# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 182/1438 # Paper ref. 9/07681F # # # # #============================================================================== data_global #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author ; Prof. A. Guy Orpen, School of Chemistry, Cantocks Close, University of Bristol. Bristol. BS8 1TS. ; _publ_contact_author_phone '0117 928 7648' _publ_contact_author_fax '0117 929 0509' _publ_contact_author_email Guy.Orpen@bris.ac.uk _publ_requested_journal 'Journal Chem. Soc.,Chem. Commun.' _publ_requested_coeditor_name ? _publ_contact_letter ; ; #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Cation-controlled formation of [{MCl4}n]2n- chains in [4,4'-bipyH2][MCl4] (M = Mn, Cd): an alternative to the A2MCl4 <100> layer perovskite structure. ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Gillon, Amy L.' ; School of Chemistry University of Bristol Cantocks Close BS8 1TS. Bristol, UK ; 'Orpen, A. Guy' ; School of Chemistry University of Bristol Cantocks Close BS8 1TS. Bristol, UK ; 'Starbuck, Jonathan' ; School of Chemistry University of Bristol Cantocks Close BS8 1TS. Bristol, UK ; 'Wang, Xi-Meng' ; School of Chemistry University of Bristol Cantocks Close BS8 1TS. Bristol, UK ; 'Rodriguez, Maria Y.' ; Departemento de Fisica Fundamental II Universidad de La Laguna 38204 La Laguna Spain ; 'Ruiz, Catalina' ; Departemento de Fisica Fundamental II Unioversidad de La Laguna 38204 La Laguna Spain ; #============================================================================== # 4. TEXT # # # # data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H10 Cl4 N2 Zn' _chemical_formula_weight 365.37 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 7.6507(12) _cell_length_b 19.765(4) _cell_length_c 9.5012(18) _cell_angle_alpha 90.00 _cell_angle_beta 108.826(15) _cell_angle_gamma 90.00 _cell_volume 1359.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 101 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.785 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 2.569 _exptl_absorpt_correction_type 'SADABS (Sheldrick, 1997)' _exptl_absorpt_correction_T_min 0.711925 _exptl_absorpt_correction_T_max 0.831103 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8553 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_sigmaI/netI 0.0471 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3112 _reflns_number_gt 2264 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SMART (Siemens, 1995b)' _computing_data_reduction 'SMART (Siemens, 1995b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Siemens, 1995a)' _computing_publication_material 'SHELXTL (Siemens, 1995a)' _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^)+(0.0251P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0024(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3112 _refine_ls_number_parameters 155 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0480 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0554 _refine_ls_wR_factor_gt 0.0510 _refine_ls_goodness_of_fit_ref 0.917 _refine_ls_restrained_S_all 0.917 _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 Zn1 Zn 0.39824(4) 0.628954(13) 0.29363(3) 0.02167(9) Uani 1 1 d . . . Cl1 Cl 0.47256(9) 0.72941(3) 0.20623(7) 0.02994(16) Uani 1 1 d . . . Cl2 Cl 0.62824(9) 0.59625(3) 0.50546(6) 0.02808(15) Uani 1 1 d . . . Cl3 Cl 0.12533(8) 0.63731(3) 0.33515(7) 0.02930(15) Uani 1 1 d . . . Cl4 Cl 0.38560(9) 0.54926(3) 0.12083(7) 0.02766(15) Uani 1 1 d . . . N1 N 0.7538(3) 0.70262(12) 0.0366(2) 0.0336(5) Uani 1 1 d . . . H1A H 0.6858 0.7230 0.0830 0.040 Uiso 1 1 calc R . . N2 N 1.2798(3) 0.54215(11) -0.3398(2) 0.0293(5) Uani 1 1 d . . . H2A H 1.3482 0.5216 -0.3856 0.035 Uiso 1 1 calc R . . C1 C 0.7317(4) 0.63706(15) 0.0096(3) 0.0404(7) Uani 1 1 d . . . H1B H 0.6454 0.6125 0.0425 0.048 Uiso 1 1 calc R . . C2 C 0.8325(4) 0.60406(14) -0.0655(3) 0.0365(7) Uani 1 1 d . . . H2B H 0.8143 0.5571 -0.0860 0.044 Uiso 1 1 calc R . . C3 C 0.9611(3) 0.63967(11) -0.1114(2) 0.0213(5) Uani 1 1 d . . . C4 C 0.9824(4) 0.70806(12) -0.0776(3) 0.0299(6) Uani 1 1 d . . . H4A H 1.0711 0.7338 -0.1052 0.036 Uiso 1 1 calc R . . C5 C 0.8757(4) 0.73866(14) -0.0043(3) 0.0364(7) Uani 1 1 d . . . H5A H 0.8891 0.7857 0.0173 0.044 Uiso 1 1 calc R . . C6 C 1.1445(4) 0.50741(13) -0.3127(3) 0.0295(6) Uani 1 1 d . . . H6A H 1.1229 0.4615 -0.3431 0.035 Uiso 1 1 calc R . . C7 C 1.0373(3) 0.53814(12) -0.2411(3) 0.0261(6) Uani 1 1 d . . . H7A H 0.9393 0.5139 -0.2235 0.031 Uiso 1 1 calc R . . C8 C 1.0714(3) 0.60495(11) -0.1939(2) 0.0198(5) Uani 1 1 d . . . C9 C 1.2130(3) 0.63900(12) -0.2261(3) 0.0281(6) Uani 1 1 d . . . H9A H 1.2389 0.6848 -0.1968 0.034 Uiso 1 1 calc R . . C10 C 1.3152(4) 0.60621(13) -0.3006(3) 0.0321(6) Uani 1 1 d . . . H10A H 1.4111 0.6295 -0.3238 0.039 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 Zn1 0.02235(16) 0.02005(15) 0.02354(15) 0.00015(12) 0.00871(12) 0.00087(12) Cl1 0.0374(4) 0.0194(3) 0.0418(4) 0.0008(3) 0.0249(3) 0.0008(3) Cl2 0.0246(3) 0.0373(4) 0.0224(3) -0.0002(3) 0.0076(3) 0.0078(3) Cl3 0.0223(3) 0.0313(3) 0.0366(3) 0.0021(3) 0.0126(3) 0.0025(3) Cl4 0.0346(4) 0.0209(3) 0.0256(3) -0.0036(2) 0.0070(3) -0.0013(3) N1 0.0271(13) 0.0520(15) 0.0238(11) -0.0043(10) 0.0110(10) 0.0102(11) N2 0.0297(13) 0.0350(13) 0.0271(11) -0.0005(10) 0.0144(10) 0.0112(10) C1 0.0374(17) 0.053(2) 0.0401(16) -0.0041(14) 0.0260(15) -0.0110(14) C2 0.0416(18) 0.0339(15) 0.0431(17) -0.0061(13) 0.0264(15) -0.0118(13) C3 0.0212(13) 0.0234(13) 0.0191(12) 0.0018(10) 0.0064(10) -0.0002(10) C4 0.0308(15) 0.0253(13) 0.0382(15) -0.0023(11) 0.0176(13) -0.0021(11) C5 0.0395(17) 0.0318(16) 0.0412(16) -0.0058(13) 0.0175(14) 0.0031(13) C6 0.0326(16) 0.0229(13) 0.0305(14) -0.0017(11) 0.0064(12) 0.0042(11) C7 0.0257(14) 0.0223(13) 0.0302(14) -0.0011(11) 0.0088(12) -0.0017(10) C8 0.0197(13) 0.0199(12) 0.0193(12) 0.0029(10) 0.0057(10) 0.0010(10) C9 0.0344(15) 0.0229(14) 0.0324(14) 0.0002(11) 0.0180(12) -0.0022(11) C10 0.0326(16) 0.0343(15) 0.0363(15) 0.0028(12) 0.0208(13) 0.0004(12) _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 Zn1 Cl3 2.2526(7) . ? Zn1 Cl4 2.2546(7) . ? Zn1 Cl1 2.2934(7) . ? Zn1 Cl2 2.2977(8) . ? N1 C1 1.321(3) . ? N1 C5 1.327(3) . ? N2 C10 1.323(3) . ? N2 C6 1.335(3) . ? C1 C2 1.372(4) . ? C2 C3 1.389(3) . ? C3 C4 1.387(3) . ? C3 C8 1.492(3) . ? C4 C5 1.373(3) . ? C6 C7 1.366(3) . ? C7 C8 1.392(3) . ? C8 C9 1.391(3) . ? C9 C10 1.375(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl3 Zn1 Cl4 110.76(3) . . ? Cl3 Zn1 Cl1 110.61(3) . . ? Cl4 Zn1 Cl1 107.37(3) . . ? Cl3 Zn1 Cl2 111.00(3) . . ? Cl4 Zn1 Cl2 106.39(3) . . ? Cl1 Zn1 Cl2 110.58(3) . . ? C1 N1 C5 121.8(2) . . ? C10 N2 C6 122.6(2) . . ? N1 C1 C2 120.6(2) . . ? C1 C2 C3 119.7(3) . . ? C4 C3 C2 117.6(2) . . ? C4 C3 C8 121.7(2) . . ? C2 C3 C8 120.7(2) . . ? C5 C4 C3 120.1(2) . . ? N1 C5 C4 120.1(3) . . ? N2 C6 C7 119.7(2) . . ? C6 C7 C8 120.2(2) . . ? C9 C8 C7 117.8(2) . . ? C9 C8 C3 120.4(2) . . ? C7 C8 C3 121.8(2) . . ? C10 C9 C8 119.9(2) . . ? N2 C10 C9 119.8(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.492 _refine_diff_density_min -0.411 _refine_diff_density_rms 0.074 data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H5 Cl2 Mn0.50 N' _chemical_formula_weight 177.47 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 '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 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 15.526(2) _cell_length_b 12.660(3) _cell_length_c 6.914(2) _cell_angle_alpha 90.00 _cell_angle_beta 114.896(16) _cell_angle_gamma 90.00 _cell_volume 1232.6(5) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 74 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description column _exptl_crystal_colour orange _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.913 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 708 _exptl_absorpt_coefficient_mu 1.912 _exptl_absorpt_correction_type 'SADABS (Sheldrick, 1997)' _exptl_absorpt_correction_T_min 0.530558 _exptl_absorpt_correction_T_max 0.745554 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3826 _diffrn_reflns_av_R_equivalents 0.0189 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1389 _reflns_number_gt 1237 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SMART (Siemens, 1995b)' _computing_data_reduction 'SMART (Siemens, 1995b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Siemens, 1995a)' _computing_publication_material 'SHELXTL (Siemens, 1995a)' _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^)+(0.0319P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0032(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1389 _refine_ls_number_parameters 79 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0233 _refine_ls_R_factor_gt 0.0199 _refine_ls_wR_factor_ref 0.0513 _refine_ls_wR_factor_gt 0.0505 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.974 _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 Mn1 Mn 0.0000 0.41970(2) 0.2500 0.01199(10) Uani 1 2 d S . . Cl1 Cl -0.11234(3) 0.28441(3) 0.01725(6) 0.01707(11) Uani 1 1 d . . . Cl2 Cl 0.09967(2) 0.43883(3) 0.02453(5) 0.01311(10) Uani 1 1 d . . . N1 N -0.26862(9) 0.41709(10) -0.3572(2) 0.0170(3) Uani 1 1 d . . . H1A H -0.2094 0.4154 -0.2609 0.020 Uiso 1 1 calc R . . C1 C -0.30527(11) 0.50934(13) -0.4509(2) 0.0176(3) Uani 1 1 d . . . H1B H -0.2677 0.5717 -0.4115 0.021 Uiso 1 1 calc R . . C2 C -0.39697(11) 0.51366(12) -0.6036(2) 0.0146(3) Uani 1 1 d . . . H2A H -0.4237 0.5792 -0.6677 0.018 Uiso 1 1 calc R . . C3 C -0.45100(11) 0.42107(11) -0.6646(2) 0.0122(3) Uani 1 1 d . . . C4 C -0.41073(11) 0.32731(12) -0.5597(2) 0.0163(3) Uani 1 1 d . . . H4A H -0.4465 0.2637 -0.5950 0.020 Uiso 1 1 calc R . . C5 C -0.31893(11) 0.32737(12) -0.4049(3) 0.0178(3) Uani 1 1 d . . . H5A H -0.2913 0.2639 -0.3321 0.021 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 Mn1 0.01169(18) 0.01089(17) 0.01223(18) 0.000 0.00390(13) 0.000 Cl1 0.01602(19) 0.01260(19) 0.0176(2) -0.00044(13) 0.00219(15) -0.00216(13) Cl2 0.01300(19) 0.01145(18) 0.01478(19) 0.00067(12) 0.00574(15) 0.00024(12) N1 0.0102(7) 0.0262(7) 0.0136(7) -0.0013(5) 0.0039(6) 0.0001(5) C1 0.0194(8) 0.0194(8) 0.0157(7) -0.0024(6) 0.0091(7) -0.0062(6) C2 0.0182(8) 0.0136(7) 0.0134(7) -0.0004(6) 0.0080(6) -0.0022(6) C3 0.0135(8) 0.0131(7) 0.0117(7) -0.0012(5) 0.0070(6) -0.0001(6) C4 0.0164(8) 0.0132(7) 0.0185(8) -0.0001(6) 0.0066(6) -0.0005(6) C5 0.0184(8) 0.0178(8) 0.0173(8) 0.0018(6) 0.0074(6) 0.0040(6) _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 Mn1 Cl1 2.4904(6) 2 ? Mn1 Cl1 2.4904(6) . ? Mn1 Cl2 2.5946(7) 5_565 ? Mn1 Cl2 2.5947(6) 6_566 ? Mn1 Cl2 2.6294(6) 2 ? Mn1 Cl2 2.6294(6) . ? Cl2 Mn1 2.5946(7) 5_565 ? N1 C5 1.339(2) . ? N1 C1 1.340(2) . ? C1 C2 1.371(2) . ? C2 C3 1.399(2) . ? C3 C4 1.394(2) . ? C3 C3 1.482(3) 2_453 ? C4 C5 1.376(2) . ? 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 Cl1 Mn1 Cl1 93.09(3) 2 . ? Cl1 Mn1 Cl2 170.827(12) 2 5_565 ? Cl1 Mn1 Cl2 87.84(2) . 5_565 ? Cl1 Mn1 Cl2 87.84(2) 2 6_566 ? Cl1 Mn1 Cl2 170.829(12) . 6_566 ? Cl2 Mn1 Cl2 92.69(3) 5_565 6_566 ? Cl1 Mn1 Cl2 96.151(19) 2 2 ? Cl1 Mn1 Cl2 91.119(18) . 2 ? Cl2 Mn1 Cl2 92.953(19) 5_565 2 ? Cl2 Mn1 Cl2 79.711(19) 6_566 2 ? Cl1 Mn1 Cl2 91.119(19) 2 . ? Cl1 Mn1 Cl2 96.152(19) . . ? Cl2 Mn1 Cl2 79.709(19) 5_565 . ? Cl2 Mn1 Cl2 92.950(19) 6_566 . ? Cl2 Mn1 Cl2 169.43(2) 2 . ? Mn1 Cl2 Mn1 100.292(19) 5_565 . ? C5 N1 C1 122.36(14) . . ? N1 C1 C2 119.93(14) . . ? C1 C2 C3 119.68(15) . . ? C4 C3 C2 118.42(14) . . ? C4 C3 C3 119.97(9) . 2_453 ? C2 C3 C3 121.61(9) . 2_453 ? C5 C4 C3 119.67(14) . . ? N1 C5 C4 119.87(14) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.373 _refine_diff_density_min -0.243 _refine_diff_density_rms 0.063 data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H10 Cd Cl4 N2' _chemical_formula_weight 412.40 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' 'N' 'N' 0.0061 0.0033 '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 C2/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 15.612(3) _cell_length_b 12.746(2) _cell_length_c 7.0261(12) _cell_angle_alpha 90.00 _cell_angle_beta 114.984(3) _cell_angle_gamma 90.00 _cell_volume 1267.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 106 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour cream _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.162 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 800 _exptl_absorpt_coefficient_mu 2.542 _exptl_absorpt_correction_type 'SADABS (Sheldrick, 1997)' _exptl_absorpt_correction_T_min 0.465552 _exptl_absorpt_correction_T_max 0.694163 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 diffracrometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6367 _diffrn_reflns_av_R_equivalents 0.0509 _diffrn_reflns_av_sigmaI/netI 0.0432 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 27.45 _reflns_number_total 1448 _reflns_number_gt 1259 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SMART (Siemens, 1995b)' _computing_data_reduction 'SMART (Siemens, 1995b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Siemens, 1995a)' _computing_publication_material 'SHELXTL (Siemens, 1995a)' _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^)+(0.0215P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0044(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1448 _refine_ls_number_parameters 79 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0267 _refine_ls_R_factor_gt 0.0245 _refine_ls_wR_factor_ref 0.0587 _refine_ls_wR_factor_gt 0.0584 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 0.0000 0.41743(2) 0.2500 0.01501(12) Uani 1 2 d S . . Cl1 Cl -0.11524(5) 0.27929(6) 0.00967(11) 0.01841(17) Uani 1 1 d . . . Cl2 Cl 0.10370(5) 0.43840(5) 0.02646(11) 0.01587(17) Uani 1 1 d . . . N1 N -0.27105(18) 0.4155(2) -0.3578(4) 0.0205(6) Uani 1 1 d . . . H1A H -0.2124 0.4139 -0.2612 0.025 Uiso 1 1 calc R . . C1 C -0.3066(2) 0.5071(2) -0.4519(5) 0.0206(7) Uani 1 1 d . . . H1B H -0.2690 0.5688 -0.4125 0.025 Uiso 1 1 calc R . . C2 C -0.3972(2) 0.5114(2) -0.6052(5) 0.0177(6) Uani 1 1 d . . . H2A H -0.4232 0.5763 -0.6705 0.021 Uiso 1 1 calc R . . C3 C -0.4513(2) 0.4193(2) -0.6650(4) 0.0155(6) Uani 1 1 d . . . C4 C -0.4116(2) 0.3261(2) -0.5594(5) 0.0190(6) Uani 1 1 d . . . H4A H -0.4471 0.2629 -0.5948 0.023 Uiso 1 1 calc R . . C5 C -0.3210(2) 0.3264(2) -0.4045(5) 0.0208(7) Uani 1 1 d . . . H5A H -0.2940 0.2637 -0.3308 0.025 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 Cd1 0.01458(18) 0.01558(18) 0.01348(18) 0.000 0.00456(12) 0.000 Cl1 0.0171(4) 0.0151(4) 0.0171(4) -0.0002(3) 0.0014(3) -0.0024(3) Cl2 0.0157(3) 0.0153(4) 0.0165(4) 0.0010(3) 0.0066(3) 0.0005(3) N1 0.0155(13) 0.0297(15) 0.0153(13) -0.0018(11) 0.0056(10) -0.0005(11) C1 0.0217(15) 0.0238(17) 0.0183(16) -0.0019(12) 0.0103(13) -0.0054(13) C2 0.0211(15) 0.0162(15) 0.0162(15) -0.0009(11) 0.0081(13) -0.0031(12) C3 0.0197(15) 0.0147(15) 0.0134(15) 0.0006(11) 0.0083(12) 0.0024(12) C4 0.0196(15) 0.0169(16) 0.0191(16) 0.0013(12) 0.0069(13) 0.0015(12) C5 0.0219(15) 0.0211(17) 0.0191(16) 0.0018(12) 0.0085(13) 0.0024(13) _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 Cl1 2.5733(8) . ? Cd1 Cl1 2.5733(8) 2 ? Cd1 Cl2 2.6672(8) 5_565 ? Cd1 Cl2 2.6673(8) 6_566 ? Cd1 Cl2 2.7031(7) 2 ? Cd1 Cl2 2.7032(7) . ? Cl2 Cd1 2.6673(8) 5_565 ? N1 C5 1.337(4) . ? N1 C1 1.341(4) . ? C1 C2 1.370(4) . ? C2 C3 1.402(4) . ? C3 C4 1.399(4) . ? C3 C3 1.484(6) 2_453 ? C4 C5 1.372(4) . ? 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 Cl1 Cd1 Cl1 93.65(4) . 2 ? Cl1 Cd1 Cl2 87.27(2) . 5_565 ? Cl1 Cd1 Cl2 172.03(2) 2 5_565 ? Cl1 Cd1 Cl2 172.03(2) . 6_566 ? Cl1 Cd1 Cl2 87.27(2) 2 6_566 ? Cl2 Cd1 Cl2 92.91(3) 5_565 6_566 ? Cl1 Cd1 Cl2 91.41(2) . 2 ? Cl1 Cd1 Cl2 96.35(2) 2 2 ? Cl2 Cd1 Cl2 91.54(2) 5_565 2 ? Cl2 Cd1 Cl2 80.62(2) 6_566 2 ? Cl1 Cd1 Cl2 96.35(3) . . ? Cl1 Cd1 Cl2 91.41(2) 2 . ? Cl2 Cd1 Cl2 80.62(2) 5_565 . ? Cl2 Cd1 Cl2 91.53(2) 6_566 . ? Cl2 Cd1 Cl2 168.65(3) 2 . ? Cd1 Cl2 Cd1 99.38(2) 5_565 . ? C5 N1 C1 122.7(3) . . ? N1 C1 C2 119.8(3) . . ? C1 C2 C3 119.6(3) . . ? C4 C3 C2 118.4(3) . . ? C4 C3 C3 120.06(19) . 2_453 ? C2 C3 C3 121.57(18) . 2_453 ? C5 C4 C3 119.7(3) . . ? N1 C5 C4 119.7(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.745 _refine_diff_density_min -0.987 _refine_diff_density_rms 0.118