#------------------------------------------------------------------------------ #$Date: 2016-03-26 14:43:29 +0200 (Sat, 26 Mar 2016) $ #$Revision: 180274 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/11/60/7116054.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7116054 loop_ _publ_author_name 'P. Steiniger' 'G. Bendt' 'D. Blaser' 'C. Wolper' 'S. Schulz' _publ_section_title ; Germane vs. digermane formation ; _journal_name_full Chem.Commun. _journal_page_first 15461 _journal_paper_doi 10.1039/C4cc07921C _journal_volume 50 _journal_year 2014 _chemical_formula_moiety 'C12 H30 Ge N2 Se2 Si' _chemical_formula_sum 'C12 H30 Ge N2 Se2 Si' _chemical_formula_weight 460.98 _chemical_name_systematic ; ? ; _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2013 _cell_angle_alpha 90 _cell_angle_beta 97.731(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.3441(8) _cell_length_b 9.0775(5) _cell_length_c 13.8753(7) _cell_measurement_reflns_used 15465 _cell_measurement_temperature 100(1) _cell_measurement_theta_max 30.63 _cell_measurement_theta_min 2.61 _cell_volume 1915.07(17) _computing_cell_refinement 'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009' _computing_data_collection 'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009' _computing_data_reduction 'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009' _computing_molecular_graphics 'BRUKER AXS Inc. 2008 Vers. 2008/4' _computing_publication_material 'BRUKER AXS Inc. 2013 Vers. 2013/4' _computing_structure_refinement 'BRUKER AXS Inc. 2013 Vers. 2013/4' _computing_structure_solution 'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009' _diffrn_ambient_temperature 100(1) _diffrn_detector_area_resol_mean 512 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.979 _diffrn_measurement_device_type ; Bruker D8 KAPPA series II with APEX II area detector system ; _diffrn_measurement_method ; Data collection strategy APEX 2/COSMO ; _diffrn_radiation_monochromator 'Triumph Goebel mirror' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_unetI/netI 0.0149 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.979 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 31347 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.979 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.884 _diffrn_reflns_theta_min 2.613 _exptl_absorpt_coefficient_mu 5.453 _exptl_absorpt_correction_T_max 0.75 _exptl_absorpt_correction_T_min 0.58 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; BRUKER AXS SMART APEX 2 Vers. 3.0-2009 R.H. Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.599 _exptl_crystal_description block _exptl_crystal_F_000 920 _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.080 _refine_diff_density_max 0.374 _refine_diff_density_min -0.290 _refine_diff_density_rms 0.061 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 88 _refine_ls_number_reflns 2949 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.064 _refine_ls_R_factor_all 0.0205 _refine_ls_R_factor_gt 0.0159 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0176P)^2^+1.2813P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.0385 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2653 _reflns_number_total 2949 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c4cc07921c2.cif _cod_data_source_block pst_022m _cod_database_code 7116054 #BEGIN Tags that were not found in dictionaries: _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.495 _shelx_estimated_absorpt_t_max 0.670 _shelxl_version_number 2013-4 _shelx_res_file ; TITL pst_022m in C2/c CELL 0.71073 15.3441 9.0775 13.8753 90.000 97.731 90.000 ZERR 4.00 0.0008 0.0005 0.0007 0.000 0.002 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H N SI GE SE UNIT 48 120 8 4 4 8 TEMP -173 OMIT 0 4 1 OMIT -3 3 2 OMIT -8 0 2 OMIT 8 4 3 OMIT 8 2 2 OMIT 2 2 5 OMIT -2 4 1 SIZE .08 .12 .15 L.S. 14 ACTA FMAP 2 PLAN 10 WGHT 0.017600 1.281300 FVAR 0.05752 SE1 6 0.432910 0.025695 0.130667 11.00000 0.02106 0.01215 = 0.02401 -0.00515 0.00437 -0.00352 GE1 5 0.500000 0.187265 0.250000 10.50000 0.01323 0.00802 = 0.01664 0.00000 0.00381 0.00000 SI1 4 0.500000 0.476548 0.250000 10.50000 0.01654 0.00871 = 0.01568 0.00000 0.00234 0.00000 N1 3 0.563808 0.339630 0.206021 11.00000 0.01411 0.00918 = 0.01840 0.00023 0.00478 -0.00100 C1 1 0.651861 0.341420 0.175241 11.00000 0.01495 0.01596 = 0.01865 0.00146 0.00528 -0.00159 C2 1 0.660867 0.483134 0.117782 11.00000 0.02454 0.02063 = 0.02540 0.00446 0.00831 -0.00409 AFIX 137 H2A 2 0.613958 0.487407 0.062447 11.00000 -1.50000 H2B 2 0.718173 0.484371 0.093988 11.00000 -1.50000 H2C 2 0.656242 0.568429 0.160093 11.00000 -1.50000 AFIX 0 C3 1 0.662296 0.208116 0.110381 11.00000 0.02188 0.02114 = 0.03109 -0.00438 0.01212 0.00047 AFIX 137 H3A 2 0.655798 0.117408 0.147046 11.00000 -1.50000 H3B 2 0.720682 0.210246 0.089183 11.00000 -1.50000 H3C 2 0.617094 0.211269 0.053350 11.00000 -1.50000 AFIX 0 C4 1 0.723466 0.336896 0.263920 11.00000 0.01565 0.03013 = 0.02670 0.00309 0.00171 -0.00052 AFIX 137 H4A 2 0.715726 0.420345 0.306769 11.00000 -1.50000 H4B 2 0.781522 0.342930 0.242131 11.00000 -1.50000 H4C 2 0.718838 0.244528 0.299440 11.00000 -1.50000 AFIX 0 C5 1 0.439987 0.598259 0.155556 11.00000 0.03119 0.01836 = 0.02499 0.00746 0.00516 0.00602 AFIX 137 H5A 2 0.407455 0.537737 0.104350 11.00000 -1.50000 H5B 2 0.482166 0.660583 0.127339 11.00000 -1.50000 H5C 2 0.398727 0.660570 0.185231 11.00000 -1.50000 AFIX 0 C6 1 0.398676 0.174627 0.030311 11.00000 0.03194 0.02653 = 0.02012 -0.00114 0.00125 0.00060 AFIX 137 H6A 2 0.343334 0.220867 0.041971 11.00000 -1.50000 H6B 2 0.390841 0.127622 -0.033855 11.00000 -1.50000 H6C 2 0.444745 0.249818 0.032668 11.00000 -1.50000 AFIX 0 HKLF 4 REM pst_022m in C2/c REM R1 = 0.0159 for 2653 Fo > 4sig(Fo) and 0.0205 for all 2949 data REM 88 parameters refined using 0 restraints END WGHT 0.0176 1.2812 REM Highest difference peak 0.374, deepest hole -0.290, 1-sigma level 0.061 Q1 1 0.6526 0.4152 0.1424 11.00000 0.05 0.37 Q2 1 0.4758 0.0196 0.1072 11.00000 0.05 0.37 Q3 1 0.3948 0.0212 0.1695 11.00000 0.05 0.37 Q4 1 0.5474 0.4040 0.2305 11.00000 0.05 0.36 Q5 1 0.5376 0.2009 0.2103 11.00000 0.05 0.36 Q6 1 0.4771 0.5448 0.1966 11.00000 0.05 0.33 Q7 1 0.6846 0.3406 0.2165 11.00000 0.05 0.31 Q8 1 0.4578 -0.0196 0.1614 11.00000 0.05 0.31 Q9 1 0.6040 0.3428 0.1794 11.00000 0.05 0.30 Q10 1 0.6583 0.2747 0.1488 11.00000 0.05 0.30 ; _shelx_res_checksum 91672 #END Tags that were not found in dictionaries loop_ _space_group_symop_operation_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' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy Se1 Se 0.43291(2) 0.02569(2) 0.13067(2) 0.01895(4) Uani 1 1 d . . . Ge1 Ge 0.5000 0.18727(2) 0.2500 0.01247(4) Uani 1 2 d S T P Si1 Si 0.5000 0.47655(5) 0.2500 0.01363(9) Uani 1 2 d S T P N1 N 0.56381(6) 0.33963(10) 0.20602(7) 0.01366(18) Uani 1 1 d . . . C1 C 0.65186(8) 0.34142(13) 0.17524(9) 0.0162(2) Uani 1 1 d . . . C2 C 0.66087(9) 0.48313(14) 0.11778(10) 0.0231(3) Uani 1 1 d . . . H2A H 0.6140 0.4874 0.0624 0.035 Uiso 1 1 calc R U . H2B H 0.7182 0.4844 0.0940 0.035 Uiso 1 1 calc R U . H2C H 0.6562 0.5684 0.1601 0.035 Uiso 1 1 calc R U . C3 C 0.66230(9) 0.20812(15) 0.11038(11) 0.0239(3) Uani 1 1 d . . . H3A H 0.6558 0.1174 0.1470 0.036 Uiso 1 1 calc R U . H3B H 0.7207 0.2102 0.0892 0.036 Uiso 1 1 calc R U . H3C H 0.6171 0.2113 0.0533 0.036 Uiso 1 1 calc R U . C4 C 0.72347(9) 0.33690(16) 0.26392(10) 0.0243(3) Uani 1 1 d . . . H4A H 0.7157 0.4203 0.3068 0.036 Uiso 1 1 calc R U . H4B H 0.7815 0.3429 0.2421 0.036 Uiso 1 1 calc R U . H4C H 0.7188 0.2445 0.2994 0.036 Uiso 1 1 calc R U . C5 C 0.43999(9) 0.59826(15) 0.15556(10) 0.0247(3) Uani 1 1 d . . . H5A H 0.4075 0.5377 0.1043 0.037 Uiso 1 1 calc R U . H5B H 0.4822 0.6606 0.1273 0.037 Uiso 1 1 calc R U . H5C H 0.3987 0.6606 0.1852 0.037 Uiso 1 1 calc R U . C6 C 0.39868(10) 0.17463(15) 0.03031(10) 0.0264(3) Uani 1 1 d . . . H6A H 0.3433 0.2209 0.0420 0.040 Uiso 1 1 calc R U . H6B H 0.3908 0.1276 -0.0339 0.040 Uiso 1 1 calc R U . H6C H 0.4447 0.2498 0.0327 0.040 Uiso 1 1 calc R U . 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 Se1 0.02106(7) 0.01215(6) 0.02401(7) -0.00515(4) 0.00437(5) -0.00352(4) Ge1 0.01323(8) 0.00802(7) 0.01664(9) 0.000 0.00381(6) 0.000 Si1 0.0165(2) 0.00871(19) 0.0157(2) 0.000 0.00234(16) 0.000 N1 0.0141(4) 0.0092(4) 0.0184(5) 0.0002(3) 0.0048(4) -0.0010(3) C1 0.0150(5) 0.0160(5) 0.0187(6) 0.0015(4) 0.0053(4) -0.0016(4) C2 0.0245(6) 0.0206(6) 0.0254(7) 0.0045(5) 0.0083(5) -0.0041(5) C3 0.0219(6) 0.0211(6) 0.0311(7) -0.0044(5) 0.0121(5) 0.0005(5) C4 0.0156(6) 0.0301(7) 0.0267(7) 0.0031(5) 0.0017(5) -0.0005(5) C5 0.0312(7) 0.0184(6) 0.0250(7) 0.0075(5) 0.0052(5) 0.0060(5) C6 0.0319(7) 0.0265(7) 0.0201(6) -0.0011(5) 0.0012(5) 0.0006(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' 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 C6 Se1 Ge1 96.92(4) . . N1 Ge1 N1 82.89(6) 2_655 . N1 Ge1 Se1 115.95(3) 2_655 2_655 N1 Ge1 Se1 120.03(3) . 2_655 N1 Ge1 Se1 120.03(3) 2_655 . N1 Ge1 Se1 115.95(3) . . Se1 Ge1 Se1 102.528(10) 2_655 . N1 Ge1 Si1 41.44(3) 2_655 . N1 Ge1 Si1 41.45(3) . . Se1 Ge1 Si1 128.736(5) 2_655 . Se1 Ge1 Si1 128.736(5) . . N1 Si1 N1 89.00(6) 2_655 . N1 Si1 C5 114.96(6) 2_655 . N1 Si1 C5 115.16(6) . . N1 Si1 C5 115.16(6) 2_655 2_655 N1 Si1 C5 114.96(6) . 2_655 C5 Si1 C5 107.14(9) . 2_655 N1 Si1 Ge1 44.50(3) 2_655 . N1 Si1 Ge1 44.50(3) . . C5 Si1 Ge1 126.43(5) . . C5 Si1 Ge1 126.43(5) 2_655 . C1 N1 Si1 132.47(8) . . C1 N1 Ge1 130.79(7) . . Si1 N1 Ge1 94.05(5) . . N1 C1 C3 109.58(10) . . N1 C1 C2 108.16(10) . . C3 C1 C2 109.56(10) . . N1 C1 C4 110.68(10) . . C3 C1 C4 109.27(11) . . C2 C1 C4 109.57(10) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Se1 C6 1.9611(14) . Se1 Ge1 2.34390(18) . Ge1 N1 1.8451(9) 2_655 Ge1 N1 1.8452(9) . Ge1 Se1 2.34389(18) 2_655 Ge1 Si1 2.6260(5) . Si1 N1 1.7425(10) 2_655 Si1 N1 1.7425(10) . Si1 C5 1.8604(13) . Si1 C5 1.8604(13) 2_655 N1 C1 1.4708(15) . C1 C3 1.5292(17) . C1 C2 1.5295(17) . C1 C4 1.5359(18) .