Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global #============================================================================== _journal_coden_Cambridge 222 # SUBMISSION DETAILS # ================== _publ_contact_author_name 'Professor Gillian Reid' _publ_contact_author_address ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; _publ_contact_author_email gr@soton.ac.uk _publ_contact_author_fax '023 8059 3781' _publ_contact_author_phone '023 8059 3609' _publ_contact_letter ; June 2007 This file contains crystallographic data in cif format for five crystal structures. It is being offered as supplementary information to accompany a paper being submitted to Dalton Trans. Gillian Reid ; _publ_requested_journal 'Dalton Trans.' _publ_requested_category ? #============================================================================ # TITLE AND AUTHOR LIST # ===================== _publ_section_title ; Thio- and seleno-ether complexes with Group 4 tetrahalides and tin tetrachloride: preparation and use in CVD for metal chalcogenide films ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. # Note order: Family_name, first name(s) or initials (or mixture). loop_ _publ_author_name _publ_author_address 'Reid, Stuart D.' ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; 'Hector, Andrew L.' ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; 'Levason, William' ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; 'Reid, Gillian' ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; 'Waller, Benjamin J.' ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; 'Webster, Michael' ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; #============================================================================ # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique (to this file) identifier. #============================================================================ # 06sdr001a data_06sdr001a _database_code_depnum_ccdc_archive 'CCDC 650170' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2006-03-02 _chemical_name_systematic ; Bis(triethylselenonium) hexaiodozirconate(IV) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C6 H15 Se 1+), I6 Zr 2-' _chemical_formula_sum 'C12 H30 I6 Se2 Zr' _chemical_formula_weight 1184.90 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 '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 cubic _symmetry_space_group_name_H-M 'P a -3' _symmetry_Int_Tables_number 205 # Superceded ** _symmetry_space_group_name_Hall '-P 2ac 2ab 3' # Superceded ** 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' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-1/2' _cell_length_a 14.1964(10) _cell_length_b 14.1964(10) _cell_length_c 14.1964(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2861.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1234 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 # 0.15 +/- 0.02 _exptl_crystal_size_mid 0.10 # 0.10 _exptl_crystal_size_min 0.08 # 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.751 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 9.399 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4260 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'G.M. Sheldrick, (2003). SADABS. Version 2.10. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 22678 _diffrn_reflns_av_R_equivalents 0.0593 _diffrn_reflns_av_sigmaI/netI 0.0174 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 25.42 _reflns_number_total 885 _reflns_number_gt 664 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0667P)^2^+9.9960P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 885 _refine_ls_number_parameters 33 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0608 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1340 _refine_ls_wR_factor_gt 0.1181 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.083 _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 Zr1 Zr 0.0000 0.5000 0.0000 0.0662(6) Uani 1 6 d S . . I1 I 0.04375(5) 0.31167(5) 0.05634(5) 0.0829(4) Uani 1 1 d . . . Se1 Se 0.24264(9) 0.24264(9) 0.24264(9) 0.1156(8) Uani 1 3 d S . . C1 C 0.2038(15) 0.3705(15) 0.2794(14) 0.182(8) Uani 1 1 d D . . H1A H 0.2540 0.4030 0.3153 0.219 Uiso 1 1 calc R . . H1B H 0.1869 0.4089 0.2237 0.219 Uiso 1 1 calc R . . C2 C 0.1187(13) 0.3514(16) 0.3405(14) 0.168(7) Uani 1 1 d D . . H2A H 0.0925 0.4112 0.3629 0.251 Uiso 1 1 calc R . . H2B H 0.1374 0.3128 0.3946 0.251 Uiso 1 1 calc R . . H2C H 0.0710 0.3177 0.3036 0.251 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 Zr1 0.0662(6) 0.0662(6) 0.0662(6) 0.0015(5) 0.0015(5) -0.0015(5) I1 0.0938(6) 0.0674(5) 0.0874(5) 0.0074(3) -0.0043(3) 0.0028(3) Se1 0.1156(8) 0.1156(8) 0.1156(8) -0.0211(7) -0.0211(7) -0.0211(7) C1 0.22(2) 0.153(17) 0.172(17) -0.010(14) -0.016(16) 0.031(16) C2 0.144(15) 0.194(18) 0.164(15) 0.000(13) -0.002(13) -0.028(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 Zr1 I1 2.8589(7) 23_665 ? Zr1 I1 2.8589(7) 11_455 ? Zr1 I1 2.8589(7) 8 ? Zr1 I1 2.8589(7) 13_565 ? Zr1 I1 2.8589(7) 20_565 ? Zr1 I1 2.8589(7) . ? Se1 C1 1.97(2) 9 ? Se1 C1 1.97(2) . ? Se1 C1 1.97(2) 5 ? C1 C2 1.512(9) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 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 I1 Zr1 I1 180.0 23_665 11_455 ? I1 Zr1 I1 89.86(2) 23_665 8 ? I1 Zr1 I1 90.14(2) 11_455 8 ? I1 Zr1 I1 90.14(2) 23_665 13_565 ? I1 Zr1 I1 89.86(2) 11_455 13_565 ? I1 Zr1 I1 89.86(2) 8 13_565 ? I1 Zr1 I1 90.14(2) 23_665 20_565 ? I1 Zr1 I1 89.86(2) 11_455 20_565 ? I1 Zr1 I1 180.0 8 20_565 ? I1 Zr1 I1 90.14(2) 13_565 20_565 ? I1 Zr1 I1 89.86(2) 23_665 . ? I1 Zr1 I1 90.14(2) 11_455 . ? I1 Zr1 I1 90.14(2) 8 . ? I1 Zr1 I1 180.00(3) 13_565 . ? I1 Zr1 I1 89.86(2) 20_565 . ? C1 Se1 C1 95.1(8) 9 . ? C1 Se1 C1 95.1(8) 9 5 ? C1 Se1 C1 95.1(8) . 5 ? C2 C1 Se1 102.1(15) . . ? C2 C1 H1A 111.3 . . ? Se1 C1 H1A 111.3 . . ? C2 C1 H1B 111.3 . . ? Se1 C1 H1B 111.3 . . ? H1A C1 H1B 109.2 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.42 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.880 _refine_diff_density_min -1.309 _refine_diff_density_rms 0.131 #===END OF CIF ============================================================== # 06sdr003 data_06sdr003 _database_code_depnum_ccdc_archive 'CCDC 650171' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2006-08-27 _audit_update_record ; 2007-06-09 Moved cation into unit cell. Relabelled CH2Cl2 atoms (removed S). Relabelled HnA to Hn where only one H on C. (mw) ; _chemical_name_systematic ; Bis(6-methyl-5,7,12,13-tetrahydrodibenzo[c,g]selenoninium) hexachlorotitanate(IV) dichloromethane solvate ; # Cation name from ACD/ILAB Web service (ACD/IUPAC Name 8.0) at Daresbury. # Used unique SMILES to create cation. Hope the name is correct! # SMILES string: C[Se+]1Cc2ccccc2CCc3ccccc3C1 # I'm surprised numbering did not start at Se. I.E. # 1-methyl-2,7,8,13-tetrahydrodibenzo[c,g]selenoninium. mw 10-09-2006 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C17 H19 Se1 1+)2, Cl6 Ti1 2-, 2(C H2 Cl2)' _chemical_formula_sum 'C36 H42 Cl10 Se2 Ti' _chemical_formula_weight 1035.02 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 # Superceded ** _symmetry_space_group_name_Hall '-P 1' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0027(10) _cell_length_b 9.955(2) _cell_length_c 12.413(3) _cell_angle_alpha 97.211(10) _cell_angle_beta 109.899(10) _cell_angle_gamma 93.532(10) _cell_volume 1031.3(3) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4211 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.667 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 518 _exptl_absorpt_coefficient_mu 2.647 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7315 # 0.6196 _exptl_absorpt_correction_T_max 1.0000 # 0.9490 _exptl_absorpt_process_details 'G.M. Sheldrick, (2003). SADABS. Version 2.10. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 15187 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0388 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4638 _reflns_number_gt 3971 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0266P)^2^+0.9361P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4638 _refine_ls_number_parameters 223 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0436 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0675 _refine_ls_wR_factor_gt 0.0632 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 Ti1 Ti 0.5000 0.5000 0.0000 0.01320(12) Uani 1 2 d S . . Se1 Se 0.05158(2) 0.42461(2) 0.162801(18) 0.01686(7) Uani 1 1 d . . . Cl1 Cl 0.70001(6) 0.61323(6) 0.16564(5) 0.02152(13) Uani 1 1 d . . . Cl2 Cl 0.30661(6) 0.59563(6) 0.06469(5) 0.02024(12) Uani 1 1 d . . . Cl3 Cl 0.51461(6) 0.69058(6) -0.09194(5) 0.01877(12) Uani 1 1 d . . . C1 C 0.2594(3) 0.4110(2) 0.27929(19) 0.0193(5) Uani 1 1 d . . . H1A H 0.2634 0.3180 0.2998 0.023 Uiso 1 1 calc R . . H1B H 0.3445 0.4288 0.2475 0.023 Uiso 1 1 calc R . . C2 C 0.2848(2) 0.5133(2) 0.38518(19) 0.0183(5) Uani 1 1 d . . . C3 C 0.3033(3) 0.6518(3) 0.3772(2) 0.0230(5) Uani 1 1 d . . . H3 H 0.2984 0.6785 0.3053 0.028 Uiso 1 1 calc R . . C4 C 0.3287(3) 0.7508(3) 0.4726(2) 0.0263(5) Uani 1 1 d . . . H4 H 0.3397 0.8446 0.4661 0.032 Uiso 1 1 calc R . . C5 C 0.3379(3) 0.7107(3) 0.5780(2) 0.0256(5) Uani 1 1 d . . . H5 H 0.3556 0.7775 0.6441 0.031 Uiso 1 1 calc R . . C6 C 0.3214(3) 0.5750(3) 0.5864(2) 0.0223(5) Uani 1 1 d . . . H6 H 0.3297 0.5495 0.6593 0.027 Uiso 1 1 calc R . . C7 C 0.2929(2) 0.4727(2) 0.4912(2) 0.0192(5) Uani 1 1 d . . . C8 C 0.2739(3) 0.3261(2) 0.5083(2) 0.0212(5) Uani 1 1 d . . . H8A H 0.3335 0.3194 0.5904 0.025 Uiso 1 1 calc R . . H8B H 0.3224 0.2706 0.4600 0.025 Uiso 1 1 calc R . . C9 C 0.0987(3) 0.2649(3) 0.4771(2) 0.0217(5) Uani 1 1 d . . . H9A H 0.0919 0.2188 0.5417 0.026 Uiso 1 1 calc R . . H9B H 0.0320 0.3410 0.4720 0.026 Uiso 1 1 calc R . . C10 C 0.0282(3) 0.1645(2) 0.3655(2) 0.0200(5) Uani 1 1 d . . . C11 C 0.0469(3) 0.0264(3) 0.3714(2) 0.0242(5) Uani 1 1 d . . . H11 H 0.1106 0.0014 0.4427 0.029 Uiso 1 1 calc R . . C12 C -0.0241(3) -0.0745(3) 0.2768(2) 0.0276(6) Uani 1 1 d . . . H12 H -0.0076 -0.1670 0.2832 0.033 Uiso 1 1 calc R . . C13 C -0.1196(3) -0.0400(3) 0.1727(2) 0.0278(6) Uani 1 1 d . . . H13 H -0.1726 -0.1091 0.1082 0.033 Uiso 1 1 calc R . . C14 C -0.1373(3) 0.0952(3) 0.1631(2) 0.0241(5) Uani 1 1 d . . . H14 H -0.2016 0.1187 0.0912 0.029 Uiso 1 1 calc R . . C15 C -0.0620(3) 0.1984(2) 0.2575(2) 0.0190(5) Uani 1 1 d . . . C16 C -0.0851(3) 0.3418(2) 0.2383(2) 0.0210(5) Uani 1 1 d . . . H16A H -0.0653 0.3986 0.3142 0.025 Uiso 1 1 calc R . . H16B H -0.1975 0.3446 0.1900 0.025 Uiso 1 1 calc R . . C17 C 0.0583(3) 0.2787(2) 0.0472(2) 0.0218(5) Uani 1 1 d . . . H17A H 0.1244 0.3112 0.0052 0.033 Uiso 1 1 calc R . . H17B H -0.0497 0.2482 -0.0074 0.033 Uiso 1 1 calc R . . H17C H 0.1037 0.2025 0.0851 0.033 Uiso 1 1 calc R . . C18 C 0.4794(3) 0.9496(3) 0.1813(2) 0.0296(6) Uani 1 1 d . . . H18A H 0.4783 0.8682 0.1262 0.036 Uiso 1 1 calc R . . H18B H 0.5298 1.0292 0.1610 0.036 Uiso 1 1 calc R . . Cl4 Cl 0.28249(8) 0.97588(8) 0.16873(7) 0.04241(18) Uani 1 1 d . . . Cl5 Cl 0.59072(9) 0.92667(8) 0.32323(6) 0.03980(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0134(3) 0.0141(3) 0.0127(3) 0.0036(2) 0.0050(2) 0.0014(2) Se1 0.01698(11) 0.01922(13) 0.01535(12) 0.00472(9) 0.00611(9) 0.00273(9) Cl1 0.0227(3) 0.0199(3) 0.0173(3) 0.0023(2) 0.0019(2) -0.0008(2) Cl2 0.0210(3) 0.0224(3) 0.0220(3) 0.0067(2) 0.0119(2) 0.0061(2) Cl3 0.0192(3) 0.0183(3) 0.0212(3) 0.0085(2) 0.0082(2) 0.0026(2) C1 0.0178(11) 0.0257(13) 0.0153(11) 0.0036(10) 0.0062(9) 0.0051(9) C2 0.0120(10) 0.0251(13) 0.0178(11) 0.0028(10) 0.0054(8) 0.0020(9) C3 0.0219(12) 0.0274(13) 0.0205(12) 0.0053(10) 0.0083(9) -0.0003(10) C4 0.0242(12) 0.0225(13) 0.0313(14) 0.0018(11) 0.0096(10) 0.0011(10) C5 0.0231(12) 0.0304(14) 0.0218(12) -0.0023(11) 0.0087(10) 0.0001(10) C6 0.0180(11) 0.0325(14) 0.0164(11) 0.0019(10) 0.0072(9) 0.0005(10) C7 0.0107(10) 0.0267(13) 0.0198(11) 0.0044(10) 0.0043(9) 0.0032(9) C8 0.0189(11) 0.0267(13) 0.0180(11) 0.0075(10) 0.0047(9) 0.0041(10) C9 0.0225(11) 0.0262(13) 0.0187(11) 0.0075(10) 0.0090(9) 0.0012(10) C10 0.0179(11) 0.0228(12) 0.0228(12) 0.0074(10) 0.0107(9) 0.0004(9) C11 0.0230(12) 0.0262(13) 0.0264(13) 0.0116(11) 0.0099(10) 0.0041(10) C12 0.0324(13) 0.0201(13) 0.0366(15) 0.0078(11) 0.0187(12) 0.0038(11) C13 0.0292(13) 0.0252(14) 0.0307(14) -0.0017(11) 0.0166(11) -0.0056(11) C14 0.0204(11) 0.0306(14) 0.0231(12) 0.0068(11) 0.0096(10) -0.0008(10) C15 0.0177(11) 0.0211(12) 0.0216(12) 0.0058(10) 0.0103(9) 0.0021(9) C16 0.0165(11) 0.0277(13) 0.0230(12) 0.0077(10) 0.0108(9) 0.0044(10) C17 0.0219(11) 0.0256(13) 0.0194(12) 0.0017(10) 0.0095(9) 0.0037(10) C18 0.0269(13) 0.0328(15) 0.0288(14) 0.0041(12) 0.0102(11) 0.0000(11) Cl4 0.0288(3) 0.0445(4) 0.0497(5) 0.0035(4) 0.0093(3) 0.0069(3) Cl5 0.0431(4) 0.0362(4) 0.0357(4) 0.0098(3) 0.0058(3) 0.0097(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 Ti1 Cl1 2.3213(7) . ? Ti1 Cl1 2.3213(7) 2_665 ? Ti1 Cl3 2.3526(7) . ? Ti1 Cl3 2.3526(7) 2_665 ? Ti1 Cl2 2.3551(6) . ? Ti1 Cl2 2.3551(6) 2_665 ? Se1 C17 1.929(2) . ? Se1 C1 1.962(2) . ? Se1 C16 1.981(2) . ? C1 C2 1.499(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.399(3) . ? C2 C7 1.405(3) . ? C3 C4 1.385(3) . ? C3 H3 0.9500 . ? C4 C5 1.392(4) . ? C4 H4 0.9500 . ? C5 C6 1.371(4) . ? C5 H5 0.9500 . ? C6 C7 1.399(3) . ? C6 H6 0.9500 . ? C7 C8 1.508(3) . ? C8 C9 1.554(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.515(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.403(3) . ? C10 C15 1.406(3) . ? C11 C12 1.382(4) . ? C11 H11 0.9500 . ? C12 C13 1.385(4) . ? C12 H12 0.9500 . ? C13 C14 1.381(4) . ? C13 H13 0.9500 . ? C14 C15 1.399(3) . ? C14 H14 0.9500 . ? C15 C16 1.492(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 Cl5 1.757(3) . ? C18 Cl4 1.765(3) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Ti1 Cl1 180.00(3) . 2_665 ? Cl1 Ti1 Cl3 89.07(2) . . ? Cl1 Ti1 Cl3 90.93(2) 2_665 . ? Cl1 Ti1 Cl3 90.93(2) . 2_665 ? Cl1 Ti1 Cl3 89.07(2) 2_665 2_665 ? Cl3 Ti1 Cl3 180.00(2) . 2_665 ? Cl1 Ti1 Cl2 90.30(2) . . ? Cl1 Ti1 Cl2 89.70(2) 2_665 . ? Cl3 Ti1 Cl2 89.07(2) . . ? Cl3 Ti1 Cl2 90.93(2) 2_665 . ? Cl1 Ti1 Cl2 89.70(2) . 2_665 ? Cl1 Ti1 Cl2 90.30(2) 2_665 2_665 ? Cl3 Ti1 Cl2 90.93(2) . 2_665 ? Cl3 Ti1 Cl2 89.07(2) 2_665 2_665 ? Cl2 Ti1 Cl2 180.00(2) . 2_665 ? C17 Se1 C1 97.19(10) . . ? C17 Se1 C16 104.02(10) . . ? C1 Se1 C16 98.53(10) . . ? C2 C1 Se1 109.11(15) . . ? C2 C1 H1A 109.9 . . ? Se1 C1 H1A 109.9 . . ? C2 C1 H1B 109.9 . . ? Se1 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? C3 C2 C7 120.0(2) . . ? C3 C2 C1 118.5(2) . . ? C7 C2 C1 121.5(2) . . ? C4 C3 C2 121.0(2) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 119.1(2) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C6 C5 C4 120.1(2) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C7 122.2(2) . . ? C5 C6 H6 118.9 . . ? C7 C6 H6 118.9 . . ? C6 C7 C2 117.6(2) . . ? C6 C7 C8 118.5(2) . . ? C2 C7 C8 123.9(2) . . ? C7 C8 C9 114.28(19) . . ? C7 C8 H8A 108.7 . . ? C9 C8 H8A 108.7 . . ? C7 C8 H8B 108.7 . . ? C9 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? C10 C9 C8 116.33(19) . . ? C10 C9 H9A 108.2 . . ? C8 C9 H9A 108.2 . . ? C10 C9 H9B 108.2 . . ? C8 C9 H9B 108.2 . . ? H9A C9 H9B 107.4 . . ? C11 C10 C15 117.4(2) . . ? C11 C10 C9 117.7(2) . . ? C15 C10 C9 124.8(2) . . ? C12 C11 C10 122.2(2) . . ? C12 C11 H11 118.9 . . ? C10 C11 H11 118.9 . . ? C11 C12 C13 119.6(2) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C14 C13 C12 119.7(2) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C13 C14 C15 121.0(2) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C14 C15 C10 119.9(2) . . ? C14 C15 C16 117.3(2) . . ? C10 C15 C16 122.8(2) . . ? C15 C16 Se1 115.53(15) . . ? C15 C16 H16A 108.4 . . ? Se1 C16 H16A 108.4 . . ? C15 C16 H16B 108.4 . . ? Se1 C16 H16B 108.4 . . ? H16A C16 H16B 107.5 . . ? Se1 C17 H17A 109.5 . . ? Se1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Se1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Cl5 C18 Cl4 110.75(14) . . ? Cl5 C18 H18A 109.5 . . ? Cl4 C18 H18A 109.5 . . ? Cl5 C18 H18B 109.5 . . ? Cl4 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.488 _refine_diff_density_min -0.503 _refine_diff_density_rms 0.089 #===END OF CIF ============================================================== # 07sdr016 data_07sdr016 _database_code_depnum_ccdc_archive 'CCDC 650172' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2007-04-27 _chemical_name_systematic ; trans-tetrachlorobis(diethylselenide)tin(IV) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H20 Cl4 Se2 Sn' _chemical_formula_sum 'C8 H20 Cl4 Se2 Sn' _chemical_formula_weight 534.65 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 # Superceded ** _symmetry_space_group_name_Hall '-P 2ybc' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.1244(10) _cell_length_b 11.5362(10) _cell_length_c 10.2435(10) _cell_angle_alpha 90.00 _cell_angle_beta 97.662(6) _cell_angle_gamma 90.00 _cell_volume 834.38(16) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1996 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.128 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 508 _exptl_absorpt_coefficient_mu 6.507 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5272 # 0.1806 _exptl_absorpt_correction_T_max 1.0000 # 0.2456 _exptl_absorpt_process_details 'G.M. Sheldrick, (2003). SADABS. Version 2.10. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 15395 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0252 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 10.24 _diffrn_reflns_theta_max 27.54 _reflns_number_total 1808 _reflns_number_gt 1759 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP III (Ferrugia, 1997)' _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0212P)^2^+1.0430P] 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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0060(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1808 _refine_ls_number_parameters 71 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0238 _refine_ls_R_factor_gt 0.0229 _refine_ls_wR_factor_ref 0.0563 _refine_ls_wR_factor_gt 0.0558 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.128 _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 Sn1 Sn 0.0000 0.0000 0.0000 0.01584(11) Uani 1 2 d S . . Cl1 Cl -0.10488(9) 0.19604(5) 0.03378(6) 0.02193(15) Uani 1 1 d . . . Cl2 Cl -0.21299(8) -0.07267(5) 0.14819(6) 0.02168(15) Uani 1 1 d . . . Se1 Se 0.27739(3) 0.01939(2) 0.20642(2) 0.01825(11) Uani 1 1 d . . . C1 C 0.4199(4) 0.1554(2) 0.1573(3) 0.0243(5) Uani 1 1 d . . . H1A H 0.4895 0.1349 0.0831 0.029 Uiso 1 1 calc R . . H1B H 0.3305 0.2188 0.1279 0.029 Uiso 1 1 calc R . . C2 C 0.5583(4) 0.1963(2) 0.2726(3) 0.0273(6) Uani 1 1 d . . . H2A H 0.6274 0.2640 0.2462 0.041 Uiso 1 1 calc R . . H2B H 0.6480 0.1340 0.3008 0.041 Uiso 1 1 calc R . . H2C H 0.4892 0.2176 0.3456 0.041 Uiso 1 1 calc R . . C3 C 0.1414(4) 0.0938(2) 0.3395(2) 0.0215(5) Uani 1 1 d . . . H3A H 0.1504 0.1792 0.3320 0.026 Uiso 1 1 calc R . . H3B H 0.0058 0.0720 0.3239 0.026 Uiso 1 1 calc R . . C4 C 0.2266(4) 0.0557(3) 0.4767(3) 0.0288(6) Uani 1 1 d . . . H4A H 0.1584 0.0931 0.5423 0.043 Uiso 1 1 calc R . . H4B H 0.3604 0.0782 0.4922 0.043 Uiso 1 1 calc R . . H4C H 0.2161 -0.0286 0.4841 0.043 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 Sn1 0.01472(15) 0.01563(14) 0.01667(15) 0.00148(7) 0.00024(9) -0.00197(7) Cl1 0.0218(3) 0.0173(3) 0.0263(3) 0.0015(2) 0.0018(2) 0.0015(2) Cl2 0.0211(3) 0.0222(3) 0.0222(3) 0.0012(2) 0.0049(2) -0.0050(2) Se1 0.01740(16) 0.01757(16) 0.01915(16) -0.00072(8) 0.00007(10) 0.00052(8) C1 0.0212(12) 0.0229(12) 0.0284(13) 0.0020(10) 0.0024(10) -0.0042(10) C2 0.0239(13) 0.0256(13) 0.0323(14) -0.0061(11) 0.0032(11) -0.0045(10) C3 0.0185(11) 0.0231(12) 0.0234(12) -0.0023(10) 0.0052(9) 0.0012(9) C4 0.0281(13) 0.0322(14) 0.0255(13) -0.0012(11) 0.0016(10) 0.0022(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 Sn1 Cl1 2.4211(6) . ? Sn1 Cl1 2.4211(6) 3 ? Sn1 Cl2 2.4339(6) 3 ? Sn1 Cl2 2.4339(6) . ? Sn1 Se1 2.7041(4) . ? Sn1 Se1 2.7041(4) 3 ? Se1 C1 1.970(3) . ? Se1 C3 1.972(2) . ? C1 C2 1.509(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.520(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 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 Cl1 Sn1 Cl1 180.00(4) . 3 ? Cl1 Sn1 Cl2 89.85(2) . 3 ? Cl1 Sn1 Cl2 90.15(2) 3 3 ? Cl1 Sn1 Cl2 90.15(2) . . ? Cl1 Sn1 Cl2 89.85(2) 3 . ? Cl2 Sn1 Cl2 180.00(4) 3 . ? Cl1 Sn1 Se1 91.047(16) . . ? Cl1 Sn1 Se1 88.953(16) 3 . ? Cl2 Sn1 Se1 90.444(17) 3 . ? Cl2 Sn1 Se1 89.556(17) . . ? Cl1 Sn1 Se1 88.953(16) . 3 ? Cl1 Sn1 Se1 91.047(16) 3 3 ? Cl2 Sn1 Se1 89.556(18) 3 3 ? Cl2 Sn1 Se1 90.444(17) . 3 ? Se1 Sn1 Se1 180.000(13) . 3 ? C1 Se1 C3 98.46(11) . . ? C1 Se1 Sn1 102.36(8) . . ? C3 Se1 Sn1 101.61(8) . . ? C2 C1 Se1 110.77(18) . . ? C2 C1 H1A 109.5 . . ? Se1 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? Se1 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 Se1 109.92(18) . . ? C4 C3 H3A 109.7 . . ? Se1 C3 H3A 109.7 . . ? C4 C3 H3B 109.7 . . ? Se1 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Sn1 Se1 C1 C2 168.37(17) . . . . ? Sn1 Se1 C3 C4 149.19(17) . . . . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 0.616 _refine_diff_density_min -0.792 _refine_diff_density_rms 0.100 #===END OF CIF ============================================================== # 06sdr002 data_06sdr002 _database_code_depnum_ccdc_archive 'CCDC 650173' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2006-08-27 _audit_update_record '2007-06-09 Moved cation into cell' _chemical_name_systematic ; Bis(diethylchloromethylselenonium) hexachlorohafnate(IV) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C5.37 H13.12 Cl0.63 Se 1+)2, Cl6 Hf 2-' _chemical_formula_sum 'C10.74 H26.24 Cl7.26 Hf Se2' _chemical_formula_weight 749.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 # Superceded ** _symmetry_space_group_name_Hall '-C 2yc' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.780(4) _cell_length_b 9.477(2) _cell_length_c 16.330(3) _cell_angle_alpha 90.00 _cell_angle_beta 119.486(10) _cell_angle_gamma 90.00 _cell_volume 2260.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2756 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.201 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 8.685 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7180 # 0.5433 _exptl_absorpt_correction_T_max 1.0000 # 0.8455 _exptl_absorpt_process_details 'G.M. Sheldrick, (2003). SADABS. Version 2.10. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 20228 _diffrn_reflns_av_R_equivalents 0.0658 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 27.56 _reflns_number_total 2601 _reflns_number_gt 2062 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. During the refinement it rapidly became clear that one of the ethyl groups of the cation was not well behaved. For C5(CH2) & C6(CH3) the C5-C6 bond was too long for a C-C bond (1.7 Angstrom) with C6 having an anomalous displacement ellipsoid. Replacing C6 with a Cl atom (Cl4) gave a better fit to the data, made sense of the C5-Cl4 bond but with largish adp values. The final model which gave the best fit to the data, had a refined variable amount of Cl4 and C6(H3) (total occupancy = 1) with the two atoms given the same coordinates and adp values. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0226P)^2^+3.3998P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2601 _refine_ls_number_parameters 98 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0526 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0573 _refine_ls_wR_factor_gt 0.0534 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 Hf1 Hf 0.7500 0.7500 0.5000 0.01781(8) Uani 1 2 d S . . Cl1 Cl 0.66471(7) 0.97013(11) 0.43782(7) 0.0239(2) Uani 1 1 d . . . Cl2 Cl 0.84214(8) 0.80612(12) 0.42468(8) 0.0251(3) Uani 1 1 d . . . Cl3 Cl 0.63848(7) 0.62575(11) 0.35823(7) 0.0251(3) Uani 1 1 d . . . Se1 Se 0.90549(3) 0.16570(4) 0.41618(3) 0.02074(12) Uani 1 1 d . B . C1 C 0.8837(3) 0.1758(5) 0.5233(3) 0.0229(10) Uani 1 1 d D . . H1A H 0.8434 0.2573 0.5148 0.028 Uiso 1 1 calc R . . H1B H 0.8516 0.0892 0.5250 0.028 Uiso 1 1 calc R . . C2 C 0.9715(3) 0.1912(5) 0.6158(3) 0.0266(11) Uani 1 1 d D . . H2A H 0.9574 0.1956 0.6673 0.040 Uiso 1 1 calc R . . H2B H 1.0029 0.2780 0.6150 0.040 Uiso 1 1 calc R . . H2C H 1.0112 0.1099 0.6251 0.040 Uiso 1 1 calc R . . C3 C 0.9341(3) 0.3628(4) 0.4099(3) 0.0247(10) Uani 1 1 d D . . H3A H 0.8922 0.4236 0.4207 0.030 Uiso 1 1 calc R . . H3B H 0.9975 0.3829 0.4599 0.030 Uiso 1 1 calc R . . C4 C 0.9246(3) 0.3968(5) 0.3147(3) 0.0284(11) Uani 1 1 d D . . H4A H 0.9399 0.4963 0.3131 0.043 Uiso 1 1 calc R . . H4B H 0.8614 0.3792 0.2653 0.043 Uiso 1 1 calc R . . H4C H 0.9663 0.3370 0.3041 0.043 Uiso 1 1 calc R . . C5 C 0.7774(3) 0.1618(5) 0.3164(3) 0.0236(10) Uani 1 1 d . . . H5A H 0.7751 0.1602 0.2546 0.028 Uiso 1 1 calc R A 1 H5B H 0.7486 0.0739 0.3220 0.028 Uiso 1 1 calc R A 1 Cl4 Cl 0.71448(11) 0.30670(19) 0.32011(11) 0.0304(7) Uani 0.626(7) 1 d P B 1 C6 C 0.71448(11) 0.30670(19) 0.32011(11) 0.0304(7) Uani 0.374(7) 1 d P B 2 H6A H 0.6511 0.2994 0.2688 0.046 Uiso 0.374(7) 1 calc PR B 2 H6B H 0.7418 0.3941 0.3131 0.046 Uiso 0.374(7) 1 calc PR B 2 H6C H 0.7153 0.3077 0.3805 0.046 Uiso 0.374(7) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hf1 0.02136(15) 0.01519(13) 0.02119(15) 0.00028(11) 0.01378(12) -0.00028(11) Cl1 0.0264(6) 0.0183(5) 0.0293(6) 0.0010(5) 0.0155(5) 0.0026(5) Cl2 0.0280(6) 0.0262(6) 0.0301(6) 0.0022(5) 0.0212(5) 0.0002(5) Cl3 0.0297(7) 0.0209(6) 0.0235(6) -0.0002(5) 0.0122(5) -0.0033(5) Se1 0.0250(3) 0.0167(2) 0.0240(2) -0.00114(19) 0.0147(2) 0.00022(19) C1 0.028(3) 0.023(2) 0.027(2) 0.000(2) 0.021(2) -0.001(2) C2 0.028(3) 0.032(3) 0.026(3) -0.003(2) 0.018(2) -0.005(2) C3 0.033(3) 0.016(2) 0.016(2) 0.0005(19) 0.006(2) 0.007(2) C4 0.033(3) 0.028(3) 0.027(3) 0.000(2) 0.016(2) -0.007(2) C5 0.024(3) 0.025(2) 0.021(2) -0.003(2) 0.010(2) -0.006(2) Cl4 0.0209(11) 0.0471(12) 0.0235(10) 0.0028(8) 0.0111(8) 0.0040(7) C6 0.0209(11) 0.0471(12) 0.0235(10) 0.0028(8) 0.0111(8) 0.0040(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hf1 Cl3 2.4460(11) 7_666 ? Hf1 Cl3 2.4460(11) . ? Hf1 Cl1 2.4495(11) . ? Hf1 Cl1 2.4495(11) 7_666 ? Hf1 Cl2 2.4613(10) 7_666 ? Hf1 Cl2 2.4613(10) . ? Se1 C3 1.944(4) . ? Se1 C5 1.956(4) . ? Se1 C1 1.958(4) . ? C1 C2 1.511(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.517(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 Cl4 1.751(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl3 Hf1 Cl3 180.0 7_666 . ? Cl3 Hf1 Cl1 90.06(4) 7_666 . ? Cl3 Hf1 Cl1 89.94(4) . . ? Cl3 Hf1 Cl1 89.94(4) 7_666 7_666 ? Cl3 Hf1 Cl1 90.06(4) . 7_666 ? Cl1 Hf1 Cl1 180.0 . 7_666 ? Cl3 Hf1 Cl2 90.41(4) 7_666 7_666 ? Cl3 Hf1 Cl2 89.59(4) . 7_666 ? Cl1 Hf1 Cl2 90.50(4) . 7_666 ? Cl1 Hf1 Cl2 89.51(4) 7_666 7_666 ? Cl3 Hf1 Cl2 89.59(4) 7_666 . ? Cl3 Hf1 Cl2 90.41(4) . . ? Cl1 Hf1 Cl2 89.50(4) . . ? Cl1 Hf1 Cl2 90.49(4) 7_666 . ? Cl2 Hf1 Cl2 180.0 7_666 . ? C3 Se1 C5 99.94(18) . . ? C3 Se1 C1 99.19(17) . . ? C5 Se1 C1 97.67(18) . . ? C2 C1 Se1 112.2(3) . . ? C2 C1 H1A 109.2 . . ? Se1 C1 H1A 109.2 . . ? C2 C1 H1B 109.2 . . ? Se1 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 Se1 110.7(3) . . ? C4 C3 H3A 109.5 . . ? Se1 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? Se1 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Cl4 C5 Se1 113.0(2) . . ? Cl4 C5 H5A 109.0 . . ? Se1 C5 H5A 109.0 . . ? Cl4 C5 H5B 109.0 . . ? Se1 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 Se1 C1 C2 -74.4(3) . . . . ? C5 Se1 C1 C2 -175.9(3) . . . . ? C5 Se1 C3 C4 -62.2(3) . . . . ? C1 Se1 C3 C4 -161.8(3) . . . . ? C3 Se1 C5 Cl4 -44.2(3) . . . . ? C1 Se1 C5 Cl4 56.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.398 _refine_diff_density_min -0.814 _refine_diff_density_rms 0.167 #===END OF CIF ============================================================== # 06sdr005 data_06sdr005 _database_code_depnum_ccdc_archive 'CCDC 650174' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2006-08-28 _audit_update_record '2007-06-09 Moved cation to be in cell' _chemical_name_systematic ; Bis(diethylchloromethylselenonium) hexachlorozirconate(IV) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C5.67 H13.99 Cl0.33 Se 1+)2, Cl6 Zr 2-' _chemical_formula_sum 'C11.33 H27.99 Cl6.67 Se2 Zr' _chemical_formula_weight 649.93 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 # Superceded ** _symmetry_space_group_name_Hall '-C 2yc' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.859(2) _cell_length_b 9.4791(10) _cell_length_c 16.388(2) _cell_angle_alpha 90.00 _cell_angle_beta 119.333(5) _cell_angle_gamma 90.00 _cell_volume 2283.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2746 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.891 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1270 _exptl_absorpt_coefficient_mu 4.443 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6384 # 0.4702 _exptl_absorpt_correction_T_max 1.0000 # 0.6649 _exptl_absorpt_process_details 'G.M. Sheldrick, (2003). SADABS. Version 2.10. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 16339 _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 27.54 _reflns_number_total 2630 _reflns_number_gt 2522 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. During the refinement it rapidly became clear that one of the ethyl groups of the cation was not well behaved. For C5(CH2) & C6(CH3) the C5-C6 bond was too long for a C-C bond (1.7 Angstrom) with C6 having an anomalous displacement ellipsoid. Replacing C6 with a Cl atom (Cl4) gave a better fit to the data, made sense of the C5-Cl4 bond but with largish adp values. The final model which gave the best fit to the data, had a refined variable amount of Cl4 and C6(H3) (total occupancy = 1) with the two atoms given the same coordinates and adp values. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0145P)^2^+7.4400P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2630 _refine_ls_number_parameters 98 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0239 _refine_ls_R_factor_gt 0.0224 _refine_ls_wR_factor_ref 0.0534 _refine_ls_wR_factor_gt 0.0525 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 Zr1 Zr 0.7500 0.7500 0.5000 0.01269(8) Uani 1 2 d S . . Cl1 Cl 0.66516(4) 0.97172(5) 0.43787(4) 0.01998(12) Uani 1 1 d . . . Cl2 Cl 0.86139(4) 0.87468(6) 0.64154(4) 0.02125(12) Uani 1 1 d . . . Cl3 Cl 0.65771(4) 0.69423(6) 0.57575(4) 0.02117(12) Uani 1 1 d . . . Se1 Se 0.905192(14) 0.16603(2) 0.415943(15) 0.01596(7) Uani 1 1 d . B . C1 C 0.88334(15) 0.1754(2) 0.52237(15) 0.0182(4) Uani 1 1 d . . . H1A H 0.8438 0.2574 0.5145 0.022 Uiso 1 1 calc R . . H1B H 0.8508 0.0891 0.5235 0.022 Uiso 1 1 calc R . . C2 C 0.97096(16) 0.1888(3) 0.61495(16) 0.0240(5) Uani 1 1 d . . . H2A H 0.9568 0.1930 0.6662 0.036 Uiso 1 1 calc R . . H2B H 1.0028 0.2751 0.6148 0.036 Uiso 1 1 calc R . . H2C H 1.0098 0.1069 0.6237 0.036 Uiso 1 1 calc R . . C3 C 0.93530(15) 0.3636(2) 0.41022(16) 0.0192(4) Uani 1 1 d . . . H3A H 0.8940 0.4252 0.4211 0.023 Uiso 1 1 calc R . . H3B H 0.9984 0.3826 0.4600 0.023 Uiso 1 1 calc R . . C4 C 0.92624(17) 0.3969(3) 0.31536(16) 0.0249(5) Uani 1 1 d . . . H4A H 0.9414 0.4963 0.3136 0.037 Uiso 1 1 calc R . . H4B H 0.8636 0.3790 0.2662 0.037 Uiso 1 1 calc R . . H4C H 0.9679 0.3370 0.3051 0.037 Uiso 1 1 calc R . . C5 C 0.77819(15) 0.1623(2) 0.31651(15) 0.0206(5) Uani 1 1 d . . . H5A H 0.7762 0.1611 0.2551 0.025 Uiso 1 1 calc R A 1 H5B H 0.7495 0.0742 0.3218 0.025 Uiso 1 1 calc R A 1 Cl4 Cl 0.71645(8) 0.30350(17) 0.32001(9) 0.0347(5) Uani 0.336(5) 1 d P B 1 C6 C 0.71645(8) 0.30350(17) 0.32001(9) 0.0347(5) Uani 0.664(5) 1 d P B 2 H6A H 0.6536 0.2960 0.2688 0.052 Uiso 0.664(5) 1 calc PR B 2 H6B H 0.7436 0.3911 0.3133 0.052 Uiso 0.664(5) 1 calc PR B 2 H6C H 0.7168 0.3042 0.3800 0.052 Uiso 0.664(5) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.01423(14) 0.01205(14) 0.01389(15) 0.00025(10) 0.00852(12) -0.00037(9) Cl1 0.0206(2) 0.0155(2) 0.0236(3) 0.00146(19) 0.0107(2) 0.00265(18) Cl2 0.0243(3) 0.0194(3) 0.0165(2) -0.00075(19) 0.0073(2) -0.0046(2) Cl3 0.0219(3) 0.0250(3) 0.0230(3) 0.0013(2) 0.0159(2) -0.0007(2) Se1 0.01796(12) 0.01397(11) 0.01700(12) -0.00140(7) 0.00938(9) 0.00008(7) C1 0.0206(11) 0.0205(11) 0.0178(11) -0.0012(8) 0.0128(9) -0.0010(8) C2 0.0209(11) 0.0329(13) 0.0185(11) -0.0027(9) 0.0099(10) -0.0015(9) C3 0.0225(11) 0.0145(10) 0.0196(11) -0.0035(8) 0.0095(9) -0.0043(8) C4 0.0295(12) 0.0253(12) 0.0225(12) -0.0003(9) 0.0147(10) -0.0078(10) C5 0.0198(11) 0.0244(11) 0.0140(11) -0.0032(8) 0.0056(9) -0.0051(8) Cl4 0.0208(7) 0.0607(10) 0.0215(7) 0.0051(6) 0.0095(5) 0.0005(6) C6 0.0208(7) 0.0607(10) 0.0215(7) 0.0051(6) 0.0095(5) 0.0005(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 Cl2 2.4568(6) . ? Zr1 Cl2 2.4568(6) 7_666 ? Zr1 Cl1 2.4643(5) 7_666 ? Zr1 Cl1 2.4643(5) . ? Zr1 Cl3 2.4767(6) 7_666 ? Zr1 Cl3 2.4767(5) . ? Se1 C1 1.953(2) . ? Se1 C3 1.954(2) . ? Se1 C5 1.955(2) . ? C1 C2 1.518(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.519(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 Cl4 1.713(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? 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 Cl2 Zr1 Cl2 180.0 . 7_666 ? Cl2 Zr1 Cl1 89.983(19) . 7_666 ? Cl2 Zr1 Cl1 90.02(2) 7_666 7_666 ? Cl2 Zr1 Cl1 90.017(19) . . ? Cl2 Zr1 Cl1 89.983(19) 7_666 . ? Cl1 Zr1 Cl1 180.000(1) 7_666 . ? Cl2 Zr1 Cl3 89.61(2) . 7_666 ? Cl2 Zr1 Cl3 90.39(2) 7_666 7_666 ? Cl1 Zr1 Cl3 90.524(19) 7_666 7_666 ? Cl1 Zr1 Cl3 89.476(19) . 7_666 ? Cl2 Zr1 Cl3 90.39(2) . . ? Cl2 Zr1 Cl3 89.61(2) 7_666 . ? Cl1 Zr1 Cl3 89.476(19) 7_666 . ? Cl1 Zr1 Cl3 90.524(19) . . ? Cl3 Zr1 Cl3 180.0 7_666 . ? C1 Se1 C3 99.58(9) . . ? C1 Se1 C5 97.84(10) . . ? C3 Se1 C5 100.45(9) . . ? C2 C1 Se1 112.30(15) . . ? C2 C1 H1A 109.1 . . ? Se1 C1 H1A 109.1 . . ? C2 C1 H1B 109.1 . . ? Se1 C1 H1B 109.1 . . ? H1A C1 H1B 107.9 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 Se1 110.50(15) . . ? C4 C3 H3A 109.5 . . ? Se1 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? Se1 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Cl4 C5 Se1 113.16(12) . . ? Cl4 C5 H5A 108.9 . . ? Se1 C5 H5A 108.9 . . ? Cl4 C5 H5B 108.9 . . ? Se1 C5 H5B 108.9 . . ? H5A C5 H5B 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 Se1 C1 C2 -74.49(18) . . . . ? C5 Se1 C1 C2 -176.55(17) . . . . ? C1 Se1 C3 C4 -161.87(16) . . . . ? C5 Se1 C3 C4 -61.98(18) . . . . ? C1 Se1 C5 Cl4 56.53(14) . . . . ? C3 Se1 C5 Cl4 -44.78(15) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.716 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.083 #===END OF CIF ============================================================== # #===END OF FILE =============================================================