data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Reid, G.' _publ_contact_author_email GR@SOTON.AC.UK _publ_section_title ; Supramolecular assemblies of germanium(II) halides with O-, S- and Se-donor macrocycles the effects of donor atom type upon structure ; loop_ _publ_author_name G.Reid W.Levason A.Hector M.Webster W.Zhang # Attachment '- GeX2_all8_3.cif' data_10wz304d _database_code_depnum_ccdc_archive 'CCDC 781120' #TrackingRef '- GeX2_all8_3.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2010-03-23 _audit_author_name 'Webster, M.' _chemical_name_systematic ; Dichloro(1,4,7,10,13,16-hexathiacyclooctadecane-S,S')germanium(II) ; # C12H24S6 = [18]aneS6 = 1,4,7,10,13,16-hexathiacyclooctadecane _chemical_name_common ;Dichloro(1,4,7,10,13,16-hexathiacyclooctadecane- S,S')germanium(ii) ; _chemical_melting_point ? _chemical_formula_moiety 'C12 H24 Cl2 Ge S6' _chemical_formula_sum 'C12 H24 Cl2 Ge S6' _chemical_formula_weight 504.16 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' S S 0.1246 0.1234 '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' Ge Ge 0.1547 1.8001 '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' _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' 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 23.563(7) _cell_length_b 5.0739(15) _cell_length_c 17.060(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.987(15) _cell_angle_gamma 90.00 _cell_volume 2014.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 15216 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.662 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 2.399 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5983 # shelxl 0.8895 _exptl_absorpt_correction_T_max 1.0000 # 0.9764 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. 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 '10cm confocal mirrors' _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_% ? _diffrn_reflns_number 11383 _diffrn_reflns_av_R_equivalents 0.1109 _diffrn_reflns_av_sigmaI/netI 0.0969 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.20 _diffrn_reflns_theta_max 27.54 _reflns_number_total 2314 _reflns_number_gt 1507 _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 ? _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^)+(0.0000P)^2^+28.7914P] 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 2314 _refine_ls_number_parameters 96 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1401 _refine_ls_R_factor_gt 0.0770 _refine_ls_wR_factor_ref 0.1433 _refine_ls_wR_factor_gt 0.1201 _refine_ls_goodness_of_fit_ref 1.186 _refine_ls_restrained_S_all 1.186 _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 Ge1 Ge 0.5000 0.5373(2) 0.2500 0.0246(3) Uani 1 2 d S . . Cl1 Cl 0.53188(7) 0.8307(4) 0.16460(10) 0.0302(4) Uani 1 1 d . . . S1 S 0.60525(7) 0.5473(3) 0.34439(10) 0.0226(4) Uani 1 1 d . . . S2 S 0.64561(8) 0.7644(4) 0.53180(10) 0.0284(4) Uani 1 1 d . . . S3 S 0.75730(7) 0.1325(3) 0.65296(10) 0.0224(4) Uani 1 1 d . . . C1 C 0.5839(3) 0.3831(13) 0.4302(4) 0.0242(15) Uani 1 1 d . . . H1A H 0.5457 0.3009 0.4144 0.029 Uiso 1 1 calc R . . H1B H 0.6117 0.2411 0.4481 0.029 Uiso 1 1 calc R . . C2 C 0.5810(3) 0.5732(14) 0.4992(4) 0.0264(16) Uani 1 1 d . . . H2A H 0.5720 0.4701 0.5450 0.032 Uiso 1 1 calc R . . H2B H 0.5488 0.6970 0.4835 0.032 Uiso 1 1 calc R . . C3 C 0.7008(3) 0.5156(14) 0.5534(4) 0.0227(15) Uani 1 1 d . . . H3A H 0.6965 0.3867 0.5093 0.027 Uiso 1 1 calc R . . H3B H 0.7388 0.6007 0.5557 0.027 Uiso 1 1 calc R . . C4 C 0.6995(3) 0.3682(14) 0.6308(4) 0.0229(15) Uani 1 1 d . . . H4A H 0.6623 0.2746 0.6276 0.027 Uiso 1 1 calc R . . H4B H 0.7019 0.4971 0.6748 0.027 Uiso 1 1 calc R . . C5 C 0.8165(3) 0.3641(14) 0.6715(4) 0.0232(15) Uani 1 1 d . . . H5A H 0.8221 0.4468 0.6207 0.028 Uiso 1 1 calc R . . H5B H 0.8065 0.5053 0.7070 0.028 Uiso 1 1 calc R . . C6 C 0.8727(3) 0.2356(14) 0.7093(4) 0.0241(15) Uani 1 1 d . . . H6A H 0.8687 0.1789 0.7637 0.029 Uiso 1 1 calc R . . H6B H 0.9035 0.3698 0.7139 0.029 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 Ge1 0.0208(6) 0.0196(6) 0.0314(6) 0.000 -0.0017(4) 0.000 Cl1 0.0303(9) 0.0349(11) 0.0253(9) -0.0020(8) 0.0034(7) -0.0063(8) S1 0.0221(9) 0.0200(9) 0.0244(9) 0.0014(7) -0.0005(7) -0.0018(7) S2 0.0329(10) 0.0224(10) 0.0270(9) 0.0005(7) -0.0041(7) 0.0026(8) S3 0.0207(9) 0.0200(9) 0.0256(9) 0.0023(7) 0.0004(7) -0.0015(7) C1 0.029(4) 0.020(4) 0.023(4) 0.004(3) 0.002(3) -0.001(3) C2 0.023(4) 0.028(4) 0.029(4) 0.003(3) 0.004(3) 0.002(3) C3 0.020(3) 0.028(4) 0.020(3) 0.004(3) 0.003(3) 0.008(3) C4 0.024(3) 0.027(4) 0.018(3) -0.002(3) 0.002(3) 0.003(3) C5 0.023(4) 0.018(4) 0.029(4) -0.002(3) 0.006(3) -0.005(3) C6 0.020(3) 0.025(4) 0.026(4) -0.007(3) -0.001(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 # Ge1 Cl1 3.985(2) 1_545 ? # Ge1 Cl1 3.985(2) 2_645 ? Ge1 Cl1 2.290(2) 2_655 ? Ge1 Cl1 2.290(2) . ? Ge1 S1 2.7383(17) . ? Ge1 S1 2.7383(17) 2_655 ? S1 C6 1.821(7) 7_656 ? S1 C1 1.822(7) . ? S2 C3 1.808(6) . ? S2 C2 1.817(7) . ? S3 C4 1.808(7) . ? S3 C5 1.813(7) . ? C1 C2 1.532(9) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.523(9) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.525(9) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 S1 1.821(7) 7_656 ? C6 H6A 0.9900 . ? C6 H6B 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 Ge1 Cl1 98.91(10) 2_655 . ? Cl1 Ge1 S1 88.33(6) 2_655 . ? Cl1 Ge1 S1 90.30(6) . . ? Cl1 Ge1 S1 90.30(6) 2_655 2_655 ? Cl1 Ge1 S1 88.33(6) . 2_655 ? S1 Ge1 S1 177.89(9) . 2_655 ? Cl1 Ge1 Cl1 156.44(6) 2_655 1_545 ? Cl1 Ge1 Cl1 104.65(6) . 1_545 ? S1 Ge1 Cl1 91.52(5) . 1_545 ? S1 Ge1 Cl1 90.38(5) 2_655 1_545 ? Cl1 Ge1 Cl1 104.65(6) 2_655 2_645 ? Cl1 Ge1 Cl1 156.44(6) . 2_645 ? S1 Ge1 Cl1 90.38(5) . 2_645 ? S1 Ge1 Cl1 91.52(5) 2_655 2_645 ? Cl1 Ge1 Cl1 51.79(6) 1_545 2_645 ? C6 S1 C1 100.4(3) 7_656 . ? C6 S1 Ge1 89.6(2) 7_656 . ? C1 S1 Ge1 97.2(2) . . ? C3 S2 C2 103.3(3) . . ? C4 S3 C5 98.2(3) . . ? C2 C1 S1 112.4(5) . . ? C2 C1 H1A 109.1 . . ? S1 C1 H1A 109.1 . . ? C2 C1 H1B 109.1 . . ? S1 C1 H1B 109.1 . . ? H1A C1 H1B 107.9 . . ? C1 C2 S2 115.9(5) . . ? C1 C2 H2A 108.3 . . ? S2 C2 H2A 108.3 . . ? C1 C2 H2B 108.3 . . ? S2 C2 H2B 108.3 . . ? H2A C2 H2B 107.4 . . ? C4 C3 S2 114.1(5) . . ? C4 C3 H3A 108.7 . . ? S2 C3 H3A 108.7 . . ? C4 C3 H3B 108.7 . . ? S2 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? C3 C4 S3 112.9(5) . . ? C3 C4 H4A 109.0 . . ? S3 C4 H4A 109.0 . . ? C3 C4 H4B 109.0 . . ? S3 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? C6 C5 S3 113.0(5) . . ? C6 C5 H5A 109.0 . . ? S3 C5 H5A 109.0 . . ? C6 C5 H5B 109.0 . . ? S3 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? C5 C6 S1 114.9(5) . 7_656 ? C5 C6 H6A 108.5 . . ? S1 C6 H6A 108.5 7_656 . ? C5 C6 H6B 108.5 . . ? S1 C6 H6B 108.5 7_656 . ? H6A C6 H6B 107.5 . . ? 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 S1 C1 C2 S2 -54.1(6) . . . . ? S2 C3 C4 S3 -177.1(4) . . . . ? S3 C5 C6 S1 54.0(6) . . . 7_656 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.654 _refine_diff_density_min -0.738 _refine_diff_density_rms 0.178 #===END OF CIF ============================================================== # 09wz813.cif CCDC-781121 data_09wz813 _database_code_depnum_ccdc_archive 'CCDC 781121' #TrackingRef '- GeX2_all8_3.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2010-03-22 _audit_author_name 'Webster, M.' _chemical_name_systematic ; Chloro(1,4,7-trioxa-10,13,16-trithiacyclooctadecane)germanium(II) trichlorogermanate ; # C12H24O3S3 = [18]aneO3S3 # 1,4,7-trioxa-10,13,16-trithiacyclooctadecane (iLab defaults) _chemical_name_common ; Chloro(1,4,7-trioxa-10,13,16- trithiacyclooctadecane)germanium(ii) trichlorogermanate ; _chemical_melting_point ? _chemical_formula_moiety 'C12 H24 Cl1 Ge1 O3 S3 1+, Cl3 Ge1 1-' _chemical_formula_sum 'C12 H24 Cl4 Ge2 O3 S3' _chemical_formula_weight 599.47 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' Ge Ge 0.1547 1.8001 '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' _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' 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 13.906(3) _cell_length_b 11.583(2) _cell_length_c 14.273(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.159(10) _cell_angle_gamma 90.00 _cell_volume 2275.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5276 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.750 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 3.396 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7534 # shelxl 0.7276 _exptl_absorpt_correction_T_max 1.0000 # 0.9352 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. 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 '10cm confocal mirrors' _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_% ? _diffrn_reflns_number 25335 _diffrn_reflns_av_R_equivalents 0.0860 _diffrn_reflns_av_sigmaI/netI 0.0811 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 27.54 _reflns_number_total 5190 _reflns_number_gt 3651 _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^)+(0.0000P)^2^+16.9448P] 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 5190 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1209 _refine_ls_R_factor_gt 0.0738 _refine_ls_wR_factor_ref 0.1338 _refine_ls_wR_factor_gt 0.1174 _refine_ls_goodness_of_fit_ref 1.182 _refine_ls_restrained_S_all 1.182 _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 Ge1 Ge 0.81568(5) 0.02470(6) 0.16979(5) 0.01974(17) Uani 1 1 d . . . Cl1 Cl 0.89257(12) 0.17487(13) 0.11310(11) 0.0238(4) Uani 1 1 d . . . S1 S 0.95954(12) 0.02792(14) 0.32540(11) 0.0199(3) Uani 1 1 d . . . S2 S 0.80900(14) 0.06976(16) 0.47252(12) 0.0309(4) Uani 1 1 d . . . S3 S 0.72643(12) 0.19071(15) 0.27142(12) 0.0233(4) Uani 1 1 d . . . O1 O 0.6715(3) 0.1091(4) 0.0601(3) 0.0251(10) Uani 1 1 d . . . O2 O 0.7881(3) -0.0642(4) 0.0073(3) 0.0255(10) Uani 1 1 d . . . O3 O 0.9597(3) -0.0854(4) 0.1285(3) 0.0196(9) Uani 1 1 d . . . C1 C 0.9228(5) -0.0888(6) 0.3990(4) 0.0214(14) Uani 1 1 d . . . H1A H 0.9279 -0.1637 0.3666 0.026 Uiso 1 1 calc R . . H1B H 0.9669 -0.0910 0.4599 0.026 Uiso 1 1 calc R . . C2 C 0.8185(5) -0.0708(6) 0.4178(5) 0.0246(15) Uani 1 1 d . . . H2A H 0.8004 -0.1322 0.4603 0.029 Uiso 1 1 calc R . . H2B H 0.7735 -0.0749 0.3576 0.029 Uiso 1 1 calc R . . C3 C 0.6812(5) 0.1041(7) 0.4395(5) 0.0325(17) Uani 1 1 d . . . H3A H 0.6421 0.0471 0.4695 0.039 Uiso 1 1 calc R . . H3B H 0.6686 0.1810 0.4656 0.039 Uiso 1 1 calc R . . C4 C 0.6463(5) 0.1053(6) 0.3340(5) 0.0253(15) Uani 1 1 d . . . H4A H 0.5798 0.1378 0.3222 0.030 Uiso 1 1 calc R . . H4B H 0.6437 0.0252 0.3096 0.030 Uiso 1 1 calc R . . C5 C 0.6382(5) 0.2459(6) 0.1751(5) 0.0289(16) Uani 1 1 d . . . H5A H 0.5848 0.2840 0.2025 0.035 Uiso 1 1 calc R . . H5B H 0.6701 0.3055 0.1404 0.035 Uiso 1 1 calc R . . C6 C 0.5948(5) 0.1550(6) 0.1052(5) 0.0276(16) Uani 1 1 d . . . H6A H 0.5644 0.0930 0.1386 0.033 Uiso 1 1 calc R . . H6B H 0.5444 0.1898 0.0576 0.033 Uiso 1 1 calc R . . C7 C 0.6384(5) 0.0334(6) -0.0171(5) 0.0299(16) Uani 1 1 d . . . H7A H 0.5902 0.0734 -0.0637 0.036 Uiso 1 1 calc R . . H7B H 0.6072 -0.0356 0.0063 0.036 Uiso 1 1 calc R . . C8 C 0.7238(5) -0.0012(7) -0.0620(5) 0.0309(17) Uani 1 1 d . . . H8A H 0.7030 -0.0503 -0.1180 0.037 Uiso 1 1 calc R . . H8B H 0.7569 0.0679 -0.0828 0.037 Uiso 1 1 calc R . . C9 C 0.8752(5) -0.1000(6) -0.0268(5) 0.0233(14) Uani 1 1 d . . . H9A H 0.9115 -0.0320 -0.0450 0.028 Uiso 1 1 calc R . . H9B H 0.8595 -0.1504 -0.0830 0.028 Uiso 1 1 calc R . . C10 C 0.9349(5) -0.1648(6) 0.0518(4) 0.0243(15) Uani 1 1 d . . . H10A H 0.8973 -0.2304 0.0723 0.029 Uiso 1 1 calc R . . H10B H 0.9945 -0.1955 0.0302 0.029 Uiso 1 1 calc R . . C11 C 1.0265(5) -0.1358(6) 0.2045(4) 0.0213(14) Uani 1 1 d . . . H11A H 1.0838 -0.1678 0.1796 0.026 Uiso 1 1 calc R . . H11B H 0.9944 -0.1990 0.2350 0.026 Uiso 1 1 calc R . . C12 C 1.0571(5) -0.0420(6) 0.2747(5) 0.0233(14) Uani 1 1 d . . . H12A H 1.0924 0.0177 0.2434 0.028 Uiso 1 1 calc R . . H12B H 1.1033 -0.0750 0.3270 0.028 Uiso 1 1 calc R . . Ge2 Ge 0.33836(6) 0.29943(7) 0.88551(5) 0.0307(2) Uani 1 1 d . . . Cl2 Cl 0.39691(15) 0.45966(17) 0.82133(18) 0.0482(6) Uani 1 1 d . . . Cl3 Cl 0.20523(12) 0.27903(15) 0.77162(12) 0.0296(4) Uani 1 1 d . . . Cl4 Cl 0.43132(13) 0.16849(16) 0.81698(15) 0.0393(5) 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 Ge1 0.0236(4) 0.0178(3) 0.0178(3) 0.0003(3) 0.0031(3) -0.0026(3) Cl1 0.0310(9) 0.0175(8) 0.0243(8) 0.0008(6) 0.0081(7) -0.0055(7) S1 0.0252(8) 0.0183(8) 0.0158(7) 0.0001(6) 0.0017(6) -0.0010(7) S2 0.0389(11) 0.0325(10) 0.0208(9) -0.0062(7) 0.0019(8) 0.0088(8) S3 0.0257(9) 0.0216(9) 0.0232(8) 0.0006(7) 0.0058(7) 0.0020(7) O1 0.021(2) 0.030(3) 0.023(2) -0.001(2) 0.000(2) 0.004(2) O2 0.028(3) 0.031(3) 0.017(2) -0.0002(19) 0.003(2) 0.000(2) O3 0.023(2) 0.022(2) 0.014(2) -0.0039(17) 0.0025(18) 0.0009(19) C1 0.027(4) 0.019(3) 0.019(3) 0.005(3) 0.004(3) 0.002(3) C2 0.026(4) 0.025(4) 0.024(3) 0.002(3) 0.005(3) 0.001(3) C3 0.042(4) 0.031(4) 0.028(4) 0.001(3) 0.016(3) 0.013(4) C4 0.015(3) 0.033(4) 0.030(4) 0.004(3) 0.011(3) 0.002(3) C5 0.029(4) 0.026(4) 0.034(4) 0.009(3) 0.011(3) 0.008(3) C6 0.024(4) 0.029(4) 0.030(4) 0.007(3) 0.003(3) 0.009(3) C7 0.029(4) 0.028(4) 0.029(4) -0.008(3) -0.007(3) 0.000(3) C8 0.037(4) 0.034(4) 0.020(3) 0.001(3) -0.001(3) 0.007(3) C9 0.031(4) 0.017(3) 0.022(3) -0.006(3) 0.005(3) 0.003(3) C10 0.029(4) 0.025(4) 0.020(3) -0.008(3) 0.007(3) 0.002(3) C11 0.022(3) 0.023(4) 0.018(3) 0.001(3) 0.001(3) 0.003(3) C12 0.021(3) 0.026(4) 0.023(3) 0.002(3) 0.002(3) 0.000(3) Ge2 0.0309(4) 0.0370(5) 0.0239(4) -0.0033(3) 0.0027(3) -0.0032(4) Cl2 0.0383(11) 0.0232(10) 0.0836(17) -0.0010(10) 0.0103(11) -0.0038(9) Cl3 0.0254(9) 0.0290(10) 0.0335(9) 0.0033(7) 0.0005(7) 0.0012(7) Cl4 0.0297(10) 0.0286(10) 0.0598(13) 0.0068(9) 0.0074(9) 0.0068(8) _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 Ge1 Cl1 2.2515(17) . ? Ge1 O3 2.514(4) . ? Ge1 O2 2.516(4) . ? Ge1 O1 2.556(4) . ? Ge1 S1 2.7703(17) . ? Ge1 S3 2.8022(18) . ? Ge1 S2 4.366(2) . ? S1 C12 1.815(7) . ? S1 C1 1.829(6) . ? S2 C3 1.818(8) . ? S2 C2 1.818(7) . ? S3 C4 1.817(6) . ? S3 C5 1.824(7) . ? O1 C6 1.425(8) . ? O1 C7 1.432(8) . ? O2 C9 1.430(8) . ? O2 C8 1.436(8) . ? O3 C10 1.434(7) . ? O3 C11 1.447(7) . ? C1 C2 1.527(9) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.515(9) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.515(10) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.482(10) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.498(9) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.499(9) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? Ge2 Cl2 2.271(2) . ? Ge2 Cl3 2.2959(19) . ? Ge2 Cl4 2.299(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Ge1 O3 82.70(11) . . ? Cl1 Ge1 O2 90.15(11) . . ? O3 Ge1 O2 66.32(14) . . ? Cl1 Ge1 O1 81.71(12) . . ? O3 Ge1 O1 129.20(14) . . ? O2 Ge1 O1 65.70(15) . . ? Cl1 Ge1 S1 87.25(6) . . ? O3 Ge1 S1 71.72(10) . . ? O2 Ge1 S1 137.94(11) . . ? O1 Ge1 S1 154.17(11) . . ? Cl1 Ge1 S3 85.63(6) . . ? O3 Ge1 S3 153.59(10) . . ? O2 Ge1 S3 137.48(11) . . ? O1 Ge1 S3 71.82(11) . . ? S1 Ge1 S3 84.16(5) . . ? Cl1 Ge1 S2 109.95(5) . . ? O3 Ge1 S2 114.98(10) . . ? O2 Ge1 S2 159.90(11) . . ? O1 Ge1 S2 115.80(10) . . ? S1 Ge1 S2 47.11(4) . . ? S3 Ge1 S2 48.13(4) . . ? C12 S1 C1 100.6(3) . . ? C12 S1 Ge1 99.8(2) . . ? C1 S1 Ge1 102.8(2) . . ? C3 S2 C2 102.3(3) . . ? C3 S2 Ge1 85.8(2) . . ? C2 S2 Ge1 57.0(2) . . ? C4 S3 C5 99.7(3) . . ? C4 S3 Ge1 103.2(2) . . ? C5 S3 Ge1 98.7(2) . . ? C6 O1 C7 113.4(5) . . ? C6 O1 Ge1 116.0(4) . . ? C7 O1 Ge1 112.1(4) . . ? C9 O2 C8 112.9(5) . . ? C9 O2 Ge1 114.0(4) . . ? C8 O2 Ge1 115.2(4) . . ? C10 O3 C11 111.9(5) . . ? C10 O3 Ge1 113.0(4) . . ? C11 O3 Ge1 118.5(3) . . ? C2 C1 S1 110.5(4) . . ? C2 C1 H1A 109.6 . . ? S1 C1 H1A 109.6 . . ? C2 C1 H1B 109.6 . . ? S1 C1 H1B 109.6 . . ? H1A C1 H1B 108.1 . . ? C1 C2 S2 109.1(5) . . ? C1 C2 H2A 109.9 . . ? S2 C2 H2A 109.9 . . ? C1 C2 H2B 109.9 . . ? S2 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? C4 C3 S2 115.0(5) . . ? C4 C3 H3A 108.5 . . ? S2 C3 H3A 108.5 . . ? C4 C3 H3B 108.5 . . ? S2 C3 H3B 108.5 . . ? H3A C3 H3B 107.5 . . ? C3 C4 S3 111.2(5) . . ? C3 C4 H4A 109.4 . . ? S3 C4 H4A 109.4 . . ? C3 C4 H4B 109.4 . . ? S3 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C6 C5 S3 114.5(5) . . ? C6 C5 H5A 108.6 . . ? S3 C5 H5A 108.6 . . ? C6 C5 H5B 108.6 . . ? S3 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? O1 C6 C5 107.7(6) . . ? O1 C6 H6A 110.2 . . ? C5 C6 H6A 110.2 . . ? O1 C6 H6B 110.2 . . ? C5 C6 H6B 110.2 . . ? H6A C6 H6B 108.5 . . ? O1 C7 C8 108.0(6) . . ? O1 C7 H7A 110.1 . . ? C8 C7 H7A 110.1 . . ? O1 C7 H7B 110.1 . . ? C8 C7 H7B 110.1 . . ? H7A C7 H7B 108.4 . . ? O2 C8 C7 107.4(5) . . ? O2 C8 H8A 110.2 . . ? C7 C8 H8A 110.2 . . ? O2 C8 H8B 110.2 . . ? C7 C8 H8B 110.2 . . ? H8A C8 H8B 108.5 . . ? O2 C9 C10 107.3(5) . . ? O2 C9 H9A 110.3 . . ? C10 C9 H9A 110.3 . . ? O2 C9 H9B 110.3 . . ? C10 C9 H9B 110.3 . . ? H9A C9 H9B 108.5 . . ? O3 C10 C9 107.3(5) . . ? O3 C10 H10A 110.3 . . ? C9 C10 H10A 110.3 . . ? O3 C10 H10B 110.3 . . ? C9 C10 H10B 110.3 . . ? H10A C10 H10B 108.5 . . ? O3 C11 C12 107.5(5) . . ? O3 C11 H11A 110.2 . . ? C12 C11 H11A 110.2 . . ? O3 C11 H11B 110.2 . . ? C12 C11 H11B 110.2 . . ? H11A C11 H11B 108.5 . . ? C11 C12 S1 115.6(5) . . ? C11 C12 H12A 108.4 . . ? S1 C12 H12A 108.4 . . ? C11 C12 H12B 108.4 . . ? S1 C12 H12B 108.4 . . ? H12A C12 H12B 107.4 . . ? Cl2 Ge2 Cl3 95.60(8) . . ? Cl2 Ge2 Cl4 96.43(8) . . ? Cl3 Ge2 Cl4 94.38(7) . . ? 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 S1 C1 C2 S2 -56.7(5) . . . . ? S2 C3 C4 S3 -49.3(7) . . . . ? S3 C5 C6 O1 -63.8(6) . . . . ? O1 C7 C8 O2 63.0(7) . . . . ? O2 C9 C10 O3 -63.2(6) . . . . ? O3 C11 C12 S1 58.7(6) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.919 _refine_diff_density_min -0.710 _refine_diff_density_rms 0.173 #===END OF CIF ============================================================== # 10wz211.cif CCDC-781122 data_10wz211 _database_code_depnum_ccdc_archive 'CCDC 781122' #TrackingRef '- GeX2_all8_3.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2010-03-28 _audit_author_name 'Webster, M.' _chemical_name_systematic ; chloro(1,4,7-trioxa-10,13,16-trithiacyclooctadecane)germanium(II) trifluoromethanesulfonate ; # [F3CSO3]- = triflate anion = trifluoromethanesulphonate # trifluoromethanesulfonate (iLab (defaults & selected options) & chemspider) # The CSD uses 'f' for the nearly all and 'ph' for two entries - 'f' wins. # # C12H24O3S3 = [18]aneO3S3 = # 1,4,7-trioxa-10,13,16-trithiacyclooctadecane (iLab defaults) _chemical_name_common ; chloro(1,4,7-trioxa-10,13,16- trithiacyclooctadecane)germanium(ii) trifluoromethanesulfonate ; _chemical_melting_point ? _chemical_formula_moiety 'C12 H24 Cl Ge O3 S3 1+, C F3 O3 S 1-' _chemical_formula_sum 'C13 H24 Cl F3 Ge O6 S4' _chemical_formula_weight 569.60 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' Ge Ge 0.1547 1.8001 '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' _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' 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 14.504(4) _cell_length_b 11.482(4) _cell_length_c 14.671(5) _cell_angle_alpha 90.00 _cell_angle_beta 115.585(15) _cell_angle_gamma 90.00 _cell_volume 2203.7(12) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 31939 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.717 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 1.942 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5022 # 0.8295 _exptl_absorpt_correction_T_max 1.0000 # 0.9808 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. 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 '10cm confocal mirrors' _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_% ? _diffrn_reflns_number 22647 _diffrn_reflns_av_R_equivalents 0.2154 _diffrn_reflns_av_sigmaI/netI 0.1714 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4312 _reflns_number_gt 2390 _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 ? _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^)+(0.0000P)^2^+28.2100P] 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 4312 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2110 _refine_ls_R_factor_gt 0.1093 _refine_ls_wR_factor_ref 0.1987 _refine_ls_wR_factor_gt 0.1631 _refine_ls_goodness_of_fit_ref 1.165 _refine_ls_restrained_S_all 1.165 _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 Ge1 Ge 0.18688(9) 0.47653(11) 0.26918(9) 0.0254(3) Uani 1 1 d . . . Cl1 Cl 0.1051(2) 0.3241(2) 0.1667(2) 0.0319(7) Uani 1 1 d . . . S1 S 0.0342(2) 0.4683(3) 0.3403(2) 0.0284(7) Uani 1 1 d . . . S2 S 0.1903(2) 0.4150(3) 0.5714(2) 0.0331(7) Uani 1 1 d . . . S3 S 0.2860(2) 0.2960(3) 0.4308(2) 0.0320(7) Uani 1 1 d . . . O1 O 0.3436(6) 0.3869(7) 0.2574(6) 0.035(2) Uani 1 1 d . . . O2 O 0.2210(6) 0.5597(7) 0.1375(6) 0.0325(19) Uani 1 1 d . . . O3 O 0.0422(6) 0.5870(6) 0.1527(5) 0.0288(18) Uani 1 1 d . . . C1 C 0.0782(8) 0.5827(10) 0.4366(8) 0.028(3) Uani 1 1 d . . . H1A H 0.0773 0.6587 0.4043 0.034 Uiso 1 1 calc R . . H1B H 0.0316 0.5877 0.4697 0.034 Uiso 1 1 calc R . . C2 C 0.1844(9) 0.5567(10) 0.5140(9) 0.033(3) Uani 1 1 d . . . H2A H 0.2064 0.6175 0.5671 0.040 Uiso 1 1 calc R . . H2B H 0.2319 0.5581 0.4817 0.040 Uiso 1 1 calc R . . C3 C 0.3245(9) 0.3814(12) 0.6196(9) 0.039(3) Uani 1 1 d . . . H3A H 0.3632 0.4390 0.6726 0.046 Uiso 1 1 calc R . . H3B H 0.3364 0.3038 0.6521 0.046 Uiso 1 1 calc R . . C4 C 0.3671(9) 0.3809(10) 0.5421(8) 0.031(3) Uani 1 1 d . . . H4A H 0.4368 0.3474 0.5725 0.038 Uiso 1 1 calc R . . H4B H 0.3720 0.4620 0.5215 0.038 Uiso 1 1 calc R . . C5 C 0.3798(9) 0.2487(10) 0.3865(10) 0.036(3) Uani 1 1 d . . . H5A H 0.4367 0.2093 0.4429 0.043 Uiso 1 1 calc R . . H5B H 0.3473 0.1906 0.3320 0.043 Uiso 1 1 calc R . . C6 C 0.4237(9) 0.3449(12) 0.3473(9) 0.041(3) Uani 1 1 d . . . H6A H 0.4505 0.4083 0.3978 0.050 Uiso 1 1 calc R . . H6B H 0.4803 0.3149 0.3333 0.050 Uiso 1 1 calc R . . C7 C 0.3794(9) 0.4647(12) 0.2032(10) 0.045(3) Uani 1 1 d . . . H7A H 0.4328 0.4265 0.1886 0.054 Uiso 1 1 calc R . . H7B H 0.4087 0.5359 0.2434 0.054 Uiso 1 1 calc R . . C8 C 0.2894(10) 0.4943(11) 0.1077(9) 0.045(4) Uani 1 1 d . . . H8A H 0.3102 0.5420 0.0636 0.054 Uiso 1 1 calc R . . H8B H 0.2556 0.4227 0.0708 0.054 Uiso 1 1 calc R . . C9 C 0.1336(9) 0.6071(10) 0.0536(8) 0.031(3) Uani 1 1 d . . . H9A H 0.0921 0.5439 0.0088 0.037 Uiso 1 1 calc R . . H9B H 0.1556 0.6605 0.0138 0.037 Uiso 1 1 calc R . . C10 C 0.0723(9) 0.6722(10) 0.0980(9) 0.034(3) Uani 1 1 d . . . H10A H 0.1142 0.7342 0.1442 0.041 Uiso 1 1 calc R . . H10B H 0.0113 0.7083 0.0438 0.041 Uiso 1 1 calc R . . C11 C -0.0251(8) 0.6383(10) 0.1902(9) 0.033(3) Uani 1 1 d . . . H11A H -0.0827 0.6774 0.1344 0.039 Uiso 1 1 calc R . . H11B H 0.0124 0.6973 0.2423 0.039 Uiso 1 1 calc R . . C12 C -0.0648(8) 0.5449(10) 0.2347(8) 0.032(3) Uani 1 1 d . . . H12A H -0.1033 0.4877 0.1812 0.039 Uiso 1 1 calc R . . H12B H -0.1133 0.5802 0.2578 0.039 Uiso 1 1 calc R . . S4 S 0.3196(2) 0.7462(3) 0.4063(2) 0.0352(8) Uani 1 1 d . . . F1 F 0.3347(7) 0.8347(11) 0.2517(7) 0.106(4) Uani 1 1 d . . . F2 F 0.3070(7) 0.9598(8) 0.3435(10) 0.106(4) Uani 1 1 d . . . F3 F 0.4536(6) 0.8885(9) 0.3916(7) 0.086(3) Uani 1 1 d . . . O4 O 0.3769(6) 0.6474(7) 0.3956(7) 0.047(2) Uani 1 1 d . . . O5 O 0.3537(7) 0.7875(8) 0.5068(6) 0.053(2) Uani 1 1 d . . . O6 O 0.2110(6) 0.7415(8) 0.3492(7) 0.052(3) Uani 1 1 d . . . C13 C 0.3515(10) 0.8561(15) 0.3418(12) 0.062(5) 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 Ge1 0.0296(7) 0.0236(6) 0.0245(7) -0.0008(6) 0.0131(5) -0.0016(6) Cl1 0.0404(17) 0.0264(15) 0.0296(16) -0.0062(12) 0.0160(14) -0.0061(13) S1 0.0294(16) 0.0296(15) 0.0259(15) -0.0022(13) 0.0118(13) -0.0022(14) S2 0.0366(18) 0.0330(17) 0.0320(18) 0.0039(14) 0.0169(15) 0.0003(14) S3 0.0354(18) 0.0338(17) 0.0273(17) 0.0009(13) 0.0141(14) 0.0015(14) O1 0.038(5) 0.044(5) 0.025(5) 0.002(4) 0.016(4) 0.001(4) O2 0.035(5) 0.035(5) 0.035(5) 0.003(4) 0.022(4) 0.005(4) O3 0.033(4) 0.028(4) 0.027(4) 0.002(3) 0.015(4) 0.003(4) C1 0.025(6) 0.026(6) 0.032(7) -0.002(5) 0.011(5) -0.001(5) C2 0.034(7) 0.032(7) 0.031(7) 0.001(5) 0.012(6) -0.004(5) C3 0.034(7) 0.049(8) 0.025(7) 0.007(6) 0.006(6) 0.004(6) C4 0.036(7) 0.022(6) 0.030(7) -0.006(5) 0.009(6) -0.001(5) C5 0.038(7) 0.027(6) 0.044(8) -0.001(6) 0.019(7) 0.007(6) C6 0.032(7) 0.057(9) 0.036(8) 0.006(7) 0.016(7) 0.009(6) C7 0.040(8) 0.054(8) 0.058(9) 0.012(8) 0.038(7) 0.019(7) C8 0.072(10) 0.039(8) 0.042(8) 0.015(6) 0.042(8) 0.017(7) C9 0.039(7) 0.025(6) 0.028(7) 0.009(5) 0.014(6) 0.013(5) C10 0.036(7) 0.037(7) 0.028(7) 0.006(5) 0.012(6) 0.006(6) C11 0.026(7) 0.041(7) 0.029(7) -0.003(6) 0.009(6) 0.001(6) C12 0.031(6) 0.040(8) 0.025(6) -0.005(5) 0.012(5) -0.001(6) S4 0.0367(18) 0.0334(17) 0.0332(18) 0.0027(14) 0.0129(15) 0.0013(14) F1 0.073(7) 0.177(12) 0.051(6) 0.052(7) 0.010(5) -0.020(7) F2 0.063(6) 0.063(6) 0.178(12) 0.063(7) 0.041(7) 0.011(5) F3 0.033(5) 0.120(8) 0.088(7) 0.056(6) 0.009(5) -0.018(5) O4 0.041(5) 0.034(5) 0.059(6) -0.013(4) 0.013(5) 0.003(4) O5 0.057(6) 0.068(7) 0.034(5) -0.013(5) 0.021(5) -0.009(5) O6 0.032(5) 0.058(6) 0.064(7) 0.012(5) 0.019(5) 0.003(5) C13 0.038(9) 0.095(13) 0.059(11) 0.071(9) 0.027(8) 0.041(8) _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 # Ge1 S2 4.469(4) . ? Ge1 Cl1 2.278(3) . ? Ge1 O2 2.390(7) . ? Ge1 O3 2.416(7) . ? Ge1 O1 2.567(8) . ? Ge1 S1 2.828(3) . ? Ge1 S3 3.007(3) . ? S1 C12 1.821(11) . ? S1 C1 1.829(11) . ? S2 C3 1.801(12) . ? S2 C2 1.817(11) . ? S3 C5 1.826(11) . ? S3 C4 1.829(11) . ? O1 C6 1.413(14) . ? O1 C7 1.434(14) . ? O2 C9 1.440(13) . ? O2 C8 1.453(13) . ? O3 C11 1.437(12) . ? O3 C10 1.448(13) . ? C1 C2 1.497(15) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.510(15) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.507(16) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.484(17) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.507(15) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.494(15) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? S4 O5 1.420(9) . ? S4 O6 1.431(9) . ? S4 O4 1.454(9) . ? S4 C13 1.754(13) . ? F1 C13 1.262(18) . ? F2 C13 1.360(18) . ? F3 C13 1.389(17) . ? 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 Ge1 O2 90.2(2) . . ? Cl1 Ge1 O3 83.7(2) . . ? O2 Ge1 O3 68.8(2) . . ? Cl1 Ge1 O1 82.6(2) . . ? O2 Ge1 O1 66.9(2) . . ? O3 Ge1 O1 133.4(2) . . ? Cl1 Ge1 S1 87.17(10) . . ? O2 Ge1 S1 141.27(19) . . ? O3 Ge1 S1 72.48(18) . . ? O1 Ge1 S1 150.26(19) . . ? Cl1 Ge1 S3 85.75(10) . . ? O2 Ge1 S3 135.82(19) . . ? O3 Ge1 S3 153.27(18) . . ? O1 Ge1 S3 68.96(18) . . ? S1 Ge1 S3 82.52(9) . . ? Cl1 Ge1 S2 108.23(9) . . ? O2 Ge1 S2 161.3(2) . . ? O3 Ge1 S2 114.77(17) . . ? O1 Ge1 S2 111.86(18) . . ? S1 Ge1 S2 45.86(7) . . ? S3 Ge1 S2 46.53(7) . . ? C12 S1 C1 101.2(5) . . ? C12 S1 Ge1 97.2(4) . . ? C1 S1 Ge1 101.1(4) . . ? C3 S2 C2 101.5(6) . . ? C3 S2 Ge1 88.3(4) . . ? C2 S2 Ge1 54.6(4) . . ? C5 S3 C4 100.7(6) . . ? C5 S3 Ge1 95.8(4) . . ? C4 S3 Ge1 103.9(4) . . ? C6 O1 C7 112.4(9) . . ? C6 O1 Ge1 118.0(6) . . ? C7 O1 Ge1 109.3(6) . . ? C9 O2 C8 113.7(8) . . ? C9 O2 Ge1 115.4(6) . . ? C8 O2 Ge1 116.3(6) . . ? C11 O3 C10 110.6(8) . . ? C11 O3 Ge1 118.1(6) . . ? C10 O3 Ge1 111.7(6) . . ? C2 C1 S1 110.2(8) . . ? C2 C1 H1A 109.6 . . ? S1 C1 H1A 109.6 . . ? C2 C1 H1B 109.6 . . ? S1 C1 H1B 109.6 . . ? H1A C1 H1B 108.1 . . ? C1 C2 S2 110.9(8) . . ? C1 C2 H2A 109.5 . . ? S2 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? S2 C2 H2B 109.5 . . ? H2A C2 H2B 108.0 . . ? C4 C3 S2 115.4(8) . . ? C4 C3 H3A 108.4 . . ? S2 C3 H3A 108.4 . . ? C4 C3 H3B 108.4 . . ? S2 C3 H3B 108.4 . . ? H3A C3 H3B 107.5 . . ? C3 C4 S3 111.1(8) . . ? C3 C4 H4A 109.4 . . ? S3 C4 H4A 109.4 . . ? C3 C4 H4B 109.4 . . ? S3 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C6 C5 S3 114.8(8) . . ? C6 C5 H5A 108.6 . . ? S3 C5 H5A 108.6 . . ? C6 C5 H5B 108.6 . . ? S3 C5 H5B 108.6 . . ? H5A C5 H5B 107.5 . . ? O1 C6 C5 107.1(10) . . ? O1 C6 H6A 110.3 . . ? C5 C6 H6A 110.3 . . ? O1 C6 H6B 110.3 . . ? C5 C6 H6B 110.3 . . ? H6A C6 H6B 108.6 . . ? O1 C7 C8 106.5(10) . . ? O1 C7 H7A 110.4 . . ? C8 C7 H7A 110.4 . . ? O1 C7 H7B 110.4 . . ? C8 C7 H7B 110.4 . . ? H7A C7 H7B 108.6 . . ? O2 C8 C7 105.7(9) . . ? O2 C8 H8A 110.6 . . ? C7 C8 H8A 110.6 . . ? O2 C8 H8B 110.6 . . ? C7 C8 H8B 110.6 . . ? H8A C8 H8B 108.7 . . ? O2 C9 C10 106.5(9) . . ? O2 C9 H9A 110.4 . . ? C10 C9 H9A 110.4 . . ? O2 C9 H9B 110.4 . . ? C10 C9 H9B 110.4 . . ? H9A C9 H9B 108.6 . . ? O3 C10 C9 106.2(9) . . ? O3 C10 H10A 110.5 . . ? C9 C10 H10A 110.5 . . ? O3 C10 H10B 110.5 . . ? C9 C10 H10B 110.5 . . ? H10A C10 H10B 108.7 . . ? O3 C11 C12 109.1(9) . . ? O3 C11 H11A 109.9 . . ? C12 C11 H11A 109.9 . . ? O3 C11 H11B 109.9 . . ? C12 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? C11 C12 S1 114.0(8) . . ? C11 C12 H12A 108.7 . . ? S1 C12 H12A 108.7 . . ? C11 C12 H12B 108.7 . . ? S1 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? O5 S4 O6 115.0(6) . . ? O5 S4 O4 114.4(6) . . ? O6 S4 O4 116.3(6) . . ? O5 S4 C13 105.4(8) . . ? O6 S4 C13 101.1(6) . . ? O4 S4 C13 102.0(6) . . ? F1 C13 F2 108.1(11) . . ? F1 C13 F3 106.4(11) . . ? F2 C13 F3 99.4(14) . . ? F1 C13 S4 116.7(14) . . ? F2 C13 S4 112.5(10) . . ? F3 C13 S4 112.2(8) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.814 _refine_diff_density_min -0.822 _refine_diff_density_rms 0.183 #===END OF CIF ============================================================== # 09wz815.cif CCDC-781123 data_09wz815 _database_code_depnum_ccdc_archive 'CCDC 781123' #TrackingRef '- GeX2_all8_3.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2010-03-21 _audit_author_name 'Webster, M.' _chemical_name_systematic ; Chloro(1,4,7-trioxa-10,13-dithiacyclopentadecane)germanium(II) trichlorogermanate ; # C10H20O3S2 # 1,4,7-trioxa-10,13-dithiacyclopentadecane (iLab defaults) # 1,4,7-trioxa-10,13-dithiacyclopentadecane (iLab selected options) _chemical_name_common ; Chloro(1,4,7-trioxa-10,13- dithiacyclopentadecane)germanium(ii) trichlorogermanate ; _chemical_melting_point ? _chemical_formula_moiety 'C10 H20 Cl Ge O3 S2 1+, Cl3 Ge 1-' _chemical_formula_sum 'C10 H20 Cl4 Ge2 O3 S2' _chemical_formula_weight 539.36 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' Ge Ge 0.1547 1.8001 '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' _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' 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 8.5320(10) _cell_length_b 10.355(2) _cell_length_c 21.696(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.029(10) _cell_angle_gamma 90.00 _cell_volume 1893.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4508 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.892 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 3.964 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8651 # shelxl 0.5356 _exptl_absorpt_correction_T_max 1.0000 # 0.8903 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. 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 '10cm confocal mirrors' _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_% ? _diffrn_reflns_number 25518 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4335 _reflns_number_gt 3788 _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 ? _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^)+(0.0000P)^2^+3.4511P] 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 4335 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0617 _refine_ls_wR_factor_gt 0.0580 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.137 _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 Ge1 Ge 0.10355(3) 0.52608(3) 0.201374(13) 0.01666(8) Uani 1 1 d . . . Cl1 Cl -0.08180(8) 0.41414(7) 0.24905(3) 0.02379(15) Uani 1 1 d . . . S1 S 0.29611(8) 0.34035(7) 0.24556(3) 0.01963(15) Uani 1 1 d . . . S2 S 0.07521(8) 0.37726(7) 0.10965(3) 0.01794(14) Uani 1 1 d . . . O1 O 0.1369(2) 0.68068(19) 0.08834(11) 0.0304(5) Uani 1 1 d . . . O2 O 0.3971(2) 0.56926(19) 0.16998(9) 0.0200(4) Uani 1 1 d . . . O3 O -0.1433(2) 0.59836(18) 0.11848(9) 0.0208(4) Uani 1 1 d . . . C1 C 0.2631(3) 0.2134(3) 0.18627(15) 0.0253(6) Uani 1 1 d . . . H1A H 0.3437 0.2212 0.1582 0.030 Uiso 1 1 calc R . . H1B H 0.2769 0.1280 0.2070 0.030 Uiso 1 1 calc R . . C2 C 0.0982(3) 0.2207(3) 0.14759(15) 0.0237(6) Uani 1 1 d . . . H2A H 0.0165 0.2093 0.1749 0.028 Uiso 1 1 calc R . . H2B H 0.0850 0.1513 0.1159 0.028 Uiso 1 1 calc R . . C3 C -0.1383(3) 0.3816(3) 0.08361(14) 0.0213(6) Uani 1 1 d . . . H3A H -0.1671 0.3226 0.0477 0.026 Uiso 1 1 calc R . . H3B H -0.1948 0.3532 0.1178 0.026 Uiso 1 1 calc R . . C4 C -0.1852(3) 0.5180(3) 0.06473(13) 0.0220(6) Uani 1 1 d . . . H4A H -0.1288 0.5468 0.0306 0.026 Uiso 1 1 calc R . . H4B H -0.3009 0.5229 0.0498 0.026 Uiso 1 1 calc R . . C5 C -0.1277(4) 0.7334(3) 0.10606(16) 0.0281(7) Uani 1 1 d . . . H5A H -0.1094 0.7806 0.1462 0.034 Uiso 1 1 calc R . . H5B H -0.2287 0.7650 0.0820 0.034 Uiso 1 1 calc R . . C6 C 0.0037(4) 0.7633(3) 0.07067(18) 0.0355(8) Uani 1 1 d . . . H6A H -0.0348 0.7534 0.0254 0.043 Uiso 1 1 calc R . . H6B H 0.0370 0.8543 0.0784 0.043 Uiso 1 1 calc R . . C7 C 0.2838(3) 0.7443(3) 0.10642(14) 0.0247(6) Uani 1 1 d . . . H7A H 0.2821 0.7929 0.1456 0.030 Uiso 1 1 calc R . . H7B H 0.3032 0.8061 0.0736 0.030 Uiso 1 1 calc R . . C8 C 0.4120(3) 0.6447(3) 0.11580(14) 0.0258(7) Uani 1 1 d . . . H8A H 0.4034 0.5881 0.0787 0.031 Uiso 1 1 calc R . . H8B H 0.5172 0.6874 0.1213 0.031 Uiso 1 1 calc R . . C9 C 0.5063(3) 0.4638(3) 0.17717(13) 0.0206(6) Uani 1 1 d . . . H9A H 0.6157 0.4960 0.1776 0.025 Uiso 1 1 calc R . . H9B H 0.4806 0.4028 0.1419 0.025 Uiso 1 1 calc R . . C10 C 0.4941(3) 0.3962(3) 0.23797(13) 0.0192(6) Uani 1 1 d . . . H10A H 0.5308 0.4562 0.2728 0.023 Uiso 1 1 calc R . . H10B H 0.5667 0.3211 0.2423 0.023 Uiso 1 1 calc R . . Ge2 Ge 0.57264(3) 0.05069(3) 0.070454(14) 0.02082(8) Uani 1 1 d . . . Cl2 Cl 0.80772(8) 0.05155(7) 0.03292(3) 0.02255(15) Uani 1 1 d . . . Cl3 Cl 0.68036(8) 0.12373(7) 0.16939(3) 0.02308(15) Uani 1 1 d . . . Cl4 Cl 0.48251(8) 0.25092(7) 0.03377(3) 0.02453(16) 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 Ge1 0.01465(14) 0.01881(15) 0.01661(15) -0.00028(11) 0.00276(11) -0.00027(11) Cl1 0.0167(3) 0.0327(4) 0.0230(4) 0.0056(3) 0.0063(3) -0.0003(3) S1 0.0146(3) 0.0231(3) 0.0208(4) 0.0044(3) 0.0015(3) 0.0010(3) S2 0.0166(3) 0.0179(3) 0.0190(3) -0.0006(3) 0.0019(3) 0.0008(3) O1 0.0143(10) 0.0186(10) 0.0574(15) 0.0065(10) 0.0029(10) 0.0012(8) O2 0.0175(9) 0.0265(10) 0.0171(10) 0.0058(8) 0.0060(8) 0.0027(8) O3 0.0222(10) 0.0151(9) 0.0247(11) -0.0005(8) 0.0028(8) -0.0018(8) C1 0.0210(14) 0.0190(14) 0.0342(17) -0.0008(12) -0.0010(12) 0.0022(12) C2 0.0205(14) 0.0165(14) 0.0326(17) 0.0013(12) -0.0004(12) 0.0003(11) C3 0.0160(13) 0.0213(14) 0.0242(15) -0.0031(12) -0.0046(11) -0.0015(11) C4 0.0200(14) 0.0242(15) 0.0204(15) 0.0021(12) -0.0017(11) 0.0009(12) C5 0.0226(15) 0.0181(14) 0.0427(19) 0.0048(13) 0.0026(13) -0.0010(12) C6 0.0207(15) 0.0268(17) 0.060(2) 0.0165(16) 0.0115(15) 0.0076(13) C7 0.0239(15) 0.0237(15) 0.0253(16) 0.0061(12) 0.0003(12) -0.0074(12) C8 0.0153(13) 0.0401(18) 0.0223(15) 0.0114(13) 0.0032(11) -0.0031(13) C9 0.0140(13) 0.0263(15) 0.0218(15) -0.0014(12) 0.0035(11) 0.0004(11) C10 0.0118(12) 0.0239(14) 0.0212(15) 0.0010(11) 0.0004(10) 0.0022(11) Ge2 0.01832(15) 0.01837(15) 0.02497(17) -0.00156(12) 0.00094(12) -0.00276(12) Cl2 0.0223(3) 0.0209(3) 0.0245(4) 0.0006(3) 0.0039(3) 0.0030(3) Cl3 0.0227(3) 0.0279(4) 0.0182(3) 0.0036(3) 0.0021(3) -0.0001(3) Cl4 0.0258(4) 0.0244(4) 0.0217(4) -0.0011(3) -0.0015(3) 0.0065(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 Ge1 Cl1 2.3297(8) . ? Ge1 S2 2.4985(8) . ? Ge1 S1 2.6120(8) . ? Ge1 O3 2.654(2) . ? Ge1 O2 2.7335(19) . ? Ge1 O1 2.979(2) . ? Ge1 Cl3 3.2650(9) 2_655 ? S1 C10 1.817(3) . ? S1 C1 1.830(3) . ? S2 C2 1.814(3) . ? S2 C3 1.821(3) . ? O1 C7 1.416(3) . ? O1 C6 1.426(3) . ? O2 C9 1.428(3) . ? O2 C8 1.434(3) . ? O3 C4 1.431(3) . ? O3 C5 1.434(3) . ? C1 C2 1.523(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.508(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.488(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.494(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.511(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? Ge2 Cl2 2.2800(8) . ? Ge2 Cl4 2.3090(8) . ? Ge2 Cl3 2.3249(8) . ? 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 Ge1 S2 93.39(3) . . ? Cl1 Ge1 S1 84.40(3) . . ? S2 Ge1 S1 79.33(3) . . ? Cl1 Ge1 O3 85.37(5) . . ? S2 Ge1 O3 70.54(5) . . ? S1 Ge1 O3 147.46(5) . . ? Cl1 Ge1 O2 154.74(4) . . ? S2 Ge1 O2 83.13(5) . . ? S1 Ge1 O2 70.35(4) . . ? O3 Ge1 O2 116.47(6) . . ? Cl1 Ge1 O1 142.36(4) . . ? S2 Ge1 O1 71.68(5) . . ? S1 Ge1 O1 124.19(4) . . ? O3 Ge1 O1 57.23(6) . . ? O2 Ge1 O1 59.83(5) . . ? Cl1 Ge1 Cl3 95.97(3) . 2_655 ? S2 Ge1 Cl3 147.78(2) . 2_655 ? S1 Ge1 Cl3 71.03(2) . 2_655 ? O3 Ge1 Cl3 140.88(4) . 2_655 ? O2 Ge1 Cl3 75.37(4) . 2_655 ? O1 Ge1 Cl3 115.24(5) . 2_655 ? C10 S1 C1 101.99(13) . . ? C10 S1 Ge1 105.80(9) . . ? C1 S1 Ge1 104.63(10) . . ? C2 S2 C3 101.21(13) . . ? C2 S2 Ge1 101.51(10) . . ? C3 S2 Ge1 101.48(10) . . ? C7 O1 C6 115.4(2) . . ? C7 O1 Ge1 102.51(16) . . ? C6 O1 Ge1 111.65(18) . . ? C9 O2 C8 111.5(2) . . ? C9 O2 Ge1 117.08(15) . . ? C8 O2 Ge1 119.75(15) . . ? C4 O3 C5 115.6(2) . . ? C4 O3 Ge1 117.30(15) . . ? C5 O3 Ge1 108.38(16) . . ? C2 C1 S1 112.2(2) . . ? C2 C1 H1A 109.2 . . ? S1 C1 H1A 109.2 . . ? C2 C1 H1B 109.2 . . ? S1 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? C1 C2 S2 108.6(2) . . ? C1 C2 H2A 110.0 . . ? S2 C2 H2A 110.0 . . ? C1 C2 H2B 110.0 . . ? S2 C2 H2B 110.0 . . ? H2A C2 H2B 108.3 . . ? C4 C3 S2 108.50(19) . . ? C4 C3 H3A 110.0 . . ? S2 C3 H3A 110.0 . . ? C4 C3 H3B 110.0 . . ? S2 C3 H3B 110.0 . . ? H3A C3 H3B 108.4 . . ? O3 C4 C3 107.5(2) . . ? O3 C4 H4A 110.2 . . ? C3 C4 H4A 110.2 . . ? O3 C4 H4B 110.2 . . ? C3 C4 H4B 110.2 . . ? H4A C4 H4B 108.5 . . ? O3 C5 C6 113.6(3) . . ? O3 C5 H5A 108.9 . . ? C6 C5 H5A 108.9 . . ? O3 C5 H5B 108.9 . . ? C6 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? O1 C6 C5 111.7(3) . . ? O1 C6 H6A 109.3 . . ? C5 C6 H6A 109.3 . . ? O1 C6 H6B 109.3 . . ? C5 C6 H6B 109.3 . . ? H6A C6 H6B 107.9 . . ? O1 C7 C8 108.3(2) . . ? O1 C7 H7A 110.0 . . ? C8 C7 H7A 110.0 . . ? O1 C7 H7B 110.0 . . ? C8 C7 H7B 110.0 . . ? H7A C7 H7B 108.4 . . ? O2 C8 C7 109.3(2) . . ? O2 C8 H8A 109.8 . . ? C7 C8 H8A 109.8 . . ? O2 C8 H8B 109.8 . . ? C7 C8 H8B 109.8 . . ? H8A C8 H8B 108.3 . . ? O2 C9 C10 108.4(2) . . ? O2 C9 H9A 110.0 . . ? C10 C9 H9A 110.0 . . ? O2 C9 H9B 110.0 . . ? C10 C9 H9B 110.0 . . ? H9A C9 H9B 108.4 . . ? C9 C10 S1 114.77(19) . . ? C9 C10 H10A 108.6 . . ? S1 C10 H10A 108.6 . . ? C9 C10 H10B 108.6 . . ? S1 C10 H10B 108.6 . . ? H10A C10 H10B 107.6 . . ? Cl2 Ge2 Cl4 97.90(3) . . ? Cl2 Ge2 Cl3 94.94(3) . . ? Cl4 Ge2 Cl3 95.06(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.678 _refine_diff_density_min -0.472 _refine_diff_density_rms 0.098 #===END OF CIF ============================================================== # 10wz304b.cif CCDC-781124 data_10wz304b _database_code_depnum_ccdc_archive 'CCDC 781124' #TrackingRef '- GeX2_all8_3.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2010-03-23 _audit_author_name 'Webster, M.' _chemical_name_systematic ; (1,5-diselenacyclo-octane-Se,Se')dichlorogermanium(II) ; # C6H12Se2 = [8]aneSe2 = 1,5-diselenacyclo-octane _chemical_name_common (1,5-diselenacyclo-octane-Se,Se')dichlorogermanium(ii) _chemical_melting_point ? _chemical_formula_moiety 'C6 H12 Cl2 Ge Se2' _chemical_formula_sum 'C6 H12 Cl2 Ge Se2' _chemical_formula_weight 385.57 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' Ge Ge 0.1547 1.8001 '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 orthorhombic _symmetry_space_group_name_H-M 'C m c 21' _space_group_IT_number 36 _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' _cell_length_a 9.049(2) _cell_length_b 11.602(3) _cell_length_c 10.610(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1114.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 745 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.299 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 9.707 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5910 # shelxl 0.3435 _exptl_absorpt_correction_T_max 0.7456 # 0.4436 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. 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_% ? _diffrn_reflns_number 5289 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.0519 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 27.50 _reflns_number_total 1243 _reflns_number_gt 1140 _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 ? _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^)+(0.0210P)^2^+1.4519P] 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 SHELXL _refine_ls_extinction_coef 0.0025(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(2) _chemical_absolute_configuration ad _refine_ls_number_reflns 1243 _refine_ls_number_parameters 59 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0354 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_ref 0.0704 _refine_ls_wR_factor_gt 0.0671 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.046 _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 Ge1 Ge 0.0000 0.07748(6) 0.43307(5) 0.0298(3) Uani 1 2 d S . . Cl1 Cl 0.0000 0.27003(14) 0.39027(17) 0.0354(4) Uani 1 2 d S . . Cl2 Cl 0.0000 0.09112(15) 0.64948(17) 0.0331(5) Uani 1 2 d S . . Se1 Se 0.31327(6) 0.07354(4) 0.45700(5) 0.02869(19) Uani 1 1 d . . . C1 C 0.3560(6) 0.1162(5) 0.2829(5) 0.0348(14) Uani 1 1 d . . . H1A H 0.2744 0.0876 0.2292 0.042 Uiso 1 1 calc R . . H1B H 0.3560 0.2014 0.2770 0.042 Uiso 1 1 calc R . . C2 C 0.5000 0.0723(6) 0.2293(7) 0.0354(18) Uani 1 2 d S . . H2A H 0.5000 -0.0127 0.2380 0.042 Uiso 1 2 calc SR . . H2B H 0.5000 0.0895 0.1379 0.042 Uiso 1 2 calc SR . . C3 C 0.3553(6) 0.2167(5) 0.5463(6) 0.0445(15) Uani 1 1 d . . . H3A H 0.2744 0.2717 0.5281 0.053 Uiso 1 1 calc R . . H3B H 0.3527 0.2005 0.6378 0.053 Uiso 1 1 calc R . . C4 C 0.5000 0.2755(6) 0.5168(7) 0.045(2) Uani 1 2 d S . . H4A H 0.5000 0.2932 0.4256 0.054 Uiso 1 2 calc SR . . H4B H 0.5000 0.3503 0.5618 0.054 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 Ge1 0.0455(4) 0.0245(4) 0.0193(6) -0.0016(3) 0.000 0.000 Cl1 0.0435(10) 0.0308(9) 0.0319(10) 0.0104(7) 0.000 0.000 Cl2 0.0485(12) 0.0350(9) 0.0158(9) 0.0008(7) 0.000 0.000 Se1 0.0376(3) 0.0287(3) 0.0198(3) 0.0013(2) 0.0013(3) 0.00764(19) C1 0.044(3) 0.035(4) 0.025(3) 0.000(2) -0.004(2) 0.006(2) C2 0.037(4) 0.046(5) 0.023(4) 0.001(3) 0.000 0.000 C3 0.050(3) 0.049(4) 0.035(3) -0.019(3) -0.007(3) 0.016(3) C4 0.075(6) 0.022(4) 0.040(5) -0.015(3) 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 # Ge1 Cl2 3.589(2) 3_554 ? Ge1 Cl1 2.2796(18) . ? Ge1 Cl2 2.302(2) . ? Ge1 Se1 2.8467(8) 4 ? Ge1 Se1 2.8467(8) . ? Se1 C3 1.950(6) . ? Se1 C1 1.951(5) . ? C1 C2 1.511(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C1 1.511(6) 4_655 ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.509(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C3 1.509(7) 4_655 ? C4 H4A 0.9900 . ? C4 H4B 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 Ge1 Cl2 97.55(7) . . ? Cl1 Ge1 Se1 91.920(17) . 4 ? Cl2 Ge1 Se1 84.958(16) . 4 ? Cl1 Ge1 Se1 91.920(17) . . ? Cl2 Ge1 Se1 84.958(16) . . ? Se1 Ge1 Se1 169.60(3) 4 . ? Cl1 Ge1 Cl2 111.54(6) . 3_554 ? Cl2 Ge1 Cl2 150.92(4) . 3_554 ? Se1 Ge1 Cl2 93.786(16) 4 3_554 ? Se1 Ge1 Cl2 93.786(16) . 3_554 ? C3 Se1 C1 101.8(3) . . ? C3 Se1 Ge1 102.94(17) . . ? C1 Se1 Ge1 96.24(16) . . ? C2 C1 Se1 116.2(4) . . ? C2 C1 H1A 108.2 . . ? Se1 C1 H1A 108.2 . . ? C2 C1 H1B 108.2 . . ? Se1 C1 H1B 108.2 . . ? H1A C1 H1B 107.4 . . ? C1 C2 C1 119.3(7) 4_655 . ? C1 C2 H2A 107.5 4_655 . ? C1 C2 H2A 107.5 . . ? C1 C2 H2B 107.5 4_655 . ? C1 C2 H2B 107.5 . . ? H2A C2 H2B 107.0 . . ? C4 C3 Se1 117.0(4) . . ? C4 C3 H3A 108.0 . . ? Se1 C3 H3A 108.0 . . ? C4 C3 H3B 108.0 . . ? Se1 C3 H3B 108.0 . . ? H3A C3 H3B 107.3 . . ? C3 C4 C3 120.4(6) 4_655 . ? C3 C4 H4A 107.2 4_655 . ? C3 C4 H4A 107.2 . . ? C3 C4 H4B 107.2 4_655 . ? C3 C4 H4B 107.2 . . ? H4A C4 H4B 106.9 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.685 _refine_diff_density_min -0.617 _refine_diff_density_rms 0.119 #===END OF CIF ============================================================== # 09wz819.cif CCDC-781125 data_09wz819 _database_code_depnum_ccdc_archive 'CCDC 781125' #TrackingRef '- GeX2_all8_3.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2010-03-22 _audit_author_name 'Webster, M.' _chemical_name_systematic ; (1,5,9,13-tetraselenacyclohexadecane)bis(dichlorogermanium(II)) dichloromethane solvate ; # C12H24Se4 = [16]aneSe4 # 1,5,9,13-tetraselenacyclohexadecane (iLab default & selected) _chemical_name_common ; (1,5,9,13- tetraselenacyclohexadecane)bis(dichlorogermanium(ii)) dichloromethane solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C12 H24 Cl4 Ge2 Se4, C H2 Cl2' _chemical_formula_sum 'C13 H26 Cl6 Ge2 Se4' _chemical_formula_weight 856.06 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' Ge Ge 0.1547 1.8001 '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 tetragonal _symmetry_space_group_name_H-M 'P -4 21 m' _space_group_IT_number 113 _space_group_name_Hall 'P -4 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' '-y+1/2, -x+1/2, z' 'y+1/2, x+1/2, z' _cell_length_a 15.6517(15) _cell_length_b 15.6517(15) _cell_length_c 5.2707(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1291.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1623 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.202 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 8.586 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7728 # shelxl 0.5848 _exptl_absorpt_correction_T_max 1.0000 # 0.7827 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. 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 '10cm confocal mirrors' _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_% ? _diffrn_reflns_number 10552 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0302 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.49 _reflns_number_total 1539 _reflns_number_gt 1459 _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 ? _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^)+(0.0000P)^2^+0.9680P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.061(13) _chemical_absolute_configuration ad _refine_ls_number_reflns 1539 _refine_ls_number_parameters 73 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0229 _refine_ls_R_factor_gt 0.0199 _refine_ls_wR_factor_ref 0.0414 _refine_ls_wR_factor_gt 0.0401 _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_restrained_S_all 1.122 _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 Ge1 Ge 0.231519(18) 0.268481(18) 0.31809(9) 0.01692(10) Uani 1 2 d S . . Cl1 Cl 0.31334(5) 0.18666(5) 0.5808(2) 0.0274(2) Uani 1 2 d S . . Cl2 Cl 0.16005(5) 0.33995(5) 0.6287(2) 0.0272(2) Uani 1 2 d S . . Se1 Se 0.350431(17) 0.407172(17) 0.30359(6) 0.01677(8) Uani 1 1 d . . . C1 C 0.40338(19) 0.36134(18) -0.0048(6) 0.0180(6) Uani 1 1 d . . . H1A H 0.3589 0.3375 -0.1183 0.022 Uiso 1 1 calc R . . H1B H 0.4337 0.4074 -0.0968 0.022 Uiso 1 1 calc R . . C2 C 0.46619(18) 0.29150(17) 0.0709(6) 0.0176(6) Uani 1 1 d . . . H2A H 0.5038 0.3134 0.2071 0.021 Uiso 1 1 calc R . . H2B H 0.4339 0.2424 0.1402 0.021 Uiso 1 1 calc R . . C3 C 0.52120(17) 0.26089(18) -0.1492(6) 0.0197(6) Uani 1 1 d . . . H3A H 0.4834 0.2367 -0.2816 0.024 Uiso 1 1 calc R . . H3B H 0.5588 0.2143 -0.0881 0.024 Uiso 1 1 calc R . . Cl3 Cl 0.44580(14) 0.05420(14) 0.3396(10) 0.0633(11) Uani 0.50 2 d SPD . . Cl4 Cl 0.45211(16) 0.04789(16) -0.0096(7) 0.0554(8) Uani 0.50 2 d SPD . . C4 C 0.4765(4) 0.0235(4) 0.305(2) 0.040(3) Uani 0.50 2 d SPD . . H4A H 0.4960 0.0762 0.3907 0.048 Uiso 0.25 1 calc PR . . H4B H 0.4238 0.0040 0.3907 0.048 Uiso 0.25 1 calc PR . . 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 Ge1 0.01753(13) 0.01753(13) 0.0157(2) 0.00019(15) -0.00019(15) -0.00293(16) Cl1 0.0238(3) 0.0238(3) 0.0347(6) 0.0088(4) -0.0088(4) -0.0053(4) Cl2 0.0272(3) 0.0272(3) 0.0271(6) -0.0065(3) 0.0065(3) -0.0013(4) Se1 0.02031(14) 0.01638(13) 0.01363(14) -0.00033(13) 0.00088(14) 0.00024(11) C1 0.0185(14) 0.0203(15) 0.0151(14) 0.0005(12) 0.0016(12) 0.0014(13) C2 0.0200(14) 0.0164(14) 0.0165(15) 0.0011(12) 0.0018(13) 0.0008(11) C3 0.0170(13) 0.0176(14) 0.0245(17) 0.0008(14) -0.0013(13) -0.0010(11) Cl3 0.0356(9) 0.0356(9) 0.119(3) -0.0043(16) 0.0043(16) 0.0068(12) Cl4 0.0533(12) 0.0533(12) 0.060(2) 0.0096(13) -0.0096(13) -0.0211(15) C4 0.026(3) 0.026(3) 0.068(7) 0.007(5) -0.007(5) 0.003(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 Ge1 Cl2 2.2765(11) . ? Ge1 Cl1 2.2799(12) . ? Ge1 Se1 2.8604(4) . ? Ge1 Se1 2.8604(4) 7 ? Se1 C1 1.961(3) . ? Se1 C3 1.971(3) 3_565 ? C1 C2 1.523(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.522(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 Se1 1.971(3) 4_655 ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? Cl3 C4 1.730(9) 2_655 ? Cl4 C4 1.742(11) . ? C4 Cl3 1.730(9) 2_655 ? C4 H4A 0.9900 . ? C4 H4B 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 Ge1 Cl1 96.62(5) . . ? Cl2 Ge1 Se1 88.053(10) . . ? Cl1 Ge1 Se1 94.418(10) . . ? Cl2 Ge1 Se1 88.053(10) . 7 ? Cl1 Ge1 Se1 94.418(10) . 7 ? Se1 Ge1 Se1 170.701(19) . 7 ? C1 Se1 C3 99.57(12) . 3_565 ? C1 Se1 Ge1 91.12(9) . . ? C3 Se1 Ge1 88.85(8) 3_565 . ? C2 C1 Se1 108.5(2) . . ? C2 C1 H1A 110.0 . . ? Se1 C1 H1A 110.0 . . ? C2 C1 H1B 110.0 . . ? Se1 C1 H1B 110.0 . . ? H1A C1 H1B 108.4 . . ? C3 C2 C1 113.0(3) . . ? C3 C2 H2A 109.0 . . ? C1 C2 H2A 109.0 . . ? C3 C2 H2B 109.0 . . ? C1 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? C2 C3 Se1 114.38(19) . 4_655 ? C2 C3 H3A 108.7 . . ? Se1 C3 H3A 108.7 4_655 . ? C2 C3 H3B 108.7 . . ? Se1 C3 H3B 108.7 4_655 . ? H3A C3 H3B 107.6 . . ? Cl3 C4 Cl4 114.2(8) 2_655 . ? Cl3 C4 H4A 108.7 2_655 . ? Cl4 C4 H4A 108.7 . . ? Cl3 C4 H4B 108.7 2_655 . ? Cl4 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.347 _refine_diff_density_min -0.326 _refine_diff_density_rms 0.080 #===END OF CIF ============================================================== # 10wz304c.cif CCDC-781126 data_10wz304c _database_code_depnum_ccdc_archive 'CCDC 781126' #TrackingRef '- GeX2_all8_3.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2010-03-24 _audit_author_name 'Webster, M.' _chemical_name_systematic ; dibromo(1,5,9,13-tetraselenacyclohexadecane-Se,Se')germanium(II) ; # C12H24Se4 = [16]aneSe4 = 1,5,9,13-tetraselenacyclohexadecane _chemical_name_common ;dibromo(1,5,9,13-tetraselenacyclohexadecane- Se,Se')germanium(ii) ; _chemical_melting_point ? _chemical_formula_moiety 'C12 H24 Br2 Ge Se4' _chemical_formula_sum 'C12 H24 Br2 Ge Se4' _chemical_formula_weight 716.56 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' Ge Ge 0.1547 1.8001 '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' 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 'P 2/c' _space_group_IT_number 13 _space_group_name_Hall '-P 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 13.375(4) _cell_length_b 5.0372(10) _cell_length_c 16.368(5) _cell_angle_alpha 90.00 _cell_angle_beta 113.220(10) _cell_angle_gamma 90.00 _cell_volume 1013.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7642 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.348 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 668 _exptl_absorpt_coefficient_mu 12.626 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6068 # shelxl 0.2532 _exptl_absorpt_correction_T_max 0.7456 # 0.3373 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. 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_% ? _diffrn_reflns_number 10053 _diffrn_reflns_av_R_equivalents 0.0576 _diffrn_reflns_av_sigmaI/netI 0.0630 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 27.56 _reflns_number_total 2336 _reflns_number_gt 1837 _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 ? _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^)+(0.0480P)^2^+3.6046P] 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 2336 _refine_ls_number_parameters 87 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.1015 _refine_ls_wR_factor_gt 0.0897 _refine_ls_goodness_of_fit_ref 0.921 _refine_ls_restrained_S_all 0.921 _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 Ge1 Ge 0.0000 -0.14901(15) 0.2500 0.0228(2) Uani 1 2 d S . . Br1 Br -0.06237(5) -0.45823(11) 0.12400(4) 0.02925(18) Uani 1 1 d . . . Se1 Se -0.20853(4) -0.19418(11) 0.25390(4) 0.02396(16) Uani 1 1 d . . . Se2 Se -0.60836(5) 0.14422(11) 0.09845(4) 0.02990(18) Uani 1 1 d . . . C1 C -0.2721(5) 0.0561(11) 0.1551(4) 0.0293(13) Uani 1 1 d . . . H1A H -0.2207 0.2050 0.1635 0.035 Uiso 1 1 calc R . . H1B H -0.2809 -0.0350 0.0991 0.035 Uiso 1 1 calc R . . C2 C -0.3816(5) 0.1686(12) 0.1456(4) 0.0320(13) Uani 1 1 d . . . H2A H -0.3726 0.2624 0.2013 0.038 Uiso 1 1 calc R . . H2B H -0.4050 0.3012 0.0970 0.038 Uiso 1 1 calc R . . C3 C -0.4704(5) -0.0365(11) 0.1263(4) 0.0286(12) Uani 1 1 d . . . H3A H -0.4544 -0.1528 0.1788 0.034 Uiso 1 1 calc R . . H3B H -0.4741 -0.1484 0.0755 0.034 Uiso 1 1 calc R . . C4 C -0.7008(5) -0.1694(11) 0.0811(4) 0.0268(12) Uani 1 1 d . . . H4A H -0.7013 -0.2716 0.0293 0.032 Uiso 1 1 calc R . . H4B H -0.6709 -0.2849 0.1342 0.032 Uiso 1 1 calc R . . C5 C -0.8170(5) -0.0893(12) 0.0657(4) 0.0293(13) Uani 1 1 d . . . H5A H -0.8632 -0.2502 0.0512 0.035 Uiso 1 1 calc R . . H5B H -0.8452 0.0306 0.0136 0.035 Uiso 1 1 calc R . . C6 C -0.8271(5) 0.0496(11) 0.1452(4) 0.0297(13) Uani 1 1 d . . . H6A H -0.9023 0.1159 0.1280 0.036 Uiso 1 1 calc R . . H6B H -0.7772 0.2039 0.1630 0.036 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 Ge1 0.0222(4) 0.0237(4) 0.0237(4) 0.000 0.0105(4) 0.000 Br1 0.0301(3) 0.0326(3) 0.0245(3) -0.0048(2) 0.0102(3) -0.0016(2) Se1 0.0230(3) 0.0268(3) 0.0234(3) -0.0008(2) 0.0106(2) -0.0002(2) Se2 0.0267(3) 0.0271(3) 0.0372(4) 0.0015(2) 0.0140(3) 0.0041(2) C1 0.029(3) 0.034(3) 0.027(3) 0.005(2) 0.014(3) 0.001(2) C2 0.028(3) 0.033(3) 0.033(3) 0.008(2) 0.011(3) 0.001(2) C3 0.027(3) 0.030(3) 0.029(3) 0.003(2) 0.012(3) 0.002(2) C4 0.032(3) 0.025(3) 0.026(3) -0.001(2) 0.014(3) 0.000(2) C5 0.028(3) 0.035(3) 0.023(3) -0.005(2) 0.009(2) -0.003(2) C6 0.035(3) 0.026(3) 0.034(3) 0.007(2) 0.019(3) 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 # Ge1 Br1 3.9623(11) 2_565 ? # Ge1 Br1 3.9623(11) 1_565 ? Ge1 Br1 2.4533(9) . ? Ge1 Br1 2.4533(9) 2 ? Ge1 Se1 2.8240(10) 2 ? Ge1 Se1 2.8240(10) . ? Se1 C6 1.960(6) 2_455 ? Se1 C1 1.960(6) . ? Se2 C3 1.944(6) . ? Se2 C4 1.957(5) . ? C1 C2 1.521(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.510(8) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.526(8) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.530(8) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 Se1 1.960(6) 2_455 ? C6 H6A 0.9900 . ? C6 H6B 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 Br1 Ge1 Br1 101.17(4) . 2 ? Br1 Ge1 Se1 86.64(2) . 2 ? Br1 Ge1 Se1 87.50(2) 2 2 ? Br1 Ge1 Se1 87.50(2) . . ? Br1 Ge1 Se1 86.64(2) 2 . ? Se1 Ge1 Se1 170.76(4) 2 . ? Br1 Ge1 Br1 157.99(2) . 2_565 ? Br1 Ge1 Br1 100.84(3) 2 2_565 ? Se1 Ge1 Br1 94.32(2) 2 2_565 ? Se1 Ge1 Br1 93.79(2) . 2_565 ? Br1 Ge1 Br1 100.84(3) . 1_565 ? Br1 Ge1 Br1 157.99(2) 2 1_565 ? Se1 Ge1 Br1 93.79(2) 2 1_565 ? Se1 Ge1 Br1 94.32(2) . 1_565 ? Br1 Ge1 Br1 57.16(3) 2_565 1_565 ? C6 Se1 C1 100.0(3) 2_455 . ? C6 Se1 Ge1 93.12(18) 2_455 . ? C1 Se1 Ge1 92.33(17) . . ? C3 Se2 C4 98.2(2) . . ? C2 C1 Se1 114.3(4) . . ? C2 C1 H1A 108.7 . . ? Se1 C1 H1A 108.7 . . ? C2 C1 H1B 108.7 . . ? Se1 C1 H1B 108.7 . . ? H1A C1 H1B 107.6 . . ? C3 C2 C1 114.3(5) . . ? C3 C2 H2A 108.7 . . ? C1 C2 H2A 108.7 . . ? C3 C2 H2B 108.7 . . ? C1 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? C2 C3 Se2 108.9(4) . . ? C2 C3 H3A 109.9 . . ? Se2 C3 H3A 109.9 . . ? C2 C3 H3B 109.9 . . ? Se2 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? C5 C4 Se2 110.8(4) . . ? C5 C4 H4A 109.5 . . ? Se2 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? Se2 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C4 C5 C6 113.9(5) . . ? C4 C5 H5A 108.8 . . ? C6 C5 H5A 108.8 . . ? C4 C5 H5B 108.8 . . ? C6 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? C5 C6 Se1 110.9(4) . 2_455 ? C5 C6 H6A 109.5 . . ? Se1 C6 H6A 109.5 2_455 . ? C5 C6 H6B 109.5 . . ? Se1 C6 H6B 109.5 2_455 . ? H6A C6 H6B 108.0 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.703 _refine_diff_density_min -0.957 _refine_diff_density_rms 0.180 #===END OF CIF ============================================================== # 10wz328b.cif CCDC-781127 data_10wz328b _database_code_depnum_ccdc_archive 'CCDC 781127' #TrackingRef '- GeX2_all8_3.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2010-05-11 _audit_author_name 'Webster, M.' _chemical_name_systematic ; (1,5,9,13-tetraselenacyclohexadecane)bis(di-iodogermanium(II)) tetraiodogermanium(IV) ; # C12H24Se4 = [16]aneSe4 = # 1,5,9,13-tetraselenacyclohexadecane (iLab default & selected) _chemical_name_common ; (1,5,9,13-tetraselenacyclohexadecane)bis(di- iodogermanium(ii)) tetraiodogermanium(IV) ; _chemical_melting_point ? _chemical_formula_moiety 'C12 H24 Ge2 I4 Se4, Ge I4' _chemical_formula_sum 'C12 H24 Ge3 I8 Se4' _chemical_formula_structural '(Ge I2)2 (C12 H24 Se4) (Ge I4)' _chemical_formula_weight 1717.12 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' Ge Ge 0.1547 1.8001 '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' 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 'C 2/c' _space_group_IT_number 15 _space_group_name_Hall '-C 2yc ' 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 16.599(4) _cell_length_b 17.659(3) _cell_length_c 12.181(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.159(10) _cell_angle_gamma 90.00 _cell_volume 3446.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3915 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Fragment _exptl_crystal_colour Violet _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.309 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3008 _exptl_absorpt_coefficient_mu 13.994 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6098 # shelxl 0.4873 _exptl_absorpt_correction_T_max 1.0000 # 0.6045 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. 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 '10cm confocal mirrors' _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_% ? _diffrn_reflns_number 18576 _diffrn_reflns_av_R_equivalents 0.0545 _diffrn_reflns_av_sigmaI/netI 0.0444 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.43 _diffrn_reflns_theta_max 27.53 _reflns_number_total 3940 _reflns_number_gt 3268 _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 'DIRDIF-99 (Beurskens, 1999)' _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^)+(0.0000P)^2^+349.9185P] 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 3940 _refine_ls_number_parameters 123 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0840 _refine_ls_R_factor_gt 0.0667 _refine_ls_wR_factor_ref 0.1420 _refine_ls_wR_factor_gt 0.1320 _refine_ls_goodness_of_fit_ref 1.110 _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 Ge1 Ge 0.23495(9) 0.05651(7) 0.14616(11) 0.0230(3) Uani 1 1 d . . . Ge2 Ge 0.0000 0.30357(14) 0.2500 0.0341(5) Uani 1 2 d S . . I1 I 0.13212(6) 0.15930(5) 0.02625(8) 0.0347(2) Uani 1 1 d . . . I2 I 0.28908(10) -0.01820(6) -0.01363(10) 0.0580(4) Uani 1 1 d . . . I3 I -0.10958(7) 0.22220(7) 0.12082(9) 0.0471(3) Uani 1 1 d . . . I4 I 0.07324(7) 0.38305(6) 0.13488(8) 0.0380(2) Uani 1 1 d . . . Se1 Se 0.36372(8) 0.16466(7) 0.16118(12) 0.0264(3) Uani 1 1 d . . . Se2 Se 0.40020(10) 0.45688(8) 0.39303(18) 0.0528(5) Uani 1 1 d D . . C1 C 0.5000 0.0663(11) 0.2500 0.042(6) Uani 1 2 d S . . H1A H 0.5309 0.0332 0.3125 0.050 Uiso 0.50 1 calc PR . . H1B H 0.4691 0.0332 0.1875 0.050 Uiso 0.50 1 calc PR . . C2 C 0.4369(8) 0.1140(8) 0.2931(13) 0.034(3) Uani 1 1 d . . . H2A H 0.4665 0.1519 0.3491 0.040 Uiso 1 1 calc R . . H2B H 0.4037 0.0810 0.3305 0.040 Uiso 1 1 calc R . . C3 C 0.3178(8) 0.2429(7) 0.2414(12) 0.027(3) Uani 1 1 d . A . H3A H 0.2692 0.2667 0.1875 0.032 Uiso 1 1 calc R . . H3B H 0.2976 0.2188 0.3026 0.032 Uiso 1 1 calc R . . C4 C 0.3813(8) 0.3050(7) 0.2938(10) 0.022(2) Uani 1 1 d . . . H4A H 0.4173 0.2878 0.3678 0.026 Uiso 1 1 calc R A . H4B H 0.4173 0.3164 0.2427 0.026 Uiso 1 1 calc R . . C5 C 0.3325(8) 0.3753(7) 0.3103(12) 0.026(3) Uani 1 1 d . A . H5A H 0.2908 0.3606 0.3515 0.031 Uiso 1 1 calc R . . H5B H 0.3017 0.3944 0.2346 0.031 Uiso 1 1 calc R . . C6A C 0.424(2) 0.497(2) 0.253(2) 0.060(11) Uiso 0.55(4) 1 d PD A 1 H6A1 H 0.4252 0.4525 0.2042 0.072 Uiso 0.55(4) 1 calc PR A 1 H6A2 H 0.3739 0.5268 0.2141 0.072 Uiso 0.55(4) 1 calc PR A 1 C7A C 0.5000 0.546(2) 0.2500 0.039(10) Uiso 0.55(4) 2 d SPD . 1 H7A1 H 0.5145 0.5789 0.3181 0.047 Uiso 0.27(2) 1 calc PR A 1 H7A2 H 0.4855 0.5789 0.1819 0.047 Uiso 0.27(2) 1 calc PR A 1 C6B C 0.457(2) 0.5167(13) 0.305(3) 0.033(9) Uiso 0.45(4) 1 d PD A 2 H6B1 H 0.4168 0.5469 0.2471 0.039 Uiso 0.45(4) 1 calc PR A 2 H6B2 H 0.4979 0.5511 0.3543 0.039 Uiso 0.45(4) 1 calc PR A 2 C7B C 0.5000 0.457(2) 0.2500 0.022(9) Uiso 0.45(4) 2 d SPD . 2 H7B1 H 0.5396 0.4248 0.3060 0.026 Uiso 0.23(2) 1 calc PR A 2 H7B2 H 0.4604 0.4248 0.1940 0.026 Uiso 0.23(2) 1 calc PR A 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 Ge1 0.0281(7) 0.0193(6) 0.0224(6) 0.0012(5) 0.0078(5) -0.0033(5) Ge2 0.0334(11) 0.0462(13) 0.0277(10) 0.000 0.0169(9) 0.000 I1 0.0461(6) 0.0208(4) 0.0292(5) 0.0008(3) -0.0043(4) -0.0014(4) I2 0.1198(12) 0.0239(5) 0.0493(6) -0.0059(4) 0.0560(7) -0.0052(6) I3 0.0374(6) 0.0725(8) 0.0328(5) -0.0062(5) 0.0115(4) -0.0085(5) I4 0.0440(6) 0.0423(5) 0.0359(5) -0.0018(4) 0.0249(4) -0.0001(4) Se1 0.0292(7) 0.0173(6) 0.0375(7) -0.0022(5) 0.0169(6) -0.0012(5) Se2 0.0290(8) 0.0172(7) 0.0933(14) -0.0115(8) -0.0175(8) 0.0039(6) C1 0.030(11) 0.014(9) 0.080(17) 0.000 0.011(11) 0.000 C2 0.025(7) 0.032(7) 0.051(9) 0.020(6) 0.024(6) 0.003(6) C3 0.021(6) 0.026(6) 0.041(8) -0.009(6) 0.021(6) -0.002(5) C4 0.022(6) 0.019(6) 0.021(6) 0.003(5) 0.000(5) 0.001(5) C5 0.018(6) 0.021(6) 0.039(7) 0.001(5) 0.010(5) -0.002(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ge1 I1 2.6530(16) . ? Ge1 I2 2.6928(17) . ? Ge1 Se2 2.792(2) 4_545 ? Ge1 Se1 2.8364(19) . ? Ge2 I4 2.5112(17) 2 ? Ge2 I4 2.5112(17) . ? Ge2 I3 2.5204(18) . ? Ge2 I3 2.5204(18) 2 ? Se1 C3 1.958(12) . ? Se1 C2 1.959(14) . ? Se2 C6B 1.915(14) . ? Se2 C5 1.939(13) . ? Se2 C6A 1.975(15) . ? Se2 Ge1 2.792(2) 4 ? C1 C2 1.540(17) 2_655 ? C1 C2 1.540(17) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.539(17) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.525(17) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6A C7A 1.54(3) . ? C6A H6A1 0.9900 . ? C6A H6A2 0.9900 . ? C7A C6A 1.54(3) 2_655 ? C7A H7A1 0.9900 . ? C7A H7A2 0.9900 . ? C6B C7B 1.53(3) . ? C6B H6B1 0.9900 . ? C6B H6B2 0.9900 . ? C7B C6B 1.53(3) 2_655 ? C7B H7B1 0.9900 . ? C7B H7B2 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 # C6B Se2 C6A 23.7(12) . . ? I1 Ge1 I2 103.03(6) . . ? I1 Ge1 Se2 87.96(6) . 4_545 ? I2 Ge1 Se2 88.44(7) . 4_545 ? I1 Ge1 Se1 86.58(5) . . ? I2 Ge1 Se1 89.33(6) . . ? Se2 Ge1 Se1 173.48(7) 4_545 . ? I4 Ge2 I4 112.04(10) 2 . ? I4 Ge2 I3 106.95(4) 2 . ? I4 Ge2 I3 110.23(4) . . ? I4 Ge2 I3 110.23(4) 2 2 ? I4 Ge2 I3 106.95(4) . 2 ? I3 Ge2 I3 110.48(11) . 2 ? C3 Se1 C2 98.7(6) . . ? C3 Se1 Ge1 97.0(4) . . ? C2 Se1 Ge1 92.3(4) . . ? C6B Se2 C5 114.9(10) . . ? C5 Se2 C6A 92.1(11) . . ? C6B Se2 Ge1 92.7(9) . 4 ? C5 Se2 Ge1 92.8(4) . 4 ? C6A Se2 Ge1 87.6(11) . 4 ? C2 C1 C2 113.7(15) 2_655 . ? C2 C1 H1A 108.8 2_655 . ? C2 C1 H1A 108.8 . . ? C2 C1 H1B 108.8 2_655 . ? C2 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? C1 C2 Se1 107.5(8) . . ? C1 C2 H2A 110.2 . . ? Se1 C2 H2A 110.2 . . ? C1 C2 H2B 110.2 . . ? Se1 C2 H2B 110.2 . . ? H2A C2 H2B 108.5 . . ? C4 C3 Se1 113.3(8) . . ? C4 C3 H3A 108.9 . . ? Se1 C3 H3A 108.9 . . ? C4 C3 H3B 108.9 . . ? Se1 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? C5 C4 C3 107.7(10) . . ? C5 C4 H4A 110.2 . . ? C3 C4 H4A 110.2 . . ? C5 C4 H4B 110.2 . . ? C3 C4 H4B 110.2 . . ? H4A C4 H4B 108.5 . . ? C4 C5 Se2 114.7(8) . . ? C4 C5 H5A 108.6 . . ? Se2 C5 H5A 108.6 . . ? C4 C5 H5B 108.6 . . ? Se2 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? C7A C6A Se2 124.8(18) . . ? C7A C6A H6A1 106.1 . . ? Se2 C6A H6A1 106.1 . . ? C7A C6A H6A2 106.1 . . ? Se2 C6A H6A2 106.1 . . ? H6A1 C6A H6A2 106.3 . . ? C6A C7A C6A 112(4) . 2_655 ? C6A C7A H7A1 109.2 . . ? C6A C7A H7A1 109.2 2_655 . ? C6A C7A H7A2 109.2 . . ? C6A C7A H7A2 109.2 2_655 . ? H7A1 C7A H7A2 107.9 . . ? C7B C6B Se2 102.7(12) . . ? C7B C6B H6B1 111.2 . . ? Se2 C6B H6B1 111.2 . . ? C7B C6B H6B2 111.2 . . ? Se2 C6B H6B2 111.2 . . ? H6B1 C6B H6B2 109.1 . . ? C6B C7B C6B 92(2) 2_655 . ? C6B C7B H7B1 113.2 2_655 . ? C6B C7B H7B1 113.2 . . ? C6B C7B H7B2 113.2 2_655 . ? C6B C7B H7B2 113.2 . . ? H7B1 C7B H7B2 110.6 . . ? 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 # Se2 Ge1 Se1 C3 94.2(8) 4_545 . . . ? # Se2 Ge1 Se1 C2 -166.7(8) 4_545 . . . ? I1 Ge1 Se1 C3 61.1(4) . . . . ? I2 Ge1 Se1 C3 164.2(4) . . . . ? I1 Ge1 Se1 C2 160.2(4) . . . . ? I2 Ge1 Se1 C2 -96.7(4) . . . . ? C2 C1 C2 Se1 68.5(5) 2_655 . . . ? C3 Se1 C2 C1 -162.5(9) . . . . ? Ge1 Se1 C2 C1 100.1(9) . . . . ? C2 Se1 C3 C4 71.6(10) . . . . ? Ge1 Se1 C3 C4 165.1(9) . . . . ? Se1 C3 C4 C5 157.8(9) . . . . ? C3 C4 C5 Se2 172.7(9) . . . . ? C6B Se2 C5 C4 79.1(14) . . . . ? C6A Se2 C5 C4 85.7(14) . . . . ? Ge1 Se2 C5 C4 173.4(9) 4 . . . ? C6B Se2 C6A C7A 9(2) . . . . ? C5 Se2 C6A C7A -156(3) . . . . ? Ge1 Se2 C6A C7A 111(3) 4 . . . ? Se2 C6A C7A C6A 87(3) . . . 2_655 ? C5 Se2 C6B C7B -51(2) . . . . ? C6A Se2 C6B C7B -67(3) . . . . ? Ge1 Se2 C6B C7B -145.1(16) 4 . . . ? Se2 C6B C7B C6B -176(3) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 3.192 _refine_diff_density_min -5.464 _refine_diff_density_rms 0.347 #===END OF CIF ============================================================== # # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # #===END OF FILE =============================================================