# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_address ; Faculty of Chemical Engineering and Llight Industry Guangdong University of Technology Guangzhou, Guangdong 510000 P. R. China ; _publ_contact_author_email panchuny@gdut.edu.cn _publ_contact_author_fax '86 020 83710051' _publ_contact_author_phone '86 020 83710051' _publ_requested_coeditor_name ? #========================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; A new Conformer of Indium Germanate InGe3O7.5(en) Conformational Polymorphism in germanate family ; _publ_section_title_footnote ; ? ; loop_ _publ_author_name _publ_author_address 'Chun-Yang Pan' ; Current address: Faculty of Chemical Engineering and Llight Industry Guangdong University of Technology Guangzhou, Guangdong 510000 P. R. China State Key Laboratory of The Structural Chemistry Fujian Institute of Research on the structure of matter Chinese Academy of Sciences Fuzhou, Fujian 350002 P. R. China ; 'Shou-Tian Zheng' ; State Key Laboratory of The Structural Chemistry Fujian Institute of Research on the structure of matter Chinese Academy of Sciences Fuzhou, Fujian 350002 P. R. China ; 'Guo-Yu Yang' '' _publ_contact_author_name 'Dr Chun-Yang Pan' #===================================================================== data_1 _database_code_depnum_ccdc_archive 'CCDC 632452' #TrackingRef '- enInGe.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C2 H8 Ge3 In N2 O7.5' _chemical_formula_weight 512.8319 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' O O 0.0106 0.0060 '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' In In -0.7276 1.3100 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.826(4) _cell_length_b 8.287(3) _cell_length_c 9.222(4) _cell_angle_alpha 71.887(17) _cell_angle_beta 85.343(18) _cell_angle_gamma 63.734(12) _cell_volume 508.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1523 _cell_measurement_theta_min 2.3275 _cell_measurement_theta_max 27.4835 _exptl_crystal_description prism _exptl_crystal_colour white _exptl_crystal_size_max 0.2800 _exptl_crystal_size_mid 0.0800 _exptl_crystal_size_min 0.0300 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.348 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 412 _exptl_absorpt_coefficient_mu 11.043 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.6477 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 3910 _diffrn_reflns_av_R_equivalents 0.0151 _diffrn_reflns_av_sigmaI/netI 0.0255 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 27.47 _reflns_number_total 2289 _reflns_number_gt 2089 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker XSCANS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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 'calc w=1/[\s^2^(Fo^2^)+(0.0277P)^2^+0.0000P] 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 contrs _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2289 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0226 _refine_ls_R_factor_gt 0.0196 _refine_ls_wR_factor_ref 0.0488 _refine_ls_wR_factor_gt 0.0474 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 In1 In 0.00423(3) -0.00866(3) 0.31344(2) 0.01144(7) Uani 1 1 d . . . Ge1 Ge -0.09275(5) -0.38321(5) 0.82106(4) 0.01201(9) Uani 1 1 d . . . Ge2 Ge 0.24780(4) -0.42129(4) 0.61521(3) 0.00880(8) Uani 1 1 d . . . Ge3 Ge 0.32984(4) -0.44078(5) 0.27840(3) 0.00944(8) Uani 1 1 d . . . O1 O 0.0016(9) -0.4365(8) 0.9963(6) 0.0305(13) Uani 0.50 1 d P . . O2 O -0.1776(9) -0.1342(9) 0.7296(6) 0.0138(13) Uani 0.45 1 d P . . O2' O -0.1273(9) -0.1689(8) 0.7991(7) 0.0269(13) Uani 0.55 1 d P . . O3 O 0.0749(3) -0.4944(3) 0.7009(3) 0.0150(5) Uani 1 1 d . . . O4 O 0.1572(3) -0.1773(3) 0.5418(2) 0.0120(4) Uani 1 1 d . . . O5 O 0.1701(3) -0.2109(3) 0.2059(2) 0.0182(5) Uani 1 1 d . . . O6 O 0.3281(3) -0.5380(3) 0.4768(2) 0.0151(5) Uani 1 1 d . . . O7 O 0.2945(3) -0.5853(4) 0.1927(3) 0.0246(6) Uani 1 1 d . . . O8 O 0.5688(3) -0.4866(3) 0.2430(2) 0.0149(5) Uani 1 1 d . . . N1 N -0.1986(4) -0.1423(4) 0.3933(3) 0.0200(6) Uani 1 1 d . . . H1A H -0.1442 -0.2610 0.3877 0.024 Uiso 1 1 calc R . . H1B H -0.2221 -0.1480 0.4915 0.024 Uiso 1 1 calc R . . N2 N -0.2290(4) 0.1477(4) 0.1216(3) 0.0239(7) Uani 1 1 d . . . H2A H -0.3073 0.2632 0.1287 0.029 Uiso 1 1 calc R . . H2B H -0.1770 0.1619 0.0306 0.029 Uiso 1 1 calc R . . C1 C -0.3795(5) -0.0310(6) 0.2979(5) 0.0293(9) Uani 1 1 d . . . H1C H -0.4616 0.0759 0.3327 0.035 Uiso 1 1 calc R . . H1D H -0.4452 -0.1088 0.3064 0.035 Uiso 1 1 calc R . . C2 C -0.3379(6) 0.0381(6) 0.1335(5) 0.0340(10) Uani 1 1 d . . . H2C H -0.2648 -0.0690 0.0963 0.041 Uiso 1 1 calc R . . H2D H -0.4568 0.1168 0.0709 0.041 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 In1 0.01392(12) 0.00752(12) 0.01317(11) -0.00439(9) 0.00302(8) -0.00452(9) Ge1 0.01161(16) 0.01721(19) 0.01217(16) -0.00783(14) 0.00300(12) -0.00880(14) Ge2 0.00764(15) 0.00665(16) 0.01152(15) -0.00342(12) 0.00164(12) -0.00239(13) Ge3 0.00789(16) 0.00836(17) 0.01246(16) -0.00550(13) 0.00167(12) -0.00256(13) O1 0.042(3) 0.033(4) 0.012(2) 0.005(3) -0.013(2) -0.019(3) O2 0.011(3) 0.011(3) 0.012(3) 0.005(3) -0.002(2) -0.003(2) O2' 0.035(4) 0.016(3) 0.040(4) -0.017(3) 0.022(3) -0.017(3) O3 0.0131(11) 0.0125(12) 0.0241(12) -0.0095(10) 0.0084(9) -0.0084(10) O4 0.0150(11) 0.0048(11) 0.0134(10) -0.0030(9) 0.0001(8) -0.0016(9) O5 0.0207(12) 0.0107(12) 0.0137(10) -0.0048(9) -0.0013(9) 0.0023(10) O6 0.0212(12) 0.0085(11) 0.0149(10) -0.0054(9) 0.0065(9) -0.0057(10) O7 0.0135(12) 0.0327(16) 0.0447(15) -0.0314(13) 0.0129(11) -0.0139(11) O8 0.0095(10) 0.0212(13) 0.0132(10) -0.0031(9) 0.0009(8) -0.0075(10) N1 0.0162(14) 0.0124(15) 0.0263(15) 0.0003(12) -0.0033(12) -0.0052(12) N2 0.0275(16) 0.0173(16) 0.0144(13) -0.0048(12) -0.0012(12) 0.0013(13) C1 0.0154(18) 0.021(2) 0.046(2) -0.0050(18) -0.0072(16) -0.0057(16) C2 0.032(2) 0.029(2) 0.036(2) -0.0139(19) -0.0156(17) -0.0032(18) _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 In1 O2' 2.077(6) 2_556 ? In1 O5 2.092(2) . ? In1 O2 2.107(7) 2_556 ? In1 O4 2.218(2) . ? In1 O4 2.244(2) 2_556 ? In1 N1 2.268(3) . ? In1 N2 2.269(3) . ? Ge1 O2' 1.621(6) . ? Ge1 O1 1.677(5) . ? Ge1 O7 1.731(2) 2_546 ? Ge1 O3 1.768(2) . ? Ge1 O2 1.791(7) . ? Ge1 O1 1.807(5) 2_547 ? Ge2 O4 1.734(2) . ? Ge2 O6 1.749(2) . ? Ge2 O8 1.751(2) 2_646 ? Ge2 O3 1.754(2) . ? Ge3 O5 1.695(2) . ? Ge3 O7 1.747(2) . ? Ge3 O6 1.757(2) . ? Ge3 O8 1.760(2) . ? O1 O1 1.045(10) 2_547 ? O1 Ge1 1.807(5) 2_547 ? O2 O2' 0.689(6) . ? O2 In1 2.107(7) 2_556 ? O2' In1 2.077(6) 2_556 ? O4 In1 2.244(2) 2_556 ? O7 Ge1 1.731(2) 2_546 ? O8 Ge2 1.751(2) 2_646 ? N1 C1 1.474(4) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C2 1.473(5) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? C1 C2 1.509(6) . ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? C2 H2C 0.9700 . ? C2 H2D 0.9700 . ? 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 O2' In1 O5 92.06(17) 2_556 . ? O2' In1 O2 18.93(17) 2_556 2_556 ? O5 In1 O2 96.0(2) . 2_556 ? O2' In1 O4 108.0(2) 2_556 . ? O5 In1 O4 95.23(9) . . ? O2 In1 O4 89.23(16) 2_556 . ? O2' In1 O4 92.17(16) 2_556 2_556 ? O5 In1 O4 172.36(8) . 2_556 ? O2 In1 O4 85.97(19) 2_556 2_556 ? O4 In1 O4 77.40(9) . 2_556 ? O2' In1 N1 164.6(2) 2_556 . ? O5 In1 N1 92.78(11) . . ? O2 In1 N1 170.33(19) 2_556 . ? O4 In1 N1 86.04(9) . . ? O4 In1 N1 84.77(10) 2_556 . ? O2' In1 N2 88.3(2) 2_556 . ? O5 In1 N2 92.48(10) . . ? O2 In1 N2 106.59(17) 2_556 . ? O4 In1 N2 161.57(10) . . ? O4 In1 N2 94.00(9) 2_556 . ? N1 In1 N2 76.87(11) . . ? O2' Ge1 O1 85.9(3) . . ? O2' Ge1 O7 116.4(2) . 2_546 ? O1 Ge1 O7 117.9(2) . 2_546 ? O2' Ge1 O3 114.2(2) . . ? O1 Ge1 O3 113.4(2) . . ? O7 Ge1 O3 107.96(11) 2_546 . ? O2' Ge1 O2 22.6(2) . . ? O1 Ge1 O2 108.3(3) . . ? O7 Ge1 O2 102.0(2) 2_546 . ? O3 Ge1 O2 105.9(2) . . ? O2' Ge1 O1 120.2(3) . 2_547 ? O1 Ge1 O1 34.6(3) . 2_547 ? O7 Ge1 O1 95.3(2) 2_546 2_547 ? O3 Ge1 O1 100.2(2) . 2_547 ? O2 Ge1 O1 142.1(3) . 2_547 ? O4 Ge2 O6 113.94(11) . . ? O4 Ge2 O8 111.13(11) . 2_646 ? O6 Ge2 O8 109.59(11) . 2_646 ? O4 Ge2 O3 112.59(11) . . ? O6 Ge2 O3 102.80(11) . . ? O8 Ge2 O3 106.24(11) 2_646 . ? O5 Ge3 O7 111.85(12) . . ? O5 Ge3 O6 114.62(11) . . ? O7 Ge3 O6 106.97(12) . . ? O5 Ge3 O8 114.52(12) . . ? O7 Ge3 O8 102.14(11) . . ? O6 Ge3 O8 105.70(10) . . ? O1 O1 Ge1 79.5(5) 2_547 . ? O1 O1 Ge1 65.9(5) 2_547 2_547 ? Ge1 O1 Ge1 145.4(3) . 2_547 ? O2' O2 Ge1 64.7(8) . . ? O2' O2 In1 78.0(9) . 2_556 ? Ge1 O2 In1 124.4(3) . 2_556 ? O2 O2' Ge1 92.7(10) . . ? O2 O2' In1 83.1(9) . 2_556 ? Ge1 O2' In1 137.6(3) . 2_556 ? Ge2 O3 Ge1 123.35(13) . . ? Ge2 O4 In1 124.17(11) . . ? Ge2 O4 In1 120.93(11) . 2_556 ? In1 O4 In1 102.60(9) . 2_556 ? Ge3 O5 In1 131.27(12) . . ? Ge2 O6 Ge3 128.64(13) . . ? Ge1 O7 Ge3 129.75(13) 2_546 . ? Ge2 O8 Ge3 124.77(12) 2_646 . ? C1 N1 In1 110.5(2) . . ? C1 N1 H1A 109.6 . . ? In1 N1 H1A 109.6 . . ? C1 N1 H1B 109.6 . . ? In1 N1 H1B 109.6 . . ? H1A N1 H1B 108.1 . . ? C2 N2 In1 108.8(2) . . ? C2 N2 H2A 109.9 . . ? In1 N2 H2A 109.9 . . ? C2 N2 H2B 109.9 . . ? In1 N2 H2B 109.9 . . ? H2A N2 H2B 108.3 . . ? N1 C1 C2 109.3(3) . . ? N1 C1 H1C 109.8 . . ? C2 C1 H1C 109.8 . . ? N1 C1 H1D 109.8 . . ? C2 C1 H1D 109.8 . . ? H1C C1 H1D 108.3 . . ? N2 C2 C1 109.9(3) . . ? N2 C2 H2C 109.7 . . ? C1 C2 H2C 109.7 . . ? N2 C2 H2D 109.7 . . ? C1 C2 H2D 109.7 . . ? H2C C2 H2D 108.2 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O3 0.90 2.25 3.110(4) 160.1 2_546 N1 H1A O6 0.90 2.63 3.113(4) 114.1 2_546 N1 H1B O2 0.90 2.30 3.142(7) 156.5 . N2 H2A O8 0.90 2.40 3.244(4) 156.0 1_465 N2 H2B O5 0.90 2.09 2.935(4) 155.6 2 _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.792 _refine_diff_density_min -0.933 _refine_diff_density_rms 0.135