Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Chaudhuri, N. R.' 'Das, Debasis' 'Laskar, I. R.' 'Maji, T. K.' 'Mostafa, G.' 'Welch, Alan' _publ_contact_author_name 'Prof N R Chaudhuri' _publ_contact_author_address ; Department of Chemistry Indian Association for the Cultivation of Science Jadavpur Calcutta 700 032 INDIA ; _publ_contact_author_email 'ICNRC@MAHENDRA.IACS.RES.IN' _publ_section_title ; Flexibility in co-ordinative behaviour of N-(3-hydroxypropyl)ethane - 1,2-diamine toward cadmium(II) halides: syntheses, crystal structrues adn solid state thermal studies ; data_complex1 _database_code_CSD 174453 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C5 H14 Cd Cl2 N2 O' _chemical_formula_structural ? # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_sum 'C5 H14 Cd Cl2 N2 O' _chemical_formula_weight 301.49 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd 0.1185 4.6533 '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' C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 8.0338(9) _cell_length_b 9.4550(1) _cell_length_c 13.122(4) _cell_angle_alpha 90 _cell_angle_beta 95.97(2) _cell_angle_gamma 90 _cell_volume 991.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5 _cell_measurement_theta_max 61 _exptl_crystal_description paralleopiped _exptl_crystal_colour colourless _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.53 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.020 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 22.229 _exptl_crystal_density_meas_temp ? _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_correction_T_min 0.556 _exptl_absorpt_correction_T_max 0.997 _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'CAD4 Enraf-Nonius diffractometer' _diffrn_measurement_method '\w-2\q' _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? # number of measured reflections (redundant set) _diffrn_reflns_number 2186 _diffrn_reflns_av_R_equivalents 0.0542 _diffrn_reflns_av_sigmaI/netI 0.0307 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 5.54 _diffrn_reflns_theta_max 74.95 _diffrn_reflns_reduction_process ; ? ; # number of unique reflections _reflns_number_total 2040 # number of observed reflections (> n sig(I)) _reflns_number_gt 2011 _reflns_threshold_expression 'I>2\\s(I)' _computing_data_collection 'CAD4 Software (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD4 Software (Enraf-Nonius, 1989)' _computing_data_reduction 'HELENA (Spek, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON-99 (SPEK, 1999) & ZORTEP (Zsolnai, 1995)' _computing_publication_material 'PLATON (Spek, 1999)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2 for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2 > 2sigma(F^2) is used only for calculating -R-factor-obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2 are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1267P)^2^+1.2020P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment 'noref' _refine_ls_extinction_method shelxl _refine_ls_extinction_coef 0.0081(6) _refine_ls_extinction_expression 'FC^*^=KFC[1+0.001XFC^2^\L^3^/SIN(2\Q)]^-1/4^' _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack none _refine_ls_number_reflns 2040 _refine_ls_number_parameters 101 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0884 _refine_ls_R_factor_gt 0.0581 _refine_ls_wR_factor_ref 0.1447 _refine_ls_wR_factor_gt 0.1443 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max -0.001 _refine_ls_shift/su_mean 0.000 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv Cd1 Cd Uani 0.04050(3) 0.09419(3) 0.87891(2) 1.000 0.0114(2) Cl2 Cl Uani -0.19827(11) 0.26903(10) 0.86593(8) 1.000 0.0165(3) Cl3 Cl Uani 0.14447(11) 0.12317(11) 1.07548(7) 1.000 0.0139(3) O O Uani 0.0349(3) 0.5111(3) 0.7968(2) 1.000 0.0179(8) N1 N Uani 0.2668(5) -0.0616(4) 0.8698(3) 1.000 0.0170(12) N2 N Uani 0.2492(4) 0.2440(4) 0.8197(3) 1.000 0.0145(12) C1 C Uani 0.4132(5) 0.0233(5) 0.8478(3) 1.000 0.0199(12) C2 C Uani 0.3645(5) 0.1425(4) 0.7759(3) 1.000 0.0152(12) C3 C Uani 0.3432(5) 0.3399(5) 0.8942(3) 1.000 0.0177(12) C4 C Uani 0.2321(5) 0.4488(4) 0.9415(3) 1.000 0.0111(12) C5 C Uani 0.1620(5) 0.5629(5) 0.8696(3) 1.000 0.0159(12) H H Uiso -0.0279(3) 0.4361(3) 0.8182(2) 1.000 0.0220 H1A H Uiso 0.2891(5) -0.1079(4) 0.9296(3) 1.000 0.0200 H1B H Uiso 0.2420(5) -0.1257(4) 0.8198(3) 1.000 0.0200 H1C H Uiso 0.4928(5) -0.0372(5) 0.8180(3) 1.000 0.0240 H1D H Uiso 0.4676(5) 0.0612(5) 0.9115(3) 1.000 0.0240 H2 H Uiso 0.1996(4) 0.2976(4) 0.7675(3) 1.000 0.0170 H2A H Uiso 0.4644(5) 0.1923(4) 0.7605(3) 1.000 0.0180 H2B H Uiso 0.3102(5) 0.1046(4) 0.7122(3) 1.000 0.0180 H3A H Uiso 0.4272(5) 0.3896(5) 0.8600(3) 1.000 0.0210 H3B H Uiso 0.4010(5) 0.2837(5) 0.9487(3) 1.000 0.0210 H4A H Uiso 0.1396(5) 0.3992(4) 0.9675(3) 1.000 0.0130 H4B H Uiso 0.2970(5) 0.4930(4) 0.9994(3) 1.000 0.0130 H5A H Uiso 0.1168(5) 0.6381(5) 0.9088(3) 1.000 0.0190 H5B H Uiso 0.2514(5) 0.6025(5) 0.8342(3) 1.000 0.0190 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 0.0084(3) 0.0112(3) 0.0126(3) 0.0003(1) -0.0089(2) -0.0010(1) Cl2 0.0080(5) 0.0139(5) 0.0259(6) 0.0005(4) -0.0059(4) 0.0034(3) Cl3 0.0150(5) 0.0116(5) 0.0129(5) 0.0004(3) -0.0096(4) -0.0070(3) O 0.0154(14) 0.0182(15) 0.0183(14) 0.0026(11) -0.0072(11) -0.0028(11) N1 0.016(2) 0.012(2) 0.021(2) 0.002(2) -0.0072(14) -0.0001(14) N2 0.011(2) 0.013(2) 0.018(2) 0.0010(13) -0.0050(12) -0.0009(12) C1 0.013(2) 0.016(2) 0.029(2) -0.002(2) -0.006(2) 0.0033(15) C2 0.012(2) 0.013(2) 0.020(2) -0.001(2) -0.0019(15) 0.0014(14) C3 0.014(2) 0.015(2) 0.023(2) -0.005(2) -0.003(2) -0.0007(15) C4 0.010(2) 0.010(2) 0.012(2) -0.0028(15) -0.0052(13) -0.0014(14) C5 0.013(2) 0.014(2) 0.019(2) -0.003(2) -0.006(2) -0.002(2) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All esds are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 Cl2 2.5246(12) . . yes Cd1 Cl3 2.6416(12) . . yes Cd1 N1 2.353(4) . . yes Cd1 N2 2.386(4) . . yes Cd1 O 2.451(3) . 2_546 yes Cd1 Cl3 2.6410(13) . 3_557 yes O C5 1.411(5) . . yes O H 0.930(4) . . no N1 C1 1.477(6) . . yes N2 C2 1.490(5) . . yes N2 C3 1.481(6) . . yes N1 H1A 0.900(6) . . no N1 H1B 0.900(5) . . no N2 H2 0.910(5) . . no C1 C2 1.496(6) . . no C3 C4 1.535(6) . . no C4 C5 1.504(6) . . no C1 H1C 0.970(6) . . no C1 H1D 0.971(6) . . no C2 H2A 0.970(6) . . no C2 H2B 0.970(6) . . no C3 H3A 0.970(6) . . no C3 H3B 0.970(6) . . no C4 H4A 0.970(6) . . no C4 H4B 0.970(6) . . no C5 H5A 0.970(6) . . no C5 H5B 0.970(6) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl2 Cd1 Cl3 99.14(4) . . . yes Cl2 Cd1 N1 172.91(10) . . . yes Cl2 Cd1 N2 98.28(9) . . . yes Cl2 Cd1 O 91.99(7) . . 2_546 yes Cl2 Cd1 Cl3 94.78(4) . . 3_557 yes Cl3 Cd1 N1 86.96(10) . . . yes Cl3 Cd1 N2 95.44(10) . . . yes Cl3 Cd1 O 166.84(7) . . 2_546 yes Cl3 Cd1 Cl3 89.29(4) . . 3_557 yes N1 Cd1 N2 77.42(13) . . . yes O Cd1 N1 82.43(12) 2_546 . . yes Cl3 Cd1 N1 88.87(10) 3_557 . . yes O Cd1 N2 89.84(11) 2_546 . . yes Cl3 Cd1 N2 165.20(9) 3_557 . . yes Cl3 Cd1 O 82.76(7) 3_557 . 2_546 yes Cd1 Cl3 Cd1 90.71(4) . . 3_557 yes Cd1 O C5 128.0(2) 2_556 . . yes Cd1 O H 116.1(2) 2_556 . . no C5 O H 115.9(3) . . . no Cd1 N1 C1 107.8(3) . . . yes Cd1 N2 C2 103.3(2) . . . yes C2 N2 C3 110.7(3) . . . yes Cd1 N2 C3 118.4(3) . . . yes Cd1 N1 H1B 110.2(4) . . . no Cd1 N1 H1A 110.2(4) . . . no H1A N1 H1B 108.5(5) . . . no C1 N1 H1A 110.1(5) . . . no C1 N1 H1B 110.1(5) . . . no C3 N2 H2 108.0(4) . . . no Cd1 N2 H2 108.0(3) . . . no C2 N2 H2 108.0(4) . . . no N1 C1 C2 111.8(3) . . . yes N2 C2 C1 112.0(3) . . . yes N2 C3 C4 113.5(3) . . . yes C3 C4 C5 115.0(3) . . . no O C5 C4 111.9(4) . . . yes N1 C1 H1C 109.3(5) . . . no N1 C1 H1D 109.2(4) . . . no C2 C1 H1C 109.3(4) . . . no C2 C1 H1D 109.3(5) . . . no H1C C1 H1D 107.9(5) . . . no N2 C2 H2A 109.2(4) . . . no N2 C2 H2B 109.2(4) . . . no C1 C2 H2A 109.2(4) . . . no C1 C2 H2B 109.3(4) . . . no H2A C2 H2B 107.9(5) . . . no N2 C3 H3A 108.8(4) . . . no N2 C3 H3B 108.9(5) . . . no C4 C3 H3A 108.9(5) . . . no C4 C3 H3B 108.9(4) . . . no H3A C3 H3B 107.7(5) . . . no C3 C4 H4A 108.5(4) . . . no C3 C4 H4B 108.5(4) . . . no C5 C4 H4A 108.5(4) . . . no C5 C4 H4B 108.5(4) . . . no H4A C4 H4B 107.6(5) . . . no O C5 H5A 109.2(4) . . . no O C5 H5B 109.2(4) . . . no C4 C5 H5A 109.2(4) . . . no C4 C5 H5B 109.3(4) . . . no H5A C5 H5B 107.9(6) . . . no 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 Cl2 Cd1 Cl3 Cd1 94.73(4) . . . 3_557 no N1 Cd1 Cl3 Cd1 -88.91(10) . . . 3_557 no N2 Cd1 Cl3 Cd1 -165.95(9) . . . 3_557 no Cl3 Cd1 Cl3 Cd1 0.00(4) 3_557 . . 3_557 no Cl3 Cd1 N1 C1 -88.4(3) . . . . no N2 Cd1 N1 C1 7.9(3) . . . . no O Cd1 N1 C1 99.4(3) 2_546 . . . no Cl3 Cd1 N1 C1 -177.7(3) 3_557 . . . no Cl2 Cd1 N2 C2 -153.4(2) . . . . no Cl2 Cd1 N2 C3 83.9(3) . . . . no Cl3 Cd1 N2 C2 106.5(2) . . . . no Cl3 Cd1 N2 C3 -16.2(3) . . . . no N1 Cd1 N2 C2 20.9(2) . . . . no N1 Cd1 N2 C3 -101.9(3) . . . . no O Cd1 N2 C2 -61.4(2) 2_546 . . . no O Cd1 N2 C3 175.8(3) 2_546 . . . no Cl2 Cd1 O C5 4.0(3) . . 2_546 2_546 no N1 Cd1 O C5 -171.6(3) . . 2_546 2_546 no N2 Cd1 O C5 -94.3(3) . . 2_546 2_546 no Cl2 Cd1 Cl3 Cd1 -99.11(4) . . 3_557 3_557 no Cl3 Cd1 Cl3 Cd1 0.00(4) . . 3_557 3_557 no N1 Cd1 Cl3 Cd1 86.98(10) . . 3_557 3_557 no Cd1 O C5 C4 -149.6(3) 2_556 . . . no H O C5 H5B 151.5(5) . . . . no H O C5 C4 30.4(5) . . . . no H O C5 H5A -90.7(5) . . . . no Cd1 O C5 H5A 89.4(5) 2_556 . . . no Cd1 O C5 H5B -28.4(6) 2_556 . . . no Cd1 N1 C1 C2 -37.0(4) . . . . no C3 N2 C2 C1 78.7(4) . . . . no Cd1 N2 C3 C4 -61.8(4) . . . . no Cd1 N2 C2 C1 -49.0(3) . . . . no C2 N2 C3 C4 179.3(3) . . . . no N1 C1 C2 N2 62.0(4) . . . . no N2 C3 C4 C5 -70.6(5) . . . . no C3 C4 C5 O 72.4(4) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cd1 O 4.085(3) . . no Cd1 H 3.361(3) . . no Cd1 H4A 3.180(4) . . no Cd1 H2 3.809(4) . 2_546 no Cd1 H1A 3.837(4) . 3_557 no Cl2 O 3.150(3) . . no Cl2 N1 3.476(4) . 2_556 no Cl3 N2 3.463(4) . 4_555 no Cl3 O 3.369(3) . 4_555 no Cl2 H4A 3.147(4) . . no Cl2 H 2.222(3) . . no Cl2 H5B 3.054(4) . 2_546 no Cl2 H4B 3.018(4) . 3_567 no Cl2 H2A 3.001(4) . 1_455 no Cl2 H1B 2.622(4) . 2_556 no Cl2 H5A 3.088(4) . 3_567 no Cl3 H5A 3.104(5) . 3_567 no Cl3 H4A 2.968(4) . . no Cl3 H2 2.622(4) . 4_555 no O Cd1 4.085(3) . . no O Cl2 3.150(3) . . no O N2 3.054(5) . . no O Cl3 3.369(3) . 4_554 no O H2 2.466(5) . . no O H2B 2.901(5) . 2_556 no N1 Cl2 3.476(4) . 2_546 no N2 O 3.054(5) . . no N2 Cl3 3.463(4) . 4_554 no N2 H 2.872(4) . . no C1 H3B 2.802(6) . . no C3 H1D 2.819(7) . . no C5 H1B 3.098(6) . 1_565 no C5 H2 2.874(6) . . no H Cd1 3.361(3) . . no H Cl2 2.222(3) . . no H N2 2.872(4) . . no H H2 2.398(4) . . no H H4A 2.285(5) . . no H H1B 2.435(5) . 2_556 no H1A Cd1 3.837(4) . 3_557 no H1B C5 3.098(6) . 1_545 no H1B H5B 2.577(6) . 1_545 no H1B Cl2 2.622(4) . 2_546 no H1B H 2.435(5) . 2_546 no H1C H3A 2.581(6) . 2_646 no H1D C3 2.819(7) . . no H1D H3B 2.237(7) . . no H1D H1D 2.599(6) . 3_657 no H2 O 2.466(5) . . no H2 C5 2.874(6) . . no H2 H 2.398(4) . . no H2 Cd1 3.809(4) . 2_556 no H2 Cl3 2.622(4) . 4_554 no H2A Cl2 3.001(4) . 1_655 no H2A H3A 2.314(6) . . no H2B O 2.901(5) . 2_546 no H3A H2A 2.314(6) . . no H3A H5B 2.462(6) . . no H3A H1C 2.581(6) . 2_656 no H3B C1 2.802(6) . . no H3B H1D 2.237(7) . . no H4A Cd1 3.180(4) . . no H4A Cl2 3.147(4) . . no H4A Cl3 2.968(4) . . no H4A H 2.285(5) . . no H4B Cl2 3.018(4) . 3_567 no H5A Cl2 3.088(4) . 3_567 no H5A Cl3 3.104(5) . 3_567 no H5B H1B 2.577(6) . 1_565 no H5B H3A 2.462(6) . . no H5B Cl2 3.054(4) . 2_556 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # O H Cl2 0.930(4) 2.222(3) 3.150(3) 174.8(3) . yes N1 H1B Cl2 0.900(5) 2.622(4) 3.476(4) 158.6(4) 2_546 yes N2 H2 O 0.910(5) 2.466(5) 3.054(5) 122.6(4) . yes N2 H2 Cl3 0.910(5) 2.622(4) 3.463(4) 154.1(4) 4_554 yes _diffrn_measured_fraction_theta_max 1.00 _diffrn_reflns_theta_full 74.95 _diffrn_measured_fraction_theta_full 1.00 _refine_diff_density_max 2.374 _refine_diff_density_min -4.200 _refine_diff_density_rms 0.319 # = = = END data_complex2 _database_code_CSD 174454 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C5 H14 Br2 Cd N2 O' _chemical_formula_sum 'C5 H14 Br2 Cd N2 O' _chemical_formula_weight 390.40 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' 'Br' 'Br' -0.2901 2.4595 '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' '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.113(3) _cell_length_b 7.187(3) _cell_length_c 16.420(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.03(3) _cell_angle_gamma 90.00 _cell_volume 1033.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 20 _exptl_crystal_description paralleopiped _exptl_crystal_colour ? _exptl_crystal_size_max .26 _exptl_crystal_size_mid .21 _exptl_crystal_size_min .13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 736 _exptl_absorpt_coefficient_mu 9.798 _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_correction_T_min 0.336 _exptl_absorpt_correction_T_max 0.889 _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 P4 diffracometer' _diffrn_measurement_method '\w-2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1812 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1812 _reflns_number_gt 1682 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ZORTEP (Zsolnai, 1994),' _computing_publication_material 'Platon99 (Spek, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+4.8454P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1812 _refine_ls_number_parameters 100 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0871 _refine_ls_wR_factor_gt 0.0867 _refine_ls_goodness_of_fit_ref 1.123 _refine_ls_restrained_S_all 1.123 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd Cd 0.30526(4) 0.03955(6) 0.01505(3) 0.02068(16) Uani 1 1 d . . . Br1 Br 0.42839(6) 0.11306(9) -0.11993(4) 0.02262(18) Uani 1 1 d . . . Br2 Br 0.18832(6) -0.28733(9) -0.04919(4) 0.02447(18) Uani 1 1 d . . . O O -0.0538(4) -0.1698(6) 0.0624(3) 0.0269(10) Uani 1 1 d . . . H1O H 0.0134 -0.1934 0.0301 0.032 Uiso 1 1 calc R . . N1 N 0.4080(6) 0.3531(8) 0.0630(3) 0.0288(12) Uani 1 1 d . . . H1A H 0.5076 0.3602 0.0650 0.035 Uiso 1 1 calc R . . H1B H 0.3568 0.4413 0.0274 0.035 Uiso 1 1 calc R . . N2 N 0.1938(5) 0.1358(7) 0.1271(3) 0.0176(10) Uani 1 1 d . . . H2 H 0.0912 0.1317 0.1027 0.021 Uiso 1 1 calc R . . C1 C 0.3864(8) 0.3782(10) 0.1507(4) 0.0304(15) Uani 1 1 d . . . H1C H 0.3991 0.5078 0.1678 0.036 Uiso 1 1 calc R . . H1D H 0.4598 0.3040 0.1919 0.036 Uiso 1 1 calc R . . C2 C 0.2236(7) 0.3129(9) 0.1434(4) 0.0299(15) Uani 1 1 d . . . H2A H 0.2003 0.3423 0.1961 0.036 Uiso 1 1 calc R . . H2B H 0.1545 0.3849 0.0991 0.036 Uiso 1 1 calc R . . C3 C 0.2227(7) -0.0099(10) 0.2066(4) 0.0298(15) Uani 1 1 d . . . H3A H 0.3313 -0.0134 0.2346 0.036 Uiso 1 1 calc R . . H3B H 0.1724 0.0388 0.2470 0.036 Uiso 1 1 calc R . . C4 C 0.1713(8) -0.1960(10) 0.1862(4) 0.0353(16) Uani 1 1 d . . . H4A H 0.2055 -0.2722 0.2367 0.042 Uiso 1 1 calc R . . H4B H 0.2185 -0.2443 0.1443 0.042 Uiso 1 1 calc R . . C5 C 0.0023(7) -0.2143(10) 0.1527(4) 0.0295(15) Uani 1 1 d . . . H5A H -0.0269 -0.3407 0.1617 0.035 Uiso 1 1 calc R . . H5B H -0.0461 -0.1319 0.1843 0.035 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd 0.0150(2) 0.0327(3) 0.0197(3) -0.00101(18) 0.01368(19) 0.00091(17) Br1 0.0164(3) 0.0368(4) 0.0191(3) 0.0024(3) 0.0123(2) 0.0034(2) Br2 0.0164(3) 0.0333(4) 0.0274(3) -0.0028(3) 0.0121(2) 0.0012(2) O 0.018(2) 0.050(3) 0.017(2) -0.011(2) 0.0131(17) 0.000(2) N1 0.024(3) 0.040(3) 0.025(3) 0.006(2) 0.010(2) -0.005(2) N2 0.017(2) 0.029(3) 0.012(2) -0.006(2) 0.0127(19) 0.002(2) C1 0.032(3) 0.042(4) 0.019(3) -0.019(3) 0.010(3) -0.005(3) C2 0.022(3) 0.034(4) 0.037(4) -0.017(3) 0.015(3) -0.008(3) C3 0.019(3) 0.040(4) 0.032(4) 0.009(3) 0.010(3) 0.004(3) C4 0.036(4) 0.047(4) 0.027(4) 0.008(3) 0.015(3) 0.005(3) C5 0.034(3) 0.039(4) 0.018(3) -0.003(3) 0.011(3) 0.013(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 Cd N2 2.435(4) . ? Cd O 2.477(4) 3 ? Cd N1 2.483(6) . ? Cd Br2 2.6733(12) . ? Cd Br1 2.7842(12) 3_655 ? Cd Br1 2.7971(10) . ? Br1 Cd 2.7842(12) 3_655 ? O C5 1.463(7) . ? O Cd 2.477(4) 3 ? N1 C1 1.517(8) . ? N2 C2 1.313(8) . ? N2 C3 1.637(8) . ? C1 C2 1.530(9) . ? C3 C4 1.426(10) . ? C4 C5 1.491(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cd O 76.15(15) . 3 ? N2 Cd N1 72.69(17) . . ? O Cd N1 91.96(17) 3 . ? N2 Cd Br2 110.11(12) . . ? O Cd Br2 85.30(11) 3 . ? N1 Cd Br2 175.41(12) . . ? N2 Cd Br1 96.83(12) . 3_655 ? O Cd Br1 172.47(9) 3 3_655 ? N1 Cd Br1 88.48(13) . 3_655 ? Br2 Cd Br1 94.72(3) . 3_655 ? N2 Cd Br1 152.56(12) . . ? O Cd Br1 92.20(10) 3 . ? N1 Cd Br1 83.16(12) . . ? Br2 Cd Br1 93.25(3) . . ? Br1 Cd Br1 95.31(3) 3_655 . ? Cd Br1 Cd 84.69(3) 3_655 . ? C5 O Cd 128.1(3) . 3 ? C1 N1 Cd 105.8(4) . . ? C2 N2 C3 118.6(5) . . ? C2 N2 Cd 108.9(4) . . ? C3 N2 Cd 114.3(3) . . ? N1 C1 C2 105.5(5) . . ? N2 C2 C1 117.1(6) . . ? C4 C3 N2 116.3(6) . . ? C3 C4 C5 114.1(6) . . ? O C5 C4 113.0(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.933 _refine_diff_density_min -2.081 _refine_diff_density_rms 0.171 # = = = END data_complex3 _database_code_CSD 174455 _audit_creation_method SHELXL 97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C5 H14 Cd I2 N2 O' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C5 H14 Cd I2 N2 O' _chemical_formula_weight 484.38 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 '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' 'C' 'C' 0.0033 0.0016 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' 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 14.0470(10) _cell_length_b 10.6900(10) _cell_length_c 15.965(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.510(10) _cell_angle_gamma 90.00 _cell_volume 2389.9(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 32 _cell_measurement_theta_min 10 _cell_measurement_theta_max 20 _exptl_crystal_description paralleopiped _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.692 _exptl_crystal_density_method ? _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 6.955 _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_correction_T_min .516 _exptl_absorpt_correction_T_max .877 _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Siemens P4 diffracometer' _diffrn_measurement_method '\w-2\q' _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2671 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0451 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2113 _reflns_number_observed 1613 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ZORTEP (Zsolnai, 1994)' _computing_publication_material 'Platon 99 (Spek, 1999)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0389P)^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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00126(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2113 _refine_ls_number_parameters 103 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0609 _refine_ls_R_factor_obs 0.0394 _refine_ls_wR_factor_all 0.0887 _refine_ls_wR_factor_obs 0.0800 _refine_ls_goodness_of_fit_all 1.035 _refine_ls_goodness_of_fit_obs 1.075 _refine_ls_restrained_S_all 1.035 _refine_ls_restrained_S_obs 1.075 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group I2 I -0.10274(5) 0.39073(7) 0.35959(4) 0.0567(2) Uani 1 d . . Cd2 Cd 0.0000 0.25815(9) 0.2500 0.0425(3) Uani 1 d S . I1 I 0.12082(5) 0.09740(6) 0.34749(4) 0.0528(2) Uani 1 d . . Cd1 Cd 0.0000 0.0000 0.5000 0.0623(4) Uani 1 d S . N1 N -0.0018(6) -0.1972(7) 0.4523(5) 0.053(2) Uani 1 d . . H1A H 0.0495(6) -0.2116(7) 0.4233(5) 0.063 Uiso 1 calc R . H1B H -0.0009(6) -0.2515(7) 0.4954(5) 0.063 Uiso 1 calc R . N2 N -0.1424(5) -0.0029(7) 0.4058(5) 0.047(2) Uani 1 d . . H2 H -0.1346(5) 0.0544(7) 0.3648(5) 0.056 Uiso 1 calc R . C1 C -0.0887(14) -0.2122(14) 0.3981(15) 0.203(13) Uani 1 d . . H1C H -0.0710(14) -0.2614(14) 0.3507(15) 0.244 Uiso 1 calc R . H1D H -0.1298(14) -0.2654(14) 0.4289(15) 0.244 Uiso 1 calc R . C2 C -0.1418(11) -0.1266(12) 0.3671(9) 0.105(6) Uani 1 d . . H2A H -0.2068(11) -0.1578(12) 0.3644(9) 0.126 Uiso 1 calc R . H2B H -0.1259(11) -0.1149(12) 0.3096(9) 0.126 Uiso 1 calc R . C3 C -0.2295(7) 0.0313(11) 0.4463(6) 0.061(3) Uani 1 d . . H3A H -0.2214(7) 0.1152(11) 0.4687(6) 0.073 Uiso 1 calc R . H3B H -0.2355(7) -0.0246(11) 0.4934(6) 0.073 Uiso 1 calc R . C4 C -0.3221(8) 0.0272(11) 0.3911(6) 0.065(3) Uani 1 d . . H4A H -0.3748(8) 0.0347(11) 0.4265(6) 0.078 Uiso 1 calc R . H4B H -0.3273(8) -0.0538(11) 0.3638(6) 0.078 Uiso 1 calc R . C5 C -0.3323(9) 0.1288(11) 0.3236(7) 0.069(3) Uani 1 d . . H5A H -0.2784(9) 0.1247(11) 0.2893(7) 0.083 Uiso 1 calc R . H5B H -0.3899(9) 0.1137(11) 0.2873(7) 0.083 Uiso 1 calc R . O O -0.3368(7) 0.2492(8) 0.3591(6) 0.104(3) Uani 1 d . . H H -0.2986(7) 0.2954(8) 0.3381(6) 0.124 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I2 0.0621(4) 0.0587(4) 0.0515(4) -0.0018(3) 0.0171(3) 0.0138(3) Cd2 0.0441(5) 0.0476(5) 0.0363(5) 0.000 0.0070(4) 0.000 I1 0.0486(4) 0.0671(4) 0.0435(3) 0.0128(3) 0.0086(3) 0.0131(3) Cd1 0.0445(6) 0.0568(6) 0.0818(8) -0.0270(6) -0.0196(6) 0.0135(5) N1 0.055(5) 0.044(4) 0.059(5) 0.000(4) 0.008(4) 0.015(4) N2 0.048(5) 0.054(5) 0.038(4) 0.002(3) -0.002(3) -0.001(4) C1 0.181(19) 0.081(11) 0.318(28) -0.109(15) -0.169(20) 0.069(12) C2 0.110(12) 0.083(10) 0.111(11) -0.044(8) -0.055(10) 0.026(9) C3 0.049(6) 0.090(8) 0.042(5) 0.004(5) 0.001(5) -0.002(6) C4 0.054(6) 0.079(8) 0.060(6) -0.005(6) -0.002(5) -0.002(6) C5 0.072(8) 0.079(8) 0.058(6) 0.005(6) 0.013(6) 0.024(7) O 0.095(7) 0.066(5) 0.155(9) 0.004(6) 0.046(7) -0.002(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I2 Cd2 2.7477(8) . ? Cd2 I2 2.7477(8) 2 ? Cd2 I1 2.8000(9) 2 ? Cd2 I1 2.8000(9) . ? I1 Cd1 3.2470(7) . ? Cd1 N1 2.241(7) 5_556 ? Cd1 N1 2.241(7) . ? Cd1 N2 2.406(7) . ? Cd1 N2 2.406(7) 5_556 ? Cd1 I1 3.2470(7) 5_556 ? N1 C1 1.45(2) . ? N2 C2 1.460(13) . ? N2 C3 1.474(12) . ? C1 C2 1.26(2) . ? C3 C4 1.512(13) . ? C4 C5 1.529(14) . ? C5 O 1.410(13) . ? 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 I2 Cd2 I2 117.90(4) 2 . ? I2 Cd2 I1 106.76(2) 2 2 ? I2 Cd2 I1 110.17(2) . 2 ? I2 Cd2 I1 110.17(2) 2 . ? I2 Cd2 I1 106.76(2) . . ? I1 Cd2 I1 104.28(4) 2 . ? Cd2 I1 Cd1 106.50(2) . . ? N1 Cd1 N1 180.0 5_556 . ? N1 Cd1 N2 102.2(3) 5_556 . ? N1 Cd1 N2 77.8(3) . . ? N1 Cd1 N2 77.8(3) 5_556 5_556 ? N1 Cd1 N2 102.2(3) . 5_556 ? N2 Cd1 N2 180.0 . 5_556 ? N1 Cd1 I1 92.3(2) 5_556 5_556 ? N1 Cd1 I1 87.7(2) . 5_556 ? N2 Cd1 I1 90.4(2) . 5_556 ? N2 Cd1 I1 89.6(2) 5_556 5_556 ? N1 Cd1 I1 87.7(2) 5_556 . ? N1 Cd1 I1 92.3(2) . . ? N2 Cd1 I1 89.6(2) . . ? N2 Cd1 I1 90.4(2) 5_556 . ? I1 Cd1 I1 180.0 5_556 . ? C1 N1 Cd1 107.1(7) . . ? C2 N2 C3 116.3(10) . . ? C2 N2 Cd1 104.1(6) . . ? C3 N2 Cd1 113.7(5) . . ? C2 C1 N1 126.9(13) . . ? C1 C2 N2 121.0(12) . . ? N2 C3 C4 116.3(8) . . ? C3 C4 C5 114.8(10) . . ? O C5 C4 111.7(10) . . ? _diffrn_measured_fraction_theta_max 1.00 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.00 _refine_diff_density_max 0.751 _refine_diff_density_min -0.666 _refine_diff_density_rms 0.151 # END