C3D C2D C1D 122.3(12) . . ? C5D C6D C1D 119.4(11) . . ? C1A C6A C5A 120.8(12) . . ? C3C C2C C1C 118.6(11) . . ? C6B C5B C4B 124.6(11) . . ? C5C C4C C3C 119.6(12) . . ? C2B C3B C4B 120.4(11) . . ? C4A C3A C2A 118.2(11) . . ? C4A C5A C6A 119.9(12) . . ? C4D C3D C2D 119.5(12) . . ? C6D C5D C4D 121.0(12) . . ? C4C C5C C6C 121.6(12) . . ? C3D C4D C5D 119.7(11) . . ? C5A C4A C3A 121.0(11) . . ? C3 C2 C1 113.2(10) . . ? C2 C3 S1 115.6(10) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.610 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.103 # Attachment 'compound_3b.cif' data_6246 _database_code_depnum_ccdc_archive 'CCDC 637516' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H34 Cl3 Cr N2 P2 S' _chemical_formula_weight 686.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 11.213(2) _cell_length_b 16.453(3) _cell_length_c 34.766(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6414(2) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 1629 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 20.36 _exptl_crystal_description NEEDLE _exptl_crystal_colour BLUE _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.423 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2840 _exptl_absorpt_coefficient_mu 0.796 _exptl_absorpt_correction_type 'Sadabs, (sheldrick 2001)' _exptl_absorpt_correction_T_min 0.8700 _exptl_absorpt_correction_T_max 0.9843 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35350 _diffrn_reflns_av_R_equivalents 0.1304 _diffrn_reflns_av_sigmaI/netI 0.0807 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5646 _reflns_number_gt 4232 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+12.9333P] 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 5646 _refine_ls_number_parameters 363 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1024 _refine_ls_R_factor_gt 0.0713 _refine_ls_wR_factor_ref 0.1432 _refine_ls_wR_factor_gt 0.1314 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1 Cr 0.53924(7) 0.50233(5) 0.09892(2) 0.0211(2) Uani 1 1 d . . . P1 P 0.69041(12) 0.56715(8) 0.14246(4) 0.0202(3) Uani 1 1 d . . . P2 P 0.53182(11) 0.65181(8) 0.09948(4) 0.0198(3) Uani 1 1 d . . . S1 S 0.59600(15) 0.84908(9) 0.26078(4) 0.0418(4) Uani 1 1 d . . . Cl1 Cl 0.39908(11) 0.50063(8) 0.14563(4) 0.0288(3) Uani 1 1 d . . . Cl2 Cl 0.59723(13) 0.36904(8) 0.10980(4) 0.0389(4) Uani 1 1 d . . . Cl3 Cl 0.40053(13) 0.48799(9) 0.05074(4) 0.0377(4) Uani 1 1 d . . . N1 N 0.6325(3) 0.6615(2) 0.13573(11) 0.0187(9) Uani 1 1 d . . . N2 N 0.6690(4) 0.5119(2) 0.05812(12) 0.0266(10) Uani 1 1 d . . . C1 C 0.6585(5) 0.7396(3) 0.15555(14) 0.0264(12) Uani 1 1 d . . . H1A H 0.6162 0.7830 0.1419 0.032 Uiso 1 1 calc R . . H1B H 0.7440 0.7506 0.1531 0.032 Uiso 1 1 calc R . . C2 C 0.6254(5) 0.7445(3) 0.19784(14) 0.0314(13) Uani 1 1 d . . . H2A H 0.5506 0.7152 0.2023 0.038 Uiso 1 1 calc R . . H2B H 0.6878 0.7187 0.2134 0.038 Uiso 1 1 calc R . . C3 C 0.6113(5) 0.8318(3) 0.20972(15) 0.0330(13) Uani 1 1 d . . . H3A H 0.5409 0.8541 0.1968 0.040 Uiso 1 1 calc R . . H3B H 0.6808 0.8623 0.2005 0.040 Uiso 1 1 calc R . . C4 C 0.4619(7) 0.7959(5) 0.2717(2) 0.081(3) Uani 1 1 d . . . H4A H 0.3993 0.8133 0.2542 0.121 Uiso 1 1 calc R . . H4B H 0.4383 0.8076 0.2980 0.121 Uiso 1 1 calc R . . H4C H 0.4749 0.7380 0.2688 0.121 Uiso 1 1 calc R . . C5 C 0.7455(5) 0.5163(3) 0.03703(15) 0.0286(12) Uani 1 1 d . . . C6 C 0.8478(5) 0.5219(4) 0.01117(19) 0.0468(17) Uani 1 1 d . . . H6A H 0.8345 0.4864 -0.0110 0.056 Uiso 1 1 calc R . . H6B H 0.9192 0.5027 0.0246 0.056 Uiso 1 1 calc R . . C7 C 0.8684(6) 0.6069(4) -0.0026(2) 0.0531(18) Uani 1 1 d . . . H7A H 0.7984 0.6259 -0.0163 0.080 Uiso 1 1 calc R . . H7B H 0.9368 0.6078 -0.0197 0.080 Uiso 1 1 calc R . . H7C H 0.8834 0.6420 0.0193 0.080 Uiso 1 1 calc R . . C1A C 0.8445(4) 0.5662(3) 0.12607(14) 0.0240(12) Uani 1 1 d . . . C2A C 0.9002(5) 0.4908(4) 0.12645(18) 0.0449(16) Uani 1 1 d . . . H2A1 H 0.8569 0.4445 0.1338 0.054 Uiso 1 1 calc R . . C3A C 1.0185(6) 0.4831(5) 0.1161(2) 0.067(2) Uani 1 1 d . . . H3A1 H 1.0556 0.4319 0.1165 0.080 Uiso 1 1 calc R . . C4A C 1.0826(6) 0.5519(5) 0.1051(2) 0.062(2) Uani 1 1 d . . . H4A1 H 1.1637 0.5476 0.0985 0.074 Uiso 1 1 calc R . . C5A C 1.0264(6) 0.6260(5) 0.10390(19) 0.0554(19) Uani 1 1 d . . . H5A H 1.0690 0.6723 0.0960 0.066 Uiso 1 1 calc R . . C6A C 0.9070(5) 0.6334(4) 0.11427(17) 0.0401(15) Uani 1 1 d . . . H6A1 H 0.8693 0.6843 0.1132 0.048 Uiso 1 1 calc R . . C1B C 0.7079(4) 0.5518(3) 0.19384(14) 0.0233(12) Uani 1 1 d . . . C2B C 0.8077(5) 0.5794(3) 0.21330(15) 0.0322(13) Uani 1 1 d . . . H2B1 H 0.8717 0.6019 0.1994 0.039 Uiso 1 1 calc R . . C3B C 0.8145(5) 0.5744(4) 0.25286(16) 0.0428(15) Uani 1 1 d . . . H3B1 H 0.8830 0.5932 0.2657 0.051 Uiso 1 1 calc R . . C4B C 0.7222(6) 0.5422(4) 0.27341(17) 0.0447(16) Uani 1 1 d . . . H4B1 H 0.7258 0.5402 0.3004 0.054 Uiso 1 1 calc R . . C5B C 0.6249(6) 0.5129(4) 0.25448(17) 0.0496(18) Uani 1 1 d . . . H5B H 0.5629 0.4886 0.2686 0.060 Uiso 1 1 calc R . . C6B C 0.6160(5) 0.5183(3) 0.21489(16) 0.0357(14) Uani 1 1 d . . . H6B1 H 0.5472 0.4992 0.2023 0.043 Uiso 1 1 calc R . . C1C C 0.5856(4) 0.7042(3) 0.05662(14) 0.0222(11) Uani 1 1 d . . . C2C C 0.5384(5) 0.6813(3) 0.02142(14) 0.0272(12) Uani 1 1 d . . . H2C H 0.4821 0.6391 0.0200 0.033 Uiso 1 1 calc R . . C3C C 0.5749(5) 0.7212(3) -0.01178(15) 0.0340(14) Uani 1 1 d . . . H3C H 0.5412 0.7071 -0.0356 0.041 Uiso 1 1 calc R . . C4C C 0.6596(5) 0.7808(3) -0.00992(15) 0.0325(13) Uani 1 1 d . . . H4C1 H 0.6835 0.8077 -0.0325 0.039 Uiso 1 1 calc R . . C5C C 0.7104(5) 0.8021(3) 0.02507(15) 0.0302(13) Uani 1 1 d . . . H5C H 0.7703 0.8420 0.0260 0.036 Uiso 1 1 calc R . . C6C C 0.6732(5) 0.7647(3) 0.05837(15) 0.0275(12) Uani 1 1 d . . . H6C H 0.7064 0.7797 0.0822 0.033 Uiso 1 1 calc R . . C1D C 0.4039(4) 0.7106(3) 0.11476(14) 0.0230(11) Uani 1 1 d . . . C2D C 0.3496(5) 0.7686(3) 0.09123(15) 0.0298(13) Uani 1 1 d . . . H2D H 0.3787 0.7777 0.0662 0.036 Uiso 1 1 calc R . . C3D C 0.2534(5) 0.8124(3) 0.10457(17) 0.0358(14) Uani 1 1 d . . . H3D H 0.2169 0.8510 0.0885 0.043 Uiso 1 1 calc R . . C4D C 0.2108(5) 0.8003(3) 0.14083(17) 0.0352(14) Uani 1 1 d . . . H4D H 0.1462 0.8314 0.1498 0.042 Uiso 1 1 calc R . . C5D C 0.2623(5) 0.7425(3) 0.16451(17) 0.0388(15) Uani 1 1 d . . . H5D H 0.2323 0.7340 0.1894 0.047 Uiso 1 1 calc R . . C6D C 0.3579(5) 0.6976(3) 0.15145(15) 0.0302(13) Uani 1 1 d . . . H6D H 0.3922 0.6578 0.1674 0.036 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0223(4) 0.0194(4) 0.0214(4) -0.0009(3) 0.0044(4) -0.0015(4) P1 0.0211(7) 0.0195(7) 0.0199(7) 0.0031(5) 0.0004(6) 0.0016(6) P2 0.0212(7) 0.0211(7) 0.0171(7) 0.0011(5) -0.0009(6) 0.0018(6) S1 0.0575(10) 0.0409(9) 0.0270(8) -0.0099(7) -0.0034(8) 0.0086(8) Cl1 0.0258(7) 0.0359(8) 0.0248(7) -0.0003(6) 0.0081(6) -0.0015(6) Cl2 0.0391(8) 0.0234(7) 0.0543(10) 0.0052(6) 0.0124(7) 0.0053(6) Cl3 0.0416(8) 0.0445(9) 0.0269(7) -0.0030(6) -0.0040(7) -0.0165(7) N1 0.022(2) 0.013(2) 0.021(2) -0.0036(17) -0.0049(18) 0.0016(17) N2 0.031(3) 0.023(2) 0.025(2) -0.0014(19) 0.008(2) -0.001(2) C1 0.032(3) 0.022(3) 0.025(3) -0.005(2) -0.007(2) -0.004(2) C2 0.047(4) 0.027(3) 0.020(3) -0.003(2) -0.001(3) 0.002(3) C3 0.045(4) 0.032(3) 0.022(3) -0.001(2) -0.003(3) 0.005(3) C4 0.103(7) 0.086(6) 0.054(5) -0.013(4) 0.034(5) -0.028(5) C5 0.037(3) 0.024(3) 0.025(3) 0.001(2) -0.003(3) 0.000(3) C6 0.034(3) 0.053(4) 0.053(4) 0.013(3) 0.024(3) 0.004(3) C7 0.045(4) 0.047(4) 0.067(5) 0.018(3) 0.021(4) 0.001(3) C1A 0.020(3) 0.031(3) 0.021(3) 0.002(2) -0.001(2) 0.002(2) C2A 0.031(3) 0.045(4) 0.059(4) 0.015(3) 0.014(3) 0.012(3) C3A 0.045(4) 0.082(6) 0.074(5) 0.017(4) 0.018(4) 0.035(4) C4A 0.026(3) 0.107(7) 0.053(5) -0.006(4) 0.005(3) 0.006(4) C5A 0.036(4) 0.078(5) 0.053(4) -0.001(4) 0.014(3) -0.012(4) C6A 0.034(3) 0.037(3) 0.049(4) 0.001(3) 0.010(3) -0.002(3) C1B 0.024(3) 0.020(3) 0.026(3) 0.005(2) -0.003(2) 0.003(2) C2B 0.031(3) 0.038(3) 0.028(3) 0.001(3) -0.001(3) -0.004(3) C3B 0.039(4) 0.057(4) 0.033(3) -0.002(3) -0.010(3) 0.000(3) C4B 0.047(4) 0.061(4) 0.026(3) 0.006(3) -0.007(3) 0.002(3) C5B 0.044(4) 0.077(5) 0.028(3) 0.016(3) -0.005(3) -0.017(3) C6B 0.030(3) 0.049(4) 0.029(3) 0.009(3) -0.007(3) -0.011(3) C1C 0.026(3) 0.018(3) 0.022(3) 0.000(2) 0.000(2) 0.003(2) C2C 0.032(3) 0.026(3) 0.023(3) -0.001(2) 0.000(2) 0.002(2) C3C 0.047(4) 0.038(3) 0.018(3) 0.000(2) -0.002(3) 0.008(3) C4C 0.042(3) 0.030(3) 0.025(3) 0.008(2) 0.013(3) 0.007(3) C5C 0.032(3) 0.022(3) 0.036(3) 0.002(2) 0.008(3) -0.005(2) C6C 0.032(3) 0.027(3) 0.023(3) -0.002(2) 0.002(2) 0.001(2) C1D 0.019(3) 0.029(3) 0.021(3) -0.004(2) -0.001(2) 0.001(2) C2D 0.032(3) 0.035(3) 0.022(3) -0.001(2) 0.000(2) 0.008(3) C3D 0.030(3) 0.033(3) 0.045(4) 0.003(3) -0.007(3) 0.014(3) C4D 0.028(3) 0.032(3) 0.046(4) -0.005(3) 0.006(3) 0.013(3) C5D 0.044(4) 0.033(3) 0.040(3) 0.001(3) 0.015(3) 0.015(3) C6D 0.033(3) 0.029(3) 0.028(3) 0.007(2) 0.005(3) 0.009(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 Cr1 N2 2.038(4) . ? Cr1 Cl1 2.2600(15) . ? Cr1 Cl3 2.2979(16) . ? Cr1 Cl2 2.3186(16) . ? Cr1 P2 2.4609(15) . ? Cr1 P1 2.5102(15) . ? P1 N1 1.698(4) . ? P1 C1B 1.815(5) . ? P1 C1A 1.820(5) . ? P2 N1 1.700(4) . ? P2 C1D 1.810(5) . ? P2 C1C 1.824(5) . ? S1 C4 1.780(8) . ? S1 C3 1.806(5) . ? N1 C1 1.487(6) . ? N2 C5 1.130(6) . ? C1 C2 1.518(7) . ? C2 C3 1.504(7) . ? C5 C6 1.461(8) . ? C6 C7 1.496(8) . ? C1A C6A 1.372(7) . ? C1A C2A 1.388(7) . ? C2A C3A 1.380(8) . ? C3A C4A 1.394(10) . ? C4A C5A 1.373(10) . ? C5A C6A 1.391(8) . ? C1B C6B 1.378(7) . ? C1B C2B 1.385(7) . ? C2B C3B 1.380(7) . ? C3B C4B 1.365(8) . ? C4B C5B 1.362(8) . ? C5B C6B 1.383(8) . ? C1C C2C 1.385(7) . ? C1C C6C 1.400(7) . ? C2C C3C 1.389(7) . ? C3C C4C 1.367(8) . ? C4C C5C 1.388(7) . ? C5C C6C 1.376(7) . ? C1D C6D 1.392(7) . ? C1D C2D 1.396(7) . ? C2D C3D 1.377(7) . ? C3D C4D 1.363(8) . ? C4D C5D 1.384(8) . ? C5D C6D 1.379(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cr1 Cl1 175.93(13) . . ? N2 Cr1 Cl3 89.07(13) . . ? Cl1 Cr1 Cl3 92.97(6) . . ? N2 Cr1 Cl2 89.21(12) . . ? Cl1 Cr1 Cl2 93.79(6) . . ? Cl3 Cr1 Cl2 102.21(6) . . ? N2 Cr1 P2 87.28(12) . . ? Cl1 Cr1 P2 89.03(5) . . ? Cl3 Cr1 P2 94.90(5) . . ? Cl2 Cr1 P2 162.47(6) . . ? N2 Cr1 P1 84.54(13) . . ? Cl1 Cr1 P1 92.38(5) . . ? Cl3 Cr1 P1 160.08(6) . . ? Cl2 Cr1 P1 96.56(6) . . ? P2 Cr1 P1 66.01(5) . . ? N1 P1 C1B 107.7(2) . . ? N1 P1 C1A 109.1(2) . . ? C1B P1 C1A 101.8(2) . . ? N1 P1 Cr1 92.70(14) . . ? C1B P1 Cr1 127.39(17) . . ? C1A P1 Cr1 116.66(17) . . ? N1 P2 C1D 105.0(2) . . ? N1 P2 C1C 110.0(2) . . ? C1D P2 C1C 104.4(2) . . ? N1 P2 Cr1 94.40(14) . . ? C1D P2 Cr1 124.31(17) . . ? C1C P2 Cr1 117.02(16) . . ? C4 S1 C3 102.3(3) . . ? C1 N1 P1 130.6(3) . . ? C1 N1 P2 123.7(3) . . ? P1 N1 P2 105.7(2) . . ? C5 N2 Cr1 176.2(4) . . ? N1 C1 C2 116.6(4) . . ? C3 C2 C1 110.0(4) . . ? C2 C3 S1 115.5(4) . . ? N2 C5 C6 177.5(6) . . ? C5 C6 C7 112.2(5) . . ? C6A C1A C2A 119.5(5) . . ? C6A C1A P1 124.9(4) . . ? C2A C1A P1 115.6(4) . . ? C3A C2A C1A 120.8(6) . . ? C2A C3A C4A 119.5(7) . . ? C5A C4A C3A 119.5(6) . . ? C4A C5A C6A 120.7(7) . . ? C1A C6A C5A 119.9(6) . . ? C6B C1B C2B 118.4(5) . . ? C6B C1B P1 119.8(4) . . ? C2B C1B P1 121.5(4) . . ? C3B C2B C1B 120.8(5) . . ? C4B C3B C2B 120.2(6) . . ? C5B C4B C3B 119.5(6) . . ? C4B C5B C6B 121.1(6) . . ? C1B C6B C5B 120.0(5) . . ? C2C C1C C6C 120.0(5) . . ? C2C C1C P2 117.9(4) . . ? C6C C1C P2 122.2(4) . . ? C1C C2C C3C 119.6(5) . . ? C4C C3C C2C 120.3(5) . . ? C3C C4C C5C 120.5(5) . . ? C6C C5C C4C 120.0(5) . . ? C5C C6C C1C 119.6(5) . . ? C6D C1D C2D 118.7(5) . . ? C6D C1D P2 118.7(4) . . ? C2D C1D P2 122.6(4) . . ? C3D C2D C1D 120.1(5) . . ? C4D C3D C2D 120.7(5) . . ? C3D C4D C5D 120.3(5) . . ? C6D C5D C4D 119.8(5) . . ? C5D C6D C1D 120.5(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.401 _refine_diff_density_min -0.445 _refine_diff_density_rms 0.088