# 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 _publ_contact_author_name 'Herbert Roesky' _publ_contact_author_email HROESKY@GWDG.DE _publ_section_title ; Synthesis of Phosphine Substituted ?-Diketiminate Based Isomeric Ge(II) Complexes ; loop_ _publ_author_name 'Herbert Roesky' 'Anukul Jana' 'Dastagiri Reddy Nareddula' 'Prinson P. Samuel' 'Carola Schulzke' # Attachment '2and5.cif' data_nd3 _database_code_depnum_ccdc_archive 'CCDC 741341' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H50 Cl Ge N2 P' _chemical_formula_weight 709.84 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' P P 0.1023 0.0942 '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 orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.060(2) _cell_length_b 25.670(5) _cell_length_c 29.272(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7559(3) _cell_formula_units_Z 8 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 62047 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 52.0 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.247 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2992 _exptl_absorpt_coefficient_mu 0.954 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6051 _exptl_absorpt_correction_T_max 0.8803 _exptl_absorpt_process_details 'face indexed' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 IPDSII _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59909 _diffrn_reflns_av_R_equivalents 0.1146 _diffrn_reflns_av_sigmaI/netI 0.0791 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 26.02 _reflns_number_total 14663 _reflns_number_gt 12018 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0350P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.017(7) _refine_ls_number_reflns 14663 _refine_ls_number_parameters 847 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.0911 _refine_ls_wR_factor_gt 0.0861 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.002 _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 0.07763(4) 0.471333(15) 0.086484(14) 0.03274(10) Uani 1 1 d . . . Ge2 Ge 0.26015(4) 0.759533(15) 0.219803(13) 0.03219(9) Uani 1 1 d . . . Cl1 Cl -0.15270(9) 0.47036(5) 0.08004(4) 0.0480(3) Uani 1 1 d . . . Cl2 Cl 0.48988(9) 0.75830(4) 0.21786(4) 0.0474(3) Uani 1 1 d . . . P1 P 0.24796(10) 0.29922(4) -0.00199(3) 0.0340(2) Uani 1 1 d . . . P2 P 0.10847(9) 0.76587(4) 0.04277(3) 0.0320(2) Uani 1 1 d . . . N1 N 0.1067(3) 0.42005(11) 0.03676(11) 0.0290(7) Uani 1 1 d . . . N2 N 0.0809(3) 0.41588(12) 0.13284(10) 0.0310(7) Uani 1 1 d . . . N3 N 0.2442(3) 0.68511(12) 0.20144(10) 0.0323(7) Uani 1 1 d . . . N4 N 0.2383(3) 0.78231(11) 0.15556(10) 0.0288(6) Uani 1 1 d . . . C1 C 0.1517(3) 0.44124(14) -0.00696(13) 0.0274(8) Uani 1 1 d . . . C2 C 0.2866(3) 0.45447(14) -0.01278(13) 0.0321(8) Uani 1 1 d . . . C3 C 0.3254(4) 0.47601(17) -0.05425(14) 0.0394(10) Uani 1 1 d . . . H3 H 0.4162 0.4847 -0.0589 0.047 Uiso 1 1 calc R . . C4 C 0.2345(4) 0.48507(15) -0.08901(13) 0.0396(9) Uani 1 1 d . . . H4 H 0.2629 0.4999 -0.1171 0.047 Uiso 1 1 calc R . . C5 C 0.1032(4) 0.47251(16) -0.08241(14) 0.0389(9) Uani 1 1 d . . . H5 H 0.0417 0.4783 -0.1065 0.047 Uiso 1 1 calc R . . C6 C 0.0576(3) 0.45151(14) -0.04137(13) 0.0311(8) Uani 1 1 d . . . C7 C 0.3905(3) 0.44795(15) 0.02428(15) 0.0377(9) Uani 1 1 d . . . H7 H 0.3471 0.4312 0.0513 0.045 Uiso 1 1 calc R . . C8 C 0.4440(4) 0.50112(16) 0.03922(16) 0.0471(11) Uani 1 1 d . . . H8A H 0.4835 0.5189 0.0129 0.071 Uiso 1 1 calc R . . H8B H 0.5118 0.4963 0.0629 0.071 Uiso 1 1 calc R . . H8C H 0.3710 0.5222 0.0514 0.071 Uiso 1 1 calc R . . C9 C 0.5063(4) 0.41292(17) 0.00879(18) 0.0492(12) Uani 1 1 d . . . H9A H 0.5535 0.4296 -0.0166 0.074 Uiso 1 1 calc R . . H9B H 0.4714 0.3792 -0.0013 0.074 Uiso 1 1 calc R . . H9C H 0.5678 0.4077 0.0343 0.074 Uiso 1 1 calc R . . C10 C -0.0917(3) 0.44160(15) -0.03584(14) 0.0343(9) Uani 1 1 d . . . H10 H -0.1060 0.4228 -0.0063 0.041 Uiso 1 1 calc R . . C11 C -0.1648(4) 0.49435(16) -0.03325(15) 0.0405(10) Uani 1 1 d . . . H11A H -0.1607 0.5116 -0.0631 0.061 Uiso 1 1 calc R . . H11B H -0.1222 0.5164 -0.0102 0.061 Uiso 1 1 calc R . . H11C H -0.2579 0.4885 -0.0248 0.061 Uiso 1 1 calc R . . C12 C -0.1492(4) 0.4084(2) -0.07409(15) 0.0489(11) Uani 1 1 d . . . H12A H -0.1406 0.4271 -0.1032 0.073 Uiso 1 1 calc R . . H12B H -0.2433 0.4015 -0.0679 0.073 Uiso 1 1 calc R . . H12C H -0.1007 0.3754 -0.0758 0.073 Uiso 1 1 calc R . . C13 C 0.0833(3) 0.33313(14) -0.00093(13) 0.0326(8) Uani 1 1 d . . . H13A H 0.0718 0.3533 -0.0295 0.039 Uiso 1 1 calc R . . H13B H 0.0113 0.3069 0.0006 0.039 Uiso 1 1 calc R . . C14 C 0.0729(3) 0.36934(14) 0.03955(13) 0.0282(8) Uani 1 1 d . . . C15 C 0.0357(3) 0.34607(13) 0.08089(13) 0.0287(8) Uani 1 1 d . . . H15 H -0.0046 0.3127 0.0785 0.034 Uiso 1 1 calc R . . C16 C 0.0502(3) 0.36545(14) 0.12484(13) 0.0277(8) Uani 1 1 d . . . C17 C 0.0366(4) 0.32866(15) 0.16434(14) 0.0367(9) Uani 1 1 d . . . H17A H 0.1213 0.3266 0.1808 0.055 Uiso 1 1 calc R . . H17B H 0.0124 0.2940 0.1530 0.055 Uiso 1 1 calc R . . H17C H -0.0328 0.3413 0.1850 0.055 Uiso 1 1 calc R . . C18 C 0.1175(3) 0.43228(14) 0.17871(13) 0.0300(8) Uani 1 1 d . . . C19 C 0.0210(3) 0.45010(14) 0.20961(13) 0.0301(8) Uani 1 1 d . . . C20 C 0.0641(4) 0.46843(16) 0.25180(13) 0.0389(9) Uani 1 1 d . . . H20 H 0.0006 0.4814 0.2729 0.047 Uiso 1 1 calc R . . C21 C 0.1970(4) 0.46824(18) 0.26379(14) 0.0408(10) Uani 1 1 d . . . H21 H 0.2239 0.4808 0.2929 0.049 Uiso 1 1 calc R . . C22 C 0.2900(4) 0.44982(17) 0.23339(13) 0.0391(10) Uani 1 1 d . . . H22 H 0.3811 0.4496 0.2419 0.047 Uiso 1 1 calc R . . C23 C 0.2534(4) 0.43141(15) 0.19037(12) 0.0365(9) Uani 1 1 d . . . C24 C -0.1260(4) 0.44982(15) 0.19937(13) 0.0347(9) Uani 1 1 d . . . H24 H -0.1386 0.4328 0.1689 0.042 Uiso 1 1 calc R . . C25 C -0.1791(4) 0.50556(18) 0.19583(17) 0.0502(12) Uani 1 1 d . . . H25A H -0.1723 0.5226 0.2257 0.075 Uiso 1 1 calc R . . H25B H -0.2723 0.5047 0.1862 0.075 Uiso 1 1 calc R . . H25C H -0.1266 0.5250 0.1734 0.075 Uiso 1 1 calc R . . C26 C -0.2038(4) 0.4176(2) 0.23497(14) 0.0480(11) Uani 1 1 d . . . H26A H -0.1645 0.3828 0.2375 0.072 Uiso 1 1 calc R . . H26B H -0.2968 0.4145 0.2253 0.072 Uiso 1 1 calc R . . H26C H -0.1997 0.4351 0.2647 0.072 Uiso 1 1 calc R . . C27 C 0.3590(4) 0.4099(2) 0.15856(16) 0.0560(14) Uani 1 1 d . . . H27 H 0.3168 0.4036 0.1281 0.067 Uiso 1 1 calc R . . C28 C 0.4727(4) 0.4480(2) 0.15182(18) 0.0649(15) Uani 1 1 d . . . H28A H 0.4372 0.4817 0.1420 0.097 Uiso 1 1 calc R . . H28B H 0.5334 0.4345 0.1284 0.097 Uiso 1 1 calc R . . H28C H 0.5209 0.4523 0.1807 0.097 Uiso 1 1 calc R . . C29 C 0.4113(5) 0.3573(2) 0.1766(2) 0.0696(16) Uani 1 1 d . . . H29A H 0.4600 0.3629 0.2052 0.104 Uiso 1 1 calc R . . H29B H 0.4709 0.3417 0.1539 0.104 Uiso 1 1 calc R . . H29C H 0.3363 0.3338 0.1822 0.104 Uiso 1 1 calc R . . C30 C 0.2255(3) 0.25276(14) 0.04485(13) 0.0356(9) Uani 1 1 d . . . C31 C 0.3173(4) 0.25555(17) 0.08031(15) 0.0434(10) Uani 1 1 d . . . H31 H 0.3934 0.2772 0.0773 0.052 Uiso 1 1 calc R . . C32 C 0.2985(5) 0.22694(19) 0.12008(16) 0.0556(13) Uani 1 1 d . . . H32 H 0.3615 0.2292 0.1442 0.067 Uiso 1 1 calc R . . C33 C 0.1887(5) 0.19535(18) 0.12461(17) 0.0588(14) Uani 1 1 d . . . H33 H 0.1760 0.1762 0.1520 0.071 Uiso 1 1 calc R . . C34 C 0.0977(4) 0.19127(16) 0.09008(16) 0.0475(10) Uani 1 1 d . . . H34 H 0.0231 0.1689 0.0933 0.057 Uiso 1 1 calc R . . C35 C 0.1151(4) 0.22023(15) 0.04999(15) 0.0386(9) Uani 1 1 d . . . H35 H 0.0514 0.2178 0.0261 0.046 Uiso 1 1 calc R . . C36 C 0.2264(3) 0.26131(16) -0.05436(13) 0.0344(8) Uani 1 1 d . . . C37 C 0.2184(3) 0.20723(16) -0.05692(14) 0.0376(9) Uani 1 1 d . . . H37 H 0.2173 0.1873 -0.0296 0.045 Uiso 1 1 calc R . . C38 C 0.2119(3) 0.18179(18) -0.09915(15) 0.0423(10) Uani 1 1 d . . . H38 H 0.2052 0.1449 -0.1003 0.051 Uiso 1 1 calc R . . C39 C 0.2152(4) 0.21024(19) -0.13913(16) 0.0467(11) Uani 1 1 d . . . H39 H 0.2096 0.1930 -0.1678 0.056 Uiso 1 1 calc R . . C40 C 0.2267(4) 0.2638(2) -0.13737(14) 0.0483(11) Uani 1 1 d . . . H40 H 0.2312 0.2833 -0.1649 0.058 Uiso 1 1 calc R . . C41 C 0.2317(4) 0.28906(16) -0.09568(14) 0.0429(10) Uani 1 1 d . . . H41 H 0.2388 0.3260 -0.0950 0.051 Uiso 1 1 calc R . . C42 C 0.1989(3) 0.65130(15) 0.23812(13) 0.0322(9) Uani 1 1 d . . . C43 C 0.2897(3) 0.62640(16) 0.26716(13) 0.0347(9) Uani 1 1 d . . . C44 C 0.2384(4) 0.59868(15) 0.30453(13) 0.0378(9) Uani 1 1 d . . . H44 H 0.2980 0.5820 0.3250 0.045 Uiso 1 1 calc R . . C45 C 0.1044(4) 0.59505(16) 0.31226(14) 0.0396(10) Uani 1 1 d . . . H45 H 0.0721 0.5764 0.3380 0.047 Uiso 1 1 calc R . . C46 C 0.0162(4) 0.61874(16) 0.28240(15) 0.0402(10) Uani 1 1 d . . . H46 H -0.0766 0.6149 0.2874 0.048 Uiso 1 1 calc R . . C47 C 0.0598(3) 0.64801(15) 0.24530(13) 0.0344(9) Uani 1 1 d . . . C48 C 0.4397(3) 0.62706(15) 0.25986(14) 0.0356(9) Uani 1 1 d . . . H48 H 0.4586 0.6474 0.2314 0.043 Uiso 1 1 calc R . . C49 C 0.5103(4) 0.65396(19) 0.29968(15) 0.0463(11) Uani 1 1 d . . . H49A H 0.4814 0.6904 0.3015 0.069 Uiso 1 1 calc R . . H49B H 0.6067 0.6527 0.2948 0.069 Uiso 1 1 calc R . . H49C H 0.4882 0.6361 0.3283 0.069 Uiso 1 1 calc R . . C50 C 0.4939(4) 0.57174(17) 0.25321(17) 0.0489(11) Uani 1 1 d . . . H50A H 0.4799 0.5515 0.2812 0.073 Uiso 1 1 calc R . . H50B H 0.5892 0.5734 0.2464 0.073 Uiso 1 1 calc R . . H50C H 0.4473 0.5549 0.2278 0.073 Uiso 1 1 calc R . . C51 C -0.0369(3) 0.67545(17) 0.21301(15) 0.0421(10) Uani 1 1 d . . . H51 H -0.0010 0.7112 0.2075 0.050 Uiso 1 1 calc R . . C52 C -0.0474(4) 0.6486(2) 0.16649(17) 0.0559(12) Uani 1 1 d . . . H52A H 0.0404 0.6477 0.1520 0.084 Uiso 1 1 calc R . . H52B H -0.1093 0.6680 0.1470 0.084 Uiso 1 1 calc R . . H52C H -0.0801 0.6130 0.1706 0.084 Uiso 1 1 calc R . . C53 C -0.1754(4) 0.6820(2) 0.23353(18) 0.0559(13) Uani 1 1 d . . . H53A H -0.2173 0.6477 0.2369 0.084 Uiso 1 1 calc R . . H53B H -0.2296 0.7038 0.2134 0.084 Uiso 1 1 calc R . . H53C H -0.1682 0.6986 0.2636 0.084 Uiso 1 1 calc R . . C54 C 0.2919(4) 0.60944(16) 0.15253(15) 0.0448(10) Uani 1 1 d . . . H54A H 0.3860 0.5995 0.1532 0.067 Uiso 1 1 calc R . . H54B H 0.2541 0.6006 0.1227 0.067 Uiso 1 1 calc R . . H54C H 0.2438 0.5906 0.1765 0.067 Uiso 1 1 calc R . . C55 C 0.2794(3) 0.66689(15) 0.16045(13) 0.0316(8) Uani 1 1 d . . . C56 C 0.3026(3) 0.69990(15) 0.12289(13) 0.0309(8) Uani 1 1 d . . . H56 H 0.3441 0.6845 0.0970 0.037 Uiso 1 1 calc R . . C57 C 0.2712(3) 0.75284(14) 0.11947(12) 0.0290(8) Uani 1 1 d . . . C58 C 0.2716(3) 0.77612(15) 0.07251(12) 0.0342(9) Uani 1 1 d . . . H58A H 0.3436 0.7600 0.0542 0.041 Uiso 1 1 calc R . . H58B H 0.2899 0.8139 0.0747 0.041 Uiso 1 1 calc R . . C59 C 0.1972(3) 0.83630(15) 0.14878(13) 0.0287(8) Uani 1 1 d . . . C60 C 0.0609(3) 0.84918(15) 0.14982(13) 0.0309(8) Uani 1 1 d . . . C61 C 0.0253(4) 0.90112(16) 0.14298(14) 0.0387(10) Uani 1 1 d . . . H61 H -0.0662 0.9103 0.1432 0.046 Uiso 1 1 calc R . . C62 C 0.1192(4) 0.93947(16) 0.13589(14) 0.0410(10) Uani 1 1 d . . . H62 H 0.0925 0.9745 0.1308 0.049 Uiso 1 1 calc R . . C63 C 0.2527(4) 0.92640(14) 0.13634(13) 0.0377(9) Uani 1 1 d . . . H63 H 0.3173 0.9530 0.1326 0.045 Uiso 1 1 calc R . . C64 C 0.2944(3) 0.87504(15) 0.14209(12) 0.0313(8) Uani 1 1 d . . . C65 C -0.0470(3) 0.80949(16) 0.16092(13) 0.0353(9) Uani 1 1 d . . . H65 H -0.0068 0.7739 0.1585 0.042 Uiso 1 1 calc R . . C66 C -0.1647(4) 0.8120(2) 0.12814(15) 0.0477(11) Uani 1 1 d . . . H66A H -0.2080 0.8461 0.1308 0.072 Uiso 1 1 calc R . . H66B H -0.2284 0.7845 0.1358 0.072 Uiso 1 1 calc R . . H66C H -0.1332 0.8071 0.0967 0.072 Uiso 1 1 calc R . . C67 C -0.0939(4) 0.81721(17) 0.21060(14) 0.0423(10) Uani 1 1 d . . . H67A H -0.0204 0.8096 0.2315 0.063 Uiso 1 1 calc R . . H67B H -0.1681 0.7936 0.2170 0.063 Uiso 1 1 calc R . . H67C H -0.1229 0.8533 0.2149 0.063 Uiso 1 1 calc R . . C68 C 0.4426(3) 0.86336(15) 0.14112(12) 0.0312(8) Uani 1 1 d . . . H68 H 0.4551 0.8249 0.1440 0.037 Uiso 1 1 calc R . . C69 C 0.5119(4) 0.88992(17) 0.18155(14) 0.0430(10) Uani 1 1 d . . . H69A H 0.5015 0.9278 0.1790 0.065 Uiso 1 1 calc R . . H69B H 0.6067 0.8811 0.1813 0.065 Uiso 1 1 calc R . . H69C H 0.4719 0.8779 0.2102 0.065 Uiso 1 1 calc R . . C70 C 0.5068(3) 0.88135(16) 0.09591(14) 0.0357(9) Uani 1 1 d . . . H70A H 0.4612 0.8647 0.0702 0.054 Uiso 1 1 calc R . . H70B H 0.6009 0.8715 0.0957 0.054 Uiso 1 1 calc R . . H70C H 0.4990 0.9193 0.0932 0.054 Uiso 1 1 calc R . . C71 C 0.1387(3) 0.80434(15) -0.00910(14) 0.0328(9) Uani 1 1 d . . . C72 C 0.1634(3) 0.85793(16) -0.00467(16) 0.0390(10) Uani 1 1 d . . . H72 H 0.1716 0.8727 0.0250 0.047 Uiso 1 1 calc R . . C73 C 0.1761(4) 0.88973(17) -0.04280(17) 0.0443(11) Uani 1 1 d . . . H73 H 0.1944 0.9258 -0.0391 0.053 Uiso 1 1 calc R . . C74 C 0.1622(4) 0.86918(17) -0.08611(17) 0.0439(10) Uani 1 1 d . . . H74 H 0.1712 0.8910 -0.1121 0.053 Uiso 1 1 calc R . . C75 C 0.1353(4) 0.81681(17) -0.09153(15) 0.0425(10) Uani 1 1 d . . . H75 H 0.1239 0.8027 -0.1213 0.051 Uiso 1 1 calc R . . C76 C 0.1248(3) 0.78464(16) -0.05342(13) 0.0357(9) Uani 1 1 d . . . H76 H 0.1078 0.7485 -0.0576 0.043 Uiso 1 1 calc R . . C77 C 0.1277(3) 0.69855(15) 0.02423(13) 0.0326(8) Uani 1 1 d . . . C78 C 0.2387(4) 0.67906(14) 0.00126(13) 0.0344(8) Uani 1 1 d . . . H78 H 0.3058 0.7024 -0.0087 0.041 Uiso 1 1 calc R . . C79 C 0.2526(4) 0.62637(15) -0.00719(13) 0.0396(9) Uani 1 1 d . . . H79 H 0.3286 0.6138 -0.0230 0.047 Uiso 1 1 calc R . . C80 C 0.1552(4) 0.59182(16) 0.00744(14) 0.0410(10) Uani 1 1 d . . . H80 H 0.1651 0.5556 0.0019 0.049 Uiso 1 1 calc R . . C81 C 0.0451(4) 0.61001(15) 0.02979(14) 0.0376(9) Uani 1 1 d . . . H81 H -0.0217 0.5863 0.0396 0.045 Uiso 1 1 calc R . . C82 C 0.0305(4) 0.66309(15) 0.03828(14) 0.0357(9) Uani 1 1 d . . . H82 H -0.0464 0.6753 0.0538 0.043 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1 0.0431(2) 0.02572(18) 0.0294(2) -0.00079(19) 0.00140(18) -0.00059(17) Ge2 0.0400(2) 0.02970(19) 0.02688(19) -0.00061(18) -0.00162(18) 0.00081(17) Cl1 0.0459(5) 0.0644(7) 0.0337(6) 0.0024(6) 0.0006(4) 0.0212(5) Cl2 0.0412(5) 0.0433(6) 0.0578(7) 0.0135(6) -0.0170(5) -0.0082(4) P1 0.0325(4) 0.0334(5) 0.0362(5) -0.0038(4) 0.0026(5) -0.0026(4) P2 0.0318(5) 0.0338(5) 0.0304(5) -0.0026(5) 0.0019(4) 0.0002(4) N1 0.0296(15) 0.0224(15) 0.0350(18) 0.0020(14) -0.0002(13) -0.0017(12) N2 0.0281(14) 0.0343(17) 0.0306(17) -0.0079(14) 0.0001(13) -0.0020(13) N3 0.0284(14) 0.0350(17) 0.0335(17) 0.0044(14) 0.0028(14) 0.0003(14) N4 0.0298(14) 0.0304(16) 0.0264(16) -0.0058(13) 0.0017(13) -0.0009(13) C1 0.0339(18) 0.0228(18) 0.025(2) 0.0004(16) 0.0049(16) -0.0004(14) C2 0.0367(19) 0.0283(19) 0.031(2) -0.0027(17) 0.0050(16) 0.0004(15) C3 0.0373(19) 0.041(2) 0.040(2) -0.003(2) 0.0114(18) -0.0054(18) C4 0.052(2) 0.038(2) 0.029(2) 0.0004(18) 0.011(2) -0.0046(18) C5 0.045(2) 0.040(2) 0.032(2) -0.004(2) -0.0003(18) -0.0025(18) C6 0.0382(19) 0.0260(18) 0.029(2) -0.0012(16) 0.0031(17) 0.0019(15) C7 0.0320(19) 0.037(2) 0.044(2) 0.0023(19) 0.0014(18) -0.0011(17) C8 0.043(2) 0.044(3) 0.055(3) -0.002(2) -0.011(2) 0.0010(18) C9 0.036(2) 0.039(2) 0.073(4) 0.002(2) -0.001(2) -0.0021(18) C10 0.036(2) 0.035(2) 0.032(2) 0.0011(17) -0.0025(17) -0.0040(16) C11 0.044(2) 0.040(2) 0.037(2) 0.005(2) -0.0007(18) 0.0045(18) C12 0.044(2) 0.057(3) 0.046(3) -0.007(2) -0.008(2) -0.005(2) C13 0.0353(18) 0.0301(19) 0.032(2) 0.0022(17) 0.0000(17) -0.0011(16) C14 0.0262(16) 0.0287(19) 0.030(2) -0.0023(16) 0.0000(16) -0.0005(15) C15 0.0327(17) 0.0237(17) 0.030(2) -0.0015(17) 0.0016(16) -0.0009(14) C16 0.0268(17) 0.0242(18) 0.032(2) 0.0024(16) 0.0020(15) 0.0016(14) C17 0.041(2) 0.033(2) 0.036(2) 0.0013(19) 0.0001(18) 0.0015(17) C18 0.0352(19) 0.0272(19) 0.028(2) 0.0007(16) -0.0030(16) -0.0028(15) C19 0.0339(18) 0.0258(18) 0.031(2) 0.0007(17) -0.0022(16) -0.0024(15) C20 0.050(2) 0.034(2) 0.032(2) -0.0048(19) 0.0039(18) 0.0016(19) C21 0.050(2) 0.042(2) 0.030(2) -0.003(2) -0.0056(18) -0.0062(19) C22 0.036(2) 0.047(2) 0.034(2) 0.0028(19) -0.0080(17) -0.0025(17) C23 0.0369(19) 0.043(2) 0.029(2) 0.0002(18) -0.0057(18) 0.0004(19) C24 0.041(2) 0.036(2) 0.027(2) -0.0014(18) 0.0035(17) 0.0036(17) C25 0.048(2) 0.044(3) 0.059(3) -0.009(2) -0.004(2) 0.0131(19) C26 0.040(2) 0.066(3) 0.038(3) 0.005(2) 0.0016(18) -0.008(2) C27 0.030(2) 0.099(4) 0.039(3) -0.011(3) -0.0056(19) 0.007(2) C28 0.046(2) 0.092(4) 0.056(3) 0.020(3) 0.012(2) 0.013(3) C29 0.052(3) 0.061(3) 0.095(4) -0.025(3) 0.014(3) 0.011(2) C30 0.0373(19) 0.032(2) 0.038(2) -0.0086(18) -0.0018(17) 0.0045(16) C31 0.0435(19) 0.038(2) 0.048(3) -0.008(2) -0.0086(19) 0.0081(17) C32 0.081(3) 0.045(3) 0.040(3) 0.001(2) -0.023(2) 0.013(2) C33 0.102(4) 0.033(3) 0.042(3) 0.006(2) 0.007(3) 0.019(3) C34 0.064(3) 0.034(2) 0.044(3) 0.006(2) 0.016(2) 0.0070(19) C35 0.043(2) 0.030(2) 0.043(2) 0.0003(19) 0.0003(19) 0.0057(17) C36 0.0294(17) 0.035(2) 0.039(2) 0.0003(19) 0.0019(16) 0.0012(16) C37 0.037(2) 0.038(2) 0.037(2) -0.0008(19) 0.0011(17) 0.0001(17) C38 0.037(2) 0.044(2) 0.046(3) -0.014(2) 0.0032(18) -0.0037(17) C39 0.040(2) 0.055(3) 0.045(3) -0.017(2) 0.0012(19) 0.0024(19) C40 0.050(2) 0.062(3) 0.033(2) -0.001(2) 0.0034(19) 0.009(2) C41 0.054(2) 0.036(2) 0.039(2) 0.0001(19) 0.008(2) 0.0016(19) C42 0.037(2) 0.031(2) 0.028(2) -0.0059(17) 0.0017(16) -0.0004(16) C43 0.038(2) 0.032(2) 0.033(2) -0.0013(18) -0.0005(16) 0.0001(16) C44 0.038(2) 0.038(2) 0.037(2) 0.0039(18) -0.0063(19) 0.0039(18) C45 0.043(2) 0.037(2) 0.038(2) 0.0028(19) 0.0060(19) -0.0058(18) C46 0.039(2) 0.036(2) 0.046(3) 0.002(2) 0.005(2) -0.0045(17) C47 0.037(2) 0.033(2) 0.033(2) -0.0004(18) 0.0013(17) 0.0002(17) C48 0.036(2) 0.035(2) 0.036(2) 0.0032(18) -0.0057(17) 0.0042(17) C49 0.036(2) 0.060(3) 0.044(3) 0.002(2) -0.0072(18) -0.0048(19) C50 0.045(2) 0.041(3) 0.061(3) 0.001(2) 0.000(2) 0.0114(19) C51 0.0333(18) 0.046(2) 0.047(3) 0.008(2) -0.0008(19) -0.0044(17) C52 0.047(2) 0.066(3) 0.054(3) 0.003(3) -0.012(2) -0.010(2) C53 0.042(2) 0.054(3) 0.072(4) 0.017(3) 0.004(2) 0.003(2) C54 0.059(3) 0.036(2) 0.040(3) 0.002(2) -0.001(2) 0.0005(19) C55 0.0308(18) 0.036(2) 0.028(2) 0.0004(17) 0.0019(16) 0.0036(16) C56 0.0337(18) 0.032(2) 0.027(2) -0.0042(18) 0.0043(15) 0.0042(15) C57 0.0281(16) 0.032(2) 0.0267(18) -0.0037(16) 0.0003(14) -0.0043(15) C58 0.0332(18) 0.039(2) 0.030(2) -0.0038(17) 0.0039(16) -0.0005(16) C59 0.0333(18) 0.028(2) 0.0252(19) -0.0012(16) -0.0030(15) 0.0041(15) C60 0.0335(19) 0.034(2) 0.0255(19) -0.0009(17) 0.0006(16) 0.0035(16) C61 0.0352(19) 0.041(2) 0.040(2) 0.002(2) 0.0019(18) 0.0102(18) C62 0.050(2) 0.032(2) 0.041(2) -0.0014(19) 0.003(2) 0.0111(19) C63 0.051(2) 0.0264(19) 0.036(2) 0.0075(17) 0.007(2) 0.0024(19) C64 0.038(2) 0.033(2) 0.023(2) -0.0032(17) -0.0008(15) -0.0010(16) C65 0.0308(19) 0.038(2) 0.037(2) -0.0012(19) 0.0020(16) 0.0008(16) C66 0.039(2) 0.062(3) 0.042(3) -0.006(2) -0.0005(19) 0.0064(19) C67 0.041(2) 0.046(2) 0.039(2) -0.006(2) 0.0042(19) -0.0008(18) C68 0.0359(19) 0.030(2) 0.028(2) 0.0050(16) 0.0011(16) -0.0015(16) C69 0.044(2) 0.048(3) 0.037(3) -0.002(2) -0.0047(18) 0.0010(19) C70 0.036(2) 0.036(2) 0.035(2) 0.0061(19) 0.0032(16) -0.0053(16) C71 0.0290(17) 0.031(2) 0.038(2) -0.0021(18) -0.0035(16) 0.0065(15) C72 0.0324(19) 0.039(2) 0.045(3) -0.002(2) -0.0033(18) 0.0074(16) C73 0.043(2) 0.032(2) 0.058(3) 0.008(2) -0.002(2) 0.0074(17) C74 0.041(2) 0.045(3) 0.046(3) 0.015(2) 0.002(2) 0.0044(18) C75 0.042(2) 0.049(3) 0.037(2) 0.000(2) 0.0016(19) 0.0067(18) C76 0.0356(18) 0.039(2) 0.032(2) -0.0036(18) -0.0008(17) -0.0022(17) C77 0.0315(18) 0.036(2) 0.030(2) 0.0008(18) -0.0034(16) -0.0008(16) C78 0.0366(18) 0.0327(19) 0.034(2) -0.0013(17) -0.0006(18) -0.0038(17) C79 0.046(2) 0.039(2) 0.033(2) -0.0049(18) -0.007(2) 0.009(2) C80 0.056(2) 0.028(2) 0.039(2) 0.001(2) -0.009(2) -0.0032(19) C81 0.044(2) 0.029(2) 0.040(2) 0.0028(18) -0.0055(19) -0.0067(17) C82 0.0355(19) 0.037(2) 0.034(2) 0.0023(19) -0.0033(17) -0.0062(17) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 1.967(3) . ? Ge1 N1 1.984(3) . ? Ge1 Cl1 2.3250(11) . ? Ge2 N4 1.982(3) . ? Ge2 N3 1.991(3) . ? Ge2 Cl2 2.3121(11) . ? P1 C36 1.829(4) . ? P1 C30 1.831(4) . ? P1 C13 1.872(4) . ? P2 C77 1.822(4) . ? P2 C71 1.837(4) . ? P2 C58 1.876(4) . ? N1 C14 1.348(4) . ? N1 C1 1.462(5) . ? N2 C16 1.351(5) . ? N2 C18 1.455(5) . ? N3 C55 1.336(5) . ? N3 C42 1.454(5) . ? N4 C57 1.341(4) . ? N4 C59 1.460(4) . ? C1 C6 1.407(5) . ? C1 C2 1.409(5) . ? C2 C3 1.390(5) . ? C2 C7 1.516(5) . ? C3 C4 1.388(6) . ? C4 C5 1.374(5) . ? C5 C6 1.394(5) . ? C6 C10 1.533(5) . ? C7 C8 1.531(5) . ? C7 C9 1.540(5) . ? C10 C12 1.521(6) . ? C10 C11 1.543(5) . ? C13 C14 1.509(5) . ? C14 C15 1.400(5) . ? C15 C16 1.387(5) . ? C16 C17 1.499(5) . ? C18 C19 1.403(5) . ? C18 C23 1.409(5) . ? C19 C20 1.391(5) . ? C19 C24 1.509(5) . ? C20 C21 1.381(5) . ? C21 C22 1.375(5) . ? C22 C23 1.394(5) . ? C23 C27 1.517(6) . ? C24 C25 1.531(6) . ? C24 C26 1.544(5) . ? C27 C28 1.519(7) . ? C27 C29 1.542(7) . ? C30 C31 1.391(5) . ? C30 C35 1.398(5) . ? C31 C32 1.390(6) . ? C32 C33 1.377(7) . ? C33 C34 1.367(7) . ? C34 C35 1.400(6) . ? C36 C37 1.393(5) . ? C36 C41 1.405(5) . ? C37 C38 1.399(6) . ? C38 C39 1.380(6) . ? C39 C40 1.380(6) . ? C40 C41 1.383(6) . ? C42 C43 1.402(5) . ? C42 C47 1.418(5) . ? C43 C44 1.404(5) . ? C43 C48 1.525(5) . ? C44 C45 1.369(5) . ? C45 C46 1.386(6) . ? C46 C47 1.392(6) . ? C47 C51 1.528(5) . ? C48 C49 1.530(6) . ? C48 C50 1.534(5) . ? C51 C53 1.526(5) . ? C51 C52 1.529(6) . ? C54 C55 1.498(5) . ? C55 C56 1.408(5) . ? C56 C57 1.399(5) . ? C57 C58 1.499(5) . ? C59 C64 1.408(5) . ? C59 C60 1.411(5) . ? C60 C61 1.395(5) . ? C60 C65 1.523(5) . ? C61 C62 1.380(6) . ? C62 C63 1.384(6) . ? C63 C64 1.394(5) . ? C64 C68 1.521(5) . ? C65 C66 1.526(5) . ? C65 C67 1.542(5) . ? C68 C69 1.534(5) . ? C68 C70 1.543(5) . ? C71 C76 1.399(5) . ? C71 C72 1.404(5) . ? C72 C73 1.389(6) . ? C73 C74 1.380(7) . ? C74 C75 1.380(6) . ? C75 C76 1.392(6) . ? C77 C78 1.396(5) . ? C77 C82 1.398(5) . ? C78 C79 1.382(5) . ? C79 C80 1.389(6) . ? C80 C81 1.369(6) . ? C81 C82 1.393(5) . ? 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 91.35(12) . . ? N2 Ge1 Cl1 93.70(9) . . ? N1 Ge1 Cl1 94.61(8) . . ? N4 Ge2 N3 91.03(12) . . ? N4 Ge2 Cl2 95.26(9) . . ? N3 Ge2 Cl2 93.49(9) . . ? C36 P1 C30 105.45(17) . . ? C36 P1 C13 99.00(16) . . ? C30 P1 C13 100.45(16) . . ? C77 P2 C71 104.26(17) . . ? C77 P2 C58 100.28(17) . . ? C71 P2 C58 99.41(16) . . ? C14 N1 C1 119.4(3) . . ? C14 N1 Ge1 124.0(3) . . ? C1 N1 Ge1 116.2(2) . . ? C16 N2 C18 119.7(3) . . ? C16 N2 Ge1 124.7(3) . . ? C18 N2 Ge1 115.6(2) . . ? C55 N3 C42 122.5(3) . . ? C55 N3 Ge2 123.8(3) . . ? C42 N3 Ge2 113.5(2) . . ? C57 N4 C59 119.9(3) . . ? C57 N4 Ge2 123.6(2) . . ? C59 N4 Ge2 116.1(2) . . ? C6 C1 C2 121.0(3) . . ? C6 C1 N1 119.2(3) . . ? C2 C1 N1 119.6(3) . . ? C3 C2 C1 118.2(3) . . ? C3 C2 C7 118.3(3) . . ? C1 C2 C7 123.4(3) . . ? C4 C3 C2 121.4(3) . . ? C5 C4 C3 119.4(4) . . ? C4 C5 C6 121.9(4) . . ? C5 C6 C1 117.9(3) . . ? C5 C6 C10 118.5(3) . . ? C1 C6 C10 123.5(3) . . ? C2 C7 C8 110.4(3) . . ? C2 C7 C9 112.1(3) . . ? C8 C7 C9 109.8(3) . . ? C12 C10 C6 112.8(3) . . ? C12 C10 C11 110.3(3) . . ? C6 C10 C11 109.1(3) . . ? C14 C13 P1 111.1(2) . . ? N1 C14 C15 122.1(3) . . ? N1 C14 C13 122.0(3) . . ? C15 C14 C13 115.7(3) . . ? C16 C15 C14 128.4(3) . . ? N2 C16 C15 121.9(3) . . ? N2 C16 C17 119.4(3) . . ? C15 C16 C17 118.7(3) . . ? C19 C18 C23 121.3(3) . . ? C19 C18 N2 120.9(3) . . ? C23 C18 N2 117.7(3) . . ? C20 C19 C18 117.8(3) . . ? C20 C19 C24 118.9(3) . . ? C18 C19 C24 123.2(3) . . ? C21 C20 C19 121.7(4) . . ? C22 C21 C20 119.7(4) . . ? C21 C22 C23 121.4(3) . . ? C22 C23 C18 118.0(3) . . ? C22 C23 C27 119.6(3) . . ? C18 C23 C27 122.4(3) . . ? C19 C24 C25 110.5(3) . . ? C19 C24 C26 111.5(3) . . ? C25 C24 C26 111.7(3) . . ? C23 C27 C28 111.8(4) . . ? C23 C27 C29 110.4(4) . . ? C28 C27 C29 110.6(4) . . ? C31 C30 C35 118.5(4) . . ? C31 C30 P1 116.3(3) . . ? C35 C30 P1 124.6(3) . . ? C32 C31 C30 120.5(4) . . ? C33 C32 C31 120.1(4) . . ? C34 C33 C32 120.7(5) . . ? C33 C34 C35 119.7(4) . . ? C30 C35 C34 120.4(4) . . ? C37 C36 C41 117.5(4) . . ? C37 C36 P1 125.6(3) . . ? C41 C36 P1 116.6(3) . . ? C36 C37 C38 121.0(4) . . ? C39 C38 C37 120.1(4) . . ? C38 C39 C40 119.8(4) . . ? C39 C40 C41 120.2(4) . . ? C40 C41 C36 121.4(4) . . ? C43 C42 C47 121.8(4) . . ? C43 C42 N3 121.0(3) . . ? C47 C42 N3 117.0(3) . . ? C42 C43 C44 117.6(3) . . ? C42 C43 C48 123.7(3) . . ? C44 C43 C48 118.6(3) . . ? C45 C44 C43 121.7(4) . . ? C44 C45 C46 119.7(4) . . ? C45 C46 C47 121.8(4) . . ? C46 C47 C42 117.3(3) . . ? C46 C47 C51 122.1(3) . . ? C42 C47 C51 120.6(3) . . ? C43 C48 C49 111.0(3) . . ? C43 C48 C50 111.1(3) . . ? C49 C48 C50 110.5(3) . . ? C53 C51 C47 112.8(4) . . ? C53 C51 C52 109.7(3) . . ? C47 C51 C52 112.8(4) . . ? N3 C55 C56 122.3(4) . . ? N3 C55 C54 120.4(3) . . ? C56 C55 C54 117.2(3) . . ? C57 C56 C55 127.1(4) . . ? N4 C57 C56 123.2(3) . . ? N4 C57 C58 119.9(3) . . ? C56 C57 C58 116.9(3) . . ? C57 C58 P2 111.5(2) . . ? C64 C59 C60 120.8(3) . . ? C64 C59 N4 119.5(3) . . ? C60 C59 N4 119.6(3) . . ? C61 C60 C59 118.1(3) . . ? C61 C60 C65 119.1(3) . . ? C59 C60 C65 122.7(3) . . ? C62 C61 C60 121.8(4) . . ? C61 C62 C63 119.3(4) . . ? C62 C63 C64 121.5(4) . . ? C63 C64 C59 118.4(3) . . ? C63 C64 C68 118.6(3) . . ? C59 C64 C68 123.0(3) . . ? C60 C65 C66 113.0(3) . . ? C60 C65 C67 109.5(3) . . ? C66 C65 C67 110.5(3) . . ? C64 C68 C69 110.1(3) . . ? C64 C68 C70 111.5(3) . . ? C69 C68 C70 109.8(3) . . ? C76 C71 C72 117.2(4) . . ? C76 C71 P2 123.8(3) . . ? C72 C71 P2 118.7(3) . . ? C73 C72 C71 121.2(4) . . ? C74 C73 C72 120.3(4) . . ? C73 C74 C75 119.8(4) . . ? C74 C75 C76 120.0(4) . . ? C75 C76 C71 121.4(4) . . ? C78 C77 C82 117.9(4) . . ? C78 C77 P2 124.6(3) . . ? C82 C77 P2 117.1(3) . . ? C79 C78 C77 121.2(4) . . ? C78 C79 C80 119.9(4) . . ? C81 C80 C79 120.0(4) . . ? C80 C81 C82 120.3(4) . . ? C81 C82 C77 120.7(4) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.453 _refine_diff_density_min -0.492 _refine_diff_density_rms 0.058 data_ndr9 _database_code_depnum_ccdc_archive 'CCDC 741342' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H50 Cl Ge N2 P' _chemical_formula_weight 709.84 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' P P 0.1023 0.0942 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.003(2) _cell_length_b 11.678(2) _cell_length_c 16.335(3) _cell_angle_alpha 86.03(3) _cell_angle_beta 87.29(3) _cell_angle_gamma 67.40(3) _cell_volume 1932.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 36083 _cell_measurement_theta_min 3.8 _cell_measurement_theta_max 54.3 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.220 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 0.932 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.4211 _exptl_absorpt_correction_T_max 0.5706 _exptl_absorpt_process_details 'face indexed' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 IPDSII _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17957 _diffrn_reflns_av_R_equivalents 0.0832 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 27.04 _reflns_number_total 8316 _reflns_number_gt 7725 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0736P)^2^+0.5013P] 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 8316 _refine_ls_number_parameters 425 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0467 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1199 _refine_ls_wR_factor_gt 0.1177 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _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 0.486267(19) 0.416868(17) 0.289564(12) 0.02236(8) Uani 1 1 d . . . Cl1 Cl 0.29927(5) 0.42766(5) 0.22743(3) 0.03218(13) Uani 1 1 d . . . P1 P 0.63107(4) 0.27391(4) 0.19285(3) 0.01905(11) Uani 1 1 d . . . N1 N 0.51613(15) 0.25839(14) 0.35215(9) 0.0186(3) Uani 1 1 d . . . N2 N 0.78732(15) 0.00262(14) 0.15271(9) 0.0192(3) Uani 1 1 d . . . C1 C 0.7907(2) 0.2816(2) 0.20468(12) 0.0268(4) Uani 1 1 d . . . C2 C 0.8968(2) 0.1806(2) 0.23595(13) 0.0316(4) Uani 1 1 d . . . H2 H 0.8888 0.1029 0.2477 0.038 Uiso 1 1 calc R . . C3 C 1.0152(2) 0.1929(3) 0.25011(15) 0.0435(6) Uani 1 1 d . . . H3 H 1.0869 0.1239 0.2724 0.052 Uiso 1 1 calc R . . C4 C 1.0287(3) 0.3042(3) 0.23209(17) 0.0503(8) Uani 1 1 d . . . H4 H 1.1100 0.3117 0.2410 0.060 Uiso 1 1 calc R . . C5 C 0.9237(3) 0.4054(3) 0.20095(18) 0.0522(8) Uani 1 1 d . . . H5 H 0.9333 0.4822 0.1885 0.063 Uiso 1 1 calc R . . C6 C 0.8039(3) 0.3954(2) 0.18774(16) 0.0394(5) Uani 1 1 d . . . H6 H 0.7316 0.4656 0.1673 0.047 Uiso 1 1 calc R . . C7 C 0.59014(19) 0.29508(17) 0.08562(12) 0.0229(4) Uani 1 1 d . . . C8 C 0.6624(2) 0.3343(2) 0.02615(13) 0.0321(5) Uani 1 1 d . . . H8 H 0.7391 0.3461 0.0409 0.038 Uiso 1 1 calc R . . C9 C 0.6225(3) 0.3564(2) -0.05491(15) 0.0409(6) Uani 1 1 d . . . H9 H 0.6716 0.3838 -0.0954 0.049 Uiso 1 1 calc R . . C10 C 0.5116(3) 0.3386(2) -0.07652(14) 0.0424(6) Uani 1 1 d . . . H10 H 0.4851 0.3532 -0.1321 0.051 Uiso 1 1 calc R . . C11 C 0.4382(3) 0.2994(2) -0.01783(15) 0.0380(5) Uani 1 1 d . . . H11 H 0.3618 0.2876 -0.0331 0.046 Uiso 1 1 calc R . . C12 C 0.4772(2) 0.27772(19) 0.06307(13) 0.0287(4) Uani 1 1 d . . . H12 H 0.4273 0.2510 0.1034 0.034 Uiso 1 1 calc R . . C13 C 0.49305(18) 0.26719(16) 0.43936(11) 0.0194(3) Uani 1 1 d . . . C14 C 0.37240(18) 0.27138(17) 0.47495(12) 0.0209(4) Uani 1 1 d . . . C15 C 0.3549(2) 0.28076(19) 0.55948(12) 0.0262(4) Uani 1 1 d . . . H15 H 0.2746 0.2829 0.5847 0.031 Uiso 1 1 calc R . . C16 C 0.4519(2) 0.2871(2) 0.60772(12) 0.0307(4) Uani 1 1 d . . . H16 H 0.4375 0.2942 0.6653 0.037 Uiso 1 1 calc R . . C17 C 0.5705(2) 0.2831(2) 0.57193(13) 0.0313(4) Uani 1 1 d . . . H17 H 0.6371 0.2870 0.6054 0.038 Uiso 1 1 calc R . . C18 C 0.59296(19) 0.27360(19) 0.48762(12) 0.0247(4) Uani 1 1 d . . . C19 C 0.26134(18) 0.26815(18) 0.42429(12) 0.0226(4) Uani 1 1 d . . . H19 H 0.2932 0.2574 0.3659 0.027 Uiso 1 1 calc R . . C20 C 0.2197(2) 0.1601(2) 0.45206(14) 0.0312(5) Uani 1 1 d . . . H20A H 0.2962 0.0815 0.4494 0.047 Uiso 1 1 calc R . . H20B H 0.1515 0.1593 0.4159 0.047 Uiso 1 1 calc R . . H20C H 0.1849 0.1704 0.5086 0.047 Uiso 1 1 calc R . . C21 C 0.1424(2) 0.3913(2) 0.42794(14) 0.0322(5) Uani 1 1 d . . . H21A H 0.1094 0.4037 0.4847 0.048 Uiso 1 1 calc R . . H21B H 0.0729 0.3893 0.3934 0.048 Uiso 1 1 calc R . . H21C H 0.1688 0.4596 0.4080 0.048 Uiso 1 1 calc R . . C22 C 0.7250(2) 0.2671(2) 0.45032(14) 0.0308(4) Uani 1 1 d . . . H22 H 0.7149 0.2825 0.3896 0.037 Uiso 1 1 calc R . . C23 C 0.7658(3) 0.3679(3) 0.4822(2) 0.0484(7) Uani 1 1 d . . . H23A H 0.6932 0.4491 0.4752 0.073 Uiso 1 1 calc R . . H23B H 0.8435 0.3696 0.4511 0.073 Uiso 1 1 calc R . . H23C H 0.7865 0.3493 0.5405 0.073 Uiso 1 1 calc R . . C24 C 0.8324(2) 0.1389(3) 0.4664(2) 0.0467(6) Uani 1 1 d . . . H24A H 0.8408 0.1194 0.5257 0.070 Uiso 1 1 calc R . . H24B H 0.9163 0.1383 0.4428 0.070 Uiso 1 1 calc R . . H24C H 0.8093 0.0767 0.4409 0.070 Uiso 1 1 calc R . . C25 C 0.5798(2) 0.03318(17) 0.37229(12) 0.0241(4) Uani 1 1 d . . . H25A H 0.5862 0.0492 0.4297 0.036 Uiso 1 1 calc R . . H25B H 0.6579 -0.0382 0.3564 0.036 Uiso 1 1 calc R . . H25C H 0.5008 0.0153 0.3659 0.036 Uiso 1 1 calc R . . C26 C 0.57112(17) 0.14608(16) 0.31818(11) 0.0177(3) Uani 1 1 d . . . C27 C 0.62225(17) 0.13521(16) 0.23865(11) 0.0181(3) Uani 1 1 d . . . C28 C 0.68326(17) 0.01780(16) 0.19714(11) 0.0181(3) Uani 1 1 d . . . C29 C 0.62004(19) -0.07749(19) 0.20420(13) 0.0251(4) Uani 1 1 d . . . H29A H 0.6174 -0.1067 0.1497 0.038 Uiso 1 1 calc R . . H29B H 0.5302 -0.0394 0.2267 0.038 Uiso 1 1 calc R . . H29C H 0.6717 -0.1479 0.2407 0.038 Uiso 1 1 calc R . . C30 C 0.85555(17) -0.11202(17) 0.11597(11) 0.0188(3) Uani 1 1 d . . . C31 C 0.94242(18) -0.21403(17) 0.16359(12) 0.0219(4) Uani 1 1 d . . . C32 C 0.84526(18) -0.12010(18) 0.03110(12) 0.0211(4) Uani 1 1 d . . . C33 C 0.9192(2) -0.23124(19) -0.00458(12) 0.0261(4) Uani 1 1 d . . . H33 H 0.9115 -0.2382 -0.0615 0.031 Uiso 1 1 calc R . . C34 C 1.0043(2) -0.33258(19) 0.04174(13) 0.0278(4) Uani 1 1 d . . . H34 H 1.0538 -0.4081 0.0166 0.033 Uiso 1 1 calc R . . C35 C 1.01588(19) -0.32237(18) 0.12449(13) 0.0255(4) Uani 1 1 d . . . H35 H 1.0756 -0.3911 0.1555 0.031 Uiso 1 1 calc R . . C36 C 0.76166(19) -0.00703(18) -0.02122(12) 0.0232(4) Uani 1 1 d . . . H36 H 0.7016 0.0555 0.0164 0.028 Uiso 1 1 calc R . . C37 C 0.8509(2) 0.0501(2) -0.06679(18) 0.0446(6) Uani 1 1 d . . . H37A H 0.8957 0.0785 -0.0270 0.067 Uiso 1 1 calc R . . H37B H 0.7978 0.1208 -0.1026 0.067 Uiso 1 1 calc R . . H37C H 0.9165 -0.0124 -0.1000 0.067 Uiso 1 1 calc R . . C38 C 0.6771(3) -0.0357(3) -0.0812(2) 0.0530(7) Uani 1 1 d . . . H38A H 0.7339 -0.0979 -0.1182 0.080 Uiso 1 1 calc R . . H38B H 0.6258 0.0403 -0.1132 0.080 Uiso 1 1 calc R . . H38C H 0.6172 -0.0682 -0.0507 0.080 Uiso 1 1 calc R . . C39 C 0.9607(2) -0.20569(18) 0.25433(12) 0.0261(4) Uani 1 1 d . . . H39 H 0.8859 -0.1312 0.2738 0.031 Uiso 1 1 calc R . . C40 C 1.0885(3) -0.1878(3) 0.26851(15) 0.0426(6) Uani 1 1 d . . . H40A H 1.1638 -0.2613 0.2521 0.064 Uiso 1 1 calc R . . H40B H 1.0944 -0.1761 0.3268 0.064 Uiso 1 1 calc R . . H40C H 1.0891 -0.1145 0.2358 0.064 Uiso 1 1 calc R . . C41 C 0.9584(2) -0.3195(2) 0.30572(13) 0.0355(5) Uani 1 1 d . . . H41A H 0.8773 -0.3317 0.2954 0.053 Uiso 1 1 calc R . . H41B H 0.9618 -0.3066 0.3641 0.053 Uiso 1 1 calc R . . H41C H 1.0347 -0.3931 0.2906 0.053 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 0.02627(13) 0.01146(12) 0.02634(12) -0.00057(8) 0.00331(8) -0.00441(8) Cl1 0.0205(2) 0.0314(3) 0.0339(3) 0.0116(2) -0.00236(18) -0.00004(19) P1 0.0191(2) 0.0143(2) 0.0224(2) -0.00023(18) 0.00137(17) -0.00529(17) N1 0.0191(7) 0.0137(7) 0.0201(7) -0.0003(6) 0.0005(6) -0.0032(6) N2 0.0199(7) 0.0133(7) 0.0210(7) 0.0003(6) -0.0011(6) -0.0028(6) C1 0.0272(10) 0.0300(11) 0.0284(9) -0.0072(8) 0.0049(8) -0.0163(8) C2 0.0259(10) 0.0385(12) 0.0322(10) -0.0090(9) -0.0005(8) -0.0131(9) C3 0.0305(12) 0.0681(19) 0.0381(12) -0.0175(12) -0.0008(9) -0.0232(12) C4 0.0416(14) 0.085(2) 0.0451(13) -0.0305(14) 0.0118(11) -0.0442(16) C5 0.0650(19) 0.0658(19) 0.0523(15) -0.0224(14) 0.0199(14) -0.0535(17) C6 0.0449(13) 0.0362(13) 0.0469(13) -0.0079(11) 0.0085(11) -0.0264(11) C7 0.0282(9) 0.0128(8) 0.0231(8) 0.0005(7) 0.0002(7) -0.0031(7) C8 0.0384(11) 0.0235(10) 0.0314(10) 0.0022(8) 0.0049(9) -0.0099(9) C9 0.0541(15) 0.0294(12) 0.0293(11) 0.0075(9) 0.0075(10) -0.0074(11) C10 0.0556(15) 0.0285(12) 0.0260(10) 0.0056(9) -0.0067(10) 0.0022(10) C11 0.0401(12) 0.0301(12) 0.0358(11) 0.0009(9) -0.0109(10) -0.0038(10) C12 0.0314(10) 0.0204(10) 0.0302(10) -0.0006(8) -0.0026(8) -0.0052(8) C13 0.0213(8) 0.0138(8) 0.0206(8) 0.0002(7) -0.0019(7) -0.0039(7) C14 0.0204(9) 0.0141(8) 0.0248(9) 0.0009(7) -0.0013(7) -0.0032(7) C15 0.0278(10) 0.0236(10) 0.0249(9) -0.0004(8) 0.0018(7) -0.0076(8) C16 0.0396(12) 0.0315(11) 0.0205(9) -0.0017(8) -0.0007(8) -0.0129(9) C17 0.0359(11) 0.0341(11) 0.0277(10) -0.0014(9) -0.0073(8) -0.0168(9) C18 0.0244(9) 0.0216(9) 0.0279(9) 0.0019(8) -0.0062(7) -0.0085(8) C19 0.0202(8) 0.0206(9) 0.0243(9) 0.0015(7) -0.0013(7) -0.0053(7) C20 0.0305(10) 0.0329(11) 0.0343(10) 0.0058(9) -0.0059(8) -0.0172(9) C21 0.0222(9) 0.0296(11) 0.0369(11) 0.0023(9) -0.0029(8) -0.0016(8) C22 0.0246(10) 0.0345(12) 0.0346(10) 0.0023(9) -0.0046(8) -0.0131(9) C23 0.0397(13) 0.0382(14) 0.0748(19) -0.0009(13) -0.0032(13) -0.0233(12) C24 0.0276(11) 0.0371(14) 0.0707(18) -0.0028(13) 0.0046(11) -0.0079(10) C25 0.0306(10) 0.0132(8) 0.0242(9) 0.0020(7) -0.0011(7) -0.0041(7) C26 0.0146(7) 0.0131(8) 0.0227(8) 0.0012(7) -0.0039(6) -0.0024(6) C27 0.0154(8) 0.0126(8) 0.0233(8) 0.0003(7) -0.0018(6) -0.0020(6) C28 0.0167(8) 0.0141(8) 0.0197(8) 0.0013(7) -0.0048(6) -0.0017(6) C29 0.0215(9) 0.0206(9) 0.0332(10) -0.0066(8) 0.0019(7) -0.0076(7) C30 0.0161(8) 0.0137(8) 0.0245(8) -0.0008(7) 0.0010(6) -0.0034(6) C31 0.0202(8) 0.0159(9) 0.0252(9) 0.0014(7) -0.0002(7) -0.0027(7) C32 0.0183(8) 0.0190(9) 0.0238(9) -0.0004(7) 0.0002(7) -0.0049(7) C33 0.0278(10) 0.0237(10) 0.0243(9) -0.0052(8) 0.0021(7) -0.0067(8) C34 0.0278(10) 0.0160(9) 0.0346(10) -0.0047(8) 0.0054(8) -0.0032(8) C35 0.0234(9) 0.0153(9) 0.0312(10) 0.0012(7) 0.0019(7) -0.0007(7) C36 0.0220(9) 0.0206(9) 0.0224(8) -0.0002(7) -0.0031(7) -0.0030(7) C37 0.0329(12) 0.0306(12) 0.0574(15) 0.0179(11) 0.0060(11) -0.0021(9) C38 0.0545(16) 0.0390(14) 0.0612(17) -0.0020(13) -0.0341(14) -0.0094(12) C39 0.0259(9) 0.0184(9) 0.0248(9) 0.0021(7) -0.0018(7) 0.0012(7) C40 0.0452(14) 0.0541(16) 0.0320(11) 0.0054(11) -0.0112(10) -0.0228(12) C41 0.0392(12) 0.0298(11) 0.0272(10) 0.0060(9) 0.0053(9) -0.0036(9) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 1.9700(16) . ? Ge1 Cl1 2.2934(8) . ? Ge1 P1 2.4300(11) . ? P1 C27 1.7718(18) . ? P1 C7 1.806(2) . ? P1 C1 1.813(2) . ? N1 C26 1.361(2) . ? N1 C13 1.439(2) . ? N2 C28 1.285(2) . ? N2 C30 1.419(2) . ? C1 C2 1.390(3) . ? C1 C6 1.399(3) . ? C2 C3 1.396(3) . ? C3 C4 1.375(4) . ? C4 C5 1.382(5) . ? C5 C6 1.395(4) . ? C7 C8 1.390(3) . ? C7 C12 1.403(3) . ? C8 C9 1.390(3) . ? C9 C10 1.379(4) . ? C10 C11 1.389(4) . ? C11 C12 1.385(3) . ? C13 C14 1.409(3) . ? C13 C18 1.410(3) . ? C14 C15 1.391(3) . ? C14 C19 1.522(3) . ? C15 C16 1.383(3) . ? C16 C17 1.390(3) . ? C17 C18 1.392(3) . ? C18 C22 1.525(3) . ? C19 C21 1.530(3) . ? C19 C20 1.534(3) . ? C22 C24 1.523(3) . ? C22 C23 1.540(3) . ? C25 C26 1.510(2) . ? C26 C27 1.385(3) . ? C27 C28 1.473(3) . ? C28 C29 1.518(2) . ? C30 C32 1.409(3) . ? C30 C31 1.416(2) . ? C31 C35 1.393(3) . ? C31 C39 1.520(3) . ? C32 C33 1.391(3) . ? C32 C36 1.518(3) . ? C33 C34 1.393(3) . ? C34 C35 1.381(3) . ? C36 C38 1.519(3) . ? C36 C37 1.526(3) . ? C39 C40 1.528(3) . ? C39 C41 1.530(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 Cl1 95.63(6) . . ? N1 Ge1 P1 80.49(5) . . ? Cl1 Ge1 P1 93.16(3) . . ? C27 P1 C7 111.93(9) . . ? C27 P1 C1 112.41(10) . . ? C7 P1 C1 109.88(10) . . ? C27 P1 Ge1 97.91(7) . . ? C7 P1 Ge1 119.40(7) . . ? C1 P1 Ge1 104.75(7) . . ? C26 N1 C13 121.15(15) . . ? C26 N1 Ge1 123.02(12) . . ? C13 N1 Ge1 115.29(12) . . ? C28 N2 C30 119.89(15) . . ? C2 C1 C6 119.3(2) . . ? C2 C1 P1 121.80(16) . . ? C6 C1 P1 118.72(18) . . ? C1 C2 C3 120.1(2) . . ? C4 C3 C2 120.5(3) . . ? C3 C4 C5 119.9(2) . . ? C4 C5 C6 120.5(2) . . ? C5 C6 C1 119.7(3) . . ? C8 C7 C12 119.45(19) . . ? C8 C7 P1 122.15(16) . . ? C12 C7 P1 118.29(15) . . ? C7 C8 C9 120.0(2) . . ? C10 C9 C8 120.1(2) . . ? C9 C10 C11 120.6(2) . . ? C12 C11 C10 119.6(2) . . ? C11 C12 C7 120.2(2) . . ? C14 C13 C18 121.18(17) . . ? C14 C13 N1 120.41(16) . . ? C18 C13 N1 118.40(16) . . ? C15 C14 C13 118.03(18) . . ? C15 C14 C19 119.52(17) . . ? C13 C14 C19 122.44(17) . . ? C16 C15 C14 121.53(19) . . ? C15 C16 C17 119.96(19) . . ? C16 C17 C18 120.73(19) . . ? C17 C18 C13 118.56(18) . . ? C17 C18 C22 119.54(18) . . ? C13 C18 C22 121.88(18) . . ? C14 C19 C21 110.21(17) . . ? C14 C19 C20 112.52(15) . . ? C21 C19 C20 109.83(17) . . ? C24 C22 C18 111.42(18) . . ? C24 C22 C23 110.4(2) . . ? C18 C22 C23 111.5(2) . . ? N1 C26 C27 121.52(16) . . ? N1 C26 C25 117.05(16) . . ? C27 C26 C25 121.37(17) . . ? C26 C27 C28 125.12(16) . . ? C26 C27 P1 114.08(14) . . ? C28 C27 P1 120.22(13) . . ? N2 C28 C27 117.44(16) . . ? N2 C28 C29 122.22(17) . . ? C27 C28 C29 120.27(16) . . ? C32 C30 C31 120.57(17) . . ? C32 C30 N2 119.73(16) . . ? C31 C30 N2 119.47(17) . . ? C35 C31 C30 118.27(18) . . ? C35 C31 C39 120.00(17) . . ? C30 C31 C39 121.68(17) . . ? C33 C32 C30 118.79(17) . . ? C33 C32 C36 120.65(17) . . ? C30 C32 C36 120.45(17) . . ? C32 C33 C34 121.16(19) . . ? C35 C34 C33 119.44(19) . . ? C34 C35 C31 121.74(18) . . ? C32 C36 C38 113.15(18) . . ? C32 C36 C37 109.18(16) . . ? C38 C36 C37 110.5(2) . . ? C31 C39 C40 111.18(17) . . ? C31 C39 C41 112.26(18) . . ? C40 C39 C41 109.81(18) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.04 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.211 _refine_diff_density_min -1.222 _refine_diff_density_rms 0.082