Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Cameron Jones' _publ_contact_author_address ; School of Chemistry Cardiff University Main Building Cardiff University Cardiff CF10 3AT UNITED KINGDOM ; _publ_contact_author_email JONESCA6@CARDIFF.AC.UK _publ_section_title ; Complexes of a Gallium Heterocycle with Transition Metal Sandwich, Half Sandwich and Dialkyl Fragments ; loop_ _publ_author_name 'Cameron Jones' 'S. Aldridge' 'Robert J. Baker' 'Natalie D. Coombs' 'Richard P. Rose' 'Andrea Rossin' ; D.Willock ; data_compound13 _database_code_depnum_ccdc_archive 'CCDC 603226' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H50 Ga N2 V' _chemical_formula_weight 655.46 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' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.340(3) _cell_length_b 16.734(3) _cell_length_c 15.496(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.39(3) _cell_angle_gamma 90.00 _cell_volume 3453.1(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.261 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 1.078 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.713 _exptl_absorpt_correction_T_max 0.909 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _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 18418 _diffrn_reflns_av_R_equivalents 0.0941 _diffrn_reflns_av_sigmaI/netI 0.0947 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 25.31 _reflns_number_total 6267 _reflns_number_gt 4238 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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 'calc w=1/[\s^2^(Fo^2^)+(0.0479P)^2^+3.0801P] 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 6267 _refine_ls_number_parameters 390 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0997 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.1360 _refine_ls_wR_factor_gt 0.1184 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 Ga1 Ga 0.26997(3) 0.01678(3) 0.76996(3) 0.02199(16) Uani 1 1 d . . . V1 V 0.27570(5) -0.13426(4) 0.77602(4) 0.0237(2) Uani 1 1 d . . . N1 N 0.3613(3) 0.09943(19) 0.7447(2) 0.0249(8) Uani 1 1 d . . . N2 N 0.1783(2) 0.09967(19) 0.7941(2) 0.0225(8) Uani 1 1 d . . . C1 C 0.3183(3) 0.1739(2) 0.7565(3) 0.0281(10) Uani 1 1 d . . . H1 H 0.3537 0.2220 0.7469 0.034 Uiso 1 1 calc R . . C2 C 0.2238(3) 0.1742(2) 0.7823(3) 0.0269(10) Uani 1 1 d . . . H2 H 0.1894 0.2228 0.7921 0.032 Uiso 1 1 calc R . . C3 C 0.4570(3) 0.0932(2) 0.7084(3) 0.0235(9) Uani 1 1 d . . . C4 C 0.4695(3) 0.1194(2) 0.6233(3) 0.0266(10) Uani 1 1 d . . . C5 C 0.5635(3) 0.1109(3) 0.5896(3) 0.0319(11) Uani 1 1 d . . . H5 H 0.5733 0.1296 0.5329 0.038 Uiso 1 1 calc R . . C6 C 0.6430(3) 0.0757(3) 0.6371(3) 0.0356(11) Uani 1 1 d . . . H6 H 0.7064 0.0696 0.6129 0.043 Uiso 1 1 calc R . . C7 C 0.6290(3) 0.0497(3) 0.7199(3) 0.0327(11) Uani 1 1 d . . . H7 H 0.6835 0.0255 0.7523 0.039 Uiso 1 1 calc R . . C8 C 0.5374(3) 0.0577(3) 0.7574(3) 0.0293(10) Uani 1 1 d . . . C9 C 0.3841(3) 0.1550(3) 0.5662(3) 0.0324(11) Uani 1 1 d . . . H9 H 0.3229 0.1566 0.6005 0.039 Uiso 1 1 calc R . . C10 C 0.4080(4) 0.2405(3) 0.5396(4) 0.0622(17) Uani 1 1 d . . . H10A H 0.4168 0.2741 0.5913 0.093 Uiso 1 1 calc R . . H10B H 0.3525 0.2614 0.5018 0.093 Uiso 1 1 calc R . . H10C H 0.4699 0.2408 0.5085 0.093 Uiso 1 1 calc R . . C11 C 0.3606(4) 0.1024(4) 0.4871(3) 0.0601(16) Uani 1 1 d . . . H11A H 0.4197 0.0997 0.4525 0.090 Uiso 1 1 calc R . . H11B H 0.3041 0.1253 0.4522 0.090 Uiso 1 1 calc R . . H11C H 0.3431 0.0486 0.5059 0.090 Uiso 1 1 calc R . . C12 C 0.5283(4) 0.0335(3) 0.8520(3) 0.0380(12) Uani 1 1 d . . . H12 H 0.4617 0.0068 0.8564 0.046 Uiso 1 1 calc R . . C13 C 0.6090(4) -0.0245(3) 0.8867(4) 0.0519(14) Uani 1 1 d . . . H13A H 0.6067 -0.0731 0.8514 0.078 Uiso 1 1 calc R . . H13B H 0.5971 -0.0382 0.9467 0.078 Uiso 1 1 calc R . . H13C H 0.6752 0.0006 0.8844 0.078 Uiso 1 1 calc R . . C14 C 0.5286(4) 0.1094(3) 0.9084(3) 0.0490(14) Uani 1 1 d . . . H14A H 0.5234 0.0943 0.9690 0.073 Uiso 1 1 calc R . . H14B H 0.4715 0.1432 0.8897 0.073 Uiso 1 1 calc R . . H14C H 0.5913 0.1388 0.9022 0.073 Uiso 1 1 calc R . . C15 C 0.0785(3) 0.0987(2) 0.8203(2) 0.0205(9) Uani 1 1 d . . . C16 C 0.0554(3) 0.1306(2) 0.9009(3) 0.0238(9) Uani 1 1 d . . . C17 C -0.0446(3) 0.1312(2) 0.9236(3) 0.0280(10) Uani 1 1 d . . . H17 H -0.0608 0.1540 0.9772 0.034 Uiso 1 1 calc R . . C18 C -0.1200(3) 0.0992(3) 0.8694(3) 0.0325(11) Uani 1 1 d . . . H18 H -0.1877 0.1004 0.8852 0.039 Uiso 1 1 calc R . . C19 C -0.0965(3) 0.0655(3) 0.7922(3) 0.0308(10) Uani 1 1 d . . . H19 H -0.1489 0.0428 0.7558 0.037 Uiso 1 1 calc R . . C20 C 0.0009(3) 0.0634(2) 0.7656(3) 0.0245(9) Uani 1 1 d . . . C21 C 0.1353(3) 0.1616(3) 0.9659(3) 0.0333(11) Uani 1 1 d . . . H21 H 0.2019 0.1560 0.9402 0.040 Uiso 1 1 calc R . . C22 C 0.1378(4) 0.1119(4) 1.0492(3) 0.0520(14) Uani 1 1 d . . . H22A H 0.0731 0.1164 1.0756 0.078 Uiso 1 1 calc R . . H22B H 0.1914 0.1317 1.0896 0.078 Uiso 1 1 calc R . . H22C H 0.1506 0.0558 1.0355 0.078 Uiso 1 1 calc R . . C23 C 0.1191(4) 0.2496(3) 0.9854(4) 0.0519(14) Uani 1 1 d . . . H23A H 0.1225 0.2807 0.9321 0.078 Uiso 1 1 calc R . . H23B H 0.1714 0.2679 1.0279 0.078 Uiso 1 1 calc R . . H23C H 0.0531 0.2568 1.0088 0.078 Uiso 1 1 calc R . . C24 C 0.0237(3) 0.0282(3) 0.6792(3) 0.0346(11) Uani 1 1 d . . . H24 H 0.0846 -0.0062 0.6889 0.041 Uiso 1 1 calc R . . C25 C -0.0602(4) -0.0249(3) 0.6389(3) 0.0478(13) Uani 1 1 d . . . H25A H -0.0825 -0.0623 0.6825 0.072 Uiso 1 1 calc R . . H25B H -0.0350 -0.0549 0.5904 0.072 Uiso 1 1 calc R . . H25C H -0.1169 0.0086 0.6180 0.072 Uiso 1 1 calc R . . C26 C 0.0499(4) 0.0934(3) 0.6154(3) 0.0542(15) Uani 1 1 d . . . H26A H -0.0085 0.1282 0.6037 0.081 Uiso 1 1 calc R . . H26B H 0.0687 0.0688 0.5613 0.081 Uiso 1 1 calc R . . H26C H 0.1063 0.1252 0.6401 0.081 Uiso 1 1 calc R . . C27 C 0.2781(4) -0.1538(3) 0.6296(3) 0.0355(11) Uani 1 1 d . . . C28 C 0.3595(4) -0.1022(3) 0.6556(3) 0.0378(12) Uani 1 1 d . . . H28 H 0.3678 -0.0486 0.6371 0.045 Uiso 1 1 calc R . . C29 C 0.4255(4) -0.1444(3) 0.7137(3) 0.0461(13) Uani 1 1 d . . . H29 H 0.4861 -0.1244 0.7409 0.055 Uiso 1 1 calc R . . C30 C 0.3856(4) -0.2211(3) 0.7243(3) 0.0432(13) Uani 1 1 d . . . H30 H 0.4144 -0.2623 0.7599 0.052 Uiso 1 1 calc R . . C31 C 0.2952(4) -0.2262(3) 0.6726(3) 0.0366(12) Uani 1 1 d . . . H31 H 0.2527 -0.2717 0.6679 0.044 Uiso 1 1 calc R . . C32 C 0.1924(4) -0.1349(4) 0.5664(3) 0.0590(16) Uani 1 1 d . . . H32A H 0.2046 -0.1589 0.5103 0.089 Uiso 1 1 calc R . . H32B H 0.1862 -0.0768 0.5599 0.089 Uiso 1 1 calc R . . H32C H 0.1301 -0.1566 0.5875 0.089 Uiso 1 1 calc R . . C33 C 0.1309(3) -0.1851(3) 0.8276(3) 0.0282(10) Uani 1 1 d . . . C34 C 0.1474(3) -0.1087(3) 0.8641(3) 0.0326(11) Uani 1 1 d . . . H34 H 0.1046 -0.0637 0.8556 0.039 Uiso 1 1 calc R . . C35 C 0.2392(4) -0.1105(3) 0.9159(3) 0.0377(12) Uani 1 1 d . . . H35 H 0.2683 -0.0671 0.9480 0.045 Uiso 1 1 calc R . . C36 C 0.2788(4) -0.1876(3) 0.9112(3) 0.0421(12) Uani 1 1 d . . . H36 H 0.3392 -0.2063 0.9399 0.051 Uiso 1 1 calc R . . C37 C 0.2126(4) -0.2325(3) 0.8561(3) 0.0354(11) Uani 1 1 d . . . H37 H 0.2221 -0.2868 0.8406 0.043 Uiso 1 1 calc R . . C38 C 0.0420(4) -0.2107(3) 0.7701(3) 0.0447(13) Uani 1 1 d . . . H38A H 0.0621 -0.2537 0.7318 0.067 Uiso 1 1 calc R . . H38B H 0.0172 -0.1651 0.7353 0.067 Uiso 1 1 calc R . . H38C H -0.0113 -0.2299 0.8057 0.067 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 Ga1 0.0207(3) 0.0172(3) 0.0287(3) -0.0025(2) 0.00671(18) -0.0010(2) V1 0.0271(4) 0.0179(4) 0.0267(4) -0.0023(3) 0.0047(3) -0.0010(3) N1 0.026(2) 0.0132(17) 0.037(2) -0.0037(16) 0.0098(16) -0.0039(15) N2 0.023(2) 0.0159(18) 0.0295(19) -0.0027(15) 0.0051(15) 0.0040(14) C1 0.026(2) 0.019(2) 0.041(3) -0.004(2) 0.0103(19) -0.0037(19) C2 0.026(2) 0.015(2) 0.040(3) -0.005(2) 0.0075(19) -0.0022(19) C3 0.018(2) 0.017(2) 0.036(2) -0.0054(19) 0.0064(18) -0.0044(17) C4 0.026(2) 0.020(2) 0.035(2) -0.0035(19) 0.0068(19) -0.0038(18) C5 0.031(3) 0.031(3) 0.035(2) -0.008(2) 0.011(2) -0.006(2) C6 0.021(2) 0.039(3) 0.048(3) -0.010(2) 0.014(2) -0.005(2) C7 0.024(2) 0.027(2) 0.047(3) -0.005(2) -0.001(2) -0.0030(19) C8 0.024(2) 0.020(2) 0.045(3) -0.004(2) 0.0078(19) -0.0094(19) C9 0.029(3) 0.032(3) 0.036(3) -0.002(2) 0.0024(19) -0.004(2) C10 0.055(4) 0.044(3) 0.085(4) 0.026(3) -0.010(3) -0.004(3) C11 0.061(4) 0.068(4) 0.050(3) -0.016(3) -0.013(3) 0.005(3) C12 0.034(3) 0.037(3) 0.043(3) 0.012(2) 0.001(2) -0.008(2) C13 0.039(3) 0.052(3) 0.063(3) 0.021(3) -0.009(3) -0.008(3) C14 0.060(4) 0.055(3) 0.032(3) 0.005(3) 0.006(2) -0.007(3) C15 0.018(2) 0.019(2) 0.025(2) 0.0017(18) 0.0030(17) 0.0038(17) C16 0.025(2) 0.021(2) 0.026(2) 0.0020(19) 0.0015(17) 0.0039(18) C17 0.030(3) 0.023(2) 0.032(2) 0.003(2) 0.0121(19) 0.0069(19) C18 0.021(2) 0.029(3) 0.048(3) 0.006(2) 0.008(2) 0.0011(19) C19 0.025(2) 0.028(2) 0.039(3) 0.008(2) -0.0028(19) -0.004(2) C20 0.023(2) 0.019(2) 0.031(2) 0.0078(19) 0.0002(17) 0.0005(18) C21 0.029(3) 0.038(3) 0.033(2) -0.007(2) 0.0002(19) 0.004(2) C22 0.048(4) 0.065(4) 0.042(3) 0.005(3) -0.005(2) 0.008(3) C23 0.053(4) 0.039(3) 0.063(3) -0.026(3) -0.007(3) 0.004(3) C24 0.035(3) 0.039(3) 0.029(2) -0.001(2) -0.0046(19) 0.002(2) C25 0.051(3) 0.045(3) 0.045(3) -0.013(3) -0.013(2) 0.002(3) C26 0.079(4) 0.057(4) 0.027(3) 0.001(3) 0.005(3) 0.004(3) C27 0.044(3) 0.035(3) 0.029(2) -0.013(2) 0.013(2) 0.002(2) C28 0.050(3) 0.021(2) 0.045(3) -0.005(2) 0.026(2) -0.005(2) C29 0.028(3) 0.049(3) 0.063(3) -0.018(3) 0.010(2) 0.000(2) C30 0.038(3) 0.037(3) 0.056(3) -0.005(3) 0.008(2) 0.016(2) C31 0.041(3) 0.027(3) 0.043(3) -0.015(2) 0.014(2) -0.002(2) C32 0.068(4) 0.080(4) 0.030(3) -0.008(3) 0.000(3) 0.018(3) C33 0.037(3) 0.023(2) 0.026(2) 0.0010(19) 0.0105(19) -0.008(2) C34 0.043(3) 0.026(2) 0.030(2) 0.006(2) 0.014(2) -0.003(2) C35 0.048(3) 0.041(3) 0.024(2) 0.000(2) 0.004(2) -0.011(2) C36 0.048(3) 0.047(3) 0.031(3) 0.011(2) -0.005(2) 0.004(3) C37 0.048(3) 0.021(2) 0.038(3) 0.003(2) 0.008(2) 0.004(2) C38 0.038(3) 0.047(3) 0.050(3) 0.002(3) 0.011(2) -0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 N1 1.899(3) . ? Ga1 N2 1.901(3) . ? Ga1 V1 2.5303(9) . ? V1 C30 2.246(5) . ? V1 C31 2.248(4) . ? V1 C37 2.253(4) . ? V1 C36 2.275(4) . ? V1 C29 2.276(5) . ? V1 C35 2.285(4) . ? V1 C34 2.292(4) . ? V1 C28 2.294(4) . ? V1 C27 2.295(4) . ? V1 C33 2.297(4) . ? N1 C1 1.389(5) . ? N1 C3 1.428(5) . ? N2 C2 1.404(5) . ? N2 C15 1.416(5) . ? C1 C2 1.344(5) . ? C3 C8 1.408(6) . ? C3 C4 1.410(6) . ? C4 C5 1.393(6) . ? C4 C9 1.522(6) . ? C5 C6 1.386(6) . ? C6 C7 1.378(6) . ? C7 C8 1.390(6) . ? C8 C12 1.533(6) . ? C9 C11 1.526(7) . ? C9 C10 1.528(6) . ? C12 C13 1.524(7) . ? C12 C14 1.540(7) . ? C15 C16 1.410(5) . ? C15 C20 1.426(6) . ? C16 C17 1.399(6) . ? C16 C21 1.514(6) . ? C17 C18 1.381(6) . ? C18 C19 1.375(6) . ? C19 C20 1.387(6) . ? C20 C24 1.511(6) . ? C21 C23 1.521(6) . ? C21 C22 1.533(7) . ? C24 C26 1.527(7) . ? C24 C25 1.534(6) . ? C27 C31 1.395(6) . ? C27 C28 1.427(7) . ? C27 C32 1.495(7) . ? C28 C29 1.410(7) . ? C29 C30 1.403(7) . ? C30 C31 1.410(7) . ? C33 C37 1.398(6) . ? C33 C34 1.410(6) . ? C33 C38 1.504(6) . ? C34 C35 1.425(6) . ? C35 C36 1.397(7) . ? C36 C37 1.409(6) . ? 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 Ga1 N2 86.39(14) . . ? N1 Ga1 V1 135.78(10) . . ? N2 Ga1 V1 137.74(10) . . ? C30 V1 C31 36.58(17) . . ? C30 V1 C37 89.86(18) . . ? C31 V1 C37 87.48(17) . . ? C30 V1 C36 95.66(19) . . ? C31 V1 C36 113.05(18) . . ? C37 V1 C36 36.24(17) . . ? C30 V1 C29 36.15(17) . . ? C31 V1 C29 60.34(18) . . ? C37 V1 C29 123.05(19) . . ? C36 V1 C29 113.1(2) . . ? C30 V1 C35 129.17(19) . . ? C31 V1 C35 146.69(18) . . ? C37 V1 C35 59.77(17) . . ? C36 V1 C35 35.67(17) . . ? C29 V1 C35 131.08(19) . . ? C30 V1 C34 149.28(18) . . ? C31 V1 C34 132.40(17) . . ? C37 V1 C34 59.43(16) . . ? C36 V1 C34 59.87(17) . . ? C29 V1 C34 166.35(18) . . ? C35 V1 C34 36.28(16) . . ? C30 V1 C28 60.09(18) . . ? C31 V1 C28 59.86(17) . . ? C37 V1 C28 146.56(17) . . ? C36 V1 C28 149.02(19) . . ? C29 V1 C28 35.94(18) . . ? C35 V1 C28 150.72(17) . . ? C34 V1 C28 149.05(17) . . ? C30 V1 C27 60.47(18) . . ? C31 V1 C27 35.76(16) . . ? C37 V1 C27 117.94(17) . . ? C36 V1 C27 148.67(19) . . ? C29 V1 C27 60.39(18) . . ? C35 V1 C27 168.34(18) . . ? C34 V1 C27 132.08(17) . . ? C28 V1 C27 36.22(17) . . ? C30 V1 C33 117.67(18) . . ? C31 V1 C33 97.45(16) . . ? C37 V1 C33 35.76(16) . . ? C36 V1 C33 60.25(17) . . ? C29 V1 C33 153.80(18) . . ? C35 V1 C33 60.22(16) . . ? C34 V1 C33 35.79(15) . . ? C28 V1 C33 146.08(17) . . ? C27 V1 C33 110.66(16) . . ? C30 V1 Ga1 130.70(14) . . ? C31 V1 Ga1 131.44(13) . . ? C37 V1 Ga1 137.56(12) . . ? C36 V1 Ga1 115.13(13) . . ? C29 V1 Ga1 94.81(14) . . ? C35 V1 Ga1 81.60(13) . . ? C34 V1 Ga1 79.27(11) . . ? C28 V1 Ga1 75.60(12) . . ? C27 V1 Ga1 96.18(12) . . ? C33 V1 Ga1 111.03(11) . . ? C1 N1 C3 120.2(3) . . ? C1 N1 Ga1 110.6(3) . . ? C3 N1 Ga1 128.8(3) . . ? C2 N2 C15 118.0(3) . . ? C2 N2 Ga1 109.6(3) . . ? C15 N2 Ga1 132.4(3) . . ? C2 C1 N1 116.4(4) . . ? C1 C2 N2 117.1(4) . . ? C8 C3 C4 120.4(4) . . ? C8 C3 N1 119.3(4) . . ? C4 C3 N1 120.2(4) . . ? C5 C4 C3 118.5(4) . . ? C5 C4 C9 118.8(4) . . ? C3 C4 C9 122.6(4) . . ? C6 C5 C4 121.5(4) . . ? C7 C6 C5 119.1(4) . . ? C6 C7 C8 122.0(4) . . ? C7 C8 C3 118.4(4) . . ? C7 C8 C12 119.7(4) . . ? C3 C8 C12 121.7(4) . . ? C4 C9 C11 110.6(4) . . ? C4 C9 C10 111.3(4) . . ? C11 C9 C10 111.0(4) . . ? C13 C12 C8 114.3(4) . . ? C13 C12 C14 110.3(4) . . ? C8 C12 C14 109.1(4) . . ? C16 C15 N2 120.5(3) . . ? C16 C15 C20 119.7(4) . . ? N2 C15 C20 119.8(3) . . ? C17 C16 C15 119.1(4) . . ? C17 C16 C21 118.3(4) . . ? C15 C16 C21 122.5(4) . . ? C18 C17 C16 121.0(4) . . ? C19 C18 C17 119.6(4) . . ? C18 C19 C20 122.3(4) . . ? C19 C20 C15 118.2(4) . . ? C19 C20 C24 121.0(4) . . ? C15 C20 C24 120.7(4) . . ? C16 C21 C23 111.2(4) . . ? C16 C21 C22 110.7(4) . . ? C23 C21 C22 110.7(4) . . ? C20 C24 C26 111.2(4) . . ? C20 C24 C25 114.0(4) . . ? C26 C24 C25 109.9(4) . . ? C31 C27 C28 106.9(4) . . ? C31 C27 C32 126.4(5) . . ? C28 C27 C32 126.7(5) . . ? C31 C27 V1 70.3(2) . . ? C28 C27 V1 71.9(2) . . ? C32 C27 V1 124.2(3) . . ? C29 C28 C27 108.3(4) . . ? C29 C28 V1 71.3(3) . . ? C27 C28 V1 71.9(2) . . ? C30 C29 C28 107.8(5) . . ? C30 C29 V1 70.8(3) . . ? C28 C29 V1 72.7(3) . . ? C29 C30 C31 107.8(5) . . ? C29 C30 V1 73.1(3) . . ? C31 C30 V1 71.8(3) . . ? C27 C31 C30 109.2(4) . . ? C27 C31 V1 74.0(2) . . ? C30 C31 V1 71.6(3) . . ? C37 C33 C34 106.7(4) . . ? C37 C33 C38 126.8(4) . . ? C34 C33 C38 126.5(4) . . ? C37 C33 V1 70.4(3) . . ? C34 C33 V1 71.9(2) . . ? C38 C33 V1 123.3(3) . . ? C33 C34 C35 108.4(4) . . ? C33 C34 V1 72.3(2) . . ? C35 C34 V1 71.6(3) . . ? C36 C35 C34 107.8(4) . . ? C36 C35 V1 71.8(3) . . ? C34 C35 V1 72.1(3) . . ? C35 C36 C37 107.4(4) . . ? C35 C36 V1 72.5(3) . . ? C37 C36 V1 71.0(3) . . ? C33 C37 C36 109.7(4) . . ? C33 C37 V1 73.9(2) . . ? C36 C37 V1 72.8(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.31 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.665 _refine_diff_density_min -0.505 _refine_diff_density_rms 0.085 # Attachment 'cmpd14.cif' data_compound14 _database_code_depnum_ccdc_archive 'CCDC 603227' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H50 Cr Ga N2' _chemical_formula_weight 656.52 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.338(3) _cell_length_b 16.529(3) _cell_length_c 15.433(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.67(3) _cell_angle_gamma 90.00 _cell_volume 3401.0(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.282 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1388 _exptl_absorpt_coefficient_mu 1.139 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.794 _exptl_absorpt_correction_T_max 0.924 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _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 22448 _diffrn_reflns_av_R_equivalents 0.1574 _diffrn_reflns_av_sigmaI/netI 0.1426 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 25.02 _reflns_number_total 5978 _reflns_number_gt 3535 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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 'calc w=1/[\s^2^(Fo^2^)+(0.0640P)^2^+0.6320P] 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 5978 _refine_ls_number_parameters 389 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1363 _refine_ls_R_factor_gt 0.0696 _refine_ls_wR_factor_ref 0.1627 _refine_ls_wR_factor_gt 0.1369 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 Ga1 Ga 0.26776(4) 0.01393(3) 0.76566(5) 0.0222(2) Uani 1 1 d . . . Cr1 Cr 0.27454(6) -0.13245(5) 0.77206(7) 0.0260(3) Uani 1 1 d . . . N1 N 0.3597(3) 0.0975(3) 0.7407(3) 0.0262(12) Uani 1 1 d . . . N2 N 0.1747(3) 0.0972(3) 0.7909(3) 0.0208(11) Uani 1 1 d . . . C1 C 0.3161(4) 0.1730(3) 0.7522(4) 0.0296(15) Uani 1 1 d . . . H1 H 0.3515 0.2218 0.7421 0.036 Uiso 1 1 calc R . . C2 C 0.2201(4) 0.1730(3) 0.7787(4) 0.0272(15) Uani 1 1 d . . . H2 H 0.1850 0.2220 0.7886 0.033 Uiso 1 1 calc R . . C3 C 0.4553(4) 0.0943(3) 0.7014(4) 0.0222(13) Uani 1 1 d . . . C4 C 0.4692(4) 0.1220(3) 0.6167(4) 0.0273(15) Uani 1 1 d . . . C5 C 0.5639(4) 0.1177(3) 0.5816(4) 0.0339(16) Uani 1 1 d . . . H5 H 0.5740 0.1388 0.5253 0.041 Uiso 1 1 calc R . . C6 C 0.6434(4) 0.0830(3) 0.6274(5) 0.0359(17) Uani 1 1 d . . . H6 H 0.7075 0.0797 0.6023 0.043 Uiso 1 1 calc R . . C7 C 0.6295(4) 0.0534(4) 0.7095(5) 0.0350(16) Uani 1 1 d . . . H7 H 0.6839 0.0279 0.7397 0.042 Uiso 1 1 calc R . . C8 C 0.5372(4) 0.0598(3) 0.7496(4) 0.0287(15) Uani 1 1 d . . . C9 C 0.3841(4) 0.1570(4) 0.5617(4) 0.0341(16) Uani 1 1 d . . . H9 H 0.3214 0.1543 0.5956 0.041 Uiso 1 1 calc R . . C10 C 0.4042(5) 0.2460(4) 0.5397(5) 0.058(2) Uani 1 1 d . . . H10A H 0.4111 0.2774 0.5934 0.087 Uiso 1 1 calc R . . H10B H 0.3481 0.2674 0.5042 0.087 Uiso 1 1 calc R . . H10C H 0.4662 0.2501 0.5075 0.087 Uiso 1 1 calc R . . C11 C 0.3671(6) 0.1091(5) 0.4783(5) 0.063(2) Uani 1 1 d . . . H11A H 0.4277 0.1110 0.4441 0.094 Uiso 1 1 calc R . . H11B H 0.3108 0.1326 0.4447 0.094 Uiso 1 1 calc R . . H11C H 0.3517 0.0527 0.4925 0.094 Uiso 1 1 calc R . . C12 C 0.5273(4) 0.0330(4) 0.8436(5) 0.0361(17) Uani 1 1 d . . . H12 H 0.4607 0.0058 0.8480 0.043 Uiso 1 1 calc R . . C13 C 0.6068(5) -0.0272(4) 0.8752(5) 0.054(2) Uani 1 1 d . . . H13A H 0.6099 -0.0724 0.8342 0.081 Uiso 1 1 calc R . . H13B H 0.5894 -0.0477 0.9324 0.081 Uiso 1 1 calc R . . H13C H 0.6722 -0.0003 0.8792 0.081 Uiso 1 1 calc R . . C14 C 0.5257(5) 0.1068(4) 0.9016(5) 0.0495(19) Uani 1 1 d . . . H14A H 0.5186 0.0898 0.9619 0.074 Uiso 1 1 calc R . . H14B H 0.4690 0.1415 0.8842 0.074 Uiso 1 1 calc R . . H14C H 0.5885 0.1370 0.8962 0.074 Uiso 1 1 calc R . . C15 C 0.0741(4) 0.0968(3) 0.8202(4) 0.0224(14) Uani 1 1 d . . . C16 C 0.0530(4) 0.1295(3) 0.9010(4) 0.0230(14) Uani 1 1 d . . . C17 C -0.0477(4) 0.1321(3) 0.9262(4) 0.0287(15) Uani 1 1 d . . . H17 H -0.0635 0.1557 0.9803 0.034 Uiso 1 1 calc R . . C18 C -0.1223(4) 0.1014(3) 0.8742(5) 0.0359(17) Uani 1 1 d . . . H18 H -0.1900 0.1049 0.8914 0.043 Uiso 1 1 calc R . . C19 C -0.1005(4) 0.0655(3) 0.7973(5) 0.0334(16) Uani 1 1 d . . . H19 H -0.1534 0.0420 0.7633 0.040 Uiso 1 1 calc R . . C20 C -0.0026(4) 0.0622(3) 0.7667(4) 0.0264(14) Uani 1 1 d . . . C21 C 0.1335(4) 0.1606(3) 0.9640(4) 0.0334(16) Uani 1 1 d . . . H21 H 0.1998 0.1552 0.9360 0.040 Uiso 1 1 calc R . . C22 C 0.1358(5) 0.1086(4) 1.0461(5) 0.0481(19) Uani 1 1 d . . . H22A H 0.0693 0.1085 1.0714 0.072 Uiso 1 1 calc R . . H22B H 0.1850 0.1308 1.0881 0.072 Uiso 1 1 calc R . . H22C H 0.1547 0.0530 1.0314 0.072 Uiso 1 1 calc R . . C23 C 0.1183(5) 0.2502(4) 0.9872(5) 0.049(2) Uani 1 1 d . . . H23A H 0.1235 0.2833 0.9348 0.074 Uiso 1 1 calc R . . H23B H 0.1700 0.2669 1.0300 0.074 Uiso 1 1 calc R . . H23C H 0.0518 0.2575 1.0115 0.074 Uiso 1 1 calc R . . C24 C 0.0195(4) 0.0244(4) 0.6805(4) 0.0337(15) Uani 1 1 d . . . H24 H 0.0795 -0.0112 0.6896 0.040 Uiso 1 1 calc R . . C25 C -0.0653(5) -0.0284(4) 0.6434(5) 0.049(2) Uani 1 1 d . . . H25A H -0.0812 -0.0707 0.6853 0.074 Uiso 1 1 calc R . . H25B H -0.0442 -0.0535 0.5893 0.074 Uiso 1 1 calc R . . H25C H -0.1248 0.0050 0.6318 0.074 Uiso 1 1 calc R . . C26 C 0.0473(6) 0.0888(4) 0.6138(5) 0.054(2) Uani 1 1 d . . . H26A H -0.0104 0.1244 0.6023 0.081 Uiso 1 1 calc R . . H26B H 0.0662 0.0624 0.5599 0.081 Uiso 1 1 calc R . . H26C H 0.1039 0.1209 0.6367 0.081 Uiso 1 1 calc R . . C27 C 0.2680(4) -0.1541(4) 0.6301(4) 0.0367(17) Uani 1 1 d . . . C28 C 0.3414(5) -0.0949(4) 0.6488(5) 0.0409(19) Uani 1 1 d . . . H28 H 0.3405 -0.0410 0.6272 0.049 Uiso 1 1 calc R . . C29 C 0.4153(5) -0.1272(4) 0.7036(5) 0.049(2) Uani 1 1 d . . . H29 H 0.4740 -0.1000 0.7243 0.059 Uiso 1 1 calc R . . C30 C 0.3881(5) -0.2082(4) 0.7236(5) 0.049(2) Uani 1 1 d . . . H30 H 0.4235 -0.2445 0.7611 0.059 Uiso 1 1 calc R . . C31 C 0.2974(4) -0.2237(4) 0.6762(4) 0.0376(17) Uani 1 1 d . . . H31 H 0.2621 -0.2736 0.6757 0.045 Uiso 1 1 calc R . . C32 C 0.1785(5) -0.1462(5) 0.5698(5) 0.056(2) Uani 1 1 d . . . H32A H 0.1950 -0.1672 0.5126 0.084 Uiso 1 1 calc R . . H32B H 0.1595 -0.0890 0.5647 0.084 Uiso 1 1 calc R . . H32C H 0.1224 -0.1771 0.5927 0.084 Uiso 1 1 calc R . . C33 C 0.1350(4) -0.1804(3) 0.8289(4) 0.0262(14) Uani 1 1 d . . . C34 C 0.1540(4) -0.1007(3) 0.8586(4) 0.0279(15) Uani 1 1 d . . . H34 H 0.1116 -0.0553 0.8487 0.033 Uiso 1 1 calc R . . C35 C 0.2480(4) -0.1001(4) 0.9063(4) 0.0350(16) Uani 1 1 d . . . H35 H 0.2783 -0.0549 0.9347 0.042 Uiso 1 1 calc R . . C36 C 0.2873(5) -0.1801(4) 0.9031(4) 0.0426(18) Uani 1 1 d . . . H36 H 0.3490 -0.1982 0.9286 0.051 Uiso 1 1 calc R . . C37 C 0.2181(5) -0.2271(4) 0.8552(5) 0.0398(18) Uani 1 1 d . . . H37 H 0.2263 -0.2829 0.8424 0.048 Uiso 1 1 calc R . . C38 C 0.0450(4) -0.2094(4) 0.7755(5) 0.0435(19) Uani 1 1 d . . . H38A H 0.0648 -0.2545 0.7385 0.065 Uiso 1 1 calc R . . H38B H 0.0192 -0.1650 0.7391 0.065 Uiso 1 1 calc R . . H38C H -0.0075 -0.2274 0.8142 0.065 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 Ga1 0.0180(3) 0.0159(3) 0.0332(4) -0.0025(3) 0.0092(3) -0.0017(3) Cr1 0.0228(5) 0.0168(5) 0.0391(7) -0.0040(5) 0.0108(4) -0.0013(4) N1 0.019(2) 0.019(2) 0.042(3) -0.003(2) 0.011(2) -0.005(2) N2 0.015(2) 0.017(2) 0.032(3) -0.001(2) 0.010(2) 0.0026(19) C1 0.027(3) 0.013(3) 0.050(5) -0.004(3) 0.011(3) -0.005(2) C2 0.026(3) 0.013(3) 0.044(4) -0.002(3) 0.013(3) -0.001(2) C3 0.018(3) 0.016(3) 0.033(4) -0.004(3) 0.003(3) -0.002(2) C4 0.024(3) 0.016(3) 0.043(4) -0.004(3) 0.010(3) -0.007(2) C5 0.039(4) 0.027(3) 0.036(4) -0.003(3) 0.019(3) -0.005(3) C6 0.027(3) 0.029(4) 0.053(5) -0.010(3) 0.018(3) -0.005(3) C7 0.016(3) 0.027(3) 0.062(5) -0.007(4) 0.004(3) -0.001(3) C8 0.029(3) 0.016(3) 0.042(4) -0.009(3) 0.008(3) -0.008(3) C9 0.030(3) 0.031(4) 0.042(4) -0.001(3) 0.011(3) -0.005(3) C10 0.054(5) 0.032(4) 0.086(7) 0.024(4) -0.010(4) -0.005(3) C11 0.069(5) 0.065(5) 0.054(6) -0.012(5) -0.001(4) 0.007(4) C12 0.031(3) 0.028(4) 0.050(5) 0.011(3) 0.008(3) -0.008(3) C13 0.040(4) 0.055(5) 0.067(6) 0.021(4) -0.003(4) -0.006(3) C14 0.061(5) 0.048(4) 0.040(5) 0.003(4) 0.013(4) -0.003(4) C15 0.016(3) 0.018(3) 0.034(4) 0.009(3) 0.007(3) 0.003(2) C16 0.024(3) 0.014(3) 0.031(4) 0.006(3) 0.004(3) -0.001(2) C17 0.026(3) 0.027(3) 0.034(4) 0.005(3) 0.017(3) 0.005(3) C18 0.020(3) 0.020(3) 0.069(5) 0.008(3) 0.010(3) 0.004(3) C19 0.018(3) 0.022(3) 0.059(5) 0.008(3) 0.002(3) -0.002(3) C20 0.027(3) 0.014(3) 0.038(4) 0.001(3) -0.001(3) 0.002(3) C21 0.033(3) 0.027(3) 0.041(4) -0.008(3) 0.006(3) 0.007(3) C22 0.045(4) 0.059(5) 0.040(5) 0.000(4) -0.005(4) 0.009(4) C23 0.056(4) 0.029(4) 0.062(6) -0.020(4) -0.006(4) 0.004(3) C24 0.032(3) 0.030(3) 0.039(4) 0.001(3) -0.005(3) -0.003(3) C25 0.052(4) 0.040(4) 0.056(6) -0.009(4) -0.016(4) 0.003(3) C26 0.081(5) 0.048(5) 0.033(5) 0.006(4) 0.009(4) 0.009(4) C27 0.035(3) 0.035(4) 0.041(5) -0.017(3) 0.015(3) -0.001(3) C28 0.051(4) 0.022(3) 0.052(5) -0.011(3) 0.032(4) -0.006(3) C29 0.024(3) 0.053(5) 0.071(6) -0.028(4) 0.016(4) -0.012(3) C30 0.034(4) 0.029(4) 0.085(6) -0.016(4) 0.014(4) 0.005(3) C31 0.038(4) 0.023(3) 0.053(5) -0.013(3) 0.021(3) -0.004(3) C32 0.070(5) 0.058(5) 0.040(5) -0.010(4) 0.011(4) 0.003(4) C33 0.032(3) 0.019(3) 0.028(4) 0.003(3) 0.013(3) -0.006(3) C34 0.038(3) 0.020(3) 0.027(4) 0.007(3) 0.011(3) 0.007(3) C35 0.037(4) 0.030(3) 0.039(4) 0.000(3) 0.003(3) -0.006(3) C36 0.038(4) 0.049(4) 0.040(5) 0.010(4) -0.009(3) 0.005(3) C37 0.045(4) 0.022(3) 0.053(5) 0.013(3) 0.015(4) 0.008(3) C38 0.030(3) 0.037(4) 0.064(5) -0.003(4) 0.014(3) -0.011(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 Ga1 N1 1.894(4) . ? Ga1 N2 1.901(4) . ? Ga1 Cr1 2.4231(11) . ? Cr1 C30 2.119(6) . ? Cr1 C31 2.141(6) . ? Cr1 C37 2.172(6) . ? Cr1 C36 2.172(7) . ? Cr1 C35 2.179(7) . ? Cr1 C29 2.183(6) . ? Cr1 C34 2.185(5) . ? Cr1 C28 2.214(6) . ? Cr1 C27 2.218(7) . ? Cr1 C33 2.226(5) . ? N1 C1 1.391(7) . ? N1 C3 1.429(6) . ? N2 C2 1.406(6) . ? N2 C15 1.428(6) . ? C1 C2 1.355(7) . ? C3 C4 1.401(8) . ? C3 C8 1.423(8) . ? C4 C5 1.391(7) . ? C4 C9 1.513(8) . ? C5 C6 1.382(9) . ? C6 C7 1.376(9) . ? C7 C8 1.397(7) . ? C8 C12 1.527(9) . ? C9 C11 1.523(9) . ? C9 C10 1.535(8) . ? C12 C14 1.514(9) . ? C12 C13 1.523(9) . ? C15 C16 1.395(8) . ? C15 C20 1.416(8) . ? C16 C17 1.410(7) . ? C16 C21 1.517(8) . ? C17 C18 1.359(9) . ? C18 C19 1.366(9) . ? C19 C20 1.402(7) . ? C20 C24 1.507(8) . ? C21 C22 1.531(9) . ? C21 C23 1.539(8) . ? C24 C25 1.527(8) . ? C24 C26 1.533(9) . ? C27 C31 1.403(9) . ? C27 C28 1.408(8) . ? C27 C32 1.499(9) . ? C28 C29 1.387(10) . ? C29 C30 1.423(9) . ? C30 C31 1.419(9) . ? C33 C37 1.400(8) . ? C33 C34 1.415(8) . ? C33 C38 1.515(8) . ? C34 C35 1.435(8) . ? C35 C36 1.424(8) . ? C36 C37 1.401(9) . ? 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 Ga1 N2 86.81(17) . . ? N1 Ga1 Cr1 135.46(13) . . ? N2 Ga1 Cr1 137.58(13) . . ? C30 Cr1 C31 38.9(2) . . ? C30 Cr1 C37 92.7(3) . . ? C31 Cr1 C37 87.7(2) . . ? C30 Cr1 C36 94.4(3) . . ? C31 Cr1 C36 112.3(3) . . ? C37 Cr1 C36 37.6(2) . . ? C30 Cr1 C35 128.2(3) . . ? C31 Cr1 C35 149.4(2) . . ? C37 Cr1 C35 63.0(2) . . ? C36 Cr1 C35 38.2(2) . . ? C30 Cr1 C29 38.6(2) . . ? C31 Cr1 C29 63.4(2) . . ? C37 Cr1 C29 129.2(3) . . ? C36 Cr1 C29 114.8(3) . . ? C35 Cr1 C29 128.1(3) . . ? C30 Cr1 C34 154.8(3) . . ? C31 Cr1 C34 135.6(2) . . ? C37 Cr1 C34 62.5(2) . . ? C36 Cr1 C34 63.7(2) . . ? C35 Cr1 C34 38.4(2) . . ? C29 Cr1 C34 161.0(2) . . ? C30 Cr1 C28 63.4(3) . . ? C31 Cr1 C28 62.3(2) . . ? C37 Cr1 C28 149.9(2) . . ? C36 Cr1 C28 151.5(3) . . ? C35 Cr1 C28 146.0(2) . . ? C29 Cr1 C28 36.8(3) . . ? C34 Cr1 C28 141.3(2) . . ? C30 Cr1 C27 64.1(3) . . ? C31 Cr1 C27 37.5(2) . . ? C37 Cr1 C27 117.6(3) . . ? C36 Cr1 C27 149.4(3) . . ? C35 Cr1 C27 167.3(2) . . ? C29 Cr1 C27 62.5(3) . . ? C34 Cr1 C27 129.4(2) . . ? C28 Cr1 C27 37.0(2) . . ? C30 Cr1 C33 122.9(2) . . ? C31 Cr1 C33 99.1(2) . . ? C37 Cr1 C33 37.1(2) . . ? C36 Cr1 C33 63.1(2) . . ? C35 Cr1 C33 63.4(2) . . ? C29 Cr1 C33 161.0(2) . . ? C34 Cr1 C33 37.4(2) . . ? C28 Cr1 C33 143.2(3) . . ? C27 Cr1 C33 108.8(2) . . ? C30 Cr1 Ga1 127.00(18) . . ? C31 Cr1 Ga1 132.94(19) . . ? C37 Cr1 Ga1 136.89(17) . . ? C36 Cr1 Ga1 113.69(19) . . ? C35 Cr1 Ga1 77.68(16) . . ? C29 Cr1 Ga1 88.42(19) . . ? C34 Cr1 Ga1 75.98(15) . . ? C28 Cr1 Ga1 72.55(16) . . ? C27 Cr1 Ga1 96.90(17) . . ? C33 Cr1 Ga1 109.94(15) . . ? C1 N1 C3 118.0(4) . . ? C1 N1 Ga1 110.7(3) . . ? C3 N1 Ga1 130.6(4) . . ? C2 N2 C15 117.3(4) . . ? C2 N2 Ga1 109.3(3) . . ? C15 N2 Ga1 133.4(3) . . ? C2 C1 N1 116.1(5) . . ? C1 C2 N2 117.1(5) . . ? C4 C3 C8 119.8(5) . . ? C4 C3 N1 121.8(5) . . ? C8 C3 N1 118.3(5) . . ? C5 C4 C3 119.5(6) . . ? C5 C4 C9 118.4(6) . . ? C3 C4 C9 122.1(5) . . ? C6 C5 C4 121.0(6) . . ? C7 C6 C5 119.7(5) . . ? C6 C7 C8 121.6(6) . . ? C7 C8 C3 118.2(6) . . ? C7 C8 C12 120.0(6) . . ? C3 C8 C12 121.8(5) . . ? C4 C9 C11 111.5(5) . . ? C4 C9 C10 111.0(5) . . ? C11 C9 C10 109.6(6) . . ? C14 C12 C13 111.1(6) . . ? C14 C12 C8 109.3(5) . . ? C13 C12 C8 114.5(5) . . ? C16 C15 C20 121.1(5) . . ? C16 C15 N2 119.8(5) . . ? C20 C15 N2 119.2(5) . . ? C15 C16 C17 118.5(5) . . ? C15 C16 C21 123.1(5) . . ? C17 C16 C21 118.3(5) . . ? C18 C17 C16 120.8(6) . . ? C17 C18 C19 120.3(5) . . ? C18 C19 C20 122.3(6) . . ? C19 C20 C15 116.9(6) . . ? C19 C20 C24 121.4(6) . . ? C15 C20 C24 121.7(5) . . ? C16 C21 C22 109.7(5) . . ? C16 C21 C23 112.3(5) . . ? C22 C21 C23 110.4(6) . . ? C20 C24 C25 114.0(5) . . ? C20 C24 C26 111.2(5) . . ? C25 C24 C26 109.7(6) . . ? C31 C27 C28 106.5(6) . . ? C31 C27 C32 126.3(6) . . ? C28 C27 C32 127.1(6) . . ? C31 C27 Cr1 68.3(4) . . ? C28 C27 Cr1 71.3(4) . . ? C32 C27 Cr1 127.4(4) . . ? C29 C28 C27 109.5(6) . . ? C29 C28 Cr1 70.4(4) . . ? C27 C28 Cr1 71.7(4) . . ? C28 C29 C30 108.3(6) . . ? C28 C29 Cr1 72.8(3) . . ? C30 C29 Cr1 68.3(3) . . ? C31 C30 C29 106.1(6) . . ? C31 C30 Cr1 71.4(3) . . ? C29 C30 Cr1 73.2(3) . . ? C27 C31 C30 109.5(6) . . ? C27 C31 Cr1 74.2(4) . . ? C30 C31 Cr1 69.7(3) . . ? C37 C33 C34 106.7(6) . . ? C37 C33 C38 126.3(6) . . ? C34 C33 C38 127.0(5) . . ? C37 C33 Cr1 69.4(3) . . ? C34 C33 Cr1 69.7(3) . . ? C38 C33 Cr1 123.9(4) . . ? C33 C34 C35 108.5(5) . . ? C33 C34 Cr1 72.9(3) . . ? C35 C34 Cr1 70.6(3) . . ? C36 C35 C34 107.0(5) . . ? C36 C35 Cr1 70.6(4) . . ? C34 C35 Cr1 71.0(4) . . ? C37 C36 C35 107.2(6) . . ? C37 C36 Cr1 71.2(4) . . ? C35 C36 Cr1 71.2(4) . . ? C33 C37 C36 110.5(6) . . ? C33 C37 Cr1 73.5(3) . . ? C36 C37 Cr1 71.2(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.456 _refine_diff_density_min -0.871 _refine_diff_density_rms 0.100 # Attachment 'cmpd17.cif' data_compound17 _database_code_depnum_ccdc_archive 'CCDC 603228' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H104 Ga K Mn N4 Si4' _chemical_formula_weight 1061.51 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 12.697(3) _cell_length_b 14.656(3) _cell_length_c 17.878(4) _cell_angle_alpha 108.31(3) _cell_angle_beta 96.90(3) _cell_angle_gamma 92.94(3) _cell_volume 3121.5(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.129 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1150 _exptl_absorpt_coefficient_mu 0.811 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.803 _exptl_absorpt_correction_T_max 0.888 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _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 20196 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0536 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10864 _reflns_number_gt 8908 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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. During the course of refinement a heavily disordered molecule of hexane of crystallisation was located in the crystal lattice. All attempts to model its disorder were unsatisfactory. As a result the SQUEEZE program of the PLATON suite of programs was utilised to remove the contribution of the electron density of this disordered molecule from the observed structure factors. In the final refinement, the contribution of one molecule of hexane per asymmetric unit to the empirical formula, formula weight and F(000) vales of the structure was included. After this refinement a residual electron density peak of 2.204 ang. was observed at ca. 0.4 ang. from Ga1. ; _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^)+(0.1068P)^2^+5.2546P] 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 10864 _refine_ls_number_parameters 560 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0818 _refine_ls_R_factor_gt 0.0709 _refine_ls_wR_factor_ref 0.1980 _refine_ls_wR_factor_gt 0.1914 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.061 _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 Ga1 Ga 0.67566(3) 0.16312(3) 0.32354(3) 0.03250(18) Uani 1 1 d . . . Mn1 Mn 0.66882(5) 0.25451(5) 0.21577(4) 0.0359(2) Uani 1 1 d . . . K1 K 0.79928(8) -0.05117(7) 0.28041(6) 0.0445(3) Uani 1 1 d . . . Si1 Si 0.84124(13) 0.16021(11) 0.09016(9) 0.0527(4) Uani 1 1 d . . . Si2 Si 0.88286(12) 0.37727(10) 0.21368(9) 0.0505(4) Uani 1 1 d . . . Si3 Si 0.49937(12) 0.42822(10) 0.25364(9) 0.0510(4) Uani 1 1 d . . . Si4 Si 0.42144(11) 0.21623(10) 0.14114(8) 0.0471(3) Uani 1 1 d . . . N1 N 0.6135(3) 0.0614(2) 0.3572(2) 0.0363(8) Uani 1 1 d . . . N2 N 0.8013(3) 0.1570(2) 0.3951(2) 0.0313(7) Uani 1 1 d . . . N3 N 0.9230(5) -0.1914(4) 0.1891(3) 0.0724(15) Uani 1 1 d . . . N4 N 0.8610(4) -0.1973(3) 0.3453(3) 0.0527(11) Uani 1 1 d . . . C1 C 0.6805(3) 0.0474(3) 0.4205(3) 0.0348(9) Uani 1 1 d . . . H1 H 0.6587 0.0052 0.4479 0.042 Uiso 1 1 calc R . . C2 C 0.7774(3) 0.0974(3) 0.4400(3) 0.0323(9) Uani 1 1 d . . . H2 H 0.8273 0.0926 0.4824 0.039 Uiso 1 1 calc R . . C3 C 0.5034(3) 0.0290(3) 0.3497(3) 0.0415(11) Uani 1 1 d . . . C4 C 0.4369(4) 0.0850(4) 0.4016(3) 0.0490(12) Uani 1 1 d . . . C5 C 0.3323(4) 0.0484(4) 0.3956(4) 0.0631(15) Uani 1 1 d . . . H5 H 0.2877 0.0844 0.4308 0.076 Uiso 1 1 calc R . . C6 C 0.2915(4) -0.0377(4) 0.3409(4) 0.0665(17) Uani 1 1 d . . . H6 H 0.2198 -0.0616 0.3386 0.080 Uiso 1 1 calc R . . C7 C 0.3549(4) -0.0901(4) 0.2886(4) 0.0621(15) Uani 1 1 d . . . H7 H 0.3253 -0.1490 0.2493 0.074 Uiso 1 1 calc R . . C8 C 0.4611(4) -0.0588(4) 0.2921(3) 0.0519(13) Uani 1 1 d . B . C9 C 0.4788(4) 0.1824(4) 0.4626(3) 0.0517(12) Uani 1 1 d . . . H9 H 0.5460 0.2049 0.4469 0.062 Uiso 1 1 calc R . . C10 C 0.4001(5) 0.2583(4) 0.4642(4) 0.0659(16) Uani 1 1 d . . . H10A H 0.3829 0.2628 0.4106 0.099 Uiso 1 1 calc R . . H10B H 0.4322 0.3211 0.5008 0.099 Uiso 1 1 calc R . . H10C H 0.3348 0.2398 0.4821 0.099 Uiso 1 1 calc R . . C11 C 0.5056(4) 0.1748(5) 0.5453(4) 0.0638(15) Uani 1 1 d . . . H11A H 0.4410 0.1527 0.5621 0.096 Uiso 1 1 calc R . . H11B H 0.5343 0.2382 0.5828 0.096 Uiso 1 1 calc R . . H11C H 0.5589 0.1285 0.5445 0.096 Uiso 1 1 calc R . . C12 C 0.5297(5) -0.1211(4) 0.2370(4) 0.0734(19) Uani 1 1 d D . . H12 H 0.6008 -0.1119 0.2705 0.088 Uiso 1 1 calc R A 1 C13 C 0.4967(8) -0.2333(5) 0.2120(7) 0.072(3) Uani 0.672(12) 1 d PD B 1 H13A H 0.5484 -0.2687 0.1803 0.108 Uiso 0.672(12) 1 calc PR B 1 H13B H 0.4257 -0.2486 0.1804 0.108 Uiso 0.672(12) 1 calc PR B 1 H13C H 0.4956 -0.2522 0.2599 0.108 Uiso 0.672(12) 1 calc PR B 1 C13A C 0.5815(16) -0.1977(14) 0.2432(17) 0.092(9) Uani 0.328(12) 1 d PD B 2 H13D H 0.6255 -0.2176 0.2005 0.138 Uiso 0.328(12) 1 calc PR B 2 H13E H 0.5294 -0.2514 0.2389 0.138 Uiso 0.328(12) 1 calc PR B 2 H13F H 0.6271 -0.1794 0.2949 0.138 Uiso 0.328(12) 1 calc PR B 2 C14 C 0.5511(8) -0.0919(6) 0.1721(5) 0.062(3) Uani 0.672(12) 1 d PD B 1 H14A H 0.6074 -0.1282 0.1470 0.093 Uiso 0.672(12) 1 calc PR B 1 H14B H 0.5745 -0.0227 0.1909 0.093 Uiso 0.672(12) 1 calc PR B 1 H14C H 0.4863 -0.1045 0.1332 0.093 Uiso 0.672(12) 1 calc PR B 1 C14A C 0.4680(17) -0.1414(16) 0.1491(11) 0.084(7) Uani 0.328(12) 1 d PD B 2 H14D H 0.5184 -0.1582 0.1106 0.126 Uiso 0.328(12) 1 calc PR B 2 H14E H 0.4352 -0.0834 0.1459 0.126 Uiso 0.328(12) 1 calc PR B 2 H14F H 0.4124 -0.1950 0.1370 0.126 Uiso 0.328(12) 1 calc PR B 2 C15 C 0.8871(3) 0.2313(3) 0.4286(2) 0.0317(9) Uani 1 1 d . . . C16 C 0.9822(3) 0.2235(3) 0.3930(3) 0.0339(9) Uani 1 1 d . . . C17 C 1.0632(4) 0.2987(3) 0.4255(3) 0.0416(10) Uani 1 1 d . . . H17 H 1.1267 0.2956 0.4019 0.050 Uiso 1 1 calc R . . C18 C 1.0541(4) 0.3767(3) 0.4900(3) 0.0453(11) Uani 1 1 d . . . H18 H 1.1108 0.4265 0.5110 0.054 Uiso 1 1 calc R . . C19 C 0.9618(4) 0.3826(3) 0.5247(3) 0.0414(10) Uani 1 1 d . . . H19 H 0.9562 0.4366 0.5700 0.050 Uiso 1 1 calc R . . C20 C 0.8769(3) 0.3111(3) 0.4945(3) 0.0358(9) Uani 1 1 d . . . C21 C 0.9976(3) 0.1349(3) 0.3258(3) 0.0384(10) Uani 1 1 d . . . H21 H 0.9282 0.1141 0.2896 0.046 Uiso 1 1 calc R . . C22 C 1.0823(4) 0.1472(4) 0.2754(3) 0.0546(13) Uani 1 1 d . . . H22A H 1.0691 0.2022 0.2567 0.082 Uiso 1 1 calc R . . H22B H 1.0794 0.0884 0.2295 0.082 Uiso 1 1 calc R . . H22C H 1.1528 0.1588 0.3075 0.082 Uiso 1 1 calc R . . C23 C 1.0236(4) 0.0527(3) 0.3600(3) 0.0419(10) Uani 1 1 d . . . H23A H 1.0934 0.0693 0.3933 0.063 Uiso 1 1 calc R . . H23B H 1.0248 -0.0073 0.3162 0.063 Uiso 1 1 calc R . . H23C H 0.9690 0.0441 0.3922 0.063 Uiso 1 1 calc R . . C24 C 0.7768(4) 0.3223(3) 0.5348(3) 0.0429(11) Uani 1 1 d . . . H24 H 0.7215 0.2698 0.5012 0.052 Uiso 1 1 calc R . . C25 C 0.7964(4) 0.3112(4) 0.6174(3) 0.0543(13) Uani 1 1 d . . . H25A H 0.8533 0.3596 0.6508 0.081 Uiso 1 1 calc R . . H25B H 0.8174 0.2465 0.6126 0.081 Uiso 1 1 calc R . . H25C H 0.7309 0.3205 0.6417 0.081 Uiso 1 1 calc R . . C26 C 0.7325(4) 0.4189(4) 0.5396(3) 0.0571(13) Uani 1 1 d . . . H26A H 0.7795 0.4715 0.5793 0.086 Uiso 1 1 calc R . . H26B H 0.6611 0.4187 0.5550 0.086 Uiso 1 1 calc R . . H26C H 0.7288 0.4284 0.4875 0.086 Uiso 1 1 calc R . . C27 C 0.8285(4) 0.2502(3) 0.1858(3) 0.0422(10) Uani 1 1 d . . . H27 H 0.8687 0.2258 0.2261 0.051 Uiso 1 1 calc R . . C28 C 0.5295(4) 0.3154(3) 0.1798(3) 0.0418(10) Uani 1 1 d . . . H28 H 0.5450 0.3338 0.1326 0.050 Uiso 1 1 calc R . . C29 C 0.8088(6) 0.0363(4) 0.0959(4) 0.0680(16) Uani 1 1 d . . . H29A H 0.8519 0.0292 0.1427 0.102 Uiso 1 1 calc R . . H29B H 0.8245 -0.0124 0.0478 0.102 Uiso 1 1 calc R . . H29C H 0.7330 0.0274 0.1004 0.102 Uiso 1 1 calc R . . C30 C 0.7488(6) 0.1741(5) 0.0055(4) 0.0747(18) Uani 1 1 d . . . H30A H 0.6758 0.1748 0.0182 0.112 Uiso 1 1 calc R . . H30B H 0.7522 0.1200 -0.0428 0.112 Uiso 1 1 calc R . . H30C H 0.7699 0.2348 -0.0031 0.112 Uiso 1 1 calc R . . C31 C 0.9800(6) 0.1599(6) 0.0601(4) 0.083(2) Uani 1 1 d . . . H31A H 0.9960 0.2181 0.0461 0.125 Uiso 1 1 calc R . . H31B H 0.9829 0.1026 0.0140 0.125 Uiso 1 1 calc R . . H31C H 1.0325 0.1588 0.1046 0.125 Uiso 1 1 calc R . . C32 C 0.8249(6) 0.4346(4) 0.1399(4) 0.0716(18) Uani 1 1 d . . . H32A H 0.8558 0.4102 0.0905 0.107 Uiso 1 1 calc R . . H32B H 0.8412 0.5048 0.1620 0.107 Uiso 1 1 calc R . . H32C H 0.7475 0.4189 0.1287 0.107 Uiso 1 1 calc R . . C33 C 0.8492(5) 0.4436(4) 0.3150(3) 0.0576(14) Uani 1 1 d . . . H33A H 0.7716 0.4400 0.3133 0.086 Uiso 1 1 calc R . . H33B H 0.8780 0.5113 0.3311 0.086 Uiso 1 1 calc R . . H33C H 0.8803 0.4139 0.3536 0.086 Uiso 1 1 calc R . . C34 C 1.0333(5) 0.3990(5) 0.2246(5) 0.089(2) Uani 1 1 d . . . H34A H 1.0659 0.3767 0.2675 0.133 Uiso 1 1 calc R . . H34B H 1.0539 0.4682 0.2375 0.133 Uiso 1 1 calc R . . H34C H 1.0578 0.3634 0.1746 0.133 Uiso 1 1 calc R . . C35 C 0.5831(6) 0.5360(4) 0.2491(4) 0.078(2) Uani 1 1 d . . . H35A H 0.6585 0.5297 0.2643 0.117 Uiso 1 1 calc R . . H35B H 0.5623 0.5951 0.2859 0.117 Uiso 1 1 calc R . . H35C H 0.5721 0.5391 0.1948 0.117 Uiso 1 1 calc R . . C36 C 0.3573(6) 0.4596(5) 0.2396(5) 0.088(2) Uani 1 1 d . . . H36A H 0.3389 0.4623 0.1855 0.132 Uiso 1 1 calc R . . H36B H 0.3503 0.5225 0.2783 0.132 Uiso 1 1 calc R . . H36C H 0.3091 0.4102 0.2476 0.132 Uiso 1 1 calc R . . C37 C 0.5274(5) 0.4245(4) 0.3575(3) 0.0639(15) Uani 1 1 d . . . H37A H 0.4827 0.3709 0.3628 0.096 Uiso 1 1 calc R . . H37B H 0.5116 0.4854 0.3949 0.096 Uiso 1 1 calc R . . H37C H 0.6027 0.4151 0.3694 0.096 Uiso 1 1 calc R . . C38 C 0.3105(5) 0.2397(5) 0.0715(4) 0.080(2) Uani 1 1 d . . . H38A H 0.2771 0.2969 0.0999 0.120 Uiso 1 1 calc R . . H38B H 0.2571 0.1838 0.0520 0.120 Uiso 1 1 calc R . . H38C H 0.3395 0.2507 0.0263 0.120 Uiso 1 1 calc R . . C39 C 0.3611(5) 0.1869(5) 0.2219(4) 0.0718(17) Uani 1 1 d . . . H39A H 0.4165 0.1693 0.2566 0.108 Uiso 1 1 calc R . . H39B H 0.3060 0.1327 0.1983 0.108 Uiso 1 1 calc R . . H39C H 0.3291 0.2433 0.2532 0.108 Uiso 1 1 calc R . . C40 C 0.4744(5) 0.1025(4) 0.0803(4) 0.0690(16) Uani 1 1 d . . . H40A H 0.5048 0.1145 0.0360 0.103 Uiso 1 1 calc R . . H40B H 0.4161 0.0508 0.0593 0.103 Uiso 1 1 calc R . . H40C H 0.5297 0.0834 0.1140 0.103 Uiso 1 1 calc R . . C41 C 1.0118(7) -0.1583(5) 0.1545(4) 0.090(2) Uani 1 1 d . . . H41A H 1.0396 -0.2143 0.1187 0.135 Uiso 1 1 calc R . . H41B H 1.0687 -0.1223 0.1973 0.135 Uiso 1 1 calc R . . H41C H 0.9859 -0.1163 0.1245 0.135 Uiso 1 1 calc R . . C42 C 0.8401(8) -0.2399(7) 0.1270(5) 0.115(3) Uani 1 1 d U . . H42A H 0.8135 -0.1950 0.1001 0.173 Uiso 1 1 calc R . . H42B H 0.7820 -0.2643 0.1491 0.173 Uiso 1 1 calc R . . H42C H 0.8672 -0.2940 0.0887 0.173 Uiso 1 1 calc R . . C43 C 0.9657(6) -0.2529(4) 0.2348(4) 0.0727(18) Uani 1 1 d . . . H43A H 0.9841 -0.3133 0.1968 0.087 Uiso 1 1 calc R . . H43B H 1.0327 -0.2192 0.2689 0.087 Uiso 1 1 calc R . . C44 C 0.8954(6) -0.2784(4) 0.2851(4) 0.0696(17) Uani 1 1 d . . . H44A H 0.9322 -0.3197 0.3122 0.084 Uiso 1 1 calc R . . H44B H 0.8313 -0.3174 0.2505 0.084 Uiso 1 1 calc R . . C45 C 0.7699(6) -0.2312(6) 0.3771(6) 0.096(2) Uani 1 1 d . . . H45A H 0.7921 -0.2790 0.4022 0.143 Uiso 1 1 calc R . . H45B H 0.7115 -0.2607 0.3335 0.143 Uiso 1 1 calc R . . H45C H 0.7458 -0.1763 0.4166 0.143 Uiso 1 1 calc R . . C46 C 0.9440(5) -0.1546(4) 0.4116(3) 0.0627(15) Uani 1 1 d . . . H46A H 0.9171 -0.1022 0.4517 0.094 Uiso 1 1 calc R . . H46B H 1.0048 -0.1287 0.3930 0.094 Uiso 1 1 calc R . . H46C H 0.9666 -0.2037 0.4351 0.094 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 Ga1 0.0274(3) 0.0297(3) 0.0449(3) 0.0189(2) 0.00356(19) 0.00378(18) Mn1 0.0362(4) 0.0308(4) 0.0445(4) 0.0182(3) 0.0036(3) 0.0047(3) K1 0.0403(6) 0.0353(5) 0.0559(6) 0.0138(5) 0.0008(5) 0.0076(4) Si1 0.0623(9) 0.0489(8) 0.0497(8) 0.0168(7) 0.0172(7) 0.0038(7) Si2 0.0541(9) 0.0399(7) 0.0605(9) 0.0225(7) 0.0071(7) -0.0060(6) Si3 0.0555(9) 0.0383(7) 0.0577(8) 0.0150(6) -0.0011(7) 0.0159(6) Si4 0.0414(7) 0.0427(7) 0.0559(8) 0.0170(6) -0.0020(6) 0.0054(6) N1 0.0284(18) 0.0327(18) 0.051(2) 0.0219(17) -0.0015(16) -0.0009(15) N2 0.0260(17) 0.0300(17) 0.0412(19) 0.0170(15) 0.0034(14) 0.0009(14) N3 0.112(5) 0.058(3) 0.052(3) 0.019(2) 0.013(3) 0.039(3) N4 0.058(3) 0.042(2) 0.065(3) 0.025(2) 0.010(2) 0.012(2) C1 0.028(2) 0.033(2) 0.048(2) 0.0211(19) 0.0045(18) 0.0025(17) C2 0.025(2) 0.031(2) 0.044(2) 0.0162(18) 0.0048(17) 0.0038(16) C3 0.030(2) 0.040(2) 0.063(3) 0.032(2) 0.000(2) 0.0024(19) C4 0.033(2) 0.043(3) 0.076(3) 0.029(3) 0.004(2) 0.002(2) C5 0.029(3) 0.061(3) 0.106(5) 0.036(3) 0.011(3) 0.007(2) C6 0.029(3) 0.054(3) 0.118(5) 0.034(3) 0.000(3) 0.000(2) C7 0.035(3) 0.049(3) 0.098(4) 0.026(3) -0.011(3) -0.005(2) C8 0.031(2) 0.042(3) 0.081(4) 0.022(3) -0.004(2) 0.003(2) C9 0.037(3) 0.047(3) 0.074(3) 0.020(3) 0.018(2) -0.001(2) C10 0.075(4) 0.047(3) 0.084(4) 0.026(3) 0.024(3) 0.007(3) C11 0.042(3) 0.070(4) 0.078(4) 0.019(3) 0.013(3) 0.009(3) C12 0.037(3) 0.068(4) 0.092(5) -0.001(3) 0.004(3) -0.016(3) C13 0.063(7) 0.036(4) 0.114(8) 0.022(5) 0.006(5) 0.007(4) C13A 0.058(13) 0.066(13) 0.17(2) 0.085(15) -0.021(14) 0.005(10) C14 0.061(6) 0.052(5) 0.064(5) 0.012(4) -0.005(4) 0.006(4) C14A 0.072(15) 0.071(14) 0.112(18) 0.034(13) 0.020(13) -0.002(11) C15 0.025(2) 0.029(2) 0.042(2) 0.0166(18) -0.0021(17) -0.0003(16) C16 0.028(2) 0.034(2) 0.045(2) 0.0221(19) 0.0022(17) -0.0004(17) C17 0.030(2) 0.044(3) 0.054(3) 0.021(2) 0.0042(19) -0.0023(19) C18 0.037(3) 0.038(2) 0.061(3) 0.021(2) -0.001(2) -0.008(2) C19 0.038(2) 0.034(2) 0.048(3) 0.011(2) -0.001(2) 0.0020(19) C20 0.032(2) 0.033(2) 0.044(2) 0.0160(19) 0.0030(18) 0.0049(17) C21 0.029(2) 0.043(2) 0.049(3) 0.021(2) 0.0095(19) 0.0040(18) C22 0.048(3) 0.056(3) 0.064(3) 0.022(3) 0.019(3) 0.007(2) C23 0.036(2) 0.038(2) 0.054(3) 0.018(2) 0.007(2) 0.0107(19) C24 0.034(2) 0.040(2) 0.049(3) 0.006(2) 0.007(2) 0.0015(19) C25 0.052(3) 0.056(3) 0.059(3) 0.020(3) 0.020(2) 0.007(2) C26 0.050(3) 0.058(3) 0.067(3) 0.022(3) 0.013(3) 0.023(3) C27 0.047(3) 0.037(2) 0.047(3) 0.020(2) 0.006(2) -0.001(2) C28 0.044(3) 0.036(2) 0.049(3) 0.019(2) 0.002(2) 0.010(2) C29 0.084(4) 0.043(3) 0.076(4) 0.015(3) 0.019(3) 0.006(3) C30 0.089(5) 0.080(4) 0.055(3) 0.023(3) 0.010(3) 0.005(4) C31 0.083(5) 0.100(5) 0.074(4) 0.028(4) 0.036(4) 0.008(4) C32 0.111(5) 0.048(3) 0.063(4) 0.030(3) 0.012(3) -0.006(3) C33 0.063(3) 0.045(3) 0.059(3) 0.016(2) -0.008(3) -0.005(2) C34 0.063(4) 0.072(4) 0.128(6) 0.032(4) 0.015(4) -0.018(3) C35 0.105(5) 0.038(3) 0.087(4) 0.021(3) -0.006(4) 0.011(3) C36 0.073(5) 0.074(4) 0.097(5) 0.002(4) -0.007(4) 0.043(4) C37 0.074(4) 0.060(3) 0.056(3) 0.017(3) 0.008(3) 0.016(3) C38 0.070(4) 0.069(4) 0.091(5) 0.025(4) -0.026(4) 0.002(3) C39 0.046(3) 0.078(4) 0.101(5) 0.042(4) 0.014(3) 0.001(3) C40 0.068(4) 0.046(3) 0.083(4) 0.012(3) 0.004(3) 0.001(3) C41 0.143(7) 0.078(5) 0.068(4) 0.028(4) 0.055(5) 0.045(5) C42 0.120(5) 0.106(5) 0.105(5) 0.018(4) -0.006(4) 0.027(4) C43 0.110(5) 0.056(3) 0.060(3) 0.022(3) 0.023(3) 0.036(4) C44 0.099(5) 0.045(3) 0.066(4) 0.019(3) 0.010(3) 0.018(3) C45 0.074(5) 0.083(5) 0.157(7) 0.069(5) 0.040(5) 0.013(4) C46 0.078(4) 0.050(3) 0.067(4) 0.032(3) 0.003(3) 0.009(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 Ga1 N1 1.940(3) . ? Ga1 N2 1.946(3) . ? Ga1 Mn1 2.6658(10) . ? Ga1 K1 3.4925(15) . ? Mn1 C28 2.143(4) . ? Mn1 C27 2.158(5) . ? K1 N4 2.839(4) . ? K1 N3 2.863(5) . ? K1 C2 3.052(4) . ? K1 C1 3.081(5) . ? K1 N2 3.093(4) . ? K1 N1 3.150(4) . ? Si1 C27 1.833(5) . ? Si1 C30 1.871(7) . ? Si1 C29 1.879(6) . ? Si1 C31 1.902(7) . ? Si2 C27 1.843(5) . ? Si2 C32 1.875(6) . ? Si2 C33 1.880(6) . ? Si2 C34 1.897(7) . ? Si3 C28 1.854(5) . ? Si3 C37 1.868(6) . ? Si3 C35 1.887(7) . ? Si3 C36 1.891(6) . ? Si4 C28 1.846(5) . ? Si4 C39 1.864(6) . ? Si4 C38 1.885(6) . ? Si4 C40 1.888(6) . ? N1 C1 1.407(5) . ? N1 C3 1.430(5) . ? N2 C2 1.404(5) . ? N2 C15 1.429(5) . ? N3 C42 1.412(10) . ? N3 C43 1.477(7) . ? N3 C41 1.480(9) . ? N4 C46 1.440(7) . ? N4 C44 1.458(7) . ? N4 C45 1.477(8) . ? C1 C2 1.348(6) . ? C3 C8 1.403(7) . ? C3 C4 1.424(7) . ? C4 C5 1.386(7) . ? C4 C9 1.522(7) . ? C5 C6 1.361(8) . ? C6 C7 1.380(9) . ? C7 C8 1.389(7) . ? C8 C12 1.513(8) . ? C9 C11 1.517(8) . ? C9 C10 1.529(8) . ? C12 C13A 1.357(13) . ? C12 C14 1.406(10) . ? C12 C13 1.582(9) . ? C12 C14A 1.599(16) . ? C15 C20 1.400(6) . ? C15 C16 1.425(6) . ? C16 C17 1.396(6) . ? C16 C21 1.507(6) . ? C17 C18 1.367(7) . ? C18 C19 1.384(7) . ? C19 C20 1.393(6) . ? C20 C24 1.525(6) . ? C21 C22 1.521(6) . ? C21 C23 1.545(6) . ? C24 C25 1.527(7) . ? C24 C26 1.531(7) . ? C43 C44 1.454(9) . ? 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 Ga1 N2 84.16(14) . . ? N1 Ga1 Mn1 147.69(11) . . ? N2 Ga1 Mn1 125.93(10) . . ? N1 Ga1 K1 63.55(11) . . ? N2 Ga1 K1 61.83(11) . . ? Mn1 Ga1 K1 116.82(3) . . ? C28 Mn1 C27 134.12(18) . . ? C28 Mn1 Ga1 122.97(14) . . ? C27 Mn1 Ga1 102.88(12) . . ? N4 K1 N3 63.88(13) . . ? N4 K1 C2 95.25(12) . . ? N3 K1 C2 148.01(14) . . ? N4 K1 C1 93.01(13) . . ? N3 K1 C1 156.89(13) . . ? C2 K1 C1 25.38(11) . . ? N4 K1 N2 118.45(12) . . ? N3 K1 N2 145.71(15) . . ? C2 K1 N2 26.41(10) . . ? C1 K1 N2 44.70(10) . . ? N4 K1 N1 113.69(12) . . ? N3 K1 N1 164.92(15) . . ? C2 K1 N1 44.22(10) . . ? C1 K1 N1 26.07(10) . . ? N2 K1 N1 49.29(9) . . ? N4 K1 Ga1 142.24(10) . . ? N3 K1 Ga1 153.44(11) . . ? C2 K1 Ga1 49.52(8) . . ? C1 K1 Ga1 49.51(8) . . ? N2 K1 Ga1 33.68(6) . . ? N1 K1 Ga1 33.45(6) . . ? C27 Si1 C30 112.6(3) . . ? C27 Si1 C29 109.0(2) . . ? C30 Si1 C29 107.9(3) . . ? C27 Si1 C31 115.1(3) . . ? C30 Si1 C31 106.3(3) . . ? C29 Si1 C31 105.6(3) . . ? C27 Si2 C32 110.9(3) . . ? C27 Si2 C33 108.3(2) . . ? C32 Si2 C33 109.7(3) . . ? C27 Si2 C34 115.8(3) . . ? C32 Si2 C34 107.4(3) . . ? C33 Si2 C34 104.4(3) . . ? C28 Si3 C37 111.7(2) . . ? C28 Si3 C35 111.0(3) . . ? C37 Si3 C35 107.2(3) . . ? C28 Si3 C36 115.2(3) . . ? C37 Si3 C36 106.6(3) . . ? C35 Si3 C36 104.6(3) . . ? C28 Si4 C39 112.7(3) . . ? C28 Si4 C38 113.7(3) . . ? C39 Si4 C38 107.9(3) . . ? C28 Si4 C40 110.2(3) . . ? C39 Si4 C40 107.0(3) . . ? C38 Si4 C40 104.9(3) . . ? C1 N1 C3 115.7(3) . . ? C1 N1 Ga1 111.2(3) . . ? C3 N1 Ga1 128.3(3) . . ? C1 N1 K1 74.2(2) . . ? C3 N1 K1 129.4(3) . . ? Ga1 N1 K1 83.00(12) . . ? C2 N2 C15 117.6(3) . . ? C2 N2 Ga1 110.5(3) . . ? C15 N2 Ga1 125.6(3) . . ? C2 N2 K1 75.2(2) . . ? C15 N2 K1 130.3(3) . . ? Ga1 N2 K1 84.49(12) . . ? C42 N3 C43 113.3(6) . . ? C42 N3 C41 108.8(6) . . ? C43 N3 C41 107.7(6) . . ? C42 N3 K1 96.9(5) . . ? C43 N3 K1 111.0(3) . . ? C41 N3 K1 118.9(4) . . ? C46 N4 C44 111.8(5) . . ? C46 N4 C45 107.2(5) . . ? C44 N4 C45 109.6(5) . . ? C46 N4 K1 108.0(3) . . ? C44 N4 K1 111.0(3) . . ? C45 N4 K1 109.2(4) . . ? C2 C1 N1 116.0(4) . . ? C2 C1 K1 76.1(3) . . ? N1 C1 K1 79.7(2) . . ? C1 C2 N2 117.1(4) . . ? C1 C2 K1 78.5(3) . . ? N2 C2 K1 78.4(2) . . ? C8 C3 C4 119.9(4) . . ? C8 C3 N1 120.1(4) . . ? C4 C3 N1 120.1(4) . . ? C5 C4 C3 118.3(5) . . ? C5 C4 C9 120.3(5) . . ? C3 C4 C9 121.3(4) . . ? C6 C5 C4 122.0(6) . . ? C5 C6 C7 119.6(5) . . ? C6 C7 C8 121.6(5) . . ? C7 C8 C3 118.6(5) . . ? C7 C8 C12 119.9(5) . . ? C3 C8 C12 121.4(4) . . ? C11 C9 C4 111.6(4) . . ? C11 C9 C10 109.9(5) . . ? C4 C9 C10 111.8(5) . . ? C13A C12 C14 113.7(13) . . ? C13A C12 C8 130.0(14) . . ? C14 C12 C8 116.1(6) . . ? C13A C12 C13 46.0(9) . . ? C14 C12 C13 112.5(7) . . ? C8 C12 C13 114.5(6) . . ? C13A C12 C14A 111.7(15) . . ? C14 C12 C14A 46.5(9) . . ? C8 C12 C14A 105.4(10) . . ? C13 C12 C14A 79.3(9) . . ? C20 C15 C16 120.7(4) . . ? C20 C15 N2 120.4(4) . . ? C16 C15 N2 118.9(4) . . ? C17 C16 C15 117.5(4) . . ? C17 C16 C21 121.0(4) . . ? C15 C16 C21 121.4(4) . . ? C18 C17 C16 122.1(4) . . ? C17 C18 C19 119.7(4) . . ? C18 C19 C20 121.3(4) . . ? C19 C20 C15 118.6(4) . . ? C19 C20 C24 118.8(4) . . ? C15 C20 C24 122.6(4) . . ? C16 C21 C22 116.0(4) . . ? C16 C21 C23 109.0(4) . . ? C22 C21 C23 109.1(4) . . ? C20 C24 C25 112.0(4) . . ? C20 C24 C26 111.1(4) . . ? C25 C24 C26 110.6(4) . . ? Si1 C27 Si2 122.7(3) . . ? Si1 C27 Mn1 114.4(2) . . ? Si2 C27 Mn1 105.6(2) . . ? Si4 C28 Si3 117.0(3) . . ? Si4 C28 Mn1 106.9(2) . . ? Si3 C28 Mn1 115.1(2) . . ? C44 C43 N3 115.8(6) . . ? C43 C44 N4 115.6(5) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 2.204 _refine_diff_density_min -0.651 _refine_diff_density_rms 0.103 # Attachment 'cmpd8.cif' data_compound8 _database_code_depnum_ccdc_archive 'CCDC 603229' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H57 Co Ga K N4 O' _chemical_formula_weight 753.63 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 11.860(2) _cell_length_b 14.192(3) _cell_length_c 23.631(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.05(3) _cell_angle_gamma 90.00 _cell_volume 3955.3(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.266 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 1.238 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.671 _exptl_absorpt_correction_T_max 0.789 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _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 21460 _diffrn_reflns_av_R_equivalents 0.0609 _diffrn_reflns_av_sigmaI/netI 0.0789 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 26.38 _reflns_number_total 7999 _reflns_number_gt 5464 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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 'calc w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+3.6428P] 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 7999 _refine_ls_number_parameters 428 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0890 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1066 _refine_ls_wR_factor_gt 0.0946 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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 Ga1 Ga 0.67268(3) 0.76529(2) 0.078620(15) 0.02544(11) Uani 1 1 d . . . Co2 Co 0.73952(4) 0.66584(3) 0.01687(2) 0.03476(15) Uani 1 1 d . . . K1 K 0.61171(8) 0.46667(6) 0.09640(4) 0.0579(3) Uani 1 1 d . . . O1 O 0.5078(3) 0.6064(2) 0.00014(14) 0.0697(9) Uani 1 1 d . . . N1 N 0.6875(2) 0.89630(17) 0.09359(11) 0.0258(6) Uani 1 1 d . . . N2 N 0.5691(2) 0.76211(17) 0.13497(11) 0.0261(6) Uani 1 1 d . . . N3 N 0.8180(3) 0.3520(2) 0.12415(14) 0.0478(8) Uani 1 1 d . . . N4 N 0.5891(3) 0.2794(2) 0.14298(14) 0.0444(8) Uani 1 1 d . . . C1 C 0.6203(3) 0.9212(2) 0.13653(13) 0.0271(7) Uani 1 1 d . . . H1 H 0.6180 0.9841 0.1502 0.033 Uiso 1 1 calc R . . C2 C 0.5594(3) 0.8525(2) 0.15743(14) 0.0273(7) Uani 1 1 d . . . H2 H 0.5116 0.8646 0.1864 0.033 Uiso 1 1 calc R . . C3 C 0.7800(3) 0.9568(2) 0.08374(14) 0.0271(8) Uani 1 1 d . . . C4 C 0.7813(3) 1.0023(2) 0.03100(15) 0.0334(8) Uani 1 1 d . . . C5 C 0.8732(3) 1.0605(3) 0.02276(17) 0.0459(10) Uani 1 1 d . . . H5 H 0.8754 1.0918 -0.0126 0.055 Uiso 1 1 calc R . . C6 C 0.9609(3) 1.0730(3) 0.06540(19) 0.0527(11) Uani 1 1 d . . . H6 H 1.0225 1.1133 0.0593 0.063 Uiso 1 1 calc R . . C7 C 0.9595(3) 1.0277(3) 0.11645(18) 0.0467(10) Uani 1 1 d . . . H7 H 1.0203 1.0373 0.1454 0.056 Uiso 1 1 calc R . . C8 C 0.8711(3) 0.9679(2) 0.12698(15) 0.0341(8) Uani 1 1 d . . . C9 C 0.6819(3) 0.9950(2) -0.01501(15) 0.0355(8) Uani 1 1 d . . . H9 H 0.6356 0.9390 -0.0063 0.043 Uiso 1 1 calc R . . C10 C 0.6078(3) 1.0824(3) -0.01264(18) 0.0509(11) Uani 1 1 d . . . H10A H 0.5788 1.0860 0.0246 0.076 Uiso 1 1 calc R . . H10B H 0.5440 1.0787 -0.0425 0.076 Uiso 1 1 calc R . . H10C H 0.6529 1.1388 -0.0185 0.076 Uiso 1 1 calc R . . C11 C 0.7171(3) 0.9824(3) -0.07505(17) 0.0532(11) Uani 1 1 d . . . H11A H 0.7618 1.0370 -0.0848 0.080 Uiso 1 1 calc R . . H11B H 0.6492 0.9771 -0.1023 0.080 Uiso 1 1 calc R . . H11C H 0.7628 0.9251 -0.0764 0.080 Uiso 1 1 calc R . . C12 C 0.8761(3) 0.9165(3) 0.18322(15) 0.0402(9) Uani 1 1 d . . . H12 H 0.8075 0.8752 0.1818 0.048 Uiso 1 1 calc R . . C13 C 0.9804(4) 0.8524(3) 0.19184(19) 0.0602(12) Uani 1 1 d . . . H13A H 0.9805 0.8094 0.1594 0.090 Uiso 1 1 calc R . . H13B H 0.9781 0.8158 0.2269 0.090 Uiso 1 1 calc R . . H13C H 1.0493 0.8909 0.1948 0.090 Uiso 1 1 calc R . . C14 C 0.8712(3) 0.9845(3) 0.23354(17) 0.0559(11) Uani 1 1 d . . . H14A H 0.9383 1.0253 0.2367 0.084 Uiso 1 1 calc R . . H14B H 0.8697 0.9483 0.2688 0.084 Uiso 1 1 calc R . . H14C H 0.8027 1.0233 0.2273 0.084 Uiso 1 1 calc R . . C15 C 0.5319(3) 0.6841(2) 0.16609(14) 0.0292(8) Uani 1 1 d . . . C16 C 0.6082(3) 0.6403(2) 0.20781(15) 0.0381(9) Uani 1 1 d . . . C17 C 0.5688(4) 0.5639(3) 0.23773(17) 0.0520(11) Uani 1 1 d . . . H17 H 0.6193 0.5331 0.2657 0.062 Uiso 1 1 calc R . . C18 C 0.4595(4) 0.5323(3) 0.22773(18) 0.0528(11) Uani 1 1 d . . . H18 H 0.4349 0.4805 0.2487 0.063 Uiso 1 1 calc R . . C19 C 0.3860(4) 0.5754(3) 0.18773(17) 0.0506(11) Uani 1 1 d . . . H19 H 0.3102 0.5531 0.1812 0.061 Uiso 1 1 calc R . . C20 C 0.4197(3) 0.6519(2) 0.15587(15) 0.0358(9) Uani 1 1 d . . . C21 C 0.7282(3) 0.6749(3) 0.22156(17) 0.0480(10) Uani 1 1 d . . . H21 H 0.7372 0.7306 0.1965 0.058 Uiso 1 1 calc R . . C22 C 0.7521(5) 0.7092(5) 0.2826(2) 0.0970(19) Uani 1 1 d . . . H22A H 0.6981 0.7590 0.2897 0.146 Uiso 1 1 calc R . . H22B H 0.8295 0.7342 0.2886 0.146 Uiso 1 1 calc R . . H22C H 0.7442 0.6566 0.3087 0.146 Uiso 1 1 calc R . . C23 C 0.8151(4) 0.6025(4) 0.2074(3) 0.0903(18) Uani 1 1 d . . . H23A H 0.8044 0.5442 0.2284 0.135 Uiso 1 1 calc R . . H23B H 0.8916 0.6271 0.2183 0.135 Uiso 1 1 calc R . . H23C H 0.8056 0.5896 0.1665 0.135 Uiso 1 1 calc R . . C24 C 0.3330(3) 0.7009(3) 0.11498(17) 0.0495(11) Uani 1 1 d . . . H24 H 0.3744 0.7404 0.0889 0.059 Uiso 1 1 calc R . . C25 C 0.2582(4) 0.7659(3) 0.1461(2) 0.0684(14) Uani 1 1 d . . . H25A H 0.2166 0.7287 0.1720 0.103 Uiso 1 1 calc R . . H25B H 0.2042 0.7981 0.1183 0.103 Uiso 1 1 calc R . . H25C H 0.3055 0.8126 0.1679 0.103 Uiso 1 1 calc R . . C26 C 0.2576(4) 0.6327(4) 0.0787(2) 0.0779(15) Uani 1 1 d . . . H26A H 0.3047 0.5919 0.0574 0.117 Uiso 1 1 calc R . . H26B H 0.2048 0.6682 0.0521 0.117 Uiso 1 1 calc R . . H26C H 0.2148 0.5940 0.1033 0.117 Uiso 1 1 calc R . . C27 C 0.8406(4) 0.7215(3) -0.04238(19) 0.0537(11) Uani 1 1 d . . . H27 H 0.8176 0.7660 -0.0714 0.064 Uiso 1 1 calc R . . C28 C 0.8874(3) 0.7433(3) 0.0128(2) 0.0524(11) Uani 1 1 d . . . H28 H 0.8997 0.8047 0.0284 0.063 Uiso 1 1 calc R . . C29 C 0.9134(4) 0.6565(4) 0.0413(2) 0.0737(15) Uani 1 1 d . . . H29 H 0.9469 0.6492 0.0794 0.088 Uiso 1 1 calc R . . C30 C 0.8807(5) 0.5846(4) 0.0034(3) 0.0872(19) Uani 1 1 d . . . H30 H 0.8893 0.5191 0.0110 0.105 Uiso 1 1 calc R . . C31 C 0.8330(5) 0.6240(3) -0.0480(2) 0.0765(17) Uani 1 1 d . . . H31 H 0.8014 0.5904 -0.0806 0.092 Uiso 1 1 calc R . . C32 C 0.6043(4) 0.6296(3) 0.00735(16) 0.0448(10) Uani 1 1 d . . . C33 C 0.8220(6) 0.3251(4) 0.0650(2) 0.101(2) Uani 1 1 d . . . H33A H 0.8828 0.2790 0.0625 0.151 Uiso 1 1 calc R . . H33B H 0.8367 0.3809 0.0426 0.151 Uiso 1 1 calc R . . H33C H 0.7493 0.2971 0.0502 0.151 Uiso 1 1 calc R . . C34 C 0.9263(4) 0.3971(3) 0.1443(2) 0.0647(13) Uani 1 1 d . . . H34A H 0.9243 0.4183 0.1836 0.097 Uiso 1 1 calc R . . H34B H 0.9387 0.4513 0.1200 0.097 Uiso 1 1 calc R . . H34C H 0.9881 0.3517 0.1426 0.097 Uiso 1 1 calc R . . C35 C 0.7999(4) 0.2702(3) 0.15924(19) 0.0571(11) Uani 1 1 d . . . H35A H 0.8019 0.2908 0.1994 0.069 Uiso 1 1 calc R . . H35B H 0.8632 0.2255 0.1568 0.069 Uiso 1 1 calc R . . C36 C 0.6898(4) 0.2194(3) 0.14281(19) 0.0550(11) Uani 1 1 d . . . H36A H 0.6914 0.1924 0.1043 0.066 Uiso 1 1 calc R . . H36B H 0.6834 0.1664 0.1695 0.066 Uiso 1 1 calc R . . C37 C 0.5716(5) 0.3022(3) 0.2016(2) 0.0744(15) Uani 1 1 d . . . H37A H 0.5624 0.2439 0.2228 0.112 Uiso 1 1 calc R . . H37B H 0.5033 0.3410 0.2020 0.112 Uiso 1 1 calc R . . H37C H 0.6373 0.3371 0.2194 0.112 Uiso 1 1 calc R . . C38 C 0.4894(4) 0.2292(3) 0.1163(2) 0.0695(13) Uani 1 1 d . . . H38A H 0.5000 0.2148 0.0766 0.104 Uiso 1 1 calc R . . H38B H 0.4220 0.2688 0.1174 0.104 Uiso 1 1 calc R . . H38C H 0.4794 0.1704 0.1369 0.104 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 Ga1 0.0276(2) 0.02226(19) 0.0272(2) -0.00168(15) 0.00596(15) -0.00150(15) Co2 0.0472(3) 0.0242(2) 0.0356(3) -0.00205(19) 0.0169(2) 0.0003(2) K1 0.0647(7) 0.0337(5) 0.0697(7) 0.0062(4) -0.0195(5) -0.0071(4) O1 0.064(2) 0.071(2) 0.074(2) -0.0266(17) 0.0076(18) -0.0274(17) N1 0.0240(15) 0.0216(13) 0.0322(16) 0.0003(11) 0.0054(13) -0.0015(11) N2 0.0288(15) 0.0247(14) 0.0258(15) 0.0002(11) 0.0076(12) -0.0008(11) N3 0.056(2) 0.0437(19) 0.043(2) -0.0020(15) 0.0003(17) -0.0066(15) N4 0.055(2) 0.0367(18) 0.043(2) -0.0033(14) 0.0123(17) -0.0033(15) C1 0.0273(19) 0.0240(17) 0.030(2) -0.0046(14) 0.0026(15) 0.0032(14) C2 0.0288(19) 0.0262(18) 0.0277(19) -0.0022(13) 0.0069(15) 0.0031(14) C3 0.0234(18) 0.0212(16) 0.037(2) -0.0034(14) 0.0063(15) -0.0020(13) C4 0.0271(19) 0.0307(18) 0.043(2) 0.0008(16) 0.0086(16) -0.0069(15) C5 0.039(2) 0.047(2) 0.052(3) 0.0088(19) 0.009(2) -0.0124(18) C6 0.038(2) 0.050(2) 0.071(3) 0.002(2) 0.009(2) -0.0196(19) C7 0.030(2) 0.049(2) 0.060(3) -0.006(2) -0.0026(19) -0.0080(18) C8 0.025(2) 0.0339(19) 0.043(2) -0.0048(16) 0.0041(17) 0.0009(15) C9 0.032(2) 0.0344(19) 0.040(2) 0.0120(16) 0.0030(17) -0.0088(15) C10 0.039(2) 0.062(3) 0.050(3) -0.008(2) -0.003(2) 0.010(2) C11 0.052(3) 0.060(3) 0.048(3) -0.003(2) 0.007(2) 0.001(2) C12 0.032(2) 0.049(2) 0.038(2) -0.0015(17) -0.0034(17) 0.0044(17) C13 0.056(3) 0.065(3) 0.057(3) 0.000(2) -0.005(2) 0.021(2) C14 0.044(3) 0.075(3) 0.047(3) -0.008(2) -0.002(2) 0.010(2) C15 0.038(2) 0.0242(17) 0.0269(19) -0.0017(14) 0.0109(16) 0.0023(15) C16 0.043(2) 0.037(2) 0.036(2) 0.0023(16) 0.0122(18) 0.0105(17) C17 0.070(3) 0.042(2) 0.046(3) 0.0144(19) 0.014(2) 0.024(2) C18 0.074(3) 0.034(2) 0.055(3) 0.0119(19) 0.027(2) 0.002(2) C19 0.060(3) 0.042(2) 0.052(3) 0.0073(19) 0.016(2) -0.017(2) C20 0.041(2) 0.0311(19) 0.037(2) 0.0034(15) 0.0117(18) -0.0084(16) C21 0.046(3) 0.063(3) 0.035(2) 0.0069(19) 0.0029(19) 0.019(2) C22 0.068(4) 0.156(6) 0.067(4) -0.021(4) 0.005(3) -0.022(4) C23 0.054(3) 0.094(4) 0.123(5) 0.004(3) 0.011(3) 0.028(3) C24 0.041(2) 0.061(3) 0.046(3) 0.022(2) -0.001(2) -0.019(2) C25 0.060(3) 0.052(3) 0.088(4) 0.009(2) -0.012(3) 0.004(2) C26 0.056(3) 0.106(4) 0.068(4) -0.012(3) -0.010(3) -0.015(3) C27 0.065(3) 0.050(3) 0.052(3) 0.001(2) 0.032(2) -0.010(2) C28 0.038(2) 0.051(3) 0.073(3) -0.013(2) 0.031(2) -0.0056(19) C29 0.040(3) 0.104(4) 0.079(4) 0.021(3) 0.016(3) 0.019(3) C30 0.085(4) 0.047(3) 0.140(6) 0.003(3) 0.063(4) 0.026(3) C31 0.095(4) 0.061(3) 0.085(4) -0.032(3) 0.066(3) -0.021(3) C32 0.061(3) 0.036(2) 0.037(2) -0.0129(17) 0.006(2) -0.0109(19) C33 0.140(6) 0.111(5) 0.056(4) -0.021(3) 0.029(4) -0.055(4) C34 0.049(3) 0.070(3) 0.074(3) -0.012(2) -0.001(2) -0.004(2) C35 0.060(3) 0.051(3) 0.060(3) 0.009(2) 0.001(2) 0.010(2) C36 0.069(3) 0.038(2) 0.059(3) 0.0058(19) 0.011(2) 0.002(2) C37 0.098(4) 0.061(3) 0.070(4) -0.015(2) 0.034(3) -0.010(3) C38 0.070(3) 0.057(3) 0.081(4) -0.003(2) 0.007(3) -0.011(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 N1 1.897(2) . ? Ga1 N2 1.905(3) . ? Ga1 Co2 2.2347(7) . ? Co2 C32 1.677(4) . ? Co2 C31 2.071(4) . ? Co2 C28 2.081(4) . ? Co2 C30 2.085(5) . ? Co2 C29 2.086(5) . ? Co2 C27 2.092(4) . ? K1 O1 2.758(3) 3_665 ? K1 N4 2.899(3) . ? K1 N3 2.954(3) . ? K1 C32 3.121(4) . ? K1 O1 3.167(4) . ? K1 C16 3.609(4) . ? K1 C15 3.669(3) . ? K1 C17 3.698(4) . ? O1 C32 1.186(5) . ? O1 K1 2.758(3) 3_665 ? N1 C1 1.400(4) . ? N1 C3 1.431(4) . ? N2 C2 1.397(4) . ? N2 C15 1.425(4) . ? N3 C33 1.454(6) . ? N3 C35 1.455(5) . ? N3 C34 1.468(5) . ? N4 C37 1.459(5) . ? N4 C38 1.466(5) . ? N4 C36 1.467(5) . ? C1 C2 1.339(4) . ? C3 C4 1.405(5) . ? C3 C8 1.415(5) . ? C4 C5 1.397(5) . ? C4 C9 1.520(5) . ? C5 C6 1.382(5) . ? C6 C7 1.369(5) . ? C7 C8 1.392(5) . ? C8 C12 1.511(5) . ? C9 C10 1.525(5) . ? C9 C11 1.531(5) . ? C12 C13 1.533(5) . ? C12 C14 1.537(5) . ? C15 C20 1.403(5) . ? C15 C16 1.411(5) . ? C16 C17 1.402(5) . ? C16 C21 1.508(5) . ? C17 C18 1.369(6) . ? C18 C19 1.361(6) . ? C19 C20 1.403(5) . ? C20 C24 1.506(5) . ? C21 C23 1.517(6) . ? C21 C22 1.519(6) . ? C24 C26 1.519(6) . ? C24 C25 1.521(6) . ? C27 C31 1.393(6) . ? C27 C28 1.398(6) . ? C28 C29 1.422(6) . ? C29 C30 1.387(7) . ? C30 C31 1.401(8) . ? C35 C36 1.507(6) . ? 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 Ga1 N2 86.96(11) . . ? N1 Ga1 Co2 135.10(8) . . ? N2 Ga1 Co2 137.80(8) . . ? C32 Co2 C31 113.1(2) . . ? C32 Co2 C28 162.74(19) . . ? C31 Co2 C28 66.30(18) . . ? C32 Co2 C30 125.6(2) . . ? C31 Co2 C30 39.4(2) . . ? C28 Co2 C30 65.86(19) . . ? C32 Co2 C29 157.1(2) . . ? C31 Co2 C29 66.2(2) . . ? C28 Co2 C29 39.92(18) . . ? C30 Co2 C29 38.8(2) . . ? C32 Co2 C27 129.32(19) . . ? C31 Co2 C27 39.08(17) . . ? C28 Co2 C27 39.14(16) . . ? C30 Co2 C27 65.2(2) . . ? C29 Co2 C27 65.80(19) . . ? C32 Co2 Ga1 83.19(13) . . ? C31 Co2 Ga1 156.76(13) . . ? C28 Co2 Ga1 93.15(11) . . ? C30 Co2 Ga1 142.6(2) . . ? C29 Co2 Ga1 105.51(17) . . ? C27 Co2 Ga1 117.79(11) . . ? O1 K1 N4 84.82(10) 3_665 . ? O1 K1 N3 108.54(10) 3_665 . ? N4 K1 N3 61.20(9) . . ? O1 K1 C32 75.24(10) 3_665 . ? N4 K1 C32 159.66(10) . . ? N3 K1 C32 121.44(11) . . ? O1 K1 O1 60.92(10) 3_665 . ? N4 K1 O1 143.29(9) . . ? N3 K1 O1 139.01(10) . . ? C32 K1 O1 21.73(8) . . ? O1 K1 C16 144.65(10) 3_665 . ? N4 K1 C16 109.88(9) . . ? N3 K1 C16 106.67(9) . . ? C32 K1 C16 89.11(9) . . ? O1 K1 C16 93.62(8) . . ? O1 K1 C15 123.57(9) 3_665 . ? N4 K1 C15 124.19(9) . . ? N3 K1 C15 127.64(8) . . ? C32 K1 C15 71.90(9) . . ? O1 K1 C15 72.34(8) . . ? C16 K1 C15 22.34(7) . . ? O1 K1 C17 141.23(11) 3_665 . ? N4 K1 C17 88.39(9) . . ? N3 K1 C17 101.22(10) . . ? C32 K1 C17 109.63(9) . . ? O1 K1 C17 109.57(8) . . ? C16 K1 C17 22.08(8) . . ? C15 K1 C17 38.21(8) . . ? C32 O1 K1 128.8(3) . 3_665 ? C32 O1 K1 76.9(3) . . ? K1 O1 K1 119.08(10) 3_665 . ? C1 N1 C3 118.1(2) . . ? C1 N1 Ga1 109.50(19) . . ? C3 N1 Ga1 128.0(2) . . ? C2 N2 C15 118.4(3) . . ? C2 N2 Ga1 109.2(2) . . ? C15 N2 Ga1 129.6(2) . . ? C33 N3 C35 111.1(4) . . ? C33 N3 C34 108.0(4) . . ? C35 N3 C34 109.8(3) . . ? C33 N3 K1 92.4(3) . . ? C35 N3 K1 113.4(2) . . ? C34 N3 K1 120.5(2) . . ? C37 N4 C38 109.1(4) . . ? C37 N4 C36 109.2(3) . . ? C38 N4 C36 109.7(3) . . ? C37 N4 K1 100.7(2) . . ? C38 N4 K1 112.6(3) . . ? C36 N4 K1 115.1(2) . . ? C2 C1 N1 117.0(3) . . ? C1 C2 N2 117.4(3) . . ? C4 C3 C8 120.7(3) . . ? C4 C3 N1 120.0(3) . . ? C8 C3 N1 119.2(3) . . ? C5 C4 C3 118.4(3) . . ? C5 C4 C9 119.9(3) . . ? C3 C4 C9 121.5(3) . . ? C6 C5 C4 120.9(4) . . ? C7 C6 C5 120.2(4) . . ? C6 C7 C8 121.6(4) . . ? C7 C8 C3 118.1(3) . . ? C7 C8 C12 119.4(3) . . ? C3 C8 C12 122.5(3) . . ? C4 C9 C10 108.9(3) . . ? C4 C9 C11 113.8(3) . . ? C10 C9 C11 110.1(3) . . ? C8 C12 C13 111.1(3) . . ? C8 C12 C14 112.2(3) . . ? C13 C12 C14 111.4(3) . . ? C20 C15 C16 120.2(3) . . ? C20 C15 N2 120.3(3) . . ? C16 C15 N2 119.5(3) . . ? C20 C15 K1 86.18(19) . . ? C16 C15 K1 76.46(19) . . ? N2 C15 K1 108.26(18) . . ? C17 C16 C15 118.0(4) . . ? C17 C16 C21 120.1(3) . . ? C15 C16 C21 121.9(3) . . ? C17 C16 K1 82.5(2) . . ? C15 C16 K1 81.2(2) . . ? C21 C16 K1 107.3(2) . . ? C18 C17 C16 121.8(4) . . ? C18 C17 K1 86.6(3) . . ? C16 C17 K1 75.4(2) . . ? C19 C18 C17 119.9(4) . . ? C18 C19 C20 121.5(4) . . ? C15 C20 C19 118.6(3) . . ? C15 C20 C24 122.1(3) . . ? C19 C20 C24 119.2(3) . . ? C16 C21 C23 112.3(4) . . ? C16 C21 C22 112.7(4) . . ? C23 C21 C22 111.2(4) . . ? C20 C24 C26 112.9(4) . . ? C20 C24 C25 111.4(3) . . ? C26 C24 C25 108.7(4) . . ? C31 C27 C28 108.9(4) . . ? C31 C27 Co2 69.7(2) . . ? C28 C27 Co2 70.0(2) . . ? C27 C28 C29 107.1(4) . . ? C27 C28 Co2 70.8(2) . . ? C29 C28 Co2 70.2(2) . . ? C30 C29 C28 107.5(5) . . ? C30 C29 Co2 70.6(3) . . ? C28 C29 Co2 69.9(2) . . ? C29 C30 C31 109.0(5) . . ? C29 C30 Co2 70.6(3) . . ? C31 C30 Co2 69.8(3) . . ? C27 C31 C30 107.4(5) . . ? C27 C31 Co2 71.3(2) . . ? C30 C31 Co2 70.8(3) . . ? O1 C32 Co2 178.2(4) . . ? O1 C32 K1 81.3(3) . . ? Co2 C32 K1 100.28(17) . . ? N3 C35 C36 114.3(3) . . ? N4 C36 C35 113.9(3) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.918 _refine_diff_density_min -0.737 _refine_diff_density_rms 0.079 # Attachment 'compd16.cif' data_compound16 _database_code_depnum_ccdc_archive 'CCDC 603230' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H112 Ga2 K N6 O V' _chemical_formula_weight 1331.18 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c 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 22.944(5) _cell_length_b 12.436(3) _cell_length_c 27.243(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.47(3) _cell_angle_gamma 90.00 _cell_volume 7689(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.150 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2840 _exptl_absorpt_coefficient_mu 0.912 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.676 _exptl_absorpt_correction_T_max 0.809 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _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 12562 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.0609 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6726 _reflns_number_gt 5407 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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 'calc w=1/[\s^2^(Fo^2^)+(0.0624P)^2^+74.8804P] 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 6726 _refine_ls_number_parameters 452 _refine_ls_number_restraints 61 _refine_ls_R_factor_all 0.0907 _refine_ls_R_factor_gt 0.0736 _refine_ls_wR_factor_ref 0.1981 _refine_ls_wR_factor_gt 0.1903 _refine_ls_goodness_of_fit_ref 1.141 _refine_ls_restrained_S_all 1.153 _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 Ga1 Ga 0.42900(2) 0.33574(5) 0.22717(2) 0.0235(2) Uani 1 1 d . . . V1 V 0.5000 0.18414(10) 0.2500 0.0227(3) Uani 1 2 d S . . K1 K 0.42562(14) 0.0724(2) 0.05723(11) 0.0434(7) Uani 0.50 1 d P . . O1 O 0.3272(6) -0.0764(11) 0.0380(5) 0.089(4) Uani 0.50 1 d PDU . . N1 N 0.3887(2) 0.3922(4) 0.16372(17) 0.0275(10) Uani 1 1 d . . . N2 N 0.3838(2) 0.4420(4) 0.25681(17) 0.0275(10) Uani 1 1 d . . . N3 N 0.5413(3) -0.0235(7) 0.0461(3) 0.077(2) Uani 1 1 d . . . C1 C 0.3527(2) 0.4781(5) 0.1732(2) 0.0292(13) Uani 1 1 d . . . H1 H 0.3301 0.5163 0.1468 0.035 Uiso 1 1 calc R . . C2 C 0.3510(2) 0.5048(5) 0.2202(2) 0.0312(13) Uani 1 1 d . . . H2 H 0.3283 0.5641 0.2286 0.037 Uiso 1 1 calc R . . C3 C 0.3684(2) 0.3365(5) 0.1183(2) 0.0282(12) Uani 1 1 d . . . C4 C 0.3987(3) 0.3461(5) 0.0771(2) 0.0335(14) Uani 1 1 d . . . C5 C 0.3759(3) 0.2942(6) 0.0329(3) 0.0454(17) Uani 1 1 d . . . H5 H 0.3958 0.3010 0.0049 0.055 Uiso 1 1 calc R . . C6 C 0.3257(3) 0.2341(6) 0.0290(3) 0.0496(18) Uani 1 1 d . . . H6 H 0.3112 0.1993 -0.0014 0.059 Uiso 1 1 calc R . . C7 C 0.2964(3) 0.2241(6) 0.0690(3) 0.0474(17) Uani 1 1 d . . . H7 H 0.2618 0.1812 0.0662 0.057 Uiso 1 1 calc R . . C8 C 0.3162(3) 0.2756(5) 0.1140(2) 0.0340(14) Uani 1 1 d . . . C9 C 0.4526(3) 0.4170(5) 0.0784(2) 0.0399(15) Uani 1 1 d . . . H9 H 0.4693 0.4294 0.1140 0.048 Uiso 1 1 calc R . . C10 C 0.5008(4) 0.3656(8) 0.0529(3) 0.074(3) Uani 1 1 d . . . H10A H 0.5106 0.2946 0.0673 0.111 Uiso 1 1 calc R . . H10B H 0.5360 0.4113 0.0576 0.111 Uiso 1 1 calc R . . H10C H 0.4866 0.3580 0.0173 0.111 Uiso 1 1 calc R . . C11 C 0.4338(4) 0.5273(7) 0.0550(3) 0.072(3) Uani 1 1 d . . . H11A H 0.4688 0.5720 0.0541 0.107 Uiso 1 1 calc R . . H11B H 0.4073 0.5631 0.0749 0.107 Uiso 1 1 calc R . . H11C H 0.4134 0.5165 0.0211 0.107 Uiso 1 1 calc R . . C12 C 0.2799(3) 0.2665(5) 0.1562(3) 0.0373(15) Uani 1 1 d . . . H12 H 0.3018 0.3042 0.1858 0.045 Uiso 1 1 calc R . . C13 C 0.2712(3) 0.1481(6) 0.1709(3) 0.0529(19) Uani 1 1 d . . . H13A H 0.2476 0.1105 0.1432 0.079 Uiso 1 1 calc R . . H13B H 0.2507 0.1457 0.2001 0.079 Uiso 1 1 calc R . . H13C H 0.3097 0.1130 0.1788 0.079 Uiso 1 1 calc R . . C14 C 0.2194(3) 0.3225(6) 0.1428(3) 0.0523(19) Uani 1 1 d . . . H14A H 0.2002 0.2962 0.1105 0.078 Uiso 1 1 calc R . . H14B H 0.2252 0.4004 0.1411 0.078 Uiso 1 1 calc R . . H14C H 0.1946 0.3062 0.1682 0.078 Uiso 1 1 calc R . . C15 C 0.3797(2) 0.4688(5) 0.3070(2) 0.0298(13) Uani 1 1 d . . . C16 C 0.3418(2) 0.4080(5) 0.3332(2) 0.0320(14) Uani 1 1 d . . . C17 C 0.3372(3) 0.4364(5) 0.3823(2) 0.0367(15) Uani 1 1 d . . . H17 H 0.3134 0.3945 0.4008 0.044 Uiso 1 1 calc R . . C18 C 0.3670(3) 0.5249(6) 0.4041(2) 0.0406(16) Uani 1 1 d . . . H18 H 0.3625 0.5451 0.4370 0.049 Uiso 1 1 calc R . . C19 C 0.4039(3) 0.5848(5) 0.3779(2) 0.0368(15) Uani 1 1 d . . . H19 H 0.4250 0.6445 0.3934 0.044 Uiso 1 1 calc R . . C20 C 0.4101(2) 0.5576(5) 0.3292(2) 0.0304(13) Uani 1 1 d . . . C21 C 0.3030(3) 0.3187(5) 0.3079(3) 0.0381(15) Uani 1 1 d . . . H21 H 0.3234 0.2884 0.2810 0.046 Uiso 1 1 calc R . . C22 C 0.2919(3) 0.2254(6) 0.3423(3) 0.0482(18) Uani 1 1 d . . . H22A H 0.2663 0.2500 0.3659 0.072 Uiso 1 1 calc R . . H22B H 0.3295 0.2006 0.3605 0.072 Uiso 1 1 calc R . . H22C H 0.2727 0.1661 0.3224 0.072 Uiso 1 1 calc R . . C23 C 0.2434(3) 0.3658(6) 0.2830(3) 0.0478(17) Uani 1 1 d . . . H23A H 0.2222 0.3960 0.3084 0.072 Uiso 1 1 calc R . . H23B H 0.2198 0.3086 0.2651 0.072 Uiso 1 1 calc R . . H23C H 0.2507 0.4224 0.2596 0.072 Uiso 1 1 calc R . . C24 C 0.4482(3) 0.6269(5) 0.3012(2) 0.0329(14) Uani 1 1 d . . . H24 H 0.4513 0.5898 0.2691 0.040 Uiso 1 1 calc R . . C25 C 0.4187(3) 0.7370(5) 0.2886(3) 0.0443(17) Uani 1 1 d . . . H25A H 0.3799 0.7261 0.2688 0.066 Uiso 1 1 calc R . . H25B H 0.4433 0.7801 0.2697 0.066 Uiso 1 1 calc R . . H25C H 0.4140 0.7747 0.3194 0.066 Uiso 1 1 calc R . . C26 C 0.5108(3) 0.6428(5) 0.3281(3) 0.0415(16) Uani 1 1 d . . . H26A H 0.5094 0.6795 0.3598 0.062 Uiso 1 1 calc R . . H26B H 0.5332 0.6866 0.3075 0.062 Uiso 1 1 calc R . . H26C H 0.5300 0.5727 0.3344 0.062 Uiso 1 1 calc R . . C27 C 0.6125(3) 0.0240(6) 0.2266(3) 0.0451(17) Uani 1 1 d . . . H27A H 0.6303 -0.0078 0.1995 0.068 Uiso 1 1 calc R . . H27B H 0.6022 -0.0331 0.2486 0.068 Uiso 1 1 calc R . . H27C H 0.6406 0.0735 0.2455 0.068 Uiso 1 1 calc R . . C28 C 0.5583(3) 0.0841(5) 0.2058(2) 0.0324(14) Uani 1 1 d . . . C29 C 0.4993(3) 0.0442(5) 0.1975(2) 0.0330(14) Uani 1 1 d . . . H29 H 0.4875 -0.0258 0.2061 0.040 Uiso 1 1 calc R . . C30 C 0.4612(3) 0.1241(5) 0.1747(2) 0.0373(15) Uani 1 1 d . . . H30 H 0.4197 0.1184 0.1656 0.045 Uiso 1 1 calc R . . C31 C 0.4962(3) 0.2142(5) 0.1678(2) 0.0344(14) Uani 1 1 d . . . H31 H 0.4823 0.2806 0.1534 0.041 Uiso 1 1 calc R . . C32 C 0.5555(3) 0.1892(5) 0.1860(2) 0.0330(14) Uani 1 1 d . . . H32 H 0.5882 0.2357 0.1851 0.040 Uiso 1 1 calc R . . C33 C 0.5850(6) 0.0530(10) 0.0712(4) 0.107(4) Uani 1 1 d . . . H33A H 0.6244 0.0210 0.0742 0.161 Uiso 1 1 calc R . . H33B H 0.5755 0.0694 0.1043 0.161 Uiso 1 1 calc R . . H33C H 0.5841 0.1194 0.0517 0.161 Uiso 1 1 calc R . . C34 C 0.5454(6) -0.1240(11) 0.0747(5) 0.121(5) Uani 1 1 d . . . H34A H 0.5823 -0.1608 0.0710 0.182 Uiso 1 1 calc R . . H34B H 0.5120 -0.1704 0.0623 0.182 Uiso 1 1 calc R . . H34C H 0.5448 -0.1077 0.1098 0.182 Uiso 1 1 calc R . . C35 C 0.5435(13) -0.059(2) 0.0017(11) 0.040(7) Uani 0.25 1 d PU . 1 C36 C 0.4812(14) -0.017(3) 0.0388(12) 0.054(8) Uani 0.25 1 d PU . 1 C37 C 0.5593(15) -0.009(3) -0.0006(13) 0.055(8) Uani 0.25 1 d PU . 2 C38 C 0.4963(15) 0.049(3) 0.0397(12) 0.057(8) Uani 0.25 1 d PU . 2 C39 C 0.2378(11) -0.059(2) -0.0321(9) 0.131(10) Uani 0.50 1 d PDU . . H39A H 0.2355 0.0099 -0.0499 0.196 Uiso 0.50 1 calc PR . . H39B H 0.1982 -0.0810 -0.0269 0.196 Uiso 0.50 1 calc PR . . H39C H 0.2548 -0.1136 -0.0517 0.196 Uiso 0.50 1 calc PR . . C40 C 0.2720(9) -0.047(2) 0.0119(8) 0.108(8) Uani 0.50 1 d PDU . . H40A H 0.2452 -0.0723 0.0349 0.130 Uiso 0.50 1 calc PR . . H40B H 0.2730 0.0317 0.0156 0.130 Uiso 0.50 1 calc PR . . C41 C 0.3294(10) -0.150(2) 0.0731(8) 0.113(8) Uani 0.50 1 d PDU . . H41A H 0.3284 -0.2207 0.0559 0.136 Uiso 0.50 1 calc PR . . H41B H 0.2918 -0.1447 0.0866 0.136 Uiso 0.50 1 calc PR . . C42 C 0.3731(6) -0.1585(13) 0.1135(6) 0.059(4) Uani 0.50 1 d PDU . . H42A H 0.4110 -0.1716 0.1021 0.088 Uiso 0.50 1 calc PR . . H42B H 0.3641 -0.2182 0.1347 0.088 Uiso 0.50 1 calc PR . . H42C H 0.3751 -0.0913 0.1325 0.088 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga1 0.0204(3) 0.0249(3) 0.0247(3) -0.0001(3) 0.0013(2) 0.0001(2) V1 0.0220(6) 0.0227(7) 0.0233(7) 0.000 0.0031(5) 0.000 K1 0.0480(17) 0.0457(16) 0.0374(16) 0.0014(13) 0.0097(13) 0.0075(14) O1 0.083(6) 0.095(6) 0.091(7) -0.005(5) 0.019(5) 0.034(5) N1 0.025(2) 0.031(3) 0.026(3) 0.003(2) -0.001(2) -0.001(2) N2 0.027(2) 0.028(2) 0.028(3) -0.001(2) 0.003(2) 0.005(2) N3 0.068(5) 0.101(6) 0.054(5) 0.012(4) -0.016(4) 0.009(5) C1 0.025(3) 0.030(3) 0.031(3) 0.006(3) -0.002(2) 0.002(2) C2 0.025(3) 0.027(3) 0.040(4) 0.001(3) 0.001(3) 0.003(2) C3 0.027(3) 0.029(3) 0.027(3) 0.007(2) -0.002(2) 0.003(2) C4 0.037(3) 0.035(3) 0.026(3) 0.001(3) -0.004(3) 0.003(3) C5 0.042(4) 0.060(4) 0.032(4) -0.009(3) -0.003(3) 0.003(3) C6 0.039(4) 0.066(5) 0.039(4) -0.017(4) -0.011(3) 0.001(4) C7 0.032(3) 0.054(4) 0.052(5) -0.011(4) -0.010(3) -0.002(3) C8 0.026(3) 0.034(3) 0.039(4) 0.000(3) -0.006(3) 0.004(3) C9 0.049(4) 0.047(4) 0.024(3) -0.001(3) 0.009(3) -0.015(3) C10 0.067(5) 0.098(7) 0.066(6) -0.040(5) 0.038(5) -0.044(5) C11 0.106(7) 0.057(5) 0.044(5) 0.012(4) -0.011(5) -0.026(5) C12 0.027(3) 0.040(4) 0.044(4) 0.003(3) 0.001(3) -0.006(3) C13 0.042(4) 0.054(4) 0.061(5) 0.004(4) 0.000(3) -0.012(3) C14 0.027(3) 0.061(5) 0.070(5) 0.014(4) 0.010(3) -0.001(3) C15 0.025(3) 0.036(3) 0.028(3) 0.001(3) 0.001(2) 0.009(3) C16 0.021(3) 0.039(3) 0.035(3) 0.000(3) 0.005(2) 0.011(3) C17 0.027(3) 0.051(4) 0.032(3) 0.003(3) 0.005(3) 0.006(3) C18 0.033(3) 0.058(4) 0.032(4) -0.004(3) 0.009(3) 0.010(3) C19 0.034(3) 0.039(3) 0.037(4) -0.012(3) 0.003(3) 0.004(3) C20 0.021(3) 0.034(3) 0.036(3) -0.002(3) 0.004(2) 0.005(2) C21 0.027(3) 0.043(4) 0.046(4) -0.001(3) 0.010(3) -0.001(3) C22 0.044(4) 0.045(4) 0.059(5) 0.004(3) 0.018(3) -0.008(3) C23 0.032(3) 0.053(4) 0.057(5) -0.006(4) 0.001(3) -0.002(3) C24 0.031(3) 0.027(3) 0.040(4) 0.002(3) 0.003(3) 0.002(3) C25 0.038(4) 0.033(3) 0.062(5) -0.002(3) 0.009(3) 0.005(3) C26 0.032(3) 0.042(4) 0.049(4) -0.002(3) 0.001(3) 0.001(3) C27 0.036(4) 0.050(4) 0.048(4) -0.006(3) 0.002(3) 0.007(3) C28 0.038(3) 0.032(3) 0.028(3) -0.006(3) 0.006(3) 0.006(3) C29 0.035(3) 0.032(3) 0.032(3) -0.009(3) 0.006(3) -0.005(3) C30 0.033(3) 0.054(4) 0.025(3) -0.010(3) 0.005(3) 0.001(3) C31 0.041(3) 0.042(3) 0.021(3) 0.004(3) 0.009(3) 0.011(3) C32 0.036(3) 0.034(3) 0.030(3) -0.012(3) 0.009(3) -0.007(3) C33 0.119(10) 0.125(10) 0.080(8) -0.024(7) 0.023(7) -0.022(8) C34 0.126(11) 0.120(10) 0.124(11) 0.030(9) 0.036(9) 0.013(9) C35 0.041(9) 0.041(9) 0.039(9) -0.004(6) 0.007(6) 0.003(6) C36 0.055(10) 0.058(10) 0.051(10) 0.002(7) 0.011(7) 0.003(7) C37 0.057(10) 0.057(10) 0.052(10) -0.002(7) 0.008(7) 0.000(7) C38 0.059(10) 0.058(10) 0.055(10) -0.001(7) 0.007(7) 0.002(7) C39 0.130(11) 0.125(11) 0.134(11) -0.001(7) 0.012(7) 0.007(7) C40 0.113(10) 0.111(10) 0.100(9) -0.004(7) 0.016(7) -0.003(7) C41 0.111(10) 0.121(10) 0.113(10) 0.004(7) 0.036(7) -0.027(7) C42 0.048(6) 0.064(7) 0.067(7) 0.016(5) 0.016(5) 0.012(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. The anion of the compound was found to sit on a 2-fold rotation axis. The K(OEt2)(tmeda) cation of the compound was found to be site disordered over a centre of inversion. Disorder was also found within the ethylene fragment of the site disordered tmeda nolecule. This was successfully modelled, though the ethylene protons have not been included in the refinement. However, the empirical formula, formula weight and F(000) values used in the final refinement take into account the contribution from these protons. ; 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 Ga1 N2 1.930(4) . ? Ga1 N1 1.966(5) . ? Ga1 V1 2.5093(12) . ? V1 C30 2.241(6) . ? V1 C30 2.241(6) 2_655 ? V1 C29 2.251(6) . ? V1 C29 2.251(6) 2_655 ? V1 C31 2.259(6) . ? V1 C31 2.259(6) 2_655 ? V1 C28 2.294(6) 2_655 ? V1 C28 2.294(6) . ? V1 C32 2.306(6) . ? V1 C32 2.306(6) 2_655 ? V1 Ga1 2.5093(12) 2_655 ? K1 O1 2.907(15) . ? K1 N3 2.965(9) . ? K1 C5 3.022(8) . ? K1 C6 3.061(8) . ? K1 N3 3.082(9) 5_655 ? K1 C30 3.248(7) . ? K1 C4 3.516(7) . ? O1 C41 1.323(16) . ? O1 C40 1.404(15) . ? N1 C1 1.398(7) . ? N1 C3 1.433(7) . ? N2 C2 1.396(7) . ? N2 C15 1.423(7) . ? N3 C35 1.30(3) . ? N3 C38 1.36(3) . ? N3 C36 1.37(3) . ? N3 C37 1.41(4) . ? N3 C34 1.468(14) . ? N3 C33 1.475(13) . ? N3 K1 3.082(9) 5_655 ? C1 C2 1.330(8) . ? C3 C8 1.407(8) . ? C3 C4 1.410(8) . ? C4 C5 1.398(9) . ? C4 C9 1.516(9) . ? C5 C6 1.363(10) . ? C6 C7 1.369(10) . ? C7 C8 1.398(9) . ? C8 C12 1.522(9) . ? C9 C10 1.530(10) . ? C9 C11 1.547(10) . ? C12 C14 1.547(9) . ? C12 C13 1.547(9) . ? C15 C20 1.395(8) . ? C15 C16 1.421(8) . ? C16 C17 1.404(8) . ? C16 C21 1.523(9) . ? C17 C18 1.383(9) . ? C18 C19 1.401(9) . ? C19 C20 1.397(8) . ? C20 C24 1.512(8) . ? C21 C22 1.536(9) . ? C21 C23 1.548(9) . ? C24 C26 1.526(8) . ? C24 C25 1.545(8) . ? C27 C28 1.490(9) . ? C28 C32 1.413(9) . ? C28 C29 1.429(8) . ? C29 C30 1.406(9) . ? C30 C31 1.407(9) . ? C31 C32 1.412(9) . ? C35 C36 1.50(4) 5_655 ? C35 K1 1.85(3) 5_655 ? C36 C35 1.50(4) 5_655 ? C37 C38 1.61(5) 5_655 ? C37 K1 1.81(3) 5_655 ? C38 C37 1.61(5) 5_655 ? C39 C40 1.340(17) . ? C41 C42 1.380(16) . ? 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 Ga1 N1 84.9(2) . . ? N2 Ga1 V1 141.30(14) . . ? N1 Ga1 V1 133.64(14) . . ? C30 V1 C30 141.1(4) . 2_655 ? C30 V1 C29 36.5(2) . . ? C30 V1 C29 106.8(2) 2_655 . ? C30 V1 C29 106.8(2) . 2_655 ? C30 V1 C29 36.5(2) 2_655 2_655 ? C29 V1 C29 78.7(3) . 2_655 ? C30 V1 C31 36.4(2) . . ? C30 V1 C31 156.2(2) 2_655 . ? C29 V1 C31 60.2(2) . . ? C29 V1 C31 138.9(2) 2_655 . ? C30 V1 C31 156.2(2) . 2_655 ? C30 V1 C31 36.4(2) 2_655 2_655 ? C29 V1 C31 138.9(2) . 2_655 ? C29 V1 C31 60.2(2) 2_655 2_655 ? C31 V1 C31 161.0(3) . 2_655 ? C30 V1 C28 96.7(2) . 2_655 ? C30 V1 C28 61.5(2) 2_655 2_655 ? C29 V1 C28 87.9(2) . 2_655 ? C29 V1 C28 36.6(2) 2_655 2_655 ? C31 V1 C28 132.0(2) . 2_655 ? C31 V1 C28 60.6(2) 2_655 2_655 ? C30 V1 C28 61.5(2) . . ? C30 V1 C28 96.7(2) 2_655 . ? C29 V1 C28 36.6(2) . . ? C29 V1 C28 87.9(2) 2_655 . ? C31 V1 C28 60.6(2) . . ? C31 V1 C28 132.0(2) 2_655 . ? C28 V1 C28 114.3(3) 2_655 . ? C30 V1 C32 60.4(2) . . ? C30 V1 C32 120.8(2) 2_655 . ? C29 V1 C32 59.6(2) . . ? C29 V1 C32 123.2(2) 2_655 . ? C31 V1 C32 36.0(2) . . ? C31 V1 C32 143.1(2) 2_655 . ? C28 V1 C32 147.3(2) 2_655 . ? C28 V1 C32 35.8(2) . . ? C30 V1 C32 120.8(2) . 2_655 ? C30 V1 C32 60.4(2) 2_655 2_655 ? C29 V1 C32 123.2(2) . 2_655 ? C29 V1 C32 59.6(2) 2_655 2_655 ? C31 V1 C32 143.1(2) . 2_655 ? C31 V1 C32 36.0(2) 2_655 2_655 ? C28 V1 C32 35.8(2) 2_655 2_655 ? C28 V1 C32 147.3(2) . 2_655 ? C32 V1 C32 176.8(3) . 2_655 ? C30 V1 Ga1 129.29(17) . 2_655 ? C30 V1 Ga1 82.38(17) 2_655 2_655 ? C29 V1 Ga1 133.02(15) . 2_655 ? C29 V1 Ga1 118.65(16) 2_655 2_655 ? C31 V1 Ga1 92.89(17) . 2_655 ? C31 V1 Ga1 72.62(16) 2_655 2_655 ? C28 V1 Ga1 133.23(15) 2_655 2_655 ? C28 V1 Ga1 97.49(16) . 2_655 ? C32 V1 Ga1 75.89(15) . 2_655 ? C32 V1 Ga1 101.68(16) 2_655 2_655 ? C30 V1 Ga1 82.38(17) . . ? C30 V1 Ga1 129.29(17) 2_655 . ? C29 V1 Ga1 118.65(16) . . ? C29 V1 Ga1 133.02(15) 2_655 . ? C31 V1 Ga1 72.62(16) . . ? C31 V1 Ga1 92.89(17) 2_655 . ? C28 V1 Ga1 97.49(16) 2_655 . ? C28 V1 Ga1 133.23(15) . . ? C32 V1 Ga1 101.68(16) . . ? C32 V1 Ga1 75.89(15) 2_655 . ? Ga1 V1 Ga1 82.59(5) 2_655 . ? O1 K1 N3 114.1(3) . . ? O1 K1 C5 106.4(3) . . ? N3 K1 C5 131.3(2) . . ? O1 K1 C6 80.8(3) . . ? N3 K1 C6 152.4(2) . . ? C5 K1 C6 25.88(19) . . ? O1 K1 N3 90.0(3) . 5_655 ? N3 K1 N3 58.8(2) . 5_655 ? C5 K1 N3 96.7(2) . 5_655 ? C6 K1 N3 100.1(2) . 5_655 ? O1 K1 C30 112.3(3) . . ? N3 K1 C30 94.7(2) . . ? C5 K1 C30 93.84(19) . . ? C6 K1 C30 100.82(19) . . ? N3 K1 C30 151.5(2) 5_655 . ? O1 K1 C4 119.6(3) . . ? N3 K1 C4 125.8(2) . . ? C5 K1 C4 23.14(16) . . ? C6 K1 C4 42.31(17) . . ? N3 K1 C4 113.8(2) 5_655 . ? C30 K1 C4 71.38(17) . . ? C41 O1 C40 118.7(17) . . ? C41 O1 K1 111.5(12) . . ? C40 O1 K1 123.2(13) . . ? C1 N1 C3 113.7(4) . . ? C1 N1 Ga1 109.0(4) . . ? C3 N1 Ga1 129.6(4) . . ? C2 N2 C15 116.8(5) . . ? C2 N2 Ga1 110.5(4) . . ? C15 N2 Ga1 132.7(4) . . ? C35 N3 C38 104.0(19) . . ? C35 N3 C36 93.6(19) . . ? C38 N3 C36 38.0(17) . . ? C35 N3 C37 30.9(15) . . ? C38 N3 C37 97(2) . . ? C36 N3 C37 107(2) . . ? C35 N3 C34 101.1(16) . . ? C38 N3 C34 128.3(17) . . ? C36 N3 C34 96.5(17) . . ? C37 N3 C34 125.6(17) . . ? C35 N3 C33 122.4(16) . . ? C38 N3 C33 94.8(17) . . ? C36 N3 C33 129.1(17) . . ? C37 N3 C33 93.9(17) . . ? C34 N3 C33 108.4(9) . . ? C35 N3 K1 113.1(13) . . ? C38 N3 K1 22.2(15) . . ? C36 N3 K1 24.7(15) . . ? C37 N3 K1 115.4(14) . . ? C34 N3 K1 106.1(7) . . ? C33 N3 K1 104.5(7) . . ? C35 N3 K1 14.5(14) . 5_655 ? C38 N3 K1 107.4(15) . 5_655 ? C36 N3 K1 105.0(14) . 5_655 ? C37 N3 K1 18.8(16) . 5_655 ? C34 N3 K1 108.1(7) . 5_655 ? C33 N3 K1 108.0(6) . 5_655 ? K1 N3 K1 121.2(2) . 5_655 ? C2 C1 N1 118.1(5) . . ? C1 C2 N2 117.3(5) . . ? C8 C3 C4 119.4(5) . . ? C8 C3 N1 119.8(5) . . ? C4 C3 N1 120.7(5) . . ? C5 C4 C3 118.8(6) . . ? C5 C4 C9 119.4(6) . . ? C3 C4 C9 121.7(5) . . ? C5 C4 K1 58.2(4) . . ? C3 C4 K1 99.2(4) . . ? C9 C4 K1 113.9(4) . . ? C6 C5 C4 121.7(7) . . ? C6 C5 K1 78.7(5) . . ? C4 C5 K1 98.7(4) . . ? C5 C6 C7 119.7(6) . . ? C5 C6 K1 75.4(4) . . ? C7 C6 K1 100.2(5) . . ? C6 C7 C8 121.5(6) . . ? C7 C8 C3 118.9(6) . . ? C7 C8 C12 119.0(6) . . ? C3 C8 C12 122.0(5) . . ? C4 C9 C10 112.8(6) . . ? C4 C9 C11 109.2(6) . . ? C10 C9 C11 111.0(7) . . ? C8 C12 C14 111.0(5) . . ? C8 C12 C13 111.9(6) . . ? C14 C12 C13 110.1(5) . . ? C20 C15 C16 120.5(5) . . ? C20 C15 N2 120.1(5) . . ? C16 C15 N2 119.3(5) . . ? C17 C16 C15 118.9(6) . . ? C17 C16 C21 119.6(5) . . ? C15 C16 C21 121.4(5) . . ? C18 C17 C16 120.5(6) . . ? C17 C18 C19 120.2(6) . . ? C20 C19 C18 120.6(6) . . ? C15 C20 C19 119.3(6) . . ? C15 C20 C24 121.5(5) . . ? C19 C20 C24 119.2(5) . . ? C16 C21 C22 114.4(6) . . ? C16 C21 C23 110.0(5) . . ? C22 C21 C23 109.8(5) . . ? C20 C24 C26 113.9(5) . . ? C20 C24 C25 110.4(5) . . ? C26 C24 C25 110.0(5) . . ? C32 C28 C29 105.8(5) . . ? C32 C28 C27 126.7(6) . . ? C29 C28 C27 127.2(6) . . ? C32 C28 V1 72.6(3) . . ? C29 C28 V1 70.1(3) . . ? C27 C28 V1 126.2(4) . . ? C30 C29 C28 109.7(5) . . ? C30 C29 V1 71.4(3) . . ? C28 C29 V1 73.3(3) . . ? C29 C30 C31 107.0(5) . . ? C29 C30 V1 72.2(3) . . ? C31 C30 V1 72.5(4) . . ? C29 C30 K1 110.2(4) . . ? C31 C30 K1 95.3(4) . . ? V1 C30 K1 167.5(3) . . ? C30 C31 C32 108.6(6) . . ? C30 C31 V1 71.1(3) . . ? C32 C31 V1 73.8(3) . . ? C31 C32 C28 108.9(5) . . ? C31 C32 V1 70.2(3) . . ? C28 C32 V1 71.6(3) . . ? N3 C35 C36 114(2) . 5_655 ? N3 C35 K1 155(2) . 5_655 ? C36 C35 K1 64.5(16) 5_655 5_655 ? N3 C36 C35 114(3) . 5_655 ? N3 C37 C38 104(3) . 5_655 ? N3 C37 K1 147(3) . 5_655 ? C38 C37 K1 62.4(17) 5_655 5_655 ? N3 C38 C37 113(3) . 5_655 ? C39 C40 O1 142(2) . . ? O1 C41 C42 125.0(18) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.354 _refine_diff_density_min -0.499 _refine_diff_density_rms 0.103 # Attachment 'compd6.cif' data_compound6 _database_code_depnum_ccdc_archive 'CCDC 603231' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H57 Ga K N4 O3 V' _chemical_formula_weight 801.66 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 31.855(6) _cell_length_b 10.205(2) _cell_length_c 25.904(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8421(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.265 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3376 _exptl_absorpt_coefficient_mu 1.000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.705 _exptl_absorpt_correction_T_max 0.889 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _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 48240 _diffrn_reflns_av_R_equivalents 0.1080 _diffrn_reflns_av_sigmaI/netI 0.1110 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.36 _reflns_number_total 15263 _reflns_number_gt 11676 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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. The asymmetric unit contains two crystallographically independent molecules which show no significant geometric differences. ; _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^)+(0.0407P)^2^+7.7162P] 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 0.010(11) _refine_ls_number_reflns 15263 _refine_ls_number_parameters 926 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0889 _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.1252 _refine_ls_wR_factor_gt 0.1140 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.036 _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 Ga1 Ga 0.785008(18) 0.38586(6) 0.73655(2) 0.02687(15) Uani 1 1 d . . . Ga2 Ga 0.506642(17) 0.19203(6) 0.92973(2) 0.02391(15) Uani 1 1 d . . . V1 V 0.75365(3) 0.16540(10) 0.73749(4) 0.0348(3) Uani 1 1 d . . . V2 V 0.52558(3) 0.41775(10) 0.95358(4) 0.0272(2) Uani 1 1 d . . . K1 K 0.83086(4) 0.23080(14) 0.54227(5) 0.0376(3) Uani 1 1 d . . . K2 K 0.59939(4) 0.36621(15) 0.78078(5) 0.0423(4) Uani 1 1 d . . . O1 O 0.79360(15) 0.2214(5) 0.63244(15) 0.0539(14) Uani 1 1 d . . . O2 O 0.68335(18) 0.0831(7) 0.6634(2) 0.088(2) Uani 1 1 d . . . O3 O 0.68240(14) 0.3626(5) 0.75676(17) 0.0549(13) Uani 1 1 d . . . O4 O 0.52901(13) 0.3962(5) 0.83566(15) 0.0436(11) Uani 1 1 d . . . O5 O 0.60826(14) 0.5369(5) 0.9184(2) 0.0659(16) Uani 1 1 d . . . O6 O 0.59018(14) 0.2341(5) 1.00296(15) 0.0445(11) Uani 1 1 d . . . N1 N 0.79868(15) 0.5250(5) 0.69081(16) 0.0280(11) Uani 1 1 d . . . N2 N 0.80578(15) 0.4926(5) 0.79004(16) 0.0303(12) Uani 1 1 d . . . N3 N 0.76765(18) 0.0468(7) 0.5115(2) 0.0540(17) Uani 1 1 d . . . N4 N 0.84560(18) -0.0278(6) 0.5740(2) 0.0520(16) Uani 1 1 d . . . N5 N 0.47059(14) 0.0681(5) 0.96025(16) 0.0269(11) Uani 1 1 d . . . N6 N 0.52140(14) 0.0585(5) 0.88238(15) 0.0268(11) Uani 1 1 d . . . N7 N 0.58030(18) 0.4324(6) 0.6780(2) 0.0479(15) Uani 1 1 d . . . N8 N 0.5902(2) 0.6349(6) 0.7620(2) 0.0537(16) Uani 1 1 d . . . C1 C 0.81568(19) 0.6297(6) 0.7191(2) 0.0304(14) Uani 1 1 d . . . H1 H 0.8250 0.7078 0.7027 0.036 Uiso 1 1 calc R . . C2 C 0.81819(18) 0.6135(6) 0.7709(2) 0.0330(15) Uani 1 1 d . . . H2 H 0.8279 0.6814 0.7929 0.040 Uiso 1 1 calc R . . C3 C 0.80732(17) 0.5258(6) 0.63636(19) 0.0255(13) Uani 1 1 d . . . C4 C 0.77526(18) 0.5392(6) 0.6010(2) 0.0294(14) Uani 1 1 d . . . C5 C 0.78510(19) 0.5441(6) 0.5482(2) 0.0337(14) Uani 1 1 d . . . H5 H 0.7631 0.5493 0.5235 0.040 Uiso 1 1 calc R . . C6 C 0.82638(19) 0.5414(6) 0.5316(2) 0.0347(15) Uani 1 1 d . . . H6 H 0.8328 0.5509 0.4960 0.042 Uiso 1 1 calc R . . C7 C 0.85825(19) 0.5247(6) 0.5671(2) 0.0351(15) Uani 1 1 d . . . H7 H 0.8864 0.5193 0.5553 0.042 Uiso 1 1 calc R . . C8 C 0.85020(17) 0.5157(6) 0.6197(2) 0.0300(14) Uani 1 1 d . . . C9 C 0.72967(19) 0.5530(7) 0.6194(2) 0.0363(16) Uani 1 1 d . . . H9 H 0.7255 0.4905 0.6487 0.044 Uiso 1 1 calc R . . C10 C 0.7217(2) 0.6900(8) 0.6397(3) 0.0533(19) Uani 1 1 d . . . H10A H 0.7447 0.7155 0.6628 0.080 Uiso 1 1 calc R . . H10B H 0.6951 0.6915 0.6587 0.080 Uiso 1 1 calc R . . H10C H 0.7203 0.7515 0.6107 0.080 Uiso 1 1 calc R . . C11 C 0.6976(2) 0.5185(9) 0.5774(2) 0.056(2) Uani 1 1 d . . . H11A H 0.6998 0.5816 0.5490 0.084 Uiso 1 1 calc R . . H11B H 0.6692 0.5219 0.5920 0.084 Uiso 1 1 calc R . . H11C H 0.7032 0.4301 0.5644 0.084 Uiso 1 1 calc R . . C12 C 0.88564(18) 0.4873(7) 0.6570(2) 0.0372(15) Uani 1 1 d . . . H12 H 0.8734 0.4853 0.6925 0.045 Uiso 1 1 calc R . . C13 C 0.9186(2) 0.5973(8) 0.6559(3) 0.055(2) Uani 1 1 d . . . H13A H 0.9320 0.5998 0.6218 0.083 Uiso 1 1 calc R . . H13B H 0.9399 0.5805 0.6824 0.083 Uiso 1 1 calc R . . H13C H 0.9050 0.6815 0.6628 0.083 Uiso 1 1 calc R . . C14 C 0.9053(2) 0.3536(8) 0.6470(3) 0.065(2) Uani 1 1 d . . . H14A H 0.8835 0.2859 0.6488 0.098 Uiso 1 1 calc R . . H14B H 0.9268 0.3361 0.6730 0.098 Uiso 1 1 calc R . . H14C H 0.9180 0.3529 0.6126 0.098 Uiso 1 1 calc R . . C15 C 0.81598(18) 0.4554(6) 0.8421(2) 0.0289(14) Uani 1 1 d . . . C16 C 0.85559(18) 0.4049(7) 0.8536(2) 0.0376(16) Uani 1 1 d . . . C17 C 0.8637(2) 0.3608(7) 0.9036(2) 0.0438(17) Uani 1 1 d . . . H17 H 0.8901 0.3225 0.9117 0.053 Uiso 1 1 calc R . . C18 C 0.8331(2) 0.3730(7) 0.9419(2) 0.0520(19) Uani 1 1 d . . . H18 H 0.8389 0.3446 0.9761 0.062 Uiso 1 1 calc R . . C19 C 0.7945(2) 0.4262(7) 0.9303(2) 0.0505(18) Uani 1 1 d . . . H19 H 0.7738 0.4328 0.9566 0.061 Uiso 1 1 calc R . . C20 C 0.78485(19) 0.4707(7) 0.8802(2) 0.0373(16) Uani 1 1 d . . . C21 C 0.8898(2) 0.3919(7) 0.8125(2) 0.0461(18) Uani 1 1 d . . . H21 H 0.8760 0.3985 0.7779 0.055 Uiso 1 1 calc R . . C22 C 0.9209(3) 0.4993(10) 0.8161(4) 0.099(3) Uani 1 1 d U . . H22A H 0.9351 0.4954 0.8496 0.148 Uiso 1 1 calc R . . H22B H 0.9065 0.5838 0.8125 0.148 Uiso 1 1 calc R . . H22C H 0.9417 0.4900 0.7884 0.148 Uiso 1 1 calc R . . C23 C 0.9119(4) 0.2622(12) 0.8148(5) 0.126(4) Uani 1 1 d U . . H23A H 0.9230 0.2405 0.7806 0.189 Uiso 1 1 calc R . . H23B H 0.8920 0.1942 0.8256 0.189 Uiso 1 1 calc R . . H23C H 0.9350 0.2670 0.8396 0.189 Uiso 1 1 calc R . . C24 C 0.7423(2) 0.5279(7) 0.8688(2) 0.0459(18) Uani 1 1 d . . . H24 H 0.7399 0.5376 0.8305 0.055 Uiso 1 1 calc R . . C25 C 0.7372(2) 0.6647(8) 0.8927(3) 0.069(2) Uani 1 1 d . . . H25A H 0.7416 0.6594 0.9301 0.104 Uiso 1 1 calc R . . H25B H 0.7088 0.6974 0.8856 0.104 Uiso 1 1 calc R . . H25C H 0.7579 0.7245 0.8776 0.104 Uiso 1 1 calc R . . C26 C 0.7070(2) 0.4370(8) 0.8865(3) 0.065(2) Uani 1 1 d . . . H26A H 0.7119 0.3487 0.8728 0.098 Uiso 1 1 calc R . . H26B H 0.6801 0.4701 0.8737 0.098 Uiso 1 1 calc R . . H26C H 0.7065 0.4337 0.9243 0.098 Uiso 1 1 calc R . . C27 C 0.7899(3) 0.1255(8) 0.8110(3) 0.069(3) Uani 1 1 d . . . H27 H 0.8028 0.1941 0.8300 0.083 Uiso 1 1 calc R . . C28 C 0.7496(3) 0.0728(12) 0.8163(3) 0.080(3) Uani 1 1 d . . . H28 H 0.7300 0.0996 0.8418 0.096 Uiso 1 1 calc R . . C29 C 0.7423(4) -0.0159(11) 0.7826(4) 0.091(3) Uani 1 1 d . . . H29 H 0.7162 -0.0596 0.7784 0.109 Uiso 1 1 calc R . . C30 C 0.7745(4) -0.0371(9) 0.7558(4) 0.085(3) Uani 1 1 d . . . H30 H 0.7763 -0.1029 0.7299 0.102 Uiso 1 1 calc R . . C31 C 0.8070(3) 0.0478(12) 0.7687(4) 0.086(3) Uani 1 1 d . . . H31 H 0.8340 0.0538 0.7535 0.103 Uiso 1 1 calc R . . C32 C 0.7790(2) 0.2047(6) 0.6732(2) 0.0384(16) Uani 1 1 d . . . C33 C 0.7099(2) 0.1120(8) 0.6911(3) 0.055(2) Uani 1 1 d . . . C34 C 0.7108(2) 0.2919(7) 0.7495(2) 0.0402(17) Uani 1 1 d . . . C35 C 0.7329(3) 0.0957(10) 0.5406(4) 0.092(3) Uani 1 1 d U . . H35A H 0.7246 0.1816 0.5272 0.137 Uiso 1 1 calc R . . H35B H 0.7410 0.1043 0.5770 0.137 Uiso 1 1 calc R . . H35C H 0.7092 0.0348 0.5377 0.137 Uiso 1 1 calc R . . C36 C 0.7538(2) 0.0408(9) 0.4566(3) 0.068(2) Uani 1 1 d . . . H36A H 0.7325 -0.0278 0.4527 0.103 Uiso 1 1 calc R . . H36B H 0.7779 0.0208 0.4345 0.103 Uiso 1 1 calc R . . H36C H 0.7418 0.1255 0.4465 0.103 Uiso 1 1 calc R . . C37 C 0.7835(3) -0.0886(8) 0.5272(3) 0.074(3) Uani 1 1 d . . . H37A H 0.7590 -0.1481 0.5293 0.089 Uiso 1 1 calc R . . H37B H 0.8018 -0.1217 0.4992 0.089 Uiso 1 1 calc R . . C38 C 0.8066(3) -0.0985(9) 0.5756(3) 0.068(2) Uani 1 1 d . . . H38A H 0.7891 -0.0636 0.6039 0.082 Uiso 1 1 calc R . . H38B H 0.8124 -0.1919 0.5830 0.082 Uiso 1 1 calc R . . C39 C 0.8611(3) -0.0273(10) 0.6287(3) 0.082(3) Uani 1 1 d . . . H39A H 0.8696 -0.1162 0.6385 0.123 Uiso 1 1 calc R . . H39B H 0.8387 0.0029 0.6516 0.123 Uiso 1 1 calc R . . H39C H 0.8853 0.0317 0.6316 0.123 Uiso 1 1 calc R . . C40 C 0.8781(2) -0.0865(8) 0.5415(3) 0.061(2) Uani 1 1 d . . . H40A H 0.8844 -0.1750 0.5540 0.092 Uiso 1 1 calc R . . H40B H 0.9035 -0.0327 0.5430 0.092 Uiso 1 1 calc R . . H40C H 0.8680 -0.0911 0.5058 0.092 Uiso 1 1 calc R . . C41 C 0.47385(18) -0.0512(6) 0.9360(2) 0.0326(14) Uani 1 1 d . . . H41 H 0.4584 -0.1254 0.9474 0.039 Uiso 1 1 calc R . . C42 C 0.50023(18) -0.0578(6) 0.8950(2) 0.0327(15) Uani 1 1 d . . . H42 H 0.5042 -0.1364 0.8760 0.039 Uiso 1 1 calc R . . C43 C 0.43971(17) 0.0840(6) 1.0000(2) 0.0269(13) Uani 1 1 d . . . C44 C 0.39894(19) 0.1252(6) 0.9880(2) 0.0360(15) Uani 1 1 d . . . C45 C 0.3699(2) 0.1397(7) 1.0286(3) 0.0490(18) Uani 1 1 d . . . H45 H 0.3422 0.1690 1.0213 0.059 Uiso 1 1 calc R . . C46 C 0.3809(2) 0.1124(8) 1.0778(3) 0.055(2) Uani 1 1 d . . . H46 H 0.3605 0.1209 1.1045 0.066 Uiso 1 1 calc R . . C47 C 0.4210(2) 0.0726(7) 1.0903(2) 0.0459(18) Uani 1 1 d . . . H47 H 0.4281 0.0544 1.1252 0.055 Uiso 1 1 calc R . . C48 C 0.45097(18) 0.0590(6) 1.0519(2) 0.0343(15) Uani 1 1 d . . . C49 C 0.38578(19) 0.1565(8) 0.9331(3) 0.056(2) Uani 1 1 d . . . H49 H 0.4114 0.1872 0.9144 0.067 Uiso 1 1 calc R . . C50 C 0.3530(3) 0.2672(9) 0.9297(4) 0.091(3) Uani 1 1 d . . . H50A H 0.3256 0.2340 0.9409 0.137 Uiso 1 1 calc R . . H50B H 0.3511 0.2981 0.8940 0.137 Uiso 1 1 calc R . . H50C H 0.3615 0.3398 0.9522 0.137 Uiso 1 1 calc R . . C51 C 0.3702(3) 0.0387(11) 0.9057(3) 0.089(3) Uani 1 1 d . . . H51A H 0.3901 -0.0334 0.9103 0.133 Uiso 1 1 calc R . . H51B H 0.3672 0.0583 0.8689 0.133 Uiso 1 1 calc R . . H51C H 0.3428 0.0134 0.9199 0.133 Uiso 1 1 calc R . . C52 C 0.4952(2) 0.0193(8) 1.0660(2) 0.0465(19) Uani 1 1 d . . . H52 H 0.5122 0.0184 1.0335 0.056 Uiso 1 1 calc R . . C53 C 0.4975(2) -0.1165(7) 1.0897(3) 0.0537(19) Uani 1 1 d . . . H53A H 0.4844 -0.1153 1.1239 0.081 Uiso 1 1 calc R . . H53B H 0.5270 -0.1430 1.0929 0.081 Uiso 1 1 calc R . . H53C H 0.4827 -0.1790 1.0675 0.081 Uiso 1 1 calc R . . C54 C 0.5145(3) 0.1199(8) 1.1023(3) 0.071(3) Uani 1 1 d . . . H54A H 0.5164 0.2048 1.0847 0.107 Uiso 1 1 calc R . . H54B H 0.5427 0.0912 1.1124 0.107 Uiso 1 1 calc R . . H54C H 0.4969 0.1287 1.1331 0.107 Uiso 1 1 calc R . . C55 C 0.54452(18) 0.0607(6) 0.83506(19) 0.0268(13) Uani 1 1 d . . . C56 C 0.58818(18) 0.0590(6) 0.8359(2) 0.0286(13) Uani 1 1 d . . . C57 C 0.6099(2) 0.0632(6) 0.7893(2) 0.0386(16) Uani 1 1 d . . . H57 H 0.6397 0.0649 0.7897 0.046 Uiso 1 1 calc R . . C58 C 0.5895(2) 0.0651(6) 0.7431(2) 0.0414(16) Uani 1 1 d . . . H58 H 0.6050 0.0648 0.7117 0.050 Uiso 1 1 calc R . . C59 C 0.5460(2) 0.0675(6) 0.7422(2) 0.0387(15) Uani 1 1 d . . . H59 H 0.5320 0.0707 0.7098 0.046 Uiso 1 1 calc R . . C60 C 0.5223(2) 0.0655(6) 0.7872(2) 0.0350(15) Uani 1 1 d . . . C61 C 0.61269(19) 0.0470(7) 0.8864(2) 0.0402(16) Uani 1 1 d . . . H61 H 0.5919 0.0459 0.9153 0.048 Uiso 1 1 calc R . . C62 C 0.6369(2) -0.0814(8) 0.8883(3) 0.061(2) Uani 1 1 d . . . H62A H 0.6170 -0.1549 0.8880 0.092 Uiso 1 1 calc R . . H62B H 0.6537 -0.0847 0.9199 0.092 Uiso 1 1 calc R . . H62C H 0.6554 -0.0875 0.8581 0.092 Uiso 1 1 calc R . . C63 C 0.6414(2) 0.1661(8) 0.8945(3) 0.057(2) Uani 1 1 d . . . H63A H 0.6591 0.1516 0.9249 0.086 Uiso 1 1 calc R . . H63B H 0.6242 0.2446 0.8998 0.086 Uiso 1 1 calc R . . H63C H 0.6591 0.1781 0.8640 0.086 Uiso 1 1 calc R . . C64 C 0.4745(2) 0.0635(7) 0.7848(2) 0.0458(18) Uani 1 1 d . . . H64 H 0.4646 0.0131 0.8156 0.055 Uiso 1 1 calc R . . C65 C 0.4563(2) -0.0045(9) 0.7373(3) 0.081(3) Uani 1 1 d . . . H65A H 0.4258 -0.0109 0.7407 0.121 Uiso 1 1 calc R . . H65B H 0.4683 -0.0926 0.7343 0.121 Uiso 1 1 calc R . . H65C H 0.4633 0.0464 0.7064 0.121 Uiso 1 1 calc R . . C66 C 0.4563(3) 0.1964(10) 0.7889(5) 0.103(4) Uani 1 1 d . . . H66A H 0.4659 0.2376 0.8210 0.155 Uiso 1 1 calc R . . H66B H 0.4256 0.1904 0.7891 0.155 Uiso 1 1 calc R . . H66C H 0.4654 0.2493 0.7594 0.155 Uiso 1 1 calc R . . C67 C 0.4811(3) 0.5911(8) 0.9578(3) 0.061(2) Uani 1 1 d . . . H67 H 0.4778 0.6499 0.9297 0.073 Uiso 1 1 calc R . . C68 C 0.4582(2) 0.4809(7) 0.9663(3) 0.0458(17) Uani 1 1 d . . . H68 H 0.4364 0.4490 0.9445 0.055 Uiso 1 1 calc R . . C69 C 0.4715(2) 0.4222(7) 1.0118(3) 0.0453(17) Uani 1 1 d . . . H69 H 0.4602 0.3452 1.0270 0.054 Uiso 1 1 calc R . . C70 C 0.5045(2) 0.4970(10) 1.0311(3) 0.060(2) Uani 1 1 d . . . H70 H 0.5202 0.4792 1.0616 0.072 Uiso 1 1 calc R . . C71 C 0.5106(3) 0.6031(8) 0.9976(4) 0.077(3) Uani 1 1 d . . . H71 H 0.5309 0.6706 1.0013 0.092 Uiso 1 1 calc R . . C72 C 0.52629(18) 0.3988(6) 0.8806(2) 0.0334(15) Uani 1 1 d . . . C73 C 0.57668(19) 0.4939(6) 0.9332(3) 0.0397(15) Uani 1 1 d . . . C74 C 0.56431(19) 0.2993(6) 0.9828(2) 0.0340(15) Uani 1 1 d . . . C75 C 0.5346(2) 0.4169(9) 0.6742(3) 0.074(3) Uani 1 1 d . . . H75A H 0.5209 0.4726 0.7000 0.111 Uiso 1 1 calc R . . H75B H 0.5271 0.3251 0.6804 0.111 Uiso 1 1 calc R . . H75C H 0.5252 0.4427 0.6396 0.111 Uiso 1 1 calc R . . C76 C 0.6009(3) 0.3470(9) 0.6407(3) 0.076(3) Uani 1 1 d . . . H76A H 0.5934 0.3744 0.6057 0.114 Uiso 1 1 calc R . . H76B H 0.5918 0.2564 0.6463 0.114 Uiso 1 1 calc R . . H76C H 0.6314 0.3527 0.6452 0.114 Uiso 1 1 calc R . . C77 C 0.5935(3) 0.5664(8) 0.6695(3) 0.066(2) Uani 1 1 d . . . H77A H 0.5839 0.5940 0.6348 0.079 Uiso 1 1 calc R . . H77B H 0.6245 0.5692 0.6696 0.079 Uiso 1 1 calc R . . C78 C 0.5774(3) 0.6644(8) 0.7088(3) 0.067(2) Uani 1 1 d . . . H78A H 0.5878 0.7527 0.6995 0.080 Uiso 1 1 calc R . . H78B H 0.5463 0.6665 0.7071 0.080 Uiso 1 1 calc R . . C79 C 0.5618(3) 0.7022(8) 0.7982(3) 0.066(2) Uani 1 1 d . . . H79A H 0.5626 0.7968 0.7916 0.099 Uiso 1 1 calc R . . H79B H 0.5709 0.6850 0.8337 0.099 Uiso 1 1 calc R . . H79C H 0.5331 0.6698 0.7934 0.099 Uiso 1 1 calc R . . C80 C 0.6342(3) 0.6757(9) 0.7712(3) 0.077(3) Uani 1 1 d . . . H80A H 0.6374 0.7683 0.7619 0.115 Uiso 1 1 calc R . . H80B H 0.6530 0.6224 0.7499 0.115 Uiso 1 1 calc R . . H80C H 0.6411 0.6636 0.8077 0.115 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 Ga1 0.0269(3) 0.0353(4) 0.0184(3) -0.0041(3) 0.0015(3) -0.0038(3) Ga2 0.0281(3) 0.0256(3) 0.0180(3) -0.0007(3) 0.0024(3) -0.0017(3) V1 0.0390(6) 0.0395(6) 0.0259(5) -0.0082(5) 0.0084(5) -0.0097(5) V2 0.0290(5) 0.0243(6) 0.0283(5) -0.0022(5) 0.0018(4) 0.0009(4) K1 0.0440(8) 0.0375(9) 0.0311(7) -0.0048(6) 0.0101(6) -0.0094(7) K2 0.0400(8) 0.0422(9) 0.0446(8) 0.0041(7) 0.0078(7) 0.0027(7) O1 0.071(3) 0.065(4) 0.026(2) -0.015(2) 0.020(2) -0.017(3) O2 0.063(4) 0.138(6) 0.062(3) -0.036(4) 0.002(3) -0.057(4) O3 0.031(3) 0.075(4) 0.059(3) -0.012(3) 0.004(2) 0.006(3) O4 0.054(3) 0.055(3) 0.023(2) 0.004(2) 0.011(2) -0.002(2) O5 0.037(3) 0.067(4) 0.094(4) 0.020(3) 0.014(3) -0.009(3) O6 0.046(3) 0.047(3) 0.039(2) 0.002(2) -0.011(2) 0.013(2) N1 0.032(3) 0.030(3) 0.022(2) -0.006(2) 0.003(2) 0.003(2) N2 0.034(3) 0.042(3) 0.015(2) -0.004(2) 0.001(2) 0.000(2) N3 0.047(4) 0.077(5) 0.038(3) 0.007(3) -0.004(3) -0.017(3) N4 0.044(3) 0.049(4) 0.063(4) 0.013(3) 0.010(3) -0.001(3) N5 0.035(3) 0.028(3) 0.018(2) -0.002(2) 0.007(2) 0.000(2) N6 0.039(3) 0.024(3) 0.017(2) -0.002(2) 0.006(2) -0.003(2) N7 0.059(4) 0.042(4) 0.042(3) 0.009(3) -0.008(3) -0.015(3) N8 0.075(4) 0.048(4) 0.037(3) -0.003(3) 0.000(3) 0.001(3) C1 0.041(3) 0.021(3) 0.029(3) -0.004(3) 0.004(3) -0.004(3) C2 0.036(3) 0.039(4) 0.024(3) -0.005(3) 0.000(3) 0.004(3) C3 0.028(3) 0.025(3) 0.024(3) -0.005(3) 0.004(2) -0.005(3) C4 0.035(3) 0.026(4) 0.027(3) 0.003(3) 0.000(3) -0.005(3) C5 0.038(3) 0.042(4) 0.021(3) -0.006(3) -0.001(3) -0.004(3) C6 0.045(4) 0.040(4) 0.019(3) -0.005(3) 0.004(3) -0.008(3) C7 0.036(4) 0.038(4) 0.032(3) -0.012(3) 0.007(3) -0.002(3) C8 0.033(3) 0.027(4) 0.031(3) -0.008(3) 0.002(3) -0.005(3) C9 0.034(3) 0.051(4) 0.024(3) 0.010(3) 0.001(3) -0.007(3) C10 0.042(4) 0.064(5) 0.054(4) -0.002(4) 0.008(3) 0.007(4) C11 0.035(4) 0.094(7) 0.039(4) -0.006(4) -0.003(3) 0.003(4) C12 0.034(3) 0.043(4) 0.035(3) -0.006(3) -0.002(3) 0.004(3) C13 0.037(4) 0.064(5) 0.065(5) -0.009(4) -0.008(4) -0.001(4) C14 0.058(5) 0.065(6) 0.073(5) -0.006(5) -0.009(4) 0.018(4) C15 0.037(3) 0.029(4) 0.020(3) -0.010(3) 0.000(3) -0.001(3) C16 0.035(4) 0.053(5) 0.025(3) -0.007(3) -0.001(3) 0.000(3) C17 0.042(4) 0.062(5) 0.028(3) 0.002(3) -0.007(3) -0.003(3) C18 0.063(5) 0.059(5) 0.034(4) -0.002(3) -0.004(3) -0.007(4) C19 0.046(4) 0.082(6) 0.023(3) -0.009(4) 0.007(3) -0.004(4) C20 0.038(4) 0.046(4) 0.027(3) -0.012(3) 0.004(3) 0.000(3) C21 0.034(4) 0.072(6) 0.032(3) -0.008(4) -0.006(3) 0.008(4) C22 0.098(5) 0.104(6) 0.095(5) -0.009(5) 0.032(5) -0.027(5) C23 0.118(6) 0.128(7) 0.133(6) -0.003(6) 0.050(5) 0.008(5) C24 0.045(4) 0.066(5) 0.027(3) -0.001(3) 0.003(3) 0.002(4) C25 0.057(5) 0.076(6) 0.074(5) -0.010(5) -0.005(4) 0.015(4) C26 0.038(4) 0.070(6) 0.088(6) -0.016(5) 0.006(4) -0.004(4) C27 0.107(7) 0.047(5) 0.053(5) 0.021(4) -0.047(5) -0.021(5) C28 0.084(7) 0.126(9) 0.031(4) 0.028(5) 0.026(4) 0.034(7) C29 0.117(9) 0.088(8) 0.068(6) 0.012(6) 0.007(6) -0.056(7) C30 0.098(8) 0.046(6) 0.110(9) -0.030(5) -0.001(7) 0.007(5) C31 0.041(5) 0.143(10) 0.075(6) 0.069(7) 0.023(4) 0.026(6) C32 0.042(4) 0.036(4) 0.036(4) -0.013(3) 0.005(3) -0.007(3) C33 0.051(5) 0.074(6) 0.039(4) -0.021(4) 0.020(3) -0.029(4) C34 0.042(4) 0.054(5) 0.025(3) -0.003(3) 0.000(3) -0.016(4) C35 0.083(5) 0.117(6) 0.075(5) -0.025(5) -0.004(4) -0.015(5) C36 0.054(5) 0.106(7) 0.045(4) -0.001(5) -0.011(4) -0.009(5) C37 0.116(7) 0.062(6) 0.045(4) 0.005(4) -0.010(5) -0.051(6) C38 0.073(6) 0.065(6) 0.067(5) 0.004(5) 0.006(4) -0.018(5) C39 0.086(6) 0.097(8) 0.063(5) 0.009(5) 0.018(5) 0.024(6) C40 0.066(5) 0.064(6) 0.054(4) 0.003(4) 0.003(4) -0.005(4) C41 0.042(3) 0.026(3) 0.030(3) 0.004(3) 0.006(3) 0.000(3) C42 0.043(4) 0.024(4) 0.031(3) -0.008(3) 0.000(3) -0.001(3) C43 0.031(3) 0.021(3) 0.029(3) -0.002(3) 0.007(3) -0.005(3) C44 0.035(3) 0.035(4) 0.038(3) 0.011(3) 0.005(3) -0.006(3) C45 0.036(4) 0.054(5) 0.057(4) 0.006(4) 0.013(3) 0.003(3) C46 0.051(5) 0.066(6) 0.049(4) -0.002(4) 0.029(4) 0.001(4) C47 0.056(5) 0.055(5) 0.027(3) -0.002(3) 0.009(3) 0.000(4) C48 0.030(3) 0.046(4) 0.027(3) 0.005(3) 0.006(3) -0.006(3) C49 0.027(3) 0.087(6) 0.054(4) 0.019(5) -0.005(3) -0.005(4) C50 0.070(5) 0.095(8) 0.108(7) 0.049(7) -0.033(6) 0.003(5) C51 0.086(6) 0.122(9) 0.059(5) -0.019(6) -0.024(5) 0.019(6) C52 0.043(4) 0.068(5) 0.029(3) 0.011(3) -0.001(3) -0.003(4) C53 0.062(5) 0.052(5) 0.047(4) -0.001(4) 0.001(4) 0.012(4) C54 0.067(5) 0.067(6) 0.080(6) 0.034(5) -0.036(5) -0.015(5) C55 0.040(4) 0.022(3) 0.018(3) -0.005(2) 0.008(2) -0.001(3) C56 0.042(4) 0.023(3) 0.021(3) 0.003(3) 0.004(3) -0.004(3) C57 0.036(4) 0.044(4) 0.035(3) -0.001(3) 0.008(3) -0.006(3) C58 0.062(4) 0.039(4) 0.023(3) 0.000(3) 0.015(3) -0.002(3) C59 0.056(4) 0.038(4) 0.022(3) 0.003(3) 0.006(3) 0.005(3) C60 0.053(4) 0.033(4) 0.019(3) -0.001(3) 0.006(3) 0.005(3) C61 0.036(3) 0.058(5) 0.027(3) -0.004(3) 0.002(3) -0.001(3) C62 0.060(5) 0.083(6) 0.041(4) -0.011(4) -0.011(4) 0.007(5) C63 0.043(4) 0.076(6) 0.053(4) -0.025(4) 0.009(3) -0.008(4) C64 0.050(4) 0.064(5) 0.023(3) 0.008(3) -0.002(3) 0.016(4) C65 0.068(5) 0.103(7) 0.072(5) -0.026(6) 0.007(5) -0.031(5) C66 0.065(6) 0.087(8) 0.157(10) -0.013(7) -0.045(6) 0.002(5) C67 0.075(5) 0.044(5) 0.063(5) 0.005(4) 0.023(5) 0.036(4) C68 0.039(4) 0.048(5) 0.050(4) -0.010(4) 0.001(3) 0.014(4) C69 0.050(4) 0.037(4) 0.050(4) -0.003(3) 0.017(3) 0.009(4) C70 0.047(4) 0.096(7) 0.037(4) -0.031(5) -0.001(3) 0.008(5) C71 0.064(6) 0.039(5) 0.126(8) -0.053(6) 0.058(6) -0.025(4) C72 0.027(3) 0.028(4) 0.046(4) -0.002(3) 0.006(3) 0.001(3) C73 0.043(4) 0.033(4) 0.043(3) 0.002(3) -0.005(3) 0.002(3) C74 0.039(4) 0.038(4) 0.025(3) -0.004(3) 0.000(3) -0.001(3) C75 0.066(6) 0.086(7) 0.071(5) -0.005(5) -0.024(4) -0.007(5) C76 0.108(7) 0.068(6) 0.052(5) -0.016(4) 0.016(5) -0.017(5) C77 0.097(6) 0.060(6) 0.041(4) 0.005(4) 0.002(4) -0.011(5) C78 0.095(6) 0.047(5) 0.058(5) 0.012(4) -0.005(5) 0.000(5) C79 0.087(6) 0.047(5) 0.063(5) 0.004(4) 0.014(4) 0.013(5) C80 0.077(6) 0.079(7) 0.074(6) -0.011(5) -0.005(5) -0.002(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 N2 1.883(5) . ? Ga1 N1 1.900(5) . ? Ga1 V1 2.4618(13) . ? Ga2 N5 1.882(4) . ? Ga2 N6 1.893(4) . ? Ga2 V2 2.4599(12) . ? V1 C32 1.893(6) . ? V1 C34 1.904(8) . ? V1 C33 1.918(8) . ? V1 C29 2.217(9) . ? V1 C30 2.221(9) . ? V1 C31 2.232(8) . ? V1 C28 2.253(7) . ? V1 C27 2.264(7) . ? V2 C73 1.879(7) . ? V2 C74 1.886(7) . ? V2 C72 1.901(6) . ? V2 C71 2.260(7) . ? V2 C68 2.266(6) . ? V2 C70 2.267(6) . ? V2 C67 2.268(7) . ? V2 C69 2.290(6) . ? K1 O1 2.622(4) . ? K1 O6 2.714(4) 3_654 ? K1 N4 2.804(6) . ? K1 N3 2.866(6) . ? K1 C6 3.185(7) . ? K1 C7 3.190(6) . ? K1 C5 3.517(7) . ? K2 O4 2.672(4) . ? K2 O3 2.717(5) . ? K2 N8 2.800(6) . ? K2 N7 2.813(5) . ? K2 C57 3.118(7) . ? K2 C58 3.239(7) . ? K2 C77 3.538(8) . ? O1 C32 1.167(7) . ? O2 C33 1.148(8) . ? O3 C34 1.173(8) . ? O4 C72 1.168(7) . ? O5 C73 1.163(7) . ? O6 C74 1.181(7) . ? O6 K1 2.714(4) 3_655 ? N1 C1 1.403(7) . ? N1 C3 1.437(6) . ? N2 C2 1.387(8) . ? N2 C15 1.437(7) . ? N3 C35 1.430(10) . ? N3 C36 1.492(8) . ? N3 C37 1.527(11) . ? N4 C38 1.436(9) . ? N4 C40 1.461(9) . ? N4 C39 1.500(9) . ? N5 C41 1.374(7) . ? N5 C43 1.433(7) . ? N6 C42 1.404(7) . ? N6 C55 1.430(6) . ? N7 C77 1.447(9) . ? N7 C76 1.457(9) . ? N7 C75 1.469(9) . ? N8 C78 1.469(8) . ? N8 C79 1.473(9) . ? N8 C80 1.480(10) . ? C1 C2 1.355(7) . ? C3 C4 1.378(7) . ? C3 C8 1.437(8) . ? C4 C5 1.405(8) . ? C4 C9 1.535(8) . ? C5 C6 1.383(8) . ? C6 C7 1.380(8) . ? C7 C8 1.388(7) . ? C8 C12 1.515(8) . ? C9 C10 1.515(9) . ? C9 C11 1.533(8) . ? C12 C14 1.522(10) . ? C12 C13 1.538(9) . ? C15 C16 1.395(8) . ? C15 C20 1.409(8) . ? C16 C17 1.397(8) . ? C16 C21 1.530(8) . ? C17 C18 1.397(9) . ? C18 C19 1.378(9) . ? C19 C20 1.407(9) . ? C20 C24 1.505(9) . ? C21 C22 1.480(11) . ? C21 C23 1.500(13) . ? C24 C26 1.528(10) . ? C24 C25 1.536(10) . ? C27 C28 1.399(12) . ? C27 C31 1.457(12) . ? C28 C29 1.279(13) . ? C29 C30 1.255(13) . ? C30 C31 1.392(13) . ? C37 C38 1.456(10) . ? C41 C42 1.355(8) . ? C43 C44 1.400(8) . ? C43 C48 1.414(8) . ? C44 C45 1.410(8) . ? C44 C49 1.515(9) . ? C45 C46 1.351(9) . ? C46 C47 1.379(10) . ? C47 C48 1.387(8) . ? C48 C52 1.510(9) . ? C49 C51 1.482(11) . ? C49 C50 1.541(11) . ? C52 C53 1.517(10) . ? C52 C54 1.523(10) . ? C55 C56 1.391(8) . ? C55 C60 1.428(8) . ? C56 C57 1.392(8) . ? C56 C61 1.529(8) . ? C57 C58 1.362(8) . ? C58 C59 1.387(8) . ? C59 C60 1.390(8) . ? C60 C64 1.525(9) . ? C61 C62 1.521(10) . ? C61 C63 1.534(9) . ? C64 C66 1.479(11) . ? C64 C65 1.526(10) . ? C67 C68 1.360(10) . ? C67 C71 1.400(12) . ? C68 C69 1.390(9) . ? C69 C70 1.392(10) . ? C70 C71 1.401(12) . ? C77 C78 1.517(11) . ? 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 Ga1 N1 86.9(2) . . ? N2 Ga1 V1 131.61(15) . . ? N1 Ga1 V1 141.47(14) . . ? N5 Ga2 N6 86.57(19) . . ? N5 Ga2 V2 132.31(14) . . ? N6 Ga2 V2 140.89(14) . . ? C32 V1 C34 107.7(3) . . ? C32 V1 C33 79.6(3) . . ? C34 V1 C33 76.9(3) . . ? C32 V1 C29 135.2(4) . . ? C34 V1 C29 111.3(4) . . ? C33 V1 C29 88.5(4) . . ? C32 V1 C30 104.9(4) . . ? C34 V1 C30 144.1(4) . . ? C33 V1 C30 94.9(4) . . ? C29 V1 C30 32.9(3) . . ? C32 V1 C31 96.2(3) . . ? C34 V1 C31 148.3(3) . . ? C33 V1 C31 128.8(4) . . ? C29 V1 C31 59.0(4) . . ? C30 V1 C31 36.4(3) . . ? C32 V1 C28 155.5(3) . . ? C34 V1 C28 95.5(3) . . ? C33 V1 C28 114.0(4) . . ? C29 V1 C28 33.2(3) . . ? C30 V1 C28 55.5(4) . . ? C31 V1 C28 59.3(3) . . ? C32 V1 C27 124.1(3) . . ? C34 V1 C27 110.5(3) . . ? C33 V1 C27 147.8(3) . . ? C29 V1 C27 59.4(3) . . ? C30 V1 C27 60.1(3) . . ? C31 V1 C27 37.8(3) . . ? C28 V1 C27 36.1(3) . . ? C32 V1 Ga1 67.96(19) . . ? C34 V1 Ga1 70.89(19) . . ? C33 V1 Ga1 123.2(3) . . ? C29 V1 Ga1 146.5(3) . . ? C30 V1 Ga1 137.0(3) . . ? C31 V1 Ga1 100.7(3) . . ? C28 V1 Ga1 114.6(3) . . ? C27 V1 Ga1 88.0(2) . . ? C73 V2 C74 79.1(3) . . ? C73 V2 C72 75.7(3) . . ? C74 V2 C72 109.1(3) . . ? C73 V2 C71 88.8(3) . . ? C74 V2 C71 118.2(4) . . ? C72 V2 C71 126.1(4) . . ? C73 V2 C68 138.1(3) . . ? C74 V2 C68 138.1(3) . . ? C72 V2 C68 100.6(3) . . ? C71 V2 C68 59.2(3) . . ? C73 V2 C70 110.9(3) . . ? C74 V2 C70 93.8(3) . . ? C72 V2 C70 157.1(3) . . ? C71 V2 C70 36.1(3) . . ? C68 V2 C70 59.3(3) . . ? C73 V2 C67 103.4(3) . . ? C74 V2 C67 152.7(3) . . ? C72 V2 C67 97.7(3) . . ? C71 V2 C67 36.0(3) . . ? C68 V2 C67 34.9(3) . . ? C70 V2 C67 59.6(3) . . ? C73 V2 C69 145.9(3) . . ? C74 V2 C69 103.9(2) . . ? C72 V2 C69 131.8(3) . . ? C71 V2 C69 59.4(3) . . ? C68 V2 C69 35.5(2) . . ? C70 V2 C69 35.6(3) . . ? C67 V2 C69 58.9(3) . . ? C73 V2 Ga2 121.9(2) . . ? C74 V2 Ga2 70.20(19) . . ? C72 V2 Ga2 69.99(19) . . ? C71 V2 Ga2 149.16(19) . . ? C68 V2 Ga2 94.0(2) . . ? C70 V2 Ga2 118.9(3) . . ? C67 V2 Ga2 126.1(3) . . ? C69 V2 Ga2 89.99(19) . . ? O1 K1 O6 138.97(15) . 3_654 ? O1 K1 N4 77.31(17) . . ? O6 K1 N4 88.07(15) 3_654 . ? O1 K1 N3 84.59(15) . . ? O6 K1 N3 123.70(16) 3_654 . ? N4 K1 N3 65.32(18) . . ? O1 K1 C6 95.35(15) . . ? O6 K1 C6 89.82(15) 3_654 . ? N4 K1 C6 165.86(17) . . ? N3 K1 C6 126.62(18) . . ? O1 K1 C7 88.76(15) . . ? O6 K1 C7 79.09(15) 3_654 . ? N4 K1 C7 141.28(17) . . ? N3 K1 C7 149.82(19) . . ? C6 K1 C7 25.02(14) . . ? O1 K1 C5 78.86(15) . . ? O6 K1 C5 112.92(14) 3_654 . ? N4 K1 C5 155.82(15) . . ? N3 K1 C5 108.45(17) . . ? C6 K1 C5 23.15(14) . . ? C7 K1 C5 41.39(15) . . ? O4 K2 O3 160.06(14) . . ? O4 K2 N8 83.85(17) . . ? O3 K2 N8 94.31(18) . . ? O4 K2 N7 107.14(16) . . ? O3 K2 N7 89.82(16) . . ? N8 K2 N7 65.03(17) . . ? O4 K2 C57 99.55(16) . . ? O3 K2 C57 84.15(17) . . ? N8 K2 C57 174.05(16) . . ? N7 K2 C57 109.16(17) . . ? O4 K2 C58 100.80(16) . . ? O3 K2 C58 90.71(17) . . ? N8 K2 C58 150.03(17) . . ? N7 K2 C58 85.49(17) . . ? C57 K2 C58 24.65(15) . . ? O4 K2 C77 108.83(18) . . ? O3 K2 C77 82.70(18) . . ? N8 K2 C77 44.56(17) . . ? N7 K2 C77 22.90(17) . . ? C57 K2 C77 129.49(17) . . ? C58 K2 C77 107.27(17) . . ? C32 O1 K1 173.0(5) . . ? C34 O3 K2 142.8(5) . . ? C72 O4 K2 126.5(4) . . ? C74 O6 K1 145.0(4) . 3_655 ? C1 N1 C3 115.7(5) . . ? C1 N1 Ga1 109.4(3) . . ? C3 N1 Ga1 131.3(4) . . ? C2 N2 C15 120.4(5) . . ? C2 N2 Ga1 110.6(3) . . ? C15 N2 Ga1 128.1(4) . . ? C35 N3 C36 106.7(6) . . ? C35 N3 C37 115.6(7) . . ? C36 N3 C37 108.4(6) . . ? C35 N3 K1 99.7(5) . . ? C36 N3 K1 120.0(5) . . ? C37 N3 K1 106.6(4) . . ? C38 N4 C40 115.0(6) . . ? C38 N4 C39 105.1(6) . . ? C40 N4 C39 108.2(6) . . ? C38 N4 K1 109.7(5) . . ? C40 N4 K1 109.6(4) . . ? C39 N4 K1 109.2(5) . . ? C41 N5 C43 118.7(5) . . ? C41 N5 Ga2 110.9(3) . . ? C43 N5 Ga2 130.1(4) . . ? C42 N6 C55 117.4(5) . . ? C42 N6 Ga2 109.8(3) . . ? C55 N6 Ga2 132.2(4) . . ? C77 N7 C76 109.5(6) . . ? C77 N7 C75 112.3(7) . . ? C76 N7 C75 109.8(6) . . ? C77 N7 K2 107.9(4) . . ? C76 N7 K2 112.7(5) . . ? C75 N7 K2 104.6(4) . . ? C78 N8 C79 109.3(6) . . ? C78 N8 C80 110.9(6) . . ? C79 N8 C80 110.3(6) . . ? C78 N8 K2 113.1(5) . . ? C79 N8 K2 114.2(4) . . ? C80 N8 K2 98.6(5) . . ? C2 C1 N1 116.6(6) . . ? C1 C2 N2 116.5(6) . . ? C4 C3 C8 120.8(5) . . ? C4 C3 N1 120.7(5) . . ? C8 C3 N1 118.5(5) . . ? C3 C4 C5 119.0(5) . . ? C3 C4 C9 120.3(5) . . ? C5 C4 C9 120.7(5) . . ? C6 C5 C4 120.9(5) . . ? C6 C5 K1 64.8(4) . . ? C4 C5 K1 95.9(4) . . ? C7 C6 C5 119.7(5) . . ? C7 C6 K1 77.7(4) . . ? C5 C6 K1 92.0(4) . . ? C6 C7 C8 121.7(5) . . ? C6 C7 K1 77.3(4) . . ? C8 C7 K1 94.9(4) . . ? C7 C8 C3 117.8(5) . . ? C7 C8 C12 120.1(5) . . ? C3 C8 C12 122.0(5) . . ? C10 C9 C11 110.3(6) . . ? C10 C9 C4 110.5(5) . . ? C11 C9 C4 112.9(5) . . ? C8 C12 C14 111.6(5) . . ? C8 C12 C13 111.0(5) . . ? C14 C12 C13 111.7(6) . . ? C16 C15 C20 121.8(5) . . ? C16 C15 N2 120.2(5) . . ? C20 C15 N2 118.0(5) . . ? C15 C16 C17 119.0(5) . . ? C15 C16 C21 121.9(5) . . ? C17 C16 C21 119.1(5) . . ? C18 C17 C16 120.1(6) . . ? C19 C18 C17 120.2(6) . . ? C18 C19 C20 121.5(6) . . ? C19 C20 C15 117.2(6) . . ? C19 C20 C24 120.2(5) . . ? C15 C20 C24 122.6(5) . . ? C22 C21 C23 109.8(7) . . ? C22 C21 C16 111.7(6) . . ? C23 C21 C16 112.5(7) . . ? C20 C24 C26 111.6(6) . . ? C20 C24 C25 111.6(6) . . ? C26 C24 C25 110.6(6) . . ? C28 C27 C31 101.9(8) . . ? C28 C27 V1 71.5(4) . . ? C31 C27 V1 69.9(4) . . ? C29 C28 C27 111.9(8) . . ? C29 C28 V1 71.9(5) . . ? C27 C28 V1 72.4(4) . . ? C30 C29 C28 110.5(10) . . ? C30 C29 V1 73.7(6) . . ? C28 C29 V1 74.9(6) . . ? C29 C30 C31 111.5(9) . . ? C29 C30 V1 73.4(6) . . ? C31 C30 V1 72.2(5) . . ? C30 C31 C27 104.0(7) . . ? C30 C31 V1 71.4(5) . . ? C27 C31 V1 72.3(4) . . ? O1 C32 V1 175.7(6) . . ? O2 C33 V1 178.4(8) . . ? O3 C34 V1 175.2(6) . . ? C38 C37 N3 117.3(7) . . ? N4 C38 C37 112.2(7) . . ? C42 C41 N5 116.6(5) . . ? C41 C42 N6 116.0(5) . . ? C44 C43 C48 120.1(5) . . ? C44 C43 N5 120.7(5) . . ? C48 C43 N5 119.2(5) . . ? C43 C44 C45 118.3(5) . . ? C43 C44 C49 121.9(5) . . ? C45 C44 C49 119.8(6) . . ? C46 C45 C44 120.9(6) . . ? C45 C46 C47 121.5(6) . . ? C46 C47 C48 120.0(6) . . ? C47 C48 C43 119.3(6) . . ? C47 C48 C52 119.7(5) . . ? C43 C48 C52 121.0(5) . . ? C51 C49 C44 111.8(7) . . ? C51 C49 C50 109.9(6) . . ? C44 C49 C50 113.3(7) . . ? C48 C52 C53 112.9(6) . . ? C48 C52 C54 110.2(6) . . ? C53 C52 C54 110.3(6) . . ? C56 C55 C60 120.7(5) . . ? C56 C55 N6 120.0(5) . . ? C60 C55 N6 119.3(5) . . ? C55 C56 C57 118.8(5) . . ? C55 C56 C61 121.7(5) . . ? C57 C56 C61 119.4(5) . . ? C58 C57 C56 121.7(6) . . ? C58 C57 K2 82.7(4) . . ? C56 C57 K2 92.2(4) . . ? C57 C58 C59 119.5(5) . . ? C57 C58 K2 72.7(4) . . ? C59 C58 K2 94.9(4) . . ? C58 C59 C60 121.9(6) . . ? C59 C60 C55 117.4(5) . . ? C59 C60 C64 120.5(5) . . ? C55 C60 C64 122.0(5) . . ? C62 C61 C56 110.8(5) . . ? C62 C61 C63 112.1(6) . . ? C56 C61 C63 110.9(6) . . ? C66 C64 C60 112.1(6) . . ? C66 C64 C65 109.1(7) . . ? C60 C64 C65 114.7(5) . . ? C68 C67 C71 108.3(7) . . ? C68 C67 V2 72.4(4) . . ? C71 C67 V2 71.7(4) . . ? C67 C68 C69 109.2(7) . . ? C67 C68 V2 72.7(4) . . ? C69 C68 V2 73.2(4) . . ? C68 C69 C70 107.5(7) . . ? C68 C69 V2 71.3(4) . . ? C70 C69 V2 71.3(4) . . ? C69 C70 C71 107.7(7) . . ? C69 C70 V2 73.1(4) . . ? C71 C70 V2 71.7(4) . . ? C67 C71 C70 107.3(7) . . ? C67 C71 V2 72.3(4) . . ? C70 C71 V2 72.2(4) . . ? O4 C72 V2 174.2(5) . . ? O5 C73 V2 176.5(6) . . ? O6 C74 V2 174.4(5) . . ? N7 C77 C78 115.0(6) . . ? N7 C77 K2 49.1(3) . . ? C78 C77 K2 81.5(4) . . ? N8 C78 C77 113.6(7) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.36 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.567 _refine_diff_density_min -0.506 _refine_diff_density_rms 0.079 # Attachment 'compd7.cif' data_compound7 _database_code_depnum_ccdc_archive 'CCDC 603232' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H59 Ga K Mn N4 O2' _chemical_formula_weight 791.67 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+3/4, x+1/4, z+1/4' '-x, -y+1/2, z' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-y+5/4, x+3/4, z+3/4' '-x+1/2, -y+1, z+1/2' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'y-3/4, -x-1/4, -z-1/4' 'x, y-1/2, -z' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' 'x+1/2, y, -z+1/2' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 37.980(5) _cell_length_b 37.980(5) _cell_length_c 13.689(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 19746(6) _cell_formula_units_Z 16 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.065 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6688 _exptl_absorpt_coefficient_mu 0.916 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.863 _exptl_absorpt_correction_T_max 0.921 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _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 47391 _diffrn_reflns_av_R_equivalents 0.1052 _diffrn_reflns_av_sigmaI/netI 0.0935 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -45 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.43 _diffrn_reflns_theta_max 25.02 _reflns_number_total 8667 _reflns_number_gt 6072 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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 'calc w=1/[\s^2^(Fo^2^)+(0.0779P)^2^+44.3185P] 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 8667 _refine_ls_number_parameters 456 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1130 _refine_ls_R_factor_gt 0.0709 _refine_ls_wR_factor_ref 0.1758 _refine_ls_wR_factor_gt 0.1606 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.115 _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 Ga1 Ga 0.229368(14) 0.839164(13) 0.03551(4) 0.02518(19) Uani 1 1 d . . . Mn1 Mn 0.26656(2) 0.793263(19) -0.00477(5) 0.0290(2) Uani 1 1 d . . . K1 K 0.29580(3) 0.81917(3) 0.35282(8) 0.0368(3) Uani 1 1 d . . . O1 O 0.30965(11) 0.80637(10) 0.1682(3) 0.0498(11) Uani 1 1 d . . . O2 O 0.21769(12) 0.74763(11) 0.1015(3) 0.0590(12) Uani 1 1 d . . . N1 N 0.19499(11) 0.86526(10) -0.0349(3) 0.0282(10) Uani 1 1 d . . . N2 N 0.21465(10) 0.86564(10) 0.1465(3) 0.0261(9) Uani 1 1 d . . . N3 N 0.32616(13) 0.82376(12) 0.5432(3) 0.0413(12) Uani 1 1 d . . . N4 N 0.37020(12) 0.81172(14) 0.3564(3) 0.0473(12) Uani 1 1 d . . . C1 C 0.17844(14) 0.88952(13) 0.0254(4) 0.0344(13) Uani 1 1 d . . . H1 H 0.1610 0.9052 0.0015 0.041 Uiso 1 1 calc R . . C2 C 0.18845(13) 0.88962(13) 0.1192(4) 0.0320(12) Uani 1 1 d . . . H2 H 0.1782 0.9053 0.1652 0.038 Uiso 1 1 calc R . . C3 C 0.19062(12) 0.86795(13) -0.1377(3) 0.0276(11) Uani 1 1 d . . . C4 C 0.17348(13) 0.84097(13) -0.1891(4) 0.0312(12) Uani 1 1 d . . . C5 C 0.17082(14) 0.84384(15) -0.2911(4) 0.0374(13) Uani 1 1 d . . . H5 H 0.1597 0.8256 -0.3272 0.045 Uiso 1 1 calc R . . C6 C 0.18416(15) 0.87275(16) -0.3396(4) 0.0453(15) Uani 1 1 d . . . H6 H 0.1815 0.8746 -0.4084 0.054 Uiso 1 1 calc R . . C7 C 0.20117(15) 0.89882(15) -0.2890(4) 0.0420(14) Uani 1 1 d . . . H7 H 0.2107 0.9183 -0.3235 0.050 Uiso 1 1 calc R . . C8 C 0.20478(13) 0.89720(14) -0.1883(4) 0.0334(12) Uani 1 1 d . . . C9 C 0.15806(15) 0.80975(13) -0.1353(4) 0.0371(13) Uani 1 1 d . . . H9 H 0.1766 0.8007 -0.0898 0.044 Uiso 1 1 calc R . . C10 C 0.14747(18) 0.77914(15) -0.2027(5) 0.0565(17) Uani 1 1 d . . . H10A H 0.1291 0.7870 -0.2478 0.085 Uiso 1 1 calc R . . H10B H 0.1385 0.7596 -0.1631 0.085 Uiso 1 1 calc R . . H10C H 0.1681 0.7713 -0.2399 0.085 Uiso 1 1 calc R . . C11 C 0.12590(15) 0.82003(16) -0.0729(5) 0.0519(16) Uani 1 1 d . . . H11A H 0.1323 0.8393 -0.0289 0.078 Uiso 1 1 calc R . . H11B H 0.1183 0.7997 -0.0343 0.078 Uiso 1 1 calc R . . H11C H 0.1067 0.8276 -0.1157 0.078 Uiso 1 1 calc R . . C12 C 0.22528(14) 0.92596(14) -0.1347(5) 0.0449(15) Uani 1 1 d . . . H12 H 0.2201 0.9236 -0.0634 0.054 Uiso 1 1 calc R . . C13 C 0.21514(18) 0.96291(15) -0.1651(5) 0.0615(19) Uani 1 1 d . . . H13A H 0.2206 0.9663 -0.2345 0.092 Uiso 1 1 calc R . . H13B H 0.2284 0.9800 -0.1261 0.092 Uiso 1 1 calc R . . H13C H 0.1899 0.9664 -0.1545 0.092 Uiso 1 1 calc R . . C14 C 0.2645(2) 0.9209(2) -0.1484(7) 0.097(3) Uani 1 1 d U . . H14A H 0.2719 0.8989 -0.1167 0.145 Uiso 1 1 calc R . . H14B H 0.2772 0.9407 -0.1191 0.145 Uiso 1 1 calc R . . H14C H 0.2700 0.9197 -0.2183 0.145 Uiso 1 1 calc R . . C15 C 0.22708(12) 0.86859(12) 0.2434(3) 0.0263(11) Uani 1 1 d . . . C16 C 0.21143(13) 0.84860(13) 0.3181(4) 0.0306(12) Uani 1 1 d . . . C17 C 0.22259(15) 0.85385(14) 0.4136(4) 0.0367(13) Uani 1 1 d . . . H17 H 0.2123 0.8402 0.4643 0.044 Uiso 1 1 calc R . . C18 C 0.24807(15) 0.87810(15) 0.4371(4) 0.0412(14) Uani 1 1 d . . . H18 H 0.2546 0.8818 0.5033 0.049 Uiso 1 1 calc R . . C19 C 0.26402(15) 0.89689(14) 0.3640(4) 0.0398(14) Uani 1 1 d . . . H19 H 0.2822 0.9131 0.3802 0.048 Uiso 1 1 calc R . . C20 C 0.25424(14) 0.89281(13) 0.2659(4) 0.0314(12) Uani 1 1 d . . . C21 C 0.18256(14) 0.82222(14) 0.2959(4) 0.0378(13) Uani 1 1 d . . . H21 H 0.1816 0.8194 0.2234 0.045 Uiso 1 1 calc R . . C22 C 0.1891(2) 0.78662(19) 0.3384(7) 0.090(3) Uani 1 1 d U . . H22A H 0.2120 0.7779 0.3160 0.135 Uiso 1 1 calc R . . H22B H 0.1706 0.7704 0.3171 0.135 Uiso 1 1 calc R . . H22C H 0.1891 0.7882 0.4098 0.135 Uiso 1 1 calc R . . C23 C 0.1470(2) 0.8361(3) 0.3285(8) 0.119(3) Uani 1 1 d U . . H23A H 0.1452 0.8344 0.3997 0.178 Uiso 1 1 calc R . . H23B H 0.1283 0.8221 0.2982 0.178 Uiso 1 1 calc R . . H23C H 0.1446 0.8607 0.3086 0.178 Uiso 1 1 calc R . . C24 C 0.27187(15) 0.91443(14) 0.1869(4) 0.0415(14) Uani 1 1 d . . . H24 H 0.2583 0.9110 0.1251 0.050 Uiso 1 1 calc R . . C25 C 0.30958(19) 0.90246(18) 0.1683(6) 0.073(2) Uani 1 1 d . . . H25A H 0.3232 0.9044 0.2288 0.109 Uiso 1 1 calc R . . H25B H 0.3202 0.9174 0.1179 0.109 Uiso 1 1 calc R . . H25C H 0.3095 0.8779 0.1461 0.109 Uiso 1 1 calc R . . C26 C 0.2717(2) 0.95392(15) 0.2106(5) 0.065(2) Uani 1 1 d . . . H26A H 0.2477 0.9613 0.2275 0.098 Uiso 1 1 calc R . . H26B H 0.2798 0.9672 0.1535 0.098 Uiso 1 1 calc R . . H26C H 0.2874 0.9585 0.2659 0.098 Uiso 1 1 calc R . . C27 C 0.29145(14) 0.80157(13) 0.1002(4) 0.0349(13) Uani 1 1 d . . . C28 C 0.23687(16) 0.76642(14) 0.0589(4) 0.0387(14) Uani 1 1 d . . . C29 C 0.30477(15) 0.81146(17) -0.1094(4) 0.0445(15) Uani 1 1 d . . . C30 C 0.30984(15) 0.77460(16) -0.0893(4) 0.0439(15) Uani 1 1 d . . . H30 H 0.3304 0.7643 -0.0621 0.053 Uiso 1 1 calc R . . C31 C 0.27911(15) 0.75658(16) -0.1168(4) 0.0451(15) Uani 1 1 d . . . H31 H 0.2752 0.7320 -0.1109 0.054 Uiso 1 1 calc R . . C32 C 0.25520(15) 0.78132(16) -0.1548(4) 0.0422(14) Uani 1 1 d . . . H32 H 0.2324 0.7762 -0.1794 0.051 Uiso 1 1 calc R . . C33 C 0.27081(15) 0.81515(16) -0.1503(4) 0.0427(15) Uani 1 1 d . . . H33 H 0.2603 0.8366 -0.1711 0.051 Uiso 1 1 calc R . . C34 C 0.33227(19) 0.83861(19) -0.0924(5) 0.071(2) Uani 1 1 d . . . H34A H 0.3480 0.8397 -0.1491 0.107 Uiso 1 1 calc R . . H34B H 0.3459 0.8325 -0.0340 0.107 Uiso 1 1 calc R . . H34C H 0.3211 0.8616 -0.0829 0.107 Uiso 1 1 calc R . . C35 C 0.30294(18) 0.80366(18) 0.6079(4) 0.0607(19) Uani 1 1 d . . . H35A H 0.3136 0.8020 0.6729 0.091 Uiso 1 1 calc R . . H35B H 0.2995 0.7800 0.5812 0.091 Uiso 1 1 calc R . . H35C H 0.2801 0.8156 0.6128 0.091 Uiso 1 1 calc R . . C36 C 0.33145(19) 0.85928(16) 0.5836(5) 0.0622(19) Uani 1 1 d . . . H36A H 0.3085 0.8704 0.5953 0.093 Uiso 1 1 calc R . . H36B H 0.3449 0.8735 0.5372 0.093 Uiso 1 1 calc R . . H36C H 0.3444 0.8576 0.6454 0.093 Uiso 1 1 calc R . . C37 C 0.35994(17) 0.80489(16) 0.5349(4) 0.0496(16) Uani 1 1 d . . . H37A H 0.3550 0.7796 0.5233 0.060 Uiso 1 1 calc R . . H37B H 0.3726 0.8068 0.5980 0.060 Uiso 1 1 calc R . . C38 C 0.38326(17) 0.81798(19) 0.4561(5) 0.0592(18) Uani 1 1 d . . . H38A H 0.3867 0.8436 0.4650 0.071 Uiso 1 1 calc R . . H38B H 0.4066 0.8066 0.4629 0.071 Uiso 1 1 calc R . . C39 C 0.38766(19) 0.8356(2) 0.2863(5) 0.072(2) Uani 1 1 d . . . H39A H 0.4131 0.8314 0.2872 0.108 Uiso 1 1 calc R . . H39B H 0.3829 0.8601 0.3046 0.108 Uiso 1 1 calc R . . H39C H 0.3785 0.8312 0.2204 0.108 Uiso 1 1 calc R . . C40 C 0.37542(19) 0.77609(18) 0.3262(5) 0.0664(19) Uani 1 1 d . . . H40A H 0.4005 0.7703 0.3294 0.100 Uiso 1 1 calc R . . H40B H 0.3670 0.7732 0.2589 0.100 Uiso 1 1 calc R . . H40C H 0.3622 0.7603 0.3694 0.100 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 Ga1 0.0313(3) 0.0246(3) 0.0196(3) -0.0010(2) -0.0027(2) 0.0031(2) Mn1 0.0362(5) 0.0293(5) 0.0215(4) -0.0058(3) -0.0031(3) 0.0056(3) K1 0.0433(7) 0.0366(7) 0.0304(6) -0.0025(5) -0.0040(5) 0.0010(5) O1 0.059(3) 0.060(3) 0.030(2) -0.010(2) -0.020(2) 0.008(2) O2 0.076(3) 0.041(2) 0.060(3) 0.001(2) 0.017(2) -0.017(2) N1 0.036(2) 0.027(2) 0.022(2) 0.0017(18) -0.0037(19) 0.0054(19) N2 0.029(2) 0.028(2) 0.022(2) -0.0041(18) -0.0043(18) 0.0081(18) N3 0.056(3) 0.041(3) 0.027(2) -0.001(2) -0.005(2) -0.014(2) N4 0.046(3) 0.061(3) 0.035(3) -0.012(3) -0.003(2) 0.001(2) C1 0.035(3) 0.034(3) 0.034(3) -0.001(2) -0.008(2) 0.013(2) C2 0.039(3) 0.032(3) 0.026(3) -0.004(2) -0.004(2) 0.009(2) C3 0.027(3) 0.033(3) 0.023(3) 0.002(2) -0.002(2) 0.006(2) C4 0.030(3) 0.034(3) 0.029(3) 0.003(2) -0.003(2) 0.005(2) C5 0.046(3) 0.042(3) 0.024(3) -0.002(3) -0.004(3) 0.007(3) C6 0.054(4) 0.063(4) 0.018(3) 0.006(3) 0.002(3) 0.014(3) C7 0.042(3) 0.044(3) 0.039(3) 0.015(3) 0.007(3) 0.006(3) C8 0.027(3) 0.040(3) 0.033(3) 0.009(3) 0.001(2) 0.008(2) C9 0.047(3) 0.030(3) 0.034(3) 0.001(2) -0.007(3) -0.001(2) C10 0.073(5) 0.041(4) 0.056(4) -0.005(3) -0.018(3) -0.009(3) C11 0.049(4) 0.049(4) 0.058(4) 0.010(3) 0.004(3) -0.001(3) C12 0.036(3) 0.042(3) 0.057(4) 0.015(3) -0.013(3) -0.002(3) C13 0.068(5) 0.040(4) 0.077(5) 0.003(3) -0.021(4) 0.007(3) C14 0.065(4) 0.078(4) 0.147(6) -0.014(4) -0.020(4) -0.004(4) C15 0.031(3) 0.023(3) 0.026(3) -0.005(2) -0.003(2) 0.009(2) C16 0.031(3) 0.028(3) 0.032(3) -0.007(2) -0.001(2) 0.010(2) C17 0.049(3) 0.039(3) 0.022(3) 0.001(2) 0.001(3) 0.007(3) C18 0.059(4) 0.042(3) 0.022(3) -0.006(3) -0.006(3) 0.008(3) C19 0.044(3) 0.032(3) 0.043(3) -0.011(3) -0.013(3) -0.001(3) C20 0.039(3) 0.027(3) 0.028(3) -0.002(2) -0.002(2) 0.001(2) C21 0.038(3) 0.044(3) 0.032(3) 0.004(3) 0.001(3) -0.005(3) C22 0.099(5) 0.063(4) 0.109(5) 0.007(4) -0.036(4) -0.015(4) C23 0.086(5) 0.108(5) 0.163(6) -0.014(5) 0.013(5) -0.011(4) C24 0.049(4) 0.038(3) 0.038(3) 0.000(3) -0.008(3) -0.012(3) C25 0.076(5) 0.048(4) 0.094(6) 0.008(4) 0.027(4) 0.010(4) C26 0.085(5) 0.035(4) 0.075(5) 0.009(3) 0.014(4) 0.000(3) C27 0.041(3) 0.034(3) 0.030(3) -0.005(2) 0.003(3) 0.009(2) C28 0.052(4) 0.033(3) 0.031(3) -0.011(3) -0.001(3) 0.005(3) C29 0.044(4) 0.060(4) 0.030(3) -0.013(3) 0.010(3) -0.007(3) C30 0.041(3) 0.061(4) 0.030(3) -0.014(3) 0.003(3) 0.014(3) C31 0.053(4) 0.041(3) 0.041(3) -0.022(3) 0.008(3) 0.004(3) C32 0.045(3) 0.061(4) 0.020(3) -0.018(3) 0.000(3) 0.003(3) C33 0.054(4) 0.056(4) 0.017(3) 0.000(3) 0.009(3) 0.010(3) C34 0.072(5) 0.077(5) 0.065(5) 0.001(4) 0.013(4) -0.011(4) C35 0.079(5) 0.069(5) 0.035(4) 0.003(3) 0.006(3) -0.022(4) C36 0.076(5) 0.047(4) 0.064(4) -0.013(3) -0.022(4) -0.007(3) C37 0.062(4) 0.049(4) 0.038(3) 0.005(3) -0.012(3) -0.006(3) C38 0.054(4) 0.067(5) 0.057(4) -0.005(4) -0.011(3) -0.003(3) C39 0.071(5) 0.094(6) 0.051(4) 0.002(4) 0.008(4) -0.021(4) C40 0.069(5) 0.065(5) 0.065(5) -0.016(4) -0.003(4) 0.009(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 N1 1.902(4) . ? Ga1 N2 1.906(4) . ? Ga1 Mn1 2.3105(9) . ? Mn1 C27 1.749(6) . ? Mn1 C28 1.752(6) . ? Mn1 C31 2.126(5) . ? Mn1 C30 2.131(5) . ? Mn1 C32 2.147(5) . ? Mn1 C29 2.153(6) . ? Mn1 C33 2.165(5) . ? K1 O1 2.627(4) . ? K1 O2 2.663(4) 13_565 ? K1 N4 2.840(5) . ? K1 N3 2.855(4) . ? K1 C18 3.102(5) . ? K1 C17 3.187(5) . ? K1 C19 3.193(5) . ? K1 C20 3.425(5) . ? K1 C16 3.427(5) . ? O1 C27 1.174(6) . ? O2 C28 1.175(6) . ? O2 K1 2.663(4) 13_565 ? N1 C1 1.388(6) . ? N1 C3 1.421(6) . ? N2 C2 1.400(6) . ? N2 C15 1.412(6) . ? N3 C35 1.464(7) . ? N3 C36 1.472(7) . ? N3 C37 1.474(8) . ? N4 C40 1.429(8) . ? N4 C38 1.471(7) . ? N4 C39 1.478(8) . ? C1 C2 1.339(7) . ? C3 C4 1.403(7) . ? C3 C8 1.415(7) . ? C4 C5 1.405(7) . ? C4 C9 1.513(7) . ? C5 C6 1.379(8) . ? C6 C7 1.370(8) . ? C7 C8 1.386(7) . ? C8 C12 1.528(8) . ? C9 C10 1.537(7) . ? C9 C11 1.541(8) . ? C12 C13 1.514(8) . ? C12 C14 1.516(9) . ? C15 C16 1.405(7) . ? C15 C20 1.416(7) . ? C16 C17 1.389(7) . ? C16 C21 1.516(7) . ? C17 C18 1.374(8) . ? C18 C19 1.371(8) . ? C19 C20 1.402(7) . ? C20 C24 1.514(7) . ? C21 C22 1.493(9) . ? C21 C23 1.516(10) . ? C24 C25 1.524(8) . ? C24 C26 1.535(8) . ? C29 C33 1.413(8) . ? C29 C30 1.440(8) . ? C29 C34 1.486(9) . ? C30 C31 1.405(8) . ? C31 C32 1.406(8) . ? C32 C33 1.416(8) . ? C37 C38 1.483(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ga1 N2 85.87(16) . . ? N1 Ga1 Mn1 133.78(12) . . ? N2 Ga1 Mn1 140.14(12) . . ? C27 Mn1 C28 92.5(3) . . ? C27 Mn1 C31 126.1(2) . . ? C28 Mn1 C31 97.0(2) . . ? C27 Mn1 C30 95.1(2) . . ? C28 Mn1 C30 125.0(2) . . ? C31 Mn1 C30 38.5(2) . . ? C27 Mn1 C32 158.9(2) . . ? C28 Mn1 C32 102.9(2) . . ? C31 Mn1 C32 38.4(2) . . ? C30 Mn1 C32 64.2(2) . . ? C27 Mn1 C29 97.1(2) . . ? C28 Mn1 C29 162.1(2) . . ? C31 Mn1 C29 65.1(2) . . ? C30 Mn1 C29 39.3(2) . . ? C32 Mn1 C29 64.3(2) . . ? C27 Mn1 C33 130.3(2) . . ? C28 Mn1 C33 136.8(2) . . ? C31 Mn1 C33 64.6(2) . . ? C30 Mn1 C33 64.6(2) . . ? C32 Mn1 C33 38.4(2) . . ? C29 Mn1 C33 38.2(2) . . ? C27 Mn1 Ga1 89.90(16) . . ? C28 Mn1 Ga1 85.80(17) . . ? C31 Mn1 Ga1 143.47(17) . . ? C30 Mn1 Ga1 148.42(17) . . ? C32 Mn1 Ga1 105.36(16) . . ? C29 Mn1 Ga1 109.19(17) . . ? C33 Mn1 Ga1 88.60(16) . . ? O1 K1 O2 95.05(13) . 13_565 ? O1 K1 N4 78.40(13) . . ? O2 K1 N4 95.30(15) 13_565 . ? O1 K1 N3 143.95(14) . . ? O2 K1 N3 85.50(13) 13_565 . ? N4 K1 N3 65.70(14) . . ? O1 K1 C18 127.47(14) . . ? O2 K1 C18 119.19(15) 13_565 . ? N4 K1 C18 130.30(15) . . ? N3 K1 C18 81.52(14) . . ? O1 K1 C17 120.16(13) . . ? O2 K1 C17 99.48(14) 13_565 . ? N4 K1 C17 154.77(14) . . ? N3 K1 C17 95.10(14) . . ? C18 K1 C17 25.19(14) . . ? O1 K1 C19 107.03(14) . . ? O2 K1 C19 142.85(15) 13_565 . ? N4 K1 C19 117.87(15) . . ? N3 K1 C19 93.02(14) . . ? C18 K1 C19 25.10(14) . . ? C17 K1 C19 43.58(15) . . ? O1 K1 C20 84.79(12) . . ? O2 K1 C20 140.45(14) 13_565 . ? N4 K1 C20 123.09(14) . . ? N3 K1 C20 116.97(13) . . ? C18 K1 C20 43.19(13) . . ? C17 K1 C20 49.55(13) . . ? C19 K1 C20 24.13(12) . . ? O1 K1 C16 96.55(12) . . ? O2 K1 C16 99.41(14) 13_565 . ? N4 K1 C16 164.84(14) . . ? N3 K1 C16 118.98(13) . . ? C18 K1 C16 43.12(13) . . ? C17 K1 C16 23.89(12) . . ? C19 K1 C16 49.58(13) . . ? C20 K1 C16 41.80(12) . . ? C27 O1 K1 132.4(4) . . ? C28 O2 K1 144.6(4) . 13_565 ? C1 N1 C3 119.3(4) . . ? C1 N1 Ga1 110.8(3) . . ? C3 N1 Ga1 128.3(3) . . ? C2 N2 C15 115.9(4) . . ? C2 N2 Ga1 109.8(3) . . ? C15 N2 Ga1 133.8(3) . . ? C35 N3 C36 109.4(5) . . ? C35 N3 C37 108.5(5) . . ? C36 N3 C37 110.8(5) . . ? C35 N3 K1 106.1(3) . . ? C36 N3 K1 117.0(4) . . ? C37 N3 K1 104.6(3) . . ? C40 N4 C38 112.0(5) . . ? C40 N4 C39 109.3(5) . . ? C38 N4 C39 110.6(5) . . ? C40 N4 K1 103.2(4) . . ? C38 N4 K1 109.6(4) . . ? C39 N4 K1 112.0(4) . . ? C2 C1 N1 116.4(4) . . ? C1 C2 N2 117.2(4) . . ? C4 C3 C8 120.3(4) . . ? C4 C3 N1 119.9(4) . . ? C8 C3 N1 119.7(4) . . ? C3 C4 C5 118.3(5) . . ? C3 C4 C9 120.5(4) . . ? C5 C4 C9 121.1(5) . . ? C6 C5 C4 120.9(5) . . ? C7 C6 C5 120.3(5) . . ? C6 C7 C8 121.1(5) . . ? C7 C8 C3 118.9(5) . . ? C7 C8 C12 119.7(5) . . ? C3 C8 C12 121.3(5) . . ? C4 C9 C10 113.7(5) . . ? C4 C9 C11 112.2(4) . . ? C10 C9 C11 108.5(5) . . ? C13 C12 C14 109.5(5) . . ? C13 C12 C8 113.6(5) . . ? C14 C12 C8 110.6(5) . . ? C16 C15 N2 119.9(4) . . ? C16 C15 C20 120.1(4) . . ? N2 C15 C20 119.9(4) . . ? C17 C16 C15 118.5(5) . . ? C17 C16 C21 120.2(5) . . ? C15 C16 C21 121.2(4) . . ? C17 C16 K1 68.3(3) . . ? C15 C16 K1 83.2(3) . . ? C21 C16 K1 119.3(3) . . ? C18 C17 C16 122.1(5) . . ? C18 C17 K1 74.0(3) . . ? C16 C17 K1 87.8(3) . . ? C19 C18 C17 119.3(5) . . ? C19 C18 K1 81.1(3) . . ? C17 C18 K1 80.8(3) . . ? C18 C19 C20 121.7(5) . . ? C18 C19 K1 73.8(3) . . ? C20 C19 K1 87.3(3) . . ? C19 C20 C15 118.2(5) . . ? C19 C20 C24 120.5(5) . . ? C15 C20 C24 121.3(4) . . ? C19 C20 K1 68.6(3) . . ? C15 C20 K1 83.1(3) . . ? C24 C20 K1 119.2(3) . . ? C22 C21 C23 110.4(6) . . ? C22 C21 C16 113.6(5) . . ? C23 C21 C16 110.9(5) . . ? C20 C24 C25 111.9(5) . . ? C20 C24 C26 112.2(5) . . ? C25 C24 C26 109.3(5) . . ? O1 C27 Mn1 176.5(5) . . ? O2 C28 Mn1 178.0(5) . . ? C33 C29 C30 107.1(5) . . ? C33 C29 C34 129.4(6) . . ? C30 C29 C34 123.4(6) . . ? C33 C29 Mn1 71.3(3) . . ? C30 C29 Mn1 69.6(3) . . ? C34 C29 Mn1 126.3(4) . . ? C31 C30 C29 108.1(5) . . ? C31 C30 Mn1 70.5(3) . . ? C29 C30 Mn1 71.2(3) . . ? C30 C31 C32 108.1(5) . . ? C30 C31 Mn1 70.9(3) . . ? C32 C31 Mn1 71.6(3) . . ? C31 C32 C33 108.7(5) . . ? C31 C32 Mn1 70.0(3) . . ? C33 C32 Mn1 71.5(3) . . ? C29 C33 C32 108.0(5) . . ? C29 C33 Mn1 70.4(3) . . ? C32 C33 Mn1 70.2(3) . . ? N3 C37 C38 114.4(5) . . ? N4 C38 C37 114.8(5) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.727 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.088