Electronic Supplementary Material for CrystEngComm This Journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email ullrich.englert@ac.rwth-aachen.de _publ_contact_author_name 'Ulli Englert' _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _audit_creation_date 30-OCT-03 _audit_creation_method SHELXTL _audit_update_record ; ? ; _publ_contact_author_address ; Institut fur Anorganische Chemie RWTH Aachen Prof.-Pirlet-Str.1 52074 Aachen Germany ; _publ_contact_author_fax 0049-241-8092288 _publ_contact_author_phone 0049-241-8094666 _publ_section_title ; Structural trends in one and two dimensional coordination polymers of cadmium(II) ; _publ_section_exptl_refinement ; All H atoms were introduced in idealized positions (C---H 0.98 \%A) and included as riding with U~iso~(H) = 1.3U~eq~(non-H). ; _publ_section_references ; Bruker (1999). SAINT+. Version 6.02. Bruker AXS Inc., Madison, WI, USA. Bruker (2001). SMART. Version 5.624. Bruker AXS Inc., Madison, WI, USA. Sheldrick, G. M. (1996). SADABS. Version 2.03. University of Gottingen, Germany. Sheldrick, G. M. (1998). SHELXTL. Version 5.1. Bruker AXS Inc., Madison, WI, USA. Spek A. L. (2003). J. App. Cryst. 36, 7. ; _publ_section_acknowledgements ; Support from DFG is gratefully acknowledged. ; loop_ _publ_author_name _publ_author_address 'Chunhua Hu' ; Institut fuer Anorganische Chemie RWTH Aachen Prof.-Pirlet-Str. 1 52074 Aachen Germany ; 'Li Qi' ; Department of Chemistry Beijing Normal University Xinjiekouwai Street 19 Beijing 100875 China ; 'Ulli Englert' ; Institut fuer Anorganische Chemie RWTH Aachen Prof.-Pirlet-Str. 1 52074 Aachen Germany ; #============================================================================== data_hc135 _database_code_depnum_ccdc_archive 'CCDC 223783' _chemical_name_common 'catena-(bis(mu-chloro)-bis(pyridine)-cadmium(ii)) (Compound 1)' _audit_creation_date 30-OCT-03 _audit_creation_method SHELXTL _audit_update_record ; ? ; _chemical_name_systematic ; catena-[bis(\m-chloro)-bis(pyridine)-cadmium(ii)] (Compound 1) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H10 Cd Cl2 N2' _chemical_formula_weight 341.50 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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 3.8233(7) _cell_length_b 8.6525(15) _cell_length_c 17.748(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.562(4) _cell_angle_gamma 90.00 _cell_volume 586.91(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7842 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 28.29 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.932 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 332 _exptl_absorpt_coefficient_mu 2.282 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.875010 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (1996)' _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 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7842 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 28.29 _reflns_number_total 1457 _reflns_number_gt 1252 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXTL (Sheldrick, 1998)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL (Sheldrick, 1998)' _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^)+(0.0244P)^2^+0.0534P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1457 _refine_ls_number_parameters 70 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0274 _refine_ls_R_factor_gt 0.0219 _refine_ls_wR_factor_ref 0.0496 _refine_ls_wR_factor_gt 0.0483 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 Cd Cd 0.0000 0.0000 0.0000 0.03077(8) Uani 1 2 d S . . Cl Cl 0.50928(14) -0.13917(6) 0.07810(3) 0.03513(13) Uani 1 1 d . . . N N 0.0236(5) 0.2025(2) 0.08786(10) 0.0348(4) Uani 1 1 d . . . C1 C -0.0559(6) 0.1765(3) 0.15949(13) 0.0425(6) Uani 1 1 d . . . H1 H -0.1296 0.0724 0.1739 0.055 Uiso 1 1 calc R . . C2 C -0.0389(7) 0.2888(3) 0.21365(14) 0.0528(7) Uani 1 1 d . . . H2 H -0.0997 0.2652 0.2657 0.069 Uiso 1 1 calc R . . C3 C 0.0637(8) 0.4341(4) 0.19437(17) 0.0565(7) Uani 1 1 d . . . H3 H 0.0792 0.5161 0.2324 0.074 Uiso 1 1 calc R . . C4 C 0.1452(8) 0.4636(3) 0.1207(2) 0.0566(8) Uani 1 1 d . . . H4 H 0.2168 0.5673 0.1051 0.074 Uiso 1 1 calc R . . C5 C 0.1240(6) 0.3447(3) 0.06963(14) 0.0455(6) Uani 1 1 d . . . H5 H 0.1857 0.3654 0.0174 0.059 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 0.03438(13) 0.02925(12) 0.02873(12) -0.00246(9) 0.00191(8) -0.00441(9) Cl 0.0371(3) 0.0352(3) 0.0331(3) 0.0063(2) 0.0017(2) -0.0047(2) N 0.0393(10) 0.0307(10) 0.0344(10) -0.0032(8) 0.0003(8) -0.0022(8) C1 0.0498(14) 0.0430(14) 0.0345(12) -0.0018(10) 0.0007(10) -0.0045(11) C2 0.0567(16) 0.0641(18) 0.0376(13) -0.0125(13) 0.0039(12) -0.0030(14) C3 0.0518(16) 0.0524(16) 0.0654(18) -0.0297(15) 0.0001(14) -0.0020(14) C4 0.0596(18) 0.0319(13) 0.078(2) -0.0097(13) 0.0039(15) -0.0067(12) C5 0.0535(15) 0.0351(13) 0.0481(14) 0.0004(11) 0.0052(12) -0.0033(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd N 2.3456(18) 3 ? Cd N 2.3456(18) . ? Cd Cl 2.6487(6) 3 ? Cd Cl 2.6487(6) . ? Cd Cl 2.6520(6) 3_655 ? Cd Cl 2.6520(6) 1_455 ? Cl Cd 2.6520(6) 1_655 ? N C5 1.331(3) . ? N C1 1.334(3) . ? C1 C2 1.367(3) . ? C1 H1 0.9800 . ? C2 C3 1.363(4) . ? C2 H2 0.9800 . ? C3 C4 1.376(4) . ? C3 H3 0.9800 . ? C4 C5 1.372(4) . ? C4 H4 0.9800 . ? C5 H5 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N Cd N 180.00(13) 3 . ? N Cd Cl 88.70(5) 3 3 ? N Cd Cl 91.30(5) . 3 ? N Cd Cl 91.30(5) 3 . ? N Cd Cl 88.70(5) . . ? Cl Cd Cl 180.00(3) 3 . ? N Cd Cl 90.38(5) 3 3_655 ? N Cd Cl 89.62(5) . 3_655 ? Cl Cd Cl 92.32(2) 3 3_655 ? Cl Cd Cl 87.68(2) . 3_655 ? N Cd Cl 89.62(5) 3 1_455 ? N Cd Cl 90.38(5) . 1_455 ? Cl Cd Cl 87.68(2) 3 1_455 ? Cl Cd Cl 92.32(2) . 1_455 ? Cl Cd Cl 180.00(3) 3_655 1_455 ? Cd Cl Cd 92.32(2) . 1_655 ? C5 N C1 117.5(2) . . ? C5 N Cd 122.33(15) . . ? C1 N Cd 120.12(15) . . ? N C1 C2 122.8(2) . . ? N C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C2 C1 119.2(3) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C2 C3 C4 119.0(3) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C5 C4 C3 118.5(3) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? N C5 C4 123.0(2) . . ? N C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.531 _refine_diff_density_min -0.311 _refine_diff_density_rms 0.068 #============================================================================== data_hc200 _database_code_depnum_ccdc_archive 'CCDC 223784' _chemical_name_common 'catena-(bis(mu-bromo)-bis(pyridine)-cadmium(ii)) (Compound 2)' _audit_creation_date 30-OCT-03 _audit_creation_method SHELXTL _audit_update_record ; ? ; _chemical_name_systematic ; catena-[bis(\m-bromo)-bis(pyridine)-cadmium(ii)] (Compound 2) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H10 Br2 Cd N2' _chemical_formula_weight 430.42 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' 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnnm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, z-1/2' _cell_length_a 8.649(3) _cell_length_b 18.159(7) _cell_length_c 3.9182(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 615.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7049 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 28.29 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.76 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.323 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 404 _exptl_absorpt_coefficient_mu 8.236 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.425219 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (1996)' _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 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7049 _diffrn_reflns_av_R_equivalents 0.0541 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 28.29 _reflns_number_total 878 _reflns_number_gt 720 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXTL (Sheldrick, 1998)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL (Sheldrick, 1998)' _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^)+(0.0361P)^2^+1.2165P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 878 _refine_ls_number_parameters 47 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.0853 _refine_ls_wR_factor_gt 0.0816 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.111 _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 Cd Cd 0.0000 0.0000 0.0000 0.0330(2) Uani 1 4 d S . . Br Br -0.16073(8) 0.07548(3) -0.5000 0.0375(2) Uani 1 2 d S . . N N -0.1876(7) -0.0914(3) 0.0000 0.0400(13) Uani 1 2 d S . . C1 C -0.1471(9) -0.1609(4) 0.0000 0.053(2) Uani 1 2 d S . . H1 H -0.0367 -0.1732 0.0000 0.069 Uiso 1 2 calc SR . . C2 C -0.2531(10) -0.2176(5) 0.0000 0.068(3) Uani 1 2 d S . . H2 H -0.2191 -0.2691 0.0000 0.088 Uiso 1 2 calc SR . . C3 C -0.4044(11) -0.2005(5) 0.0000 0.068(2) Uani 1 2 d S . . H3 H -0.4829 -0.2395 0.0000 0.088 Uiso 1 2 calc SR . . C4 C -0.4458(10) -0.1305(6) 0.0000 0.078(3) Uani 1 2 d S . . H4 H -0.5556 -0.1171 0.0000 0.101 Uiso 1 2 calc SR . . C5 C -0.3369(9) -0.0775(4) 0.0000 0.065(3) Uani 1 2 d S . . H5 H -0.3705 -0.0260 0.0000 0.084 Uiso 1 2 calc SR . . 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 0.0338(3) 0.0332(3) 0.0320(4) 0.000 0.000 -0.0017(3) Br 0.0392(4) 0.0408(4) 0.0325(4) 0.000 0.000 0.0090(3) N 0.039(3) 0.038(3) 0.043(3) 0.000 0.000 -0.003(2) C1 0.046(4) 0.040(4) 0.072(6) 0.000 0.000 -0.001(3) C2 0.062(5) 0.041(4) 0.100(8) 0.000 0.000 -0.014(4) C3 0.070(6) 0.063(6) 0.070(6) 0.000 0.000 -0.027(5) C4 0.041(4) 0.078(6) 0.113(9) 0.000 0.000 -0.009(4) C5 0.040(4) 0.049(4) 0.105(8) 0.000 0.000 0.005(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 Cd N 2.321(5) . ? Cd N 2.321(5) 5 ? Cd Br 2.7657(7) 5 ? Cd Br 2.7657(7) 5_554 ? Cd Br 2.7657(7) . ? Cd Br 2.7657(7) 1_556 ? Br Cd 2.7657(7) 1_554 ? N C1 1.310(8) . ? N C5 1.315(9) . ? C1 C2 1.379(10) . ? C1 H1 0.9800 . ? C2 C3 1.345(13) . ? C2 H2 0.9800 . ? C3 C4 1.321(13) . ? C3 H3 0.9800 . ? C4 C5 1.346(11) . ? C4 H4 0.9800 . ? C5 H5 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N Cd N 180.00(18) . 5 ? N Cd Br 89.83(10) . 5 ? N Cd Br 90.17(10) 5 5 ? N Cd Br 89.83(10) . 5_554 ? N Cd Br 90.17(10) 5 5_554 ? Br Cd Br 90.20(3) 5 5_554 ? N Cd Br 90.17(10) . . ? N Cd Br 89.83(10) 5 . ? Br Cd Br 180.00(2) 5 . ? Br Cd Br 89.80(3) 5_554 . ? N Cd Br 90.17(10) . 1_556 ? N Cd Br 89.83(10) 5 1_556 ? Br Cd Br 89.80(3) 5 1_556 ? Br Cd Br 180.00(3) 5_554 1_556 ? Br Cd Br 90.20(3) . 1_556 ? Cd Br Cd 90.20(3) 1_554 . ? C1 N C5 116.5(6) . . ? C1 N Cd 120.1(5) . . ? C5 N Cd 123.3(5) . . ? N C1 C2 122.8(7) . . ? N C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C2 C1 118.3(8) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? C4 C3 C2 119.1(8) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 119.8(9) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? N C5 C4 123.4(8) . . ? N C5 H5 118.3 . . ? C4 C5 H5 118.3 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.695 _refine_diff_density_min -0.800 _refine_diff_density_rms 0.149 #============================================================================== data_hc202 _database_code_depnum_ccdc_archive 'CCDC 223785' _chemical_name_common ;(bis(iodo)-bis(pyridine)-cadmium(ii)) (Compound 3, RT dataset, 3a) ; _audit_creation_date 30-OCT-03 _audit_creation_method SHELXTL _audit_update_record ; ? ; _chemical_name_systematic ; [bis(iodo)-bis(pyridine)-cadmium(ii)] (Compound 3, RT dataset, 3a) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H10 Cd I2 N2' _chemical_formula_weight 524.40 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' 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 8.848(4) _cell_length_b 17.790(7) _cell_length_c 18.666(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2938(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 26277 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 26.24 _exptl_crystal_description plate _exptl_crystal_colour coluorless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.371 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 5.664 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.584846 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (1996)' _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 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 26277 _diffrn_reflns_av_R_equivalents 0.0637 _diffrn_reflns_av_sigmaI/netI 0.0429 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 26.24 _reflns_number_total 2939 _reflns_number_gt 1755 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXTL (Sheldrick, 1998)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL (Sheldrick, 1998)' _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^)+(0.0234P)^2^+6.6703P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2939 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0851 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.0886 _refine_ls_wR_factor_gt 0.0755 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 Cd Cd 0.34970(7) 0.14758(3) 0.38829(3) 0.0748(2) Uani 1 1 d . . . I1 I 0.23658(7) 0.06676(4) 0.49718(3) 0.0935(2) Uani 1 1 d . . . I2 I 0.23058(7) 0.26703(3) 0.32032(3) 0.0872(2) Uani 1 1 d . . . N1 N 0.4219(8) 0.0648(3) 0.3014(3) 0.0750(17) Uani 1 1 d . . . C1 C 0.4830(13) -0.0010(5) 0.3176(5) 0.107(3) Uani 1 1 d . . . H1 H 0.4945 -0.0144 0.3682 0.139 Uiso 1 1 calc R . . C2 C 0.5303(14) -0.0504(6) 0.2676(6) 0.126(4) Uani 1 1 d . . . H2 H 0.5741 -0.0987 0.2821 0.164 Uiso 1 1 calc R . . C3 C 0.5171(13) -0.0333(6) 0.1979(6) 0.116(3) Uani 1 1 d . . . H3 H 0.5480 -0.0690 0.1608 0.151 Uiso 1 1 calc R . . C4 C 0.4597(14) 0.0351(6) 0.1804(5) 0.116(3) Uani 1 1 d . . . H4 H 0.4515 0.0505 0.1302 0.151 Uiso 1 1 calc R . . C5 C 0.4143(11) 0.0812(5) 0.2334(5) 0.094(3) Uani 1 1 d . . . H5 H 0.3729 0.1303 0.2200 0.122 Uiso 1 1 calc R . . N2 N 0.5885(7) 0.1797(4) 0.4199(3) 0.0719(16) Uani 1 1 d . . . C6 C 0.6643(10) 0.1432(5) 0.4711(4) 0.083(2) Uani 1 1 d . . . H6 H 0.6097 0.1063 0.5003 0.108 Uiso 1 1 calc R . . C7 C 0.8114(11) 0.1545(6) 0.4848(5) 0.095(3) Uani 1 1 d . . . H7 H 0.8632 0.1248 0.5215 0.123 Uiso 1 1 calc R . . C8 C 0.8879(10) 0.2079(6) 0.4468(5) 0.091(3) Uani 1 1 d . . . H8 H 0.9951 0.2177 0.4561 0.119 Uiso 1 1 calc R . . C9 C 0.8129(11) 0.2466(5) 0.3964(6) 0.101(3) Uani 1 1 d . . . H9 H 0.8643 0.2860 0.3690 0.131 Uiso 1 1 calc R . . C10 C 0.6644(10) 0.2308(5) 0.3837(5) 0.087(2) Uani 1 1 d . . . H10 H 0.6119 0.2586 0.3458 0.113 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 0.0726(4) 0.0762(4) 0.0755(4) 0.0056(3) 0.0038(3) 0.0029(3) I1 0.0886(4) 0.1016(5) 0.0904(4) 0.0240(3) 0.0092(3) -0.0042(3) I2 0.0851(4) 0.0822(4) 0.0943(4) 0.0136(3) 0.0013(3) 0.0103(3) N1 0.089(5) 0.064(4) 0.073(4) 0.008(3) 0.006(3) 0.006(3) C1 0.143(10) 0.094(7) 0.085(6) 0.021(5) 0.025(6) 0.023(6) C2 0.179(12) 0.089(7) 0.110(8) 0.007(6) 0.021(8) 0.047(7) C3 0.137(10) 0.100(8) 0.111(8) -0.018(6) 0.014(7) 0.020(7) C4 0.154(10) 0.124(9) 0.070(6) -0.001(6) 0.006(6) 0.024(8) C5 0.121(8) 0.084(6) 0.076(6) 0.010(5) 0.000(5) 0.017(5) N2 0.060(4) 0.084(4) 0.071(4) 0.002(3) 0.007(3) 0.005(3) C6 0.075(6) 0.095(6) 0.080(5) 0.015(5) -0.001(5) 0.008(5) C7 0.079(7) 0.126(8) 0.079(6) 0.006(6) -0.009(5) 0.005(6) C8 0.067(6) 0.107(7) 0.100(7) -0.022(6) 0.009(5) 0.003(5) C9 0.076(7) 0.089(6) 0.137(8) 0.013(6) 0.014(6) -0.012(5) C10 0.073(6) 0.088(6) 0.099(6) 0.020(5) 0.018(5) 0.010(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 Cd N2 2.267(6) . ? Cd N1 2.281(6) . ? Cd I1 2.6833(10) . ? Cd I2 2.6901(11) . ? N1 C5 1.304(9) . ? N1 C1 1.325(10) . ? C1 C2 1.349(12) . ? C1 H1 0.9800 . ? C2 C3 1.340(12) . ? C2 H2 0.9800 . ? C3 C4 1.358(13) . ? C3 H3 0.9800 . ? C4 C5 1.347(11) . ? C4 H4 0.9800 . ? C5 H5 0.9800 . ? N2 C10 1.318(9) . ? N2 C6 1.336(9) . ? C6 C7 1.341(12) . ? C6 H6 0.9800 . ? C7 C8 1.364(12) . ? C7 H7 0.9800 . ? C8 C9 1.342(12) . ? C8 H8 0.9800 . ? C9 C10 1.365(12) . ? C9 H9 0.9800 . ? C10 H10 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cd N1 95.0(2) . . ? N2 Cd I1 106.57(16) . . ? N1 Cd I1 107.26(16) . . ? N2 Cd I2 106.81(17) . . ? N1 Cd I2 106.53(17) . . ? I1 Cd I2 129.37(3) . . ? C5 N1 C1 116.1(7) . . ? C5 N1 Cd 122.2(6) . . ? C1 N1 Cd 121.5(6) . . ? N1 C1 C2 123.0(9) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C3 C2 C1 119.7(9) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 118.1(9) . . ? C2 C3 H3 121.0 . . ? C4 C3 H3 121.0 . . ? C5 C4 C3 118.7(9) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? N1 C5 C4 124.3(8) . . ? N1 C5 H5 117.9 . . ? C4 C5 H5 117.9 . . ? C10 N2 C6 116.5(7) . . ? C10 N2 Cd 121.0(6) . . ? C6 N2 Cd 122.2(6) . . ? N2 C6 C7 123.4(8) . . ? N2 C6 H6 118.3 . . ? C7 C6 H6 118.3 . . ? C6 C7 C8 119.2(9) . . ? C6 C7 H7 120.4 . . ? C8 C7 H7 120.4 . . ? C9 C8 C7 118.4(9) . . ? C9 C8 H8 120.8 . . ? C7 C8 H8 120.8 . . ? C8 C9 C10 119.5(9) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? N2 C10 C9 122.9(9) . . ? N2 C10 H10 118.5 . . ? C9 C10 H10 118.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.24 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.628 _refine_diff_density_min -0.362 _refine_diff_density_rms 0.096 #============================================================================== data_hc201 _database_code_depnum_ccdc_archive 'CCDC 223786' _chemical_name_common ;(bis(iodo)-bis(pyridine)-cadmium(ii)) (Compound 3, 120K dataset, 3b) ; _audit_creation_date 30-OCT-03 _audit_creation_method SHELXTL _audit_update_record ; ? ; _chemical_name_systematic ; [bis(iodo)-bis(pyridine)-cadmium(ii)] (Compound 3, 120K dataset, 3b) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H10 Cd I2 N2' _chemical_formula_weight 524.40 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' 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 8.7603(19) _cell_length_b 17.436(4) _cell_length_c 18.581(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2838.1(11) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 29732 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 26.09 _exptl_crystal_description plate _exptl_crystal_colour coluorless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 5.863 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.603491 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 29732 _diffrn_reflns_av_R_equivalents 0.0452 _diffrn_reflns_av_sigmaI/netI 0.0234 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 26.09 _reflns_number_total 2816 _reflns_number_gt 2435 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXTL (Sheldrick, 1998)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL (Sheldrick, 1998)' _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^)+(0.0346P)^2^+12.5385P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2816 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0395 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0820 _refine_ls_wR_factor_gt 0.0788 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.138 _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 Cd Cd 0.34068(5) 0.14992(3) 0.38831(2) 0.03031(13) Uani 1 1 d . . . I1 I 0.23048(5) 0.06504(3) 0.49756(2) 0.03763(13) Uani 1 1 d . . . I2 I 0.22207(5) 0.27244(2) 0.31946(2) 0.03407(12) Uani 1 1 d . . . N1 N 0.4192(6) 0.0670(3) 0.3002(3) 0.0333(12) Uani 1 1 d . . . C1 C 0.4885(9) 0.0025(4) 0.3174(4) 0.0439(17) Uani 1 1 d . . . H1 H 0.5003 -0.0107 0.3684 0.057 Uiso 1 1 calc R . . C2 C 0.5447(10) -0.0471(4) 0.2663(4) 0.052(2) Uani 1 1 d . . . H2 H 0.5962 -0.0946 0.2806 0.067 Uiso 1 1 calc R . . C3 C 0.5276(9) -0.0290(4) 0.1950(4) 0.0464(17) Uani 1 1 d . . . H3 H 0.5662 -0.0636 0.1577 0.060 Uiso 1 1 calc R . . C4 C 0.4568(9) 0.0373(4) 0.1766(4) 0.0457(17) Uani 1 1 d . . . H4 H 0.4430 0.0514 0.1260 0.059 Uiso 1 1 calc R . . C5 C 0.4046(8) 0.0846(4) 0.2309(3) 0.0401(15) Uani 1 1 d . . . H5 H 0.3547 0.1329 0.2179 0.052 Uiso 1 1 calc R . . N2 N 0.5816(6) 0.1832(3) 0.4210(3) 0.0306(11) Uani 1 1 d . . . C6 C 0.6577(7) 0.1452(4) 0.4719(3) 0.0372(14) Uani 1 1 d . . . H6 H 0.6029 0.1070 0.5007 0.048 Uiso 1 1 calc R . . C7 C 0.8093(7) 0.1574(4) 0.4854(3) 0.0374(15) Uani 1 1 d . . . H7 H 0.8619 0.1281 0.5230 0.049 Uiso 1 1 calc R . . C8 C 0.8865(7) 0.2107(4) 0.4460(3) 0.0360(14) Uani 1 1 d . . . H8 H 0.9953 0.2201 0.4544 0.047 Uiso 1 1 calc R . . C9 C 0.8083(8) 0.2510(4) 0.3942(4) 0.0432(16) Uani 1 1 d . . . H9 H 0.8604 0.2905 0.3658 0.056 Uiso 1 1 calc R . . C10 C 0.6578(7) 0.2357(4) 0.3826(4) 0.0371(15) Uani 1 1 d . . . H10 H 0.6035 0.2641 0.3449 0.048 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 0.0277(2) 0.0304(2) 0.0328(2) 0.00138(18) 0.00202(18) 0.00071(18) I1 0.0331(2) 0.0407(2) 0.0392(2) 0.00894(18) 0.00276(17) -0.00310(18) I2 0.0309(2) 0.0317(2) 0.0396(2) 0.00419(17) 0.00100(17) 0.00233(17) N1 0.036(3) 0.030(3) 0.034(3) 0.000(2) 0.006(2) 0.001(2) C1 0.058(4) 0.037(4) 0.036(4) 0.006(3) 0.008(3) 0.012(3) C2 0.074(5) 0.036(4) 0.045(4) 0.008(3) 0.012(4) 0.019(4) C3 0.052(4) 0.042(4) 0.045(4) -0.005(3) 0.011(3) 0.001(3) C4 0.056(4) 0.045(4) 0.036(4) 0.002(3) -0.004(3) 0.007(4) C5 0.048(4) 0.036(3) 0.037(4) 0.000(3) -0.002(3) 0.006(3) N2 0.028(3) 0.034(3) 0.030(3) -0.002(2) 0.003(2) 0.004(2) C6 0.034(3) 0.041(4) 0.036(3) 0.002(3) 0.004(3) 0.001(3) C7 0.030(3) 0.050(4) 0.032(3) 0.003(3) -0.006(3) 0.005(3) C8 0.029(3) 0.036(3) 0.043(4) -0.011(3) 0.006(3) 0.004(3) C9 0.034(3) 0.039(4) 0.057(4) 0.001(3) 0.005(3) -0.006(3) C10 0.030(3) 0.036(4) 0.045(4) 0.005(3) 0.006(3) 0.002(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 2.272(5) . ? Cd N1 2.290(5) . ? Cd I1 2.6911(7) . ? Cd I2 2.6982(7) . ? N1 C1 1.317(8) . ? N1 C5 1.330(8) . ? C1 C2 1.375(10) . ? C1 H1 0.9800 . ? C2 C3 1.370(10) . ? C2 H2 0.9800 . ? C3 C4 1.356(10) . ? C3 H3 0.9800 . ? C4 C5 1.381(9) . ? C4 H4 0.9800 . ? C5 H5 0.9800 . ? N2 C6 1.333(8) . ? N2 C10 1.339(8) . ? C6 C7 1.369(9) . ? C6 H6 0.9800 . ? C7 C8 1.362(9) . ? C7 H7 0.9800 . ? C8 C9 1.375(10) . ? C8 H8 0.9800 . ? C9 C10 1.362(9) . ? C9 H9 0.9800 . ? C10 H10 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cd N1 94.20(18) . . ? N2 Cd I1 105.79(13) . . ? N1 Cd I1 107.43(13) . . ? N2 Cd I2 106.40(13) . . ? N1 Cd I2 106.08(13) . . ? I1 Cd I2 130.91(2) . . ? C1 N1 C5 118.4(6) . . ? C1 N1 Cd 120.3(4) . . ? C5 N1 Cd 121.1(4) . . ? N1 C1 C2 122.3(6) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C3 C2 C1 119.0(7) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C4 C3 C2 119.3(7) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 118.5(7) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? N1 C5 C4 122.5(6) . . ? N1 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? C6 N2 C10 118.0(6) . . ? C6 N2 Cd 121.8(4) . . ? C10 N2 Cd 119.7(4) . . ? N2 C6 C7 122.5(6) . . ? N2 C6 H6 118.7 . . ? C7 C6 H6 118.7 . . ? C8 C7 C6 119.3(6) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C7 C8 C9 118.5(6) . . ? C7 C8 H8 120.7 . . ? C9 C8 H8 120.7 . . ? C10 C9 C8 119.5(7) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? N2 C10 C9 122.1(6) . . ? N2 C10 H10 118.9 . . ? C9 C10 H10 118.9 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.09 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.594 _refine_diff_density_min -0.590 _refine_diff_density_rms 0.130 #============================================================================== data_hc172 _database_code_depnum_ccdc_archive 'CCDC 223787' _chemical_name_common ;catena-(bis(mu-chloro)-bis(3-chloropyridine)-cadmium(ii)) (Compound 4) ; _audit_creation_date 30-OCT-03 _audit_creation_method SHELXTL _audit_update_record ; ? ; _chemical_name_systematic ; catena-[bis(\m-chloro)-bis(3-chloropyridine)-cadmium(ii)] (Compound 4) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H8 Cd Cl4 N2' _chemical_formula_weight 410.38 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' 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 P21/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 3.8116(5) _cell_length_b 14.2606(19) _cell_length_c 11.9890(16) _cell_angle_alpha 90.00 _cell_angle_beta 91.767(4) _cell_angle_gamma 90.00 _cell_volume 651.36(15) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8491 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 28.33 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.092 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 396 _exptl_absorpt_coefficient_mu 2.472 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.678196 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (1996)' _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 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 8491 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_sigmaI/netI 0.0383 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 28.33 _reflns_number_total 1617 _reflns_number_gt 1440 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXTL (Sheldrick, 1998)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL (Sheldrick, 1998)' _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^)+(0.0451P)^2^+0.5506P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1617 _refine_ls_number_parameters 79 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0557 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1044 _refine_ls_wR_factor_gt 0.1006 _refine_ls_goodness_of_fit_ref 1.188 _refine_ls_restrained_S_all 1.188 _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 Cd Cd 0.0000 0.0000 0.0000 0.02712(16) Uani 1 2 d S . . Cl1 Cl -0.5127(3) -0.02950(8) -0.14855(10) 0.0298(3) Uani 1 1 d . . . Cl2 Cl 0.3197(4) 0.39706(9) 0.09810(14) 0.0509(4) Uani 1 1 d . . . N N 0.0076(10) 0.1618(3) -0.0472(3) 0.0279(8) Uani 1 1 d . . . C1 C 0.1393(12) 0.2250(3) 0.0255(4) 0.0295(10) Uani 1 1 d . . . H1 H 0.2293 0.2040 0.0987 0.038 Uiso 1 1 calc R . . C2 C 0.1505(13) 0.3191(3) -0.0012(4) 0.0343(11) Uani 1 1 d . . . C3 C 0.0244(15) 0.3507(4) -0.1038(5) 0.0406(12) Uani 1 1 d . . . H3 H 0.0301 0.4173 -0.1236 0.053 Uiso 1 1 calc R . . C4 C -0.1101(15) 0.2842(4) -0.1774(4) 0.0415(12) Uani 1 1 d . . . H4 H -0.2016 0.3029 -0.2514 0.054 Uiso 1 1 calc R . . C5 C -0.1142(14) 0.1919(4) -0.1457(4) 0.0358(11) Uani 1 1 d . . . H5 H -0.2121 0.1457 -0.1986 0.047 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 0.0244(3) 0.0236(2) 0.0331(3) -0.00029(18) -0.00352(18) -0.00007(18) Cl1 0.0274(6) 0.0317(5) 0.0300(6) -0.0029(4) -0.0038(4) 0.0007(4) Cl2 0.0535(9) 0.0338(7) 0.0652(10) -0.0119(6) -0.0034(7) -0.0038(6) N 0.031(2) 0.0234(19) 0.029(2) 0.0023(15) 0.0020(16) 0.0014(15) C1 0.029(2) 0.031(2) 0.029(2) 0.0021(18) 0.0015(19) 0.0026(19) C2 0.031(3) 0.029(3) 0.043(3) -0.005(2) 0.005(2) 0.000(2) C3 0.044(3) 0.030(3) 0.049(3) 0.012(2) 0.010(2) 0.009(2) C4 0.046(3) 0.043(3) 0.035(3) 0.010(2) 0.002(2) 0.008(2) C5 0.037(3) 0.039(3) 0.031(3) 0.002(2) -0.002(2) 0.003(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 Cd N 2.377(4) 3 ? Cd N 2.377(4) . ? Cd Cl1 2.6369(11) . ? Cd Cl1 2.6369(11) 3 ? Cd Cl1 2.6462(12) 1_655 ? Cd Cl1 2.6462(12) 3_455 ? Cl1 Cd 2.6462(12) 1_455 ? Cl2 C2 1.738(5) . ? N C5 1.326(6) . ? N C1 1.340(6) . ? C1 C2 1.381(7) . ? C1 H1 0.9800 . ? C2 C3 1.382(7) . ? C3 C4 1.383(8) . ? C3 H3 0.9800 . ? C4 C5 1.370(7) . ? C4 H4 0.9800 . ? C5 H5 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N Cd N 180.00(19) 3 . ? N Cd Cl1 89.53(10) 3 . ? N Cd Cl1 90.47(10) . . ? N Cd Cl1 90.47(10) 3 3 ? N Cd Cl1 89.53(10) . 3 ? Cl1 Cd Cl1 180.00(4) . 3 ? N Cd Cl1 91.14(10) 3 1_655 ? N Cd Cl1 88.86(10) . 1_655 ? Cl1 Cd Cl1 92.35(4) . 1_655 ? Cl1 Cd Cl1 87.65(4) 3 1_655 ? N Cd Cl1 88.86(10) 3 3_455 ? N Cd Cl1 91.14(10) . 3_455 ? Cl1 Cd Cl1 87.65(4) . 3_455 ? Cl1 Cd Cl1 92.35(4) 3 3_455 ? Cl1 Cd Cl1 180.00(5) 1_655 3_455 ? Cd Cl1 Cd 92.35(4) . 1_455 ? C5 N C1 118.4(4) . . ? C5 N Cd 121.3(3) . . ? C1 N Cd 120.3(3) . . ? N C1 C2 121.1(4) . . ? N C1 H1 119.4 . . ? C2 C1 H1 119.4 . . ? C1 C2 C3 120.6(5) . . ? C1 C2 Cl2 118.5(4) . . ? C3 C2 Cl2 120.9(4) . . ? C2 C3 C4 117.2(5) . . ? C2 C3 H3 121.4 . . ? C4 C3 H3 121.4 . . ? C5 C4 C3 119.3(5) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? N C5 C4 123.4(5) . . ? N C5 H5 118.3 . . ? C4 C5 H5 118.3 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.823 _refine_diff_density_min -1.231 _refine_diff_density_rms 0.121 #============================================================================== data_hc168 _database_code_depnum_ccdc_archive 'CCDC 223788' _chemical_name_common ;catena-(bis(mu-bromo)-bis(3-chloropyridine)-cadmium(ii)) (Compound 5) ; _audit_creation_date 30-OCT-03 _audit_creation_method SHELXTL _audit_update_record ; ? ; _chemical_name_systematic ; catena-[bis(\m-bromo)-bis(3-chloropyridine)-cadmium(ii)] (Compound 5) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H8 Br2 Cd Cl2 N2' _chemical_formula_weight 499.30 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 3.9079(10) _cell_length_b 14.392(4) _cell_length_c 12.238(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.895(7) _cell_angle_gamma 90.00 _cell_volume 688.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5848 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 28.38 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 468 _exptl_absorpt_coefficient_mu 7.758 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.746572 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (1996)' _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 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5848 _diffrn_reflns_av_R_equivalents 0.0658 _diffrn_reflns_av_sigmaI/netI 0.0683 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 28.38 _reflns_number_total 1707 _reflns_number_gt 1328 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXTL (Sheldrick, 1998)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL (Sheldrick, 1998)' _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^)+(0.0107P)^2^+1.1635P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1707 _refine_ls_number_parameters 79 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0725 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.0877 _refine_ls_wR_factor_gt 0.0817 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _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 Cd Cd 0.0000 0.0000 0.0000 0.03125(19) Uani 1 2 d S . . Br Br -0.51116(17) -0.02977(4) -0.15520(5) 0.03400(19) Uani 1 1 d . . . Cl Cl 0.3029(6) 0.39368(13) 0.09919(18) 0.0626(6) Uani 1 1 d . . . N N 0.0110(14) 0.1619(4) -0.0436(4) 0.0363(13) Uani 1 1 d . . . C1 C 0.1309(18) 0.2243(4) 0.0252(5) 0.0369(16) Uani 1 1 d . . . H1 H 0.2152 0.2036 0.0970 0.048 Uiso 1 1 calc R . . C2 C 0.1432(18) 0.3182(5) 0.0007(6) 0.0407(17) Uani 1 1 d . . . C3 C 0.025(2) 0.3483(5) -0.0998(6) 0.050(2) Uani 1 1 d . . . H3 H 0.0272 0.4143 -0.1193 0.065 Uiso 1 1 calc R . . C4 C -0.095(2) 0.2837(5) -0.1704(6) 0.0471(19) Uani 1 1 d . . . H4 H -0.1813 0.3030 -0.2425 0.061 Uiso 1 1 calc R . . C5 C -0.0990(18) 0.1915(5) -0.1427(5) 0.0404(17) Uani 1 1 d . . . H5 H -0.1834 0.1460 -0.1962 0.052 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 0.0292(4) 0.0278(3) 0.0366(4) 0.0003(3) -0.0048(3) -0.0002(3) Br 0.0316(4) 0.0389(4) 0.0313(3) -0.0032(3) -0.0052(3) 0.0005(3) Cl 0.0727(16) 0.0427(11) 0.0721(14) -0.0147(10) -0.0072(12) -0.0056(10) N 0.037(3) 0.038(3) 0.033(3) 0.004(2) 0.000(3) 0.006(3) C1 0.034(4) 0.041(4) 0.035(4) 0.006(3) 0.000(3) 0.003(3) C2 0.036(4) 0.035(4) 0.051(4) -0.007(3) 0.000(3) -0.003(3) C3 0.055(5) 0.033(4) 0.061(5) 0.015(4) 0.007(4) 0.009(4) C4 0.060(5) 0.049(5) 0.033(4) 0.008(3) -0.001(4) 0.003(4) C5 0.044(5) 0.042(4) 0.035(4) 0.000(3) -0.005(3) 0.000(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 N 2.391(5) . ? Cd N 2.391(5) 3 ? Cd Br 2.7484(8) 3_455 ? Cd Br 2.7484(8) 1_655 ? Cd Br 2.7682(8) 3 ? Cd Br 2.7682(8) . ? Br Cd 2.7484(8) 1_455 ? Cl C2 1.732(7) . ? N C1 1.313(8) . ? N C5 1.350(8) . ? C1 C2 1.386(9) . ? C1 H1 0.9800 . ? C2 C3 1.377(9) . ? C3 C4 1.347(10) . ? C3 H3 0.9800 . ? C4 C5 1.369(9) . ? C4 H4 0.9800 . ? C5 H5 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N Cd N 180.0 . 3 ? N Cd Br 90.99(13) . 3_455 ? N Cd Br 89.01(13) 3 3_455 ? N Cd Br 89.01(13) . 1_655 ? N Cd Br 90.99(13) 3 1_655 ? Br Cd Br 180.0 3_455 1_655 ? N Cd Br 89.25(13) . 3 ? N Cd Br 90.75(13) 3 3 ? Br Cd Br 90.21(3) 3_455 3 ? Br Cd Br 89.79(3) 1_655 3 ? N Cd Br 90.75(13) . . ? N Cd Br 89.25(13) 3 . ? Br Cd Br 89.79(3) 3_455 . ? Br Cd Br 90.21(3) 1_655 . ? Br Cd Br 180.000(19) 3 . ? Cd Br Cd 90.21(3) 1_455 . ? C1 N C5 117.7(6) . . ? C1 N Cd 122.1(4) . . ? C5 N Cd 120.1(4) . . ? N C1 C2 122.8(6) . . ? N C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C2 C1 119.2(6) . . ? C3 C2 Cl 122.5(5) . . ? C1 C2 Cl 118.3(6) . . ? C4 C3 C2 117.7(6) . . ? C4 C3 H3 121.2 . . ? C2 C3 H3 121.2 . . ? C3 C4 C5 121.0(7) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? N C5 C4 121.6(6) . . ? N C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 28.38 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.847 _refine_diff_density_min -0.815 _refine_diff_density_rms 0.158 #============================================================================== data_hc167new _database_code_depnum_ccdc_archive 'CCDC 223789' _chemical_name_common ;catena-(bis(mu-iodo)-bis(3-chloropyridine)-cadmium(ii)) (Compound 6) ; _audit_creation_date 30-OCT-03 _audit_creation_method SHELXTL _audit_update_record ; ? ; _chemical_name_systematic ; catena-[bis(\m-iodo)-bis(3-chloropyridine)-cadmium(ii)] (Compound 6) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H8 Cd Cl2 I2 N2' _chemical_formula_weight 593.28 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 4.1332(18) _cell_length_b 14.450(6) _cell_length_c 12.977(6) _cell_angle_alpha 90.00 _cell_angle_beta 89.630(10) _cell_angle_gamma 90.00 _cell_volume 775.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6600 _cell_measurement_theta_min 2.11 _cell_measurement_theta_max 28.36 _exptl_crystal_description needle _exptl_crystal_colour yellowish _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 540 _exptl_absorpt_coefficient_mu 5.717 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.746572 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (1996)' _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 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6600 _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 28.36 _reflns_number_total 1935 _reflns_number_gt 1771 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXTL (Sheldrick, 1998)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL (Sheldrick, 1998)' _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^)+(0.0221P)^2^+0.2659P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1935 _refine_ls_number_parameters 79 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0303 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0603 _refine_ls_wR_factor_gt 0.0587 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _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 Cd Cd 0.0000 0.0000 0.0000 0.03977(11) Uani 1 2 d S . . I I -0.51022(6) -0.030283(18) -0.159256(17) 0.04344(9) Uani 1 1 d . . . Cl Cl 0.2660(5) 0.39178(9) 0.10247(12) 0.1003(5) Uani 1 1 d . . . N N 0.0107(8) 0.1640(2) -0.0406(2) 0.0464(7) Uani 1 1 d . . . C1 C 0.1072(11) 0.2247(3) 0.0288(3) 0.0525(10) Uani 1 1 d . . . H1 H 0.1620 0.2027 0.0980 0.068 Uiso 1 1 calc R . . C2 C 0.1334(12) 0.3176(3) 0.0074(3) 0.0598(11) Uani 1 1 d . . . C3 C 0.0541(15) 0.3508(3) -0.0878(4) 0.0768(15) Uani 1 1 d . . . H3 H 0.0697 0.4167 -0.1047 0.100 Uiso 1 1 calc R . . C4 C -0.0482(14) 0.2868(4) -0.1583(4) 0.0783(16) Uani 1 1 d . . . H4 H -0.1116 0.3070 -0.2274 0.102 Uiso 1 1 calc R . . C5 C -0.0627(11) 0.1946(3) -0.1331(3) 0.0584(11) Uani 1 1 d . . . H5 H -0.1300 0.1501 -0.1857 0.076 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 0.0384(2) 0.03590(19) 0.0450(2) 0.00113(14) -0.00327(16) 0.00092(15) I 0.03686(15) 0.05304(16) 0.04050(14) -0.00438(10) -0.00534(10) 0.00206(10) Cl 0.1480(15) 0.0511(7) 0.1020(10) -0.0217(7) -0.0153(10) -0.0095(8) N 0.055(2) 0.0372(16) 0.0475(17) 0.0055(13) -0.0015(14) 0.0044(14) C1 0.063(3) 0.041(2) 0.053(2) 0.0025(17) -0.009(2) 0.0060(19) C2 0.073(3) 0.041(2) 0.065(3) -0.0035(19) 0.007(2) 0.001(2) C3 0.114(5) 0.040(2) 0.076(3) 0.009(2) 0.008(3) 0.005(3) C4 0.118(5) 0.057(3) 0.060(3) 0.015(2) -0.006(3) 0.012(3) C5 0.074(3) 0.052(2) 0.050(2) 0.0046(19) -0.009(2) 0.003(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 Cd N 2.428(3) 3 ? Cd N 2.428(3) . ? Cd I 2.9166(9) 1_655 ? Cd I 2.9166(9) 3_455 ? Cd I 2.9944(10) . ? Cd I 2.9944(10) 3 ? I Cd 2.9166(9) 1_455 ? Cl C2 1.726(5) . ? N C5 1.316(5) . ? N C1 1.321(5) . ? C1 C2 1.375(6) . ? C1 H1 0.9800 . ? C2 C3 1.367(7) . ? C3 C4 1.369(7) . ? C3 H3 0.9800 . ? C4 C5 1.374(7) . ? C4 H4 0.9800 . ? C5 H5 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N Cd N 180.0(2) 3 . ? N Cd I 91.08(8) 3 1_655 ? N Cd I 88.92(8) . 1_655 ? N Cd I 88.92(8) 3 3_455 ? N Cd I 91.08(8) . 3_455 ? I Cd I 180.000(14) 1_655 3_455 ? N Cd I 89.73(8) 3 . ? N Cd I 90.27(8) . . ? I Cd I 88.72(4) 1_655 . ? I Cd I 91.28(4) 3_455 . ? N Cd I 90.27(8) 3 3 ? N Cd I 89.73(8) . 3 ? I Cd I 91.28(4) 1_655 3 ? I Cd I 88.72(4) 3_455 3 ? I Cd I 180.000(6) . 3 ? Cd I Cd 88.72(4) 1_455 . ? C5 N C1 118.1(3) . . ? C5 N Cd 121.4(3) . . ? C1 N Cd 120.4(3) . . ? N C1 C2 122.3(4) . . ? N C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C3 C2 C1 120.4(4) . . ? C3 C2 Cl 120.5(4) . . ? C1 C2 Cl 119.1(4) . . ? C2 C3 C4 116.4(4) . . ? C2 C3 H3 121.8 . . ? C4 C3 H3 121.8 . . ? C3 C4 C5 120.6(4) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? N C5 C4 122.2(4) . . ? N C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.635 _refine_diff_density_min -0.461 _refine_diff_density_rms 0.099 #============================================================================== data_hc175 _database_code_depnum_ccdc_archive 'CCDC 223790' _chemical_name_common ;catena-(bis(mu-chloro)-bis(3-bromopyridine)-cadmium(ii)) (Compound 7) ; _audit_creation_date 30-OCT-03 _audit_creation_method SHELXTL _audit_update_record ; ? ; _chemical_name_systematic ; catena-[bis(\m-chloro)-bis(3-bromopyridine)-cadmium(ii)] (Compound 7) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H8 Br2 Cd Cl2 N2' _chemical_formula_weight 499.30 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 3.8538(8) _cell_length_b 14.404(3) _cell_length_c 12.082(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.377(5) _cell_angle_gamma 90.00 _cell_volume 670.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7514 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 28.29 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 468 _exptl_absorpt_coefficient_mu 7.963 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.832903 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (1996)' _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 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7514 _diffrn_reflns_av_R_equivalents 0.0462 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 28.29 _reflns_number_total 1653 _reflns_number_gt 1358 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXTL (Sheldrick, 1998)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL (Sheldrick, 1998)' _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^)+(0.0293P)^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_extinction_coef ? _refine_ls_number_reflns 1653 _refine_ls_number_parameters 79 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0410 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0658 _refine_ls_wR_factor_gt 0.0621 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.987 _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 Cd Cd 0.0000 0.0000 0.0000 0.02804(11) Uani 1 2 d S . . Cl Cl -0.5098(2) -0.03001(6) -0.14698(7) 0.0310(2) Uani 1 1 d . . . Br Br 0.32593(11) 0.39977(3) 0.10584(3) 0.04316(13) Uani 1 1 d . . . N N 0.0070(8) 0.1594(2) -0.0465(2) 0.0301(7) Uani 1 1 d . . . C1 C 0.1369(9) 0.2230(2) 0.0244(3) 0.0306(8) Uani 1 1 d . . . H1 H 0.2274 0.2026 0.0969 0.040 Uiso 1 1 calc R . . C2 C 0.1470(9) 0.3159(3) -0.0015(3) 0.0312(8) Uani 1 1 d . . . C3 C 0.0226(11) 0.3458(3) -0.1029(3) 0.0390(9) Uani 1 1 d . . . H3 H 0.0307 0.4117 -0.1230 0.051 Uiso 1 1 calc R . . C4 C -0.1129(11) 0.2814(3) -0.1752(3) 0.0411(10) Uani 1 1 d . . . H4 H -0.2046 0.3006 -0.2481 0.053 Uiso 1 1 calc R . . C5 C -0.1189(10) 0.1888(3) -0.1442(3) 0.0340(8) Uani 1 1 d . . . H5 H -0.2194 0.1432 -0.1959 0.044 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 0.0262(2) 0.0242(2) 0.0335(2) 0.00016(14) -0.00317(14) 0.00049(15) Cl 0.0288(5) 0.0338(5) 0.0303(4) -0.0021(3) -0.0037(3) 0.0002(4) Br 0.0416(3) 0.0327(2) 0.0549(3) -0.00866(17) -0.00387(19) -0.00281(18) N 0.0347(17) 0.0243(15) 0.0312(15) 0.0007(12) 0.0003(12) 0.0018(13) C1 0.035(2) 0.030(2) 0.0270(17) 0.0028(14) -0.0024(14) 0.0034(16) C2 0.0271(19) 0.031(2) 0.036(2) -0.0032(15) 0.0047(15) -0.0008(15) C3 0.044(2) 0.028(2) 0.044(2) 0.0073(16) 0.0064(18) 0.0069(17) C4 0.048(2) 0.043(2) 0.032(2) 0.0088(17) 0.0023(17) 0.0068(19) C5 0.033(2) 0.037(2) 0.0314(19) -0.0012(16) -0.0002(15) 0.0015(17) _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 N 2.364(3) 3 ? Cd N 2.364(3) . ? Cd Cl 2.6518(9) 3 ? Cd Cl 2.6518(9) . ? Cd Cl 2.6591(9) 3_455 ? Cd Cl 2.6591(9) 1_655 ? Cl Cd 2.6591(9) 1_455 ? Br C2 1.891(4) . ? N C5 1.334(4) . ? N C1 1.343(5) . ? C1 C2 1.375(5) . ? C1 H1 0.9800 . ? C2 C3 1.374(5) . ? C3 C4 1.369(6) . ? C3 H3 0.9800 . ? C4 C5 1.387(5) . ? C4 H4 0.9800 . ? C5 H5 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N Cd N 180.00(14) 3 . ? N Cd Cl 90.67(8) 3 3 ? N Cd Cl 89.33(8) . 3 ? N Cd Cl 89.33(8) 3 . ? N Cd Cl 90.67(8) . . ? Cl Cd Cl 180.00(3) 3 . ? N Cd Cl 89.24(7) 3 3_455 ? N Cd Cl 90.76(7) . 3_455 ? Cl Cd Cl 93.05(3) 3 3_455 ? Cl Cd Cl 86.95(3) . 3_455 ? N Cd Cl 90.76(7) 3 1_655 ? N Cd Cl 89.24(7) . 1_655 ? Cl Cd Cl 86.95(3) 3 1_655 ? Cl Cd Cl 93.05(3) . 1_655 ? Cl Cd Cl 180.00(4) 3_455 1_655 ? Cd Cl Cd 93.05(3) . 1_455 ? C5 N C1 118.0(3) . . ? C5 N Cd 120.8(2) . . ? C1 N Cd 121.1(2) . . ? N C1 C2 122.0(3) . . ? N C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C3 C2 C1 119.9(3) . . ? C3 C2 Br 121.6(3) . . ? C1 C2 Br 118.5(3) . . ? C4 C3 C2 118.4(4) . . ? C4 C3 H3 120.8 . . ? C2 C3 H3 120.8 . . ? C3 C4 C5 119.2(4) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? N C5 C4 122.4(4) . . ? N C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.569 _refine_diff_density_min -0.495 _refine_diff_density_rms 0.111 #============================================================================== data_hc174 _database_code_depnum_ccdc_archive 'CCDC 223791' _chemical_name_common ;catena-(bis(mu-bromo)-bis(3-bromopyridine)-cadmium(ii)) (Compound 8) ; _audit_creation_date 30-OCT-03 _audit_creation_method SHELXTL _audit_update_record ; ? ; _chemical_name_systematic ; catena-[bis(\m-bromo)-bis(3-bromopyridine)-cadmium(ii)] (Compound 8) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H8 Br4 Cd N2' _chemical_formula_weight 588.22 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 3.9452(14) _cell_length_b 14.578(5) _cell_length_c 12.286(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.029(8) _cell_angle_gamma 90.00 _cell_volume 706.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9581 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 28.36 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.765 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 540 _exptl_absorpt_coefficient_mu 12.834 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.431770 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (1996)' _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 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 9581 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0238 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 28.36 _reflns_number_total 1763 _reflns_number_gt 1595 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXTL (Sheldrick, 1998)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL (Sheldrick, 1998)' _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^)+(0.0254P)^2^+0.1975P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1763 _refine_ls_number_parameters 79 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0270 _refine_ls_R_factor_gt 0.0232 _refine_ls_wR_factor_ref 0.0554 _refine_ls_wR_factor_gt 0.0539 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.132 _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 Cd Cd 0.0000 0.0000 0.0000 0.02838(9) Uani 1 2 d S . . Br1 Br -0.51256(7) -0.03154(2) -0.15435(2) 0.03065(9) Uani 1 1 d . . . Br2 Br 0.31009(9) 0.39664(2) 0.10330(3) 0.04789(11) Uani 1 1 d . . . N N 0.0069(6) 0.15887(16) -0.0460(2) 0.0315(5) Uani 1 1 d . . . C1 C 0.1272(7) 0.2217(2) 0.0237(2) 0.0315(6) Uani 1 1 d . . . H1 H 0.2104 0.2018 0.0955 0.041 Uiso 1 1 calc R . . C2 C 0.1380(7) 0.3135(2) -0.0023(3) 0.0326(6) Uani 1 1 d . . . C3 C 0.0202(9) 0.3437(2) -0.1016(3) 0.0420(8) Uani 1 1 d . . . H3 H 0.0262 0.4089 -0.1210 0.055 Uiso 1 1 calc R . . C4 C -0.1076(9) 0.2787(2) -0.1734(3) 0.0431(8) Uani 1 1 d . . . H4 H -0.1957 0.2971 -0.2452 0.056 Uiso 1 1 calc R . . C5 C -0.1097(8) 0.1876(2) -0.1429(2) 0.0367(7) Uani 1 1 d . . . H5 H -0.2006 0.1422 -0.1944 0.048 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 0.02895(15) 0.02257(16) 0.03346(17) 0.00055(11) -0.00424(12) -0.00007(11) Br1 0.03076(15) 0.03098(17) 0.03000(16) -0.00207(11) -0.00502(11) 0.00059(11) Br2 0.0516(2) 0.03222(18) 0.0596(2) -0.01023(15) -0.00589(17) -0.00337(14) N 0.0384(13) 0.0236(12) 0.0325(13) 0.0022(10) 0.0001(10) 0.0013(10) C1 0.0350(15) 0.0279(14) 0.0316(15) 0.0003(12) -0.0016(12) 0.0017(12) C2 0.0322(15) 0.0238(14) 0.0418(17) -0.0038(12) 0.0019(12) 0.0014(12) C3 0.052(2) 0.0271(16) 0.0470(19) 0.0090(13) 0.0041(15) 0.0036(14) C4 0.056(2) 0.0392(18) 0.0340(17) 0.0076(14) -0.0043(14) 0.0044(16) C5 0.0445(17) 0.0328(16) 0.0327(16) 0.0019(12) -0.0042(13) -0.0002(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd N 2.384(2) . ? Cd N 2.384(2) 3 ? Cd Br1 2.7635(8) 3_455 ? Cd Br1 2.7635(8) 1_655 ? Cd Br1 2.7855(8) 3 ? Cd Br1 2.7855(8) . ? Br1 Cd 2.7635(8) 1_455 ? Br2 C2 1.892(3) . ? N C1 1.335(4) . ? N C5 1.336(4) . ? C1 C2 1.378(4) . ? C1 H1 0.9800 . ? C2 C3 1.370(4) . ? C3 C4 1.384(5) . ? C3 H3 0.9800 . ? C4 C5 1.379(5) . ? C4 H4 0.9800 . ? C5 H5 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N Cd N 180.00(12) . 3 ? N Cd Br1 90.70(6) . 3_455 ? N Cd Br1 89.30(6) 3 3_455 ? N Cd Br1 89.30(6) . 1_655 ? N Cd Br1 90.70(6) 3 1_655 ? Br1 Cd Br1 180.000(12) 3_455 1_655 ? N Cd Br1 89.42(6) . 3 ? N Cd Br1 90.58(6) 3 3 ? Br1 Cd Br1 90.63(3) 3_455 3 ? Br1 Cd Br1 89.37(3) 1_655 3 ? N Cd Br1 90.58(6) . . ? N Cd Br1 89.42(6) 3 . ? Br1 Cd Br1 89.37(3) 3_455 . ? Br1 Cd Br1 90.63(3) 1_655 . ? Br1 Cd Br1 180.000(9) 3 . ? Cd Br1 Cd 90.63(3) 1_455 . ? C1 N C5 118.0(3) . . ? C1 N Cd 121.3(2) . . ? C5 N Cd 120.7(2) . . ? N C1 C2 122.0(3) . . ? N C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C3 C2 C1 120.5(3) . . ? C3 C2 Br2 121.1(2) . . ? C1 C2 Br2 118.4(2) . . ? C2 C3 C4 117.5(3) . . ? C2 C3 H3 121.3 . . ? C4 C3 H3 121.3 . . ? C5 C4 C3 119.3(3) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? N C5 C4 122.7(3) . . ? N C5 H5 118.6 . . ? C4 C5 H5 118.6 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.453 _refine_diff_density_min -0.671 _refine_diff_density_rms 0.146 #========================================================================== data_hc179 _database_code_depnum_ccdc_archive 'CCDC 223792' _chemical_name_common ;catena-(bis(mu-iodo)-bis(3-bromopyridine)-cadmium(ii)) (Compound 9) ; _chemical_name_systematic ; catena-[bis(\m-iodo)-bis(3-bromopyridine)-cadmium(ii)] (Compound 9) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H8 Br2 Cd I2 N2' _chemical_formula_weight 682.20 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' Br Br -0.2901 2.4595 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 4.1429(7) _cell_length_b 14.657(3) _cell_length_c 12.946(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.162(4) _cell_angle_gamma 90.00 _cell_volume 786.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6002 _cell_measurement_theta_min 2.78 _cell_measurement_theta_max 28.32 _exptl_crystal_description prism _exptl_crystal_colour grey _exptl_crystal_size_max 0.74 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.882 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 612 _exptl_absorpt_coefficient_mu 10.380 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.412756 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (1996)' _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 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6002 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 28.32 _reflns_number_total 1957 _reflns_number_gt 1795 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXTL (Sheldrick, 1998)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL (Sheldrick, 1998)' _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^)+(0.0311P)^2^+0.0943P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1957 _refine_ls_number_parameters 79 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0302 _refine_ls_R_factor_gt 0.0274 _refine_ls_wR_factor_ref 0.0637 _refine_ls_wR_factor_gt 0.0629 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _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 Cd Cd 0.0000 0.0000 0.0000 0.03270(10) Uani 1 2 d S . . I I -0.51477(5) -0.032384(16) -0.159442(16) 0.03496(9) Uani 1 1 d . . . Br Br 0.28423(13) 0.39385(3) 0.10487(4) 0.06712(16) Uani 1 1 d . . . N N 0.0071(7) 0.16027(19) -0.0432(2) 0.0357(6) Uani 1 1 d . . . C1 C 0.1084(9) 0.2219(2) 0.0253(3) 0.0411(8) Uani 1 1 d . . . H1 H 0.1676 0.2013 0.0949 0.053 Uiso 1 1 calc R . . C2 C 0.1330(9) 0.3135(2) 0.0019(3) 0.0440(9) Uani 1 1 d . . . C3 C 0.0439(13) 0.3439(3) -0.0939(4) 0.0598(12) Uani 1 1 d . . . H3 H 0.0559 0.4088 -0.1120 0.078 Uiso 1 1 calc R . . C4 C -0.0620(13) 0.2806(3) -0.1633(4) 0.0645(13) Uani 1 1 d . . . H4 H -0.1280 0.2999 -0.2327 0.084 Uiso 1 1 calc R . . C5 C -0.0771(11) 0.1892(3) -0.1364(3) 0.0482(9) Uani 1 1 d . . . H5 H -0.1521 0.1448 -0.1877 0.063 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 0.03566(19) 0.02688(19) 0.0355(2) 0.00118(13) -0.00156(14) 0.00045(12) I 0.03376(13) 0.04028(15) 0.03082(14) -0.00309(8) -0.00359(9) 0.00188(8) Br 0.0858(4) 0.0401(2) 0.0754(4) -0.0156(2) -0.0069(3) -0.0069(2) N 0.0468(16) 0.0274(14) 0.0329(16) 0.0026(12) 0.0002(12) 0.0026(12) C1 0.053(2) 0.0336(18) 0.037(2) -0.0005(15) -0.0014(16) 0.0025(15) C2 0.051(2) 0.0310(18) 0.050(2) -0.0068(16) 0.0068(17) 0.0019(15) C3 0.088(3) 0.029(2) 0.061(3) 0.0118(19) 0.005(2) 0.003(2) C4 0.104(4) 0.050(3) 0.040(2) 0.0118(19) -0.011(2) 0.007(2) C5 0.066(3) 0.041(2) 0.037(2) 0.0001(17) -0.0047(18) 0.0034(18) _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 N 2.415(3) 3 ? Cd N 2.415(3) . ? Cd I 2.9241(4) 3_455 ? Cd I 2.9241(4) 1_655 ? Cd I 3.0015(4) . ? Cd I 3.0015(4) 3 ? I Cd 2.9241(4) 1_455 ? Br C2 1.884(4) . ? N C5 1.325(5) . ? N C1 1.333(5) . ? C1 C2 1.381(5) . ? C1 H1 0.9800 . ? C2 C3 1.368(6) . ? C3 C4 1.363(7) . ? C3 H3 0.9800 . ? C4 C5 1.386(6) . ? C4 H4 0.9800 . ? C5 H5 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N Cd N 180.00(19) 3 . ? N Cd I 89.17(7) 3 3_455 ? N Cd I 90.83(7) . 3_455 ? N Cd I 90.83(7) 3 1_655 ? N Cd I 89.17(7) . 1_655 ? I Cd I 180.000(6) 3_455 1_655 ? N Cd I 89.79(7) 3 . ? N Cd I 90.21(7) . . ? I Cd I 91.292(15) 3_455 . ? I Cd I 88.708(15) 1_655 . ? N Cd I 90.21(7) 3 3 ? N Cd I 89.79(7) . 3 ? I Cd I 88.708(15) 3_455 3 ? I Cd I 91.292(15) 1_655 3 ? I Cd I 180.000(8) . 3 ? Cd I Cd 88.708(15) 1_455 . ? C5 N C1 118.1(3) . . ? C5 N Cd 121.3(2) . . ? C1 N Cd 120.6(2) . . ? N C1 C2 122.4(4) . . ? N C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C3 C2 C1 119.7(4) . . ? C3 C2 Br 121.7(3) . . ? C1 C2 Br 118.5(3) . . ? C4 C3 C2 117.5(4) . . ? C4 C3 H3 121.3 . . ? C2 C3 H3 121.3 . . ? C3 C4 C5 120.5(4) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? N C5 C4 121.8(4) . . ? N C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.669 _refine_diff_density_min -0.896 _refine_diff_density_rms 0.157 #============================================================================== data_hc238 _database_code_depnum_ccdc_archive 'CCDC 223793' _chemical_name_common ;catena-(bis(mu-chloro)-bis(3-methylpyridine)-cadmium(ii)) (Compound 10) ; _audit_creation_date 30-OCT-03 _audit_creation_method SHELXTL _audit_update_record ; ? ; _chemical_name_systematic ; catena-[bis(\m-chloro)-bis(3-methylpyridine)-cadmium(ii)] (Compound 10) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H14 Cd Cl2 N2' _chemical_formula_weight 369.55 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 P21/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 3.8726(5) _cell_length_b 14.613(2) _cell_length_c 11.8992(17) _cell_angle_alpha 90.00 _cell_angle_beta 92.449(3) _cell_angle_gamma 90.00 _cell_volume 672.78(16) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6787 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 28.31 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.824 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 364 _exptl_absorpt_coefficient_mu 1.998 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.821507 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (1996)' _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 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6787 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 28.31 _reflns_number_total 1664 _reflns_number_gt 1309 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXTL (Sheldrick, 1998)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL (Sheldrick, 1998)' _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^)+(0.0310P)^2^+0.0595P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1664 _refine_ls_number_parameters 80 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0443 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0678 _refine_ls_wR_factor_gt 0.0638 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.005 _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 Cd Cd 0.0000 0.0000 0.0000 0.02858(11) Uani 1 2 d S . . Cl Cl -0.5206(2) -0.03369(6) -0.14804(6) 0.03288(17) Uani 1 1 d . . . N N -0.0033(6) 0.15474(17) -0.0547(2) 0.0316(6) Uani 1 1 d . . . C1 C 0.1275(8) 0.2207(2) 0.0123(3) 0.0343(7) Uani 1 1 d . . . H1 H 0.2264 0.2028 0.0862 0.045 Uiso 1 1 calc R . . C2 C 0.1324(9) 0.3124(2) -0.0159(3) 0.0382(7) Uani 1 1 d . . . C3 C -0.0054(9) 0.3359(2) -0.1217(3) 0.0428(8) Uani 1 1 d . . . H3 H -0.0051 0.3999 -0.1466 0.056 Uiso 1 1 calc R . . C4 C -0.1422(9) 0.2688(2) -0.1914(3) 0.0438(8) Uani 1 1 d . . . H4 H -0.2429 0.2848 -0.2658 0.057 Uiso 1 1 calc R . . C5 C -0.1369(8) 0.1794(2) -0.1560(3) 0.0370(7) Uani 1 1 d . . . H5 H -0.2340 0.1321 -0.2064 0.048 Uiso 1 1 calc R . . C6 C 0.2818(10) 0.3830(2) 0.0642(3) 0.0519(10) Uani 1 1 d . . . H6A H 0.0940 0.4183 0.0959 0.067 Uiso 1 1 calc R . . H6B H 0.4331 0.4242 0.0239 0.067 Uiso 1 1 calc R . . H6C H 0.4156 0.3525 0.1251 0.067 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 0.02655(17) 0.02391(16) 0.03489(18) 0.00084(13) -0.00326(11) -0.00020(13) Cl 0.0297(4) 0.0348(4) 0.0337(4) -0.0045(3) -0.0037(3) -0.0003(3) N 0.0325(14) 0.0280(14) 0.0342(14) 0.0022(11) 0.0008(11) 0.0021(10) C1 0.0325(16) 0.0320(17) 0.0380(18) 0.0032(13) -0.0034(13) -0.0002(13) C2 0.0329(17) 0.0303(17) 0.052(2) 0.0015(14) 0.0035(14) 0.0021(14) C3 0.043(2) 0.0318(18) 0.054(2) 0.0117(15) 0.0038(17) 0.0051(15) C4 0.045(2) 0.043(2) 0.043(2) 0.0122(16) -0.0035(16) 0.0011(16) C5 0.0388(18) 0.0382(18) 0.0337(17) 0.0018(14) -0.0034(14) 0.0008(14) C6 0.054(2) 0.0328(19) 0.069(3) -0.0042(17) -0.001(2) -0.0020(16) _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 N 2.353(2) 3 ? Cd N 2.353(2) . ? Cd Cl 2.6593(8) 3_455 ? Cd Cl 2.6593(8) 1_655 ? Cd Cl 2.6658(8) . ? Cd Cl 2.6658(8) 3 ? Cl Cd 2.6593(8) 1_455 ? N C1 1.336(4) . ? N C5 1.341(4) . ? C1 C2 1.382(4) . ? C1 H1 0.9800 . ? C2 C3 1.390(4) . ? C2 C6 1.504(4) . ? C3 C4 1.375(5) . ? C3 H3 0.9800 . ? C4 C5 1.373(4) . ? C4 H4 0.9800 . ? C5 H5 0.9800 . ? C6 H6A 0.9801 . ? C6 H6B 0.9801 . ? C6 H6C 0.9801 . ? 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 N Cd N 180.00(18) 3 . ? N Cd Cl 89.45(6) 3 3_455 ? N Cd Cl 90.55(6) . 3_455 ? N Cd Cl 90.55(6) 3 1_655 ? N Cd Cl 89.45(6) . 1_655 ? Cl Cd Cl 180.00(2) 3_455 1_655 ? N Cd Cl 90.02(6) 3 . ? N Cd Cl 89.98(6) . . ? Cl Cd Cl 86.69(3) 3_455 . ? Cl Cd Cl 93.31(3) 1_655 . ? N Cd Cl 89.98(6) 3 3 ? N Cd Cl 90.02(6) . 3 ? Cl Cd Cl 93.31(3) 3_455 3 ? Cl Cd Cl 86.69(3) 1_655 3 ? Cl Cd Cl 180.00(3) . 3 ? Cd Cl Cd 93.31(3) 1_455 . ? C1 N C5 117.7(3) . . ? C1 N Cd 122.1(2) . . ? C5 N Cd 120.3(2) . . ? N C1 C2 124.3(3) . . ? N C1 H1 117.8 . . ? C2 C1 H1 117.8 . . ? C1 C2 C3 116.8(3) . . ? C1 C2 C6 121.4(3) . . ? C3 C2 C6 121.8(3) . . ? C4 C3 C2 119.5(3) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C5 C4 C3 119.6(3) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? N C5 C4 122.1(3) . . ? N C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? C2 C6 H6A 109.5 . . ? C2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.528 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.091 #============================================================================== data_hc239 _database_code_depnum_ccdc_archive 'CCDC 223794' _chemical_name_common ;catena-(bis(mu-bromo)-bis(3-methylpyridine)-cadmium(ii)) (Compound 11) ; _audit_creation_date 30-OCT-03 _audit_creation_method SHELXTL _audit_update_record ; ? ; _chemical_name_systematic ; catena-[bis(\m-bromo)-bis(3-methylpyridine)-cadmium(ii)] (Compound 11) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H14 Br2 Cd N2' _chemical_formula_weight 458.47 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 3.9800(6) _cell_length_b 14.738(2) _cell_length_c 12.1051(17) _cell_angle_alpha 90.00 _cell_angle_beta 91.971(3) _cell_angle_gamma 90.00 _cell_volume 709.61(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6848 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 28.33 _exptl_crystal_description 'needle colorless 0.25x0.07x0.06 faces' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.146 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 436 _exptl_absorpt_coefficient_mu 7.149 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.678066 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (1996)' _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 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6848 _diffrn_reflns_av_R_equivalents 0.0422 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 28.33 _reflns_number_total 1765 _reflns_number_gt 1442 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXTL (Sheldrick, 1998)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL (Sheldrick, 1998)' _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^)+(0.0295P)^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_extinction_coef ? _refine_ls_number_reflns 1765 _refine_ls_number_parameters 80 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0672 _refine_ls_wR_factor_gt 0.0640 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd Cd 0.0000 0.0000 0.0000 0.03191(11) Uani 1 2 d S . . Br Br -0.52220(8) -0.03194(3) -0.15665(3) 0.03513(12) Uani 1 1 d . . . N N 0.0041(7) 0.15620(19) -0.0491(2) 0.0359(6) Uani 1 1 d . . . C1 C 0.1290(9) 0.2208(2) 0.0178(3) 0.0382(8) Uani 1 1 d . . . H1 H 0.2194 0.2021 0.0906 0.050 Uiso 1 1 calc R . . C2 C 0.1400(9) 0.3113(3) -0.0078(3) 0.0417(8) Uani 1 1 d . . . C3 C 0.0109(10) 0.3362(3) -0.1118(3) 0.0520(10) Uani 1 1 d . . . H3 H 0.0147 0.4000 -0.1348 0.068 Uiso 1 1 calc R . . C4 C -0.1211(11) 0.2716(3) -0.1818(3) 0.0537(11) Uani 1 1 d . . . H4 H -0.2158 0.2885 -0.2547 0.070 Uiso 1 1 calc R . . C5 C -0.1187(9) 0.1825(3) -0.1481(3) 0.0442(9) Uani 1 1 d . . . H5 H -0.2108 0.1363 -0.1989 0.058 Uiso 1 1 calc R . . C6 C 0.2840(11) 0.3798(3) 0.0729(3) 0.0616(12) Uani 1 1 d . . . H6A H 0.1019 0.4168 0.1015 0.080 Uiso 1 1 calc R . . H6B H 0.4435 0.4189 0.0355 0.080 Uiso 1 1 calc R . . H6C H 0.4005 0.3481 0.1343 0.080 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 0.0321(2) 0.0255(2) 0.03778(19) 0.00130(13) -0.00367(14) 0.00024(14) Br 0.0338(2) 0.0361(2) 0.03503(19) -0.00391(13) -0.00430(13) 0.00012(14) N 0.0405(16) 0.0262(16) 0.0408(15) 0.0027(11) 0.0004(12) -0.0005(12) C1 0.0408(19) 0.033(2) 0.0403(18) 0.0027(14) -0.0015(15) 0.0039(16) C2 0.043(2) 0.031(2) 0.051(2) -0.0010(15) 0.0068(16) -0.0006(16) C3 0.063(3) 0.031(2) 0.062(2) 0.0113(18) 0.006(2) -0.0007(19) C4 0.067(3) 0.045(3) 0.049(2) 0.0154(18) -0.0063(19) 0.006(2) C5 0.052(2) 0.040(2) 0.0400(19) 0.0023(15) -0.0036(16) 0.0003(18) C6 0.066(3) 0.039(3) 0.079(3) -0.011(2) -0.002(2) -0.010(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 Cd N 2.378(3) 3 ? Cd N 2.378(3) . ? Cd Br 2.7716(4) 3_455 ? Cd Br 2.7716(4) 1_655 ? Cd Br 2.8046(4) . ? Cd Br 2.8046(4) 3 ? Br Cd 2.7716(4) 1_455 ? N C1 1.335(4) . ? N C5 1.336(4) . ? C1 C2 1.370(5) . ? C1 H1 0.9800 . ? C2 C3 1.393(5) . ? C2 C6 1.505(5) . ? C3 C4 1.368(6) . ? C3 H3 0.9800 . ? C4 C5 1.375(6) . ? C4 H4 0.9800 . ? C5 H5 0.9800 . ? C6 H6A 0.9801 . ? C6 H6B 0.9801 . ? C6 H6C 0.9801 . ? 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 N Cd N 180.00(19) 3 . ? N Cd Br 89.01(7) 3 3_455 ? N Cd Br 90.99(7) . 3_455 ? N Cd Br 90.99(7) 3 1_655 ? N Cd Br 89.01(7) . 1_655 ? Br Cd Br 180.000(13) 3_455 1_655 ? N Cd Br 89.72(7) 3 . ? N Cd Br 90.28(7) . . ? Br Cd Br 88.922(15) 3_455 . ? Br Cd Br 91.078(15) 1_655 . ? N Cd Br 90.28(7) 3 3 ? N Cd Br 89.72(7) . 3 ? Br Cd Br 91.078(15) 3_455 3 ? Br Cd Br 88.922(15) 1_655 3 ? Br Cd Br 180.000(14) . 3 ? Cd Br Cd 91.078(15) 1_455 . ? C1 N C5 117.1(3) . . ? C1 N Cd 123.0(2) . . ? C5 N Cd 119.9(2) . . ? N C1 C2 124.8(3) . . ? N C1 H1 117.6 . . ? C2 C1 H1 117.6 . . ? C1 C2 C3 116.6(3) . . ? C1 C2 C6 121.3(4) . . ? C3 C2 C6 122.0(4) . . ? C4 C3 C2 119.8(4) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 118.9(3) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N C5 C4 122.8(4) . . ? N C5 H5 118.6 . . ? C4 C5 H5 118.6 . . ? C2 C6 H6A 109.5 . . ? C2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.545 _refine_diff_density_min -0.381 _refine_diff_density_rms 0.106 #============================================================================== data_hc249 _database_code_depnum_ccdc_archive 'CCDC 223795' _chemical_name_common ;(bis(iodo)-bis(3-methylpyridine)-cadmium(ii)) (Compound 12, RT dataset, 12a) ; _audit_creation_date 30-OCT-03 _audit_creation_method SHELXTL _audit_update_record ; ? ; _chemical_name_systematic ; [bis(iodo)-bis(3-methylpyridine)-cadmium(ii)] (Compound 12, RT dataset, 12a) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H14 Cd I2 N2' _chemical_formula_weight 552.45 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.6737(15) _cell_length_b 15.490(2) _cell_length_c 11.3920(19) _cell_angle_alpha 90.00 _cell_angle_beta 100.329(3) _cell_angle_gamma 90.00 _cell_volume 1679.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 22772 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 28.34 _exptl_crystal_description polygon _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.185 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 4.960 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.662479 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (1996)' _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 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 22772 _diffrn_reflns_av_R_equivalents 0.0562 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 28.34 _reflns_number_total 4188 _reflns_number_gt 3299 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXTL (Sheldrick, 1998)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL (Sheldrick, 1998)' _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^)+(0.0416P)^2^+1.3239P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4188 _refine_ls_number_parameters 156 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0490 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.0978 _refine_ls_wR_factor_gt 0.0920 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 Cd Cd 0.15977(3) 0.03054(2) 0.73960(3) 0.05304(11) Uani 1 1 d . . . I1 I 0.10496(4) -0.13201(2) 0.80014(4) 0.08077(14) Uani 1 1 d . . . I2 I 0.25359(5) 0.08760(3) 0.54544(3) 0.08055(14) Uani 1 1 d . . . N11 N -0.0377(4) 0.1102(3) 0.7431(4) 0.0570(9) Uani 1 1 d . . . N21 N 0.3050(4) 0.0849(2) 0.9040(3) 0.0555(9) Uani 1 1 d . . . C12 C -0.1265(5) 0.1244(3) 0.6410(5) 0.0598(11) Uani 1 1 d . . . H12 H -0.1037 0.1008 0.5670 0.078 Uiso 1 1 calc R . . C13 C -0.2489(5) 0.1710(3) 0.6355(6) 0.0714(14) Uani 1 1 d . . . C14 C -0.2766(7) 0.2041(4) 0.7413(7) 0.093(2) Uani 1 1 d . . . H14 H -0.3615 0.2386 0.7414 0.121 Uiso 1 1 calc R . . C15 C -0.1855(8) 0.1888(5) 0.8467(7) 0.099(2) Uani 1 1 d . . . H15 H -0.2050 0.2117 0.9223 0.129 Uiso 1 1 calc R . . C16 C -0.0686(6) 0.1417(4) 0.8439(5) 0.0725(14) Uani 1 1 d . . . H16 H -0.0041 0.1303 0.9190 0.094 Uiso 1 1 calc R . . C17 C -0.3441(7) 0.1856(6) 0.5186(7) 0.114(3) Uani 1 1 d . . . H17A H -0.3883 0.2425 0.5189 0.148 Uiso 1 1 calc R . . H17B H -0.4168 0.1408 0.5062 0.148 Uiso 1 1 calc R . . H17C H -0.2895 0.1830 0.4541 0.148 Uiso 1 1 calc R . . C22 C 0.3062(5) 0.0526(3) 1.0123(4) 0.0616(11) Uani 1 1 d . . . H22 H 0.2442 0.0038 1.0201 0.080 Uiso 1 1 calc R . . C23 C 0.3904(6) 0.0842(4) 1.1151(5) 0.0684(13) Uani 1 1 d . . . C24 C 0.4766(6) 0.1520(4) 1.1004(6) 0.0787(16) Uani 1 1 d . . . H24 H 0.5378 0.1769 1.1701 0.102 Uiso 1 1 calc R . . C25 C 0.4783(6) 0.1851(4) 0.9905(6) 0.0844(17) Uani 1 1 d . . . H25 H 0.5412 0.2331 0.9806 0.110 Uiso 1 1 calc R . . C26 C 0.3900(6) 0.1504(3) 0.8920(5) 0.0703(13) Uani 1 1 d . . . H26 H 0.3905 0.1747 0.8126 0.091 Uiso 1 1 calc R . . C27 C 0.3811(10) 0.0458(5) 1.2350(6) 0.110(2) Uani 1 1 d . . . H27A H 0.4676 0.0584 1.2915 0.143 Uiso 1 1 calc R . . H27B H 0.3688 -0.0169 1.2270 0.143 Uiso 1 1 calc R . . H27C H 0.3007 0.0708 1.2644 0.143 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 0.05461(18) 0.0541(2) 0.05072(17) 0.00214(13) 0.01010(13) 0.00157(14) I1 0.0894(3) 0.0572(2) 0.0905(3) 0.00484(17) 0.0021(2) -0.01921(17) I2 0.0956(3) 0.0891(3) 0.0637(2) 0.01149(18) 0.03262(19) -0.0011(2) N11 0.054(2) 0.056(2) 0.061(2) -0.0048(17) 0.0121(17) 0.0034(17) N21 0.056(2) 0.054(2) 0.056(2) 0.0017(17) 0.0074(16) -0.0020(16) C12 0.055(2) 0.058(3) 0.066(3) -0.001(2) 0.009(2) 0.002(2) C13 0.055(3) 0.062(3) 0.098(4) 0.015(3) 0.016(3) 0.000(2) C14 0.078(4) 0.090(4) 0.120(5) 0.009(4) 0.040(4) 0.033(3) C15 0.095(5) 0.105(5) 0.105(5) -0.022(4) 0.039(4) 0.024(4) C16 0.069(3) 0.077(4) 0.072(3) -0.016(3) 0.016(2) 0.005(3) C17 0.067(4) 0.138(7) 0.132(6) 0.047(5) 0.004(4) 0.018(4) C22 0.067(3) 0.060(3) 0.056(2) 0.002(2) 0.006(2) -0.009(2) C23 0.067(3) 0.074(3) 0.060(3) -0.007(2) 0.001(2) 0.011(3) C24 0.057(3) 0.094(4) 0.082(4) -0.029(3) 0.004(3) -0.003(3) C25 0.076(4) 0.088(4) 0.094(4) -0.022(3) 0.028(3) -0.034(3) C26 0.078(3) 0.063(3) 0.075(3) -0.005(2) 0.028(3) -0.018(3) C27 0.148(7) 0.114(6) 0.060(3) 0.004(4) -0.003(4) -0.003(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 Cd N11 2.280(4) . ? Cd N21 2.290(4) . ? Cd I2 2.6864(6) . ? Cd I1 2.6885(6) . ? N11 C16 1.330(6) . ? N11 C12 1.335(6) . ? N21 C22 1.329(6) . ? N21 C26 1.329(6) . ? C12 C13 1.378(7) . ? C12 H12 0.9800 . ? C13 C14 1.380(9) . ? C13 C17 1.494(9) . ? C14 C15 1.377(9) . ? C14 H14 0.9800 . ? C15 C16 1.351(8) . ? C15 H15 0.9800 . ? C16 H16 0.9800 . ? C17 H17A 0.9801 . ? C17 H17B 0.9801 . ? C17 H17C 0.9801 . ? C22 C23 1.390(7) . ? C22 H22 0.9800 . ? C23 C24 1.370(9) . ? C23 C27 1.507(8) . ? C24 C25 1.356(9) . ? C24 H24 0.9800 . ? C25 C26 1.391(8) . ? C25 H25 0.9800 . ? C26 H26 0.9800 . ? C27 H27A 0.9801 . ? C27 H27B 0.9801 . ? C27 H27C 0.9801 . ? 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 N11 Cd N21 100.36(14) . . ? N11 Cd I2 104.13(10) . . ? N21 Cd I2 107.71(10) . . ? N11 Cd I1 107.33(10) . . ? N21 Cd I1 104.75(9) . . ? I2 Cd I1 129.096(18) . . ? C16 N11 C12 118.9(4) . . ? C16 N11 Cd 122.1(4) . . ? C12 N11 Cd 119.0(3) . . ? C22 N21 C26 118.7(4) . . ? C22 N21 Cd 121.6(3) . . ? C26 N21 Cd 119.8(3) . . ? N11 C12 C13 122.7(5) . . ? N11 C12 H12 118.7 . . ? C13 C12 H12 118.7 . . ? C12 C13 C14 117.0(5) . . ? C12 C13 C17 120.5(6) . . ? C14 C13 C17 122.5(6) . . ? C15 C14 C13 120.3(5) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C16 C15 C14 118.7(6) . . ? C16 C15 H15 120.7 . . ? C14 C15 H15 120.7 . . ? N11 C16 C15 122.5(6) . . ? N11 C16 H16 118.8 . . ? C15 C16 H16 118.8 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N21 C22 C23 123.8(5) . . ? N21 C22 H22 118.1 . . ? C23 C22 H22 118.1 . . ? C24 C23 C22 116.4(5) . . ? C24 C23 C27 123.4(5) . . ? C22 C23 C27 120.2(6) . . ? C25 C24 C23 120.7(5) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C24 C25 C26 119.5(5) . . ? C24 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? N21 C26 C25 120.9(5) . . ? N21 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C23 C27 H27A 109.5 . . ? C23 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C23 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.045 _refine_diff_density_min -1.065 _refine_diff_density_rms 0.138 #============================================================================== data_hc248 _database_code_depnum_ccdc_archive 'CCDC 223796' _chemical_name_common ;(bis(iodo)-bis(3-methylpyridine)-cadmium(ii)) (Compound 12, 120K dataset, 12b) ; _audit_creation_date 30-OCT-03 _audit_creation_method SHELXTL _audit_update_record ; ? ; _chemical_name_systematic ; [bis(iodo)-bis(3-methylpyridine)-cadmium(ii)] (Compound 12, 120K dataset, 12b) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H14 Cd I2 N2' _chemical_formula_weight 552.45 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.5708(15) _cell_length_b 15.222(2) _cell_length_c 11.3480(18) _cell_angle_alpha 90.00 _cell_angle_beta 100.122(3) _cell_angle_gamma 90.00 _cell_volume 1627.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 12895 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 28.31 _exptl_crystal_description polygon _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.255 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 5.119 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.778347 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12895 _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_av_sigmaI/netI 0.0260 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 28.31 _reflns_number_total 4049 _reflns_number_gt 3659 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXTL (Sheldrick, 1998)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL (Sheldrick, 1998)' _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^)+(0.0239P)^2^+0.2765P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4049 _refine_ls_number_parameters 156 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0261 _refine_ls_R_factor_gt 0.0222 _refine_ls_wR_factor_ref 0.0521 _refine_ls_wR_factor_gt 0.0506 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 Cd Cd 0.16875(2) 0.025595(12) 0.737451(16) 0.02072(5) Uani 1 1 d . . . I1 I 0.10804(2) -0.139054(12) 0.799476(18) 0.03175(6) Uani 1 1 d . . . I2 I 0.26262(2) 0.084293(14) 0.541914(17) 0.03195(6) Uani 1 1 d . . . N11 N -0.0288(2) 0.10750(14) 0.7434(2) 0.0219(5) Uani 1 1 d . . . N21 N 0.3152(2) 0.07915(14) 0.9021(2) 0.0217(5) Uani 1 1 d . . . C12 C -0.1176(3) 0.12513(18) 0.6410(3) 0.0242(6) Uani 1 1 d . . . H12 H -0.0948 0.1025 0.5658 0.031 Uiso 1 1 calc R . . C13 C -0.2403(3) 0.17398(19) 0.6371(3) 0.0297(6) Uani 1 1 d . . . C14 C -0.2690(4) 0.2062(2) 0.7439(3) 0.0375(7) Uani 1 1 d . . . H14 H -0.3541 0.2418 0.7445 0.049 Uiso 1 1 calc R . . C15 C -0.1786(4) 0.1885(2) 0.8501(3) 0.0375(7) Uani 1 1 d . . . H15 H -0.1981 0.2116 0.9261 0.049 Uiso 1 1 calc R . . C16 C -0.0604(3) 0.13767(19) 0.8465(3) 0.0284(6) Uani 1 1 d . . . H16 H 0.0026 0.1231 0.9217 0.037 Uiso 1 1 calc R . . C17 C -0.3361(3) 0.1902(2) 0.5188(3) 0.0429(8) Uani 1 1 d . . . H17A H -0.3487 0.2536 0.5060 0.056 Uiso 1 1 calc R . . H17B H -0.4286 0.1627 0.5194 0.056 Uiso 1 1 calc R . . H17C H -0.2933 0.1648 0.4542 0.056 Uiso 1 1 calc R . . C22 C 0.3105(3) 0.04756(18) 1.0118(2) 0.0240(6) Uani 1 1 d . . . H22 H 0.2473 -0.0020 1.0191 0.031 Uiso 1 1 calc R . . C23 C 0.3909(3) 0.08165(19) 1.1153(3) 0.0280(6) Uani 1 1 d . . . C24 C 0.4806(3) 0.1513(2) 1.1017(3) 0.0305(7) Uani 1 1 d . . . H24 H 0.5396 0.1774 1.1723 0.040 Uiso 1 1 calc R . . C25 C 0.4868(3) 0.1838(2) 0.9894(3) 0.0316(6) Uani 1 1 d . . . H25 H 0.5507 0.2325 0.9795 0.041 Uiso 1 1 calc R . . C26 C 0.4020(3) 0.14682(19) 0.8912(3) 0.0281(6) Uani 1 1 d . . . H26 H 0.4052 0.1705 0.8114 0.037 Uiso 1 1 calc R . . C27 C 0.3789(4) 0.0451(2) 1.2359(3) 0.0430(8) Uani 1 1 d . . . H27A H 0.4698 0.0519 1.2903 0.056 Uiso 1 1 calc R . . H27B H 0.3541 -0.0173 1.2281 0.056 Uiso 1 1 calc R . . H27C H 0.3049 0.0769 1.2681 0.056 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 0.02115(10) 0.02125(10) 0.01979(10) 0.00014(7) 0.00369(7) 0.00111(7) I1 0.03329(12) 0.02269(10) 0.03700(11) 0.00150(7) -0.00008(8) -0.00793(8) I2 0.03867(12) 0.03500(11) 0.02470(10) 0.00313(7) 0.01249(8) -0.00173(8) N11 0.0215(12) 0.0200(11) 0.0241(11) -0.0013(9) 0.0038(9) 0.0016(9) N21 0.0210(11) 0.0211(11) 0.0225(11) -0.0002(9) 0.0024(9) -0.0003(9) C12 0.0226(14) 0.0241(13) 0.0261(14) 0.0015(11) 0.0043(11) -0.0012(11) C13 0.0226(14) 0.0262(14) 0.0403(17) 0.0103(12) 0.0054(12) -0.0002(12) C14 0.0319(17) 0.0346(17) 0.050(2) 0.0091(14) 0.0172(14) 0.0121(14) C15 0.0363(18) 0.0412(18) 0.0378(17) -0.0076(14) 0.0140(14) 0.0068(15) C16 0.0264(15) 0.0298(15) 0.0290(15) -0.0031(11) 0.0050(12) 0.0021(12) C17 0.0275(17) 0.051(2) 0.048(2) 0.0198(17) 0.0008(15) 0.0080(15) C22 0.0259(14) 0.0218(13) 0.0243(13) 0.0013(10) 0.0047(11) -0.0008(11) C23 0.0287(15) 0.0313(15) 0.0235(14) -0.0019(11) 0.0033(11) 0.0062(12) C24 0.0223(15) 0.0372(17) 0.0301(15) -0.0124(12) -0.0006(12) 0.0027(12) C25 0.0284(16) 0.0279(15) 0.0398(17) -0.0086(12) 0.0095(13) -0.0070(12) C26 0.0291(15) 0.0261(14) 0.0305(15) 0.0015(11) 0.0089(12) -0.0031(12) C27 0.054(2) 0.050(2) 0.0245(16) 0.0030(14) 0.0067(15) 0.0012(17) _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 N11 2.275(2) . ? Cd N21 2.280(2) . ? Cd I2 2.6888(4) . ? Cd I1 2.6941(5) . ? N11 C16 1.340(4) . ? N11 C12 1.341(3) . ? N21 C22 1.342(3) . ? N21 C26 1.343(4) . ? C12 C13 1.384(4) . ? C12 H12 0.9800 . ? C13 C14 1.379(5) . ? C13 C17 1.506(4) . ? C14 C15 1.380(5) . ? C14 H14 0.9800 . ? C15 C16 1.377(4) . ? C15 H15 0.9800 . ? C16 H16 0.9800 . ? C17 H17A 0.9801 . ? C17 H17B 0.9801 . ? C17 H17C 0.9801 . ? C22 C23 1.387(4) . ? C22 H22 0.9800 . ? C23 C24 1.390(4) . ? C23 C27 1.500(4) . ? C24 C25 1.378(4) . ? C24 H24 0.9800 . ? C25 C26 1.378(4) . ? C25 H25 0.9800 . ? C26 H26 0.9800 . ? C27 H27A 0.9801 . ? C27 H27B 0.9801 . ? C27 H27C 0.9801 . ? 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 N11 Cd N21 100.02(8) . . ? N11 Cd I2 104.01(6) . . ? N21 Cd I2 108.13(6) . . ? N11 Cd I1 106.47(6) . . ? N21 Cd I1 104.37(6) . . ? I2 Cd I1 130.047(10) . . ? C16 N11 C12 118.8(2) . . ? C16 N11 Cd 121.96(18) . . ? C12 N11 Cd 119.19(18) . . ? C22 N21 C26 118.8(2) . . ? C22 N21 Cd 121.08(18) . . ? C26 N21 Cd 120.00(19) . . ? N11 C12 C13 122.7(3) . . ? N11 C12 H12 118.6 . . ? C13 C12 H12 118.6 . . ? C14 C13 C12 117.5(3) . . ? C14 C13 C17 122.8(3) . . ? C12 C13 C17 119.8(3) . . ? C13 C14 C15 120.5(3) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 118.4(3) . . ? C16 C15 H15 120.8 . . ? C14 C15 H15 120.8 . . ? N11 C16 C15 122.0(3) . . ? N11 C16 H16 119.0 . . ? C15 C16 H16 119.0 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N21 C22 C23 123.2(3) . . ? N21 C22 H22 118.4 . . ? C23 C22 H22 118.4 . . ? C22 C23 C24 116.9(3) . . ? C22 C23 C27 120.9(3) . . ? C24 C23 C27 122.1(3) . . ? C25 C24 C23 120.3(3) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C26 C25 C24 119.1(3) . . ? C26 C25 H25 120.5 . . ? C24 C25 H25 120.5 . . ? N21 C26 C25 121.7(3) . . ? N21 C26 H26 119.2 . . ? C25 C26 H26 119.2 . . ? C23 C27 H27A 109.5 . . ? C23 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C23 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.566 _refine_diff_density_min -0.776 _refine_diff_density_rms 0.105 #============================================================================== data_hc215 _database_code_depnum_ccdc_archive 'CCDC 223797' _chemical_name_common ;net-(bis(mu-chloro)-(mu-4,4'-bipyridyl)-cadmium(ii)) (Compound 13, 120K data) ; _audit_creation_date 30-OCT-03 _audit_creation_method SHELXTL _audit_update_record ; ? ; _chemical_name_systematic ; net-[bis(\m-chloro)-(\m-4,4'-bipyridyl)-cadmium(ii)] (Compound 13, 120K data) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H8 Cd Cl2 N2' _chemical_formula_weight 339.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Orthorhombic _symmetry_space_group_name_H-M Pban loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x+1/2, y, -z' 'x, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x-1/2, -y, z' '-x, y-1/2, z' _cell_length_a 11.796(3) _cell_length_b 12.084(3) _cell_length_c 3.7716(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 537.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4051 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 26.09 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.097 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 328 _exptl_absorpt_coefficient_mu 2.491 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.769297 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 4051 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0362 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 26.09 _reflns_number_total 545 _reflns_number_gt 397 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXTL (Sheldrick, 1998)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL (Sheldrick, 1998)' _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^)+(0.0235P)^2^+0.5931P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 545 _refine_ls_number_parameters 37 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0424 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_ref 0.0643 _refine_ls_wR_factor_gt 0.0586 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.116 _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 Cd Cd 0.2500 0.2500 0.5000 0.01366(19) Uani 1 4 d S . . Cl Cl 0.2500 0.09651(9) 0.0000 0.0172(3) Uani 1 2 d S . . N N 0.0513(3) 0.2500 0.5000 0.0163(9) Uani 1 2 d S . . C1 C -0.0074(3) 0.1594(3) 0.5933(11) 0.0177(10) Uani 1 1 d . . . H1 H 0.0347 0.0929 0.6630 0.023 Uiso 1 1 calc R . . C2 C -0.1261(3) 0.1556(3) 0.5953(10) 0.0171(9) Uani 1 1 d . . . H2 H -0.1659 0.0875 0.6628 0.022 Uiso 1 1 calc R . . C3 C -0.1870(4) 0.2500 0.5000 0.0156(10) Uani 1 2 d S . . 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 0.0076(3) 0.0141(3) 0.0194(3) 0.000 0.000 0.000 Cl 0.0155(6) 0.0150(6) 0.0212(7) 0.000 -0.0010(9) 0.000 N 0.0097(18) 0.017(2) 0.022(2) -0.002(3) 0.000 0.000 C1 0.0118(17) 0.0154(19) 0.026(3) 0.0041(16) -0.0004(16) 0.0023(15) C2 0.0111(17) 0.0181(19) 0.022(3) 0.0026(16) -0.0007(16) -0.0040(15) C3 0.011(2) 0.018(2) 0.017(3) -0.003(5) 0.000 0.000 _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 N 2.344(4) . ? Cd N 2.344(4) 2 ? Cd Cl 2.6451(9) 2_556 ? Cd Cl 2.6451(9) . ? Cd Cl 2.6451(9) 2 ? Cd Cl 2.6451(9) 1_556 ? Cl Cd 2.6451(9) 1_554 ? N C1 1.342(4) . ? N C1 1.342(4) 4_556 ? C1 C2 1.402(5) . ? C1 H1 0.9800 . ? C2 C3 1.395(5) . ? C2 H2 0.9800 . ? C3 C2 1.395(5) 4_556 ? C3 C3 1.487(9) 2_455 ? 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 N Cd N 180.0 . 2 ? N Cd Cl 90.0 . 2_556 ? N Cd Cl 90.0 2 2_556 ? N Cd Cl 90.0 . . ? N Cd Cl 90.0 2 . ? Cl Cd Cl 180.0 2_556 . ? N Cd Cl 90.0 . 2 ? N Cd Cl 90.0 2 2 ? Cl Cd Cl 90.95(4) 2_556 2 ? Cl Cd Cl 89.05(4) . 2 ? N Cd Cl 90.0 . 1_556 ? N Cd Cl 90.0 2 1_556 ? Cl Cd Cl 89.05(4) 2_556 1_556 ? Cl Cd Cl 90.95(4) . 1_556 ? Cl Cd Cl 180.00(3) 2 1_556 ? Cd Cl Cd 90.95(4) . 1_554 ? C1 N C1 117.9(4) . 4_556 ? C1 N Cd 121.0(2) . . ? C1 N Cd 121.0(2) 4_556 . ? N C1 C2 122.9(4) . . ? N C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C3 C2 C1 119.1(4) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C2 118.1(5) 4_556 . ? C2 C3 C3 120.9(2) 4_556 2_455 ? C2 C3 C3 120.9(2) . 2_455 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.09 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.867 _refine_diff_density_min -0.351 _refine_diff_density_rms 0.130 data_hc216 _database_code_depnum_ccdc_archive 'CCDC 223798' _chemical_name_systematic ; net-[bis(\m-choloro)-(\m-4,4'-bipyridyl)-cadmium(ii)] (Compound 13, RT data) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H8 Cd Cl2 N2' _chemical_formula_weight 339.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Orthorhombic _symmetry_space_group_name_H-M Pban loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x+1/2, y, -z' 'x, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x-1/2, -y, z' '-x, y-1/2, z' _cell_length_a 11.749(5) _cell_length_b 12.067(5) _cell_length_c 3.7748(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 535.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4065 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 26.06 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.107 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 328 _exptl_absorpt_coefficient_mu 2.502 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.642356 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (1996)' _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 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 4065 _diffrn_reflns_av_R_equivalents 0.0463 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 26.06 _reflns_number_total 539 _reflns_number_gt 385 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXTL (Sheldrick, 1998)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL (Sheldrick, 1998)' _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^)+(0.0326P)^2^+0.3185P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 539 _refine_ls_number_parameters 37 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_gt 0.0254 _refine_ls_wR_factor_ref 0.0665 _refine_ls_wR_factor_gt 0.0590 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _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 Cd Cd 0.2500 0.2500 0.5000 0.0237(2) Uani 1 4 d S . . Cl Cl 0.2500 0.09716(9) 0.0000 0.0286(3) Uani 1 2 d S . . N N 0.0511(3) 0.2500 0.5000 0.0275(9) Uani 1 2 d S . . C1 C -0.0085(4) 0.1598(4) 0.5898(12) 0.0324(11) Uani 1 1 d . . . H1 H 0.0335 0.0930 0.6582 0.042 Uiso 1 1 calc R . . C2 C -0.1258(3) 0.1559(3) 0.5914(11) 0.0300(11) Uani 1 1 d . . . H2 H -0.1655 0.0874 0.6563 0.039 Uiso 1 1 calc R . . C3 C -0.1871(4) 0.2500 0.5000 0.0263(11) Uani 1 2 d S . . 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 0.0179(3) 0.0233(3) 0.0298(3) 0.000 0.000 0.000 Cl 0.0330(6) 0.0216(6) 0.0311(7) 0.000 -0.0022(9) 0.000 N 0.0203(19) 0.024(2) 0.038(3) -0.001(3) 0.000 0.000 C1 0.0245(19) 0.026(2) 0.047(3) 0.0036(19) -0.0031(19) 0.0023(16) C2 0.0240(18) 0.0252(19) 0.041(3) 0.0028(18) 0.0011(18) -0.0037(16) C3 0.022(2) 0.028(2) 0.028(3) -0.004(5) 0.000 0.000 _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 N 2.337(4) 2 ? Cd N 2.337(4) . ? Cd Cl 2.6389(11) . ? Cd Cl 2.6389(11) 2_556 ? Cd Cl 2.6389(11) 1_556 ? Cd Cl 2.6389(11) 2 ? Cl Cd 2.6389(11) 1_554 ? N C1 1.338(5) . ? N C1 1.338(5) 4_556 ? C1 C2 1.379(6) . ? C1 H1 0.9800 . ? C2 C3 1.388(5) . ? C2 H2 0.9800 . ? C3 C2 1.388(5) 4_556 ? C3 C3 1.479(9) 2_455 ? 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 N Cd N 180.0 2 . ? N Cd Cl 90.0 2 . ? N Cd Cl 90.0 . . ? N Cd Cl 90.0 2 2_556 ? N Cd Cl 90.0 . 2_556 ? Cl Cd Cl 180.0 . 2_556 ? N Cd Cl 90.0 2 1_556 ? N Cd Cl 90.0 . 1_556 ? Cl Cd Cl 91.32(5) . 1_556 ? Cl Cd Cl 88.68(5) 2_556 1_556 ? N Cd Cl 90.0 2 2 ? N Cd Cl 90.0 . 2 ? Cl Cd Cl 88.68(5) . 2 ? Cl Cd Cl 91.32(5) 2_556 2 ? Cl Cd Cl 180.0 1_556 2 ? Cd Cl Cd 91.32(5) . 1_554 ? C1 N C1 116.9(5) . 4_556 ? C1 N Cd 121.5(2) . . ? C1 N Cd 121.5(2) 4_556 . ? N C1 C2 123.5(4) . . ? N C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C1 C2 C3 119.3(4) . . ? C1 C2 H2 120.4 . . ? C3 C2 H2 120.4 . . ? C2 C3 C2 117.5(5) 4_556 . ? C2 C3 C3 121.2(2) 4_556 2_455 ? C2 C3 C3 121.2(2) . 2_455 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.06 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.693 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.107 data_hc217 _database_code_depnum_ccdc_archive 'CCDC 223799' _chemical_name_systematic ; net-[bis(\m-choloro)-(\m-4,4'-bipyridyl)-cadmium(ii)] (Compound 13, 450K data) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H8 Cd Cl2 N2' _chemical_formula_weight 339.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Orthorhombic _symmetry_space_group_name_H-M Pban loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x+1/2, y, -z' 'x, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x-1/2, -y, z' '-x, y-1/2, z' _cell_length_a 11.753(2) _cell_length_b 12.107(3) _cell_length_c 3.7959(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 540.13(19) _cell_formula_units_Z 2 _cell_measurement_temperature 450(2) _cell_measurement_reflns_used 4096 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 26.04 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.087 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 328 _exptl_absorpt_coefficient_mu 2.479 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.668467 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 450(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 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 4096 _diffrn_reflns_av_R_equivalents 0.0510 _diffrn_reflns_av_sigmaI/netI 0.0345 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 26.04 _reflns_number_total 543 _reflns_number_gt 372 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXTL (Sheldrick, 1998)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL (Sheldrick, 1998)' _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^)+(0.0259P)^2^+0.1269P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 543 _refine_ls_number_parameters 37 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0507 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0635 _refine_ls_wR_factor_gt 0.0563 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _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 Cd Cd 0.2500 0.2500 0.5000 0.0342(2) Uani 1 4 d S . . Cl Cl 0.2500 0.09798(10) 0.0000 0.0418(3) Uani 1 2 d S . . N N 0.0506(3) 0.2500 0.5000 0.0390(10) Uani 1 2 d S . . C1 C -0.0085(4) 0.1607(4) 0.5875(13) 0.0467(14) Uani 1 1 d . . . H1 H 0.0334 0.0940 0.6555 0.061 Uiso 1 1 calc R . . C2 C -0.1259(4) 0.1570(4) 0.5875(12) 0.0450(14) Uani 1 1 d . . . H2 H -0.1656 0.0885 0.6494 0.059 Uiso 1 1 calc R . . C3 C -0.1865(4) 0.2500 0.5000 0.0343(11) Uani 1 2 d S . . 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 0.0235(3) 0.0368(3) 0.0421(4) 0.000 0.000 0.000 Cl 0.0456(7) 0.0333(6) 0.0465(8) 0.000 -0.0016(13) 0.000 N 0.025(2) 0.039(2) 0.053(3) 0.002(4) 0.000 0.000 C1 0.032(2) 0.039(2) 0.069(4) 0.009(2) -0.002(2) 0.0055(17) C2 0.031(2) 0.039(2) 0.065(4) 0.009(2) -0.004(2) -0.0067(17) C3 0.026(2) 0.039(3) 0.038(3) -0.003(6) 0.000 0.000 _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 N 2.344(4) 2 ? Cd N 2.344(4) . ? Cd Cl 2.6438(9) 2_556 ? Cd Cl 2.6438(9) . ? Cd Cl 2.6438(9) 2 ? Cd Cl 2.6438(9) 1_556 ? Cl Cd 2.6438(9) 1_554 ? N C1 1.327(5) . ? N C1 1.327(5) 4_556 ? C1 C2 1.380(6) . ? C1 H1 0.9800 . ? C2 C3 1.373(5) . ? C2 H2 0.9800 . ? C3 C2 1.373(5) 4_556 ? C3 C3 1.494(9) 2_455 ? 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 N Cd N 180.0 2 . ? N Cd Cl 90.0 2 2_556 ? N Cd Cl 90.0 . 2_556 ? N Cd Cl 90.0 2 . ? N Cd Cl 90.0 . . ? Cl Cd Cl 180.0 2_556 . ? N Cd Cl 90.0 2 2 ? N Cd Cl 90.0 . 2 ? Cl Cd Cl 91.76(4) 2_556 2 ? Cl Cd Cl 88.24(4) . 2 ? N Cd Cl 90.0 2 1_556 ? N Cd Cl 90.0 . 1_556 ? Cl Cd Cl 88.24(4) 2_556 1_556 ? Cl Cd Cl 91.76(4) . 1_556 ? Cl Cd Cl 180.00(4) 2 1_556 ? Cd Cl Cd 91.76(4) . 1_554 ? C1 N C1 116.9(5) . 4_556 ? C1 N Cd 121.5(2) . . ? C1 N Cd 121.5(2) 4_556 . ? N C1 C2 123.3(4) . . ? N C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C3 C2 C1 119.5(4) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C2 C3 C2 117.5(5) 4_556 . ? C2 C3 C3 121.2(2) 4_556 2_455 ? C2 C3 C3 121.2(2) . 2_455 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.588 _refine_diff_density_min -0.333 _refine_diff_density_rms 0.100 #========================================================================== data_hc218 _database_code_depnum_ccdc_archive 'CCDC 223800' _chemical_name_common ; net-(bis(mu-bromo)-(mu-4,4'-bipyridyl)-cadmium(ii)) (Compound 14, 120K data) ; _audit_creation_date 30-OCT-03 _audit_creation_method SHELXTL _audit_update_record ; ? ; _chemical_name_systematic ; net-[bis(\m-bromo)-(\m-4,4'-bipyridyl)-cadmium(ii)] (Compound 14, 120K data) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H8 Br2 Cd N2' _chemical_formula_weight 428.40 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' 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pban loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x+1/2, y, -z' 'x, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x-1/2, -y, z' '-x, y-1/2, z' _cell_length_a 11.7966(14) _cell_length_b 12.5019(15) _cell_length_c 3.8851(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 572.97(12) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4865 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 26.11 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.483 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 400 _exptl_absorpt_coefficient_mu 8.845 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.588648 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 4865 _diffrn_reflns_av_R_equivalents 0.0779 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 26.11 _reflns_number_total 581 _reflns_number_gt 332 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXTL (Sheldrick, 1998)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL (Sheldrick, 1998)' _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^)+(0.0347P)^2^+1.0890P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 581 _refine_ls_number_parameters 37 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0714 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0922 _refine_ls_wR_factor_gt 0.0772 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 Cd Cd 0.2500 0.2500 0.5000 0.0162(3) Uani 1 4 d S . . Br Br 0.2500 0.09254(7) 0.0000 0.0186(3) Uani 1 2 d S . . N N 0.0497(6) 0.2500 0.5000 0.0206(18) Uani 1 2 d S . . C1 C -0.0081(6) 0.1607(6) 0.580(2) 0.024(2) Uani 1 1 d . . . H1 H 0.0339 0.0957 0.6393 0.031 Uiso 1 1 calc R . . C2 C -0.1254(6) 0.1583(6) 0.5800(18) 0.020(2) Uani 1 1 d . . . H2 H -0.1647 0.0916 0.6369 0.026 Uiso 1 1 calc R . . C3 C -0.1887(7) 0.2500 0.5000 0.021(2) Uani 1 2 d S . . 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 0.0074(5) 0.0218(5) 0.0195(5) 0.000 0.000 0.000 Br 0.0154(5) 0.0219(6) 0.0184(5) 0.000 -0.0003(7) 0.000 N 0.011(4) 0.025(4) 0.026(5) -0.009(7) 0.000 0.000 C1 0.015(4) 0.016(4) 0.040(7) 0.002(3) -0.001(4) 0.001(4) C2 0.010(3) 0.023(4) 0.027(6) 0.000(3) 0.000(3) 0.000(3) C3 0.006(4) 0.033(6) 0.025(6) -0.026(10) 0.000 0.000 _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 N 2.363(7) 2 ? Cd N 2.363(7) . ? Cd Br 2.7657(6) 2_556 ? Cd Br 2.7657(6) . ? Cd Br 2.7657(6) 2 ? Cd Br 2.7657(6) 1_556 ? Br Cd 2.7657(6) 1_554 ? N C1 1.344(8) . ? N C1 1.344(8) 4_556 ? C1 C2 1.384(10) . ? C1 H1 0.9800 . ? C2 C3 1.403(8) . ? C2 H2 0.9800 . ? C3 C2 1.403(9) 4_556 ? C3 C3 1.446(16) 2_455 ? 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 N Cd N 180.0 2 . ? N Cd Br 90.0 2 2_556 ? N Cd Br 90.0 . 2_556 ? N Cd Br 90.0 2 . ? N Cd Br 90.0 . . ? Br Cd Br 180.0 2_556 . ? N Cd Br 90.0 2 2 ? N Cd Br 90.0 . 2 ? Br Cd Br 89.24(3) 2_556 2 ? Br Cd Br 90.76(3) . 2 ? N Cd Br 90.0 2 1_556 ? N Cd Br 90.0 . 1_556 ? Br Cd Br 90.76(3) 2_556 1_556 ? Br Cd Br 89.24(3) . 1_556 ? Br Cd Br 180.00(2) 2 1_556 ? Cd Br Cd 89.24(3) . 1_554 ? C1 N C1 119.0(9) . 4_556 ? C1 N Cd 120.5(4) . . ? C1 N Cd 120.5(4) 4_556 . ? N C1 C2 121.7(7) . . ? N C1 H1 119.2 . . ? C2 C1 H1 119.2 . . ? C1 C2 C3 121.0(7) . . ? C1 C2 H2 119.5 . . ? C3 C2 H2 119.5 . . ? C2 C3 C2 115.6(8) 4_556 . ? C2 C3 C3 122.2(4) 4_556 2_455 ? C2 C3 C3 122.2(4) . 2_455 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.11 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.264 _refine_diff_density_min -0.516 _refine_diff_density_rms 0.199 data_hc219 _database_code_depnum_ccdc_archive 'CCDC 223801' _chemical_name_systematic ; net-[bis(\m-beomo)-(\m-4,4'-bipyridyl)-cadmium(ii)] (Compound 14, 293K data) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H8 Br2 Cd N2' _chemical_formula_weight 428.40 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' 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pban loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x+1/2, y, -z' 'x, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x-1/2, -y, z' '-x, y-1/2, z' _cell_length_a 11.7857(10) _cell_length_b 12.5282(10) _cell_length_c 3.9105(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 577.40(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4988 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 26.06 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.464 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 400 _exptl_absorpt_coefficient_mu 8.777 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.671891 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (1996)' _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 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 4988 _diffrn_reflns_av_R_equivalents 0.0607 _diffrn_reflns_av_sigmaI/netI 0.0370 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 26.06 _reflns_number_total 580 _reflns_number_gt 336 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXTL (Sheldrick, 1998)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL (Sheldrick, 1998)' _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^)+(0.0285P)^2^+0.3286P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 580 _refine_ls_number_parameters 37 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0702 _refine_ls_wR_factor_gt 0.0597 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 Cd Cd 0.2500 0.2500 0.5000 0.0277(2) Uani 1 4 d S . . Br Br 0.2500 0.09315(5) 0.0000 0.0325(2) Uani 1 2 d S . . N N 0.0509(4) 0.2500 0.5000 0.0337(15) Uani 1 2 d S . . C1 C -0.0089(5) 0.1627(4) 0.570(2) 0.041(2) Uani 1 1 d . . . H1 H 0.0328 0.0971 0.6221 0.053 Uiso 1 1 calc R . . C2 C -0.1252(5) 0.1585(5) 0.5726(17) 0.039(2) Uani 1 1 d . . . H2 H -0.1642 0.0914 0.6257 0.050 Uiso 1 1 calc R . . C3 C -0.1874(5) 0.2500 0.5000 0.0317(17) Uani 1 2 d S . . 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 0.0170(4) 0.0323(4) 0.0340(4) 0.000 0.000 0.000 Br 0.0342(5) 0.0293(4) 0.0340(5) 0.000 -0.0026(7) 0.000 N 0.017(3) 0.033(3) 0.051(4) 0.008(6) 0.000 0.000 C1 0.022(3) 0.029(3) 0.072(7) 0.011(4) -0.004(4) 0.000(3) C2 0.026(3) 0.030(3) 0.060(6) 0.009(3) -0.006(3) -0.001(3) C3 0.021(3) 0.037(4) 0.037(4) -0.010(11) 0.000 0.000 _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 N 2.347(5) 2 ? Cd N 2.347(5) . ? Cd Br 2.7721(5) . ? Cd Br 2.7721(5) 2_556 ? Cd Br 2.7721(5) 1_556 ? Cd Br 2.7721(5) 2 ? Br Cd 2.7721(5) 1_554 ? N C1 1.329(6) . ? N C1 1.329(6) 4_556 ? C1 C2 1.372(7) . ? C1 H1 0.9800 . ? C2 C3 1.389(7) . ? C2 H2 0.9800 . ? C3 C2 1.389(7) 4_556 ? C3 C3 1.476(13) 2_455 ? 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 N Cd N 180.0 2 . ? N Cd Br 90.0 2 . ? N Cd Br 90.0 . . ? N Cd Br 90.0 2 2_556 ? N Cd Br 90.0 . 2_556 ? Br Cd Br 180.0 . 2_556 ? N Cd Br 90.0 2 1_556 ? N Cd Br 90.0 . 1_556 ? Br Cd Br 89.71(2) . 1_556 ? Br Cd Br 90.29(2) 2_556 1_556 ? N Cd Br 90.0 2 2 ? N Cd Br 90.0 . 2 ? Br Cd Br 90.29(2) . 2 ? Br Cd Br 89.71(2) 2_556 2 ? Br Cd Br 180.0 1_556 2 ? Cd Br Cd 89.71(2) . 1_554 ? C1 N C1 116.0(6) . 4_556 ? C1 N Cd 122.0(3) . . ? C1 N Cd 122.0(3) 4_556 . ? N C1 C2 124.3(6) . . ? N C1 H1 117.9 . . ? C2 C1 H1 117.9 . . ? C1 C2 C3 119.6(6) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C2 C3 C2 116.4(6) 4_556 . ? C2 C3 C3 121.8(3) 4_556 2_455 ? C2 C3 C3 121.8(3) . 2_455 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.06 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.773 _refine_diff_density_min -0.459 _refine_diff_density_rms 0.130 #============================================================================== data_hc220 _database_code_depnum_ccdc_archive 'CCDC 223802' _chemical_name_common ;net-(bis(mu-iodo)-(mu-4,4'-bipyridyl)-cadmium(ii)) (Compound 15, 120K data) ; _audit_creation_date 30-OCT-03 _audit_creation_method SHELXTL _audit_update_record ; ? ; _chemical_name_systematic ; net-[bis(\m-iodo)-(\m-4,4'-bipyridyl)-cadmium(ii)] (Compound 15, 120K data) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H8 Cd I2 N2' _chemical_formula_weight 522.38 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' I I -0.4742 1.8119 '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 Cmmm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z' 'x, -y, z' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' _cell_length_a 11.8081(12) _cell_length_b 13.0971(13) _cell_length_c 4.1423(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 640.61(11) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3294 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 26.09 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.708 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 472 _exptl_absorpt_coefficient_mu 6.494 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.717139 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 3294 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0276 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 26.09 _reflns_number_total 395 _reflns_number_gt 356 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXTL (Sheldrick, 1998)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL (Sheldrick, 1998)' _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^)+(0.0213P)^2^+0.6583P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 395 _refine_ls_number_parameters 28 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0246 _refine_ls_R_factor_gt 0.0201 _refine_ls_wR_factor_ref 0.0462 _refine_ls_wR_factor_gt 0.0445 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 Cd Cd 0.0000 0.0000 0.0000 0.01429(19) Uani 1 8 d S . . I I 0.0000 0.16236(3) 0.5000 0.01771(16) Uani 1 4 d S . . N N 0.1989(4) 0.0000 0.0000 0.0156(12) Uani 1 4 d S . . C1 C 0.2591(4) 0.0857(4) 0.0000 0.0333(14) Uani 1 2 d S . . H1 H 0.2175 0.1505 0.0000 0.043 Uiso 1 2 calc SR . . C2 C 0.3742(4) 0.0899(4) 0.0000 0.0351(15) Uani 1 2 d S . . H2 H 0.4130 0.1561 0.0000 0.046 Uiso 1 2 calc SR . . C3 C 0.4364(5) 0.0000 0.0000 0.0164(14) Uani 1 4 d S . . 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 0.0090(3) 0.0150(4) 0.0189(4) 0.000 0.000 0.000 I 0.0217(3) 0.0134(3) 0.0180(2) 0.000 0.000 0.000 N 0.011(3) 0.015(3) 0.021(3) 0.000 0.000 0.000 C1 0.012(3) 0.019(3) 0.068(4) 0.000 0.000 0.004(2) C2 0.014(3) 0.013(3) 0.078(5) 0.000 0.000 -0.006(2) C3 0.011(3) 0.021(3) 0.017(3) 0.000 0.000 0.000 _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 N 2.349(5) 9 ? Cd N 2.349(5) . ? Cd I 2.9685(3) 9 ? Cd I 2.9685(3) . ? Cd I 2.9685(3) 9_556 ? Cd I 2.9685(3) 1_554 ? I Cd 2.9685(3) 1_556 ? N C1 1.328(5) . ? N C1 1.328(5) 11 ? C1 C2 1.361(7) . ? C1 H1 0.9800 . ? C2 C3 1.388(6) . ? C2 H2 0.9800 . ? C3 C2 1.388(6) 11 ? C3 C3 1.502(12) 9_655 ? 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 N Cd N 180.0 9 . ? N Cd I 90.0 9 9 ? N Cd I 90.0 . 9 ? N Cd I 90.0 9 . ? N Cd I 90.0 . . ? I Cd I 180.000(10) 9 . ? N Cd I 90.0 9 9_556 ? N Cd I 90.0 . 9_556 ? I Cd I 88.489(13) 9 9_556 ? I Cd I 91.511(13) . 9_556 ? N Cd I 90.0 9 1_554 ? N Cd I 90.0 . 1_554 ? I Cd I 91.511(13) 9 1_554 ? I Cd I 88.489(13) . 1_554 ? I Cd I 180.000(10) 9_556 1_554 ? Cd I Cd 88.489(13) . 1_556 ? C1 N C1 115.4(6) . 11 ? C1 N Cd 122.3(3) . . ? C1 N Cd 122.3(3) 11 . ? N C1 C2 124.7(5) . . ? N C1 H1 117.7 . . ? C2 C1 H1 117.7 . . ? C1 C2 C3 119.6(5) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C2 C3 C2 116.1(6) 11 . ? C2 C3 C3 121.9(3) 11 9_655 ? C2 C3 C3 121.9(3) . 9_655 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.09 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.872 _refine_diff_density_min -0.565 _refine_diff_density_rms 0.136 data_hc242 _database_code_depnum_ccdc_archive 'CCDC 223803' _chemical_name_systematic ; net-[bis(\m-iodo)-(\m-4,4'-bipyridyl)-cadmium(ii)] (Compound 15, 150K data) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H8 Cd I2 N2' _chemical_formula_weight 522.38 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' I I -0.4742 1.8119 '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 Cmmm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z' 'x, -y, z' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' _cell_length_a 11.837(2) _cell_length_b 13.138(3) _cell_length_c 4.1550(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 646.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2217 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 26.07 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.685 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 472 _exptl_absorpt_coefficient_mu 6.438 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.719016 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 2217 _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 3 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 26.07 _reflns_number_total 397 _reflns_number_gt 344 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXTL (Sheldrick, 1998)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL (Sheldrick, 1998)' _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^)+(0.0326P)^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_extinction_coef ? _refine_ls_number_reflns 397 _refine_ls_number_parameters 28 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0309 _refine_ls_R_factor_gt 0.0246 _refine_ls_wR_factor_ref 0.0582 _refine_ls_wR_factor_gt 0.0565 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 Cd Cd 0.0000 0.0000 0.0000 0.0177(2) Uani 1 8 d S . . I I 0.0000 0.16222(4) 0.5000 0.0218(2) Uani 1 4 d S . . N N 0.2007(6) 0.0000 0.0000 0.0198(16) Uani 1 4 d S . . C1 C 0.2589(6) 0.0859(5) 0.0000 0.039(2) Uani 1 2 d S . . H1 H 0.2174 0.1505 0.0000 0.051 Uiso 1 2 calc SR . . C2 C 0.3747(6) 0.0888(5) 0.0000 0.041(2) Uani 1 2 d S . . H2 H 0.4134 0.1548 0.0000 0.053 Uiso 1 2 calc SR . . C3 C 0.4379(7) 0.0000 0.0000 0.0179(18) Uani 1 4 d S . . 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 0.0101(4) 0.0214(4) 0.0217(5) 0.000 0.000 0.000 I 0.0255(3) 0.0192(3) 0.0208(3) 0.000 0.000 0.000 N 0.013(4) 0.019(3) 0.028(4) 0.000 0.000 0.000 C1 0.015(3) 0.026(3) 0.077(6) 0.000 0.000 0.001(3) C2 0.019(4) 0.018(3) 0.085(7) 0.000 0.000 0.001(3) C3 0.016(5) 0.021(4) 0.017(4) 0.000 0.000 0.000 _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 N 2.375(7) 9 ? Cd N 2.375(7) . ? Cd I 2.9763(5) 9 ? Cd I 2.9763(5) . ? Cd I 2.9763(5) 9_556 ? Cd I 2.9763(5) 1_554 ? I Cd 2.9763(5) 1_556 ? N C1 1.323(7) . ? N C1 1.323(7) 11 ? C1 C2 1.371(9) . ? C1 H1 0.9800 . ? C2 C3 1.386(8) . ? C2 H2 0.9800 . ? C3 C2 1.386(8) 11 ? C3 C3 1.470(17) 9_655 ? 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 N Cd N 180.0 9 . ? N Cd I 90.0 9 9 ? N Cd I 90.0 . 9 ? N Cd I 90.0 9 . ? N Cd I 90.0 . . ? I Cd I 180.000(14) 9 . ? N Cd I 90.0 9 9_556 ? N Cd I 90.0 . 9_556 ? I Cd I 88.54(2) 9 9_556 ? I Cd I 91.46(2) . 9_556 ? N Cd I 90.0 9 1_554 ? N Cd I 90.0 . 1_554 ? I Cd I 91.46(2) 9 1_554 ? I Cd I 88.54(2) . 1_554 ? I Cd I 180.000(14) 9_556 1_554 ? Cd I Cd 88.54(2) . 1_556 ? C1 N C1 117.2(8) . 11 ? C1 N Cd 121.4(4) . . ? C1 N Cd 121.4(4) 11 . ? N C1 C2 123.0(6) . . ? N C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C1 C2 C3 121.1(6) . . ? C1 C2 H2 119.5 . . ? C3 C2 H2 119.5 . . ? C2 C3 C2 114.7(8) 11 . ? C2 C3 C3 122.7(4) 11 9_655 ? C2 C3 C3 122.7(4) . 9_655 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.07 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.125 _refine_diff_density_min -0.591 _refine_diff_density_rms 0.195 data_hc243 _database_code_depnum_ccdc_archive 'CCDC 223804' _chemical_name_systematic ; net-[bis(\m-iodo)-(\m-4,4'-bipyridyl)-cadmium(ii)] (Compound 15, 180K data) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H8 Cd I2 N2' _chemical_formula_weight 522.38 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' I I -0.4742 1.8119 '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 Cmmm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z' 'x, -y, z' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' _cell_length_a 11.830(2) _cell_length_b 13.138(2) _cell_length_c 4.1569(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 646.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 2216 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 26.08 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.685 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 472 _exptl_absorpt_coefficient_mu 6.439 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.683807 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 2216 _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 3 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 26.08 _reflns_number_total 397 _reflns_number_gt 343 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXTL (Sheldrick, 1998)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL (Sheldrick, 1998)' _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^)+(0.0377P)^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_extinction_coef ? _refine_ls_number_reflns 397 _refine_ls_number_parameters 28 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0328 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0650 _refine_ls_wR_factor_gt 0.0630 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 Cd Cd 0.0000 0.0000 0.0000 0.0203(3) Uani 1 8 d S . . I I 0.0000 0.16202(4) 0.5000 0.0249(2) Uani 1 4 d S . . N N 0.2004(6) 0.0000 0.0000 0.0231(17) Uani 1 4 d S . . C1 C 0.2584(6) 0.0859(5) 0.0000 0.047(2) Uani 1 2 d S . . H1 H 0.2167 0.1504 0.0000 0.061 Uiso 1 2 calc SR . . C2 C 0.3753(6) 0.0888(5) 0.0000 0.042(2) Uani 1 2 d S . . H2 H 0.4145 0.1545 0.0000 0.055 Uiso 1 2 calc SR . . C3 C 0.4365(7) 0.0000 0.0000 0.0202(19) Uani 1 4 d S . . 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 0.0118(5) 0.0243(5) 0.0249(5) 0.000 0.000 0.000 I 0.0298(4) 0.0215(3) 0.0235(4) 0.000 0.000 0.000 N 0.014(4) 0.026(4) 0.028(5) 0.000 0.000 0.000 C1 0.017(4) 0.027(4) 0.098(7) 0.000 0.000 0.002(3) C2 0.021(4) 0.019(4) 0.086(7) 0.000 0.000 -0.004(3) C3 0.013(5) 0.023(4) 0.025(5) 0.000 0.000 0.000 _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 N 2.371(8) 9 ? Cd N 2.371(8) . ? Cd I 2.9750(6) 9 ? Cd I 2.9750(6) . ? Cd I 2.9750(6) 9_556 ? Cd I 2.9750(6) 1_554 ? I Cd 2.9750(6) 1_556 ? N C1 1.320(8) . ? N C1 1.320(8) 11 ? C1 C2 1.384(10) . ? C1 H1 0.9800 . ? C2 C3 1.374(8) . ? C2 H2 0.9800 . ? C3 C2 1.374(8) 11 ? C3 C3 1.502(17) 9_655 ? 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 N Cd N 180.0 9 . ? N Cd I 90.0 9 9 ? N Cd I 90.0 . 9 ? N Cd I 90.0 9 . ? N Cd I 90.0 . . ? I Cd I 180.000(15) 9 . ? N Cd I 90.0 9 9_556 ? N Cd I 90.0 . 9_556 ? I Cd I 88.63(2) 9 9_556 ? I Cd I 91.37(2) . 9_556 ? N Cd I 90.0 9 1_554 ? N Cd I 90.0 . 1_554 ? I Cd I 91.37(2) 9 1_554 ? I Cd I 88.63(2) . 1_554 ? I Cd I 180.000(15) 9_556 1_554 ? Cd I Cd 88.63(2) . 1_556 ? C1 N C1 117.4(9) . 11 ? C1 N Cd 121.3(4) . . ? C1 N Cd 121.3(4) 11 . ? N C1 C2 122.9(7) . . ? N C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C2 C1 120.2(6) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C2 C3 C2 116.3(8) 11 . ? C2 C3 C3 121.8(4) 11 9_655 ? C2 C3 C3 121.8(4) . 9_655 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.08 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.126 _refine_diff_density_min -0.597 _refine_diff_density_rms 0.194 data_hc244 _database_code_depnum_ccdc_archive 'CCDC 223805' _chemical_name_systematic ; net-[bis(\m-iodo)-(\m-4,4'-bipyridyl)-cadmium(ii)] (Compound 15, 210K data) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H8 Cd I2 N2' _chemical_formula_weight 522.38 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' I I -0.4742 1.8119 '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 Cmmm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z' 'x, -y, z' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' _cell_length_a 11.822(2) _cell_length_b 13.135(2) _cell_length_c 4.1591(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 645.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used 2222 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 26.04 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.686 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 472 _exptl_absorpt_coefficient_mu 6.441 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.702538 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 210(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 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 2222 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_sigmaI/netI 0.0290 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 3 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 26.04 _reflns_number_total 397 _reflns_number_gt 341 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXTL (Sheldrick, 1998)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL (Sheldrick, 1998)' _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^)+(0.0327P)^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_extinction_coef ? _refine_ls_number_reflns 397 _refine_ls_number_parameters 28 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0331 _refine_ls_R_factor_gt 0.0254 _refine_ls_wR_factor_ref 0.0609 _refine_ls_wR_factor_gt 0.0581 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 Cd Cd 0.0000 0.0000 0.0000 0.0230(3) Uani 1 8 d S . . I I 0.0000 0.16193(4) 0.5000 0.0278(2) Uani 1 4 d S . . N N 0.2000(6) 0.0000 0.0000 0.0265(18) Uani 1 4 d S . . C1 C 0.2591(6) 0.0853(5) 0.0000 0.048(2) Uani 1 2 d S . . H1 H 0.2177 0.1500 0.0000 0.063 Uiso 1 2 calc SR . . C2 C 0.3751(6) 0.0887(5) 0.0000 0.048(2) Uani 1 2 d S . . H2 H 0.4141 0.1546 0.0000 0.062 Uiso 1 2 calc SR . . C3 C 0.4371(7) 0.0000 0.0000 0.025(2) Uani 1 4 d S . . 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 0.0137(5) 0.0277(5) 0.0277(6) 0.000 0.000 0.000 I 0.0327(4) 0.0247(3) 0.0260(4) 0.000 0.000 0.000 N 0.014(4) 0.025(4) 0.040(5) 0.000 0.000 0.000 C1 0.021(4) 0.027(4) 0.097(7) 0.000 0.000 0.002(3) C2 0.020(4) 0.026(4) 0.099(7) 0.000 0.000 -0.002(3) C3 0.009(5) 0.033(5) 0.033(5) 0.000 0.000 0.000 _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 N 2.365(8) 9 ? Cd N 2.365(8) . ? Cd I 2.9746(6) 9 ? Cd I 2.9746(6) . ? Cd I 2.9746(6) 9_556 ? Cd I 2.9746(6) 1_554 ? I Cd 2.9746(6) 1_556 ? N C1 1.321(8) . ? N C1 1.321(8) 11 ? C1 C2 1.372(10) . ? C1 H1 0.9800 . ? C2 C3 1.377(8) . ? C2 H2 0.9800 . ? C3 C2 1.377(8) 11 ? C3 C3 1.486(17) 9_655 ? 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 N Cd N 180.0 9 . ? N Cd I 90.0 9 9 ? N Cd I 90.0 . 9 ? N Cd I 90.0 9 . ? N Cd I 90.0 . . ? I Cd I 180.000(15) 9 . ? N Cd I 90.0 9 9_556 ? N Cd I 90.0 . 9_556 ? I Cd I 88.71(2) 9 9_556 ? I Cd I 91.29(2) . 9_556 ? N Cd I 90.0 9 1_554 ? N Cd I 90.0 . 1_554 ? I Cd I 91.29(2) 9 1_554 ? I Cd I 88.71(2) . 1_554 ? I Cd I 180.000(15) 9_556 1_554 ? Cd I Cd 88.71(2) . 1_556 ? C1 N C1 116.1(9) . 11 ? C1 N Cd 121.9(4) . . ? C1 N Cd 121.9(4) 11 . ? N C1 C2 123.8(7) . . ? N C1 H1 118.1 . . ? C2 C1 H1 118.1 . . ? C1 C2 C3 120.3(7) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C2 C3 C2 115.7(9) 11 . ? C2 C3 C3 122.2(4) 11 9_655 ? C2 C3 C3 122.2(4) . 9_655 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.053 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.193 data_hc245 _database_code_depnum_ccdc_archive 'CCDC 223806' _chemical_name_systematic ; net-[bis(\m-iodo)-(\m-4,4'-bipyridyl)-cadmium(ii)] (Compound 15, 240K data) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H8 Cd I2 N2' _chemical_formula_weight 522.38 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' I I -0.4742 1.8119 '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 Cmmm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z' 'x, -y, z' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' _cell_length_a 11.830(2) _cell_length_b 13.150(2) _cell_length_c 4.1667(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 648.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 240(2) _cell_measurement_reflns_used 2218 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 26.01 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.677 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 472 _exptl_absorpt_coefficient_mu 6.418 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.765472 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 240(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 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 2218 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0303 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 3 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 26.01 _reflns_number_total 396 _reflns_number_gt 337 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXTL (Sheldrick, 1998)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL (Sheldrick, 1998)' _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^)+(0.0385P)^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_extinction_coef ? _refine_ls_number_reflns 396 _refine_ls_number_parameters 28 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0374 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0687 _refine_ls_wR_factor_gt 0.0643 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 Cd Cd 0.0000 0.0000 0.0000 0.0256(3) Uani 1 8 d S . . I I 0.0000 0.16177(4) 0.5000 0.0311(3) Uani 1 4 d S . . N N 0.2002(7) 0.0000 0.0000 0.0286(19) Uani 1 4 d S . . C1 C 0.2588(6) 0.0847(5) 0.0000 0.053(3) Uani 1 2 d S . . H1 H 0.2174 0.1492 0.0000 0.068 Uiso 1 2 calc SR . . C2 C 0.3757(6) 0.0881(6) 0.0000 0.053(3) Uani 1 2 d S . . H2 H 0.4150 0.1537 0.0000 0.069 Uiso 1 2 calc SR . . C3 C 0.4360(7) 0.0000 0.0000 0.025(2) Uani 1 4 d S . . 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 0.0141(5) 0.0316(5) 0.0312(6) 0.000 0.000 0.000 I 0.0366(4) 0.0272(4) 0.0294(4) 0.000 0.000 0.000 N 0.014(4) 0.029(4) 0.043(5) 0.000 0.000 0.000 C1 0.021(4) 0.028(4) 0.109(8) 0.000 0.000 -0.001(3) C2 0.017(4) 0.029(4) 0.112(8) 0.000 0.000 -0.005(3) C3 0.011(5) 0.038(5) 0.025(5) 0.000 0.000 0.000 _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 N 2.368(8) 9 ? Cd N 2.368(8) . ? Cd I 2.9775(6) 9 ? Cd I 2.9775(6) . ? Cd I 2.9775(6) 9_556 ? Cd I 2.9775(6) 1_554 ? I Cd 2.9775(6) 1_556 ? N C1 1.312(8) . ? N C1 1.312(8) 11 ? C1 C2 1.384(10) . ? C1 H1 0.9800 . ? C2 C3 1.360(9) . ? C2 H2 0.9800 . ? C3 C2 1.360(9) 11 ? C3 C3 1.515(17) 9_655 ? 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 N Cd N 180.0 9 . ? N Cd I 90.0 9 9 ? N Cd I 90.0 . 9 ? N Cd I 90.0 9 . ? N Cd I 90.0 . . ? I Cd I 180.000(16) 9 . ? N Cd I 90.0 9 9_556 ? N Cd I 90.0 . 9_556 ? I Cd I 88.80(2) 9 9_556 ? I Cd I 91.20(2) . 9_556 ? N Cd I 90.0 9 1_554 ? N Cd I 90.0 . 1_554 ? I Cd I 91.20(2) 9 1_554 ? I Cd I 88.80(2) . 1_554 ? I Cd I 180.000(16) 9_556 1_554 ? Cd I Cd 88.80(2) . 1_556 ? C1 N C1 116.2(9) . 11 ? C1 N Cd 121.9(5) . . ? C1 N Cd 121.9(5) 11 . ? N C1 C2 123.8(7) . . ? N C1 H1 118.1 . . ? C2 C1 H1 118.1 . . ? C3 C2 C1 119.7(7) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C2 116.8(9) 11 . ? C2 C3 C3 121.6(5) 11 9_655 ? C2 C3 C3 121.6(5) . 9_655 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.199 _refine_diff_density_min -0.503 _refine_diff_density_rms 0.195 data_hc246 _database_code_depnum_ccdc_archive 'CCDC 223807' _chemical_name_systematic ; net-[bis(\m-iodo)-(\m-4,4'-bipyridyl)-cadmium(ii)] (Compound 15, 270K data) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H8 Cd I2 N2' _chemical_formula_weight 522.38 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' I I -0.4742 1.8119 '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 Cmmm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z' 'x, -y, z' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' _cell_length_a 11.792(2) _cell_length_b 13.118(3) _cell_length_c 4.1585(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 643.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 270(2) _cell_measurement_reflns_used 2209 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 25.96 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.697 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 472 _exptl_absorpt_coefficient_mu 6.467 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.638711 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 270(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 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 2209 _diffrn_reflns_av_R_equivalents 0.0428 _diffrn_reflns_av_sigmaI/netI 0.0300 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 3 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 25.96 _reflns_number_total 394 _reflns_number_gt 333 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXTL (Sheldrick, 1998)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL (Sheldrick, 1998)' _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^)+(0.0332P)^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_extinction_coef ? _refine_ls_number_reflns 394 _refine_ls_number_parameters 28 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0362 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0658 _refine_ls_wR_factor_gt 0.0625 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _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 Cd Cd 0.0000 0.0000 0.0000 0.0288(3) Uani 1 8 d S . . I I 0.0000 0.16167(5) 0.5000 0.0346(3) Uani 1 4 d S . . N N 0.2003(7) 0.0000 0.0000 0.0277(18) Uani 1 4 d S . . C1 C 0.2592(7) 0.0847(5) 0.0000 0.059(3) Uani 1 2 d S . . H1 H 0.2178 0.1494 0.0000 0.077 Uiso 1 2 calc SR . . C2 C 0.3761(7) 0.0880(6) 0.0000 0.058(3) Uani 1 2 d S . . H2 H 0.4155 0.1538 0.0000 0.076 Uiso 1 2 calc SR . . C3 C 0.4364(8) 0.0000 0.0000 0.029(2) Uani 1 4 d S . . 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 0.0173(5) 0.0353(6) 0.0339(6) 0.000 0.000 0.000 I 0.0411(5) 0.0309(4) 0.0318(4) 0.000 0.000 0.000 N 0.018(4) 0.028(4) 0.038(5) 0.000 0.000 0.000 C1 0.024(4) 0.035(4) 0.119(9) 0.000 0.000 0.004(4) C2 0.023(4) 0.030(4) 0.121(9) 0.000 0.000 -0.009(3) C3 0.020(5) 0.032(5) 0.034(6) 0.000 0.000 0.000 _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 N 2.362(8) 9 ? Cd N 2.362(8) . ? Cd I 2.9700(6) 9 ? Cd I 2.9700(6) . ? Cd I 2.9700(6) 9_556 ? Cd I 2.9700(6) 1_554 ? I Cd 2.9700(6) 1_556 ? N C1 1.310(9) . ? N C1 1.310(9) 11 ? C1 C2 1.379(10) . ? C1 H1 0.9800 . ? C2 C3 1.356(9) . ? C2 H2 0.9800 . ? C3 C2 1.356(9) 11 ? C3 C3 1.500(19) 9_655 ? 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 N Cd N 180.0 9 . ? N Cd I 90.0 9 9 ? N Cd I 90.0 . 9 ? N Cd I 90.0 9 . ? N Cd I 90.0 . . ? I Cd I 180.000(17) 9 . ? N Cd I 90.0 9 9_556 ? N Cd I 90.0 . 9_556 ? I Cd I 88.87(2) 9 9_556 ? I Cd I 91.13(2) . 9_556 ? N Cd I 90.0 9 1_554 ? N Cd I 90.0 . 1_554 ? I Cd I 91.13(2) 9 1_554 ? I Cd I 88.87(2) . 1_554 ? I Cd I 180.000(17) 9_556 1_554 ? Cd I Cd 88.87(2) . 1_556 ? C1 N C1 116.0(9) . 11 ? C1 N Cd 122.0(5) . . ? C1 N Cd 122.0(5) 11 . ? N C1 C2 123.8(7) . . ? N C1 H1 118.1 . . ? C2 C1 H1 118.1 . . ? C3 C2 C1 119.8(7) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C2 116.7(9) 11 . ? C2 C3 C3 121.6(5) 11 9_655 ? C2 C3 C3 121.6(5) . 9_655 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.96 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.960 _refine_diff_density_min -0.588 _refine_diff_density_rms 0.194 data_hc223 _database_code_depnum_ccdc_archive 'CCDC 223808' _chemical_name_systematic ; net-[bis(\m-iodo)-(\m-4,4'-bipyridyl)-cadmium(ii)] (Compound 15, 293K data) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H8 Cd I2 N2' _chemical_formula_weight 522.38 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' I I -0.4742 1.8119 '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 Cmmm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z' 'x, -y, z' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' _cell_length_a 11.8280(11) _cell_length_b 13.1531(11) _cell_length_c 4.1751(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 649.54(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3349 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 26.04 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.671 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 472 _exptl_absorpt_coefficient_mu 6.404 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.686404 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (1996)' _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 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 3349 _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_av_sigmaI/netI 0.0282 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 26.04 _reflns_number_total 399 _reflns_number_gt 325 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXTL (Sheldrick, 1998)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL (Sheldrick, 1998)' _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^)+(0.0213P)^2^+0.6583P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 399 _refine_ls_number_parameters 28 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0559 _refine_ls_wR_factor_gt 0.0538 _refine_ls_goodness_of_fit_ref 1.217 _refine_ls_restrained_S_all 1.217 _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 Cd Cd 0.0000 0.0000 0.0000 0.0313(3) Uani 1 8 d S . . I I 0.0000 0.16150(5) 0.5000 0.0378(2) Uani 1 4 d S . . N N 0.1996(6) 0.0000 0.0000 0.0358(19) Uani 1 4 d S . . C1 C 0.2592(6) 0.0842(6) 0.0000 0.063(3) Uani 1 2 d S . . H1 H 0.2177 0.1487 0.0000 0.082 Uiso 1 2 calc SR . . C2 C 0.3749(6) 0.0888(5) 0.0000 0.062(3) Uani 1 2 d S . . H2 H 0.4134 0.1547 0.0000 0.080 Uiso 1 2 calc SR . . C3 C 0.4366(7) 0.0000 0.0000 0.034(2) Uani 1 4 d S . . 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 0.0190(5) 0.0367(6) 0.0383(6) 0.000 0.000 0.000 I 0.0449(4) 0.0324(4) 0.0360(4) 0.000 0.000 0.000 N 0.020(4) 0.033(5) 0.054(5) 0.000 0.000 0.000 C1 0.023(4) 0.040(5) 0.126(8) 0.000 0.000 0.005(4) C2 0.029(4) 0.026(4) 0.129(8) 0.000 0.000 -0.003(4) C3 0.017(5) 0.039(6) 0.044(6) 0.000 0.000 0.000 _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 N 2.361(7) 9 ? Cd N 2.361(7) . ? Cd I 2.9783(5) 9 ? Cd I 2.9783(5) . ? Cd I 2.9783(5) 9_556 ? Cd I 2.9783(5) 1_554 ? I Cd 2.9783(5) 1_556 ? N C1 1.312(8) . ? N C1 1.312(8) 11 ? C1 C2 1.370(9) . ? C1 H1 0.9800 . ? C2 C3 1.377(8) . ? C2 H2 0.9800 . ? C3 C2 1.377(8) 11 ? C3 C3 1.500(16) 9_655 ? 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 N Cd N 180.0 9 . ? N Cd I 90.0 9 9 ? N Cd I 90.0 . 9 ? N Cd I 90.0 9 . ? N Cd I 90.0 . . ? I Cd I 180.000(17) 9 . ? N Cd I 90.0 9 9_556 ? N Cd I 90.0 . 9_556 ? I Cd I 89.001(18) 9 9_556 ? I Cd I 90.999(18) . 9_556 ? N Cd I 90.0 9 1_554 ? N Cd I 90.0 . 1_554 ? I Cd I 90.999(18) 9 1_554 ? I Cd I 89.001(18) . 1_554 ? I Cd I 180.000(17) 9_556 1_554 ? Cd I Cd 89.001(18) . 1_556 ? C1 N C1 115.1(9) . 11 ? C1 N Cd 122.5(4) . . ? C1 N Cd 122.5(4) 11 . ? N C1 C2 125.0(7) . . ? N C1 H1 117.5 . . ? C2 C1 H1 117.5 . . ? C1 C2 C3 119.5(7) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C2 C3 C2 116.0(9) 11 . ? C2 C3 C3 122.0(4) 11 9_655 ? C2 C3 C3 122.0(4) . 9_655 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.766 _refine_diff_density_min -0.455 _refine_diff_density_rms 0.161