############################################################################## ### ### ### Electronic paper (Acta Crystallographica Section E) ### ### ### ############################################################################## # # # This CIF contains the data in a paper accepted for publication in Acta # # Crystallographica Section E. It conforms to the requirements of Notes # # for Authors for Section E, and has been peer reviewed under the auspices # # of the IUCr Commission on Journals. # # # # Full details of the Crystallographic Information File format # # are given in the paper "The Crystallographic Information File (CIF): # # a New Standard Archive File for Crystallography" by S. R. Hall, F. H. # # Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. # # # # The current version of the core CIF dictionary is obtainable from # # ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.4. # # # # Software is freely available for graphical display of the structure(s) in # # this CIF. For information consult the CIF home page http://www.iucr.org/ # # cif/home.html # # # # This file may be used for bona fide research purposes within the # # scientific community so long as proper attribution is given to the journal # # article from which it was obtained. # # # ############################################################################## data_I _audit_creation_method SHELXL-97 _chemical_name_systematic ; catena-Poly[[chloridomercury(II)]-\m-1,4-diazabicyclo[2,2,2]octane- \k^2^N:N'-[chloridomercury(II)]-di-\m-chlorido] ; _chemical_name_common ? _chemical_formula_moiety 'C3 H6 Cl2 Hg N' _chemical_formula_sum 'C3 H6 Cl2 Hg N' _chemical_formula_iupac '[Hg2 Cl4 (C6 H12 N2)]' _chemical_formula_weight 327.58 _chemical_melting_point ? _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'C m c m' _symmetry_space_group_name_Hall '-C 2c 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z-1/2' 'x+1/2, -y+1/2, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 9.2518(9) _cell_length_b 8.8244(9) _cell_length_c 14.7531(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1204.47(18) _cell_formula_units_Z 8 _cell_measurement_reflns_used 453 _cell_measurement_theta_min 3.1837 _cell_measurement_theta_max 30.2997 _cell_measurement_temperature 293(2) _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 3.613 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 26.311 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.3529 _exptl_absorpt_correction_T_max 0.6212 _exptl_special_details ; ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area-detector' _diffrn_measurement_method '\f and \w' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 1322 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0714 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measured_fraction_theta_full 0.988 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _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^ > \s(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. ; _reflns_number_total 586 _reflns_number_gt 392 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0601 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.0470 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.956 _refine_ls_number_reflns 586 _refine_ls_number_parameters 39 _refine_ls_number_restraints 6 _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0085P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.406 _refine_diff_density_min -1.591 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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' 'Hg' 'Hg' -2.3894 9.2266 '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' _computing_data_collection 'SMART (Bruker, 2007)' _computing_cell_refinement 'SAINT (Bruker, 2007)' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009)' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Hg Hg1 0.5000 0.22915(6) 0.51455(3) 0.0533(2) Uani d S 1 . . C C1 0.5000 0.0735(12) 0.6983(7) 0.036(3) Uani d S 1 . . H H1A 0.5849 0.0205 0.6763 0.043 Uiso calc PR 0.50 . . H H1B 0.4151 0.0205 0.6763 0.043 Uiso calc PR 0.50 . . C C2 0.3708(8) 0.3114(9) 0.6975(5) 0.032(2) Uani d . 1 . . H H2A 0.2843 0.2615 0.6754 0.039 Uiso calc R 1 . . H H2B 0.3704 0.4150 0.6754 0.039 Uiso calc R 1 . . Cl Cl1 0.2906(3) 0.0000 0.5000 0.0344(8) Uani d S 1 . . Cl Cl2 0.5000 0.3087(3) 0.3653(2) 0.0349(9) Uani d S 1 . . N N1 0.5000 0.2318(11) 0.6631(6) 0.022(2) Uani d SU 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Hg1 0.0692(4) 0.0785(5) 0.0122(3) 0.000 0.000 0.0076(3) C1 0.055(9) 0.017(6) 0.036(8) 0.000 0.000 0.006(5) C2 0.016(5) 0.050(6) 0.031(5) -0.003(4) -0.003(4) 0.008(4) Cl1 0.0244(17) 0.0511(18) 0.028(2) 0.000 0.000 -0.0067(17) Cl2 0.042(2) 0.043(2) 0.0198(16) 0.000 0.000 0.0094(13) N1 0.022(2) 0.022(2) 0.022(2) 0.000 0.000 0.0000(10) _geom_special_details ; All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Hg1 N1 . 2.192(8) n Hg1 Cl2 . 2.311(3) n Hg1 Cl1 9_656 2.8083(17) ? Hg1 Cl1 . 2.8083(17) n C1 N1 . 1.490(13) ? C1 C1 10_557 1.52(2) ? C1 H1A . 0.9700 ? C1 H1B . 0.9700 ? C2 N1 . 1.476(9) ? C2 C2 10_557 1.549(15) ? C2 H2A . 0.9700 ? C2 H2B . 0.9700 ? Cl1 Hg1 9_656 2.8083(17) ? N1 C2 12_655 1.476(9) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 Hg1 Cl2 . . 161.7(3) ? N1 Hg1 Cl1 . 9_656 94.82(18) ? Cl2 Hg1 Cl1 . 9_656 98.39(5) ? N1 Hg1 Cl1 . . 94.82(18) ? Cl2 Hg1 Cl1 . . 98.39(5) ? Cl1 Hg1 Cl1 9_656 . 87.21(7) ? N1 C1 C1 . 10_557 110.4(5) ? N1 C1 H1A . . 109.6 ? C1 C1 H1A 10_557 . 109.6 ? N1 C1 H1B . . 109.6 ? C1 C1 H1B 10_557 . 109.6 ? H1A C1 H1B . . 108.1 ? N1 C2 C2 . 10_557 110.1(4) ? N1 C2 H2A . . 109.6 ? C2 C2 H2A 10_557 . 109.6 ? N1 C2 H2B . . 109.6 ? C2 C2 H2B 10_557 . 109.6 ? H2A C2 H2B . . 108.2 ? Hg1 Cl1 Hg1 . 9_656 92.79(7) ? C2 N1 C2 12_655 . 108.1(8) ? C2 N1 C1 12_655 . 109.1(6) ? C2 N1 C1 . . 109.1(6) ? C2 N1 Hg1 12_655 . 110.4(5) ? C2 N1 Hg1 . . 110.4(5) ? C1 N1 Hg1 . . 109.8(6) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA C2 H2A Cl2 8_456 0.97 2.77 3.708(8) 163 C2 H2B Cl2 4_566 0.97 2.78 3.678(8) 154 data_global _journal_date_recd_electronic 2009-09-25 _journal_date_accepted 2009-10-22 _journal_name_full 'Acta Crystallographica, Section E' _journal_year 2009 _journal_volume 65 _journal_issue 11 _journal_page_first m1477 _journal_page_last m1478 _journal_paper_category QM _journal_coeditor_code SU2148 _publ_contact_author_name 'Chun-Sen Liu and Shao-Ming Fang' _publ_contact_author_address ; Zhengzhou University of Light Industry, Henan Provincial Key Laboratory of Surface & Interface Science, Henan, Zhengzhou 450002 People's Republic of China ; _publ_contact_author_email humin@zzuli.edu.cn _publ_contact_author_fax ? _publ_contact_author_phone ? _publ_section_title ;\ catena-Poly[[chloridomercury(II)]-\m-1,4-diazabicyclo[2.2.2]octane-\ \k^2^N:N'-[chloridomercury(II)]-di-\m-chlorido] ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Fang, Shao-Ming' . ; Zhengzhou University of Light Industry, Henan Provincial Key Laboratory of Surface & Interface Science, Henan, Zhengzhou 450002 People's Republic of China ; 'Xianguo Xiao' . ; College of Mechanical Engineering, Zhengzhou University, Henan, Zhengzhou 450001 People's Republic of China ; 'Hu, Min' . ; Zhengzhou University of Light Industry, Henan Provincial Key Laboratory of Surface & Interface Science, Henan, Zhengzhou 450002 People's Republic of China ; 'Ma, Song-Tao' . ; Zhengzhou University of Light Industry, Henan Provincial Key Laboratory of Surface & Interface Science, Henan, Zhengzhou 450002 People's Republic of China ; 'Liu, Chun-Sen' . ; Zhengzhou University of Light Industry, Henan Provincial Key Laboratory of Surface & Interface Science, Henan, Zhengzhou 450002 People's Republic of China ;