# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'G. Reid' _publ_contact_author_email GR@SOTON.AC.UK _publ_section_title ; ; loop_ _publ_author_name 'Fei Cheng.' J.M.Dyke 'Francesco Ferrante' A.L.Hector 'W. Levason' 'G. Reid' M.Webster 'Wenjian Zhang.' # Attachment 'GeAll7_a.cif' data_07wz011 _database_code_depnum_ccdc_archive 'CCDC 724631' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2007-08-03 _audit_author_name 'Webster, M.' _chemical_name_systematic ; Dichloro(1,2-bis(dimethylamino)ethane)germanium(II) ; # Dichlorido(N,N,N',N'-tetramethylethylenediamine)germanium(II) # tmeda ligand named: # N,N,N',N'-tetramethyl-1,2-diamino-ethane # N,N,N',N'-tetramethylethane-1,2-diamine (from iLab naming) _chemical_name_common Dichloro(1,2-bis(dimethylamino)ethane)germanium(ii) _chemical_melting_point ? _chemical_formula_moiety 'C6 H16 Cl2 Ge N2' _chemical_formula_sum 'C6 H16 Cl2 Ge N2' _chemical_formula_weight 259.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 # Superceded ** _symmetry_space_group_name_Hall '-P 2yn' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.772(2) _cell_length_b 15.488(4) _cell_length_c 9.134(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.301(16) _cell_angle_gamma 90.00 _cell_volume 1090.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 33842 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.582 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 528 _exptl_absorpt_coefficient_mu 3.247 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6257 # _exptl_absorpt_correction_T_max 1.0000 # _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_% 0 _diffrn_reflns_number 12858 _diffrn_reflns_av_R_equivalents 0.0679 _diffrn_reflns_av_sigmaI/netI 0.0537 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.91 _diffrn_reflns_theta_max 27.66 _reflns_number_total 2490 _reflns_number_gt 1822 _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^+6.6004P] 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 2490 _refine_ls_number_parameters 104 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1007 _refine_ls_R_factor_gt 0.0635 _refine_ls_wR_factor_ref 0.1337 _refine_ls_wR_factor_gt 0.1158 _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_restrained_S_all 1.131 _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 0.24996(8) 0.93186(4) 0.98314(7) 0.0353(2) Uani 1 1 d . . . Cl1 Cl 0.2234(3) 0.88803(17) 1.24572(19) 0.0741(6) Uani 1 1 d . . . Cl2 Cl 0.51307(19) 0.86787(12) 1.00041(19) 0.0508(4) Uani 1 1 d . . . N1 N 0.1072(7) 0.8175(3) 0.9072(6) 0.0420(12) Uani 1 1 d . . . N2 N 0.2638(7) 0.9386(4) 0.7161(5) 0.0410(12) Uani 1 1 d . . . C1 C 0.1718(10) 0.7360(5) 0.9797(12) 0.080(3) Uani 1 1 d . . . H1A H 0.1689 0.7406 1.0863 0.120 Uiso 1 1 calc R . . H1B H 0.2913 0.7257 0.9603 0.120 Uiso 1 1 calc R . . H1C H 0.0980 0.6880 0.9403 0.120 Uiso 1 1 calc R . . C2 C -0.0709(9) 0.8308(5) 0.9401(10) 0.064(2) Uani 1 1 d . . . H2A H -0.1452 0.7841 0.8958 0.096 Uiso 1 1 calc R . . H2B H -0.1144 0.8863 0.8992 0.096 Uiso 1 1 calc R . . H2C H -0.0721 0.8309 1.0472 0.096 Uiso 1 1 calc R . . C3 C 0.1163(17) 0.8050(7) 0.7487(9) 0.102(4) Uani 1 1 d . . . H3A H 0.2144 0.7655 0.7394 0.123 Uiso 1 1 calc R . . H3B H 0.0092 0.7746 0.7069 0.123 Uiso 1 1 calc R . . C4 C 0.1349(14) 0.8743(6) 0.6622(8) 0.084(3) Uani 1 1 d . . . H4A H 0.0210 0.9037 0.6433 0.100 Uiso 1 1 calc R . . H4B H 0.1634 0.8530 0.5660 0.100 Uiso 1 1 calc R . . C5 C 0.2032(13) 1.0246(5) 0.6710(9) 0.077(3) Uani 1 1 d . . . H5A H 0.1982 1.0301 0.5636 0.116 Uiso 1 1 calc R . . H5B H 0.2834 1.0678 0.7193 0.116 Uiso 1 1 calc R . . H5C H 0.0873 1.0338 0.6996 0.116 Uiso 1 1 calc R . . C6 C 0.4293(11) 0.9226(8) 0.6616(8) 0.084(3) Uani 1 1 d . . . H6A H 0.4739 0.8660 0.6962 0.126 Uiso 1 1 calc R . . H6B H 0.5124 0.9675 0.6985 0.126 Uiso 1 1 calc R . . H6C H 0.4128 0.9235 0.5534 0.126 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 0.0307(3) 0.0380(3) 0.0365(3) -0.0054(3) 0.0021(2) -0.0018(3) Cl1 0.0747(13) 0.1155(18) 0.0338(9) 0.0011(10) 0.0139(8) -0.0173(12) Cl2 0.0297(7) 0.0674(11) 0.0542(10) 0.0179(8) 0.0008(6) 0.0026(7) N1 0.039(3) 0.043(3) 0.044(3) -0.007(2) 0.008(2) -0.006(2) N2 0.042(3) 0.047(3) 0.033(3) 0.000(2) 0.003(2) -0.005(2) C1 0.050(4) 0.032(4) 0.159(9) 0.013(5) 0.017(5) 0.000(3) C2 0.036(4) 0.059(5) 0.096(6) -0.020(4) 0.006(4) -0.004(3) C3 0.165(11) 0.099(7) 0.048(5) -0.027(5) 0.028(6) -0.081(8) C4 0.121(8) 0.091(7) 0.032(4) -0.003(4) -0.012(4) -0.044(6) C5 0.120(8) 0.062(5) 0.046(4) 0.013(4) -0.010(4) 0.026(5) C6 0.062(5) 0.151(10) 0.044(4) 0.010(5) 0.025(4) 0.018(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ge1 N1 2.157(5) . ? Ge1 Cl2 2.2599(18) . ? Ge1 N2 2.458(5) . ? Ge1 Cl1 2.526(2) . ? N1 C2 1.468(8) . ? N1 C3 1.471(9) . ? N1 C1 1.483(9) . ? N2 C4 1.453(9) . ? N2 C5 1.454(9) . ? N2 C6 1.458(9) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.352(12) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ge1 Cl2 94.95(15) . . ? N1 Ge1 N2 78.54(19) . . ? Cl2 Ge1 N2 86.25(13) . . ? N1 Ge1 Cl1 89.09(15) . . ? Cl2 Ge1 Cl1 89.90(7) . . ? N2 Ge1 Cl1 166.65(14) . . ? C2 N1 C3 112.6(7) . . ? C2 N1 C1 107.6(6) . . ? C3 N1 C1 105.7(7) . . ? C2 N1 Ge1 106.2(4) . . ? C3 N1 Ge1 109.7(4) . . ? C1 N1 Ge1 115.1(5) . . ? C4 N2 C5 110.3(7) . . ? C4 N2 C6 111.6(7) . . ? C5 N2 C6 109.1(7) . . ? C4 N2 Ge1 101.1(4) . . ? C5 N2 Ge1 105.5(4) . . ? C6 N2 Ge1 118.9(4) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 N1 119.5(8) . . ? C4 C3 H3A 107.4 . . ? N1 C3 H3A 107.4 . . ? C4 C3 H3B 107.4 . . ? N1 C3 H3B 107.4 . . ? H3A C3 H3B 107.0 . . ? C3 C4 N2 117.8(7) . . ? C3 C4 H4A 107.9 . . ? N2 C4 H4A 107.9 . . ? C3 C4 H4B 107.9 . . ? N2 C4 H4B 107.9 . . ? H4A C4 H4B 107.2 . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl2 Ge1 N1 C2 158.8(5) . . . . ? N2 Ge1 N1 C2 -116.1(5) . . . . ? Cl1 Ge1 N1 C2 68.9(5) . . . . ? Cl2 Ge1 N1 C3 -79.3(7) . . . . ? N2 Ge1 N1 C3 5.9(7) . . . . ? Cl1 Ge1 N1 C3 -169.1(7) . . . . ? Cl2 Ge1 N1 C1 39.8(5) . . . . ? N2 Ge1 N1 C1 125.0(5) . . . . ? Cl1 Ge1 N1 C1 -50.0(5) . . . . ? N1 Ge1 N2 C4 12.9(5) . . . . ? Cl2 Ge1 N2 C4 108.7(5) . . . . ? Cl1 Ge1 N2 C4 35.2(9) . . . . ? N1 Ge1 N2 C5 127.8(5) . . . . ? Cl2 Ge1 N2 C5 -136.4(5) . . . . ? Cl1 Ge1 N2 C5 150.1(6) . . . . ? N1 Ge1 N2 C6 -109.5(6) . . . . ? Cl2 Ge1 N2 C6 -13.7(6) . . . . ? Cl1 Ge1 N2 C6 -87.2(8) . . . . ? C2 N1 C3 C4 89.5(12) . . . . ? C1 N1 C3 C4 -153.3(11) . . . . ? Ge1 N1 C3 C4 -28.6(13) . . . . ? N1 C3 C4 N2 45.8(16) . . . . ? C5 N2 C4 C3 -144.6(10) . . . . ? C6 N2 C4 C3 94.0(11) . . . . ? Ge1 N2 C4 C3 -33.4(11) . . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.66 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.782 _refine_diff_density_min -0.765 _refine_diff_density_rms 0.130 #===END OF CIF ============================================================== # 2 07wz021b.cif data_07wz021 _database_code_depnum_ccdc_archive 'CCDC 724632' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2007-11-01 _audit_author_name 'Webster, M.' _chemical_name_systematic ; (2,2'-bipyridyl)dichloridogermanium(II) ; _chemical_name_common (2,2'-bipyridyl)dichloridogermanium(ii) _chemical_melting_point ? _chemical_formula_moiety 'C10 H8 Cl2 Ge N2' _chemical_formula_sum 'C10 H8 Cl2 Ge N2' _chemical_formula_weight 299.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_Int_Tables_number 14 # Superceded ** _symmetry_space_group_name_Hall '-P 2ybc' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.8277(5) _cell_length_b 17.957(3) _cell_length_c 9.0560(10) _cell_angle_alpha 90.00 _cell_angle_beta 94.057(10) _cell_angle_gamma 90.00 _cell_volume 1107.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 18284 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.797 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 3.213 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6114 # 0.4457 _exptl_absorpt_correction_T_max 0.7456 # 0.5519 _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_% 0 _diffrn_reflns_number 19949 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0217 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.20 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2530 _reflns_number_gt 2274 _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^)+(0.0339P)^2^+0.4572P] 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 2530 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0308 _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_ref 0.0662 _refine_ls_wR_factor_gt 0.0632 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 0.75830(3) 0.467394(12) 0.41559(2) 0.03395(9) Uani 1 1 d . . . Cl1 Cl 0.55179(7) 0.54565(3) 0.24596(6) 0.04083(13) Uani 1 1 d . . . Cl2 Cl 0.96187(8) 0.35872(3) 0.56895(6) 0.04367(14) Uani 1 1 d . . . N1 N 0.5912(2) 0.37817(9) 0.33356(17) 0.0293(3) Uani 1 1 d . . . N2 N 0.9117(2) 0.43217(9) 0.23960(17) 0.0298(3) Uani 1 1 d . . . C1 C 0.4248(3) 0.35644(11) 0.3904(2) 0.0319(4) Uani 1 1 d . . . H1 H 0.3740 0.3849 0.4674 0.038 Uiso 1 1 calc R . . C2 C 0.3254(3) 0.29347(11) 0.3395(2) 0.0365(4) Uani 1 1 d . . . H2 H 0.2048 0.2798 0.3781 0.044 Uiso 1 1 calc R . . C3 C 0.4042(3) 0.25069(12) 0.2315(3) 0.0438(5) Uani 1 1 d . . . H3 H 0.3408 0.2061 0.1977 0.053 Uiso 1 1 calc R . . C4 C 0.5759(3) 0.27332(12) 0.1732(3) 0.0431(5) Uani 1 1 d . . . H4 H 0.6324 0.2443 0.0994 0.052 Uiso 1 1 calc R . . C5 C 0.6651(3) 0.33893(11) 0.2236(2) 0.0314(4) Uani 1 1 d . . . C6 C 0.8425(3) 0.37143(11) 0.1656(2) 0.0318(4) Uani 1 1 d . . . C7 C 0.9312(3) 0.34514(12) 0.0432(3) 0.0428(5) Uani 1 1 d . . . H7 H 0.8799 0.3030 -0.0098 0.051 Uiso 1 1 calc R . . C8 C 1.0965(3) 0.38161(13) -0.0008(2) 0.0426(5) Uani 1 1 d . . . H8 H 1.1586 0.3649 -0.0854 0.051 Uiso 1 1 calc R . . C9 C 1.1701(3) 0.44169(12) 0.0782(2) 0.0370(4) Uani 1 1 d . . . H9 H 1.2857 0.4660 0.0508 0.044 Uiso 1 1 calc R . . C10 C 1.0737(3) 0.46655(11) 0.1983(2) 0.0334(4) Uani 1 1 d . . . H10 H 1.1231 0.5087 0.2525 0.040 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 0.03667(14) 0.03473(14) 0.03084(13) -0.01030(8) 0.00505(9) -0.00433(8) Cl1 0.0380(3) 0.0365(3) 0.0475(3) -0.0002(2) -0.0004(2) -0.0014(2) Cl2 0.0415(3) 0.0460(3) 0.0437(3) 0.0029(2) 0.0049(2) 0.0066(2) N1 0.0320(8) 0.0272(8) 0.0291(8) -0.0029(6) 0.0042(6) 0.0007(6) N2 0.0309(8) 0.0318(9) 0.0266(8) -0.0027(6) 0.0012(6) -0.0005(6) C1 0.0345(10) 0.0297(10) 0.0323(10) -0.0008(7) 0.0080(7) 0.0028(7) C2 0.0353(10) 0.0348(10) 0.0403(11) 0.0020(8) 0.0085(8) -0.0044(8) C3 0.0494(13) 0.0349(11) 0.0480(13) -0.0099(9) 0.0088(10) -0.0122(9) C4 0.0470(12) 0.0366(11) 0.0471(12) -0.0164(9) 0.0131(10) -0.0077(9) C5 0.0319(9) 0.0308(10) 0.0319(9) -0.0061(7) 0.0048(7) -0.0004(7) C6 0.0339(10) 0.0292(10) 0.0327(10) -0.0049(7) 0.0048(7) -0.0002(7) C7 0.0476(12) 0.0381(12) 0.0445(12) -0.0132(9) 0.0150(9) -0.0060(9) C8 0.0459(12) 0.0427(12) 0.0409(12) -0.0040(9) 0.0161(9) 0.0022(9) C9 0.0323(10) 0.0430(11) 0.0363(11) 0.0051(9) 0.0062(8) -0.0011(9) C10 0.0329(10) 0.0363(11) 0.0304(10) 0.0008(8) -0.0011(8) -0.0042(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ge1 N2 2.0673(15) . ? Ge1 N1 2.0738(16) . ? Ge1 Cl1 2.4528(6) . ? Ge1 Cl2 2.7195(7) . ? N1 C1 1.338(2) . ? N1 C5 1.347(2) . ? N2 C10 1.343(2) . ? N2 C6 1.348(2) . ? C1 C2 1.381(3) . ? C1 H1 0.9500 . ? C2 C3 1.382(3) . ? C2 H2 0.9500 . ? C3 C4 1.380(3) . ? C3 H3 0.9500 . ? C4 C5 1.388(3) . ? C4 H4 0.9500 . ? C5 C6 1.474(3) . ? C6 C7 1.383(3) . ? C7 C8 1.387(3) . ? C7 H7 0.9500 . ? C8 C9 1.370(3) . ? C8 H8 0.9500 . ? C9 C10 1.385(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ge1 N1 77.50(6) . . ? N2 Ge1 Cl1 89.58(5) . . ? N1 Ge1 Cl1 86.62(5) . . ? N2 Ge1 Cl2 84.58(5) . . ? N1 Ge1 Cl2 82.93(5) . . ? Cl1 Ge1 Cl2 168.917(19) . . ? C1 N1 C5 120.30(16) . . ? C1 N1 Ge1 123.24(13) . . ? C5 N1 Ge1 116.34(12) . . ? C10 N2 C6 120.02(16) . . ? C10 N2 Ge1 123.12(13) . . ? C6 N2 Ge1 116.86(12) . . ? N1 C1 C2 121.38(17) . . ? N1 C1 H1 119.3 . . ? C2 C1 H1 119.3 . . ? C1 C2 C3 118.99(19) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C4 C3 C2 119.38(19) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 119.25(19) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? N1 C5 C4 120.56(18) . . ? N1 C5 C6 114.62(16) . . ? C4 C5 C6 124.82(17) . . ? N2 C6 C7 121.10(18) . . ? N2 C6 C5 114.27(16) . . ? C7 C6 C5 124.60(18) . . ? C6 C7 C8 118.7(2) . . ? C6 C7 H7 120.7 . . ? C8 C7 H7 120.7 . . ? C9 C8 C7 119.85(19) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 119.15(19) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? N2 C10 C9 121.14(18) . . ? N2 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.281 _refine_diff_density_min -0.475 _refine_diff_density_rms 0.064 #===END OF CIF ============================================================== # 3 08wz005c.cif data_08wz005 _database_code_depnum_ccdc_archive 'CCDC 724633' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2008-09-09 _audit_author_name 'Webster, M.' _chemical_name_systematic ; Bromido(2,2'-bipyridyl-N,N')germanium(II) tribromidogermanate ; _chemical_name_common "Bromido(2,2'-bipyridyl-N,N')germanium(ii) tribromidogermanate" _chemical_melting_point ? _chemical_formula_moiety 'C10 H8 Br Ge N2 1+, Br3 Ge 1-' _chemical_formula_sum 'C10 H8 Br4 Ge2 N2' _chemical_formula_weight 621.00 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' Ge Ge 0.1547 1.8001 '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 21/n' _space_group_IT_number 14 # New _space_group_name_Hall '-P 2yn' # New loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.620(2) _cell_length_b 11.783(3) _cell_length_c 14.296(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.299(10) _cell_angle_gamma 90.00 _cell_volume 1570.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 11646 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.627 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 13.988 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5268 # 0.3928 _exptl_absorpt_correction_T_max 1.0000 # 0.7456 _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 13128 _diffrn_reflns_av_R_equivalents 0.0488 _diffrn_reflns_av_sigmaI/netI 0.0532 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.39 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3598 _reflns_number_gt 2871 _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^)+(0.0311P)^2^+2.4767P] 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 3598 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0544 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0823 _refine_ls_wR_factor_gt 0.0759 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 0.06367(5) 0.60470(4) 0.41685(4) 0.01867(14) Uani 1 1 d . . . Ge2 Ge -0.11905(5) 0.35171(4) 0.26373(4) 0.02169(14) Uani 1 1 d . . . Br1 Br 0.16612(5) 0.58789(4) 0.27831(4) 0.02262(13) Uani 1 1 d . . . Br2 Br -0.24530(5) 0.16502(4) 0.25381(4) 0.02305(14) Uani 1 1 d . . . Br3 Br 0.08809(5) 0.29251(4) 0.39494(4) 0.02669(15) Uani 1 1 d . . . Br4 Br -0.02145(6) 0.31592(4) 0.12550(4) 0.03069(15) Uani 1 1 d . . . N1 N 0.1185(4) 0.7747(3) 0.4304(3) 0.0183(9) Uani 1 1 d . . . N2 N 0.2628(4) 0.6021(3) 0.5143(3) 0.0173(9) Uani 1 1 d . . . C1 C 0.0325(5) 0.8578(4) 0.3838(4) 0.0230(11) Uani 1 1 d . . . H1 H -0.0569 0.8383 0.3414 0.028 Uiso 1 1 calc R . . C2 C 0.0714(5) 0.9709(4) 0.3961(4) 0.0244(12) Uani 1 1 d . . . H2 H 0.0106 1.0285 0.3617 0.029 Uiso 1 1 calc R . . C3 C 0.1994(5) 0.9984(4) 0.4592(4) 0.0235(11) Uani 1 1 d . . . H3 H 0.2271 1.0757 0.4693 0.028 Uiso 1 1 calc R . . C4 C 0.2889(5) 0.9135(4) 0.5083(4) 0.0205(11) Uani 1 1 d . . . H4 H 0.3777 0.9317 0.5519 0.025 Uiso 1 1 calc R . . C5 C 0.2450(5) 0.8016(4) 0.4918(4) 0.0174(10) Uani 1 1 d . . . C6 C 0.3288(5) 0.7025(4) 0.5369(3) 0.0168(10) Uani 1 1 d . . . C7 C 0.4653(5) 0.7091(4) 0.5991(4) 0.0207(11) Uani 1 1 d . . . H7 H 0.5114 0.7805 0.6142 0.025 Uiso 1 1 calc R . . C8 C 0.5324(5) 0.6103(4) 0.6383(4) 0.0208(11) Uani 1 1 d . . . H8 H 0.6262 0.6129 0.6797 0.025 Uiso 1 1 calc R . . C9 C 0.4620(5) 0.5075(4) 0.6170(4) 0.0185(10) Uani 1 1 d . . . H9 H 0.5057 0.4393 0.6452 0.022 Uiso 1 1 calc R . . C10 C 0.3276(5) 0.5055(4) 0.5542(4) 0.0180(10) Uani 1 1 d . . . H10 H 0.2796 0.4350 0.5387 0.022 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 0.0153(2) 0.0155(3) 0.0232(3) 0.0015(2) 0.0011(2) -0.00147(19) Ge2 0.0236(3) 0.0161(3) 0.0247(3) -0.0013(2) 0.0047(2) 0.0053(2) Br1 0.0225(2) 0.0215(3) 0.0222(3) 0.00175(19) 0.0024(2) 0.00612(19) Br2 0.0178(2) 0.0236(3) 0.0273(3) -0.0014(2) 0.0049(2) -0.00157(19) Br3 0.0282(3) 0.0189(3) 0.0280(3) 0.0023(2) -0.0027(2) -0.0039(2) Br4 0.0439(3) 0.0235(3) 0.0289(3) 0.0024(2) 0.0172(3) -0.0001(2) N1 0.0166(18) 0.0124(19) 0.025(2) -0.0020(16) 0.0026(17) 0.0024(16) N2 0.0148(18) 0.012(2) 0.024(2) 0.0007(16) 0.0039(17) -0.0033(15) C1 0.016(2) 0.023(3) 0.027(3) 0.005(2) -0.001(2) 0.004(2) C2 0.026(3) 0.017(2) 0.029(3) 0.003(2) 0.005(2) 0.005(2) C3 0.031(3) 0.012(2) 0.028(3) 0.002(2) 0.007(2) 0.001(2) C4 0.019(2) 0.014(2) 0.027(3) -0.002(2) 0.003(2) 0.0011(19) C5 0.016(2) 0.016(2) 0.019(3) 0.0029(19) 0.0032(19) 0.0024(18) C6 0.018(2) 0.020(2) 0.014(3) 0.0019(18) 0.0064(19) 0.0066(19) C7 0.023(2) 0.016(2) 0.022(3) -0.003(2) 0.003(2) -0.002(2) C8 0.017(2) 0.024(2) 0.019(3) -0.001(2) 0.000(2) 0.001(2) C9 0.019(2) 0.018(2) 0.020(3) 0.0027(19) 0.0061(19) 0.0018(19) C10 0.023(2) 0.011(2) 0.020(3) 0.0021(19) 0.006(2) -0.0013(19) _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 # Ge2 Br1 3.8772(9) . ? Ge1 N1 2.068(4) . ? Ge1 N2 2.072(4) . ? Ge1 Br1 2.4285(9) . ? Ge2 Br4 2.4252(10) . ? Ge2 Br3 2.4758(8) . ? Ge2 Br2 2.4999(8) . ? N1 C1 1.348(6) . ? N1 C5 1.351(6) . ? N2 C6 1.344(6) . ? N2 C10 1.353(6) . ? C1 C2 1.384(7) . ? C1 H1 0.9500 . ? C2 C3 1.374(7) . ? C2 H2 0.9500 . ? C3 C4 1.392(7) . ? C3 H3 0.9500 . ? C4 C5 1.386(6) . ? C4 H4 0.9500 . ? C5 C6 1.474(6) . ? C6 C7 1.394(6) . ? C7 C8 1.382(7) . ? C7 H7 0.9500 . ? C8 C9 1.384(7) . ? C8 H8 0.9500 . ? C9 C10 1.381(6) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? 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 # Br4 Ge2 Br1 75.96(2) . . ? # Br3 Ge2 Br1 74.64(2) . . ? # Br2 Ge2 Br1 164.18(2) . . ? # Ge1 Br1 Ge2 71.22(2) . . ? N1 Ge1 N2 77.27(14) . . ? N1 Ge1 Br1 90.57(12) . . ? N2 Ge1 Br1 93.04(12) . . ? Br4 Ge2 Br3 99.63(3) . . ? Br4 Ge2 Br2 94.66(3) . . ? Br3 Ge2 Br2 94.82(3) . . ? C1 N1 C5 119.7(4) . . ? C1 N1 Ge1 123.1(3) . . ? C5 N1 Ge1 117.1(3) . . ? C6 N2 C10 119.9(4) . . ? C6 N2 Ge1 116.8(3) . . ? C10 N2 Ge1 123.3(3) . . ? N1 C1 C2 121.6(4) . . ? N1 C1 H1 119.2 . . ? C2 C1 H1 119.2 . . ? C3 C2 C1 118.8(4) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C2 C3 C4 120.3(4) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 118.3(4) . . ? C5 C4 H4 120.9 . . ? C3 C4 H4 120.9 . . ? N1 C5 C4 121.4(4) . . ? N1 C5 C6 113.9(4) . . ? C4 C5 C6 124.6(4) . . ? N2 C6 C7 121.1(4) . . ? N2 C6 C5 114.7(4) . . ? C7 C6 C5 124.2(4) . . ? C8 C7 C6 118.9(4) . . ? C8 C7 H7 120.5 . . ? C6 C7 H7 120.5 . . ? C7 C8 C9 119.6(4) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? C10 C9 C8 119.1(4) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? N2 C10 C9 121.3(4) . . ? N2 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.726 _refine_diff_density_min -1.015 _refine_diff_density_rms 0.178 #===END OF CIF ============================================================== # 4 07wz022a.cif data_07wz022 _database_code_depnum_ccdc_archive 'CCDC 724634' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2007-11-01 _audit_author_name 'Webster, M.' _chemical_name_systematic ; Dichlorido(1,10-phenanthroline)germanium(II) ; _chemical_name_common Dichlorido(1,10-phenanthroline)germanium(ii) _chemical_melting_point ? _chemical_formula_moiety 'C12 H8 Cl2 Ge N2' _chemical_formula_sum 'C12 H8 Cl2 Ge N2' _chemical_formula_weight 323.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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/n' _symmetry_Int_Tables_number 14 # Superceded ** _symmetry_space_group_name_Hall '-P 2yn' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.5156(10) _cell_length_b 14.772(3) _cell_length_c 12.398(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.634(10) _cell_angle_gamma 90.00 _cell_volume 1159.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2689 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.854 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 640 _exptl_absorpt_coefficient_mu 3.076 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7617 # 0.7284 _exptl_absorpt_correction_T_max 1.0000 # 0.8868 _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_% 0 _diffrn_reflns_number 14041 _diffrn_reflns_av_R_equivalents 0.0388 _diffrn_reflns_av_sigmaI/netI 0.0303 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 27.54 _reflns_number_total 2647 _reflns_number_gt 2311 _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^)+(0.0175P)^2^+1.8158P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2647 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0667 _refine_ls_wR_factor_gt 0.0618 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _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 0.12327(4) 0.437365(17) 0.13079(2) 0.01746(9) Uani 1 1 d . . . Cl1 Cl 0.07820(10) 0.35132(4) 0.27949(5) 0.02042(14) Uani 1 1 d . . . Cl2 Cl -0.25826(10) 0.39074(4) 0.02138(5) 0.02359(15) Uani 1 1 d . . . N1 N -0.0044(3) 0.55519(13) 0.18985(16) 0.0155(4) Uani 1 1 d . . . N2 N 0.3925(3) 0.49666(14) 0.26423(17) 0.0174(4) Uani 1 1 d . . . C1 C -0.1987(4) 0.58690(16) 0.1475(2) 0.0170(5) Uani 1 1 d . . . H1 H -0.2877 0.5557 0.0873 0.020 Uiso 1 1 calc R . . C2 C -0.2753(4) 0.66486(17) 0.1892(2) 0.0188(5) Uani 1 1 d . . . H2 H -0.4121 0.6871 0.1554 0.023 Uiso 1 1 calc R . . C3 C -0.1526(4) 0.70908(16) 0.2789(2) 0.0181(5) Uani 1 1 d . . . H3 H -0.2060 0.7604 0.3096 0.022 Uiso 1 1 calc R . . C4 C 0.0541(4) 0.67740(16) 0.32513(19) 0.0169(5) Uani 1 1 d . . . C5 C 0.1934(4) 0.71880(16) 0.4192(2) 0.0186(5) Uani 1 1 d . . . H5 H 0.1450 0.7690 0.4543 0.022 Uiso 1 1 calc R . . C6 C 0.3922(4) 0.68772(17) 0.4589(2) 0.0203(5) Uani 1 1 d . . . H6 H 0.4819 0.7166 0.5209 0.024 Uiso 1 1 calc R . . C7 C 0.4693(4) 0.61128(16) 0.4081(2) 0.0174(5) Uani 1 1 d . . . C8 C 0.6730(4) 0.57407(17) 0.4450(2) 0.0202(5) Uani 1 1 d . . . H8 H 0.7704 0.5998 0.5066 0.024 Uiso 1 1 calc R . . C9 C 0.7294(4) 0.50043(18) 0.3912(2) 0.0211(5) Uani 1 1 d . . . H9 H 0.8657 0.4744 0.4160 0.025 Uiso 1 1 calc R . . C10 C 0.5854(4) 0.46351(17) 0.2994(2) 0.0202(5) Uani 1 1 d . . . H10 H 0.6275 0.4135 0.2616 0.024 Uiso 1 1 calc R . . C11 C 0.3340(4) 0.56878(15) 0.31685(19) 0.0157(5) Uani 1 1 d . . . C12 C 0.1233(4) 0.60119(16) 0.27555(19) 0.0161(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 0.01938(15) 0.01728(14) 0.01618(14) -0.00127(10) 0.00514(10) 0.00091(10) Cl1 0.0211(3) 0.0208(3) 0.0184(3) 0.0016(2) 0.0026(2) -0.0036(2) Cl2 0.0215(3) 0.0212(3) 0.0248(3) -0.0014(2) -0.0010(2) -0.0020(2) N1 0.0147(10) 0.0158(9) 0.0162(10) 0.0002(8) 0.0038(8) -0.0013(8) N2 0.0158(10) 0.0184(10) 0.0184(10) -0.0002(8) 0.0050(8) -0.0006(8) C1 0.0171(12) 0.0183(11) 0.0159(11) 0.0011(9) 0.0045(9) -0.0020(9) C2 0.0177(13) 0.0201(12) 0.0183(12) 0.0035(9) 0.0037(10) 0.0029(9) C3 0.0215(13) 0.0149(11) 0.0208(12) 0.0019(9) 0.0106(10) 0.0007(9) C4 0.0209(13) 0.0152(11) 0.0161(11) 0.0028(9) 0.0070(10) -0.0024(9) C5 0.0236(13) 0.0147(11) 0.0187(12) -0.0023(9) 0.0077(10) -0.0022(10) C6 0.0217(13) 0.0209(12) 0.0184(12) -0.0010(10) 0.0047(10) -0.0053(10) C7 0.0171(12) 0.0190(12) 0.0170(12) 0.0027(9) 0.0059(9) -0.0041(9) C8 0.0182(13) 0.0266(13) 0.0151(12) 0.0028(10) 0.0027(10) -0.0051(10) C9 0.0157(12) 0.0255(13) 0.0223(13) 0.0040(10) 0.0046(10) 0.0013(10) C10 0.0181(13) 0.0200(12) 0.0236(13) 0.0016(10) 0.0074(10) -0.0010(10) C11 0.0168(12) 0.0145(11) 0.0163(11) 0.0016(9) 0.0048(9) -0.0017(9) C12 0.0160(12) 0.0164(11) 0.0157(11) -0.0003(9) 0.0038(9) -0.0014(9) _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 N1 2.132(2) . ? Ge1 N2 2.283(2) . ? Ge1 Cl1 2.3142(7) . ? Ge1 Cl2 2.6276(8) . ? N1 C1 1.336(3) . ? N1 C12 1.366(3) . ? N2 C10 1.324(3) . ? N2 C11 1.350(3) . ? C1 C2 1.401(3) . ? C1 H1 0.9500 . ? C2 C3 1.372(3) . ? C2 H2 0.9500 . ? C3 C4 1.413(3) . ? C3 H3 0.9500 . ? C4 C12 1.407(3) . ? C4 C5 1.435(3) . ? C5 C6 1.353(4) . ? C5 H5 0.9500 . ? C6 C7 1.439(4) . ? C6 H6 0.9500 . ? C7 C11 1.408(3) . ? C7 C8 1.409(4) . ? C8 C9 1.371(4) . ? C8 H8 0.9500 . ? C9 C10 1.403(4) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.430(3) . ? 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 N1 Ge1 N2 74.53(7) . . ? N1 Ge1 Cl1 92.39(6) . . ? N2 Ge1 Cl1 81.58(6) . . ? N1 Ge1 Cl2 89.59(6) . . ? N2 Ge1 Cl2 161.15(6) . . ? Cl1 Ge1 Cl2 89.14(2) . . ? C1 N1 C12 118.6(2) . . ? C1 N1 Ge1 124.19(16) . . ? C12 N1 Ge1 117.24(16) . . ? C10 N2 C11 119.1(2) . . ? C10 N2 Ge1 127.21(17) . . ? C11 N2 Ge1 113.38(15) . . ? N1 C1 C2 122.0(2) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C3 C2 C1 120.0(2) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 119.2(2) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C12 C4 C3 117.4(2) . . ? C12 C4 C5 119.3(2) . . ? C3 C4 C5 123.2(2) . . ? C6 C5 C4 121.3(2) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C5 C6 C7 120.7(2) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C11 C7 C8 116.7(2) . . ? C11 C7 C6 119.0(2) . . ? C8 C7 C6 124.3(2) . . ? C9 C8 C7 119.5(2) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C8 C9 C10 119.9(2) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? N2 C10 C9 121.7(2) . . ? N2 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? N2 C11 C7 123.1(2) . . ? N2 C11 C12 116.6(2) . . ? C7 C11 C12 120.3(2) . . ? N1 C12 C4 122.6(2) . . ? N1 C12 C11 118.0(2) . . ? C4 C12 C11 119.4(2) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.495 _refine_diff_density_min -0.428 _refine_diff_density_rms 0.090 #===END OF CIF ============================================================== # 5 08wz006a.cif data_08wz006 _database_code_depnum_ccdc_archive 'CCDC 724635' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2008-04-21 _audit_author_name 'Webster, M.' _chemical_name_systematic ; Dibromido(1,10-phenanthroline-N,N')germanium(II) ; _chemical_name_common Dibromido(1,10-phenanthroline-N,N')germanium(ii) _chemical_melting_point ? _chemical_formula_moiety 'C12 H8 Br2 Ge N2' _chemical_formula_sum 'C12 H8 Br2 Ge N2' _chemical_formula_weight 412.61 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' Ge Ge 0.1547 1.8001 '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 'C 2/c' _space_group_IT_number 15 # New _space_group_name_Hall '-C 2yc' # New 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 11.226(2) _cell_length_b 14.703(3) _cell_length_c 7.2715(10) _cell_angle_alpha 90.00 _cell_angle_beta 91.091(10) _cell_angle_gamma 90.00 _cell_volume 1200.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4795 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.284 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 9.187 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5689 # 0.2886 _exptl_absorpt_correction_T_max 0.7456 # 0.8376 _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 7867 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 27.56 _reflns_number_total 1373 _reflns_number_gt 1261 _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^)+(0.0274P)^2^+1.7014P] 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 1373 _refine_ls_number_parameters 78 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0288 _refine_ls_R_factor_gt 0.0248 _refine_ls_wR_factor_ref 0.0615 _refine_ls_wR_factor_gt 0.0595 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _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 0.5000 0.06027(3) 0.7500 0.01519(12) Uani 1 2 d S . . Br1 Br 0.69651(2) 0.075735(18) 0.53136(3) 0.01787(11) Uani 1 1 d . . . N1 N 0.44019(18) 0.17185(15) 0.5912(3) 0.0143(4) Uani 1 1 d . . . C1 C 0.3844(2) 0.16841(18) 0.4268(3) 0.0153(5) Uani 1 1 d . . . H1 H 0.3658 0.1109 0.3742 0.018 Uiso 1 1 calc R . . C2 C 0.3529(2) 0.24758(19) 0.3308(3) 0.0180(5) Uani 1 1 d . . . H2 H 0.3157 0.2434 0.2127 0.022 Uiso 1 1 calc R . . C3 C 0.3759(2) 0.33157(18) 0.4072(3) 0.0164(5) Uani 1 1 d . . . H3 H 0.3518 0.3854 0.3446 0.020 Uiso 1 1 calc R . . C4 C 0.4358(2) 0.33688(18) 0.5801(3) 0.0152(5) Uani 1 1 d . . . C5 C 0.4676(3) 0.42053(17) 0.6704(4) 0.0192(6) Uani 1 1 d . . . H5 H 0.4428 0.4767 0.6178 0.023 Uiso 1 1 calc R . . C6 C 0.4677(2) 0.25461(17) 0.6645(3) 0.0130(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 0.0182(2) 0.0138(2) 0.0135(2) 0.000 -0.00345(15) 0.000 Br1 0.01740(17) 0.02105(18) 0.01511(16) 0.00131(9) -0.00074(11) 0.00155(9) N1 0.0119(10) 0.0169(11) 0.0138(10) 0.0001(8) -0.0015(8) 0.0005(8) C1 0.0116(12) 0.0210(14) 0.0133(11) -0.0008(10) 0.0008(9) 0.0003(10) C2 0.0142(13) 0.0265(15) 0.0132(12) 0.0001(10) 0.0000(9) 0.0040(11) C3 0.0152(13) 0.0183(14) 0.0157(12) 0.0055(10) 0.0017(10) 0.0049(10) C4 0.0130(12) 0.0164(13) 0.0164(12) -0.0001(10) 0.0013(9) 0.0001(10) C5 0.0210(15) 0.0138(13) 0.0228(14) 0.0036(10) 0.0045(11) 0.0011(10) C6 0.0108(13) 0.0149(13) 0.0134(11) 0.0000(9) 0.0006(9) -0.0006(9) _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 N1 2.108(2) 2_656 ? Ge1 N1 2.108(2) . ? Ge1 Br1 2.7530(5) . ? Ge1 Br1 2.7530(5) 2_656 ? N1 C1 1.340(3) . ? N1 C6 1.362(3) . ? C1 C2 1.399(4) . ? C1 H1 0.9500 . ? C2 C3 1.376(4) . ? C2 H2 0.9500 . ? C3 C4 1.417(3) . ? C3 H3 0.9500 . ? C4 C6 1.400(4) . ? C4 C5 1.436(4) . ? C5 C5 1.356(6) 2_656 ? C5 H5 0.9500 . ? C6 C6 1.427(5) 2_656 ? 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 N1 Ge1 N1 77.83(11) 2_656 . ? N1 Ge1 Br1 90.09(6) 2_656 . ? N1 Ge1 Br1 82.52(6) . . ? N1 Ge1 Br1 82.52(6) 2_656 2_656 ? N1 Ge1 Br1 90.09(6) . 2_656 ? Br1 Ge1 Br1 170.524(19) . 2_656 ? C1 N1 C6 118.8(2) . . ? C1 N1 Ge1 126.70(18) . . ? C6 N1 Ge1 114.42(16) . . ? N1 C1 C2 121.5(2) . . ? N1 C1 H1 119.2 . . ? C2 C1 H1 119.2 . . ? C3 C2 C1 120.1(2) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 119.3(2) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C6 C4 C3 117.1(2) . . ? C6 C4 C5 118.7(2) . . ? C3 C4 C5 124.2(2) . . ? C5 C5 C4 121.02(15) 2_656 . ? C5 C5 H5 119.5 2_656 . ? C4 C5 H5 119.5 . . ? N1 C6 C4 123.1(2) . . ? N1 C6 C6 116.67(13) . 2_656 ? C4 C6 C6 120.24(14) . 2_656 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.427 _refine_diff_density_min -0.753 _refine_diff_density_rms 0.127 #===END OF CIF ============================================================== # 6 07wz201a.cif data_07wz201 _database_code_depnum_ccdc_archive 'CCDC 724636' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2007-11-20 _audit_author_name 'Webster, M.' _chemical_name_systematic ; chloro(N,N,N',N",N"-pentamethyl-diethylenetriamine)germanium(II) trichlorogermanate(II) ; # Me2NCH2CH2N(Me)CH2CH2NMe2 = C9H23N3 # Several names of ligand in CSD: N-methyl-N,N-bis(dimethylethylamino)amine. # How about 2,5,8-trimethyl-2,5,8-azanonane. # # Ligand name from iLab at dl. Used IsisDraw skc file. # N-[2-(dimethylamino)ethyl]-N,N',N'-trimethylethane-1,2-diamine _chemical_name_common ; chloro(N,N,N',N'',N''-pentamethyl- diethylenetriamine)germanium(ii) trichlorogermanate(ii) ; _chemical_melting_point ? _chemical_formula_moiety 'C9 H23 Cl Ge N3 1+, Cl3 Ge 1-' _chemical_formula_sum 'C9 H23 Cl4 Ge2 N3' _chemical_formula_weight 460.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 # Superceded ** _symmetry_space_group_name_Hall '-P 1' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.3451(10) _cell_length_b 11.813(2) _cell_length_c 13.166(3) _cell_angle_alpha 112.008(10) _cell_angle_beta 98.953(10) _cell_angle_gamma 93.393(15) _cell_volume 896.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 16701 _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 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.705 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 460 _exptl_absorpt_coefficient_mu 3.938 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6744 # _exptl_absorpt_correction_T_max 1.0000 # _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_% 0 _diffrn_reflns_number 13899 _diffrn_reflns_av_R_equivalents 0.0671 _diffrn_reflns_av_sigmaI/netI 0.0651 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.40 _diffrn_reflns_theta_max 27.74 _reflns_number_total 4100 _reflns_number_gt 3115 _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^+7.6800P] 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 4100 _refine_ls_number_parameters 168 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0943 _refine_ls_R_factor_gt 0.0602 _refine_ls_wR_factor_ref 0.1328 _refine_ls_wR_factor_gt 0.1141 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _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 0.13353(11) 0.85515(6) 0.84385(5) 0.02320(17) Uani 1 1 d . . . Ge2 Ge 0.50336(12) 0.26876(6) 0.68088(6) 0.02817(19) Uani 1 1 d . . . Cl1 Cl -0.2246(2) 0.85356(14) 0.84111(13) 0.0283(3) Uani 1 1 d . . . Cl2 Cl 0.4700(2) 0.37540(14) 0.56523(12) 0.0263(3) Uani 1 1 d . . . Cl3 Cl 0.6437(3) 0.43526(15) 0.84164(13) 0.0312(4) Uani 1 1 d . . . Cl4 Cl 0.1532(3) 0.27167(15) 0.70656(14) 0.0327(4) Uani 1 1 d . . . N1 N 0.1742(8) 0.7543(4) 0.9657(4) 0.0218(10) Uani 1 1 d . . . N2 N 0.1270(7) 0.6717(4) 0.7307(4) 0.0173(9) Uani 1 1 d . . . N3 N 0.0884(8) 0.8763(4) 0.6655(4) 0.0219(10) Uani 1 1 d . . . C1 C 0.3838(11) 0.8199(6) 1.0379(5) 0.0306(14) Uani 1 1 d . . . H1A H 0.4330 0.7786 1.0877 0.046 Uiso 1 1 calc R . . H1B H 0.3666 0.9052 1.0824 0.046 Uiso 1 1 calc R . . H1C H 0.4901 0.8193 0.9911 0.046 Uiso 1 1 calc R . . C2 C 0.0130(11) 0.7636(7) 1.0370(5) 0.0328(15) Uani 1 1 d . . . H2A H -0.1242 0.7166 0.9909 0.049 Uiso 1 1 calc R . . H2B H -0.0065 0.8502 1.0744 0.049 Uiso 1 1 calc R . . H2C H 0.0626 0.7303 1.0931 0.049 Uiso 1 1 calc R . . C3 C 0.1953(10) 0.6247(5) 0.9000(5) 0.0233(12) Uani 1 1 d . . . H3A H 0.0548 0.5733 0.8812 0.028 Uiso 1 1 calc R . . H3B H 0.3002 0.5941 0.9443 0.028 Uiso 1 1 calc R . . C4 C 0.2708(10) 0.6159(5) 0.7936(5) 0.0225(12) Uani 1 1 d . . . H4A H 0.4191 0.6589 0.8126 0.027 Uiso 1 1 calc R . . H4B H 0.2733 0.5284 0.7462 0.027 Uiso 1 1 calc R . . C5 C -0.0856(10) 0.5934(6) 0.6845(5) 0.0293(14) Uani 1 1 d . . . H5A H -0.1797 0.6289 0.6412 0.035 Uiso 1 1 calc R . . H5B H -0.1514 0.5896 0.7459 0.035 Uiso 1 1 calc R . . H5C H -0.0655 0.5102 0.6359 0.035 Uiso 1 1 calc R . . C6 C 0.2248(10) 0.6803(6) 0.6381(5) 0.0247(13) Uani 1 1 d . . . H6A H 0.2264 0.5965 0.5822 0.030 Uiso 1 1 calc R . . H6B H 0.3756 0.7199 0.6677 0.030 Uiso 1 1 calc R . . C7 C 0.1013(10) 0.7543(6) 0.5820(5) 0.0238(12) Uani 1 1 d . . . H7A H 0.1750 0.7630 0.5238 0.029 Uiso 1 1 calc R . . H7B H -0.0454 0.7108 0.5456 0.029 Uiso 1 1 calc R . . C8 C -0.0993(11) 0.9305(6) 0.6317(5) 0.0307(14) Uani 1 1 d . . . H8A H -0.0872 0.9416 0.5626 0.046 Uiso 1 1 calc R . . H8B H -0.1048 1.0105 0.6907 0.046 Uiso 1 1 calc R . . H8C H -0.2310 0.8755 0.6191 0.046 Uiso 1 1 calc R . . C9 C 0.2861(11) 0.9615(6) 0.6827(6) 0.0357(16) Uani 1 1 d . . . H9A H 0.4133 0.9268 0.7049 0.054 Uiso 1 1 calc R . . H9B H 0.2798 1.0416 0.7414 0.054 Uiso 1 1 calc R . . H9C H 0.2949 0.9720 0.6130 0.054 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 0.0252(4) 0.0193(3) 0.0239(3) 0.0073(3) 0.0044(3) 0.0026(2) Ge2 0.0334(4) 0.0226(3) 0.0335(4) 0.0141(3) 0.0110(3) 0.0076(3) Cl1 0.0226(8) 0.0329(8) 0.0362(8) 0.0181(7) 0.0108(6) 0.0100(6) Cl2 0.0278(8) 0.0306(8) 0.0216(7) 0.0112(6) 0.0068(6) 0.0011(6) Cl3 0.0333(9) 0.0368(9) 0.0273(7) 0.0180(7) 0.0022(6) 0.0041(7) Cl4 0.0333(9) 0.0311(8) 0.0367(8) 0.0157(7) 0.0113(7) -0.0015(6) N1 0.027(3) 0.022(3) 0.020(2) 0.010(2) 0.008(2) 0.009(2) N2 0.019(2) 0.018(2) 0.019(2) 0.0107(19) 0.0037(18) 0.0038(18) N3 0.023(3) 0.020(2) 0.024(2) 0.012(2) 0.000(2) 0.0021(19) C1 0.036(4) 0.029(3) 0.024(3) 0.009(3) 0.002(3) 0.000(3) C2 0.033(4) 0.046(4) 0.026(3) 0.018(3) 0.011(3) 0.015(3) C3 0.032(3) 0.019(3) 0.021(3) 0.010(2) 0.007(2) 0.008(2) C4 0.030(3) 0.020(3) 0.018(3) 0.009(2) 0.003(2) 0.008(2) C5 0.030(4) 0.024(3) 0.029(3) 0.009(3) 0.000(3) -0.002(3) C6 0.030(3) 0.027(3) 0.019(3) 0.007(2) 0.012(2) 0.006(3) C7 0.026(3) 0.028(3) 0.019(3) 0.011(2) 0.006(2) 0.005(2) C8 0.033(4) 0.032(4) 0.033(3) 0.019(3) 0.006(3) 0.010(3) C9 0.036(4) 0.036(4) 0.037(4) 0.020(3) 0.001(3) -0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ge1 N2 2.114(5) . ? Ge1 Cl1 2.2656(17) . ? Ge1 N1 2.324(5) . ? Ge1 N3 2.428(5) . ? Ge2 Cl3 2.2864(18) . ? Ge2 Cl4 2.2994(18) . ? Ge2 Cl2 2.3064(16) . ? N1 C2 1.474(8) . ? N1 C3 1.475(7) . ? N1 C1 1.485(8) . ? N2 C4 1.482(7) . ? N2 C6 1.484(7) . ? N2 C5 1.490(8) . ? N3 C7 1.466(7) . ? N3 C8 1.472(8) . ? N3 C9 1.493(8) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.520(8) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.520(8) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ge1 Cl1 98.03(14) . . ? N2 Ge1 N1 79.20(17) . . ? Cl1 Ge1 N1 92.38(13) . . ? N2 Ge1 N3 77.82(16) . . ? Cl1 Ge1 N3 90.85(13) . . ? N1 Ge1 N3 157.02(17) . . ? Cl3 Ge2 Cl4 95.79(7) . . ? Cl3 Ge2 Cl2 96.22(6) . . ? Cl4 Ge2 Cl2 95.31(6) . . ? C2 N1 C3 111.4(5) . . ? C2 N1 C1 108.6(5) . . ? C3 N1 C1 110.3(5) . . ? C2 N1 Ge1 118.0(4) . . ? C3 N1 Ge1 107.6(3) . . ? C1 N1 Ge1 100.2(3) . . ? C4 N2 C6 109.4(4) . . ? C4 N2 C5 109.4(4) . . ? C6 N2 C5 109.7(5) . . ? C4 N2 Ge1 104.7(3) . . ? C6 N2 Ge1 105.7(3) . . ? C5 N2 Ge1 117.7(4) . . ? C7 N3 C8 112.0(5) . . ? C7 N3 C9 109.9(5) . . ? C8 N3 C9 108.1(5) . . ? C7 N3 Ge1 106.1(3) . . ? C8 N3 Ge1 118.9(4) . . ? C9 N3 Ge1 101.0(4) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 C4 109.2(5) . . ? N1 C3 H3A 109.8 . . ? C4 C3 H3A 109.8 . . ? N1 C3 H3B 109.8 . . ? C4 C3 H3B 109.8 . . ? H3A C3 H3B 108.3 . . ? N2 C4 C3 110.9(5) . . ? N2 C4 H4A 109.4 . . ? C3 C4 H4A 109.4 . . ? N2 C4 H4B 109.4 . . ? C3 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 C7 111.5(5) . . ? N2 C6 H6A 109.3 . . ? C7 C6 H6A 109.3 . . ? N2 C6 H6B 109.3 . . ? C7 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? N3 C7 C6 109.5(5) . . ? N3 C7 H7A 109.8 . . ? C6 C7 H7A 109.8 . . ? N3 C7 H7B 109.8 . . ? C6 C7 H7B 109.8 . . ? H7A C7 H7B 108.2 . . ? N3 C8 H8A 109.5 . . ? N3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 H9A 109.5 . . ? N3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ge1 N1 C2 -121.4(5) . . . . ? Cl1 Ge1 N1 C2 -23.6(4) . . . . ? N3 Ge1 N1 C2 -121.4(5) . . . . ? N2 Ge1 N1 C3 5.7(4) . . . . ? Cl1 Ge1 N1 C3 103.4(4) . . . . ? N3 Ge1 N1 C3 5.6(7) . . . . ? N2 Ge1 N1 C1 121.0(4) . . . . ? Cl1 Ge1 N1 C1 -141.2(3) . . . . ? N3 Ge1 N1 C1 121.0(5) . . . . ? Cl1 Ge1 N2 C4 -123.3(3) . . . . ? N1 Ge1 N2 C4 -32.4(3) . . . . ? N3 Ge1 N2 C4 147.6(4) . . . . ? Cl1 Ge1 N2 C6 121.2(3) . . . . ? N1 Ge1 N2 C6 -147.9(4) . . . . ? N3 Ge1 N2 C6 32.1(3) . . . . ? Cl1 Ge1 N2 C5 -1.7(4) . . . . ? N1 Ge1 N2 C5 89.2(4) . . . . ? N3 Ge1 N2 C5 -90.8(4) . . . . ? N2 Ge1 N3 C7 -4.9(4) . . . . ? Cl1 Ge1 N3 C7 -102.9(4) . . . . ? N1 Ge1 N3 C7 -4.8(7) . . . . ? N2 Ge1 N3 C8 122.4(4) . . . . ? Cl1 Ge1 N3 C8 24.3(4) . . . . ? N1 Ge1 N3 C8 122.4(5) . . . . ? N2 Ge1 N3 C9 -119.6(4) . . . . ? Cl1 Ge1 N3 C9 142.3(4) . . . . ? N1 Ge1 N3 C9 -119.5(5) . . . . ? C2 N1 C3 C4 153.0(5) . . . . ? C1 N1 C3 C4 -86.2(6) . . . . ? Ge1 N1 C3 C4 22.3(6) . . . . ? C6 N2 C4 C3 170.6(5) . . . . ? C5 N2 C4 C3 -69.3(6) . . . . ? Ge1 N2 C4 C3 57.7(5) . . . . ? N1 C3 C4 N2 -54.3(6) . . . . ? C4 N2 C6 C7 -171.3(5) . . . . ? C5 N2 C6 C7 68.7(6) . . . . ? Ge1 N2 C6 C7 -59.1(5) . . . . ? C8 N3 C7 C6 -154.6(5) . . . . ? C9 N3 C7 C6 85.1(6) . . . . ? Ge1 N3 C7 C6 -23.4(5) . . . . ? N2 C6 C7 N3 55.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.74 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.787 _refine_diff_density_min -0.986 _refine_diff_density_rms 0.170 #===END OF CIF ============================================================== # 7 08wz007b_4.cif data_08wz007b _database_code_depnum_ccdc_archive 'CCDC 724642' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2009-02-23 _audit_author_name 'Webster, M.' _chemical_name_systematic ; Bromo(N-[2-(dimethylamino)ethyl]-N,N',N'-trimethylethane-1,2-diamine)- germanium(II) tribromogermanate ; # MeN{(CH2)2NMe2}2 = Me2NCH2CH2N(Me)CH2CH2NMe2 = C9H23N3 # SMILES string CN(C)CCN(C)CCN(C)C (iLab did not recognise this?) # # Ligand name from iLab at dl. Used IsisDraw skc file. # N-[2-(dimethylamino)ethyl]-N,N',N'-trimethylethane-1,2-diamine # # N,N,N'N',N"-pentamethyl-diethylenetriamine _chemical_name_common ; Bromo(N-(2-(dimethylamino)ethyl)-N,N',N'-trimethylethane-1,2- diamine)-germanium(ii) tribromogermanate ; _chemical_melting_point ? _chemical_formula_moiety 'C9 H23 Br Ge N3 1+, Br3 Ge 1-' _chemical_formula_sum 'C9 H23 Br4 Ge2 N3' _chemical_formula_structural ? _chemical_formula_weight 638.12 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' N N 0.0061 0.0033 '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' 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 21/n' _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.6108(5) _cell_length_b 14.143(3) _cell_length_c 20.132(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.332(10) _cell_angle_gamma 90.00 _cell_volume 1881.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 20221 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.252 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 11.678 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4843 # 0.1832 _exptl_absorpt_correction_T_max 0.7456 # 0.3880 _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 17117 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1160 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 27.89 _reflns_number_total 17130 _reflns_number_gt 11470 _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. >From the CIF: _diffrn_reflns_theta_max 27.89 >From the CIF: _diffrn_reflns_theta_full 27.89 >From the CIF: _reflns_number_total 17130 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 4506 The crystal was twinned about 'a' and had overlapping and non-overlapping reflections. The original data were reprocessed to index the non- overlapping reflections and used to create a HKLF 5 data file. This was used in the refinement with a BASF command. ; _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^)+(0.0452P)^2^+181.7955P] 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 17130 _refine_ls_number_parameters 169 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1655 _refine_ls_R_factor_gt 0.0961 _refine_ls_wR_factor_ref 0.2394 _refine_ls_wR_factor_gt 0.1979 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ge1 Ge 0.7198(2) 0.90633(8) 0.58112(5) 0.0190(3) Uani 1 1 d . . . Ge2 Ge 0.2969(2) 0.96652(9) 0.90285(6) 0.0192(3) Uani 1 1 d . . . Br1 Br 0.35347(18) 0.91342(9) 0.57667(6) 0.0233(3) Uani 1 1 d . . . Br2 Br 0.6691(2) 0.94223(8) 0.90787(6) 0.0233(3) Uani 1 1 d . . . Br3 Br 0.27978(18) 1.07487(8) 0.80435(5) 0.0188(3) Uani 1 1 d . . . Br4 Br 0.2209(2) 0.81828(8) 0.84396(5) 0.0230(3) Uani 1 1 d . . . N1 N 0.7511(15) 1.0564(6) 0.6328(4) 0.0148(18) Uani 1 1 d U . . N2 N 0.7594(14) 0.8676(6) 0.6836(4) 0.0130(17) Uani 1 1 d U . . N3 N 0.7138(17) 0.7385(6) 0.5738(4) 0.0181(19) Uani 1 1 d U . . C1 C 0.5823(19) 1.1220(9) 0.6251(6) 0.021(3) Uani 1 1 d U . . H1A H 0.4656 1.0976 0.6489 0.032 Uiso 1 1 calc R . . H1B H 0.5465 1.1289 0.5779 0.032 Uiso 1 1 calc R . . H1C H 0.6214 1.1837 0.6435 0.032 Uiso 1 1 calc R . . C2 C 0.9296(18) 1.0939(9) 0.5975(6) 0.023(3) Uani 1 1 d U . . H2A H 0.8932 1.1043 0.5506 0.035 Uiso 1 1 calc R . . H2B H 1.0407 1.0481 0.6009 0.035 Uiso 1 1 calc R . . H2C H 0.9723 1.1538 0.6178 0.035 Uiso 1 1 calc R . . C3 C 0.8000(19) 1.0383(7) 0.7046(5) 0.0179(19) Uani 1 1 d U . . H3A H 0.6749 1.0411 0.7306 0.021 Uiso 1 1 calc R . . H3B H 0.8944 1.0873 0.7219 0.021 Uiso 1 1 calc R . . C4 C 0.8962(18) 0.9413(8) 0.7117(5) 0.019(2) Uani 1 1 d U . . H4A H 1.0261 0.9403 0.6882 0.022 Uiso 1 1 calc R . . H4B H 0.9249 0.9279 0.7592 0.022 Uiso 1 1 calc R . . C5 C 0.569(2) 0.8562(10) 0.7245(6) 0.025(3) Uani 1 1 d U . . H5A H 0.4835 0.8063 0.7050 0.038 Uiso 1 1 calc R . . H5B H 0.4937 0.9159 0.7246 0.038 Uiso 1 1 calc R . . H5C H 0.6074 0.8390 0.7703 0.038 Uiso 1 1 calc R . . C6 C 0.867(2) 0.7758(7) 0.6824(5) 0.016(2) Uani 1 1 d U . . H6A H 0.8871 0.7523 0.7284 0.020 Uiso 1 1 calc R . . H6B H 1.0020 0.7847 0.6630 0.020 Uiso 1 1 calc R . . C7 C 0.749(2) 0.7030(7) 0.6419(5) 0.020(2) Uani 1 1 d U . . H7A H 0.8259 0.6430 0.6406 0.024 Uiso 1 1 calc R . . H7B H 0.6178 0.6904 0.6629 0.024 Uiso 1 1 calc R . . C8 C 0.8957(19) 0.7247(10) 0.5336(6) 0.025(3) Uani 1 1 d U . . H8A H 1.0106 0.7578 0.5546 0.037 Uiso 1 1 calc R . . H8B H 0.8708 0.7500 0.4889 0.037 Uiso 1 1 calc R . . H8C H 0.9264 0.6570 0.5307 0.037 Uiso 1 1 calc R . . C9 C 0.5352(18) 0.6907(9) 0.5414(6) 0.023(3) Uani 1 1 d U . . H9A H 0.5212 0.7117 0.4951 0.035 Uiso 1 1 calc R . . H9B H 0.4124 0.7070 0.5652 0.035 Uiso 1 1 calc R . . H9C H 0.5550 0.6220 0.5425 0.035 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 0.0169(6) 0.0190(6) 0.0211(6) 0.0000(5) -0.0011(5) 0.0017(7) Ge2 0.0226(7) 0.0174(6) 0.0177(6) -0.0003(5) -0.0004(6) -0.0008(7) Br1 0.0138(5) 0.0225(6) 0.0333(6) -0.0051(5) -0.0075(5) 0.0055(6) Br2 0.0210(6) 0.0192(6) 0.0292(6) 0.0020(5) -0.0077(5) -0.0024(6) Br3 0.0175(5) 0.0146(5) 0.0242(5) 0.0016(4) -0.0028(5) -0.0007(6) Br4 0.0247(7) 0.0151(5) 0.0289(6) 0.0048(5) -0.0039(6) -0.0081(7) N1 0.020(4) 0.004(4) 0.021(3) 0.000(3) 0.002(4) 0.005(4) N2 0.009(4) 0.018(3) 0.012(4) -0.009(3) 0.002(3) 0.008(3) N3 0.031(5) 0.012(4) 0.011(3) -0.002(3) 0.004(3) -0.005(5) C1 0.021(5) 0.019(6) 0.024(6) 0.005(5) 0.004(4) 0.012(5) C2 0.014(4) 0.026(7) 0.029(5) 0.000(5) -0.001(4) -0.001(6) C3 0.018(6) 0.015(3) 0.020(3) -0.006(4) -0.001(4) 0.013(4) C4 0.017(5) 0.011(3) 0.027(6) -0.001(4) -0.009(4) 0.006(3) C5 0.027(5) 0.030(7) 0.020(6) -0.007(6) 0.015(5) -0.002(5) C6 0.030(6) 0.010(3) 0.009(4) 0.001(4) 0.002(4) 0.007(4) C7 0.034(7) 0.008(3) 0.019(3) 0.004(3) -0.002(4) 0.003(5) C8 0.021(4) 0.035(8) 0.018(5) -0.013(6) -0.002(4) -0.008(7) C9 0.016(4) 0.024(7) 0.029(6) 0.000(5) -0.003(4) 0.005(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 N2 2.145(8) . ? Ge1 N1 2.370(8) . ? Ge1 N3 2.379(9) . ? Ge1 Br1 2.4234(18) . ? Ge2 Br4 2.4547(17) . ? Ge2 Br2 2.4837(19) . ? Ge2 Br3 2.5065(16) . ? N1 C1 1.457(15) . ? N1 C2 1.488(15) . ? N1 C3 1.497(13) . ? N2 C6 1.481(13) . ? N2 C4 1.484(14) . ? N2 C5 1.530(14) . ? N3 C7 1.472(12) . ? N3 C8 1.478(15) . ? N3 C9 1.498(15) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.517(15) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.518(15) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ge1 N1 78.4(3) . . ? N2 Ge1 N3 78.8(3) . . ? N1 Ge1 N3 157.2(3) . . ? N2 Ge1 Br1 98.4(3) . . ? N1 Ge1 Br1 93.2(3) . . ? N3 Ge1 Br1 91.4(3) . . ? Br4 Ge2 Br2 95.33(6) . . ? Br4 Ge2 Br3 97.76(5) . . ? Br2 Ge2 Br3 98.24(6) . . ? C1 N1 C2 109.7(8) . . ? C1 N1 C3 111.0(9) . . ? C2 N1 C3 111.4(9) . . ? C1 N1 Ge1 117.8(7) . . ? C2 N1 Ge1 99.9(6) . . ? C3 N1 Ge1 106.6(6) . . ? C6 N2 C4 109.5(9) . . ? C6 N2 C5 108.6(9) . . ? C4 N2 C5 111.8(8) . . ? C6 N2 Ge1 104.9(6) . . ? C4 N2 Ge1 104.3(6) . . ? C5 N2 Ge1 117.5(7) . . ? C7 N3 C8 110.6(10) . . ? C7 N3 C9 111.0(9) . . ? C8 N3 C9 110.2(8) . . ? C7 N3 Ge1 106.3(6) . . ? C8 N3 Ge1 98.8(7) . . ? C9 N3 Ge1 119.3(7) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 C4 109.0(8) . . ? N1 C3 H3A 109.9 . . ? C4 C3 H3A 109.9 . . ? N1 C3 H3B 109.9 . . ? C4 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? N2 C4 C3 110.4(9) . . ? N2 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? N2 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 C7 111.2(9) . . ? N2 C6 H6A 109.4 . . ? C7 C6 H6A 109.4 . . ? N2 C6 H6B 109.4 . . ? C7 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? N3 C7 C6 109.7(9) . . ? N3 C7 H7A 109.7 . . ? C6 C7 H7A 109.7 . . ? N3 C7 H7B 109.7 . . ? C6 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? N3 C8 H8A 109.5 . . ? N3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 H9A 109.5 . . ? N3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ge1 N1 C1 -120.0(8) . . . . ? N3 Ge1 N1 C1 -123.4(10) . . . . ? Br1 Ge1 N1 C1 -22.1(7) . . . . ? N2 Ge1 N1 C2 121.4(6) . . . . ? N3 Ge1 N1 C2 118.1(10) . . . . ? Br1 Ge1 N1 C2 -140.7(6) . . . . ? N2 Ge1 N1 C3 5.4(7) . . . . ? N3 Ge1 N1 C3 2.1(14) . . . . ? Br1 Ge1 N1 C3 103.3(7) . . . . ? N1 Ge1 N2 C6 -148.4(7) . . . . ? N3 Ge1 N2 C6 30.3(7) . . . . ? Br1 Ge1 N2 C6 120.0(7) . . . . ? N1 Ge1 N2 C4 -33.3(7) . . . . ? N3 Ge1 N2 C4 145.4(7) . . . . ? Br1 Ge1 N2 C4 -124.9(6) . . . . ? N1 Ge1 N2 C5 91.0(8) . . . . ? N3 Ge1 N2 C5 -90.3(8) . . . . ? Br1 Ge1 N2 C5 -0.6(8) . . . . ? N2 Ge1 N3 C7 -2.4(8) . . . . ? N1 Ge1 N3 C7 0.9(15) . . . . ? Br1 Ge1 N3 C7 -100.7(8) . . . . ? N2 Ge1 N3 C8 -117.0(7) . . . . ? N1 Ge1 N3 C8 -113.7(10) . . . . ? Br1 Ge1 N3 C8 144.7(6) . . . . ? N2 Ge1 N3 C9 123.9(8) . . . . ? N1 Ge1 N3 C9 127.2(10) . . . . ? Br1 Ge1 N3 C9 25.6(7) . . . . ? C1 N1 C3 C4 153.2(10) . . . . ? C2 N1 C3 C4 -84.3(11) . . . . ? Ge1 N1 C3 C4 23.7(11) . . . . ? C6 N2 C4 C3 172.1(9) . . . . ? C5 N2 C4 C3 -67.6(12) . . . . ? Ge1 N2 C4 C3 60.4(9) . . . . ? N1 C3 C4 N2 -57.3(12) . . . . ? C4 N2 C6 C7 -168.7(9) . . . . ? C5 N2 C6 C7 69.0(11) . . . . ? Ge1 N2 C6 C7 -57.4(9) . . . . ? C8 N3 C7 C6 80.2(11) . . . . ? C9 N3 C7 C6 -157.2(10) . . . . ? Ge1 N3 C7 C6 -26.0(12) . . . . ? N2 C6 C7 N3 57.5(13) . . . . ? _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 27.89 _diffrn_measured_fraction_theta_full 0.916 _refine_diff_density_max 1.803 _refine_diff_density_min -2.212 _refine_diff_density_rms 0.414 #===END OF CIF ============================================================== # #===END OF FILE =============================================================