# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_(1) _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis-Thiocyanato-bis(3,3',5,5'-Tetramethyl-4,4'-bipyrazole)cadmium(II), solvate with 0.66 Dichloromethane ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H28 Cd N10 S2, 0.66(C H2 Cl2)' _chemical_formula_sum 'C22.667 H29.333 Cd Cl1.333 N10 S2' _chemical_formula_weight 665.68 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' Cd Cd -0.8075 1.2024 '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' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3' _space_group_name_Hall '-R 3' _symmetry_Int_Tables_number 148 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 25.791(2) _cell_length_b 25.791(2) _cell_length_c 11.1284(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6410.5(11) _cell_formula_units_Z 9 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 13066 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 27.86 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3042 _exptl_absorpt_coefficient_mu 1.070 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7537 _exptl_absorpt_correction_T_max 0.8144 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'Siemens SMART CCD area-detector diffractometer' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 13066 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0208 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 27.86 _reflns_number_total 3332 _reflns_number_gt 3076 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT (Bruker, 1998)' _computing_cell_refinement 'SAINT-NT (Bruker, 1999)' _computing_data_reduction 'SAINT-NT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.700.00 (Farrugia, 1999)' #------------------------------- Refinement data-----------------------# _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. All non-hydrogen atoms corresponding to the metal-organic framework were refined anisotropically. CH (methyl) and NH hydrogen atoms were added geometrically, with U(iso) = 1.5U(eq) of the parent C (N) atom. In the solvent region, a set of electron density peaks indicated disorder of CH2Cl2 guest across a three-fold axis. At the same time, the guest molecule adopts three orientations, for two of which the carbon atoms reside in special positions. Thus, the partial occupancy factor for the major component of the disorder (Cl1a-C12a-Cl2a) was 0.1667 (half of the occupancy defined by disorder across 3-axis) and the second part was provided by two half-molecules (Cl1b-C12b-Cl1b^v^ and Cl1c-C12c-Cl1c^iv^, symmetry codes: (iv) 1-y, x-y, z; (v) 1-x+y, 1-x, z). In each the case, the geometry of the disorder components was restrained: C-Cl = 1.760(8) A and intramolecular Cl...Cl = 2.883(8) A. Only heavy chlorine atoms were refined anisotropically for the sake of overall convergence, while carbon atoms were left isotropic and the H atoms were not added to this disordered portion. ; _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^)+(0.0369P)^2^+17.7892P] 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_number_reflns 3332 _refine_ls_number_parameters 213 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0807 _refine_ls_wR_factor_gt 0.0786 _refine_ls_goodness_of_fit_ref 1.136 _refine_ls_restrained_S_all 1.143 _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 Cd1 Cd 0.5000 0.0000 0.0000 0.01960(9) Uani 1 2 d S . . S1 S 0.67350(3) 0.19479(3) -0.12476(7) 0.03399(17) Uani 1 1 d . . . N1 N 0.45582(10) 0.05783(9) 0.09100(18) 0.0234(4) Uani 1 1 d . . . N2 N 0.47293(10) 0.11477(9) 0.05646(18) 0.0245(4) Uani 1 1 d . . . H2 H 0.4958 0.1323 -0.0052 0.037 Uiso 1 1 calc R . . N3 N 0.35213(9) 0.13718(9) 0.47586(18) 0.0232(4) Uani 1 1 d . . . N4 N 0.30451(10) 0.08907(10) 0.42472(19) 0.0249(4) Uani 1 1 d . . . H4 H 0.2682 0.0726 0.4528 0.030 Uiso 1 1 calc R . . N5 N 0.56540(10) 0.09032(10) -0.07788(19) 0.0270(5) Uani 1 1 d . . . C2 C 0.42205(11) 0.04885(11) 0.1890(2) 0.0235(5) Uani 1 1 d . . . C3 C 0.41715(11) 0.09988(11) 0.2154(2) 0.0217(5) Uani 1 1 d . . . C4 C 0.45059(12) 0.14130(11) 0.1280(2) 0.0244(5) Uani 1 1 d . . . C5 C 0.46083(16) 0.20232(13) 0.1036(3) 0.0399(7) Uani 1 1 d . . . H5A H 0.4972 0.2317 0.1435 0.060 Uiso 1 1 calc R . . H5B H 0.4272 0.2055 0.1336 0.060 Uiso 1 1 calc R . . H5C H 0.4648 0.2097 0.0177 0.060 Uiso 1 1 calc R . . C1 C 0.39638(15) -0.00864(13) 0.2566(3) 0.0364(7) Uani 1 1 d . . . H1A H 0.3685 -0.0412 0.2055 0.055 Uiso 1 1 calc R . . H1B H 0.3755 -0.0064 0.3272 0.055 Uiso 1 1 calc R . . H1C H 0.4284 -0.0158 0.2811 0.055 Uiso 1 1 calc R . . C9 C 0.31964(12) 0.06970(11) 0.3260(2) 0.0252(5) Uani 1 1 d . . . C8 C 0.38071(11) 0.10612(11) 0.3107(2) 0.0224(5) Uani 1 1 d . . . C7 C 0.39900(12) 0.14816(11) 0.4063(2) 0.0235(5) Uani 1 1 d . . . C6 C 0.46030(12) 0.19836(13) 0.4321(3) 0.0329(6) Uani 1 1 d . . . H6A H 0.4634 0.2358 0.4067 0.049 Uiso 1 1 calc R . . H6B H 0.4894 0.1921 0.3886 0.049 Uiso 1 1 calc R . . H6C H 0.4681 0.1999 0.5176 0.049 Uiso 1 1 calc R . . C10 C 0.27426(13) 0.01860(14) 0.2537(3) 0.0394(7) Uani 1 1 d . . . H10A H 0.2611 -0.0184 0.2976 0.059 Uiso 1 1 calc R . . H10B H 0.2919 0.0168 0.1779 0.059 Uiso 1 1 calc R . . H10C H 0.2403 0.0241 0.2385 0.059 Uiso 1 1 calc R . . C11 C 0.61063(11) 0.13373(11) -0.0969(2) 0.0230(5) Uani 1 1 d . . . C12A C 0.6266(10) 0.2946(15) 0.0545(16) 0.068(8) Uiso 0.1667 1 d PD A -1 Cl1A Cl 0.6967(9) 0.3572(11) 0.0232(13) 0.159(6) Uani 0.1667 1 d PD A -1 Cl2A Cl 0.6188(7) 0.2814(6) 0.2093(16) 0.192(9) Uani 0.1667 1 d PD A -1 C12B C 0.6667(3) 0.3333(3) 0.068(2) 0.11(2) Uiso 0.25 3 d SPD B -2 Cl1B Cl 0.6136(5) 0.2624(2) 0.124(2) 0.118(6) Uani 0.1667 1 d PD B -2 C12C C 0.622(2) 0.3096(13) 0.211(2) 0.049(10) Uiso 0.0833 1 d PD C -3 Cl1C Cl 0.6321(7) 0.2598(2) 0.1198(18) 0.147(9) Uani 0.1667 1 d PD C -3 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 Cd1 0.01864(13) 0.02131(13) 0.01684(13) 0.00067(9) -0.00174(8) 0.00849(10) S1 0.0241(3) 0.0293(3) 0.0372(4) -0.0011(3) 0.0021(3) 0.0048(3) N1 0.0254(10) 0.0254(11) 0.0213(10) 0.0030(8) 0.0040(8) 0.0143(9) N2 0.0271(11) 0.0253(11) 0.0214(10) 0.0041(8) 0.0070(8) 0.0135(9) N3 0.0248(10) 0.0239(10) 0.0210(10) -0.0026(8) 0.0013(8) 0.0123(9) N4 0.0227(10) 0.0278(11) 0.0229(10) -0.0039(8) 0.0021(8) 0.0117(9) N5 0.0270(11) 0.0271(11) 0.0259(10) 0.0003(9) 0.0024(9) 0.0127(10) C2 0.0250(12) 0.0259(12) 0.0203(11) -0.0002(9) 0.0030(9) 0.0132(10) C3 0.0238(12) 0.0247(12) 0.0177(10) -0.0006(9) 0.0002(9) 0.0128(10) C4 0.0276(13) 0.0267(12) 0.0207(11) 0.0006(9) 0.0016(9) 0.0148(11) C5 0.058(2) 0.0303(15) 0.0347(15) 0.0060(12) 0.0096(14) 0.0249(15) C1 0.0502(18) 0.0312(14) 0.0329(14) 0.0081(11) 0.0168(13) 0.0243(14) C9 0.0284(13) 0.0263(13) 0.0208(11) -0.0022(9) 0.0025(10) 0.0136(11) C8 0.0271(12) 0.0221(11) 0.0198(11) 0.0001(9) 0.0011(9) 0.0137(10) C7 0.0275(12) 0.0245(12) 0.0207(11) 0.0008(9) 0.0023(9) 0.0146(11) C6 0.0280(14) 0.0328(14) 0.0307(13) -0.0071(11) 0.0013(11) 0.0099(12) C10 0.0289(14) 0.0405(16) 0.0378(15) -0.0150(13) 0.0040(12) 0.0092(13) C11 0.0238(12) 0.0261(12) 0.0212(11) -0.0017(9) -0.0021(9) 0.0139(11) Cl1A 0.160(18) 0.15(2) 0.175(13) 0.043(12) 0.043(12) 0.084(12) Cl2A 0.145(13) 0.058(7) 0.33(3) -0.018(11) -0.014(15) 0.019(8) Cl1B 0.103(8) 0.044(5) 0.212(17) -0.032(7) -0.008(10) 0.040(5) Cl1C 0.208(19) 0.170(16) 0.147(12) 0.049(11) 0.078(12) 0.158(15) _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 Cd1 N5 2.257(2) . ? Cd1 N5 2.257(2) 10_655 ? Cd1 N3 2.386(2) 6_554 ? Cd1 N3 2.386(2) 18_545 ? Cd1 N1 2.500(2) . ? Cd1 N1 2.500(2) 10_655 ? S1 C11 1.628(3) . ? N1 C2 1.341(3) . ? N1 N2 1.360(3) . ? N2 C4 1.352(3) . ? N3 C7 1.341(3) . ? N3 N4 1.359(3) . ? N3 Cd1 2.385(2) 8_545 ? N4 C9 1.343(3) . ? N5 C11 1.163(3) . ? C2 C3 1.415(3) . ? C2 C1 1.490(4) . ? C3 C4 1.382(3) . ? C3 C8 1.478(3) . ? C4 C5 1.485(4) . ? C9 C8 1.383(4) . ? C9 C10 1.487(4) . ? C8 C7 1.421(3) . ? C7 C6 1.487(4) . ? C12A Cl2A 1.748(8) . ? C12A Cl1A 1.754(8) . ? C12B Cl1B 1.762(8) . ? C12C Cl1C 1.761(8) . ? 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 N5 Cd1 N5 180.0(2) . 10_655 ? N5 Cd1 N3 84.99(8) . 6_554 ? N5 Cd1 N3 95.01(8) 10_655 6_554 ? N5 Cd1 N3 95.01(8) . 18_545 ? N5 Cd1 N3 84.99(8) 10_655 18_545 ? N3 Cd1 N3 180.00(11) 6_554 18_545 ? N5 Cd1 N1 82.42(7) . . ? N5 Cd1 N1 97.58(7) 10_655 . ? N3 Cd1 N1 97.72(7) 6_554 . ? N3 Cd1 N1 82.28(7) 18_545 . ? N5 Cd1 N1 97.58(7) . 10_655 ? N5 Cd1 N1 82.42(7) 10_655 10_655 ? N3 Cd1 N1 82.28(7) 6_554 10_655 ? N3 Cd1 N1 97.72(7) 18_545 10_655 ? N1 Cd1 N1 180.00(7) . 10_655 ? C2 N1 N2 104.38(19) . . ? C2 N1 Cd1 132.57(16) . . ? N2 N1 Cd1 122.08(14) . . ? C4 N2 N1 112.9(2) . . ? C7 N3 N4 105.00(19) . . ? C7 N3 Cd1 138.74(17) . 8_545 ? N4 N3 Cd1 115.40(15) . 8_545 ? C9 N4 N3 112.6(2) . . ? C11 N5 Cd1 159.3(2) . . ? N1 C2 C3 111.1(2) . . ? N1 C2 C1 120.6(2) . . ? C3 C2 C1 128.2(2) . . ? C4 C3 C2 105.1(2) . . ? C4 C3 C8 127.3(2) . . ? C2 C3 C8 127.4(2) . . ? N2 C4 C3 106.4(2) . . ? N2 C4 C5 122.3(2) . . ? C3 C4 C5 131.3(2) . . ? N4 C9 C8 107.0(2) . . ? N4 C9 C10 121.7(2) . . ? C8 C9 C10 131.2(2) . . ? C9 C8 C7 104.9(2) . . ? C9 C8 C3 125.8(2) . . ? C7 C8 C3 129.3(2) . . ? N3 C7 C8 110.5(2) . . ? N3 C7 C6 121.8(2) . . ? C8 C7 C6 127.7(2) . . ? N5 C11 S1 179.3(3) . . ? Cl2A C12A Cl1A 109.9(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 N5 Cd1 N1 C2 -155.7(2) . . . . ? N5 Cd1 N1 C2 24.3(2) 10_655 . . . ? N3 Cd1 N1 C2 120.4(2) 6_554 . . . ? N3 Cd1 N1 C2 -59.6(2) 18_545 . . . ? N5 Cd1 N1 N2 11.11(18) . . . . ? N5 Cd1 N1 N2 -168.89(18) 10_655 . . . ? N3 Cd1 N1 N2 -72.75(18) 6_554 . . . ? N3 Cd1 N1 N2 107.25(18) 18_545 . . . ? C2 N1 N2 C4 -0.8(3) . . . . ? Cd1 N1 N2 C4 -170.81(16) . . . . ? C7 N3 N4 C9 -0.2(3) . . . . ? Cd1 N3 N4 C9 -171.60(16) 8_545 . . . ? N3 Cd1 N5 C11 -144.4(6) 6_554 . . . ? N3 Cd1 N5 C11 35.6(6) 18_545 . . . ? N1 Cd1 N5 C11 117.1(6) . . . . ? N1 Cd1 N5 C11 -62.9(6) 10_655 . . . ? N2 N1 C2 C3 0.8(3) . . . . ? Cd1 N1 C2 C3 169.30(17) . . . . ? N2 N1 C2 C1 -177.8(2) . . . . ? Cd1 N1 C2 C1 -9.3(4) . . . . ? N1 C2 C3 C4 -0.6(3) . . . . ? C1 C2 C3 C4 177.9(3) . . . . ? N1 C2 C3 C8 175.6(2) . . . . ? C1 C2 C3 C8 -6.0(4) . . . . ? N1 N2 C4 C3 0.5(3) . . . . ? N1 N2 C4 C5 -176.8(2) . . . . ? C2 C3 C4 N2 0.1(3) . . . . ? C8 C3 C4 N2 -176.1(2) . . . . ? C2 C3 C4 C5 177.0(3) . . . . ? C8 C3 C4 C5 0.8(5) . . . . ? N3 N4 C9 C8 0.8(3) . . . . ? N3 N4 C9 C10 -178.2(3) . . . . ? N4 C9 C8 C7 -1.0(3) . . . . ? C10 C9 C8 C7 177.9(3) . . . . ? N4 C9 C8 C3 177.8(2) . . . . ? C10 C9 C8 C3 -3.3(5) . . . . ? C4 C3 C8 C9 119.3(3) . . . . ? C2 C3 C8 C9 -56.0(4) . . . . ? C4 C3 C8 C7 -62.2(4) . . . . ? C2 C3 C8 C7 122.5(3) . . . . ? N4 N3 C7 C8 -0.4(3) . . . . ? Cd1 N3 C7 C8 167.71(18) 8_545 . . . ? N4 N3 C7 C6 179.6(2) . . . . ? Cd1 N3 C7 C6 -12.3(4) 8_545 . . . ? C9 C8 C7 N3 0.9(3) . . . . ? C3 C8 C7 N3 -177.8(2) . . . . ? C9 C8 C7 C6 -179.1(3) . . . . ? C3 C8 C7 C6 2.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.86 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.581 _refine_diff_density_min -1.872 _refine_diff_density_rms 0.077 _iucr_refine_instruction_details ; #--------------------------------------------------------- TITL c1927 in R-3 CELL 0.71073 25.7908 25.7908 11.1284 90.000 90.000 120.000 ZERR 9.00 0.0022 0.0022 0.0013 0.000 0.000 0.000 LATT 3 SYMM - Y, X - Y, Z SYMM - X + Y, - X, Z SFAC C H N CD S CL UNIT 204 264 90 9 18 12 MERG 2 OMIT -1 2 0 SHEL 0.76 10 BOND 0.5 EQIV $1 1-Y, X-Y, Z EQIV $2 1-X+Y, 1-X, Z DFIX 1.760 0.008 C12A CL1A C12A CL2A C12B CL1B C12B CL1B_$1 C12B CL1B_$2 DFIX 2.883 0.008 CL1A CL2A CL1B CL1B_$1 CL1B CL1B_$2 DFIX 1.760 0.008 C12C CL1C C12C CL1C_$2 DFIX 2.883 0.008 CL1C CL1C_$2 FMAP 2 PLAN 10 SIZE 0.20 0.22 0.28 ACTA CONF LIST 1 L.S. 6 TEMP -60.00 WGHT 0.036900 17.789202 FVAR 0.09076 0.33000 CD1 4 0.500000 0.000000 0.000000 10.50000 0.01864 0.02131 = 0.01684 0.00067 -0.00174 0.00849 S1 5 0.673497 0.194790 -0.124757 11.00000 0.02414 0.02926 = 0.03716 -0.00111 0.00208 0.00480 N1 3 0.455821 0.057835 0.090997 11.00000 0.02543 0.02544 = 0.02134 0.00297 0.00399 0.01431 N2 3 0.472928 0.114773 0.056457 11.00000 0.02714 0.02533 = 0.02140 0.00406 0.00703 0.01347 AFIX 43 H2 2 0.495844 0.132277 -0.005187 11.00000 -1.50000 AFIX 0 N3 3 0.352129 0.137176 0.475862 11.00000 0.02481 0.02389 = 0.02101 -0.00258 0.00128 0.01232 N4 3 0.304515 0.089068 0.424716 11.00000 0.02274 0.02777 = 0.02288 -0.00392 0.00214 0.01173 AFIX 43 H4 2 0.268225 0.072632 0.452843 11.00000 -1.20000 AFIX 0 N5 3 0.565404 0.090316 -0.077884 11.00000 0.02698 0.02708 = 0.02589 0.00031 0.00240 0.01270 C2 1 0.422051 0.048845 0.188989 11.00000 0.02497 0.02592 = 0.02027 -0.00024 0.00302 0.01317 C3 1 0.417145 0.099881 0.215392 11.00000 0.02378 0.02465 = 0.01766 -0.00056 0.00025 0.01277 C4 1 0.450585 0.141297 0.127958 11.00000 0.02755 0.02665 = 0.02069 0.00060 0.00155 0.01479 C5 1 0.460834 0.202319 0.103585 11.00000 0.05829 0.03034 = 0.03470 0.00600 0.00955 0.02486 AFIX 137 H5A 2 0.497220 0.231663 0.143541 11.00000 -1.50000 H5B 2 0.427212 0.205479 0.133606 11.00000 -1.50000 H5C 2 0.464767 0.209682 0.017685 11.00000 -1.50000 AFIX 0 C1 1 0.396375 -0.008641 0.256602 11.00000 0.05017 0.03122 = 0.03294 0.00814 0.01684 0.02429 AFIX 137 H1A 2 0.368498 -0.041181 0.205528 11.00000 -1.50000 H1B 2 0.375539 -0.006388 0.327216 11.00000 -1.50000 H1C 2 0.428377 -0.015769 0.281069 11.00000 -1.50000 AFIX 0 C9 1 0.319639 0.069700 0.326024 11.00000 0.02838 0.02630 = 0.02082 -0.00215 0.00245 0.01357 C8 1 0.380713 0.106120 0.310661 11.00000 0.02714 0.02212 = 0.01978 0.00014 0.00115 0.01370 C7 1 0.398999 0.148158 0.406329 11.00000 0.02748 0.02446 = 0.02074 0.00081 0.00226 0.01458 C6 1 0.460296 0.198356 0.432051 11.00000 0.02802 0.03281 = 0.03066 -0.00711 0.00126 0.00986 AFIX 137 H6A 2 0.463400 0.235791 0.406690 11.00000 -1.50000 H6B 2 0.489359 0.192148 0.388635 11.00000 -1.50000 H6C 2 0.468121 0.199879 0.517610 11.00000 -1.50000 AFIX 0 C10 1 0.274265 0.018603 0.253702 11.00000 0.02890 0.04055 = 0.03777 -0.01498 0.00400 0.00923 AFIX 137 H10A 2 0.261054 -0.018419 0.297579 11.00000 -1.50000 H10B 2 0.291862 0.016810 0.177888 11.00000 -1.50000 H10C 2 0.240284 0.024091 0.238467 11.00000 -1.50000 AFIX 0 C11 1 0.610630 0.133734 -0.096911 11.00000 0.02375 0.02610 = 0.02117 -0.00173 -0.00210 0.01393 PART -1 C12A 1 0.626612 0.294610 0.054505 10.16667 0.06830 CL1A 6 0.696703 0.357206 0.023231 10.16667 0.16027 0.14953 = 0.17479 0.04260 0.04324 0.08373 CL2A 6 0.618847 0.281438 0.209305 10.16667 0.14514 0.05795 = 0.33106 -0.01849 -0.01378 0.01931 PART -2 C12B 1 0.666667 0.333333 0.067746 10.08333 0.11472 CL1B 6 0.613636 0.262393 0.123694 10.16667 0.10320 0.04386 = 0.21178 -0.03246 -0.00771 0.04011 PART -3 C12C 1 0.621853 0.309629 0.211411 10.08333 0.04881 CL1C 6 0.632092 0.259792 0.119774 10.16667 0.20805 0.16985 = 0.14699 0.04869 0.07791 0.15840 HKLF 4 REM c1927 in R-3 REM R1 = 0.0353 for 3076 Fo > 4sig(Fo) and 0.0404 for all 3332 data REM 213 parameters refined using 11 restraints END WGHT 0.0369 17.7893 REM Highest difference peak 0.581, deepest hole -1.872, 1-sigma level 0.077 Q1 1 0.6148 0.2895 0.1055 11.00000 0.05 0.58 Q2 1 0.5316 0.0208 0.0400 11.00000 0.05 0.43 Q3 1 0.5393 0.0139 -0.0163 11.00000 0.05 0.42 Q4 1 0.6164 0.3270 0.1467 11.00000 0.05 0.42 Q5 1 0.6523 0.1522 -0.1341 11.00000 0.05 0.40 Q6 1 0.3957 0.1340 0.3517 11.00000 0.05 0.39 Q7 1 0.5209 0.0387 -0.0133 11.00000 0.05 0.37 Q8 1 0.6457 0.3383 0.3171 11.00000 0.05 0.37 Q9 1 0.4108 0.0686 0.2062 11.00000 0.05 0.36 Q10 1 0.6391 0.2743 0.1666 11.00000 0.05 0.35 ; _database_code_depnum_ccdc_archive 'CCDC 947380' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_(2) _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis-Thiocyanato-mu-Hexafluorosilicato-tetrakis (3,3',5,5'-Tetramethyl-4,4'-bipyrazole)dicadmium(II), Solvate with 6 Chloroform ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H56 Cd2 F6 N18 S2 Si, 6(C H Cl3)' _chemical_formula_sum 'C48 H62 Cd2 Cl18 F6 N18 S2 Si' _chemical_formula_weight 1960.27 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 61 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 14.4685(12) _cell_length_b 22.858(3) _cell_length_c 23.048(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7622.5(15) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 42980 _cell_measurement_theta_min 4.20 _cell_measurement_theta_max 27.10 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.708 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3912 _exptl_absorpt_coefficient_mu 1.322 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7335 _exptl_absorpt_correction_T_max 0.7779 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'Siemens SMART CCD area-detector diffractometer' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 42980 _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_sigmaI/netI 0.0203 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 4.20 _diffrn_reflns_theta_max 27.10 _reflns_number_total 8386 _reflns_number_gt 7055 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT (Bruker, 1998)' _computing_cell_refinement 'SAINT-NT (Bruker, 1999)' _computing_data_reduction 'SAINT-NT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.700.00 (Farrugia, 1999)' #------------------------------- Refinement data-----------------------# _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. Si1 atom of the hexafluorosilicate resides on a center of inversion. The refinement for the framework portion was essentially standard. CH (methyl) and NH hydrogen atoms were added geometrically, with U(iso) = 1.5U(eq) of the parent C (N) atom. There are three independed solvate chloroform molecules, one of which was refined freely and anisotropically [C22-Cl = 1.709(12)-1.729(10) A]. Two other solvent molecules are disordered over two closely separated positions. The molecule referenced by carbon atom C23 adopts two orientations (partial contribution factors 0.5) with the common atom Cl4. Therefore, the occupancy factors were 0.5 for C23, Cl5, C6, C23A, Cl5A, C6A and 1.0 for Cl4. It was possible to refine this molecule anisotropically and without restraints in geometry [C-Cl = 1.63(2)-1.76(3) A]. At the same time, the molecule referenced by C24 is unequally disordered over two positions with partial contributions 0.65 (C24) and 0.35 (0.35). It was left isotropic [U(iso) (Cl) = 0.14-0.27 A^2^], two contributions of the disordered carbon atom were assigned with an equal isotropic thermal parameter (EADP) and the restraints for the C-Cl bond lengths [1.73(1) A] were applied in order to improve the stability of the refinement. In each case, the partial contributions were refined with PART -n and the hydrogen atoms added with corresponding partial occupancies. ; _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^)+(0.0850P)^2^+29.8985P] 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_number_reflns 8386 _refine_ls_number_parameters 460 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0687 _refine_ls_R_factor_gt 0.0577 _refine_ls_wR_factor_ref 0.1624 _refine_ls_wR_factor_gt 0.1557 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.025 _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 Cd1 Cd 0.01431(2) 0.135165(12) 0.384578(12) 0.02094(11) Uani 1 1 d . . . Si1 Si 0.0000 0.0000 0.5000 0.0199(3) Uani 1 2 d S . . S1 S 0.10786(12) 0.27429(7) 0.23414(7) 0.0573(4) Uani 1 1 d . . . F1 F 0.00246(19) 0.05729(11) 0.45371(12) 0.0336(6) Uani 1 1 d . . . F2 F -0.10665(18) 0.01990(12) 0.52171(12) 0.0345(6) Uani 1 1 d . . . F3 F 0.0470(2) 0.04189(12) 0.55206(11) 0.0363(6) Uani 1 1 d . . . N1 N -0.1062(3) 0.08456(15) 0.33979(16) 0.0285(8) Uani 1 1 d . . . N2 N -0.1031(3) 0.02496(16) 0.33723(17) 0.0304(8) Uani 1 1 d . . . H2 H -0.0702 0.0035 0.3606 0.046 Uiso 1 1 calc R . . N3 N -0.3833(3) 0.06741(16) 0.15992(15) 0.0285(8) Uani 1 1 d . . . N4 N -0.3163(3) 0.04185(18) 0.12891(17) 0.0325(8) Uani 1 1 d . . . H4 H -0.3210 0.0340 0.0921 0.049 Uiso 1 1 calc R . . N5 N -0.0925(3) 0.17629(16) 0.44904(16) 0.0286(8) Uani 1 1 d . . . N6 N -0.1472(3) 0.14093(16) 0.48177(17) 0.0316(8) Uani 1 1 d . . . H6 H -0.1374 0.1037 0.4866 0.047 Uiso 1 1 calc R . . N7 N -0.3641(3) 0.33768(17) 0.55332(16) 0.0302(8) Uani 1 1 d . . . N8 N -0.3716(3) 0.34877(17) 0.49558(16) 0.0322(8) Uani 1 1 d . . . H8 H -0.4074 0.3756 0.4809 0.048 Uiso 1 1 calc R . . N9 N 0.0269(3) 0.20782(19) 0.32099(19) 0.0384(9) Uani 1 1 d . . . C1 C -0.1847(4) 0.1627(2) 0.2851(3) 0.0464(13) Uani 1 1 d . . . H1A H -0.1550 0.1869 0.3142 0.070 Uiso 1 1 calc R . . H1B H -0.2510 0.1687 0.2866 0.070 Uiso 1 1 calc R . . H1C H -0.1619 0.1733 0.2469 0.070 Uiso 1 1 calc R . . C2 C -0.1634(3) 0.09987(18) 0.29664(19) 0.0270(9) Uani 1 1 d . . . C3 C -0.1963(3) 0.05015(18) 0.26692(18) 0.0259(8) Uani 1 1 d . . . C4 C -0.1560(3) 0.00310(19) 0.2949(2) 0.0321(10) Uani 1 1 d . . . C5 C -0.1657(4) -0.0610(2) 0.2852(3) 0.0530(15) Uani 1 1 d . . . H5A H -0.1493 -0.0702 0.2455 0.080 Uiso 1 1 calc R . . H5B H -0.2291 -0.0726 0.2924 0.080 Uiso 1 1 calc R . . H5C H -0.1249 -0.0818 0.3115 0.080 Uiso 1 1 calc R . . C6 C -0.4079(4) 0.0936(3) 0.2627(2) 0.0415(12) Uani 1 1 d . . . H6A H -0.3921 0.1340 0.2710 0.062 Uiso 1 1 calc R . . H6B H -0.3971 0.0699 0.2969 0.062 Uiso 1 1 calc R . . H6C H -0.4726 0.0912 0.2519 0.062 Uiso 1 1 calc R . . C7 C -0.3497(3) 0.07185(19) 0.21404(18) 0.0274(9) Uani 1 1 d . . . C8 C -0.2591(3) 0.04989(18) 0.21646(18) 0.0256(8) Uani 1 1 d . . . C9 C -0.2406(3) 0.0295(2) 0.1610(2) 0.0330(10) Uani 1 1 d . . . C10 C -0.1591(4) -0.0020(3) 0.1371(3) 0.0528(14) Uani 1 1 d . . . H10A H -0.1639 -0.0433 0.1462 0.079 Uiso 1 1 calc R . . H10B H -0.1030 0.0137 0.1541 0.079 Uiso 1 1 calc R . . H10C H -0.1571 0.0030 0.0953 0.079 Uiso 1 1 calc R . . C11 C -0.0868(4) 0.2809(2) 0.4235(3) 0.0506(15) Uani 1 1 d . . . H11A H -0.0200 0.2778 0.4261 0.076 Uiso 1 1 calc R . . H11B H -0.1069 0.3166 0.4425 0.076 Uiso 1 1 calc R . . H11C H -0.1051 0.2818 0.3831 0.076 Uiso 1 1 calc R . . C12 C -0.1304(3) 0.22930(18) 0.4527(2) 0.0304(9) Uani 1 1 d . . . C13 C -0.2098(3) 0.22807(19) 0.48773(18) 0.0288(9) Uani 1 1 d . . . C14 C -0.2180(3) 0.1703(2) 0.5057(2) 0.0329(10) Uani 1 1 d . . . C15 C -0.2862(4) 0.1400(2) 0.5434(3) 0.0506(14) Uani 1 1 d . . . H15A H -0.2922 0.0996 0.5311 0.076 Uiso 1 1 calc R . . H15B H -0.3456 0.1594 0.5403 0.076 Uiso 1 1 calc R . . H15C H -0.2652 0.1413 0.5833 0.076 Uiso 1 1 calc R . . C16 C -0.2740(5) 0.2709(3) 0.6157(2) 0.0577(18) Uani 1 1 d . . . H16A H -0.2687 0.3031 0.6429 0.087 Uiso 1 1 calc R . . H16B H -0.2147 0.2515 0.6119 0.087 Uiso 1 1 calc R . . H16C H -0.3195 0.2432 0.6299 0.087 Uiso 1 1 calc R . . C17 C -0.3037(3) 0.2938(2) 0.55771(19) 0.0323(10) Uani 1 1 d . . . C18 C -0.2725(3) 0.2766(2) 0.50214(19) 0.0300(9) Uani 1 1 d . . . C19 C -0.3174(3) 0.3134(2) 0.46404(19) 0.0325(10) Uani 1 1 d . . . C20 C -0.3130(5) 0.3181(3) 0.3997(2) 0.0517(15) Uani 1 1 d . . . H20A H -0.3729 0.3298 0.3849 0.078 Uiso 1 1 calc R . . H20B H -0.2961 0.2804 0.3834 0.078 Uiso 1 1 calc R . . H20C H -0.2670 0.3470 0.3890 0.078 Uiso 1 1 calc R . . C21 C 0.0596(3) 0.2360(2) 0.2856(2) 0.0352(10) Uani 1 1 d . . . C22 C 0.0160(7) 0.1843(5) 0.1172(4) 0.093(3) Uani 1 1 d . . . H22 H 0.0319 0.2046 0.1538 0.111 Uiso 1 1 calc R . . Cl1 Cl -0.0733(3) 0.13773(17) 0.1323(2) 0.1533(15) Uani 1 1 d . . . Cl2 Cl 0.1142(3) 0.1504(2) 0.09326(16) 0.1639(16) Uani 1 1 d . . . Cl3 Cl -0.0179(3) 0.2372(3) 0.0680(3) 0.227(3) Uani 1 1 d . . . Cl4 Cl 0.32282(16) 0.32418(9) 0.27005(11) 0.0878(7) Uani 1 1 d . . . C23 C 0.4180(16) 0.3725(9) 0.2738(11) 0.061(5) Uani 0.50 1 d P A -1 H23 H 0.4741 0.3478 0.2716 0.073 Uiso 0.50 1 calc PR A -1 Cl5 Cl 0.4258(3) 0.4208(3) 0.2183(3) 0.1060(18) Uani 0.50 1 d P A -1 Cl6 Cl 0.4184(4) 0.4044(2) 0.3432(3) 0.0939(16) Uani 0.50 1 d P A -1 C23A C 0.4195(19) 0.3599(10) 0.2991(11) 0.070(6) Uani 0.50 1 d P A -2 H23A H 0.4768 0.3453 0.2806 0.084 Uiso 0.50 1 calc PR A -2 Cl5A Cl 0.4258(6) 0.3514(6) 0.3751(3) 0.179(4) Uani 0.50 1 d P A -2 Cl6A Cl 0.4119(4) 0.4309(2) 0.2919(8) 0.211(7) Uani 0.50 1 d P A -2 C24 C -0.3960(8) -0.0194(8) 0.4334(5) 0.149(7) Uiso 0.65 1 d PD B -3 H24 H -0.4220 0.0207 0.4325 0.179 Uiso 0.65 1 calc PR B -3 Cl7 Cl -0.2815(5) -0.0185(3) 0.4565(4) 0.171(2) Uiso 0.65 1 d PD B -3 Cl8 Cl -0.4584(7) -0.0641(5) 0.4806(5) 0.216(4) Uiso 0.65 1 d PD B -3 Cl9 Cl -0.4069(6) -0.0534(4) 0.3656(4) 0.184(3) Uiso 0.65 1 d PD B -3 C24A C -0.3593(17) -0.0558(13) 0.4277(9) 0.149(7) Uiso 0.35 1 d PD C -4 H24A H -0.3338 -0.0866 0.4021 0.179 Uiso 0.35 1 calc PR C -4 Cl7A Cl -0.2970(12) 0.0072(8) 0.4125(9) 0.208(6) Uiso 0.35 1 d PD C -4 Cl8A Cl -0.3144(8) -0.0690(5) 0.4958(5) 0.139(3) Uiso 0.35 1 d PD C -4 Cl9A Cl -0.4785(15) -0.0597(12) 0.4207(13) 0.274(10) Uiso 0.35 1 d PD C -4 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 Cd1 0.02236(17) 0.01986(17) 0.02061(17) -0.00087(10) 0.00127(10) -0.00078(10) Si1 0.0238(7) 0.0152(7) 0.0208(7) 0.0022(5) 0.0003(6) 0.0003(5) S1 0.0549(9) 0.0593(9) 0.0578(9) 0.0301(7) 0.0112(7) 0.0022(7) F1 0.0432(15) 0.0243(13) 0.0334(14) 0.0118(11) 0.0023(11) 0.0000(11) F2 0.0296(13) 0.0342(14) 0.0396(14) 0.0037(12) 0.0067(11) 0.0072(11) F3 0.0468(16) 0.0301(13) 0.0318(13) -0.0055(11) -0.0059(12) -0.0055(12) N1 0.0279(18) 0.0237(17) 0.0339(19) -0.0013(15) -0.0087(15) 0.0017(14) N2 0.0302(19) 0.0230(17) 0.038(2) 0.0057(15) -0.0132(16) 0.0007(14) N3 0.0283(18) 0.0317(19) 0.0257(17) 0.0027(15) -0.0050(14) 0.0034(15) N4 0.032(2) 0.037(2) 0.0278(18) -0.0056(16) -0.0062(15) 0.0066(16) N5 0.0294(19) 0.0253(18) 0.0313(19) -0.0006(14) 0.0072(15) 0.0033(14) N6 0.035(2) 0.0219(17) 0.038(2) 0.0048(15) 0.0097(17) 0.0067(15) N7 0.0320(19) 0.0314(19) 0.0271(18) -0.0040(15) 0.0021(15) 0.0098(15) N8 0.041(2) 0.0283(18) 0.0269(18) 0.0022(15) 0.0036(16) 0.0124(16) N9 0.044(2) 0.034(2) 0.037(2) 0.0105(18) 0.0031(18) -0.0034(18) C1 0.050(3) 0.024(2) 0.065(4) -0.002(2) -0.025(3) 0.005(2) C2 0.027(2) 0.023(2) 0.031(2) 0.0012(16) -0.0063(17) 0.0024(16) C3 0.024(2) 0.025(2) 0.029(2) 0.0021(16) -0.0062(16) 0.0004(16) C4 0.033(2) 0.024(2) 0.039(2) 0.0018(18) -0.0112(19) -0.0045(17) C5 0.057(3) 0.026(2) 0.076(4) 0.000(3) -0.028(3) -0.003(2) C6 0.038(3) 0.058(3) 0.029(2) 0.004(2) 0.000(2) 0.010(2) C7 0.029(2) 0.027(2) 0.027(2) 0.0074(16) -0.0046(16) -0.0007(17) C8 0.027(2) 0.024(2) 0.026(2) 0.0011(16) -0.0063(16) 0.0001(16) C9 0.031(2) 0.033(2) 0.035(2) -0.0017(19) -0.0054(19) 0.0025(18) C10 0.044(3) 0.066(4) 0.048(3) -0.010(3) -0.005(3) 0.017(3) C11 0.059(3) 0.027(2) 0.067(4) 0.002(2) 0.030(3) 0.002(2) C12 0.037(2) 0.022(2) 0.032(2) -0.0009(17) 0.0076(18) 0.0048(17) C13 0.032(2) 0.026(2) 0.028(2) 0.0004(17) 0.0045(17) 0.0078(17) C14 0.034(2) 0.031(2) 0.034(2) 0.0056(18) 0.0074(19) 0.0090(18) C15 0.050(3) 0.040(3) 0.062(4) 0.014(3) 0.025(3) 0.007(2) C16 0.060(4) 0.084(5) 0.029(3) 0.003(3) 0.001(2) 0.044(3) C17 0.031(2) 0.037(2) 0.029(2) 0.0004(18) 0.0021(18) 0.0125(19) C18 0.033(2) 0.028(2) 0.029(2) 0.0009(17) 0.0058(18) 0.0090(17) C19 0.042(3) 0.027(2) 0.028(2) 0.0014(17) 0.0047(19) 0.0082(19) C20 0.071(4) 0.055(3) 0.029(2) 0.004(2) 0.007(2) 0.025(3) C21 0.035(2) 0.034(2) 0.037(2) 0.008(2) -0.002(2) 0.0018(19) C22 0.094(7) 0.111(8) 0.072(6) 0.032(5) -0.019(5) -0.027(6) Cl1 0.125(3) 0.144(3) 0.191(4) 0.056(3) -0.011(3) -0.046(2) Cl2 0.163(4) 0.235(5) 0.094(2) 0.014(3) 0.043(2) -0.005(3) Cl3 0.137(3) 0.285(6) 0.258(5) 0.210(5) -0.090(3) -0.084(3) Cl4 0.0834(13) 0.0562(10) 0.1237(18) 0.0131(11) -0.0332(13) -0.0157(9) C23 0.040(7) 0.037(9) 0.106(18) 0.008(9) -0.008(10) 0.011(6) Cl5 0.068(3) 0.095(3) 0.155(5) 0.048(4) 0.003(3) -0.015(2) Cl6 0.101(4) 0.055(2) 0.125(4) -0.027(3) 0.037(3) -0.010(2) C23A 0.057(9) 0.038(11) 0.11(2) -0.001(10) -0.025(13) 0.010(8) Cl5A 0.105(5) 0.321(14) 0.111(5) -0.038(7) -0.015(4) -0.043(7) Cl6A 0.076(3) 0.047(3) 0.51(2) -0.072(6) -0.065(7) 0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N9 2.223(4) . ? Cd1 N1 2.333(4) . ? Cd1 N5 2.340(4) . ? Cd1 N7 2.352(4) 4_556 ? Cd1 N3 2.376(4) 6_656 ? Cd1 F1 2.395(2) . ? Si1 F3 1.679(3) . ? Si1 F3 1.679(3) 5_556 ? Si1 F2 1.685(3) . ? Si1 F2 1.685(3) 5_556 ? Si1 F1 1.689(2) . ? Si1 F1 1.689(2) 5_556 ? S1 C21 1.632(5) . ? N1 C2 1.341(5) . ? N1 N2 1.364(5) . ? N2 C4 1.337(6) . ? N3 N4 1.338(5) . ? N3 C7 1.343(5) . ? N3 Cd1 2.376(4) 6_556 ? N4 C9 1.351(6) . ? N5 C12 1.333(5) . ? N5 N6 1.360(5) . ? N6 C14 1.345(6) . ? N7 C17 1.334(6) . ? N7 N8 1.359(5) . ? N7 Cd1 2.352(4) 4_456 ? N8 C19 1.341(6) . ? N9 C21 1.141(6) . ? C1 C2 1.492(6) . ? C2 C3 1.409(6) . ? C3 C4 1.383(6) . ? C3 C8 1.476(6) . ? C4 C5 1.488(6) . ? C6 C7 1.489(6) . ? C7 C8 1.404(6) . ? C8 C9 1.387(6) . ? C9 C10 1.488(7) . ? C11 C12 1.498(7) . ? C12 C13 1.404(6) . ? C13 C14 1.389(6) . ? C13 C18 1.470(6) . ? C14 C15 1.485(7) . ? C16 C17 1.498(7) . ? C17 C18 1.414(6) . ? C18 C19 1.379(6) . ? C19 C20 1.487(7) . ? C22 Cl2 1.709(12) . ? C22 Cl1 1.710(10) . ? C22 Cl3 1.729(10) . ? Cl4 C23A 1.75(3) . ? Cl4 C23 1.77(2) . ? C23 Cl5 1.692(19) . ? C23 Cl6 1.76(3) . ? C23A Cl6A 1.63(2) . ? C23A Cl5A 1.76(3) . ? C24 Cl7 1.741(9) . ? C24 Cl8 1.744(9) . ? C24 Cl9 1.752(9) . ? C24A Cl8A 1.726(10) . ? C24A Cl9A 1.735(10) . ? C24A Cl7A 1.736(10) . ? 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 N9 Cd1 N1 98.05(15) . . ? N9 Cd1 N5 99.95(15) . . ? N1 Cd1 N5 89.25(13) . . ? N9 Cd1 N7 98.20(15) . 4_556 ? N1 Cd1 N7 163.60(13) . 4_556 ? N5 Cd1 N7 90.09(13) . 4_556 ? N9 Cd1 N3 98.69(15) . 6_656 ? N1 Cd1 N3 87.24(13) . 6_656 ? N5 Cd1 N3 161.34(13) . 6_656 ? N7 Cd1 N3 88.17(13) 4_556 6_656 ? N9 Cd1 F1 179.27(14) . . ? N1 Cd1 F1 82.67(11) . . ? N5 Cd1 F1 80.15(11) . . ? N7 Cd1 F1 81.07(11) 4_556 . ? N3 Cd1 F1 81.22(11) 6_656 . ? F3 Si1 F3 180.00(15) . 5_556 ? F3 Si1 F2 90.27(14) . . ? F3 Si1 F2 89.73(14) 5_556 . ? F3 Si1 F2 89.73(14) . 5_556 ? F3 Si1 F2 90.27(14) 5_556 5_556 ? F2 Si1 F2 180.00(18) . 5_556 ? F3 Si1 F1 90.04(13) . . ? F3 Si1 F1 89.96(13) 5_556 . ? F2 Si1 F1 89.86(13) . . ? F2 Si1 F1 90.14(13) 5_556 . ? F3 Si1 F1 89.96(13) . 5_556 ? F3 Si1 F1 90.04(13) 5_556 5_556 ? F2 Si1 F1 90.14(13) . 5_556 ? F2 Si1 F1 89.86(13) 5_556 5_556 ? F1 Si1 F1 180.00(11) . 5_556 ? Si1 F1 Cd1 176.07(16) . . ? C2 N1 N2 104.4(3) . . ? C2 N1 Cd1 131.3(3) . . ? N2 N1 Cd1 119.3(3) . . ? C4 N2 N1 112.7(3) . . ? N4 N3 C7 105.5(3) . . ? N4 N3 Cd1 120.4(3) . 6_556 ? C7 N3 Cd1 125.3(3) . 6_556 ? N3 N4 C9 112.7(4) . . ? C12 N5 N6 105.4(3) . . ? C12 N5 Cd1 132.6(3) . . ? N6 N5 Cd1 119.8(3) . . ? C14 N6 N5 112.0(4) . . ? C17 N7 N8 105.5(3) . . ? C17 N7 Cd1 129.9(3) . 4_456 ? N8 N7 Cd1 119.1(3) . 4_456 ? C19 N8 N7 111.8(4) . . ? C21 N9 Cd1 157.9(4) . . ? N1 C2 C3 111.0(4) . . ? N1 C2 C1 120.7(4) . . ? C3 C2 C1 128.3(4) . . ? C4 C3 C2 104.9(4) . . ? C4 C3 C8 128.6(4) . . ? C2 C3 C8 126.4(4) . . ? N2 C4 C3 106.9(4) . . ? N2 C4 C5 122.1(4) . . ? C3 C4 C5 130.9(4) . . ? N3 C7 C8 110.3(4) . . ? N3 C7 C6 121.4(4) . . ? C8 C7 C6 128.2(4) . . ? C9 C8 C7 105.3(4) . . ? C9 C8 C3 127.5(4) . . ? C7 C8 C3 127.2(4) . . ? N4 C9 C8 106.1(4) . . ? N4 C9 C10 122.7(4) . . ? C8 C9 C10 131.1(4) . . ? N5 C12 C13 110.8(4) . . ? N5 C12 C11 120.9(4) . . ? C13 C12 C11 128.2(4) . . ? C14 C13 C12 105.1(4) . . ? C14 C13 C18 126.6(4) . . ? C12 C13 C18 128.3(4) . . ? N6 C14 C13 106.7(4) . . ? N6 C14 C15 120.9(4) . . ? C13 C14 C15 132.4(4) . . ? N7 C17 C18 110.5(4) . . ? N7 C17 C16 121.2(4) . . ? C18 C17 C16 128.3(4) . . ? C19 C18 C17 104.9(4) . . ? C19 C18 C13 127.4(4) . . ? C17 C18 C13 127.7(4) . . ? N8 C19 C18 107.4(4) . . ? N8 C19 C20 121.5(4) . . ? C18 C19 C20 131.2(4) . . ? N9 C21 S1 178.1(5) . . ? Cl2 C22 Cl1 114.4(7) . . ? Cl2 C22 Cl3 110.0(6) . . ? Cl1 C22 Cl3 110.8(5) . . ? Cl5 C23 Cl6 114.6(13) . . ? Cl5 C23 Cl4 115.1(13) . . ? Cl6 C23 Cl4 107.8(13) . . ? Cl6A C23A Cl4 111.7(12) . . ? Cl6A C23A Cl5A 102.5(16) . . ? Cl4 C23A Cl5A 111.6(15) . . ? Cl7 C24 Cl8 107.9(9) . . ? Cl7 C24 Cl9 111.3(9) . . ? Cl8 C24 Cl9 104.5(8) . . ? Cl8A C24A Cl9A 116.7(18) . . ? Cl8A C24A Cl7A 97.6(12) . . ? Cl9A C24A Cl7A 123(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 N9 Cd1 N1 C2 -12.5(4) . . . . ? N5 Cd1 N1 C2 87.5(4) . . . . ? N7 Cd1 N1 C2 175.2(4) 4_556 . . . ? N3 Cd1 N1 C2 -110.9(4) 6_656 . . . ? F1 Cd1 N1 C2 167.6(4) . . . . ? N9 Cd1 N1 N2 138.5(3) . . . . ? N5 Cd1 N1 N2 -121.6(3) . . . . ? N7 Cd1 N1 N2 -33.8(7) 4_556 . . . ? N3 Cd1 N1 N2 40.1(3) 6_656 . . . ? F1 Cd1 N1 N2 -41.4(3) . . . . ? C2 N1 N2 C4 -0.4(5) . . . . ? Cd1 N1 N2 C4 -158.3(3) . . . . ? C7 N3 N4 C9 0.0(5) . . . . ? Cd1 N3 N4 C9 149.0(3) 6_556 . . . ? N9 Cd1 N5 C12 -6.1(5) . . . . ? N1 Cd1 N5 C12 -104.2(4) . . . . ? N7 Cd1 N5 C12 92.2(4) 4_556 . . . ? N3 Cd1 N5 C12 176.7(4) 6_656 . . . ? F1 Cd1 N5 C12 173.1(4) . . . . ? N9 Cd1 N5 N6 154.6(3) . . . . ? N1 Cd1 N5 N6 56.6(3) . . . . ? N7 Cd1 N5 N6 -107.0(3) 4_556 . . . ? N3 Cd1 N5 N6 -22.5(6) 6_656 . . . ? F1 Cd1 N5 N6 -26.1(3) . . . . ? C12 N5 N6 C14 0.0(5) . . . . ? Cd1 N5 N6 C14 -165.4(3) . . . . ? C17 N7 N8 C19 -0.5(5) . . . . ? Cd1 N7 N8 C19 -157.0(3) 4_456 . . . ? N1 Cd1 N9 C21 -112.7(11) . . . . ? N5 Cd1 N9 C21 156.7(11) . . . . ? N7 Cd1 N9 C21 65.1(11) 4_556 . . . ? N3 Cd1 N9 C21 -24.2(11) 6_656 . . . ? N2 N1 C2 C3 -0.1(5) . . . . ? Cd1 N1 C2 C3 154.0(3) . . . . ? N2 N1 C2 C1 -179.8(4) . . . . ? Cd1 N1 C2 C1 -25.7(7) . . . . ? N1 C2 C3 C4 0.5(5) . . . . ? C1 C2 C3 C4 -179.8(5) . . . . ? N1 C2 C3 C8 -178.8(4) . . . . ? C1 C2 C3 C8 0.8(8) . . . . ? N1 N2 C4 C3 0.7(6) . . . . ? N1 N2 C4 C5 -178.0(5) . . . . ? C2 C3 C4 N2 -0.7(5) . . . . ? C8 C3 C4 N2 178.6(4) . . . . ? C2 C3 C4 C5 177.9(6) . . . . ? C8 C3 C4 C5 -2.8(9) . . . . ? N4 N3 C7 C8 1.4(5) . . . . ? Cd1 N3 C7 C8 -145.6(3) 6_556 . . . ? N4 N3 C7 C6 -174.6(4) . . . . ? Cd1 N3 C7 C6 38.4(6) 6_556 . . . ? N3 C7 C8 C9 -2.3(5) . . . . ? C6 C7 C8 C9 173.3(5) . . . . ? N3 C7 C8 C3 176.0(4) . . . . ? C6 C7 C8 C3 -8.3(8) . . . . ? C4 C3 C8 C9 -61.9(7) . . . . ? C2 C3 C8 C9 117.2(5) . . . . ? C4 C3 C8 C7 120.1(6) . . . . ? C2 C3 C8 C7 -60.7(7) . . . . ? N3 N4 C9 C8 -1.5(5) . . . . ? N3 N4 C9 C10 176.4(5) . . . . ? C7 C8 C9 N4 2.2(5) . . . . ? C3 C8 C9 N4 -176.1(4) . . . . ? C7 C8 C9 C10 -175.4(6) . . . . ? C3 C8 C9 C10 6.3(9) . . . . ? N6 N5 C12 C13 -0.2(5) . . . . ? Cd1 N5 C12 C13 162.6(3) . . . . ? N6 N5 C12 C11 177.8(5) . . . . ? Cd1 N5 C12 C11 -19.4(7) . . . . ? N5 C12 C13 C14 0.3(5) . . . . ? C11 C12 C13 C14 -177.5(5) . . . . ? N5 C12 C13 C18 -178.9(4) . . . . ? C11 C12 C13 C18 3.3(9) . . . . ? N5 N6 C14 C13 0.2(6) . . . . ? N5 N6 C14 C15 -179.8(5) . . . . ? C12 C13 C14 N6 -0.3(5) . . . . ? C18 C13 C14 N6 179.0(4) . . . . ? C12 C13 C14 C15 179.7(6) . . . . ? C18 C13 C14 C15 -1.1(9) . . . . ? N8 N7 C17 C18 -0.1(5) . . . . ? Cd1 N7 C17 C18 152.9(3) 4_456 . . . ? N8 N7 C17 C16 177.2(5) . . . . ? Cd1 N7 C17 C16 -29.9(7) 4_456 . . . ? N7 C17 C18 C19 0.6(6) . . . . ? C16 C17 C18 C19 -176.4(6) . . . . ? N7 C17 C18 C13 -176.5(5) . . . . ? C16 C17 C18 C13 6.5(9) . . . . ? C14 C13 C18 C19 -125.3(6) . . . . ? C12 C13 C18 C19 53.8(8) . . . . ? C14 C13 C18 C17 51.1(8) . . . . ? C12 C13 C18 C17 -129.8(6) . . . . ? N7 N8 C19 C18 0.8(6) . . . . ? N7 N8 C19 C20 -179.0(5) . . . . ? C17 C18 C19 N8 -0.8(5) . . . . ? C13 C18 C19 N8 176.3(5) . . . . ? C17 C18 C19 C20 179.0(6) . . . . ? C13 C18 C19 C20 -3.9(9) . . . . ? C23A Cl4 C23 Cl5 -171(5) . . . . ? C23A Cl4 C23 Cl6 -42(4) . . . . ? C23 Cl4 C23A Cl6A 50(3) . . . . ? C23 Cl4 C23A Cl5A 164(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.133 _refine_diff_density_min -1.203 _refine_diff_density_rms 0.124 _iucr_refine_instruction_details ; #--------------------------------------------------------- TITL c2110 in Pbca CELL 0.71073 14.4685 22.8578 23.0480 90.000 90.000 90.000 ZERR 4.00 0.0012 0.0025 0.0025 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N F SI S CL CD UNIT 192 248 72 24 4 8 72 8 MERG 2 OMIT 0.00 180.00 OMIT 0 0 4 OMIT 1 3 4 OMIT 1 7 2 SHEL 0.78 5 DFIX 1.73 0.01 C24 Cl7 C24 Cl8 C24 Cl9 DFIX 1.73 0.01 C24a Cl7a C24a Cl8a C24a Cl9a EADP C24 C24A FMAP 2 PLAN 20 SIZE 0.20 0.22 0.25 ACTA BOND CONF L.S. 6 TEMP -60.00 WGHT 0.085000 29.898499 FVAR 0.16950 CD1 8 0.014307 0.135165 0.384578 11.00000 0.02236 0.01986 = 0.02061 -0.00087 0.00127 -0.00078 SI1 5 0.000000 0.000000 0.500000 10.50000 0.02376 0.01523 = 0.02080 0.00225 0.00029 0.00032 S1 6 0.107860 0.274288 0.234139 11.00000 0.05488 0.05928 = 0.05778 0.03010 0.01119 0.00220 F1 4 0.002457 0.057286 0.453709 11.00000 0.04318 0.02431 = 0.03341 0.01180 0.00226 0.00001 F2 4 -0.106651 0.019901 0.521710 11.00000 0.02962 0.03421 = 0.03965 0.00367 0.00665 0.00719 F3 4 0.046989 0.041890 0.552059 11.00000 0.04684 0.03014 = 0.03179 -0.00554 -0.00590 -0.00547 N1 3 -0.106158 0.084562 0.339785 11.00000 0.02794 0.02375 = 0.03393 -0.00134 -0.00874 0.00170 N2 3 -0.103050 0.024964 0.337233 11.00000 0.03024 0.02298 = 0.03789 0.00574 -0.01317 0.00071 AFIX 43 H2 2 -0.070162 0.003511 0.360598 11.00000 -1.50000 AFIX 0 N3 3 -0.383263 0.067415 0.159917 11.00000 0.02826 0.03171 = 0.02567 0.00272 -0.00497 0.00339 N4 3 -0.316288 0.041850 0.128907 11.00000 0.03225 0.03734 = 0.02779 -0.00563 -0.00617 0.00656 AFIX 43 H4 2 -0.320987 0.034012 0.092087 11.00000 -1.50000 AFIX 0 N5 3 -0.092471 0.176289 0.449036 11.00000 0.02938 0.02526 = 0.03130 -0.00063 0.00717 0.00327 N6 3 -0.147157 0.140927 0.481769 11.00000 0.03519 0.02190 = 0.03765 0.00481 0.00967 0.00668 AFIX 43 H6 2 -0.137435 0.103688 0.486631 11.00000 -1.50000 AFIX 0 N7 3 -0.364068 0.337680 0.553322 11.00000 0.03205 0.03140 = 0.02713 -0.00395 0.00212 0.00982 N8 3 -0.371640 0.348771 0.495577 11.00000 0.04128 0.02830 = 0.02688 0.00216 0.00365 0.01236 AFIX 43 H8 2 -0.407363 0.375553 0.480864 11.00000 -1.50000 AFIX 0 N9 3 0.026937 0.207821 0.320986 11.00000 0.04382 0.03431 = 0.03699 0.01055 0.00308 -0.00335 C1 1 -0.184672 0.162667 0.285064 11.00000 0.05047 0.02367 = 0.06518 -0.00168 -0.02504 0.00524 AFIX 137 H1A 2 -0.154960 0.186852 0.314185 11.00000 -1.50000 H1B 2 -0.250999 0.168663 0.286561 11.00000 -1.50000 H1C 2 -0.161866 0.173314 0.246923 11.00000 -1.50000 AFIX 0 C2 1 -0.163434 0.099869 0.296637 11.00000 0.02695 0.02288 = 0.03103 0.00117 -0.00625 0.00240 C3 1 -0.196270 0.050145 0.266919 11.00000 0.02376 0.02544 = 0.02857 0.00210 -0.00625 0.00037 C4 1 -0.156005 0.003104 0.294948 11.00000 0.03347 0.02372 = 0.03910 0.00182 -0.01117 -0.00453 C5 1 -0.165676 -0.060961 0.285227 11.00000 0.05706 0.02602 = 0.07601 -0.00049 -0.02775 -0.00333 AFIX 137 H5A 2 -0.149276 -0.070192 0.245460 11.00000 -1.50000 H5B 2 -0.229116 -0.072608 0.292423 11.00000 -1.50000 H5C 2 -0.124939 -0.081846 0.311463 11.00000 -1.50000 AFIX 0 C6 1 -0.407932 0.093627 0.262706 11.00000 0.03775 0.05786 = 0.02901 0.00422 -0.00014 0.01004 AFIX 137 H6A 2 -0.392067 0.133990 0.271049 11.00000 -1.50000 H6B 2 -0.397089 0.069860 0.296901 11.00000 -1.50000 H6C 2 -0.472604 0.091216 0.251873 11.00000 -1.50000 AFIX 0 C7 1 -0.349669 0.071854 0.214043 11.00000 0.02885 0.02682 = 0.02653 0.00735 -0.00458 -0.00072 C8 1 -0.259128 0.049891 0.216456 11.00000 0.02651 0.02424 = 0.02616 0.00106 -0.00628 0.00010 C9 1 -0.240596 0.029535 0.160981 11.00000 0.03082 0.03268 = 0.03538 -0.00171 -0.00542 0.00248 C10 1 -0.159054 -0.001993 0.137071 11.00000 0.04393 0.06614 = 0.04848 -0.00987 -0.00467 0.01658 AFIX 137 H10A 2 -0.163904 -0.043297 0.146236 11.00000 -1.50000 H10B 2 -0.103009 0.013744 0.154096 11.00000 -1.50000 H10C 2 -0.157103 0.003024 0.095299 11.00000 -1.50000 AFIX 0 C11 1 -0.086760 0.280900 0.423525 11.00000 0.05860 0.02662 = 0.06656 0.00228 0.02971 0.00198 AFIX 137 H11A 2 -0.020032 0.277754 0.426141 11.00000 -1.50000 H11B 2 -0.106897 0.316588 0.442465 11.00000 -1.50000 H11C 2 -0.105083 0.281777 0.383050 11.00000 -1.50000 AFIX 0 C12 1 -0.130405 0.229301 0.452734 11.00000 0.03714 0.02231 = 0.03165 -0.00090 0.00759 0.00475 C13 1 -0.209830 0.228068 0.487732 11.00000 0.03230 0.02645 = 0.02755 0.00044 0.00446 0.00784 C14 1 -0.218044 0.170306 0.505742 11.00000 0.03354 0.03119 = 0.03393 0.00563 0.00736 0.00904 C15 1 -0.286196 0.140014 0.543376 11.00000 0.05009 0.04004 = 0.06172 0.01363 0.02484 0.00698 AFIX 137 H15A 2 -0.292234 0.099607 0.531089 11.00000 -1.50000 H15B 2 -0.345646 0.159382 0.540295 11.00000 -1.50000 H15C 2 -0.265235 0.141261 0.583333 11.00000 -1.50000 AFIX 0 C16 1 -0.274034 0.270895 0.615707 11.00000 0.06005 0.08430 = 0.02888 0.00314 0.00062 0.04362 AFIX 137 H16A 2 -0.268658 0.303145 0.642852 11.00000 -1.50000 H16B 2 -0.214678 0.251533 0.611949 11.00000 -1.50000 H16C 2 -0.319547 0.243201 0.629870 11.00000 -1.50000 AFIX 0 C17 1 -0.303716 0.293760 0.557714 11.00000 0.03112 0.03685 = 0.02892 0.00044 0.00214 0.01248 C18 1 -0.272479 0.276556 0.502139 11.00000 0.03331 0.02755 = 0.02926 0.00085 0.00576 0.00897 C19 1 -0.317351 0.313413 0.464040 11.00000 0.04216 0.02704 = 0.02819 0.00135 0.00467 0.00819 C20 1 -0.312959 0.318077 0.399741 11.00000 0.07115 0.05528 = 0.02861 0.00361 0.00656 0.02543 AFIX 137 H20A 2 -0.372878 0.329827 0.384889 11.00000 -1.50000 H20B 2 -0.296119 0.280437 0.383432 11.00000 -1.50000 H20C 2 -0.267016 0.347009 0.388964 11.00000 -1.50000 AFIX 0 C21 1 0.059590 0.235989 0.285633 11.00000 0.03464 0.03366 = 0.03716 0.00817 -0.00213 0.00180 C22 1 0.016014 0.184262 0.117188 11.00000 0.09429 0.11150 = 0.07235 0.03168 -0.01934 -0.02666 AFIX 13 H22 2 0.031912 0.204629 0.153759 11.00000 -1.20000 AFIX 0 CL1 7 -0.073343 0.137731 0.132319 11.00000 0.12527 0.14402 = 0.19050 0.05631 -0.01086 -0.04571 CL2 7 0.114182 0.150432 0.093260 11.00000 0.16287 0.23470 = 0.09418 0.01437 0.04281 -0.00461 CL3 7 -0.017894 0.237237 0.068025 11.00000 0.13694 0.28542 = 0.25758 0.20985 -0.09026 -0.08411 CL4 7 0.322823 0.324183 0.270050 11.00000 0.08341 0.05620 = 0.12372 0.01309 -0.03321 -0.01569 PART -1 C23 1 0.417964 0.372538 0.273775 10.50000 0.03976 0.03719 = 0.10613 0.00829 -0.00755 0.01076 AFIX 13 H23 2 0.474058 0.347830 0.271633 10.50000 -1.20000 AFIX 0 CL5 7 0.425817 0.420814 0.218341 10.50000 0.06798 0.09543 = 0.15455 0.04830 0.00286 -0.01501 CL6 7 0.418370 0.404449 0.343178 10.50000 0.10147 0.05493 = 0.12517 -0.02671 0.03656 -0.00991 PART -2 C23A 1 0.419512 0.359942 0.299124 10.50000 0.05731 0.03778 = 0.11423 -0.00132 -0.02503 0.01000 AFIX 13 H23A 2 0.476806 0.345345 0.280635 10.50000 -1.20000 AFIX 0 CL5A 7 0.425800 0.351350 0.375064 10.50000 0.10515 0.32095 = 0.11124 -0.03843 -0.01531 -0.04260 CL6A 7 0.411947 0.430932 0.291860 10.50000 0.07555 0.04711 = 0.50902 -0.07180 -0.06538 0.00908 PART -3 C24 1 -0.396002 -0.019362 0.433371 10.65000 0.14908 AFIX 13 H24 2 -0.422005 0.020690 0.432494 10.65000 -1.20000 AFIX 0 CL7 7 -0.281494 -0.018541 0.456514 10.65000 0.17092 CL8 7 -0.458378 -0.064080 0.480568 10.65000 0.21566 CL9 7 -0.406862 -0.053361 0.365605 10.65000 0.18440 PART -4 C24A 1 -0.359287 -0.055834 0.427687 10.35000 0.14908 AFIX 13 H24A 2 -0.333824 -0.086649 0.402083 10.35000 -1.20000 AFIX 0 CL7A 7 -0.297007 0.007239 0.412549 10.35000 0.20818 CL8A 7 -0.314379 -0.069023 0.495818 10.35000 0.13926 CL9A 7 -0.478516 -0.059736 0.420683 10.35000 0.27414 HKLF 4 REM c2110 in Pbca REM R1 = 0.0577 for 7055 Fo > 4sig(Fo) and 0.0687 for all 8386 data REM 460 parameters refined using 6 restraints END WGHT 0.0850 29.8995 REM Highest difference peak 1.133, deepest hole -1.203, 1-sigma level 0.124 Q1 1 -0.4619 0.0160 0.4887 11.00000 0.05 1.13 Q2 1 0.1003 0.3075 0.2673 11.00000 0.05 0.95 Q3 1 -0.4391 -0.0721 0.4911 11.00000 0.05 0.87 Q4 1 0.0625 0.1347 0.3867 11.00000 0.05 0.85 Q5 1 -0.3820 0.0197 0.4003 11.00000 0.05 0.85 Q6 1 0.4243 0.4247 0.2359 11.00000 0.05 0.79 Q7 1 -0.2790 -0.0066 0.4447 11.00000 0.05 0.77 Q8 1 0.0198 0.1361 0.4176 11.00000 0.05 0.73 Q9 1 0.0828 0.3213 0.2900 11.00000 0.05 0.70 Q10 1 -0.0816 0.1467 0.0866 11.00000 0.05 0.69 ; _database_code_depnum_ccdc_archive 'CCDC 947381' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_(3) _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis-Thiocyanato-mu-Hexafluorosilicato-tetrakis (3,3',5,5'-Tetramethyl-4,4'-bipyrazole)dicadmium(II), Solvate with 2 Dichloromethane ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H60 Cd2 Cl4 F6 N18 S2 Si' _chemical_formula_weight 1413.91 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' F F 0.0171 0.0103 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 42/m' _space_group_name_Hall '-P 4c' _symmetry_Int_Tables_number 84 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z+1/2' 'y, -x, z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z-1/2' '-y, x, -z-1/2' _cell_length_a 19.5220(8) _cell_length_b 19.5220(8) _cell_length_c 33.791(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12878.0(16) _cell_formula_units_Z 8 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 38193 _cell_measurement_theta_min 4.09 _cell_measurement_theta_max 24.93 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5712 _exptl_absorpt_coefficient_mu 0.972 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8002 _exptl_absorpt_correction_T_max 0.8293 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'Siemens SMART CCD area-detector diffractometer' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 38193 _diffrn_reflns_av_R_equivalents 0.0484 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 4.09 _diffrn_reflns_theta_max 24.93 _reflns_number_total 11058 _reflns_number_gt 9336 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT (Bruker, 1998)' _computing_cell_refinement 'SAINT-NT (Bruker, 1999)' _computing_data_reduction 'SAINT-NT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.700.00 (Farrugia, 1999)' #------------------------------- Refinement data-----------------------# _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. Crystals of the compound are twinned by merohedry (low symmetry tetragonal (4/m) cell emulates high symmetry tetragonal lattice (4/mmm). Solution in space group P42/mbc led to badly disordered model and the subsequent refinement eventually led to divergence (R1 > 0.20). Well refinable model was found in space group P42/m, with equal contributions of twin components (twin law {0 1 0 1 0 0 0 0 -1}). The refinement for the framework portion was essentially standard. CH (methyl) and NH hydrogen atoms were added geometrically, with U(iso) = 1.5U(eq) of the parent C (N) atom. Three unique solvent molecules (one molecule in general position and two half-molecules lying across mirror planes) were located. Their atoms possess large parameters for the thermal motion, indicating possible disorder. We were not successful to resolve it. These molecules were included in calculations with fixed geometry [C-Cl = 1.750(8) and Cl...Cl = 2.880(8) A]; they were left isotropic. It was impossible to locate additional solvent molecules, although checkcif routine indicates remaining solvent accessible voids in the structure. ; _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^)+(0.1188P)^2^+0.0000P] 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_number_reflns 11058 _refine_ls_number_parameters 705 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0650 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.1544 _refine_ls_wR_factor_gt 0.1487 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.995 _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 Cd1 Cd 0.32864(3) 0.62227(3) 0.0000 0.03766(17) Uani 1 2 d S . . Cd2 Cd 0.35578(2) 0.84210(2) 0.250853(16) 0.03742(14) Uani 1 1 d . . . Cd3 Cd 0.10872(3) 0.82015(3) 0.5000 0.03692(17) Uani 1 2 d S . . Si1 Si 0.5000 0.5000 0.0000 0.0249(6) Uani 1 4 d S . . Si2 Si 0.5000 1.0000 0.25234(8) 0.0252(4) Uani 1 2 d S . . Si3 Si 0.0000 1.0000 0.5000 0.0231(6) Uani 1 4 d S . . S1 S 0.0896(2) 0.6988(3) 0.0000 0.1098(17) Uani 1 2 d S . . S2 S 0.26179(19) 0.61937(16) 0.27696(15) 0.1118(12) Uani 1 1 d . . . S3 S 0.1889(3) 0.5807(2) 0.5000 0.1179(19) Uani 1 2 d S . . F1 F 0.4248(2) 0.5440(2) 0.0000 0.0323(11) Uani 1 2 d S . . F2 F 0.5000 0.5000 0.04956(15) 0.0337(10) Uani 1 2 d S . . F3 F 0.4581(2) 0.4247(2) 0.0000 0.0343(11) Uani 1 2 d S . . F4 F 0.44057(18) 0.93730(18) 0.25222(13) 0.0326(7) Uani 1 1 d . . . F5 F 0.5000 1.0000 0.30138(17) 0.0379(12) Uani 1 2 d S . . F6 F 0.4375(2) 1.05893(19) 0.25208(14) 0.0394(8) Uani 1 1 d . . . F7 F 0.5000 1.0000 0.20200(17) 0.0383(12) Uani 1 2 d S . . F8 F 0.0362(2) 0.9216(2) 0.5000 0.0312(10) Uani 1 2 d S . . F9 F 0.0783(3) 1.0356(3) 0.5000 0.0413(13) Uani 1 2 d S . . F10 F 0.0000 1.0000 0.55000(15) 0.0357(11) Uani 1 2 d S . . N1 N 0.4011(3) 0.6748(3) 0.04789(18) 0.0467(13) Uani 1 1 d . . . N2 N 0.4694(3) 0.6682(3) 0.05089(19) 0.0473(14) Uani 1 1 d . . . H2 H 0.4940 0.6446 0.0343 0.071 Uiso 1 1 calc R . . N3 N 0.4252(4) 0.8149(3) 0.19841(19) 0.0510(15) Uani 1 1 d . . . N4 N 0.4507(3) 0.8665(3) 0.17463(18) 0.0413(13) Uani 1 1 d . . . H4 H 0.4593 0.9078 0.1829 0.062 Uiso 1 1 calc R . . N5 N 0.3173(3) 0.9061(3) 0.30467(17) 0.0417(13) Uani 1 1 d . . . N6 N 0.3640(3) 0.9399(3) 0.32649(18) 0.0419(13) Uani 1 1 d . . . H6 H 0.4040 0.9521 0.3177 0.063 Uiso 1 1 calc R . . N7 N 0.1685(3) 0.8871(3) 0.45266(19) 0.0441(13) Uani 1 1 d . . . N8 N 0.1633(3) 0.9558(3) 0.44865(19) 0.0486(14) Uani 1 1 d . . . H8 H 0.1387 0.9814 0.4642 0.073 Uiso 1 1 calc R . . N9 N 0.4395(3) 0.8032(3) 0.29526(18) 0.0415(13) Uani 1 1 d . . . N10 N 0.5053(3) 0.8229(3) 0.29275(18) 0.0433(13) Uani 1 1 d . . . H10 H 0.5213 0.8476 0.2734 0.065 Uiso 1 1 calc R . . N11 N 0.5489(3) 0.6961(3) 0.44535(18) 0.0447(14) Uani 1 1 d . . . N12 N 0.5300(3) 0.6398(3) 0.42455(19) 0.0437(14) Uani 1 1 d . . . H12 H 0.5298 0.5987 0.4345 0.066 Uiso 1 1 calc R . . N13 N 0.3072(3) 0.9257(3) 0.20593(18) 0.0428(13) Uani 1 1 d . . . N14 N 0.3309(3) 0.9910(3) 0.20616(19) 0.0495(14) Uani 1 1 d . . . H14 H 0.3591 1.0068 0.2239 0.074 Uiso 1 1 calc R . . N15 N 0.1995(3) 1.0347(3) 0.05546(18) 0.0420(13) Uani 1 1 d . . . N16 N 0.1421(3) 1.0200(3) 0.07708(19) 0.0442(14) Uani 1 1 d . . . H16 H 0.1008 1.0233 0.0676 0.066 Uiso 1 1 calc R . . N17 N 0.2336(4) 0.6807(5) 0.0000 0.054(2) Uani 1 2 d S . . N18 N 0.2828(5) 0.7540(4) 0.2530(3) 0.081(3) Uani 1 1 d . . . N19 N 0.1597(5) 0.7203(5) 0.5000 0.055(2) Uani 1 2 d S . . C1 C 0.3107(5) 0.7335(6) 0.0850(4) 0.089(3) Uani 1 1 d . . . H1A H 0.2858 0.7335 0.0601 0.133 Uiso 1 1 calc R . . H1B H 0.3086 0.7787 0.0968 0.133 Uiso 1 1 calc R . . H1C H 0.2903 0.7004 0.1028 0.133 Uiso 1 1 calc R . . C2 C 0.3821(4) 0.7151(4) 0.0777(3) 0.0524(19) Uani 1 1 d . . . C3 C 0.4405(4) 0.7331(3) 0.1004(2) 0.0451(16) Uani 1 1 d . . . C4 C 0.4959(4) 0.7018(3) 0.0820(2) 0.0488(17) Uani 1 1 d . . . C5 C 0.5681(5) 0.7029(5) 0.0929(4) 0.082(3) Uani 1 1 d . . . H5A H 0.5920 0.6666 0.0791 0.122 Uiso 1 1 calc R . . H5B H 0.5724 0.6961 0.1213 0.122 Uiso 1 1 calc R . . H5C H 0.5878 0.7468 0.0857 0.122 Uiso 1 1 calc R . . C6 C 0.3978(8) 0.6939(4) 0.1881(3) 0.101(5) Uani 1 1 d . . . H6A H 0.3918 0.6962 0.2165 0.152 Uiso 1 1 calc R . . H6B H 0.4327 0.6601 0.1818 0.152 Uiso 1 1 calc R . . H6C H 0.3549 0.6808 0.1757 0.152 Uiso 1 1 calc R . . C7 C 0.4192(5) 0.7612(4) 0.1731(3) 0.058(2) Uani 1 1 d . . . C8 C 0.4413(4) 0.7791(3) 0.1354(2) 0.0446(16) Uani 1 1 d . . . C9 C 0.4609(3) 0.8454(3) 0.1370(2) 0.0391(14) Uani 1 1 d . . . C10 C 0.4898(5) 0.8927(4) 0.1061(3) 0.064(2) Uani 1 1 d . . . H10A H 0.4530 0.9196 0.0945 0.097 Uiso 1 1 calc R . . H10B H 0.5119 0.8660 0.0855 0.097 Uiso 1 1 calc R . . H10C H 0.5230 0.9231 0.1182 0.097 Uiso 1 1 calc R . . C11 C 0.2007(4) 0.8609(5) 0.3134(3) 0.071(3) Uani 1 1 d . . . H11A H 0.1958 0.8677 0.2851 0.107 Uiso 1 1 calc R . . H11B H 0.1608 0.8791 0.3269 0.107 Uiso 1 1 calc R . . H11C H 0.2046 0.8123 0.3189 0.107 Uiso 1 1 calc R . . C12 C 0.2641(3) 0.8973(4) 0.3278(2) 0.0456(17) Uani 1 1 d . . . C13 C 0.2765(3) 0.9248(4) 0.3659(2) 0.0422(15) Uani 1 1 d . . . C14 C 0.3420(3) 0.9528(4) 0.3633(2) 0.0472(16) Uani 1 1 d . . . C15 C 0.3862(5) 0.9866(7) 0.3943(4) 0.086(3) Uani 1 1 d . . . H15A H 0.4313 0.9657 0.3942 0.129 Uiso 1 1 calc R . . H15B H 0.3654 0.9808 0.4201 0.129 Uiso 1 1 calc R . . H15C H 0.3905 1.0350 0.3884 0.129 Uiso 1 1 calc R . . C16 C 0.2250(6) 0.7933(5) 0.4162(3) 0.076(3) Uani 1 1 d . . . H16A H 0.1941 0.7743 0.3966 0.114 Uiso 1 1 calc R . . H16B H 0.2194 0.7689 0.4410 0.114 Uiso 1 1 calc R . . H16C H 0.2718 0.7886 0.4071 0.114 Uiso 1 1 calc R . . C17 C 0.2090(3) 0.8668(4) 0.4222(2) 0.0484(17) Uani 1 1 d . . . C18 C 0.2306(4) 0.9240(4) 0.4009(2) 0.0477(17) Uani 1 1 d . . . C19 C 0.2008(3) 0.9810(4) 0.4175(3) 0.0482(18) Uani 1 1 d . . . C20 C 0.2006(5) 1.0548(5) 0.4073(3) 0.073(3) Uani 1 1 d . . . H20A H 0.2424 1.0760 0.4169 0.110 Uiso 1 1 calc R . . H20B H 0.1613 1.0768 0.4195 0.110 Uiso 1 1 calc R . . H20C H 0.1978 1.0600 0.3788 0.110 Uiso 1 1 calc R . . C21 C 0.3713(4) 0.7351(4) 0.3432(3) 0.062(2) Uani 1 1 d . . . H21A H 0.3341 0.7499 0.3261 0.093 Uiso 1 1 calc R . . H21B H 0.3623 0.7501 0.3701 0.093 Uiso 1 1 calc R . . H21C H 0.3746 0.6856 0.3426 0.093 Uiso 1 1 calc R . . C22 C 0.4369(4) 0.7657(3) 0.3291(2) 0.0445(16) Uani 1 1 d . . . C23 C 0.5006(4) 0.7635(3) 0.3475(2) 0.0418(15) Uani 1 1 d . . . C24 C 0.5442(4) 0.8005(4) 0.3232(2) 0.0491(18) Uani 1 1 d . . . C25 C 0.6188(4) 0.8165(5) 0.3255(3) 0.067(2) Uani 1 1 d . . . H25A H 0.6445 0.7823 0.3109 0.100 Uiso 1 1 calc R . . H25B H 0.6333 0.8162 0.3530 0.100 Uiso 1 1 calc R . . H25C H 0.6272 0.8614 0.3142 0.100 Uiso 1 1 calc R . . C26 C 0.5547(6) 0.8209(4) 0.4315(3) 0.074(3) Uani 1 1 d . . . H26A H 0.5483 0.8257 0.4598 0.111 Uiso 1 1 calc R . . H26B H 0.5224 0.8502 0.4177 0.111 Uiso 1 1 calc R . . H26C H 0.6010 0.8341 0.4245 0.111 Uiso 1 1 calc R . . C27 C 0.5427(4) 0.7473(3) 0.4197(2) 0.0472(16) Uani 1 1 d . . . C28 C 0.5185(4) 0.7247(3) 0.3832(2) 0.0421(16) Uani 1 1 d . . . C29 C 0.5118(3) 0.6536(3) 0.3874(2) 0.0411(15) Uani 1 1 d . . . C30 C 0.4911(5) 0.5989(4) 0.3588(3) 0.060(2) Uani 1 1 d . . . H30A H 0.4937 0.5546 0.3717 0.090 Uiso 1 1 calc R . . H30B H 0.5217 0.5995 0.3362 0.090 Uiso 1 1 calc R . . H30C H 0.4446 0.6071 0.3500 0.090 Uiso 1 1 calc R . . C31 C 0.2335(5) 0.8548(4) 0.1630(3) 0.061(2) Uani 1 1 d . . . H31A H 0.2683 0.8210 0.1570 0.091 Uiso 1 1 calc R . . H31B H 0.2047 0.8618 0.1400 0.091 Uiso 1 1 calc R . . H31C H 0.2057 0.8389 0.1849 0.091 Uiso 1 1 calc R . . C32 C 0.2672(3) 0.9212(4) 0.1741(2) 0.0438(16) Uani 1 1 d . . . C33 C 0.2643(3) 0.9846(4) 0.1545(2) 0.0424(15) Uani 1 1 d . . . C34 C 0.3069(4) 1.0280(4) 0.1766(3) 0.0498(18) Uani 1 1 d . . . C35 C 0.3246(5) 1.1013(5) 0.1703(3) 0.074(3) Uani 1 1 d . . . H35A H 0.3041 1.1288 0.1911 0.111 Uiso 1 1 calc R . . H35B H 0.3073 1.1161 0.1448 0.111 Uiso 1 1 calc R . . H35C H 0.3739 1.1067 0.1710 0.111 Uiso 1 1 calc R . . C36 C 0.3243(4) 1.0331(6) 0.0677(3) 0.070(2) Uani 1 1 d . . . H36A H 0.3415 0.9903 0.0571 0.104 Uiso 1 1 calc R . . H36B H 0.3523 1.0470 0.0901 0.104 Uiso 1 1 calc R . . H36C H 0.3262 1.0682 0.0474 0.104 Uiso 1 1 calc R . . C37 C 0.2509(3) 1.0238(4) 0.0811(2) 0.0428(15) Uani 1 1 d . . . C38 C 0.2260(3) 1.0020(4) 0.1180(2) 0.0454(16) Uani 1 1 d . . . C39 C 0.1555(3) 1.0002(4) 0.1141(2) 0.0424(15) Uani 1 1 d . . . C40 C 0.1005(4) 0.9845(5) 0.1429(3) 0.065(2) Uani 1 1 d . . . H40A H 0.0631 1.0167 0.1394 0.098 Uiso 1 1 calc R . . H40B H 0.1185 0.9884 0.1695 0.098 Uiso 1 1 calc R . . H40C H 0.0840 0.9383 0.1385 0.098 Uiso 1 1 calc R . . C41 C 0.1733(9) 0.6856(7) 0.0000 0.077(4) Uani 1 2 d S . . C42 C 0.2762(5) 0.6967(6) 0.2632(3) 0.073(2) Uani 1 1 d . . . C43 C 0.1745(8) 0.6647(7) 0.5000 0.069(4) Uani 1 2 d S . . C44 C 0.1968(5) 1.0230(7) 0.2635(9) 0.198(7) Uiso 1 1 d D . . H44A H 0.2105 0.9865 0.2817 0.237 Uiso 1 1 calc R . . H44B H 0.2083 1.0083 0.2366 0.237 Uiso 1 1 calc R . . Cl1 Cl 0.2423(4) 1.0969(4) 0.2746(3) 0.219(3) Uiso 1 1 d D . . Cl2 Cl 0.1086(4) 1.0350(4) 0.2668(4) 0.250(4) Uiso 1 1 d D . . C45 C 0.3049(14) 0.3490(17) 0.0000 0.198(7) Uiso 1 2 d SD . . H45A H 0.3528 0.3642 0.0000 0.237 Uiso 1 2 calc SR . . H45B H 0.3044 0.2988 0.0000 0.237 Uiso 1 2 calc SR . . Cl3 Cl 0.2630(9) 0.3800(9) 0.04228(12) 0.413(8) Uiso 1 1 d D . . C46 C 0.1934(18) 0.9090(9) 0.0000 0.198(7) Uiso 1 2 d SD . . H46A H 0.1467 0.9274 0.0000 0.237 Uiso 1 2 calc SR . . H46B H 0.2253 0.9478 0.0000 0.237 Uiso 1 2 calc SR . . Cl4 Cl 0.2059(5) 0.8610(5) 0.04267(12) 0.257(4) Uiso 1 1 d 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 Cd1 0.0433(3) 0.0461(4) 0.0236(4) 0.000 0.000 0.0034(3) Cd2 0.0459(3) 0.0441(3) 0.0223(2) -0.00201(19) 0.00002(19) -0.0074(2) Cd3 0.0455(3) 0.0413(3) 0.0239(4) 0.000 0.000 0.0061(3) Si1 0.0269(14) 0.0329(15) 0.0150(17) 0.000 0.000 0.0024(12) Si2 0.0295(10) 0.0270(10) 0.0191(11) 0.000 0.000 -0.0022(8) Si3 0.0297(14) 0.0237(13) 0.0159(16) 0.000 0.000 0.0038(11) S1 0.068(2) 0.146(4) 0.114(4) 0.000 0.000 0.034(2) S2 0.117(2) 0.0786(18) 0.140(4) 0.0053(19) -0.003(2) -0.0228(16) S3 0.161(5) 0.066(2) 0.126(5) 0.000 0.000 0.047(3) F1 0.031(2) 0.040(2) 0.026(3) 0.000 0.000 0.0107(19) F2 0.029(2) 0.054(3) 0.017(3) 0.000 0.000 0.0089(19) F3 0.034(2) 0.041(3) 0.028(3) 0.000 0.000 -0.0096(19) F4 0.0356(18) 0.0357(18) 0.0264(18) 0.0053(14) -0.0025(14) -0.0038(13) F5 0.036(2) 0.056(3) 0.021(3) 0.000 0.000 -0.002(2) F6 0.0414(19) 0.0376(19) 0.039(2) -0.0072(15) -0.0090(16) 0.0101(14) F7 0.058(3) 0.033(2) 0.024(3) 0.000 0.000 -0.011(2) F8 0.044(3) 0.027(2) 0.023(3) 0.000 0.000 0.0065(18) F9 0.039(3) 0.042(3) 0.042(4) 0.000 0.000 0.000(2) F10 0.052(3) 0.035(2) 0.020(3) 0.000 0.000 0.002(2) N1 0.065(4) 0.043(3) 0.032(4) -0.012(2) 0.003(3) 0.001(3) N2 0.058(3) 0.047(3) 0.037(4) -0.016(3) 0.007(3) 0.006(3) N3 0.086(4) 0.035(3) 0.032(4) -0.005(2) 0.013(3) 0.001(3) N4 0.064(3) 0.033(2) 0.027(3) -0.009(2) 0.007(2) -0.009(2) N5 0.034(3) 0.065(3) 0.026(3) -0.002(3) 0.004(2) -0.001(2) N6 0.039(3) 0.056(3) 0.031(3) -0.007(2) 0.008(2) -0.004(2) N7 0.042(3) 0.055(3) 0.035(4) -0.005(2) 0.012(2) 0.000(2) N8 0.043(3) 0.061(4) 0.042(4) 0.000(3) 0.019(3) -0.002(3) N9 0.047(3) 0.048(3) 0.029(3) 0.013(2) 0.007(2) 0.006(2) N10 0.055(3) 0.045(3) 0.030(3) 0.018(2) 0.000(2) -0.004(2) N11 0.069(4) 0.036(3) 0.030(3) 0.004(2) -0.004(3) -0.003(2) N12 0.060(3) 0.038(3) 0.033(4) 0.006(2) -0.014(3) -0.004(3) N13 0.046(3) 0.053(3) 0.030(3) 0.000(2) -0.009(2) -0.001(2) N14 0.054(3) 0.057(3) 0.037(4) -0.003(3) -0.022(3) 0.005(3) N15 0.038(3) 0.062(3) 0.027(3) 0.004(2) -0.007(2) -0.001(2) N16 0.026(2) 0.076(4) 0.030(4) 0.003(3) -0.007(2) -0.002(2) N17 0.038(4) 0.078(6) 0.047(6) 0.000 0.000 0.024(4) N18 0.100(6) 0.074(6) 0.068(6) -0.014(4) 0.003(5) -0.046(5) N19 0.063(5) 0.055(5) 0.048(6) 0.000 0.000 0.012(4) C1 0.078(6) 0.102(8) 0.087(9) -0.043(7) 0.006(6) 0.015(6) C2 0.068(5) 0.046(4) 0.044(5) -0.015(3) 0.014(4) -0.003(3) C3 0.065(4) 0.037(3) 0.034(4) -0.005(3) 0.006(3) -0.004(3) C4 0.073(5) 0.040(3) 0.033(4) -0.015(3) 0.009(4) 0.002(3) C5 0.088(7) 0.076(6) 0.081(8) -0.033(6) -0.013(6) 0.007(5) C6 0.203(13) 0.045(4) 0.056(7) -0.010(4) 0.064(8) -0.022(6) C7 0.095(6) 0.032(3) 0.047(5) -0.008(3) 0.018(4) -0.007(4) C8 0.068(4) 0.038(3) 0.027(4) -0.005(3) -0.001(3) -0.002(3) C9 0.058(4) 0.042(3) 0.018(3) -0.003(3) 0.000(3) -0.001(3) C10 0.101(6) 0.057(4) 0.036(5) 0.000(4) 0.019(4) -0.022(4) C11 0.043(4) 0.095(6) 0.076(7) -0.018(5) 0.003(4) -0.024(4) C12 0.041(3) 0.067(4) 0.029(4) -0.008(3) 0.004(3) -0.005(3) C13 0.039(3) 0.057(4) 0.030(4) -0.003(3) 0.010(3) -0.002(3) C14 0.039(3) 0.064(4) 0.038(4) -0.013(3) 0.008(3) -0.005(3) C15 0.065(5) 0.135(9) 0.058(7) -0.045(6) 0.007(5) -0.023(6) C16 0.097(7) 0.082(6) 0.048(6) 0.000(4) 0.040(5) 0.018(5) C17 0.037(3) 0.076(5) 0.032(4) -0.012(3) 0.010(3) 0.009(3) C18 0.043(3) 0.073(5) 0.028(4) -0.008(3) 0.013(3) 0.000(3) C19 0.045(4) 0.059(4) 0.041(5) -0.002(3) 0.011(3) -0.003(3) C20 0.096(7) 0.071(5) 0.052(6) 0.003(4) 0.030(5) -0.011(5) C21 0.060(4) 0.070(5) 0.055(6) 0.025(4) 0.008(4) 0.002(4) C22 0.068(4) 0.035(3) 0.030(4) 0.011(3) 0.008(3) 0.003(3) C23 0.065(4) 0.031(3) 0.029(4) 0.009(3) -0.004(3) -0.002(3) C24 0.063(4) 0.046(4) 0.038(5) 0.017(3) -0.011(3) 0.001(3) C25 0.058(5) 0.088(6) 0.054(6) 0.027(5) -0.007(4) -0.012(4) C26 0.118(7) 0.036(4) 0.068(7) 0.004(4) -0.027(6) -0.005(4) C27 0.066(4) 0.039(3) 0.036(4) 0.001(3) -0.006(3) -0.002(3) C28 0.059(4) 0.036(3) 0.031(4) 0.011(3) 0.003(3) -0.002(3) C29 0.057(4) 0.036(3) 0.030(4) 0.006(3) 0.001(3) 0.002(3) C30 0.095(6) 0.044(4) 0.040(5) 0.006(3) -0.018(4) -0.004(4) C31 0.071(5) 0.060(4) 0.051(6) 0.001(4) -0.028(4) -0.010(4) C32 0.033(3) 0.065(4) 0.033(4) -0.006(3) -0.005(3) 0.006(3) C33 0.034(3) 0.062(4) 0.031(4) 0.002(3) -0.009(3) -0.002(3) C34 0.041(4) 0.060(4) 0.048(5) 0.007(3) -0.015(3) 0.002(3) C35 0.078(6) 0.070(5) 0.075(7) 0.012(5) -0.037(5) -0.016(5) C36 0.040(4) 0.117(7) 0.051(6) 0.023(5) 0.004(4) 0.009(4) C37 0.036(3) 0.062(4) 0.031(4) -0.001(3) -0.005(3) 0.004(3) C38 0.033(3) 0.068(4) 0.035(4) 0.002(3) -0.008(3) 0.004(3) C39 0.034(3) 0.058(4) 0.035(4) 0.006(3) -0.008(3) 0.001(3) C40 0.043(4) 0.100(6) 0.054(6) 0.026(5) -0.005(4) -0.006(4) C41 0.127(13) 0.064(7) 0.040(8) 0.000 0.000 -0.004(8) C42 0.071(5) 0.086(7) 0.062(6) -0.012(5) -0.008(5) -0.019(5) C43 0.097(9) 0.070(8) 0.039(8) 0.000 0.000 0.049(7) _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 Cd1 N17 2.178(8) . ? Cd1 N1 2.381(6) . ? Cd1 N1 2.381(6) 6 ? Cd1 N11 2.387(6) 3_654 ? Cd1 N11 2.387(6) 8_656 ? Cd1 F1 2.420(4) . ? Cd2 N18 2.234(7) . ? Cd2 N3 2.294(6) . ? Cd2 N5 2.331(6) . ? Cd2 N9 2.345(6) . ? Cd2 N13 2.422(6) . ? Cd2 F4 2.489(3) . ? Cd3 N19 2.188(9) . ? Cd3 N7 2.372(6) 6_556 ? Cd3 N7 2.372(6) . ? Cd3 N15 2.397(6) 7_466 ? Cd3 N15 2.397(6) 4_465 ? Cd3 F8 2.435(4) . ? Si1 F2 1.675(5) 5_665 ? Si1 F2 1.675(5) . ? Si1 F3 1.683(5) . ? Si1 F3 1.683(5) 5_665 ? Si1 F1 1.702(4) 5_665 ? Si1 F1 1.702(4) . ? Si2 F5 1.657(6) . ? Si2 F6 1.677(3) 2_675 ? Si2 F6 1.677(3) . ? Si2 F4 1.686(3) . ? Si2 F4 1.686(3) 2_675 ? Si2 F7 1.701(6) . ? Si3 F9 1.679(5) . ? Si3 F9 1.679(5) 5_576 ? Si3 F8 1.686(4) . ? Si3 F8 1.686(4) 5_576 ? Si3 F10 1.689(5) 5_576 ? Si3 F10 1.689(5) . ? S1 C41 1.654(19) . ? S2 C42 1.604(11) . ? S3 C43 1.664(13) . ? N1 C2 1.332(9) . ? N1 N2 1.344(9) . ? N2 C4 1.343(10) . ? N3 C7 1.359(10) . ? N3 N4 1.381(8) . ? N4 C9 1.351(9) . ? N5 C12 1.311(9) . ? N5 N6 1.345(8) . ? N6 C14 1.340(9) . ? N7 N8 1.352(8) . ? N7 C17 1.355(9) . ? N8 C19 1.373(10) . ? N9 N10 1.344(8) . ? N9 C22 1.359(9) . ? N10 C24 1.352(9) . ? N11 C27 1.328(9) . ? N11 N12 1.354(8) . ? N11 Cd1 2.387(6) 7_566 ? N12 C29 1.333(9) . ? N13 C32 1.333(9) . ? N13 N14 1.356(9) . ? N14 C34 1.319(10) . ? N15 C37 1.344(9) . ? N15 N16 1.368(8) . ? N15 Cd3 2.397(6) 3_664 ? N16 C39 1.334(9) . ? N17 C41 1.180(19) . ? N18 C42 1.179(13) . ? N19 C43 1.124(14) . ? C1 C2 1.459(12) . ? C2 C3 1.417(11) . ? C3 C4 1.389(10) . ? C3 C8 1.486(10) . ? C4 C5 1.457(13) . ? C6 C7 1.468(11) . ? C7 C8 1.388(12) . ? C8 C9 1.350(9) . ? C9 C10 1.505(10) . ? C11 C12 1.510(10) . ? C12 C13 1.416(11) . ? C13 C14 1.392(9) . ? C13 C18 1.483(10) . ? C14 C15 1.510(12) . ? C16 C17 1.482(12) . ? C17 C18 1.394(11) . ? C18 C19 1.376(10) . ? C19 C20 1.482(12) . ? C21 C22 1.491(11) . ? C22 C23 1.391(10) . ? C23 C24 1.386(11) . ? C23 C28 1.465(9) . ? C24 C25 1.491(11) . ? C26 C27 1.510(10) . ? C27 C28 1.393(11) . ? C28 C29 1.401(9) . ? C29 C30 1.496(11) . ? C31 C32 1.500(11) . ? C32 C33 1.405(10) . ? C33 C34 1.403(10) . ? C33 C38 1.482(10) . ? C34 C35 1.486(11) . ? C36 C37 1.514(10) . ? C37 C38 1.401(11) . ? C38 C39 1.383(9) . ? C39 C40 1.481(11) . ? C44 Cl1 1.736(8) . ? C44 Cl2 1.740(8) . ? C45 Cl3 1.754(6) 6 ? C45 Cl3 1.754(6) . ? C46 Cl4 1.737(6) 6 ? C46 Cl4 1.737(6) . ? 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 N17 Cd1 N1 106.3(2) . . ? N17 Cd1 N1 106.3(2) . 6 ? N1 Cd1 N1 85.6(3) . 6 ? N17 Cd1 N11 98.2(2) . 3_654 ? N1 Cd1 N11 154.75(19) . 3_654 ? N1 Cd1 N11 81.5(2) 6 3_654 ? N17 Cd1 N11 98.2(2) . 8_656 ? N1 Cd1 N11 81.5(2) . 8_656 ? N1 Cd1 N11 154.75(19) 6 8_656 ? N11 Cd1 N11 101.4(3) 3_654 8_656 ? N17 Cd1 F1 172.4(3) . . ? N1 Cd1 F1 79.12(16) . . ? N1 Cd1 F1 79.12(16) 6 . ? N11 Cd1 F1 77.16(15) 3_654 . ? N11 Cd1 F1 77.16(15) 8_656 . ? N18 Cd2 N3 103.0(3) . . ? N18 Cd2 N5 100.4(3) . . ? N3 Cd2 N5 156.6(2) . . ? N18 Cd2 N9 100.0(3) . . ? N3 Cd2 N9 90.4(2) . . ? N5 Cd2 N9 84.2(2) . . ? N18 Cd2 N13 106.9(3) . . ? N3 Cd2 N13 84.4(2) . . ? N5 Cd2 N13 90.1(2) . . ? N9 Cd2 N13 153.15(18) . . ? N18 Cd2 F4 176.4(3) . . ? N3 Cd2 F4 78.11(18) . . ? N5 Cd2 F4 78.45(17) . . ? N9 Cd2 F4 76.52(17) . . ? N13 Cd2 F4 76.63(16) . . ? N19 Cd3 N7 105.5(2) . 6_556 ? N19 Cd3 N7 105.5(2) . . ? N7 Cd3 N7 84.8(3) 6_556 . ? N19 Cd3 N15 97.6(2) . 7_466 ? N7 Cd3 N15 155.77(19) 6_556 7_466 ? N7 Cd3 N15 81.8(2) . 7_466 ? N19 Cd3 N15 97.6(2) . 4_465 ? N7 Cd3 N15 81.8(2) 6_556 4_465 ? N7 Cd3 N15 155.77(19) . 4_465 ? N15 Cd3 N15 102.9(3) 7_466 4_465 ? N19 Cd3 F8 171.5(3) . . ? N7 Cd3 F8 80.70(15) 6_556 . ? N7 Cd3 F8 80.70(15) . . ? N15 Cd3 F8 77.27(15) 7_466 . ? N15 Cd3 F8 77.27(15) 4_465 . ? F2 Si1 F2 180.0 5_665 . ? F2 Si1 F3 90.0 5_665 . ? F2 Si1 F3 90.0 . . ? F2 Si1 F3 90.0 5_665 5_665 ? F2 Si1 F3 90.0 . 5_665 ? F2 Si1 F1 90.0 5_665 5_665 ? F2 Si1 F1 90.0 . 5_665 ? F3 Si1 F1 88.8(2) . 5_665 ? F3 Si1 F1 91.2(2) 5_665 5_665 ? F2 Si1 F1 90.0 5_665 . ? F2 Si1 F1 90.0 . . ? F3 Si1 F1 91.2(2) . . ? F3 Si1 F1 88.8(2) 5_665 . ? F5 Si2 F6 90.30(19) . 2_675 ? F5 Si2 F6 90.30(19) . . ? F6 Si2 F6 179.4(4) 2_675 . ? F5 Si2 F4 90.14(17) . . ? F6 Si2 F4 90.16(18) 2_675 . ? F6 Si2 F4 89.84(18) . . ? F5 Si2 F4 90.14(17) . 2_675 ? F6 Si2 F4 89.84(18) 2_675 2_675 ? F6 Si2 F4 90.16(18) . 2_675 ? F4 Si2 F4 179.7(3) . 2_675 ? F6 Si2 F7 89.70(19) 2_675 . ? F6 Si2 F7 89.70(19) . . ? F4 Si2 F7 89.86(17) . . ? F4 Si2 F7 89.86(17) 2_675 . ? F9 Si3 F9 180.0(3) . 5_576 ? F9 Si3 F8 89.7(2) . . ? F9 Si3 F8 90.3(2) 5_576 . ? F9 Si3 F8 90.3(2) . 5_576 ? F9 Si3 F8 89.7(2) 5_576 5_576 ? F8 Si3 F10 90.0 . 5_576 ? F8 Si3 F10 90.0 5_576 5_576 ? F8 Si3 F10 90.0 . . ? F8 Si3 F10 90.0 5_576 . ? Si1 F1 Cd1 171.2(3) . . ? Si2 F4 Cd2 178.0(3) . . ? Si3 F8 Cd3 169.2(3) . . ? C2 N1 N2 106.0(6) . . ? C2 N1 Cd1 127.2(5) . . ? N2 N1 Cd1 126.8(4) . . ? C4 N2 N1 113.3(6) . . ? C7 N3 N4 103.2(6) . . ? C7 N3 Cd2 127.9(5) . . ? N4 N3 Cd2 119.6(4) . . ? C9 N4 N3 112.2(5) . . ? C12 N5 N6 105.9(6) . . ? C12 N5 Cd2 130.6(5) . . ? N6 N5 Cd2 118.1(4) . . ? C14 N6 N5 112.5(5) . . ? N8 N7 C17 104.9(6) . . ? N8 N7 Cd3 125.2(4) . . ? C17 N7 Cd3 129.6(5) . . ? N7 N8 C19 113.1(6) . . ? N10 N9 C22 104.0(6) . . ? N10 N9 Cd2 122.2(4) . . ? C22 N9 Cd2 133.4(5) . . ? N9 N10 C24 113.4(6) . . ? C27 N11 N12 104.3(6) . . ? C27 N11 Cd1 135.3(5) . 7_566 ? N12 N11 Cd1 113.6(4) . 7_566 ? C29 N12 N11 113.4(5) . . ? C32 N13 N14 105.5(6) . . ? C32 N13 Cd2 133.7(5) . . ? N14 N13 Cd2 119.8(4) . . ? C34 N14 N13 112.9(6) . . ? C37 N15 N16 103.5(6) . . ? C37 N15 Cd3 136.1(5) . 3_664 ? N16 N15 Cd3 114.4(4) . 3_664 ? C39 N16 N15 113.6(5) . . ? C41 N17 Cd1 153.1(10) . . ? C42 N18 Cd2 144.2(9) . . ? C43 N19 Cd3 167.9(12) . . ? N1 C2 C3 109.4(7) . . ? N1 C2 C1 122.5(8) . . ? C3 C2 C1 128.0(8) . . ? C4 C3 C2 106.0(7) . . ? C4 C3 C8 127.8(7) . . ? C2 C3 C8 126.1(7) . . ? N2 C4 C3 105.4(7) . . ? N2 C4 C5 125.3(7) . . ? C3 C4 C5 129.3(8) . . ? N3 C7 C8 110.8(6) . . ? N3 C7 C6 119.9(8) . . ? C8 C7 C6 129.0(7) . . ? C9 C8 C7 107.1(6) . . ? C9 C8 C3 127.9(7) . . ? C7 C8 C3 125.0(6) . . ? C8 C9 N4 106.7(6) . . ? C8 C9 C10 131.9(7) . . ? N4 C9 C10 121.4(6) . . ? N5 C12 C13 111.0(6) . . ? N5 C12 C11 121.2(7) . . ? C13 C12 C11 127.8(7) . . ? C14 C13 C12 104.3(6) . . ? C14 C13 C18 127.6(7) . . ? C12 C13 C18 128.1(6) . . ? N6 C14 C13 106.3(6) . . ? N6 C14 C15 122.8(7) . . ? C13 C14 C15 130.7(7) . . ? N7 C17 C18 109.6(6) . . ? N7 C17 C16 120.6(7) . . ? C18 C17 C16 129.9(7) . . ? C19 C18 C17 108.0(6) . . ? C19 C18 C13 124.9(7) . . ? C17 C18 C13 127.1(7) . . ? N8 C19 C18 104.4(6) . . ? N8 C19 C20 121.7(7) . . ? C18 C19 C20 133.9(8) . . ? N9 C22 C23 111.1(6) . . ? N9 C22 C21 121.0(7) . . ? C23 C22 C21 127.8(7) . . ? C24 C23 C22 105.6(6) . . ? C24 C23 C28 127.6(6) . . ? C22 C23 C28 126.6(6) . . ? N10 C24 C23 105.9(6) . . ? N10 C24 C25 121.4(7) . . ? C23 C24 C25 132.7(7) . . ? N11 C27 C28 111.8(6) . . ? N11 C27 C26 122.1(7) . . ? C28 C27 C26 125.9(7) . . ? C27 C28 C29 104.8(6) . . ? C27 C28 C23 130.3(6) . . ? C29 C28 C23 124.9(7) . . ? N12 C29 C28 105.7(6) . . ? N12 C29 C30 122.4(6) . . ? C28 C29 C30 131.9(7) . . ? N13 C32 C33 110.3(6) . . ? N13 C32 C31 121.0(7) . . ? C33 C32 C31 128.7(7) . . ? C34 C33 C32 104.9(6) . . ? C34 C33 C38 127.2(7) . . ? C32 C33 C38 127.9(6) . . ? N14 C34 C33 106.4(6) . . ? N14 C34 C35 123.6(7) . . ? C33 C34 C35 130.0(7) . . ? N15 C37 C38 111.3(6) . . ? N15 C37 C36 119.6(7) . . ? C38 C37 C36 129.1(6) . . ? C39 C38 C37 105.6(6) . . ? C39 C38 C33 125.1(7) . . ? C37 C38 C33 129.3(6) . . ? N16 C39 C38 106.1(6) . . ? N16 C39 C40 122.2(6) . . ? C38 C39 C40 131.6(7) . . ? N17 C41 S1 175.7(13) . . ? N18 C42 S2 176.2(10) . . ? N19 C43 S3 174.8(15) . . ? Cl1 C44 Cl2 112.4(7) . . ? Cl3 C45 Cl3 109.1(7) 6 . ? Cl4 C46 Cl4 112.2(7) 6 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag F9 Si3 F8 Cd3 0.0 . . . . ? F9 Si3 F8 Cd3 180.0 5_576 . . . ? F10 Si3 F8 Cd3 90.0 5_576 . . . ? F10 Si3 F8 Cd3 -90.0 . . . . ? N7 Cd3 F8 Si3 43.10(15) 6_556 . . . ? N7 Cd3 F8 Si3 -43.10(15) . . . . ? N15 Cd3 F8 Si3 -126.73(15) 7_466 . . . ? N15 Cd3 F8 Si3 126.73(15) 4_465 . . . ? N17 Cd1 N1 C2 20.6(7) . . . . ? N1 Cd1 N1 C2 126.3(6) 6 . . . ? N11 Cd1 N1 C2 -174.2(6) 3_654 . . . ? N11 Cd1 N1 C2 -75.5(7) 8_656 . . . ? F1 Cd1 N1 C2 -153.9(7) . . . . ? N17 Cd1 N1 N2 -161.3(6) . . . . ? N1 Cd1 N1 N2 -55.5(6) 6 . . . ? N11 Cd1 N1 N2 3.9(9) 3_654 . . . ? N11 Cd1 N1 N2 102.7(6) 8_656 . . . ? F1 Cd1 N1 N2 24.2(5) . . . . ? C2 N1 N2 C4 1.1(9) . . . . ? Cd1 N1 N2 C4 -177.3(5) . . . . ? N18 Cd2 N3 C7 4.9(8) . . . . ? N5 Cd2 N3 C7 -178.4(6) . . . . ? N9 Cd2 N3 C7 105.3(7) . . . . ? N13 Cd2 N3 C7 -101.1(7) . . . . ? F4 Cd2 N3 C7 -178.6(8) . . . . ? N18 Cd2 N3 N4 145.6(6) . . . . ? N5 Cd2 N3 N4 -37.7(9) . . . . ? N9 Cd2 N3 N4 -114.0(5) . . . . ? N13 Cd2 N3 N4 39.6(5) . . . . ? F4 Cd2 N3 N4 -37.9(5) . . . . ? C7 N3 N4 C9 -1.0(9) . . . . ? Cd2 N3 N4 C9 -150.1(5) . . . . ? N18 Cd2 N5 C12 -5.7(7) . . . . ? N3 Cd2 N5 C12 177.6(6) . . . . ? N9 Cd2 N5 C12 -104.8(7) . . . . ? N13 Cd2 N5 C12 101.5(7) . . . . ? F4 Cd2 N5 C12 177.8(7) . . . . ? N18 Cd2 N5 N6 144.5(5) . . . . ? N3 Cd2 N5 N6 -32.2(9) . . . . ? N9 Cd2 N5 N6 45.4(5) . . . . ? N13 Cd2 N5 N6 -108.3(5) . . . . ? F4 Cd2 N5 N6 -32.0(5) . . . . ? C12 N5 N6 C14 0.3(8) . . . . ? Cd2 N5 N6 C14 -156.6(5) . . . . ? N19 Cd3 N7 N8 -166.0(5) . . . . ? N7 Cd3 N7 N8 -61.4(6) 6_556 . . . ? N15 Cd3 N7 N8 98.3(5) 7_466 . . . ? N15 Cd3 N7 N8 -4.8(9) 4_465 . . . ? F8 Cd3 N7 N8 20.0(5) . . . . ? N19 Cd3 N7 C17 20.7(7) . . . . ? N7 Cd3 N7 C17 125.3(6) 6_556 . . . ? N15 Cd3 N7 C17 -75.0(6) 7_466 . . . ? N15 Cd3 N7 C17 -178.1(6) 4_465 . . . ? F8 Cd3 N7 C17 -153.3(6) . . . . ? C17 N7 N8 C19 -2.1(8) . . . . ? Cd3 N7 N8 C19 -176.8(5) . . . . ? N18 Cd2 N9 N10 152.5(5) . . . . ? N3 Cd2 N9 N10 49.3(5) . . . . ? N5 Cd2 N9 N10 -107.9(5) . . . . ? N13 Cd2 N9 N10 -29.2(8) . . . . ? F4 Cd2 N9 N10 -28.4(5) . . . . ? N18 Cd2 N9 C22 -35.1(7) . . . . ? N3 Cd2 N9 C22 -138.3(7) . . . . ? N5 Cd2 N9 C22 64.5(7) . . . . ? N13 Cd2 N9 C22 143.2(6) . . . . ? F4 Cd2 N9 C22 144.0(7) . . . . ? C22 N9 N10 C24 -0.6(8) . . . . ? Cd2 N9 N10 C24 173.8(5) . . . . ? C27 N11 N12 C29 -0.6(9) . . . . ? Cd1 N11 N12 C29 -156.5(5) 7_566 . . . ? N18 Cd2 N13 C32 -30.2(8) . . . . ? N3 Cd2 N13 C32 71.7(7) . . . . ? N5 Cd2 N13 C32 -131.1(7) . . . . ? N9 Cd2 N13 C32 151.6(6) . . . . ? F4 Cd2 N13 C32 150.8(7) . . . . ? N18 Cd2 N13 N14 163.6(5) . . . . ? N3 Cd2 N13 N14 -94.5(5) . . . . ? N5 Cd2 N13 N14 62.7(5) . . . . ? N9 Cd2 N13 N14 -14.6(8) . . . . ? F4 Cd2 N13 N14 -15.5(5) . . . . ? C32 N13 N14 C34 1.3(8) . . . . ? Cd2 N13 N14 C34 171.0(5) . . . . ? C37 N15 N16 C39 -0.7(8) . . . . ? Cd3 N15 N16 C39 -157.9(5) 3_664 . . . ? N1 Cd1 N17 C41 -134.92(17) . . . . ? N1 Cd1 N17 C41 134.92(17) 6 . . . ? N11 Cd1 N17 C41 51.41(16) 3_654 . . . ? N11 Cd1 N17 C41 -51.41(16) 8_656 . . . ? N3 Cd2 N18 C42 78.7(15) . . . . ? N5 Cd2 N18 C42 -100.0(15) . . . . ? N9 Cd2 N18 C42 -14.1(15) . . . . ? N13 Cd2 N18 C42 166.7(14) . . . . ? N7 Cd3 N19 C43 135.61(16) 6_556 . . . ? N7 Cd3 N19 C43 -135.61(16) . . . . ? N15 Cd3 N19 C43 -52.06(15) 7_466 . . . ? N15 Cd3 N19 C43 52.06(15) 4_465 . . . ? N2 N1 C2 C3 -1.2(8) . . . . ? Cd1 N1 C2 C3 177.3(5) . . . . ? N2 N1 C2 C1 -178.9(9) . . . . ? Cd1 N1 C2 C1 -0.4(13) . . . . ? N1 C2 C3 C4 0.8(9) . . . . ? C1 C2 C3 C4 178.4(10) . . . . ? N1 C2 C3 C8 178.0(7) . . . . ? C1 C2 C3 C8 -4.5(14) . . . . ? N1 N2 C4 C3 -0.6(9) . . . . ? N1 N2 C4 C5 179.0(8) . . . . ? C2 C3 C4 N2 -0.1(8) . . . . ? C8 C3 C4 N2 -177.2(7) . . . . ? C2 C3 C4 C5 -179.7(9) . . . . ? C8 C3 C4 C5 3.2(14) . . . . ? N4 N3 C7 C8 1.0(10) . . . . ? Cd2 N3 C7 C8 146.5(6) . . . . ? N4 N3 C7 C6 175.7(10) . . . . ? Cd2 N3 C7 C6 -38.8(13) . . . . ? N3 C7 C8 C9 -0.6(10) . . . . ? C6 C7 C8 C9 -174.7(11) . . . . ? N3 C7 C8 C3 -178.7(7) . . . . ? C6 C7 C8 C3 7.2(16) . . . . ? C4 C3 C8 C9 75.3(11) . . . . ? C2 C3 C8 C9 -101.2(10) . . . . ? C4 C3 C8 C7 -107.0(10) . . . . ? C2 C3 C8 C7 76.5(11) . . . . ? C7 C8 C9 N4 0.0(8) . . . . ? C3 C8 C9 N4 178.0(7) . . . . ? C7 C8 C9 C10 179.3(9) . . . . ? C3 C8 C9 C10 -2.7(14) . . . . ? N3 N4 C9 C8 0.6(8) . . . . ? N3 N4 C9 C10 -178.8(7) . . . . ? N6 N5 C12 C13 -1.1(8) . . . . ? Cd2 N5 C12 C13 151.8(5) . . . . ? N6 N5 C12 C11 179.9(7) . . . . ? Cd2 N5 C12 C11 -27.2(11) . . . . ? N5 C12 C13 C14 1.5(9) . . . . ? C11 C12 C13 C14 -179.7(8) . . . . ? N5 C12 C13 C18 -178.3(7) . . . . ? C11 C12 C13 C18 0.5(14) . . . . ? N5 N6 C14 C13 0.6(8) . . . . ? N5 N6 C14 C15 176.5(8) . . . . ? C12 C13 C14 N6 -1.2(8) . . . . ? C18 C13 C14 N6 178.6(7) . . . . ? C12 C13 C14 C15 -176.7(10) . . . . ? C18 C13 C14 C15 3.2(14) . . . . ? N8 N7 C17 C18 2.6(8) . . . . ? Cd3 N7 C17 C18 177.0(5) . . . . ? N8 N7 C17 C16 -178.4(8) . . . . ? Cd3 N7 C17 C16 -4.0(11) . . . . ? N7 C17 C18 C19 -2.3(9) . . . . ? C16 C17 C18 C19 178.8(9) . . . . ? N7 C17 C18 C13 178.7(7) . . . . ? C16 C17 C18 C13 -0.1(14) . . . . ? C14 C13 C18 C19 67.2(11) . . . . ? C12 C13 C18 C19 -113.0(10) . . . . ? C14 C13 C18 C17 -114.0(9) . . . . ? C12 C13 C18 C17 65.8(12) . . . . ? N7 N8 C19 C18 0.7(9) . . . . ? N7 N8 C19 C20 178.2(8) . . . . ? C17 C18 C19 N8 1.0(9) . . . . ? C13 C18 C19 N8 180.0(7) . . . . ? C17 C18 C19 C20 -176.1(10) . . . . ? C13 C18 C19 C20 2.9(15) . . . . ? N10 N9 C22 C23 1.0(8) . . . . ? Cd2 N9 C22 C23 -172.3(5) . . . . ? N10 N9 C22 C21 178.7(7) . . . . ? Cd2 N9 C22 C21 5.4(11) . . . . ? N9 C22 C23 C24 -1.1(9) . . . . ? C21 C22 C23 C24 -178.6(8) . . . . ? N9 C22 C23 C28 -176.1(7) . . . . ? C21 C22 C23 C28 6.4(13) . . . . ? N9 N10 C24 C23 -0.1(9) . . . . ? N9 N10 C24 C25 179.4(7) . . . . ? C22 C23 C24 N10 0.7(8) . . . . ? C28 C23 C24 N10 175.6(7) . . . . ? C22 C23 C24 C25 -178.7(9) . . . . ? C28 C23 C24 C25 -3.8(14) . . . . ? N12 N11 C27 C28 1.5(9) . . . . ? Cd1 N11 C27 C28 149.4(6) 7_566 . . . ? N12 N11 C27 C26 176.2(8) . . . . ? Cd1 N11 C27 C26 -36.0(13) 7_566 . . . ? N11 C27 C28 C29 -1.9(9) . . . . ? C26 C27 C28 C29 -176.3(9) . . . . ? N11 C27 C28 C23 176.2(7) . . . . ? C26 C27 C28 C23 1.8(14) . . . . ? C24 C23 C28 C27 66.3(12) . . . . ? C22 C23 C28 C27 -119.8(9) . . . . ? C24 C23 C28 C29 -116.0(9) . . . . ? C22 C23 C28 C29 57.9(11) . . . . ? N11 N12 C29 C28 -0.5(8) . . . . ? N11 N12 C29 C30 178.1(7) . . . . ? C27 C28 C29 N12 1.4(8) . . . . ? C23 C28 C29 N12 -176.8(7) . . . . ? C27 C28 C29 C30 -177.1(8) . . . . ? C23 C28 C29 C30 4.7(13) . . . . ? N14 N13 C32 C33 -1.4(8) . . . . ? Cd2 N13 C32 C33 -169.0(5) . . . . ? N14 N13 C32 C31 177.6(7) . . . . ? Cd2 N13 C32 C31 10.0(11) . . . . ? N13 C32 C33 C34 1.1(9) . . . . ? C31 C32 C33 C34 -177.9(8) . . . . ? N13 C32 C33 C38 179.8(7) . . . . ? C31 C32 C33 C38 0.8(13) . . . . ? N13 N14 C34 C33 -0.6(9) . . . . ? N13 N14 C34 C35 179.6(8) . . . . ? C32 C33 C34 N14 -0.3(9) . . . . ? C38 C33 C34 N14 -179.0(7) . . . . ? C32 C33 C34 C35 179.5(9) . . . . ? C38 C33 C34 C35 0.8(14) . . . . ? N16 N15 C37 C38 0.6(8) . . . . ? Cd3 N15 C37 C38 150.0(6) 3_664 . . . ? N16 N15 C37 C36 178.5(7) . . . . ? Cd3 N15 C37 C36 -32.0(11) 3_664 . . . ? N15 C37 C38 C39 -0.3(9) . . . . ? C36 C37 C38 C39 -178.0(8) . . . . ? N15 C37 C38 C33 -179.7(7) . . . . ? C36 C37 C38 C33 2.7(14) . . . . ? C34 C33 C38 C39 -118.3(9) . . . . ? C32 C33 C38 C39 63.3(12) . . . . ? C34 C33 C38 C37 61.0(12) . . . . ? C32 C33 C38 C37 -117.5(9) . . . . ? N15 N16 C39 C38 0.5(9) . . . . ? N15 N16 C39 C40 177.5(7) . . . . ? C37 C38 C39 N16 -0.1(8) . . . . ? C33 C38 C39 N16 179.3(7) . . . . ? C37 C38 C39 C40 -176.7(9) . . . . ? C33 C38 C39 C40 2.7(14) . . . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 24.93 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 1.539 _refine_diff_density_min -0.672 _refine_diff_density_rms 0.143 _iucr_refine_instruction_details ; #--------------------------------------------------------- TITL xtal10 in P4(2)/m CELL 0.71073 19.5220 19.5220 33.7908 90.000 90.000 90.000 ZERR 8.00 0.0008 0.0008 0.0030 0.000 0.000 0.000 LATT 1 SYMM - X, - Y, Z SYMM - Y, X, 1/2 + Z SYMM Y, - X, 1/2 + Z SFAC C H N F S CL SI CD UNIT 352 480 144 48 16 32 8 16 MERG 2 OMIT 0.00 180.00 OMIT 3 3 0 OMIT 3 3 4 OMIT -3 4 0 OMIT 4 4 0 OMIT 1 5 1 OMIT -1 5 1 TWIN 0.00 1.00 0.00 1.00 0.00 0.00 0.00 0.00 -1.00 2 SHEL 0.8 5 EADP C44 C45 C46 EQIV $1 X, Y, -Z DFIX 1.750 0.008 C44 Cl1 C44 Cl2 DFIX 1.750 0.008 C45 Cl3 C45 Cl3_$1 DFIX 1.750 0.008 C46 Cl4 C46 Cl4_$1 DFIX 2.880 0.008 Cl1 Cl2 Cl3 Cl3_$1 Cl4 Cl4_$1 FMAP 2 PLAN 12 SIZE 0.20 0.21 0.24 ACTA BOND CONF LIST 1 L.S. 5 TEMP -60.00 WGHT 0.118800 BASF 0.49975 FVAR 0.19681 CD1 8 0.328641 0.622265 0.000000 10.50000 0.04334 0.04607 = 0.02356 0.00000 0.00000 0.00343 CD2 8 0.355784 0.842100 0.250853 11.00000 0.04588 0.04407 = 0.02231 -0.00201 0.00002 -0.00745 CD3 8 0.108719 0.820153 0.500000 10.50000 0.04548 0.04135 = 0.02393 0.00000 0.00000 0.00610 SI1 7 0.500000 0.500000 0.000000 10.25000 0.02686 0.03290 = 0.01497 0.00000 0.00000 0.00239 SI2 7 0.500000 1.000000 0.252342 10.50000 0.02946 0.02703 = 0.01913 0.00000 0.00000 -0.00224 SI3 7 0.000000 1.000000 0.500000 10.25000 0.02973 0.02366 = 0.01592 0.00000 0.00000 0.00380 S1 5 0.089609 0.698785 0.000000 10.50000 0.06841 0.14649 = 0.11438 0.00000 0.00000 0.03405 S2 5 0.261788 0.619373 0.276965 11.00000 0.11723 0.07864 = 0.13965 0.00528 -0.00330 -0.02285 S3 5 0.188912 0.580678 0.500000 10.50000 0.16100 0.06633 = 0.12634 0.00000 0.00000 0.04697 F1 4 0.424775 0.544029 0.000000 10.50000 0.03145 0.03990 = 0.02555 0.00000 0.00000 0.01069 F2 4 0.500000 0.500000 0.049563 10.50000 0.02943 0.05421 = 0.01735 0.00000 0.00000 0.00885 F3 4 0.458064 0.424671 0.000000 10.50000 0.03374 0.04109 = 0.02821 0.00000 0.00000 -0.00960 F4 4 0.440569 0.937305 0.252222 11.00000 0.03561 0.03574 = 0.02636 0.00529 -0.00250 -0.00383 F5 4 0.500000 1.000000 0.301383 10.50000 0.03587 0.05637 = 0.02132 0.00000 0.00000 -0.00152 F6 4 0.437475 1.058930 0.252081 11.00000 0.04143 0.03755 = 0.03916 -0.00717 -0.00902 0.01014 F7 4 0.500000 1.000000 0.202002 10.50000 0.05810 0.03281 = 0.02413 0.00000 0.00000 -0.01116 F8 4 0.036178 0.921595 0.500000 10.50000 0.04402 0.02694 = 0.02255 0.00000 0.00000 0.00655 F9 4 0.078298 1.035643 0.500000 10.50000 0.03937 0.04206 = 0.04239 0.00000 0.00000 0.00028 F10 4 0.000000 1.000000 0.549996 10.50000 0.05199 0.03538 = 0.01985 0.00000 0.00000 0.00248 N1 3 0.401058 0.674786 0.047889 11.00000 0.06542 0.04277 = 0.03186 -0.01237 0.00320 0.00126 N2 3 0.469372 0.668233 0.050889 11.00000 0.05773 0.04747 = 0.03658 -0.01627 0.00713 0.00633 AFIX 43 H2 2 0.493979 0.644616 0.034317 11.00000 -1.50000 AFIX 0 N3 3 0.425235 0.814927 0.198408 11.00000 0.08649 0.03474 = 0.03176 -0.00472 0.01319 0.00099 N4 3 0.450720 0.866474 0.174628 11.00000 0.06376 0.03267 = 0.02749 -0.00865 0.00658 -0.00929 AFIX 43 H4 2 0.459251 0.907795 0.182917 11.00000 -1.50000 AFIX 0 N5 3 0.317264 0.906094 0.304675 11.00000 0.03431 0.06473 = 0.02614 -0.00166 0.00367 -0.00122 N6 3 0.363965 0.939902 0.326487 11.00000 0.03923 0.05558 = 0.03086 -0.00738 0.00754 -0.00409 AFIX 43 H6 2 0.404023 0.952072 0.317663 11.00000 -1.50000 AFIX 0 N7 3 0.168519 0.887058 0.452659 11.00000 0.04204 0.05488 = 0.03543 -0.00500 0.01184 0.00014 N8 3 0.163299 0.955785 0.448651 11.00000 0.04276 0.06144 = 0.04164 -0.00038 0.01903 -0.00245 AFIX 43 H8 2 0.138683 0.981389 0.464202 11.00000 -1.50000 AFIX 0 N9 3 0.439456 0.803170 0.295259 11.00000 0.04660 0.04847 = 0.02945 0.01302 0.00728 0.00622 N10 3 0.505300 0.822868 0.292753 11.00000 0.05485 0.04483 = 0.03008 0.01838 0.00013 -0.00441 AFIX 43 H10 2 0.521292 0.847588 0.273425 11.00000 -1.50000 AFIX 0 N11 3 0.548853 0.696063 0.445352 11.00000 0.06856 0.03555 = 0.02987 0.00376 -0.00398 -0.00285 N12 3 0.529982 0.639840 0.424549 11.00000 0.06019 0.03772 = 0.03316 0.00614 -0.01407 -0.00433 AFIX 43 H12 2 0.529761 0.598724 0.434480 11.00000 -1.50000 AFIX 0 N13 3 0.307233 0.925694 0.205931 11.00000 0.04594 0.05304 = 0.02954 -0.00045 -0.00944 -0.00078 N14 3 0.330943 0.990989 0.206157 11.00000 0.05426 0.05719 = 0.03698 -0.00302 -0.02219 0.00490 AFIX 43 H14 2 0.359079 1.006783 0.223917 11.00000 -1.50000 AFIX 0 N15 3 0.199504 1.034723 0.055460 11.00000 0.03765 0.06163 = 0.02685 0.00429 -0.00717 -0.00114 N16 3 0.142118 1.019998 0.077077 11.00000 0.02605 0.07609 = 0.03037 0.00262 -0.00660 -0.00194 AFIX 43 H16 2 0.100804 1.023256 0.067609 11.00000 -1.50000 AFIX 0 N17 3 0.233558 0.680659 0.000000 10.50000 0.03751 0.07825 = 0.04747 0.00000 0.00000 0.02422 N18 3 0.282848 0.754025 0.253043 11.00000 0.10013 0.07369 = 0.06815 -0.01375 0.00336 -0.04625 N19 3 0.159720 0.720328 0.500000 10.50000 0.06251 0.05469 = 0.04834 0.00000 0.00000 0.01200 C1 1 0.310725 0.733468 0.084971 11.00000 0.07765 0.10240 = 0.08694 -0.04294 0.00639 0.01472 AFIX 137 H1A 2 0.285834 0.733508 0.060127 11.00000 -1.50000 H1B 2 0.308595 0.778719 0.096764 11.00000 -1.50000 H1C 2 0.290305 0.700370 0.102838 11.00000 -1.50000 AFIX 0 C2 1 0.382083 0.715128 0.077728 11.00000 0.06791 0.04558 = 0.04379 -0.01500 0.01356 -0.00331 C3 1 0.440454 0.733069 0.100422 11.00000 0.06478 0.03689 = 0.03363 -0.00476 0.00645 -0.00387 C4 1 0.495878 0.701786 0.082027 11.00000 0.07301 0.04032 = 0.03315 -0.01464 0.00912 0.00194 C5 1 0.568054 0.702920 0.092943 11.00000 0.08769 0.07561 = 0.08122 -0.03286 -0.01288 0.00719 AFIX 137 H5A 2 0.592021 0.666587 0.079098 11.00000 -1.50000 H5B 2 0.572450 0.696134 0.121266 11.00000 -1.50000 H5C 2 0.587754 0.746796 0.085734 11.00000 -1.50000 AFIX 0 C6 1 0.397836 0.693884 0.188058 11.00000 0.20261 0.04509 = 0.05608 -0.01035 0.06420 -0.02173 AFIX 137 H6A 2 0.391803 0.696249 0.216519 11.00000 -1.50000 H6B 2 0.432668 0.660142 0.181807 11.00000 -1.50000 H6C 2 0.354911 0.680803 0.175732 11.00000 -1.50000 AFIX 0 C7 1 0.419219 0.761181 0.173096 11.00000 0.09544 0.03194 = 0.04683 -0.00833 0.01775 -0.00667 C8 1 0.441319 0.779085 0.135440 11.00000 0.06801 0.03844 = 0.02728 -0.00524 -0.00072 -0.00208 C9 1 0.460893 0.845371 0.136994 11.00000 0.05766 0.04194 = 0.01783 -0.00283 -0.00042 -0.00136 C10 1 0.489766 0.892722 0.106071 11.00000 0.10080 0.05661 = 0.03559 -0.00008 0.01905 -0.02166 AFIX 137 H10A 2 0.453007 0.919552 0.094549 11.00000 -1.50000 H10B 2 0.511929 0.865993 0.085538 11.00000 -1.50000 H10C 2 0.522977 0.923148 0.118193 11.00000 -1.50000 AFIX 0 C11 1 0.200652 0.860852 0.313387 11.00000 0.04319 0.09513 = 0.07565 -0.01798 0.00306 -0.02388 AFIX 137 H11A 2 0.195802 0.867723 0.285095 11.00000 -1.50000 H11B 2 0.160775 0.879148 0.326861 11.00000 -1.50000 H11C 2 0.204605 0.812260 0.318931 11.00000 -1.50000 AFIX 0 C12 1 0.264119 0.897312 0.327824 11.00000 0.04058 0.06724 = 0.02887 -0.00800 0.00356 -0.00491 C13 1 0.276511 0.924805 0.365939 11.00000 0.03928 0.05723 = 0.03016 -0.00275 0.01006 -0.00231 C14 1 0.341954 0.952759 0.363309 11.00000 0.03931 0.06407 = 0.03834 -0.01294 0.00760 -0.00474 C15 1 0.386238 0.986596 0.394297 11.00000 0.06546 0.13452 = 0.05818 -0.04509 0.00680 -0.02256 AFIX 137 H15A 2 0.431300 0.965661 0.394232 11.00000 -1.50000 H15B 2 0.365401 0.980814 0.420142 11.00000 -1.50000 H15C 2 0.390460 1.035048 0.388423 11.00000 -1.50000 AFIX 0 C16 1 0.224954 0.793303 0.416240 11.00000 0.09740 0.08162 = 0.04832 0.00039 0.03951 0.01784 AFIX 137 H16A 2 0.194082 0.774283 0.396614 11.00000 -1.50000 H16B 2 0.219387 0.768923 0.441045 11.00000 -1.50000 H16C 2 0.271843 0.788605 0.407137 11.00000 -1.50000 AFIX 0 C17 1 0.208986 0.866806 0.422235 11.00000 0.03728 0.07578 = 0.03202 -0.01187 0.00969 0.00928 C18 1 0.230602 0.924015 0.400912 11.00000 0.04272 0.07266 = 0.02771 -0.00804 0.01289 -0.00003 C19 1 0.200817 0.981022 0.417532 11.00000 0.04486 0.05884 = 0.04090 -0.00182 0.01100 -0.00276 C20 1 0.200568 1.054824 0.407295 11.00000 0.09611 0.07115 = 0.05203 0.00261 0.03002 -0.01145 AFIX 137 H20A 2 0.242356 1.075979 0.416878 11.00000 -1.50000 H20B 2 0.161349 1.076804 0.419518 11.00000 -1.50000 H20C 2 0.197837 1.060002 0.378789 11.00000 -1.50000 AFIX 0 C21 1 0.371261 0.735147 0.343211 11.00000 0.06050 0.07018 = 0.05485 0.02522 0.00819 0.00155 AFIX 137 H21A 2 0.334144 0.749886 0.326132 11.00000 -1.50000 H21B 2 0.362320 0.750119 0.370091 11.00000 -1.50000 H21C 2 0.374623 0.685586 0.342580 11.00000 -1.50000 AFIX 0 C22 1 0.436898 0.765666 0.329114 11.00000 0.06840 0.03468 = 0.03034 0.01112 0.00833 0.00322 C23 1 0.500589 0.763488 0.347518 11.00000 0.06497 0.03144 = 0.02900 0.00861 -0.00394 -0.00200 C24 1 0.544240 0.800487 0.323227 11.00000 0.06334 0.04633 = 0.03754 0.01694 -0.01107 0.00118 C25 1 0.618822 0.816503 0.325528 11.00000 0.05817 0.08831 = 0.05359 0.02746 -0.00713 -0.01197 AFIX 137 H25A 2 0.644480 0.782318 0.310891 11.00000 -1.50000 H25B 2 0.633307 0.816224 0.352987 11.00000 -1.50000 H25C 2 0.627194 0.861387 0.314203 11.00000 -1.50000 AFIX 0 C26 1 0.554688 0.820895 0.431503 11.00000 0.11829 0.03601 = 0.06789 0.00363 -0.02682 -0.00541 AFIX 137 H26A 2 0.548349 0.825750 0.459836 11.00000 -1.50000 H26B 2 0.522377 0.850151 0.417723 11.00000 -1.50000 H26C 2 0.601038 0.834094 0.424515 11.00000 -1.50000 AFIX 0 C27 1 0.542704 0.747270 0.419732 11.00000 0.06630 0.03926 = 0.03619 0.00140 -0.00570 -0.00176 C28 1 0.518486 0.724750 0.383191 11.00000 0.05947 0.03555 = 0.03113 0.01068 0.00284 -0.00158 C29 1 0.511787 0.653647 0.387381 11.00000 0.05717 0.03608 = 0.02998 0.00649 0.00085 0.00239 C30 1 0.491135 0.598891 0.358777 11.00000 0.09510 0.04432 = 0.04018 0.00577 -0.01758 -0.00374 AFIX 137 H30A 2 0.493707 0.554566 0.371664 11.00000 -1.50000 H30B 2 0.521748 0.599542 0.336170 11.00000 -1.50000 H30C 2 0.444564 0.607073 0.349958 11.00000 -1.50000 AFIX 0 C31 1 0.233501 0.854841 0.163005 11.00000 0.07118 0.05988 = 0.05148 0.00139 -0.02805 -0.00976 AFIX 137 H31A 2 0.268333 0.820968 0.156995 11.00000 -1.50000 H31B 2 0.204719 0.861794 0.139953 11.00000 -1.50000 H31C 2 0.205659 0.838858 0.184915 11.00000 -1.50000 AFIX 0 C32 1 0.267211 0.921202 0.174070 11.00000 0.03339 0.06487 = 0.03314 -0.00588 -0.00530 0.00559 C33 1 0.264264 0.984616 0.154496 11.00000 0.03421 0.06207 = 0.03084 0.00238 -0.00949 -0.00186 C34 1 0.306859 1.028049 0.176616 11.00000 0.04133 0.06011 = 0.04787 0.00698 -0.01548 0.00241 C35 1 0.324563 1.101271 0.170312 11.00000 0.07761 0.07012 = 0.07454 0.01200 -0.03707 -0.01650 AFIX 137 H35A 2 0.304051 1.128800 0.191064 11.00000 -1.50000 H35B 2 0.307255 1.116093 0.144803 11.00000 -1.50000 H35C 2 0.373938 1.106716 0.170954 11.00000 -1.50000 AFIX 0 C36 1 0.324316 1.033148 0.067734 11.00000 0.04009 0.11721 = 0.05149 0.02324 0.00414 0.00850 AFIX 137 H36A 2 0.341480 0.990286 0.057127 11.00000 -1.50000 H36B 2 0.352277 1.046980 0.090077 11.00000 -1.50000 H36C 2 0.326219 1.068181 0.047407 11.00000 -1.50000 AFIX 0 C37 1 0.250904 1.023779 0.081144 11.00000 0.03571 0.06163 = 0.03100 -0.00128 -0.00526 0.00401 C38 1 0.226007 1.001983 0.117951 11.00000 0.03286 0.06823 = 0.03505 0.00225 -0.00782 0.00446 C39 1 0.155525 1.000165 0.114055 11.00000 0.03431 0.05776 = 0.03512 0.00591 -0.00770 0.00094 C40 1 0.100537 0.984547 0.142854 11.00000 0.04254 0.09980 = 0.05381 0.02610 -0.00545 -0.00586 AFIX 137 H40A 2 0.063139 1.016710 0.139401 11.00000 -1.50000 H40B 2 0.118466 0.988389 0.169534 11.00000 -1.50000 H40C 2 0.083983 0.938310 0.138494 11.00000 -1.50000 AFIX 0 C41 1 0.173312 0.685591 0.000000 10.50000 0.12677 0.06417 = 0.03953 0.00000 0.00000 -0.00357 C42 1 0.276205 0.696654 0.263200 11.00000 0.07123 0.08553 = 0.06226 -0.01232 -0.00783 -0.01852 C43 1 0.174539 0.664708 0.500000 10.50000 0.09717 0.06995 = 0.03874 0.00000 0.00000 0.04910 C44 1 0.196753 1.023023 0.263452 11.00000 0.19783 AFIX 23 H44A 2 0.210481 0.986502 0.281700 11.00000 -1.20000 H44B 2 0.208348 1.008268 0.236553 11.00000 -1.20000 AFIX 0 CL1 6 0.242316 1.096920 0.274625 11.00000 0.21923 CL2 6 0.108639 1.034979 0.266766 11.00000 0.25036 C45 1 0.304940 0.348984 0.000000 10.50000 0.19783 AFIX 23 H45A 2 0.352779 0.364197 0.000000 10.50000 -1.20000 H45B 2 0.304371 0.298788 0.000000 10.50000 -1.20000 AFIX 0 CL3 6 0.263027 0.380003 0.042278 11.00000 0.41281 C46 1 0.193415 0.909019 0.000000 10.50000 0.19783 AFIX 23 H46A 2 0.146706 0.927413 0.000000 10.50000 -1.20000 H46B 2 0.225260 0.947825 0.000000 10.50000 -1.20000 AFIX 0 CL4 6 0.205894 0.860994 0.042669 11.00000 0.25691 HKLF 4 REM xtal10 in P4(2)/m REM R1 = 0.0559 for 9336 Fo > 4sig(Fo) and 0.0650 for all 11058 data REM 705 parameters refined using 9 restraints END WGHT 0.1187 0.0000 REM Highest difference peak 1.539, deepest hole -0.672, 1-sigma level 0.143 Q1 1 0.3347 0.8565 0.2467 11.00000 0.05 1.54 Q2 1 0.2796 0.5506 0.0000 10.50000 0.05 1.41 Q3 1 0.0570 0.7824 0.5000 10.50000 0.05 1.39 Q4 1 0.5000 1.0000 0.0000 10.25000 0.05 1.30 Q5 1 0.2453 1.0656 0.2935 11.00000 0.05 1.22 Q6 1 0.3938 0.8467 0.0000 10.50000 0.05 0.95 Q7 1 0.3201 0.3290 0.0000 10.50000 0.05 0.94 Q8 1 0.5090 0.9850 0.5000 10.50000 0.05 0.86 Q9 1 0.3200 0.8657 0.0000 10.50000 0.05 0.85 Q10 1 0.1092 1.0576 0.2597 11.00000 0.05 0.85 ; _database_code_depnum_ccdc_archive 'CCDC 947382' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_(4) _audit_creation_method SHELXL-97 _chemical_name_systematic ; mu-Hexafluorosilicato-bis(3,3',5,5'-Tetramethyl-4,4'-bipyrazole) cadmium(II), Hexahydrate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C20 H28 Cd F6 N8 Si), 6(H2 O)' _chemical_formula_sum 'C20 H40 Cd F6 N8 O6 Si' _chemical_formula_weight 743.09 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.6869(10) _cell_length_b 15.5383(9) _cell_length_c 15.8770(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.047(8) _cell_angle_gamma 90.00 _cell_volume 3376.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 4.17 _cell_measurement_theta_max 26.73 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 0.759 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8448 _exptl_absorpt_correction_T_max 0.8882 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'Stoe Imaging plate diffraction system' _diffrn_measurement_method '\f oscillation scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 12133 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.0376 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 4.17 _diffrn_reflns_theta_max 26.73 _reflns_number_total 3490 _reflns_number_gt 3109 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS Software (Stoe & Cie, 2000)' _computing_cell_refinement 'IPDS Software (Stoe & Cie, 2000)' _computing_data_reduction 'IPDS Software (Stoe & Cie, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.70.01 (Farrugia, 1999)' #------------------------------- Refinement data-----------------------# _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 crystals were twinned. They emulate orthorhombic-C lattice by pseudomerohedry (a common case of monoclinic cell with beta appr. 90), giving R(int) = 0.049. Solution in the orthorhombic-C space groups (for example, Cmcm) was possible leading to the poorly refinable models (R1 over 0.15), which involve disorder of either SiF62- or Me4bpz moieties, and systematically Fo2 >> Fc2. Therefore, the data frames were integrated for the monoclinic cell (beta = 90.047(8)) and the structure successfully solved and refined as twin in monoclinic space group C2/c. The twin law was {-1 0 0 0 -1 0 0 0 1} and the refined parameter BASF = 0.49734 was indicative for the equal contributions from the twin domains. Atoms of the framework were freely refined anisotropically and CH (methyl) and NH hydrogen atoms were added geometrically, with U(iso) = 1.5U(eq) of the parent C (N) atoms. The solvate water molecules are disordred over two positions (separated at 1.0-1.5 A). In this way, two independed molecules are equally disordered by symmetry (O3 and O4) and were refined with partial contribution factors of 0.5. Two other molecules were unequally disordered and in both cases the partial occupancies of 0.65 and 0.35 were suggested by the refinement of thermal parameters (U(iso) = 0.14-0.17 A^2^). All disordered water molecules were refined isotropically and the OH hydrogen atoms were not added. ; _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^)+(0.0576P)^2^+0.0000P] 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_number_reflns 3490 _refine_ls_number_parameters 194 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0339 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0795 _refine_ls_wR_factor_gt 0.0788 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.002 _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 Cd1 Cd 0.0000 -0.016052(16) 0.7500 0.01762(10) Uani 1 2 d S . . Si1 Si 0.0000 0.0000 1.0000 0.0218(2) Uani 1 2 d S . . F1 F -0.02551(14) -0.01322(13) 0.89567(15) 0.0296(5) Uani 1 1 d . . . F2 F -0.0113(2) 0.10664(12) 0.98842(13) 0.0328(5) Uani 1 1 d . . . F3 F 0.11920(16) 0.00636(15) 0.97583(14) 0.0333(6) Uani 1 1 d . . . N1 N 0.1087(2) 0.09683(19) 0.7760(2) 0.0303(8) Uani 1 1 d . . . N2 N 0.0852(2) 0.15123(19) 0.8393(2) 0.0324(7) Uani 1 1 d . . . H2 H 0.0437 0.1391 0.8790 0.049 Uiso 1 1 calc R . . N3 N 0.3805(2) 0.3843(2) 0.72454(19) 0.0296(8) Uani 1 1 d . . . N4 N 0.3265(2) 0.3875(2) 0.6532(2) 0.0358(8) Uani 1 1 d . . . H4 H 0.3377 0.4226 0.6116 0.054 Uiso 1 1 calc R . . C1 C 0.2167(3) 0.0987(3) 0.6517(3) 0.0540(13) Uani 1 1 d . . . H1A H 0.2218 0.0370 0.6596 0.081 Uiso 1 1 calc R . . H1B H 0.2813 0.1227 0.6425 0.081 Uiso 1 1 calc R . . H1C H 0.1757 0.1107 0.6033 0.081 Uiso 1 1 calc R . . C2 C 0.1726(2) 0.1385(2) 0.7286(2) 0.0318(11) Uani 1 1 d . . . C3 C 0.1904(2) 0.2217(2) 0.7621(3) 0.0301(10) Uani 1 1 d . . . C4 C 0.1336(3) 0.2265(2) 0.8335(3) 0.0339(9) Uani 1 1 d . . . C5 C 0.1227(5) 0.2945(4) 0.8991(4) 0.0656(16) Uani 1 1 d . . . H5A H 0.0540 0.3032 0.9111 0.098 Uiso 1 1 calc R . . H5B H 0.1511 0.3478 0.8789 0.098 Uiso 1 1 calc R . . H5C H 0.1561 0.2766 0.9501 0.098 Uiso 1 1 calc R . . C6 C 0.3803(4) 0.3003(4) 0.8561(3) 0.0621(16) Uani 1 1 d . . . H6A H 0.4511 0.3029 0.8539 0.093 Uiso 1 1 calc R . . H6B H 0.3601 0.2424 0.8709 0.093 Uiso 1 1 calc R . . H6C H 0.3566 0.3404 0.8982 0.093 Uiso 1 1 calc R . . C7 C 0.3395(3) 0.3235(2) 0.7725(2) 0.0312(10) Uani 1 1 d . . . C8 C 0.2575(3) 0.2888(2) 0.7302(2) 0.0315(10) Uani 1 1 d . . . C9 C 0.2533(3) 0.3300(3) 0.6544(3) 0.0360(8) Uani 1 1 d . . . C10 C 0.1808(4) 0.3245(4) 0.5839(3) 0.0598(15) Uani 1 1 d . . . H10A H 0.2072 0.2890 0.5391 0.090 Uiso 1 1 calc R . . H10B H 0.1676 0.3817 0.5624 0.090 Uiso 1 1 calc R . . H10C H 0.1206 0.2991 0.6045 0.090 Uiso 1 1 calc R . . O1A O -0.0301(10) 0.5253(8) 0.5974(10) 0.152(5) Uiso 0.65 1 d P . . O1B O 0.0370(17) 0.5160(14) 0.528(2) 0.144(9) Uiso 0.35 1 d P . . O2A O 0.1596(9) 0.5563(9) 0.6139(8) 0.146(4) Uiso 0.65 1 d P . . O2B O 0.1694(18) 0.5324(14) 0.5176(17) 0.141(8) Uiso 0.35 1 d P . . O3 O -0.0517(10) 0.4647(10) 0.7624(18) 0.165(6) Uiso 0.50 1 d P . . O4 O 0.4835(15) 0.1418(10) 0.7207(10) 0.175(7) Uiso 0.50 1 d P . . 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 Cd1 0.01690(13) 0.01462(13) 0.02135(18) 0.000 0.0039(5) 0.000 Si1 0.0279(5) 0.0200(5) 0.0174(6) -0.0012(3) 0.0081(13) -0.0015(12) F1 0.0382(15) 0.0319(10) 0.0187(12) -0.0026(7) 0.0031(9) -0.0009(7) F2 0.0484(14) 0.0210(8) 0.0290(11) 0.0001(7) 0.0097(11) 0.0021(12) F3 0.0298(10) 0.0384(13) 0.0318(18) -0.0060(13) 0.0096(9) -0.0027(9) N1 0.0297(13) 0.0242(15) 0.037(2) -0.0018(11) 0.0022(12) -0.0094(11) N2 0.0368(16) 0.0244(15) 0.036(2) 0.0017(13) 0.0131(13) -0.0111(13) N3 0.0300(14) 0.0281(15) 0.031(2) 0.0048(11) -0.0015(12) -0.0119(12) N4 0.0322(15) 0.0438(19) 0.0313(19) 0.0157(14) -0.0022(13) -0.0161(13) C1 0.048(2) 0.061(3) 0.053(3) -0.023(2) 0.020(2) -0.028(2) C2 0.0241(14) 0.0307(17) 0.041(3) 0.0003(14) 0.0003(14) -0.0108(13) C3 0.0338(14) 0.0261(15) 0.030(3) 0.0031(16) -0.0020(17) -0.0115(12) C4 0.0408(19) 0.0228(18) 0.038(2) 0.0010(15) 0.0060(17) -0.0141(15) C5 0.087(4) 0.043(3) 0.067(4) -0.020(2) 0.036(3) -0.027(3) C6 0.075(3) 0.061(3) 0.051(3) 0.027(2) -0.022(2) -0.044(3) C7 0.0402(17) 0.0279(17) 0.025(3) 0.0022(12) -0.0032(13) -0.0141(14) C8 0.0352(16) 0.0256(16) 0.034(3) 0.0013(13) 0.0009(14) -0.0118(13) C9 0.0331(17) 0.040(2) 0.035(2) 0.0058(17) -0.0016(16) -0.0149(15) C10 0.051(3) 0.076(4) 0.052(4) 0.021(3) -0.021(2) -0.030(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 Cd1 N3 2.288(3) 3_445 ? Cd1 N3 2.288(3) 4_546 ? Cd1 N1 2.336(3) . ? Cd1 N1 2.336(3) 2_556 ? Cd1 F1 2.340(2) . ? Cd1 F1 2.340(2) 2_556 ? Si1 F2 1.6745(19) . ? Si1 F2 1.6745(19) 5_557 ? Si1 F3 1.679(2) . ? Si1 F1 1.705(2) . ? N1 C2 1.323(4) . ? N1 N2 1.352(4) . ? N2 C4 1.347(4) . ? N3 C7 1.338(5) . ? N3 N4 1.353(4) . ? N4 C9 1.343(5) . ? C1 C2 1.496(6) . ? C2 C3 1.418(5) . ? C3 C4 1.378(6) . ? C3 C8 1.480(5) . ? C4 C5 1.490(6) . ? C6 C7 1.484(6) . ? C7 C8 1.414(5) . ? C8 C9 1.364(6) . ? C9 C10 1.498(6) . ? O1A O1B 1.44(3) . ? O1B O1B 1.44(5) 5_566 ? O2A O2B 1.58(3) . ? O3 O3 1.47(3) 2_556 ? O4 O4 1.04(3) 2_656 ? 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 N3 Cd1 N3 94.82(16) 3_445 4_546 ? N3 Cd1 N1 173.83(10) 3_445 . ? N3 Cd1 N1 91.26(12) 4_546 . ? N3 Cd1 N1 91.26(12) 3_445 2_556 ? N3 Cd1 N1 173.83(11) 4_546 2_556 ? N1 Cd1 N1 82.69(15) . 2_556 ? N3 Cd1 F1 94.59(9) 3_445 . ? N3 Cd1 F1 86.87(9) 4_546 . ? N1 Cd1 F1 84.65(9) . . ? N1 Cd1 F1 93.72(9) 2_556 . ? N3 Cd1 F1 86.87(9) 3_445 2_556 ? N3 Cd1 F1 94.59(9) 4_546 2_556 ? N1 Cd1 F1 93.72(9) . 2_556 ? N1 Cd1 F1 84.65(9) 2_556 2_556 ? F1 Cd1 F1 177.84(10) . 2_556 ? F2 Si1 F2 180.0 . 5_557 ? F2 Si1 F3 89.62(12) . 5_557 ? F2 Si1 F3 90.38(12) 5_557 5_557 ? F2 Si1 F3 90.38(12) . . ? F2 Si1 F3 89.62(12) 5_557 . ? F3 Si1 F3 180.00(3) 5_557 . ? F2 Si1 F1 89.63(10) . . ? F2 Si1 F1 90.37(10) 5_557 . ? F3 Si1 F1 90.96(10) 5_557 . ? F3 Si1 F1 89.04(10) . . ? F2 Si1 F1 90.37(10) . 5_557 ? F2 Si1 F1 89.63(10) 5_557 5_557 ? F3 Si1 F1 89.04(10) 5_557 5_557 ? F3 Si1 F1 90.96(10) . 5_557 ? F1 Si1 F1 180.000(1) . 5_557 ? Si1 F1 Cd1 158.75(11) . . ? C2 N1 N2 105.9(3) . . ? C2 N1 Cd1 133.5(3) . . ? N2 N1 Cd1 116.7(2) . . ? C4 N2 N1 112.1(3) . . ? C7 N3 N4 105.9(3) . . ? C7 N3 Cd1 132.7(2) . 3 ? N4 N3 Cd1 120.8(2) . 3 ? C9 N4 N3 111.7(3) . . ? N1 C2 C3 110.2(3) . . ? N1 C2 C1 121.9(3) . . ? C3 C2 C1 127.8(4) . . ? C4 C3 C2 105.2(3) . . ? C4 C3 C8 126.5(4) . . ? C2 C3 C8 128.3(4) . . ? N2 C4 C3 106.6(3) . . ? N2 C4 C5 121.3(4) . . ? C3 C4 C5 132.1(3) . . ? N3 C7 C8 109.4(3) . . ? N3 C7 C6 121.5(3) . . ? C8 C7 C6 129.1(3) . . ? C9 C8 C7 105.9(3) . . ? C9 C8 C3 127.4(3) . . ? C7 C8 C3 126.8(4) . . ? N4 C9 C8 107.1(3) . . ? N4 C9 C10 121.4(4) . . ? C8 C9 C10 131.3(3) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.699 _refine_diff_density_min -0.593 _refine_diff_density_rms 0.092 _iucr_refine_instruction_details ; #--------------------------------------------------------- TITL ip71 in C2/c CELL 0.71073 13.6869 15.5383 15.8770 90.000 90.047 90.000 ZERR 4.00 0.0010 0.0009 0.0012 0.000 0.008 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N O F SI CD UNIT 80 160 32 24 24 4 4 MERG 2 OMIT 0.00 180.00 OMIT 0 4 1 OMIT 1 3 0 OMIT -1 5 1 OMIT 1 5 1 TWIN -1.00 0.00 0.00 0.00 -1.00 0.00 0.00 0.00 1.00 2 SHEL 0.79 5 EQIV $1 0.5-X, 0.5+Y, 1.5-Z RTAB O..O N2 F2 RTAB O..O N4 F3_$1 RTAB H..O H2 F2 RTAB H..O H4 F3_$1 RTAB XHY N2 H2 F2 RTAB XHY N4 H4 F3_$1 FMAP 2 PLAN 10 SIZE 0.16 0.20 0.23 ACTA LIST 4 L.S. 8 TEMP -60.00 WGHT 0.057600 BASF 0.49734 FVAR 0.31606 CD1 7 0.000000 -0.016052 0.750000 10.50000 0.01690 0.01462 = 0.02135 0.00000 0.00391 0.00000 SI1 6 0.000000 0.000000 1.000000 10.50000 0.02786 0.02005 = 0.01736 -0.00122 0.00806 -0.00151 F1 5 -0.025511 -0.013220 0.895669 11.00000 0.03825 0.03193 = 0.01870 -0.00264 0.00311 -0.00093 F2 5 -0.011350 0.106644 0.988417 11.00000 0.04836 0.02099 = 0.02898 0.00009 0.00968 0.00210 F3 5 0.119195 0.006364 0.975826 11.00000 0.02981 0.03844 = 0.03178 -0.00596 0.00964 -0.00271 N1 3 0.108691 0.096834 0.775989 11.00000 0.02972 0.02416 = 0.03716 -0.00183 0.00224 -0.00941 N2 3 0.085208 0.151235 0.839269 11.00000 0.03682 0.02443 = 0.03601 0.00171 0.01309 -0.01109 AFIX 43 H2 2 0.043737 0.139052 0.879018 11.00000 -1.50000 AFIX 0 N3 3 0.380479 0.384280 0.724543 11.00000 0.03003 0.02810 = 0.03069 0.00483 -0.00148 -0.01187 N4 3 0.326465 0.387529 0.653185 11.00000 0.03216 0.04385 = 0.03130 0.01566 -0.00224 -0.01605 AFIX 43 H4 2 0.337749 0.422626 0.611621 11.00000 -1.50000 AFIX 0 C1 1 0.216705 0.098702 0.651725 11.00000 0.04812 0.06070 = 0.05315 -0.02281 0.01963 -0.02821 AFIX 137 H1A 2 0.221824 0.036959 0.659589 11.00000 -1.50000 H1B 2 0.281254 0.122658 0.642468 11.00000 -1.50000 H1C 2 0.175658 0.110666 0.603287 11.00000 -1.50000 AFIX 0 C2 1 0.172554 0.138537 0.728590 11.00000 0.02411 0.03068 = 0.04066 0.00027 0.00027 -0.01080 C3 1 0.190378 0.221655 0.762113 11.00000 0.03383 0.02608 = 0.03031 0.00312 -0.00197 -0.01149 C4 1 0.133561 0.226517 0.833548 11.00000 0.04078 0.02278 = 0.03820 0.00097 0.00601 -0.01414 C5 1 0.122730 0.294457 0.899128 11.00000 0.08664 0.04271 = 0.06744 -0.01966 0.03551 -0.02733 AFIX 137 H5A 2 0.053959 0.303216 0.911093 11.00000 -1.50000 H5B 2 0.151060 0.347789 0.878855 11.00000 -1.50000 H5C 2 0.156123 0.276587 0.950123 11.00000 -1.50000 AFIX 0 C6 1 0.380331 0.300302 0.856129 11.00000 0.07457 0.06067 = 0.05098 0.02724 -0.02210 -0.04390 AFIX 137 H6A 2 0.451092 0.302913 0.853943 11.00000 -1.50000 H6B 2 0.360052 0.242425 0.870900 11.00000 -1.50000 H6C 2 0.356552 0.340431 0.898183 11.00000 -1.50000 AFIX 0 C7 1 0.339473 0.323462 0.772527 11.00000 0.04021 0.02793 = 0.02539 0.00224 -0.00325 -0.01412 C8 1 0.257509 0.288789 0.730191 11.00000 0.03520 0.02561 = 0.03376 0.00130 0.00086 -0.01182 C9 1 0.253334 0.329962 0.654381 11.00000 0.03305 0.03999 = 0.03496 0.00581 -0.00158 -0.01489 C10 1 0.180803 0.324459 0.583895 11.00000 0.05147 0.07611 = 0.05168 0.02088 -0.02122 -0.02979 AFIX 137 H10A 2 0.207201 0.288981 0.539091 11.00000 -1.50000 H10B 2 0.167590 0.381741 0.562435 11.00000 -1.50000 H10C 2 0.120645 0.299092 0.604512 11.00000 -1.50000 AFIX 0 O1A 4 -0.030057 0.525287 0.597403 10.65000 0.15219 O1B 4 0.036981 0.515972 0.528425 10.35000 0.14436 O2A 4 0.159611 0.556305 0.613880 10.65000 0.14613 O2B 4 0.169422 0.532447 0.517628 10.35000 0.14114 O3 4 -0.051662 0.464692 0.762366 10.50000 0.16540 O4 4 0.483475 0.141812 0.720669 10.50000 0.17475 HKLF 4 REM ip71 in C2/c REM R1 = 0.0312 for 3109 Fo > 4sig(Fo) and 0.0339 for all 3490 data REM 194 parameters refined using 0 restraints END WGHT 0.0575 0.0000 REM Highest difference peak 0.699, deepest hole -0.593, 1-sigma level 0.092 Q1 1 0.0190 -0.0407 0.7167 11.00000 0.05 0.70 Q2 1 0.0331 0.0024 0.7233 11.00000 0.05 0.68 Q3 1 0.2000 0.5254 0.4784 11.00000 0.05 0.60 Q4 1 0.0015 0.5347 0.6742 11.00000 0.05 0.59 Q5 1 0.1954 0.4719 0.5197 11.00000 0.05 0.58 Q6 1 0.1265 0.5317 0.5434 11.00000 0.05 0.57 Q7 1 0.1532 0.5430 0.6654 11.00000 0.05 0.51 Q8 1 0.1133 0.5356 0.6941 11.00000 0.05 0.49 Q9 1 -0.0330 0.5261 0.5725 11.00000 0.05 0.48 Q10 1 0.1249 0.4667 0.4601 11.00000 0.05 0.47 ; _database_code_depnum_ccdc_archive 'CCDC 947383' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_(5) _audit_creation_method SHELXL-97 _chemical_name_systematic ; mu-Hexafluorosilicato-bis(3,3',5,5'-Tetramethyl-4,4'-bipyrazole) cadmium(II), Solvate with 1.5 Dichloromethane ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C20 H28 Cd F6 N8 Si), 1.5(C H2 Cl2)' _chemical_formula_sum 'C21.50 H31 Cd Cl3 F6 N8 Si' _chemical_formula_weight 762.38 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'I 2/a' _space_group_name_Hall '-I 2ya' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 15.8930(12) _cell_length_b 11.8892(11) _cell_length_c 16.7929(12) _cell_angle_alpha 90.00 _cell_angle_beta 91.161(3) _cell_angle_gamma 90.00 _cell_volume 3172.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 9366 _cell_measurement_theta_min 3.22 _cell_measurement_theta_max 27.87 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.596 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1532 _exptl_absorpt_coefficient_mu 1.041 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8033 _exptl_absorpt_correction_T_max 0.8348 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'Siemens SMART CCD area-detector diffractometer' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 9366 _diffrn_reflns_av_R_equivalents 0.0123 _diffrn_reflns_av_sigmaI/netI 0.0108 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 27.87 _reflns_number_total 3741 _reflns_number_gt 3579 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT (Bruker, 1998)' _computing_cell_refinement 'SAINT-NT (Bruker, 1999)' _computing_data_reduction 'SAINT-NT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.700.00 (Farrugia, 1999)' #------------------------------- Refinement data-----------------------# _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. Note: The non-standard monoclinic-I setting was selected accordingly to the latest IUCr recommendations (See A.D. Mighel, Acta Cryst. (2003). B59, 300-302). Atoms of the framework were freely refined anisotropically and CH (methyl) and NH hydrogen atoms were added geometrically, with U(iso) = 1.5U(eq) of the parent C (N) atoms. Molecule of the solvent is equally disordered across a center of inversion, however, a significant residual electron density in this region was indicative for contribution from a second minor orientation of this molecule. Therefore, the partial occupancies for the major component of the disorder were 0.5 (related by inversion) and 0.25 for C11A, Cl1A, Cl2A (these atoms were left isotropic). The major component was refined anisotropically. A set of geometry restraints was applied to the disordered portion: C-Cl distances were restrained at 1.74(1) A and intramolecular contacts Cl...Cl at 2.88(1) A. ; _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^)+(0.0320P)^2^+8.8386P] 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_number_reflns 3741 _refine_ls_number_parameters 209 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0738 _refine_ls_wR_factor_gt 0.0731 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.102 _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 Cd1 Cd 0.0000 0.5000 0.0000 0.01571(7) Uani 1 2 d S . . Si1 Si 0.2500 0.47239(7) 0.0000 0.02005(16) Uani 1 2 d S . . F1 F 0.14371(8) 0.47043(12) 0.01190(8) 0.0279(3) Uani 1 1 d . . . F2 F 0.26478(8) 0.46877(13) 0.09908(8) 0.0302(3) Uani 1 1 d . . . F3 F 0.2500 0.32995(16) 0.0000 0.0265(4) Uani 1 2 d S . . F4 F 0.2500 0.61094(18) 0.0000 0.0399(5) Uani 1 2 d S . . N1 N -0.01521(11) 0.65520(16) 0.08224(11) 0.0233(4) Uani 1 1 d . . . N2 N -0.08787(11) 0.71482(16) 0.08434(11) 0.0252(4) Uani 1 1 d . . . H2 H -0.1287 0.7081 0.0494 0.038 Uiso 1 1 calc R . . N3 N 0.02493(12) 0.89776(17) 0.38532(11) 0.0260(4) Uani 1 1 d . . . N4 N 0.09027(11) 0.93608(18) 0.34230(11) 0.0277(4) Uani 1 1 d . . . H4 H 0.1298 0.9795 0.3615 0.042 Uiso 1 1 calc R . . C1 C 0.11420(15) 0.6402(3) 0.16522(16) 0.0393(6) Uani 1 1 d . . . H1A H 0.1101 0.5588 0.1634 0.059 Uiso 1 1 calc R . . H1B H 0.1320 0.6636 0.2183 0.059 Uiso 1 1 calc R . . H1C H 0.1550 0.6655 0.1269 0.059 Uiso 1 1 calc R . . C2 C 0.03043(13) 0.69039(19) 0.14533(12) 0.0238(4) Uani 1 1 d . . . C3 C -0.01334(13) 0.77327(19) 0.18736(12) 0.0235(4) Uani 1 1 d . . . C4 C -0.08946(14) 0.7855(2) 0.14667(14) 0.0270(4) Uani 1 1 d . . . C5 C -0.16393(17) 0.8586(3) 0.16181(19) 0.0470(7) Uani 1 1 d . . . H5A H -0.1874 0.8852 0.1115 0.070 Uiso 1 1 calc R . . H5B H -0.1466 0.9224 0.1942 0.070 Uiso 1 1 calc R . . H5C H -0.2061 0.8157 0.1896 0.070 Uiso 1 1 calc R . . C6 C -0.09812(17) 0.7738(2) 0.36034(16) 0.0395(6) Uani 1 1 d . . . H6A H -0.0873 0.7384 0.4116 0.059 Uiso 1 1 calc R . . H6B H -0.1131 0.7168 0.3213 0.059 Uiso 1 1 calc R . . H6C H -0.1441 0.8269 0.3649 0.059 Uiso 1 1 calc R . . C7 C -0.02077(13) 0.83456(19) 0.33457(13) 0.0239(4) Uani 1 1 d . . . C8 C 0.01577(13) 0.83344(19) 0.25904(12) 0.0237(4) Uani 1 1 d . . . C9 C 0.08719(14) 0.8995(2) 0.26693(13) 0.0273(5) Uani 1 1 d . . . C10 C 0.15297(18) 0.9322(3) 0.20908(17) 0.0462(7) Uani 1 1 d . . . H10A H 0.1792 1.0021 0.2261 0.069 Uiso 1 1 calc R . . H10B H 0.1272 0.9422 0.1567 0.069 Uiso 1 1 calc R . . H10C H 0.1953 0.8736 0.2068 0.069 Uiso 1 1 calc R . . C11 C 0.3793(7) 0.8374(9) 0.0181(6) 0.104(5) Uani 0.50 1 d PD A -1 H11A H 0.4083 0.7655 0.0108 0.125 Uiso 0.50 1 calc PR A -1 H11B H 0.3366 0.8441 -0.0246 0.125 Uiso 0.50 1 calc PR A -1 Cl1 Cl 0.3294(3) 0.8338(3) 0.1071(2) 0.1318(14) Uani 0.50 1 d PD A -1 Cl2 Cl 0.4505(3) 0.9435(5) 0.0080(3) 0.1668(18) Uani 0.50 1 d PD A -1 C11A C 0.3677(12) 0.8353(16) 0.0467(13) 0.069(5) Uiso 0.25 1 d PD B -2 H11C H 0.3508 0.7693 0.0775 0.082 Uiso 0.25 1 calc PR B -2 H11D H 0.3999 0.8084 0.0013 0.082 Uiso 0.25 1 calc PR B -2 Cl1A Cl 0.2786(12) 0.9023(15) 0.0113(16) 0.308(10) Uiso 0.25 1 d PD B -2 Cl2A Cl 0.4323(19) 0.918(3) 0.106(2) 0.56(2) Uiso 0.25 1 d PD 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 Cd1 0.01482(10) 0.02005(11) 0.01220(10) -0.00043(7) -0.00090(7) 0.00059(7) Si1 0.0123(3) 0.0254(4) 0.0223(4) 0.000 -0.0034(3) 0.000 F1 0.0136(5) 0.0407(7) 0.0295(7) -0.0067(6) -0.0022(5) 0.0011(5) F2 0.0211(6) 0.0472(8) 0.0223(6) -0.0058(6) -0.0034(5) -0.0053(6) F3 0.0238(9) 0.0255(9) 0.0301(9) 0.000 -0.0008(7) 0.000 F4 0.0369(11) 0.0263(10) 0.0566(14) 0.000 0.0005(10) 0.000 N1 0.0228(8) 0.0265(9) 0.0207(8) -0.0069(7) -0.0005(7) -0.0007(7) N2 0.0232(8) 0.0281(9) 0.0239(9) -0.0072(7) -0.0058(7) 0.0005(7) N3 0.0251(9) 0.0338(10) 0.0194(8) -0.0078(7) 0.0032(7) -0.0057(8) N4 0.0218(9) 0.0380(11) 0.0233(9) -0.0114(8) 0.0018(7) -0.0086(8) C1 0.0266(11) 0.0518(16) 0.0393(13) -0.0217(12) -0.0087(10) 0.0091(11) C2 0.0219(9) 0.0297(11) 0.0199(9) -0.0077(8) 0.0000(8) -0.0029(8) C3 0.0212(9) 0.0287(11) 0.0206(9) -0.0080(8) 0.0015(8) -0.0029(8) C4 0.0260(10) 0.0288(11) 0.0262(11) -0.0082(9) -0.0015(8) -0.0002(9) C5 0.0336(13) 0.0524(17) 0.0544(17) -0.0234(14) -0.0118(12) 0.0156(12) C6 0.0371(13) 0.0474(15) 0.0345(13) -0.0152(11) 0.0105(10) -0.0180(12) C7 0.0229(10) 0.0266(10) 0.0222(10) -0.0074(8) 0.0023(8) -0.0041(8) C8 0.0210(9) 0.0295(11) 0.0206(10) -0.0089(8) 0.0007(8) -0.0019(8) C9 0.0246(10) 0.0354(12) 0.0219(10) -0.0095(9) 0.0033(8) -0.0049(9) C10 0.0419(15) 0.0649(19) 0.0324(13) -0.0161(13) 0.0156(11) -0.0232(14) C11 0.127(11) 0.114(10) 0.071(7) 0.028(7) 0.031(7) 0.038(8) Cl1 0.179(3) 0.110(2) 0.109(2) 0.0044(19) 0.065(2) 0.042(2) Cl2 0.151(4) 0.214(5) 0.136(4) -0.023(4) 0.037(3) 0.007(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 F1 2.3156(12) 5_565 ? Cd1 F1 2.3156(12) . ? Cd1 N3 2.3183(18) 4_445 ? Cd1 N3 2.3183(18) 8_564 ? Cd1 N1 2.3204(18) . ? Cd1 N1 2.3204(18) 5_565 ? Si1 F4 1.647(2) . ? Si1 F2 1.6762(13) . ? Si1 F2 1.6762(13) 2 ? Si1 F3 1.693(2) . ? Si1 F1 1.7051(12) . ? Si1 F1 1.7051(12) 2 ? N1 C2 1.339(3) . ? N1 N2 1.356(3) . ? N2 C4 1.343(3) . ? N3 C7 1.339(3) . ? N3 N4 1.356(3) . ? N3 Cd1 2.3183(18) 4_455 ? N4 C9 1.338(3) . ? C1 C2 1.491(3) . ? C2 C3 1.405(3) . ? C3 C4 1.385(3) . ? C3 C8 1.467(3) . ? C4 C5 1.495(3) . ? C6 C7 1.497(3) . ? C7 C8 1.406(3) . ? C8 C9 1.385(3) . ? C9 C10 1.493(3) . ? C11 Cl2 1.706(9) . ? C11 Cl1 1.707(8) . ? C11A Cl2A 1.718(10) . ? C11A Cl1A 1.721(10) . ? 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 F1 Cd1 F1 180.0 5_565 . ? F1 Cd1 N3 88.07(6) 5_565 4_445 ? F1 Cd1 N3 91.93(6) . 4_445 ? F1 Cd1 N3 91.93(6) 5_565 8_564 ? F1 Cd1 N3 88.07(6) . 8_564 ? N3 Cd1 N3 180.00(9) 4_445 8_564 ? F1 Cd1 N1 79.41(6) 5_565 . ? F1 Cd1 N1 100.59(6) . . ? N3 Cd1 N1 84.31(7) 4_445 . ? N3 Cd1 N1 95.69(7) 8_564 . ? F1 Cd1 N1 100.59(6) 5_565 5_565 ? F1 Cd1 N1 79.41(6) . 5_565 ? N3 Cd1 N1 95.69(7) 4_445 5_565 ? N3 Cd1 N1 84.31(7) 8_564 5_565 ? N1 Cd1 N1 180.00(7) . 5_565 ? F4 Si1 F2 91.47(6) . . ? F4 Si1 F2 91.47(6) . 2 ? F2 Si1 F2 177.06(12) . 2 ? F4 Si1 F3 180.0 . . ? F2 Si1 F3 88.53(6) . . ? F2 Si1 F3 88.53(6) 2 . ? F4 Si1 F1 90.78(6) . . ? F2 Si1 F1 90.15(6) . . ? F2 Si1 F1 89.81(6) 2 . ? F3 Si1 F1 89.22(6) . . ? F4 Si1 F1 90.78(6) . 2 ? F2 Si1 F1 89.81(6) . 2 ? F2 Si1 F1 90.15(6) 2 2 ? F3 Si1 F1 89.22(6) . 2 ? F1 Si1 F1 178.43(11) . 2 ? Si1 F1 Cd1 164.92(9) . . ? C2 N1 N2 105.32(17) . . ? C2 N1 Cd1 131.16(15) . . ? N2 N1 Cd1 122.01(13) . . ? C4 N2 N1 112.12(17) . . ? C7 N3 N4 105.12(17) . . ? C7 N3 Cd1 136.32(15) . 4_455 ? N4 N3 Cd1 114.34(13) . 4_455 ? C9 N4 N3 112.40(18) . . ? N1 C2 C3 110.55(19) . . ? N1 C2 C1 121.29(19) . . ? C3 C2 C1 128.12(19) . . ? C4 C3 C2 105.19(18) . . ? C4 C3 C8 127.7(2) . . ? C2 C3 C8 127.11(19) . . ? N2 C4 C3 106.81(19) . . ? N2 C4 C5 121.6(2) . . ? C3 C4 C5 131.6(2) . . ? N3 C7 C8 110.54(19) . . ? N3 C7 C6 121.65(19) . . ? C8 C7 C6 127.8(2) . . ? C9 C8 C7 105.14(18) . . ? C9 C8 C3 126.8(2) . . ? C7 C8 C3 128.01(19) . . ? N4 C9 C8 106.80(19) . . ? N4 C9 C10 121.2(2) . . ? C8 C9 C10 132.0(2) . . ? Cl2 C11 Cl1 115.2(6) . . ? Cl2A C11A Cl1A 114.3(9) . . ? 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 F4 Si1 F1 Cd1 50.6(3) . . . . ? F2 Si1 F1 Cd1 142.1(3) . . . . ? F2 Si1 F1 Cd1 -40.9(3) 2 . . . ? F3 Si1 F1 Cd1 -129.4(3) . . . . ? N3 Cd1 F1 Si1 -173.8(3) 4_445 . . . ? N3 Cd1 F1 Si1 6.2(3) 8_564 . . . ? N1 Cd1 F1 Si1 -89.3(3) . . . . ? N1 Cd1 F1 Si1 90.7(3) 5_565 . . . ? F1 Cd1 N1 C2 153.0(2) 5_565 . . . ? F1 Cd1 N1 C2 -27.0(2) . . . . ? N3 Cd1 N1 C2 63.9(2) 4_445 . . . ? N3 Cd1 N1 C2 -116.1(2) 8_564 . . . ? F1 Cd1 N1 N2 -10.80(16) 5_565 . . . ? F1 Cd1 N1 N2 169.20(16) . . . . ? N3 Cd1 N1 N2 -99.90(17) 4_445 . . . ? N3 Cd1 N1 N2 80.10(17) 8_564 . . . ? C2 N1 N2 C4 -0.4(3) . . . . ? Cd1 N1 N2 C4 167.08(15) . . . . ? C7 N3 N4 C9 0.0(3) . . . . ? Cd1 N3 N4 C9 -160.77(17) 4_455 . . . ? N2 N1 C2 C3 -0.4(2) . . . . ? Cd1 N1 C2 C3 -166.19(15) . . . . ? N2 N1 C2 C1 177.5(2) . . . . ? Cd1 N1 C2 C1 11.7(3) . . . . ? N1 C2 C3 C4 0.9(3) . . . . ? C1 C2 C3 C4 -176.7(3) . . . . ? N1 C2 C3 C8 -179.2(2) . . . . ? C1 C2 C3 C8 3.2(4) . . . . ? N1 N2 C4 C3 0.9(3) . . . . ? N1 N2 C4 C5 -179.1(2) . . . . ? C2 C3 C4 N2 -1.1(3) . . . . ? C8 C3 C4 N2 179.0(2) . . . . ? C2 C3 C4 C5 178.9(3) . . . . ? C8 C3 C4 C5 -1.0(5) . . . . ? N4 N3 C7 C8 -0.3(3) . . . . ? Cd1 N3 C7 C8 154.04(18) 4_455 . . . ? N4 N3 C7 C6 178.2(2) . . . . ? Cd1 N3 C7 C6 -27.4(4) 4_455 . . . ? N3 C7 C8 C9 0.4(3) . . . . ? C6 C7 C8 C9 -178.0(3) . . . . ? N3 C7 C8 C3 178.9(2) . . . . ? C6 C7 C8 C3 0.5(4) . . . . ? C4 C3 C8 C9 -121.1(3) . . . . ? C2 C3 C8 C9 59.0(4) . . . . ? C4 C3 C8 C7 60.7(4) . . . . ? C2 C3 C8 C7 -119.2(3) . . . . ? N3 N4 C9 C8 0.2(3) . . . . ? N3 N4 C9 C10 179.7(3) . . . . ? C7 C8 C9 N4 -0.3(3) . . . . ? C3 C8 C9 N4 -178.8(2) . . . . ? C7 C8 C9 C10 -179.8(3) . . . . ? C3 C8 C9 C10 1.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.079 _refine_diff_density_min -0.775 _refine_diff_density_rms 0.077 _iucr_refine_instruction_details ; #--------------------------------------------------------- TITL i2a in I2/a CELL 0.71073 15.8930 11.8892 16.7929 90.000 91.161 90.000 ZERR 4.00 0.0012 0.0011 0.0012 0.000 0.003 0.000 LATT 2 SYMM 1/2 - X, Y, - Z SFAC C H N F SI CL CD UNIT 86 124 32 24 4 12 4 MERG 2 OMIT 0.00 180.00 OMIT -2 0 4 OMIT -1 2 1 OMIT -1 2 5 OMIT -3 1 6 OMIT 2 0 2 OMIT -2 1 5 SHEL 0.76 7 DFIX 1.740 0.01 C11 Cl1 C11 Cl2 DFIX 1.740 0.01 C11A CL1A C11A CL2A DFIX 2.880 0.01 CL1 CL2 CL1A CL2A FMAP 2 PLAN 20 SIZE 0.18 0.22 0.22 ACTA BOND CONF L.S. 5 TEMP -60.00 WGHT 0.032000 8.838600 FVAR 0.15227 CD1 7 0.000000 0.500000 0.000000 10.50000 0.01482 0.02005 = 0.01220 -0.00043 -0.00090 0.00059 SI1 5 0.250000 0.472388 0.000000 10.50000 0.01231 0.02540 = 0.02228 0.00000 -0.00336 0.00000 F1 4 0.143714 0.470425 0.011896 11.00000 0.01361 0.04067 = 0.02946 -0.00669 -0.00220 0.00114 F2 4 0.264780 0.468768 0.099081 11.00000 0.02110 0.04717 = 0.02227 -0.00576 -0.00340 -0.00528 F3 4 0.250000 0.329951 0.000000 10.50000 0.02382 0.02552 = 0.03012 0.00000 -0.00083 0.00000 F4 4 0.250000 0.610938 0.000000 10.50000 0.03686 0.02630 = 0.05656 0.00000 0.00051 0.00000 N1 3 -0.015206 0.655201 0.082242 11.00000 0.02280 0.02649 = 0.02066 -0.00695 -0.00047 -0.00067 N2 3 -0.087873 0.714820 0.084336 11.00000 0.02321 0.02814 = 0.02390 -0.00717 -0.00579 0.00054 AFIX 43 H2 2 -0.128703 0.708082 0.049366 11.00000 -1.50000 AFIX 0 N3 3 0.024933 0.897763 0.385316 11.00000 0.02509 0.03379 = 0.01937 -0.00785 0.00316 -0.00568 N4 3 0.090269 0.936079 0.342301 11.00000 0.02178 0.03800 = 0.02329 -0.01143 0.00180 -0.00861 AFIX 43 H4 2 0.129755 0.979539 0.361534 11.00000 -1.50000 AFIX 0 C1 1 0.114203 0.640186 0.165224 11.00000 0.02656 0.05181 = 0.03925 -0.02168 -0.00873 0.00909 AFIX 137 H1A 2 0.110119 0.558820 0.163404 11.00000 -1.50000 H1B 2 0.131999 0.663609 0.218272 11.00000 -1.50000 H1C 2 0.154999 0.665466 0.126942 11.00000 -1.50000 AFIX 0 C2 1 0.030430 0.690388 0.145329 11.00000 0.02191 0.02967 = 0.01986 -0.00771 0.00000 -0.00293 C3 1 -0.013340 0.773272 0.187362 11.00000 0.02119 0.02867 = 0.02062 -0.00800 0.00147 -0.00292 C4 1 -0.089458 0.785457 0.146668 11.00000 0.02600 0.02880 = 0.02615 -0.00817 -0.00149 -0.00024 C5 1 -0.163928 0.858594 0.161812 11.00000 0.03363 0.05241 = 0.05438 -0.02344 -0.01184 0.01562 AFIX 137 H5A 2 -0.187397 0.885204 0.111478 11.00000 -1.50000 H5B 2 -0.146586 0.922392 0.194193 11.00000 -1.50000 H5C 2 -0.206133 0.815654 0.189594 11.00000 -1.50000 AFIX 0 C6 1 -0.098118 0.773797 0.360340 11.00000 0.03710 0.04743 = 0.03447 -0.01518 0.01049 -0.01804 AFIX 137 H6A 2 -0.087255 0.738379 0.411558 11.00000 -1.50000 H6B 2 -0.113095 0.716764 0.321255 11.00000 -1.50000 H6C 2 -0.144114 0.826886 0.364902 11.00000 -1.50000 AFIX 0 C7 1 -0.020771 0.834558 0.334567 11.00000 0.02294 0.02662 = 0.02219 -0.00736 0.00225 -0.00408 C8 1 0.015767 0.833445 0.259041 11.00000 0.02102 0.02951 = 0.02064 -0.00889 0.00065 -0.00190 C9 1 0.087191 0.899527 0.266930 11.00000 0.02460 0.03542 = 0.02193 -0.00955 0.00327 -0.00493 C10 1 0.152970 0.932215 0.209079 11.00000 0.04187 0.06491 = 0.03235 -0.01608 0.01557 -0.02317 AFIX 137 H10A 2 0.179184 1.002100 0.226112 11.00000 -1.50000 H10B 2 0.127185 0.942221 0.156709 11.00000 -1.50000 H10C 2 0.195281 0.873563 0.206829 11.00000 -1.50000 AFIX 0 PART -1 C11 1 0.379264 0.837363 0.018075 10.50000 0.12669 0.11430 = 0.07148 0.02785 0.03080 0.03757 AFIX 23 H11A 2 0.408344 0.765528 0.010762 10.50000 -1.20000 H11B 2 0.336637 0.844138 -0.024645 10.50000 -1.20000 AFIX 0 CL1 6 0.329404 0.833842 0.107102 10.50000 0.17875 0.11015 = 0.10906 0.00435 0.06536 0.04192 CL2 6 0.450461 0.943508 0.008026 10.50000 0.15138 0.21424 = 0.13629 -0.02286 0.03684 0.00675 PART -2 C11A 1 0.367736 0.835264 0.046738 10.25000 0.06866 AFIX 23 H11C 2 0.350799 0.769308 0.077530 10.25000 -1.20000 H11D 2 0.399850 0.808360 0.001316 10.25000 -1.20000 AFIX 0 CL1A 6 0.278602 0.902341 0.011311 10.25000 0.30841 CL2A 6 0.432289 0.917763 0.105651 10.25000 0.55613 HKLF 4 REM i2a in I2/a REM R1 = 0.0291 for 3579 Fo > 4sig(Fo) and 0.0305 for all 3741 data REM 209 parameters refined using 6 restraints END WGHT 0.0320 8.8461 REM Highest difference peak 1.079, deepest hole -0.775, 1-sigma level 0.077 Q1 1 0.2500 0.8976 0.0000 10.50000 0.05 1.08 Q2 1 0.4009 0.8750 0.1130 11.00000 0.05 0.45 Q3 1 0.3024 0.8150 0.0459 11.00000 0.05 0.45 Q4 1 0.3842 0.8579 0.0709 11.00000 0.05 0.42 Q5 1 0.3499 0.9816 -0.0082 11.00000 0.05 0.40 Q6 1 -0.0326 0.4987 0.0344 11.00000 0.05 0.38 Q7 1 0.0148 0.7389 0.1672 11.00000 0.05 0.33 Q8 1 0.1336 0.5947 0.1366 11.00000 0.05 0.33 Q9 1 0.4250 0.8948 0.0616 11.00000 0.05 0.33 Q10 1 -0.0092 0.8441 0.2931 11.00000 0.05 0.32 ; # ------------- END of CIF -----------------# _database_code_depnum_ccdc_archive 'CCDC 947384'