Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Barbara Sieklucka' 'N. Alcock' 'Maria Balanda' 'Yves Dromzee' 'William Errington' ; K.Fruczala ; 'Terence J. Kemp' 'Tomasz Korzeniak' 'Robert Podgajny' 'Michel Verdaguer' _publ_contact_author_name 'Dr Barbara Sieklucka' _publ_contact_author_address ; Faculty of Chemistry, Inorganic Molecular Materials Group Jagiellonian University Ingardena 3 Krakow 30-060 POLAND ; _publ_contact_author_email SIEKLUCK@CHEMIA.UJ.EDU.PL _publ_section_title ; Coordination polymers based on octacyanometalates(IV,V) (M=Mo, W) and aliphatic polyamine copper(II) tectons with [N3] donor atom sets ; data_cu35 _database_code_CSD 203323 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H55 Cu2 N26 O2.5 W2' _chemical_formula_weight 1338.7 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0223(6) _cell_length_b 16.6418(9) _cell_length_c 17.6382(10) _cell_angle_alpha 75.920(3) _cell_angle_beta 77.685(3) _cell_angle_gamma 71.825(3) _cell_volume 2948.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 7491 _cell_measurement_theta_min 3 _cell_measurement_theta_max 15 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 4.651 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2577 _exptl_absorpt_correction_T_max 0.6796 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cooler (Cosier & Glazer, 1986). The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.0 cm. Coverage of the unique set is over 97% complete to at least 26\% in \q. Crystal decay was found to be negligible by by repeating the initial frames at t data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for met atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 15096 _diffrn_reflns_av_R_equivalents 0.0621 _diffrn_reflns_av_sigmaI/netI 0.0674 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10085 _reflns_number_gt 7897 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.0584P)^2^+187.0555P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10085 _refine_ls_number_parameters 559 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1256 _refine_ls_R_factor_gt 0.0959 _refine_ls_wR_factor_ref 0.2479 _refine_ls_wR_factor_gt 0.2203 _refine_ls_goodness_of_fit_ref 1.174 _refine_ls_restrained_S_all 1.174 _refine_ls_shift/su_max 0.020 _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 W1 W 0.15682(6) 0.19840(5) 0.46334(5) 0.0221(2) Uani 1 1 d . . . W2 W 0.61688(7) 0.57531(5) 0.20318(5) 0.0260(2) Uani 1 1 d . . . Cu3 Cu 0.2996(2) -0.13739(15) 0.54887(16) 0.0325(6) Uani 1 1 d . . . Cu4 Cu 0.1928(2) 0.46900(16) 0.24505(15) 0.0316(6) Uani 1 1 d . . . N11 N 0.2698(13) -0.0113(11) 0.5246(10) 0.027(4) Uani 1 1 d . . . N12 N 0.1950(17) 0.3626(11) 0.3214(11) 0.034(4) Uani 1 1 d . . . N13 N -0.1213(15) 0.3484(11) 0.4663(12) 0.038(4) Uani 1 1 d . . . N14 N 0.254(2) 0.1299(14) 0.2955(13) 0.058(6) Uani 1 1 d . . . N15 N 0.030(2) 0.1539(14) 0.6487(13) 0.054(5) Uani 1 1 d . . . N16 N -0.0702(18) 0.1199(12) 0.4431(15) 0.054(6) Uani 1 1 d . . . N17 N 0.2052(17) 0.3382(11) 0.5524(10) 0.034(4) Uani 1 1 d . . . N18 N 0.4686(15) 0.1657(13) 0.4522(13) 0.046(5) Uani 1 1 d . . . N21 N 0.827(2) 0.6429(17) 0.0591(14) 0.069(7) Uani 1 1 d . . . N22 N 0.4038(16) 0.4647(13) 0.2398(11) 0.038(4) Uani 1 1 d . . . N23 N 0.7570(17) 0.4031(12) 0.1219(13) 0.044(5) Uani 1 1 d . . . N24 N 0.5408(15) 0.5292(12) 0.3965(11) 0.035(4) Uani 1 1 d . . . N25 N 0.676(2) 0.7367(18) 0.2521(15) 0.070(7) Uani 1 1 d . . . N26 N 0.3335(19) 0.7185(14) 0.2330(14) 0.058(6) Uani 1 1 d . . . N27 N 0.480(2) 0.6274(17) 0.0441(13) 0.065(7) Uani 1 1 d . . . N28 N 0.9000(18) 0.4813(14) 0.2671(14) 0.057(6) Uani 1 1 d . . . N31 N 0.264(6) 0.010(4) 0.722(4) 0.21(2) Uiso 1 1 d . . . N32 N 0.270(2) -0.1520(14) 0.6714(11) 0.050(5) Uani 1 1 d D . . N33 N 0.3241(17) -0.2658(10) 0.5673(13) 0.041(5) Uani 1 1 d . . . N34 N 0.3535(18) -0.1506(12) 0.4337(11) 0.040(4) Uani 1 1 d . . . N35 N 0.268(5) -0.0282(19) 0.232(2) 0.133(16) Uani 1 1 d . . . N41 N 0.2757(14) 0.4962(10) 0.4924(9) 0.028(4) Uani 1 1 d . . . N42 N 0.0868(15) 0.5449(11) 0.3260(9) 0.028(4) Uani 1 1 d . . . N43 N 0.1657(17) 0.5828(12) 0.1683(11) 0.042(5) Uani 1 1 d . . . N44 N 0.233(2) 0.4125(15) 0.1492(14) 0.056(6) Uani 1 1 d . . . N45 N 0.244(4) 0.224(3) 0.130(2) 0.131(15) Uani 1 1 d . . . C11 C 0.2327(15) 0.0635(11) 0.5036(11) 0.020(4) Uani 1 1 d . . . C12 C 0.1824(18) 0.3042(14) 0.3708(13) 0.034(5) Uani 1 1 d . . . C13 C -0.0251(17) 0.3002(13) 0.4645(12) 0.029(4) Uani 1 1 d . . . C14 C 0.219(2) 0.1529(14) 0.3559(12) 0.034(5) Uani 1 1 d . . . C15 C 0.0738(18) 0.1673(15) 0.5845(13) 0.036(5) Uani 1 1 d . . . C16 C 0.0111(17) 0.1456(12) 0.4492(12) 0.028(4) Uani 1 1 d . . . C17 C 0.1894(16) 0.2895(11) 0.5231(12) 0.026(4) Uani 1 1 d . . . C18 C 0.3658(19) 0.1725(14) 0.4535(13) 0.034(5) Uani 1 1 d . . . C21 C 0.754(2) 0.6194(14) 0.1078(13) 0.035(5) Uani 1 1 d . . . C22 C 0.4793(18) 0.4987(13) 0.2301(11) 0.028(4) Uani 1 1 d . . . C23 C 0.7122(19) 0.4624(13) 0.1490(11) 0.030(4) Uani 1 1 d . . . C24 C 0.5687(18) 0.5454(13) 0.3292(11) 0.026(4) Uani 1 1 d . . . C25 C 0.657(2) 0.6800(16) 0.2371(14) 0.043(6) Uani 1 1 d . . . C26 C 0.431(2) 0.6700(17) 0.2235(15) 0.047(6) Uani 1 1 d . . . C27 C 0.5308(19) 0.6083(14) 0.0964(12) 0.033(5) Uani 1 1 d . . . C28 C 0.803(2) 0.5128(15) 0.2450(14) 0.042(5) Uani 1 1 d . . . C31 C 0.401(4) -0.058(3) 0.686(3) 0.114(14) Uiso 1 1 d D . . H31A H 0.4194 -0.0418 0.6275 0.136 Uiso 1 1 calc R . . H31B H 0.4759 -0.0580 0.7088 0.136 Uiso 1 1 calc R . . C32 C 0.371(5) -0.144(3) 0.711(3) 0.140(18) Uiso 1 1 d D . . H32A H 0.4518 -0.1896 0.6999 0.168 Uiso 1 1 calc R . . H32B H 0.3432 -0.1540 0.7689 0.168 Uiso 1 1 calc R . . C33 C 0.262(3) -0.244(2) 0.7016(14) 0.071(9) Uani 1 1 d . . . H33A H 0.2852 -0.2642 0.7556 0.085 Uiso 1 1 calc R . . H33B H 0.1728 -0.2462 0.7037 0.085 Uiso 1 1 calc R . . C34 C 0.355(3) -0.3001(17) 0.6463(19) 0.067(9) Uani 1 1 d . . . H34A H 0.4445 -0.3014 0.6476 0.080 Uiso 1 1 calc R . . H34B H 0.3467 -0.3597 0.6633 0.080 Uiso 1 1 calc R . . C35 C 0.415(2) -0.2999(17) 0.5040(18) 0.058(7) Uani 1 1 d . . . H35A H 0.4152 -0.3597 0.5058 0.070 Uiso 1 1 calc R . . H35B H 0.5034 -0.3001 0.5086 0.070 Uiso 1 1 calc R . . C36 C 0.376(3) -0.2427(16) 0.4270(16) 0.053(7) Uani 1 1 d . . . H36A H 0.4443 -0.2573 0.3822 0.064 Uiso 1 1 calc R . . H36B H 0.2954 -0.2511 0.4174 0.064 Uiso 1 1 calc R . . C37 C 0.272(3) -0.0927(17) 0.3758(17) 0.070(9) Uani 1 1 d D . . H37A H 0.2443 -0.0339 0.3876 0.084 Uiso 1 1 calc R . . H37B H 0.1928 -0.1117 0.3820 0.084 Uiso 1 1 calc R . . C38 C 0.337(4) -0.089(2) 0.2910(17) 0.093(12) Uani 1 1 d D . . H38A H 0.4201 -0.0765 0.2869 0.111 Uiso 1 1 calc R . . H38B H 0.3564 -0.1471 0.2785 0.111 Uiso 1 1 calc R . . C41 C 0.2526(17) 0.5107(14) 0.4096(12) 0.035(5) Uani 1 1 d D . . H41A H 0.3048 0.4602 0.3858 0.042 Uiso 1 1 calc R . . H41B H 0.2799 0.5618 0.3783 0.042 Uiso 1 1 calc R . . C42 C 0.1117(16) 0.5244(14) 0.4069(11) 0.029(4) Uani 1 1 d D . . H42A H 0.0861 0.4716 0.4349 0.034 Uiso 1 1 calc R . . H42B H 0.0591 0.5720 0.4344 0.034 Uiso 1 1 calc R . . C43 C 0.069(2) 0.6359(13) 0.2887(13) 0.036(5) Uani 1 1 d . . . H43A H 0.1422 0.6555 0.2941 0.043 Uiso 1 1 calc R . . H43B H -0.0117 0.6717 0.3146 0.043 Uiso 1 1 calc R . . C44 C 0.062(2) 0.6447(14) 0.2024(13) 0.038(5) Uiso 1 1 d . . . H44A H -0.0212 0.6365 0.1972 0.045 Uiso 1 1 calc R . . H44B H 0.0647 0.7033 0.1739 0.045 Uiso 1 1 calc R . . C45 C 0.157(3) 0.559(2) 0.0922(14) 0.065(8) Uani 1 1 d . . . H45A H 0.0694 0.5529 0.0949 0.078 Uiso 1 1 calc R . . H45B H 0.1692 0.6066 0.0473 0.078 Uiso 1 1 calc R . . C46 C 0.252(3) 0.481(2) 0.0789(17) 0.069(8) Uani 1 1 d . . . H46A H 0.3394 0.4883 0.0719 0.083 Uiso 1 1 calc R . . H46B H 0.2414 0.4652 0.0305 0.083 Uiso 1 1 calc R . . C47 C 0.344(4) 0.325(3) 0.160(2) 0.102(13) Uani 1 1 d D . . H47A H 0.4274 0.3390 0.1531 0.122 Uiso 1 1 calc R . . H47B H 0.3289 0.2934 0.2149 0.122 Uiso 1 1 calc R . . C48 C 0.358(4) 0.266(2) 0.105(2) 0.101(13) Uani 1 1 d D . . H48A H 0.4411 0.2203 0.1066 0.121 Uiso 1 1 calc R . . H48B H 0.3564 0.2985 0.0497 0.121 Uiso 1 1 calc R . . O1S O 0.634(3) 0.8544(18) 0.3529(17) 0.037(7) Uiso 0.50 1 d P . . O2S O -0.123(3) 0.1274(19) 0.7960(18) 0.042(7) Uiso 0.50 1 d P . . O3S O 0.984(3) 0.112(2) 0.155(2) 0.051(8) Uiso 0.50 1 d P . . O4S O 0.041(3) 0.3552(19) 0.0933(17) 0.039(7) Uiso 0.50 1 d P . . O5S O 0.670(4) 0.274(3) 0.078(2) 0.067(10) Uiso 0.50 1 d P . . 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 W1 0.0102(4) 0.0194(4) 0.0375(5) -0.0073(3) -0.0043(3) -0.0031(3) W2 0.0148(4) 0.0367(5) 0.0286(4) -0.0045(3) -0.0064(3) -0.0093(3) Cu3 0.0313(13) 0.0212(12) 0.0457(15) -0.0027(10) -0.0107(11) -0.0074(10) Cu4 0.0324(13) 0.0337(13) 0.0316(13) -0.0061(10) -0.0055(10) -0.0127(11) N11 0.004(7) 0.040(10) 0.038(9) -0.013(8) -0.003(6) -0.004(6) N12 0.034(10) 0.028(9) 0.050(11) -0.018(9) -0.012(8) -0.008(8) N13 0.015(9) 0.035(10) 0.060(12) -0.011(9) -0.004(8) -0.004(8) N14 0.078(16) 0.053(13) 0.049(14) -0.009(11) 0.002(12) -0.032(12) N15 0.052(13) 0.050(13) 0.056(14) -0.016(10) 0.011(11) -0.014(10) N16 0.027(10) 0.028(10) 0.119(19) -0.036(11) -0.030(11) 0.008(8) N17 0.038(10) 0.026(9) 0.038(10) -0.013(8) -0.003(8) -0.007(8) N18 0.007(8) 0.054(12) 0.081(15) -0.028(11) -0.011(8) 0.001(8) N21 0.057(15) 0.089(18) 0.060(15) 0.009(13) -0.005(12) -0.040(14) N22 0.017(8) 0.060(12) 0.041(11) -0.007(9) -0.001(7) -0.018(9) N23 0.028(10) 0.038(11) 0.069(14) -0.021(10) 0.000(9) -0.009(8) N24 0.019(8) 0.045(11) 0.038(11) -0.004(8) -0.010(7) -0.004(7) N25 0.069(17) 0.086(18) 0.077(18) -0.025(14) -0.006(13) -0.047(15) N26 0.031(11) 0.051(13) 0.081(16) -0.025(12) -0.009(11) 0.016(10) N27 0.055(14) 0.098(19) 0.045(13) -0.005(12) -0.025(11) -0.019(13) N28 0.024(10) 0.071(14) 0.077(15) 0.007(12) -0.038(10) -0.011(10) N32 0.057(13) 0.061(13) 0.034(11) 0.003(9) -0.010(9) -0.025(11) N33 0.029(9) 0.014(8) 0.079(14) 0.011(8) -0.026(9) -0.009(7) N34 0.041(11) 0.035(10) 0.040(11) -0.005(8) -0.014(9) 0.000(8) N35 0.23(5) 0.052(17) 0.14(3) -0.004(18) -0.11(3) -0.02(2) N41 0.017(8) 0.033(9) 0.032(9) -0.003(7) -0.012(7) -0.002(7) N42 0.021(8) 0.042(10) 0.026(9) -0.013(7) -0.001(6) -0.012(7) N43 0.031(10) 0.045(11) 0.040(11) 0.017(8) -0.012(8) -0.008(8) N44 0.045(12) 0.066(14) 0.063(14) -0.029(12) -0.004(11) -0.014(11) N45 0.12(3) 0.19(4) 0.13(3) -0.08(3) 0.02(2) -0.09(3) C11 0.009(8) 0.014(9) 0.036(10) 0.000(7) -0.011(7) 0.000(7) C12 0.019(10) 0.033(11) 0.047(13) -0.007(10) 0.003(9) -0.009(8) C13 0.013(9) 0.033(11) 0.041(12) -0.010(9) 0.004(8) -0.009(8) C14 0.037(12) 0.041(12) 0.028(11) -0.006(9) -0.002(9) -0.017(10) C15 0.014(9) 0.053(13) 0.040(13) -0.022(10) 0.013(9) -0.010(9) C16 0.016(9) 0.025(10) 0.044(12) -0.004(8) -0.007(8) -0.006(8) C17 0.013(8) 0.009(8) 0.053(13) -0.007(8) -0.011(8) 0.006(7) C18 0.020(11) 0.042(12) 0.050(13) -0.019(10) -0.001(9) -0.018(9) C21 0.026(10) 0.044(12) 0.037(12) -0.015(10) 0.001(9) -0.011(9) C22 0.020(10) 0.036(11) 0.027(10) -0.007(8) 0.003(8) -0.008(9) C23 0.031(11) 0.036(12) 0.026(10) 0.004(9) -0.016(9) -0.012(9) C24 0.023(9) 0.037(11) 0.018(10) -0.004(8) 0.007(7) -0.014(8) C25 0.018(10) 0.056(15) 0.053(14) -0.007(12) -0.001(9) -0.014(10) C26 0.042(14) 0.059(16) 0.051(15) -0.021(12) -0.004(11) -0.024(13) C27 0.023(10) 0.044(12) 0.027(11) -0.010(9) 0.001(9) 0.000(9) C28 0.051(15) 0.043(13) 0.042(13) -0.007(10) -0.013(11) -0.022(11) C33 0.10(3) 0.09(2) 0.023(13) 0.024(14) -0.014(14) -0.06(2) C34 0.059(17) 0.037(14) 0.10(2) 0.021(15) -0.031(17) -0.018(13) C35 0.032(13) 0.045(14) 0.09(2) -0.009(14) 0.001(13) -0.010(11) C36 0.060(16) 0.046(14) 0.058(16) -0.030(12) 0.010(13) -0.019(12) C37 0.09(2) 0.040(15) 0.09(2) -0.015(14) -0.024(19) -0.020(15) C38 0.12(3) 0.08(2) 0.09(3) -0.04(2) -0.06(2) 0.00(2) C41 0.023(10) 0.045(13) 0.035(12) -0.009(10) -0.001(9) -0.011(9) C42 0.019(9) 0.050(12) 0.021(10) -0.009(9) 0.000(7) -0.015(9) C43 0.030(11) 0.031(11) 0.041(12) -0.002(9) 0.001(9) -0.007(9) C45 0.056(17) 0.10(2) 0.029(13) 0.003(14) -0.014(12) -0.017(16) C46 0.053(17) 0.10(2) 0.052(17) -0.020(16) 0.002(13) -0.018(17) C47 0.07(2) 0.15(4) 0.09(3) -0.05(3) 0.00(2) -0.04(3) C48 0.13(4) 0.08(3) 0.11(3) 0.00(2) -0.04(3) -0.05(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 W1 C14 2.11(2) . ? W1 C11 2.134(16) . ? W1 C12 2.14(2) . ? W1 C16 2.138(18) . ? W1 C15 2.14(2) . ? W1 C18 2.184(19) . ? W1 C13 2.184(19) . ? W1 C17 2.194(19) . ? W2 C24 2.143(18) . ? W2 C21 2.16(2) . ? W2 C25 2.16(3) . ? W2 C27 2.16(2) . ? W2 C22 2.18(2) . ? W2 C23 2.18(2) . ? W2 C28 2.18(2) . ? W2 C26 2.18(3) . ? Cu3 N11 1.971(17) . ? Cu3 N33 2.021(16) . ? Cu3 N34 2.036(19) . ? Cu3 N32 2.08(2) . ? Cu3 N16 2.431(18) 2_556 ? Cu3 N18 2.446(16) 2_656 ? Cu4 N12 1.944(19) . ? Cu4 N43 2.019(17) . ? Cu4 N44 2.03(2) . ? Cu4 N42 2.060(16) . ? Cu4 N22 2.287(16) . ? N11 C11 1.17(2) . ? N12 C12 1.16(3) . ? N13 C13 1.11(2) . ? N14 C14 1.17(3) . ? N15 C15 1.13(3) . ? N16 C16 1.14(3) . ? N16 Cu3 2.431(18) 2_556 ? N17 C17 1.13(2) . ? N18 C18 1.10(2) . ? N18 Cu3 2.446(16) 2_656 ? N21 C21 1.13(3) . ? N22 C22 1.11(2) . ? N23 C23 1.13(3) . ? N24 C24 1.15(2) . ? N25 C25 1.13(3) . ? N26 C26 1.13(3) . ? N27 C27 1.11(3) . ? N28 C28 1.14(3) . ? N31 C31 1.69(7) . ? N32 C32 1.49(5) . ? N32 C33 1.51(3) . ? N33 C35 1.43(3) . ? N33 C34 1.44(3) . ? N34 C37 1.47(3) . ? N34 C36 1.51(3) . ? N35 C38 1.43(4) . ? N41 C41 1.48(2) . ? N42 C42 1.45(2) . ? N42 C43 1.47(3) . ? N43 C44 1.42(3) . ? N43 C45 1.52(3) . ? N44 C46 1.49(4) . ? N44 C47 1.59(4) . ? N45 C48 1.55(5) . ? C31 C32 1.51(2) . ? C33 C34 1.52(4) . ? C35 C36 1.52(4) . ? C37 C38 1.51(2) . ? C41 C42 1.51(2) . ? C43 C44 1.51(3) . ? C45 C46 1.43(4) . ? C47 C48 1.51(2) . ? 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 C14 W1 C11 78.2(8) . . ? C14 W1 C12 71.9(8) . . ? C11 W1 C12 143.6(7) . . ? C14 W1 C16 73.3(8) . . ? C11 W1 C16 76.8(7) . . ? C12 W1 C16 112.8(8) . . ? C14 W1 C15 143.8(8) . . ? C11 W1 C15 72.1(8) . . ? C12 W1 C15 142.6(8) . . ? C16 W1 C15 80.1(8) . . ? C14 W1 C18 79.1(8) . . ? C11 W1 C18 72.7(7) . . ? C12 W1 C18 81.5(8) . . ? C16 W1 C18 142.3(7) . . ? C15 W1 C18 110.2(8) . . ? C14 W1 C13 113.4(8) . . ? C11 W1 C13 141.3(7) . . ? C12 W1 C13 71.7(7) . . ? C16 W1 C13 72.3(7) . . ? C15 W1 C13 80.1(8) . . ? C18 W1 C13 143.9(7) . . ? C14 W1 C17 140.0(8) . . ? C11 W1 C17 119.1(6) . . ? C12 W1 C17 75.6(8) . . ? C16 W1 C17 142.6(7) . . ? C15 W1 C17 74.4(8) . . ? C18 W1 C17 73.5(7) . . ? C13 W1 C17 76.7(7) . . ? C24 W2 C21 144.2(7) . . ? C24 W2 C25 79.0(8) . . ? C21 W2 C25 73.9(8) . . ? C24 W2 C27 141.1(7) . . ? C21 W2 C27 73.3(8) . . ? C25 W2 C27 115.9(9) . . ? C24 W2 C22 72.3(7) . . ? C21 W2 C22 141.3(7) . . ? C25 W2 C22 142.4(8) . . ? C27 W2 C22 76.2(8) . . ? C24 W2 C23 113.9(7) . . ? C21 W2 C23 76.7(8) . . ? C25 W2 C23 141.6(8) . . ? C27 W2 C23 77.7(7) . . ? C22 W2 C23 74.0(7) . . ? C24 W2 C28 75.6(8) . . ? C21 W2 C28 76.0(8) . . ? C25 W2 C28 77.9(8) . . ? C27 W2 C28 140.5(8) . . ? C22 W2 C28 116.6(8) . . ? C23 W2 C28 71.5(8) . . ? C24 W2 C26 78.2(8) . . ? C21 W2 C26 115.2(9) . . ? C25 W2 C26 73.9(8) . . ? C27 W2 C26 72.8(8) . . ? C22 W2 C26 76.8(8) . . ? C23 W2 C26 142.4(8) . . ? C28 W2 C26 144.5(9) . . ? N11 Cu3 N33 176.1(7) . . ? N11 Cu3 N34 94.3(7) . . ? N33 Cu3 N34 82.8(8) . . ? N11 Cu3 N32 97.1(8) . . ? N33 Cu3 N32 86.0(9) . . ? N34 Cu3 N32 167.3(8) . . ? N11 Cu3 N16 90.5(6) . 2_556 ? N33 Cu3 N16 87.3(6) . 2_556 ? N34 Cu3 N16 97.7(8) . 2_556 ? N32 Cu3 N16 87.8(8) . 2_556 ? N11 Cu3 N18 93.5(6) . 2_656 ? N33 Cu3 N18 88.9(7) . 2_656 ? N34 Cu3 N18 84.0(7) . 2_656 ? N32 Cu3 N18 89.7(8) . 2_656 ? N16 Cu3 N18 175.6(7) 2_556 2_656 ? N12 Cu4 N43 172.7(7) . . ? N12 Cu4 N44 94.5(8) . . ? N43 Cu4 N44 86.7(9) . . ? N12 Cu4 N42 93.1(7) . . ? N43 Cu4 N42 83.3(8) . . ? N44 Cu4 N42 158.3(8) . . ? N12 Cu4 N22 97.0(7) . . ? N43 Cu4 N22 90.1(7) . . ? N44 Cu4 N22 92.9(8) . . ? N42 Cu4 N22 106.3(6) . . ? C11 N11 Cu3 167.1(14) . . ? C12 N12 Cu4 172.1(17) . . ? C16 N16 Cu3 149.6(16) . 2_556 ? C18 N18 Cu3 175.2(19) . 2_656 ? C22 N22 Cu4 149.9(18) . . ? C32 N32 C33 105(2) . . ? C32 N32 Cu3 119(2) . . ? C33 N32 Cu3 104.7(15) . . ? C35 N33 C34 117(2) . . ? C35 N33 Cu3 109.0(15) . . ? C34 N33 Cu3 106.5(16) . . ? C37 N34 C36 109.7(19) . . ? C37 N34 Cu3 118.1(16) . . ? C36 N34 Cu3 110.4(14) . . ? C42 N42 C43 114.4(16) . . ? C42 N42 Cu4 121.6(13) . . ? C43 N42 Cu4 109.4(12) . . ? C44 N43 C45 119.6(18) . . ? C44 N43 Cu4 109.1(14) . . ? C45 N43 Cu4 103.5(16) . . ? C46 N44 C47 118(2) . . ? C46 N44 Cu4 105.9(17) . . ? C47 N44 Cu4 111.1(17) . . ? N11 C11 W1 176.9(14) . . ? N12 C12 W1 178.8(19) . . ? N13 C13 W1 176.0(17) . . ? N14 C14 W1 178.1(19) . . ? N15 C15 W1 177(2) . . ? N16 C16 W1 177.3(18) . . ? N17 C17 W1 178.2(17) . . ? N18 C18 W1 173.4(19) . . ? N21 C21 W2 179(2) . . ? N22 C22 W2 174.5(18) . . ? N23 C23 W2 177.2(18) . . ? N24 C24 W2 178.7(17) . . ? N25 C25 W2 177(2) . . ? N26 C26 W2 179(2) . . ? N27 C27 W2 176(2) . . ? N28 C28 W2 179(2) . . ? C32 C31 N31 103(4) . . ? N32 C32 C31 114(4) . . ? C34 C33 N32 109(2) . . ? N33 C34 C33 109(2) . . ? N33 C35 C36 108(2) . . ? N34 C36 C35 108(2) . . ? N34 C37 C38 114(3) . . ? N35 C38 C37 117(3) . . ? N41 C41 C42 110.5(15) . . ? N42 C42 C41 110.9(15) . . ? N42 C43 C44 107.9(17) . . ? N43 C44 C43 110.5(18) . . ? C46 C45 N43 111(2) . . ? C45 C46 N44 108(2) . . ? C48 C47 N44 116(3) . . ? C47 C48 N45 109(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N33 Cu3 N11 C11 25(15) . . . . ? N34 Cu3 N11 C11 68(7) . . . . ? N32 Cu3 N11 C11 -118(7) . . . . ? N16 Cu3 N11 C11 -30(7) 2_556 . . . ? N18 Cu3 N11 C11 152(7) 2_656 . . . ? N43 Cu4 N12 C12 -28(16) . . . . ? N44 Cu4 N12 C12 -127(12) . . . . ? N42 Cu4 N12 C12 32(12) . . . . ? N22 Cu4 N12 C12 139(12) . . . . ? N12 Cu4 N22 C22 -152(3) . . . . ? N43 Cu4 N22 C22 27(3) . . . . ? N44 Cu4 N22 C22 114(3) . . . . ? N42 Cu4 N22 C22 -56(3) . . . . ? N11 Cu3 N32 C32 -74(3) . . . . ? N33 Cu3 N32 C32 108(3) . . . . ? N34 Cu3 N32 C32 80(5) . . . . ? N16 Cu3 N32 C32 -164(3) 2_556 . . . ? N18 Cu3 N32 C32 19(3) 2_656 . . . ? N11 Cu3 N32 C33 168.7(17) . . . . ? N33 Cu3 N32 C33 -8.9(18) . . . . ? N34 Cu3 N32 C33 -38(4) . . . . ? N16 Cu3 N32 C33 78.5(18) 2_556 . . . ? N18 Cu3 N32 C33 -97.8(18) 2_656 . . . ? N11 Cu3 N33 C35 69(11) . . . . ? N34 Cu3 N33 C35 26.0(16) . . . . ? N32 Cu3 N33 C35 -147.8(16) . . . . ? N16 Cu3 N33 C35 124.1(16) 2_556 . . . ? N18 Cu3 N33 C35 -58.1(16) 2_656 . . . ? N11 Cu3 N33 C34 -164(10) . . . . ? N34 Cu3 N33 C34 153.6(17) . . . . ? N32 Cu3 N33 C34 -20.2(16) . . . . ? N16 Cu3 N33 C34 -108.2(17) 2_556 . . . ? N18 Cu3 N33 C34 69.6(16) 2_656 . . . ? N11 Cu3 N34 C37 -48.2(18) . . . . ? N33 Cu3 N34 C37 129.2(18) . . . . ? N32 Cu3 N34 C37 158(3) . . . . ? N16 Cu3 N34 C37 42.9(19) 2_556 . . . ? N18 Cu3 N34 C37 -141.2(19) 2_656 . . . ? N11 Cu3 N34 C36 -175.4(15) . . . . ? N33 Cu3 N34 C36 1.9(15) . . . . ? N32 Cu3 N34 C36 31(4) . . . . ? N16 Cu3 N34 C36 -84.4(16) 2_556 . . . ? N18 Cu3 N34 C36 91.5(16) 2_656 . . . ? N12 Cu4 N42 C42 40.6(14) . . . . ? N43 Cu4 N42 C42 -145.8(14) . . . . ? N44 Cu4 N42 C42 151(2) . . . . ? N22 Cu4 N42 C42 -57.6(15) . . . . ? N12 Cu4 N42 C43 177.5(13) . . . . ? N43 Cu4 N42 C43 -8.9(13) . . . . ? N44 Cu4 N42 C43 -72(3) . . . . ? N22 Cu4 N42 C43 79.3(13) . . . . ? N12 Cu4 N43 C44 42(7) . . . . ? N44 Cu4 N43 C44 142.5(16) . . . . ? N42 Cu4 N43 C44 -18.1(14) . . . . ? N22 Cu4 N43 C44 -124.5(15) . . . . ? N12 Cu4 N43 C45 -86(6) . . . . ? N44 Cu4 N43 C45 14.1(15) . . . . ? N42 Cu4 N43 C45 -146.5(15) . . . . ? N22 Cu4 N43 C45 107.1(15) . . . . ? N12 Cu4 N44 C46 -173.9(17) . . . . ? N43 Cu4 N44 C46 13.4(17) . . . . ? N42 Cu4 N44 C46 76(3) . . . . ? N22 Cu4 N44 C46 -76.6(17) . . . . ? N12 Cu4 N44 C47 -44(2) . . . . ? N43 Cu4 N44 C47 143(2) . . . . ? N42 Cu4 N44 C47 -154(2) . . . . ? N22 Cu4 N44 C47 53(2) . . . . ? Cu3 N11 C11 W1 4(37) . . . . ? C14 W1 C11 N11 -68(31) . . . . ? C12 W1 C11 N11 -103(31) . . . . ? C16 W1 C11 N11 8(31) . . . . ? C15 W1 C11 N11 91(31) . . . . ? C18 W1 C11 N11 -150(31) . . . . ? C13 W1 C11 N11 45(32) . . . . ? C17 W1 C11 N11 151(31) . . . . ? Cu4 N12 C12 W1 -29(100) . . . . ? C14 W1 C12 N12 161(93) . . . . ? C11 W1 C12 N12 -162(92) . . . . ? C16 W1 C12 N12 99(93) . . . . ? C15 W1 C12 N12 -5(93) . . . . ? C18 W1 C12 N12 -118(93) . . . . ? C13 W1 C12 N12 38(92) . . . . ? C17 W1 C12 N12 -43(92) . . . . ? C14 W1 C13 N13 85(27) . . . . ? C11 W1 C13 N13 -16(28) . . . . ? C12 W1 C13 N13 145(27) . . . . ? C16 W1 C13 N13 22(27) . . . . ? C15 W1 C13 N13 -60(27) . . . . ? C18 W1 C13 N13 -171(27) . . . . ? C17 W1 C13 N13 -136(27) . . . . ? C11 W1 C14 N14 -151(64) . . . . ? C12 W1 C14 N14 8(64) . . . . ? C16 W1 C14 N14 130(64) . . . . ? C15 W1 C14 N14 174(64) . . . . ? C18 W1 C14 N14 -76(64) . . . . ? C13 W1 C14 N14 68(64) . . . . ? C17 W1 C14 N14 -29(65) . . . . ? C14 W1 C15 N15 -176(46) . . . . ? C11 W1 C15 N15 148(47) . . . . ? C12 W1 C15 N15 -18(47) . . . . ? C16 W1 C15 N15 -133(47) . . . . ? C18 W1 C15 N15 85(47) . . . . ? C13 W1 C15 N15 -59(47) . . . . ? C17 W1 C15 N15 19(47) . . . . ? Cu3 N16 C16 W1 13(47) 2_556 . . . ? C14 W1 C16 N16 -147(44) . . . . ? C11 W1 C16 N16 131(44) . . . . ? C12 W1 C16 N16 -86(44) . . . . ? C15 W1 C16 N16 58(44) . . . . ? C18 W1 C16 N16 168(43) . . . . ? C13 W1 C16 N16 -25(44) . . . . ? C17 W1 C16 N16 10(45) . . . . ? C14 W1 C17 N17 58(54) . . . . ? C11 W1 C17 N17 166(54) . . . . ? C12 W1 C17 N17 22(54) . . . . ? C16 W1 C17 N17 -87(54) . . . . ? C15 W1 C17 N17 -136(54) . . . . ? C18 W1 C17 N17 107(54) . . . . ? C13 W1 C17 N17 -52(54) . . . . ? Cu3 N18 C18 W1 142(16) 2_656 . . . ? C14 W1 C18 N18 149(20) . . . . ? C11 W1 C18 N18 -131(20) . . . . ? C12 W1 C18 N18 75(19) . . . . ? C16 W1 C18 N18 -168(19) . . . . ? C15 W1 C18 N18 -68(20) . . . . ? C13 W1 C18 N18 34(20) . . . . ? C17 W1 C18 N18 -2(19) . . . . ? C24 W2 C21 N21 -11(100) . . . . ? C25 W2 C21 N21 32(100) . . . . ? C27 W2 C21 N21 156(100) . . . . ? C22 W2 C21 N21 -165(100) . . . . ? C23 W2 C21 N21 -123(100) . . . . ? C28 W2 C21 N21 -50(100) . . . . ? C26 W2 C21 N21 94(100) . . . . ? Cu4 N22 C22 W2 -29(22) . . . . ? C24 W2 C22 N22 127(19) . . . . ? C21 W2 C22 N22 -68(19) . . . . ? C25 W2 C22 N22 85(19) . . . . ? C27 W2 C22 N22 -30(19) . . . . ? C23 W2 C22 N22 -111(19) . . . . ? C28 W2 C22 N22 -170(19) . . . . ? C26 W2 C22 N22 45(19) . . . . ? C24 W2 C23 N23 67(37) . . . . ? C21 W2 C23 N23 -149(37) . . . . ? C25 W2 C23 N23 170(37) . . . . ? C27 W2 C23 N23 -73(37) . . . . ? C22 W2 C23 N23 6(37) . . . . ? C28 W2 C23 N23 132(37) . . . . ? C26 W2 C23 N23 -35(38) . . . . ? C21 W2 C24 N24 172(100) . . . . ? C25 W2 C24 N24 131(89) . . . . ? C27 W2 C24 N24 13(89) . . . . ? C22 W2 C24 N24 -25(88) . . . . ? C23 W2 C24 N24 -87(89) . . . . ? C28 W2 C24 N24 -149(89) . . . . ? C26 W2 C24 N24 55(89) . . . . ? C24 W2 C25 N25 -147(46) . . . . ? C21 W2 C25 N25 57(46) . . . . ? C27 W2 C25 N25 -5(46) . . . . ? C22 W2 C25 N25 -106(46) . . . . ? C23 W2 C25 N25 98(46) . . . . ? C28 W2 C25 N25 136(46) . . . . ? C26 W2 C25 N25 -66(46) . . . . ? C24 W2 C26 N26 -128(100) . . . . ? C21 W2 C26 N26 87(100) . . . . ? C25 W2 C26 N26 150(100) . . . . ? C27 W2 C26 N26 25(100) . . . . ? C22 W2 C26 N26 -54(100) . . . . ? C23 W2 C26 N26 -14(100) . . . . ? C28 W2 C26 N26 -172(100) . . . . ? C24 W2 C27 N27 29(33) . . . . ? C21 W2 C27 N27 -139(32) . . . . ? C25 W2 C27 N27 -76(32) . . . . ? C22 W2 C27 N27 66(32) . . . . ? C23 W2 C27 N27 142(32) . . . . ? C28 W2 C27 N27 -179(100) . . . . ? C26 W2 C27 N27 -15(32) . . . . ? C24 W2 C28 N28 -84(100) . . . . ? C21 W2 C28 N28 74(100) . . . . ? C25 W2 C28 N28 -2(100) . . . . ? C27 W2 C28 N28 114(100) . . . . ? C22 W2 C28 N28 -145(100) . . . . ? C23 W2 C28 N28 154(100) . . . . ? C26 W2 C28 N28 -40(100) . . . . ? C33 N32 C32 C31 177(4) . . . . ? Cu3 N32 C32 C31 60(5) . . . . ? N31 C31 C32 N32 68(5) . . . . ? C32 N32 C33 C34 -91(3) . . . . ? Cu3 N32 C33 C34 35(3) . . . . ? C35 N33 C34 C33 168(2) . . . . ? Cu3 N33 C34 C33 46(2) . . . . ? N32 C33 C34 N33 -56(3) . . . . ? C34 N33 C35 C36 -169(2) . . . . ? Cu3 N33 C35 C36 -48(2) . . . . ? C37 N34 C36 C35 -159(2) . . . . ? Cu3 N34 C36 C35 -28(2) . . . . ? N33 C35 C36 N34 50(3) . . . . ? C36 N34 C37 C38 -69(3) . . . . ? Cu3 N34 C37 C38 163(2) . . . . ? N34 C37 C38 N35 -174(3) . . . . ? C43 N42 C42 C41 -83(2) . . . . ? Cu4 N42 C42 C41 52(2) . . . . ? N41 C41 C42 N42 175.8(16) . . . . ? C42 N42 C43 C44 172.6(16) . . . . ? Cu4 N42 C43 C44 32.3(18) . . . . ? C45 N43 C44 C43 160(2) . . . . ? Cu4 N43 C44 C43 42(2) . . . . ? N42 C43 C44 N43 -50(2) . . . . ? C44 N43 C45 C46 -164(2) . . . . ? Cu4 N43 C45 C46 -42(3) . . . . ? N43 C45 C46 N44 57(3) . . . . ? C47 N44 C46 C45 -166(2) . . . . ? Cu4 N44 C46 C45 -40(3) . . . . ? C46 N44 C47 C48 -73(4) . . . . ? Cu4 N44 C47 C48 164(3) . . . . ? N44 C47 C48 N45 -73(4) . . . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 3.553 _refine_diff_density_min -2.695 _refine_diff_density_rms 0.336 data_crystals_cif _database_code_CSD 203324 _chemical_melting_point ? # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment mixed #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al 2001) ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; #============================================================= _cell_length_a 14.674(2) _cell_angle_alpha 62.55(1) _cell_length_b 15.215(2) _cell_angle_beta 63.44(1) _cell_length_c 16.073(2) _cell_angle_gamma 62.02(1) _cell_volume 2687.5(7) _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _chemical_absolute_configuration . loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'Cu ' 0.3201 1.2651 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126 1.1910 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'W ' -0.8490 6.8722 29.0818 1.7203 15.4300 9.2259 14.4327 0.3217 5.1198 57.0560 9.8875 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 2 _chemical_formula_sum ' C32 H60 Cu2 N26 O5 W2 ' _chemical_formula_moiety ' C32 H60 Cu2 N26 W2 , 5 (O) ' _chemical_compound_source ; ? ; _chemical_formula_weight 1383.7 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14 _cell_measurement_theta_max 15 _cell_measurement_temperature 295 _exptl_crystal_description ' prism ' _exptl_crystal_colour ' deep blue ' _exptl_crystal_size_min 0.2 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_max 0.6 _exptl_crystal_density_diffrn 1.70 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1360.000 _exptl_absorpt_coefficient_mu 5.2 # Sheldrick geometric definitions 0.36 0.60 _diffrn_measurement_device_type ; Enraf-Nonius CAD4 ; _diffrn_radiation_monochromator graphite _computing_data_collection ; Cad4 Express, (Enraf-Nonius, 1989) ; _computing_data_reduction ; RC93 (Watkin, Prout & Lilley, 1994) ; _computing_cell_refinement ; Cad4 Express, (Enraf-Nonius, 1989) ; _computing_structure_solution ; SHELXS 86 (Sheldrick, 1986) ; _diffrn_measurement_method \w/2\q _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; Azimutal absorption correction (North et al, 1968) ; _exptl_absorpt_correction_T_min 0.47 _exptl_absorpt_correction_T_max 1.00 _diffrn_standards_interval_time 3600 _diffrn_standards_interval_count 100 _diffrn_standards_number 2 _diffrn_standards_decay_% 53.56 _diffrn_ambient_temperature 295 _diffrn_reflns_number 9892 _reflns_number_total 9438 _diffrn_reflns_av_R_equivalents 0.0454 # Number of reflections with Friedels Law is 9438 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 9438 _diffrn_reflns_theta_min 1.599 _diffrn_reflns_theta_max 24.972 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.972 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _reflns_limit_h_min -15 _reflns_limit_h_max 17 _reflns_limit_k_min -15 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 19 _refine_diff_density_min -2.52 _refine_diff_density_max 3.49 _refine_diff_density_rms 0.21 _refine_ls_number_reflns 7391 _refine_ls_number_parameters 604 #_refine_ls_R_factor_ref 0.0604 _refine_ls_wR_factor_ref 0.0695 _refine_ls_goodness_of_fit_ref 1.1332 #_reflns_number_all 9438 _refine_ls_R_factor_all 0.0764 _refine_ls_wR_factor_all 0.0768 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 7391 _refine_ls_R_factor_gt 0.0604 _refine_ls_wR_factor_gt 0.0695 _refine_ls_shift/su_max 0.001209 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method = Prince modified Chebychev polynomial, (Watkin, 1994) W = [weight] * [1-(deltaF/6*sigmaF)^2]^2 12.6 -4.80 9.10 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Enraf-Nonius, (1989) Cad4 Express. North, A.C.T., Phillips, D.C. and Mathews, F.S., (1968), Acta Cryst, A24, 351-359 Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper R.I. (2001) CRYSTALS Issue 11. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. (1994), RC93, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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_occupancy _atom_site_adp_type _atom_site_attached_hydrogens W1 W 0.17171(3) 0.58961(3) 0.65561(2) 0.0191 1.0000 Uani . W2 W 0.33400(3) -0.10872(3) 0.94592(3) 0.0221 1.0000 Uani . Cu1 Cu 0.47512(9) 0.32195(9) 0.46202(8) 0.0248 1.0000 Uani . Cu2 Cu 0.0344(1) 0.26045(9) 0.87410(9) 0.0287 1.0000 Uani . C11 C 0.2852(8) 0.5036(8) 0.5531(7) 0.0244 1.0000 Uani . C12 C 0.1597(7) 0.4332(8) 0.7275(7) 0.0245 1.0000 Uani . C13 C 0.2450(8) 0.5119(8) 0.7730(7) 0.0257 1.0000 Uani . C14 C 0.6786(8) 0.3763(8) 0.4039(7) 0.0265 1.0000 Uani . C15 C 0.1471(12) 0.7278(12) 0.527(1) 0.0539 1.0000 Uani . C16 C 0.1335(9) 0.720(1) 0.6998(8) 0.0402 1.0000 Uani . C17 C 0.0162(8) 0.6094(9) 0.7690(8) 0.0360 1.0000 Uani . C18 C 0.063(1) 0.5870(9) 0.6002(8) 0.0359 1.0000 Uani . C21 C 0.2152(8) 0.0455(7) 0.9112(7) 0.0249 1.0000 Uani . C22 C 0.3501(11) -0.0065(9) 0.9952(11) 0.0473 1.0000 Uani . C23 C 0.4770(11) -0.0747(11) 0.835(1) 0.0530 1.0000 Uani . C24 C 0.324(1) -0.0835(9) 0.8038(8) 0.0380 1.0000 Uani . C25 C 0.2515(11) -0.1500(12) 1.1002(8) 0.0504 1.0000 Uani . C26 C 0.4625(8) -0.2003(7) 1.0155(8) 0.0284 1.0000 Uani . C27 C 0.3982(9) -0.2708(9) 0.9445(8) 0.0317 1.0000 Uani . C28 C 0.1904(9) -0.1405(9) 0.9743(9) 0.0388 1.0000 Uani . C31 C 0.4537(9) 0.5408(9) 0.1695(8) 0.0379 1.0000 Uani . C32 C 0.453(1) 0.4924(9) 0.2757(7) 0.0360 1.0000 Uani . C33 C 0.419(1) 0.333(1) 0.3054(8) 0.0396 1.0000 Uani . C34 C 0.4207(12) 0.2294(11) 0.381(1) 0.0516 1.0000 Uani . C35 C 0.3989(11) 0.149(1) 0.560(1) 0.0464 1.0000 Uani . C36 C 0.3902(11) 0.1783(11) 0.6414(8) 0.0482 1.0000 Uani . C37 C 0.4636(13) 0.278(1) 0.668(1) 0.0528 1.0000 Uani . C38 C 0.4417(14) 0.2185(14) 0.774(1) 0.0652 1.0000 Uani . C41 C 0.175(1) 0.284(1) 0.9876(9) 0.0439 1.0000 Uani . C42 C 0.0901(9) 0.2311(9) 1.0526(8) 0.0327 1.0000 Uani . C43 C -0.069(1) 0.380(1) 1.009(1) 0.0473 1.0000 Uani . C44 C -0.1503(9) 0.413(1) 0.959(1) 0.0468 1.0000 Uani . C45 C -0.1543(9) 0.398(1) 0.8124(11) 0.0486 1.0000 Uani . C46 C -0.078(1) 0.352(1) 0.7318(9) 0.0450 1.0000 Uani . C47 C 0.088(1) 0.2034(11) 0.6975(9) 0.0459 1.0000 Uani . C48 C 0.0577(13) 0.1974(15) 0.6220(11) 0.0684 1.0000 Uani . N11 N 0.3427(7) 0.4559(7) 0.5023(6) 0.0344 1.0000 Uani . N12 N 0.1486(7) 0.3517(7) 0.7658(7) 0.0320 1.0000 Uani . N13 N 0.2822(8) 0.4722(8) 0.8366(7) 0.0415 1.0000 Uani . N14 N 0.6027(7) 0.3561(8) 0.4329(6) 0.0347 1.0000 Uani . N15 N 0.1327(17) 0.7981(13) 0.4644(12) 0.1029 1.0000 Uani . N16 N 0.117(1) 0.790(1) 0.722(1) 0.0629 1.0000 Uani . N17 N -0.0636(8) 0.6168(9) 0.8280(8) 0.0523 1.0000 Uani . N18 N 0.006(1) 0.582(1) 0.5730(9) 0.0587 1.0000 Uani . N21 N 0.1491(7) 0.1237(7) 0.8945(7) 0.0314 1.0000 Uani . N22 N 0.359(1) 0.0475(9) 1.0195(11) 0.0644 1.0000 Uani . N23 N 0.553(1) -0.0614(13) 0.778(1) 0.0821 1.0000 Uani . N24 N 0.3163(11) -0.0719(9) 0.7335(8) 0.0574 1.0000 Uani . N25 N 0.2049(12) -0.1768(15) 1.182(1) 0.0869 1.0000 Uani . N26 N 0.5293(8) -0.2493(8) 1.0512(8) 0.0445 1.0000 Uani . N27 N 0.429(1) -0.3534(7) 0.9443(8) 0.0463 1.0000 Uani . N28 N 0.1175(9) -0.159(1) 0.991(1) 0.0586 1.0000 Uani . N31 N 0.5643(8) 0.5209(7) 0.0991(6) 0.0325 1.0000 Uani . N32 N 0.4854(7) 0.3749(7) 0.3143(6) 0.0308 1.0000 Uani . N33 N 0.3882(7) 0.2441(7) 0.4760(7) 0.0304 1.0000 Uani . N34 N 0.4763(8) 0.2240(8) 0.6044(6) 0.0372 1.0000 Uani . N35 N 0.5421(13) 0.1286(11) 0.7979(9) 0.0751 1.0000 Uani . N41 N 0.2466(9) 0.256(1) 1.0439(9) 0.0561 1.0000 Uani . N42 N 0.0051(7) 0.2717(7) 1.0080(6) 0.0298 1.0000 Uani . N43 N -0.0903(6) 0.3967(7) 0.8621(7) 0.0368 1.0000 Uani . N44 N -0.0063(7) 0.2476(7) 0.7730(6) 0.0332 1.0000 Uani . N45 N 0.0040(14) 0.1222(13) 0.660(1) 0.0788 1.0000 Uani . O1 O 0.7051(7) 0.2971(7) 0.1921(7) 0.0487 1.0000 Uani . O2 O 0.1679(8) 0.3970(9) 0.4791(9) 0.0689 1.0000 Uani . O3 O 0.3191(13) 0.3397(15) 1.1399(15) 0.1311 1.0000 Uani . O4 O 0.0035(18) -0.0113(19) 0.8528(17) 0.1739 1.0000 Uani . O5 O 0.217(3) -0.047(2) 0.6097(19) 0.2278 1.0000 Uani . H13 H 0.5591 0.5538 0.0340 0.0659 1.0000 Uiso . H14 H 0.6038 0.5496 0.1073 0.0659 1.0000 Uiso . H15 H 0.5998 0.4477 0.1110 0.0659 1.0000 Uiso . H16 H 0.4171 0.6182 0.1557 0.0659 1.0000 Uiso . H17 H 0.4125 0.5111 0.1598 0.0659 1.0000 Uiso . H18 H 0.5042 0.5125 0.2824 0.0659 1.0000 Uiso . H19 H 0.3783 0.5210 0.3164 0.0659 1.0000 Uiso . H20 H 0.5572 0.3499 0.2757 0.0659 1.0000 Uiso . H21 H 0.3431 0.3829 0.3139 0.0659 1.0000 Uiso . H22 H 0.4490 0.3256 0.2384 0.0659 1.0000 Uiso . H23 H 0.4952 0.1764 0.3692 0.0659 1.0000 Uiso . H24 H 0.3691 0.2034 0.3815 0.0659 1.0000 Uiso . H25 H 0.3128 0.2824 0.4900 0.0659 1.0000 Uiso . H26 H 0.4704 0.0951 0.5427 0.0659 1.0000 Uiso . H27 H 0.3397 0.1214 0.5805 0.0659 1.0000 Uiso . H28 H 0.4002 0.1147 0.6999 0.0659 1.0000 Uiso . H29 H 0.3177 0.2315 0.6595 0.0659 1.0000 Uiso . H30 H 0.5450 0.1705 0.6053 0.0659 1.0000 Uiso . H31 H 0.5314 0.2944 0.6450 0.0659 1.0000 Uiso . H32 H 0.4018 0.3458 0.6588 0.0659 1.0000 Uiso . H33 H 0.4172 0.2673 0.8113 0.0659 1.0000 Uiso . H34 H 0.3843 0.1893 0.7944 0.0659 1.0000 Uiso . H35 H 0.5236 0.0933 0.8671 0.0659 1.0000 Uiso . H36 H 0.5965 0.1563 0.7800 0.0659 1.0000 Uiso . H37 H 0.5652 0.0821 0.7640 0.0659 1.0000 Uiso . H43 H 0.3006 0.2887 1.0020 0.0659 1.0000 Uiso . H44 H 0.2062 0.2797 1.0986 0.0659 1.0000 Uiso . H45 H 0.2808 0.1820 1.0641 0.0659 1.0000 Uiso . H46 H 0.1387 0.3611 0.9653 0.0659 1.0000 Uiso . H47 H 0.2176 0.2581 0.9292 0.0659 1.0000 Uiso . H48 H 0.0578 0.2450 1.1168 0.0659 1.0000 Uiso . H49 H 0.1250 0.1538 1.0642 0.0659 1.0000 Uiso . H50 H -0.0255 0.2177 1.0531 0.0659 1.0000 Uiso . H51 H -0.1074 0.3801 1.0782 0.0659 1.0000 Uiso . H52 H -0.0274 0.4291 0.9734 0.0659 1.0000 Uiso . H53 H -0.1944 0.4881 0.9510 0.0659 1.0000 Uiso . H54 H -0.1984 0.3687 0.9990 0.0659 1.0000 Uiso . H55 H -0.0662 0.4559 0.8222 0.0659 1.0000 Uiso . H56 H -0.1995 0.4714 0.7839 0.0659 1.0000 Uiso . H57 H -0.2031 0.3550 0.8598 0.0659 1.0000 Uiso . H58 H -0.0348 0.3978 0.6814 0.0659 1.0000 Uiso . H59 H -0.1199 0.3446 0.7013 0.0659 1.0000 Uiso . H60 H -0.0426 0.1974 0.8053 0.0659 1.0000 Uiso . H61 H 0.1339 0.2498 0.6622 0.0659 1.0000 Uiso . H62 H 0.1297 0.1317 0.7311 0.0659 1.0000 Uiso . H63 H 0.0090 0.2685 0.5935 0.0659 1.0000 Uiso . H64 H 0.1259 0.1784 0.5689 0.0659 1.0000 Uiso . H65 H -0.0115 0.1221 0.6084 0.0659 1.0000 Uiso . H66 H -0.0617 0.1400 0.7095 0.0659 1.0000 Uiso . H67 H 0.0491 0.0536 0.6873 0.0659 1.0000 Uiso . 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 W1 0.0176(2) 0.0268(2) 0.0176(2) -0.00680(15) -0.00385(14) -0.01249(15) W2 0.0224(2) 0.0203(2) 0.0279(2) -0.00666(16) -0.00956(16) -0.00919(16) Cu1 0.0253(6) 0.0353(6) 0.0191(5) -0.0067(5) -0.0036(4) -0.0188(5) Cu2 0.0255(6) 0.0274(6) 0.0349(7) -0.0107(5) -0.0128(5) -0.0055(5) C11 0.023(5) 0.040(5) 0.018(4) -0.014(4) -0.004(4) -0.013(4) C12 0.016(4) 0.035(6) 0.025(5) -0.013(4) -0.004(4) -0.009(4) C13 0.025(5) 0.030(5) 0.031(5) -0.014(4) -0.008(4) -0.012(4) C14 0.019(5) 0.047(6) 0.025(5) -0.024(4) 0.004(4) -0.017(4) C15 0.071(9) 0.067(9) 0.052(8) 0.002(7) -0.037(7) -0.046(8) C16 0.037(6) 0.053(7) 0.032(6) -0.007(5) -0.004(5) -0.029(6) C17 0.019(5) 0.057(7) 0.047(6) -0.044(6) 0.009(5) -0.014(5) C18 0.058(7) 0.045(6) 0.032(5) -0.003(5) -0.027(5) -0.032(6) C21 0.021(5) 0.017(5) 0.037(5) -0.002(4) -0.012(4) -0.010(4) C22 0.052(8) 0.034(6) 0.074(9) -0.024(6) -0.038(7) -0.003(5) C23 0.043(7) 0.050(8) 0.051(8) 0.002(6) -0.016(6) -0.020(6) C24 0.052(7) 0.042(6) 0.034(6) -0.020(5) -0.011(5) -0.022(5) C25 0.054(8) 0.077(9) 0.023(6) -0.014(6) 0.001(5) -0.037(7) C26 0.032(6) 0.014(4) 0.038(6) -0.002(4) -0.011(5) -0.012(4) C27 0.030(5) 0.040(6) 0.032(5) -0.007(5) -0.010(4) -0.020(5) C28 0.031(6) 0.047(7) 0.044(6) -0.006(5) -0.007(5) -0.030(5) C31 0.036(6) 0.036(6) 0.031(6) -0.006(5) -0.012(5) -0.006(5) C32 0.046(7) 0.044(6) 0.021(5) -0.007(5) -0.006(4) -0.023(5) C33 0.045(7) 0.064(8) 0.028(5) -0.019(5) -0.015(5) -0.023(6) C34 0.068(9) 0.063(8) 0.046(7) -0.020(6) -0.004(6) -0.048(7) C35 0.054(8) 0.040(7) 0.050(7) -0.000(6) -0.018(6) -0.030(6) C36 0.049(7) 0.056(8) 0.025(6) 0.008(5) -0.004(5) -0.033(6) C37 0.08(1) 0.044(7) 0.041(7) -0.008(6) -0.030(7) -0.017(7) C38 0.083(11) 0.087(11) 0.039(7) -0.021(7) -0.008(7) -0.048(9) C41 0.041(7) 0.055(7) 0.048(7) -0.026(6) -0.010(5) -0.019(6) C42 0.032(6) 0.046(6) 0.029(5) -0.016(5) -0.009(4) -0.016(5) C43 0.041(7) 0.039(7) 0.052(7) -0.022(6) -0.006(6) -0.007(5) C44 0.026(6) 0.051(7) 0.052(7) -0.023(6) 0.005(5) -0.012(5) C45 0.022(6) 0.040(7) 0.073(9) -0.004(6) -0.024(6) -0.006(5) C46 0.037(7) 0.046(7) 0.046(7) 0.003(6) -0.025(6) -0.014(5) C47 0.045(7) 0.058(8) 0.035(6) -0.011(6) -0.009(5) -0.023(6) C48 0.06(1) 0.102(13) 0.049(8) -0.034(8) -0.009(7) -0.031(9) N11 0.034(5) 0.043(5) 0.028(5) -0.019(4) -0.005(4) -0.011(4) N12 0.023(4) 0.031(5) 0.042(5) -0.009(4) -0.006(4) -0.015(4) N13 0.043(6) 0.053(6) 0.035(5) -0.008(5) -0.021(4) -0.018(5) N14 0.034(5) 0.057(6) 0.023(4) -0.006(4) -0.003(4) -0.033(5) N15 0.166(18) 0.090(11) 0.08(1) 0.046(9) -0.093(12) -0.085(12) N16 0.057(7) 0.053(7) 0.093(9) -0.044(7) -0.005(6) -0.024(6) N17 0.039(6) 0.062(7) 0.062(7) -0.040(6) 0.020(5) -0.036(5) N18 0.063(8) 0.073(8) 0.072(8) -0.014(6) -0.037(6) -0.039(6) N21 0.024(4) 0.031(5) 0.046(5) -0.013(4) -0.020(4) -0.006(4) N22 0.067(8) 0.046(6) 0.114(11) -0.044(7) -0.053(8) -0.002(6) N23 0.042(7) 0.109(12) 0.064(8) -0.003(8) 0.008(6) -0.048(8) N24 0.088(9) 0.057(7) 0.041(6) -0.015(5) -0.026(6) -0.027(6) N25 0.08(1) 0.158(16) 0.045(7) -0.031(8) 0.004(7) -0.077(11) N26 0.034(5) 0.039(5) 0.065(7) -0.012(5) -0.025(5) -0.009(4) N27 0.081(8) 0.019(5) 0.047(6) -0.008(4) -0.034(6) -0.012(5) N28 0.039(6) 0.070(8) 0.082(8) -0.025(7) -0.017(6) -0.029(6) N31 0.048(5) 0.032(5) 0.022(4) -0.001(4) -0.014(4) -0.021(4) N32 0.036(5) 0.039(5) 0.018(4) -0.012(4) -0.002(3) -0.015(4) N33 0.030(5) 0.028(4) 0.047(5) -0.009(4) -0.019(4) -0.015(4) N34 0.043(5) 0.048(6) 0.023(4) -0.004(4) -0.010(4) -0.023(5) N35 0.111(12) 0.059(8) 0.051(7) -0.004(6) -0.036(8) -0.027(8) N41 0.036(6) 0.080(8) 0.078(8) -0.043(7) -0.018(5) -0.020(6) N42 0.026(4) 0.039(5) 0.033(5) -0.023(4) -0.001(4) -0.013(4) N43 0.013(4) 0.034(5) 0.056(6) -0.008(4) -0.010(4) -0.008(3) N44 0.030(5) 0.035(5) 0.033(5) -0.005(4) -0.007(4) -0.017(4) N45 0.107(12) 0.097(11) 0.057(8) -0.024(8) -0.039(8) -0.039(9) O1 0.042(5) 0.052(5) 0.057(5) -0.026(4) -0.012(4) -0.013(4) O2 0.046(6) 0.078(7) 0.109(9) -0.050(7) -0.039(6) -0.006(5) O3 0.097(11) 0.155(15) 0.170(17) -0.102(14) -0.066(11) 0.01(1) O4 0.149(18) 0.18(2) 0.157(18) 0.030(15) -0.091(15) -0.067(16) O5 0.43(4) 0.19(2) 0.19(2) 0.060(18) -0.23(3) -0.19(3) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag W1 . C11 . 2.166(9) yes W1 . C12 . 2.17(1) yes W1 . C13 . 2.16(1) yes W1 . C14 2_666 2.177(9) yes W1 . C15 . 2.182(14) yes W1 . C16 . 2.157(13) yes W1 . C17 . 2.182(9) yes W1 . C18 . 2.17(1) yes W2 . C21 . 2.163(9) yes W2 . C22 . 2.179(11) yes W2 . C23 . 2.163(13) yes W2 . C24 . 2.196(11) yes W2 . C25 . 2.145(11) yes W2 . C26 . 2.175(11) yes W2 . C27 . 2.197(11) yes W2 . C28 . 2.19(1) yes Cu1 . N11 . 2.174(9) yes Cu1 . N14 . 1.975(8) yes Cu1 . N32 . 2.083(8) yes Cu1 . N33 . 1.999(8) yes Cu1 . N34 . 2.080(9) yes Cu2 . N12 . 2.261(8) yes Cu2 . N21 . 1.961(9) yes Cu2 . N42 . 2.071(8) yes Cu2 . N43 . 2.017(9) yes Cu2 . N44 . 2.076(9) yes C11 . N11 . 1.123(13) yes C12 . N12 . 1.157(13) yes C13 . N13 . 1.153(13) yes C14 . N14 . 1.130(12) yes C15 . N15 . 1.093(18) yes C16 . N16 . 1.158(16) yes C17 . N17 . 1.125(14) yes C18 . N18 . 1.144(14) yes C21 . N21 . 1.133(13) yes C22 . N22 . 1.138(15) yes C23 . N23 . 1.113(17) yes C24 . N24 . 1.112(15) yes C25 . N25 . 1.151(17) yes C26 . N26 . 1.126(14) yes C27 . N27 . 1.120(14) yes C28 . N28 . 1.119(14) yes C31 . C32 . 1.511(15) yes C31 . N31 . 1.490(14) yes C31 . H16 . 0.998 no C31 . H17 . 1.001 no C32 . N32 . 1.500(14) yes C32 . H18 . 0.998 no C32 . H19 . 0.994 no C33 . C34 . 1.481(19) yes C33 . N32 . 1.474(14) yes C33 . H21 . 0.997 no C33 . H22 . 1.004 no C34 . N33 . 1.474(16) yes C34 . H23 . 1.004 no C34 . H24 . 1.002 no C35 . C36 . 1.499(19) yes C35 . N33 . 1.456(15) yes C35 . H26 . 0.997 no C35 . H27 . 1.002 no C36 . N34 . 1.485(15) yes C36 . H28 . 0.998 no C36 . H29 . 1.002 no C37 . C38 . 1.478(19) yes C37 . N34 . 1.489(16) yes C37 . H31 . 1.002 no C37 . H32 . 1.003 no C38 . N35 . 1.52(2) yes C38 . H33 . 1.008 no C38 . H34 . 0.991 no C41 . C42 . 1.507(16) yes C41 . N41 . 1.480(16) yes C41 . H46 . 0.998 no C41 . H47 . 1.002 no C42 . N42 . 1.455(14) yes C42 . H48 . 1.003 no C42 . H49 . 0.999 no C43 . C44 . 1.484(19) yes C43 . N42 . 1.492(14) yes C43 . H51 . 1.003 no C43 . H52 . 0.995 no C44 . N43 . 1.482(16) yes C44 . H53 . 0.997 no C44 . H54 . 0.998 no C45 . C46 . 1.49(2) yes C45 . N43 . 1.472(16) yes C45 . H56 . 1.003 no C45 . H57 . 1.005 no C46 . N44 . 1.464(15) yes C46 . H58 . 0.994 no C46 . H59 . 1.002 no C47 . C48 . 1.512(19) yes C47 . N44 . 1.487(15) yes C47 . H61 . 1.010 no C47 . H62 . 0.993 no C48 . N45 . 1.44(2) yes C48 . H63 . 1.002 no C48 . H64 . 1.003 no N31 . H13 . 0.951 no N31 . H14 . 0.950 no N31 . H15 . 0.947 no N32 . H20 . 0.946 no N33 . H25 . 0.953 no N34 . H30 . 0.955 no N35 . H35 . 0.956 no N35 . H36 . 0.945 no N35 . H37 . 0.937 no N41 . H43 . 0.958 no N41 . H44 . 0.941 no N41 . H45 . 0.949 no N42 . H50 . 0.953 no N43 . H55 . 0.955 no N44 . H60 . 0.951 no N45 . H65 . 0.950 no N45 . H66 . 0.952 no N45 . H67 . 0.954 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C11 . W1 . C12 . 74.3(4) yes C11 . W1 . C13 . 102.1(4) yes C12 . W1 . C13 . 72.5(3) yes C11 . W1 . C14 2_666 71.9(3) yes C12 . W1 . C14 2_666 124.7(4) yes C13 . W1 . C14 2_666 73.3(4) yes C11 . W1 . C15 . 86.5(5) yes C12 . W1 . C15 . 142.1(4) yes C13 . W1 . C15 . 144.6(4) yes C14 2_666 W1 . C15 . 77.1(4) yes C11 . W1 . C16 . 144.4(4) yes C12 . W1 . C16 . 136.7(4) yes C13 . W1 . C16 . 78.7(4) yes C14 2_666 W1 . C16 . 74.5(4) yes C15 . W1 . C16 . 74.9(5) yes C11 . W1 . C17 . 144.6(4) yes C12 . W1 . C17 . 75.9(4) yes C13 . W1 . C17 . 86.7(4) yes C14 2_666 W1 . C17 . 142.6(3) yes C15 . W1 . C17 . 106.0(5) yes C11 . W1 . C18 . 79.0(4) yes C12 . W1 . C18 . 73.6(4) yes C13 . W1 . C18 . 144.3(4) yes C14 2_666 W1 . C18 . 137.6(4) yes C15 . W1 . C18 . 70.8(4) yes C16 . W1 . C17 . 70.7(4) yes C16 . W1 . C18 . 120.9(5) yes C17 . W1 . C18 . 74.5(4) yes C21 . W2 . C22 . 70.6(4) yes C21 . W2 . C23 . 99.3(4) yes C22 . W2 . C23 . 78.6(6) yes C21 . W2 . C24 . 75.4(4) yes C22 . W2 . C24 . 130.4(5) yes C23 . W2 . C24 . 72.4(5) yes C21 . W2 . C25 . 94.4(5) yes C22 . W2 . C25 . 76.0(5) yes C23 . W2 . C25 . 145.2(5) yes C24 . W2 . C25 . 142.4(5) yes C21 . W2 . C26 . 142.6(4) yes C22 . W2 . C26 . 72.0(4) yes C23 . W2 . C26 . 74.2(4) yes C24 . W2 . C26 . 133.0(4) yes C25 . W2 . C26 . 75.5(5) yes C21 . W2 . C27 . 146.7(4) yes C22 . W2 . C27 . 142.6(4) yes C23 . W2 . C27 . 92.5(5) yes C24 . W2 . C27 . 78.8(4) yes C25 . W2 . C27 . 93.4(5) yes C21 . W2 . C28 . 76.0(4) yes C22 . W2 . C28 . 129.5(5) yes C23 . W2 . C28 . 144.6(5) yes C24 . W2 . C28 . 72.5(4) yes C25 . W2 . C28 . 69.9(5) yes C26 . W2 . C27 . 70.6(4) yes C26 . W2 . C28 . 129.9(4) yes C27 . W2 . C28 . 76.5(4) yes N11 . Cu1 . N14 . 102.1(4) yes N11 . Cu1 . N32 . 98.4(3) yes N14 . Cu1 . N32 . 92.9(3) yes N11 . Cu1 . N33 . 98.4(4) yes N14 . Cu1 . N33 . 159.4(4) yes N32 . Cu1 . N33 . 83.0(4) yes N11 . Cu1 . N34 . 96.3(4) yes N14 . Cu1 . N34 . 94.7(4) yes N32 . Cu1 . N34 . 161.7(4) yes N33 . Cu1 . N34 . 84.0(4) yes N12 . Cu2 . N21 . 94.7(3) yes N12 . Cu2 . N42 . 104.7(3) yes N21 . Cu2 . N42 . 94.2(4) yes N12 . Cu2 . N43 . 89.0(3) yes N21 . Cu2 . N43 . 176.0(4) yes N42 . Cu2 . N43 . 83.4(4) yes N12 . Cu2 . N44 . 97.6(3) yes N21 . Cu2 . N44 . 96.8(4) yes N42 . Cu2 . N44 . 154.1(3) yes N43 . Cu2 . N44 . 84.1(4) yes W1 . C11 . N11 . 177.4(9) yes W1 . C12 . N12 . 177.0(8) yes W1 . C13 . N13 . 178.4(9) yes W1 2_666 C14 . N14 . 177.5(9) yes W1 . C15 . N15 . 178.4(18) yes W1 . C16 . N16 . 177.7(10) yes W1 . C17 . N17 . 178.0(10) yes W1 . C18 . N18 . 177.7(10) yes W2 . C21 . N21 . 176.3(8) yes W2 . C22 . N22 . 178.9(14) yes W2 . C23 . N23 . 177.2(14) yes W2 . C24 . N24 . 177.5(11) yes W2 . C25 . N25 . 175.0(13) yes W2 . C26 . N26 . 178.8(9) yes W2 . C27 . N27 . 178.7(10) yes W2 . C28 . N28 . 178.1(11) yes C32 . C31 . N31 . 113.5(9) yes C32 . C31 . H16 . 108.074 no N31 . C31 . H16 . 108.726 no C32 . C31 . H17 . 108.312 no N31 . C31 . H17 . 108.573 no H16 . C31 . H17 . 109.566 no C31 . C32 . N32 . 115.1(9) yes C31 . C32 . H18 . 107.909 no N32 . C32 . H18 . 107.506 no C31 . C32 . H19 . 108.201 no N32 . C32 . H19 . 107.961 no H18 . C32 . H19 . 110.154 no C34 . C33 . N32 . 109.5(9) yes C34 . C33 . H21 . 110.005 no N32 . C33 . H21 . 109.491 no C34 . C33 . H22 . 109.593 no N32 . C33 . H22 . 108.860 no H21 . C33 . H22 . 109.360 no C33 . C34 . N33 . 106.5(10) yes C33 . C34 . H23 . 110.932 no N33 . C34 . H23 . 109.650 no C33 . C34 . H24 . 110.814 no N33 . C34 . H24 . 109.926 no H23 . C34 . H24 . 109.001 no C36 . C35 . N33 . 107.2(10) yes C36 . C35 . H26 . 110.461 no N33 . C35 . H26 . 109.752 no C36 . C35 . H27 . 110.212 no N33 . C35 . H27 . 109.586 no H26 . C35 . H27 . 109.592 no C35 . C36 . N34 . 107.2(9) yes C35 . C36 . H28 . 110.000 no N34 . C36 . H28 . 110.210 no C35 . C36 . H29 . 110.090 no N34 . C36 . H29 . 109.781 no H28 . C36 . H29 . 109.513 no C38 . C37 . N34 . 115.0(11) yes C38 . C37 . H31 . 108.545 no N34 . C37 . H31 . 108.284 no C38 . C37 . H32 . 108.042 no N34 . C37 . H32 . 107.797 no H31 . C37 . H32 . 109.015 no C37 . C38 . N35 . 111.9(13) yes C37 . C38 . H33 . 108.756 no N35 . C38 . H33 . 108.199 no C37 . C38 . H34 . 109.557 no N35 . C38 . H34 . 108.828 no H33 . C38 . H34 . 109.584 no C42 . C41 . N41 . 108.9(10) yes C42 . C41 . H46 . 109.318 no N41 . C41 . H46 . 110.247 no C42 . C41 . H47 . 108.935 no N41 . C41 . H47 . 109.915 no H46 . C41 . H47 . 109.486 no C41 . C42 . N42 . 111.1(9) yes C41 . C42 . H48 . 108.526 no N42 . C42 . H48 . 109.181 no C41 . C42 . H49 . 108.987 no N42 . C42 . H49 . 109.680 no H48 . C42 . H49 . 109.291 no C44 . C43 . N42 . 108.9(10) yes C44 . C43 . H51 . 109.412 no N42 . C43 . H51 . 109.145 no C44 . C43 . H52 . 110.106 no N42 . C43 . H52 . 109.576 no H51 . C43 . H52 . 109.661 no C43 . C44 . N43 . 107.4(9) yes C43 . C44 . H53 . 109.899 no N43 . C44 . H53 . 109.861 no C43 . C44 . H54 . 110.229 no N43 . C44 . H54 . 109.566 no H53 . C44 . H54 . 109.812 no C46 . C45 . N43 . 108.2(9) yes C46 . C45 . H56 . 109.299 no N43 . C45 . H56 . 110.691 no C46 . C45 . H57 . 109.420 no N43 . C45 . H57 . 110.359 no H56 . C45 . H57 . 108.853 no C45 . C46 . N44 . 108.8(10) yes C45 . C46 . H58 . 109.384 no N44 . C46 . H58 . 109.801 no C45 . C46 . H59 . 109.583 no N44 . C46 . H59 . 109.440 no H58 . C46 . H59 . 109.800 no C48 . C47 . N44 . 114.4(11) yes C48 . C47 . H61 . 108.217 no N44 . C47 . H61 . 107.561 no C48 . C47 . H62 . 108.791 no N44 . C47 . H62 . 108.543 no H61 . C47 . H62 . 109.287 no C47 . C48 . N45 . 114.5(13) yes C47 . C48 . H63 . 108.093 no N45 . C48 . H63 . 108.507 no C47 . C48 . H64 . 107.763 no N45 . C48 . H64 . 108.793 no H63 . C48 . H64 . 109.107 no Cu1 . N11 . C11 . 154.8(8) yes Cu2 . N12 . C12 . 146.1(8) yes Cu1 . N14 . C14 . 170.8(8) yes Cu2 . N21 . C21 . 175.7(9) yes C31 . N31 . H13 . 109.161 no C31 . N31 . H14 . 109.163 no H13 . N31 . H14 . 109.397 no C31 . N31 . H15 . 109.644 no H13 . N31 . H15 . 109.701 no H14 . N31 . H15 . 109.758 no Cu1 . N32 . C32 . 109.9(6) yes Cu1 . N32 . C33 . 107.8(6) yes C32 . N32 . C33 . 113.7(9) yes Cu1 . N32 . H20 . 111.477 no C32 . N32 . H20 . 106.047 no C33 . N32 . H20 . 107.969 no Cu1 . N33 . C34 . 108.0(7) yes Cu1 . N33 . C35 . 109.0(7) yes C34 . N33 . C35 . 116.2(10) yes Cu1 . N33 . H25 . 112.774 no C34 . N33 . H25 . 105.940 no C35 . N33 . H25 . 104.973 no Cu1 . N34 . C36 . 105.4(7) yes Cu1 . N34 . C37 . 113.3(7) yes C36 . N34 . C37 . 113.7(10) yes Cu1 . N34 . H30 . 111.134 no C36 . N34 . H30 . 111.271 no C37 . N34 . H30 . 102.252 no C38 . N35 . H35 . 108.306 no C38 . N35 . H36 . 109.097 no H35 . N35 . H36 . 109.330 no C38 . N35 . H37 . 108.982 no H35 . N35 . H37 . 110.046 no H36 . N35 . H37 . 111.027 no C41 . N41 . H43 . 108.521 no C41 . N41 . H44 . 109.828 no H43 . N41 . H44 . 109.637 no C41 . N41 . H45 . 109.461 no H43 . N41 . H45 . 108.951 no H44 . N41 . H45 . 110.409 no Cu2 . N42 . C42 . 122.8(6) yes Cu2 . N42 . C43 . 107.6(7) yes C42 . N42 . C43 . 114.4(9) yes Cu2 . N42 . H50 . 102.137 no C42 . N42 . H50 . 94.161 no C43 . N42 . H50 . 114.507 no Cu2 . N43 . C44 . 109.9(7) yes Cu2 . N43 . C45 . 108.6(7) yes C44 . N43 . C45 . 115.9(9) yes Cu2 . N43 . H55 . 111.824 no C44 . N43 . H55 . 104.403 no C45 . N43 . H55 . 106.179 no Cu2 . N44 . C46 . 106.6(7) yes Cu2 . N44 . C47 . 114.5(7) yes C46 . N44 . C47 . 113.6(9) yes Cu2 . N44 . H60 . 109.543 no C46 . N44 . H60 . 110.331 no C47 . N44 . H60 . 102.222 no C48 . N45 . H65 . 109.785 no C48 . N45 . H66 . 109.728 no H65 . N45 . H66 . 109.313 no C48 . N45 . H67 . 109.883 no H65 . N45 . H67 . 109.104 no H66 . N45 . H67 . 109.008 no data_W4Cudien _database_code_CSD 203325 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Cu(dien)]2 [W(CN)8] 4H2O' _chemical_formula_sum 'C16 H34 Cu2 N14 O4 W' _chemical_formula_weight 797.50 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 12.8799(1) _cell_length_b 9.9690(2) _cell_length_c 11.3691(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1459.79(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5739 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 43.109 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.814 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 5.421 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'HKL DENZO and Scalepack (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.3443 _exptl_absorpt_correction_T_max 0.7368 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f and \w scans to fill Ewald sphere' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10623 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0393 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 43.08 _reflns_number_total 10623 _reflns_number_gt 9058 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL DENZO and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution ; SIR (Altomare, Cascarano, Giacovazzo, Guagliardi, Burla, Polidori, Camalli, 1994) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 (Farrugia, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0290P)^2^+1.5523P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0059(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.402(10) _refine_ls_number_reflns 10623 _refine_ls_number_parameters 215 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0473 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0806 _refine_ls_wR_factor_gt 0.0735 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.005 _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 W1 W 0.5000 0.0000 0.302693(9) 0.01949(3) Uani 1 2 d S . . C1 C 0.3990(2) -0.1581(3) 0.3646(3) 0.0294(5) Uani 1 1 d . . . N1 N 0.3421(3) -0.2400(4) 0.3951(3) 0.0433(7) Uani 1 1 d . . . C2 C 0.3490(3) 0.0675(4) 0.2445(3) 0.0368(7) Uani 1 1 d . . . N2 N 0.2672(3) 0.1025(6) 0.2180(4) 0.0632(12) Uani 1 1 d . . . C3 C 0.5279(3) 0.1326(4) 0.1556(3) 0.0369(7) Uani 1 1 d . . . N3 N 0.5462(3) 0.2021(5) 0.0781(4) 0.0618(12) Uani 1 1 d . . . C4 C 0.4232(2) 0.0909(3) 0.4496(3) 0.0295(5) Uani 1 1 d . . . N4 N 0.3787(2) 0.1306(4) 0.5305(3) 0.0423(7) Uani 1 1 d . . . Cu1 Cu 0.29467(4) 0.13522(5) 0.67274(4) 0.04173(10) Uani 1 1 d . . . N6 N 0.3794(4) 0.2825(6) 0.7517(4) 0.0730(15) Uani 1 1 d . A . C7A C 0.3585(11) 0.3233(16) 0.8648(13) 0.061(4) Uani 0.50 1 d P A 1 H7A1 H 0.3050 0.3918 0.8666 0.073 Uiso 0.50 1 calc PR A 1 H7A2 H 0.4203 0.3569 0.9036 0.073 Uiso 0.50 1 calc PR A 1 C8A C 0.3213(13) 0.194(3) 0.9199(15) 0.076(7) Uani 0.50 1 d P A 1 H8A1 H 0.3779 0.1304 0.9265 0.091 Uiso 0.50 1 calc PR A 1 H8A2 H 0.2931 0.2106 0.9977 0.091 Uiso 0.50 1 calc PR A 1 N9A N 0.2395(9) 0.1421(10) 0.8402(10) 0.046(2) Uani 0.50 1 d P A 1 C10A C 0.1997(11) 0.001(2) 0.8641(12) 0.070(4) Uani 0.50 1 d P A 1 H10A H 0.1476 0.0034 0.9256 0.084 Uiso 0.50 1 calc PR A 1 H10B H 0.2562 -0.0559 0.8896 0.084 Uiso 0.50 1 calc PR A 1 C11A C 0.1546(15) -0.0504(18) 0.7552(18) 0.077(5) Uani 0.50 1 d P A 1 H11A H 0.0926 0.0011 0.7376 0.092 Uiso 0.50 1 calc PR A 1 H11B H 0.1333 -0.1425 0.7685 0.092 Uiso 0.50 1 calc PR A 1 C7B C 0.3288(11) 0.2683(18) 0.8819(13) 0.060(4) Uani 0.50 1 d P A 2 H7B1 H 0.3826 0.2887 0.9389 0.072 Uiso 0.50 1 calc PR A 2 H7B2 H 0.2758 0.3368 0.8898 0.072 Uiso 0.50 1 calc PR A 2 C8B C 0.2831(13) 0.142(3) 0.9145(12) 0.082(7) Uani 0.50 1 d P A 2 H8B1 H 0.2445 0.1529 0.9872 0.099 Uiso 0.50 1 calc PR A 2 H8B2 H 0.3373 0.0765 0.9275 0.099 Uiso 0.50 1 calc PR A 2 N9B N 0.2129(9) 0.0957(10) 0.8204(10) 0.046(2) Uani 0.50 1 d P A 2 C10B C 0.1698(15) -0.0431(17) 0.8214(14) 0.064(4) Uani 0.50 1 d P A 2 H10C H 0.2228 -0.1064 0.8455 0.077 Uiso 0.50 1 calc PR A 2 H10D H 0.1123 -0.0489 0.8764 0.077 Uiso 0.50 1 calc PR A 2 C11B C 0.1335(13) -0.0747(14) 0.7004(14) 0.064(3) Uani 0.50 1 d P A 2 H11C H 0.1123 -0.1676 0.6924 0.077 Uiso 0.50 1 calc PR A 2 H11D H 0.0778 -0.0160 0.6752 0.077 Uiso 0.50 1 calc PR A 2 N12 N 0.2310(5) -0.0467(5) 0.6388(7) 0.095(2) Uani 1 1 d . A . O1 O 0.4052(3) -0.2228(6) 0.8270(5) 0.0810(13) Uani 1 1 d . . . O2 O 0.1099(6) 0.0452(7) 0.4211(7) 0.129(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.01771(4) 0.02556(5) 0.01519(4) 0.000 0.000 -0.00183(7) C1 0.0306(12) 0.0333(13) 0.0242(11) 0.0016(9) -0.0002(9) -0.0068(10) N1 0.0453(16) 0.0469(16) 0.0378(16) 0.0014(13) 0.0037(13) -0.0209(13) C2 0.0312(13) 0.0525(19) 0.0267(13) 0.0042(13) -0.0056(11) 0.0056(13) N2 0.0363(16) 0.103(4) 0.050(2) 0.011(2) -0.0096(15) 0.0182(19) C3 0.0323(12) 0.0502(17) 0.0283(13) 0.0119(13) -0.0079(10) -0.0144(12) N3 0.057(2) 0.087(3) 0.0418(19) 0.033(2) -0.0156(16) -0.033(2) C4 0.0252(11) 0.0363(13) 0.0270(12) -0.0053(10) 0.0013(9) 0.0034(10) N4 0.0347(13) 0.0583(19) 0.0338(14) -0.0115(14) 0.0053(11) 0.0047(13) Cu1 0.0436(2) 0.0522(2) 0.02938(19) 0.00324(18) 0.01112(17) 0.0186(2) N6 0.076(3) 0.099(4) 0.044(2) -0.033(2) -0.023(2) 0.027(3) C7A 0.060(8) 0.078(10) 0.044(6) -0.020(6) -0.014(6) 0.015(6) C8A 0.062(9) 0.14(2) 0.025(4) 0.012(8) -0.007(6) 0.030(10) N9A 0.048(5) 0.054(6) 0.036(4) 0.014(4) 0.010(4) 0.020(4) C10A 0.077(8) 0.069(8) 0.064(8) 0.032(9) 0.034(6) 0.026(10) C11A 0.080(10) 0.058(8) 0.091(15) 0.017(10) -0.007(12) -0.015(7) C7B 0.050(7) 0.095(13) 0.035(6) -0.030(7) -0.012(5) 0.013(7) C8B 0.078(10) 0.15(2) 0.017(4) 0.000(7) 0.009(6) 0.059(12) N9B 0.051(6) 0.051(5) 0.036(5) 0.012(4) 0.016(4) 0.018(4) C10B 0.078(10) 0.061(8) 0.053(8) 0.013(7) 0.009(7) -0.001(6) C11B 0.073(9) 0.047(5) 0.073(9) 0.012(6) 0.018(7) -0.012(5) N12 0.092(4) 0.047(2) 0.147(6) 0.006(3) 0.055(4) 0.003(2) O1 0.050(2) 0.120(4) 0.073(3) -0.007(3) 0.000(2) -0.017(2) O2 0.151(6) 0.131(6) 0.104(5) -0.014(4) 0.016(4) 0.004(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 W1 C4 2.143(3) 2_655 ? W1 C4 2.143(3) . y W1 C3 2.162(3) 2_655 ? W1 C3 2.162(3) . y W1 C2 2.162(3) . y W1 C2 2.162(3) 2_655 ? W1 C1 2.161(3) 2_655 ? W1 C1 2.161(3) . y C1 N1 1.151(4) . y N1 Cu1 2.290(3) 4_546 ? C2 N2 1.149(5) . y C3 N3 1.146(5) . y C4 N4 1.153(4) . y N4 Cu1 1.947(3) . y Cu1 N9B 2.020(10) . y Cu1 N12 2.027(6) . y Cu1 N6 2.037(5) . y Cu1 N9A 2.033(11) . y Cu1 N1 2.290(3) 4_556 y N6 C7A 1.376(15) . ? N6 C7B 1.624(17) . ? C7A C8A 1.51(3) . ? C7A H7A1 0.9700 . ? C7A H7A2 0.9700 . ? C8A N9A 1.48(2) . ? C8A H8A1 0.9700 . ? C8A H8A2 0.9700 . ? N9A C10A 1.52(2) . ? C10A C11A 1.46(2) . ? C10A H10A 0.9700 . ? C10A H10B 0.9700 . ? C11A N12 1.65(2) . ? C11A H11A 0.9700 . ? C11A H11B 0.9700 . ? C7B C8B 1.43(3) . ? C7B H7B1 0.9700 . ? C7B H7B2 0.9700 . ? C8B N9B 1.48(2) . ? C8B H8B1 0.9700 . ? C8B H8B2 0.9700 . ? N9B C10B 1.491(19) . ? C10B C11B 1.49(2) . ? C10B H10C 0.9700 . ? C10B H10D 0.9700 . ? C11B N12 1.465(16) . ? C11B H11C 0.9700 . ? C11B H11D 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 W1 C4 77.57(17) 2_655 . ? C4 W1 C3 114.90(15) 2_655 2_655 ? C4 W1 C3 141.72(11) . 2_655 ? C4 W1 C3 141.72(11) 2_655 . ? C4 W1 C3 114.90(15) . . ? C3 W1 C3 78.7(2) 2_655 . ? C4 W1 C2 141.79(13) 2_655 . ? C4 W1 C2 72.01(13) . . ? C3 W1 C2 78.71(15) 2_655 . ? C3 W1 C2 73.89(13) . . ? C4 W1 C2 72.01(13) 2_655 2_655 ? C4 W1 C2 141.79(13) . 2_655 ? C3 W1 C2 73.89(13) 2_655 2_655 ? C3 W1 C2 78.71(15) . 2_655 ? C2 W1 C2 144.37(19) . 2_655 ? C4 W1 C1 77.10(12) 2_655 2_655 ? C4 W1 C1 73.48(12) . 2_655 ? C3 W1 C1 142.93(12) 2_655 2_655 ? C3 W1 C1 72.89(12) . 2_655 ? C2 W1 C1 114.46(14) . 2_655 ? C2 W1 C1 77.60(14) 2_655 2_655 ? C4 W1 C1 73.48(12) 2_655 . ? C4 W1 C1 77.10(12) . . ? C3 W1 C1 72.89(12) 2_655 . ? C3 W1 C1 142.93(12) . . ? C2 W1 C1 77.60(14) . . ? C2 W1 C1 114.46(14) 2_655 . ? C1 W1 C1 142.00(16) 2_655 . ? N1 C1 W1 177.3(3) . . ? C1 N1 Cu1 140.7(3) . 4_546 y N2 C2 W1 177.3(4) . . ? N3 C3 W1 177.7(3) . . ? N4 C4 W1 174.9(3) . . ? C4 N4 Cu1 161.2(4) . . y N4 Cu1 N9B 167.3(3) . . y N4 Cu1 N12 92.6(2) . . y N9B Cu1 N12 76.9(3) . . y N4 Cu1 N6 94.88(19) . . y N9B Cu1 N6 93.1(4) . . y N12 Cu1 N6 160.9(3) . . y N4 Cu1 N9A 166.6(3) . . y N9B Cu1 N9A 17.6(3) . . ? N12 Cu1 N9A 93.9(3) . . y N6 Cu1 N9A 75.5(4) . . y N4 Cu1 N1 99.28(14) . 4_556 y N9B Cu1 N1 89.1(3) . 4_556 y N12 Cu1 N1 96.4(2) . 4_556 y N6 Cu1 N1 99.71(18) . 4_556 y N9A Cu1 N1 91.6(3) . 4_556 y C7A N6 C7B 25.1(7) . . ? C7A N6 Cu1 121.3(8) . . ? C7B N6 Cu1 97.1(6) . . ? N6 C7A C8A 101.4(12) . . ? N6 C7A H7A1 111.5 . . ? C8A C7A H7A1 111.5 . . ? N6 C7A H7A2 111.5 . . ? C8A C7A H7A2 111.5 . . ? H7A1 C7A H7A2 109.3 . . ? N9A C8A C7A 105.6(13) . . ? N9A C8A H8A1 110.6 . . ? C7A C8A H8A1 110.6 . . ? N9A C8A H8A2 110.6 . . ? C7A C8A H8A2 110.6 . . ? H8A1 C8A H8A2 108.7 . . ? C8A N9A C10A 117.0(13) . . ? C8A N9A Cu1 109.7(9) . . ? C10A N9A Cu1 104.7(8) . . ? N9A C10A C11A 108.0(11) . . ? N9A C10A H10A 110.1 . . ? C11A C10A H10A 110.1 . . ? N9A C10A H10B 110.1 . . ? C11A C10A H10B 110.1 . . ? H10A C10A H10B 108.4 . . ? C10A C11A N12 115.8(13) . . ? C10A C11A H11A 108.3 . . ? N12 C11A H11A 108.3 . . ? C10A C11A H11B 108.3 . . ? N12 C11A H11B 108.3 . . ? H11A C11A H11B 107.4 . . ? C8B C7B N6 118.5(10) . . ? C8B C7B H7B1 107.7 . . ? N6 C7B H7B1 107.7 . . ? C8B C7B H7B2 107.7 . . ? N6 C7B H7B2 107.7 . . ? H7B1 C7B H7B2 107.1 . . ? C7B C8B N9B 109.9(13) . . ? C7B C8B H8B1 109.7 . . ? N9B C8B H8B1 109.7 . . ? C7B C8B H8B2 109.7 . . ? N9B C8B H8B2 109.7 . . ? H8B1 C8B H8B2 108.2 . . ? C8B N9B C10B 121.0(14) . . ? C8B N9B Cu1 102.8(9) . . ? C10B N9B Cu1 112.4(9) . . ? C11B C10B N9B 107.8(12) . . ? C11B C10B H10C 110.1 . . ? N9B C10B H10C 110.1 . . ? C11B C10B H10D 110.1 . . ? N9B C10B H10D 110.1 . . ? H10C C10B H10D 108.4 . . ? N12 C11B C10B 97.7(13) . . ? N12 C11B H11C 112.2 . . ? C10B C11B H11C 112.2 . . ? N12 C11B H11D 112.2 . . ? C10B C11B H11D 112.2 . . ? H11C C11B H11D 109.8 . . ? C11B N12 C11A 25.9(7) . . ? C11B N12 Cu1 115.2(7) . . ? C11A N12 Cu1 96.2(7) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 43.08 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.233 _refine_diff_density_min -1.788 _refine_diff_density_rms 0.143 data_mo4cudien _database_code_CSD 212730 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Cu(dien)]2 [Mo(CN)8] 4H2O' _chemical_formula_sum 'C16 H34 Cu2 Mo N14 O4' _chemical_formula_weight 673.56 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 12.8722(2) _cell_length_b 9.9763(1) _cell_length_c 11.3757(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1460.83(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3470 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 34.972 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.531 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 1.903 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'HKL DENZO and Scalepack (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.5810 _exptl_absorpt_correction_T_max 0.8038 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f and \w scans to fill Ewald sphere' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6352 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0350 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 34.95 _reflns_number_total 6352 _reflns_number_gt 5848 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL DENZO and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution ; SIR (Altomare, Cascarano, Giacovazzo, Guagliardi, Burla, Polidori, Camalli, 1994) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 (Farruggia, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0347P)^2^+0.7620P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0140(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.557(13) _refine_ls_number_reflns 6352 _refine_ls_number_parameters 164 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0414 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0857 _refine_ls_wR_factor_gt 0.0824 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 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 Mo1 Mo 0.5000 0.0000 0.302677(16) 0.02037(5) Uani 1 2 d S . . C1 C 0.39856(18) -0.1571(2) 0.3642(2) 0.0308(4) Uani 1 1 d . . . N1 N 0.3410(2) -0.2382(3) 0.3949(2) 0.0455(6) Uani 1 1 d . . . C2 C 0.3494(2) 0.0696(3) 0.2450(2) 0.0395(5) Uani 1 1 d . . . N2 N 0.2677(2) 0.1041(4) 0.2180(3) 0.0671(9) Uani 1 1 d . . . C3 C 0.5284(2) 0.1319(3) 0.1554(2) 0.0402(5) Uani 1 1 d . . . N3 N 0.5468(2) 0.2015(4) 0.0770(3) 0.0660(10) Uani 1 1 d . . . C4 C 0.42339(18) 0.0909(2) 0.4504(2) 0.0312(4) Uani 1 1 d . . . N4 N 0.37952(18) 0.1307(3) 0.5309(2) 0.0440(5) Uani 1 1 d . A . Cu1 Cu 0.29550(3) 0.13681(4) 0.67335(3) 0.04377(10) Uani 1 1 d . . . N6A N 0.3892(4) 0.2990(6) 0.7422(5) 0.0402(11) Uiso 0.496(7) 1 d P A 1 H6A1 H 0.4569 0.2766 0.7399 0.048 Uiso 0.496(7) 1 calc PR A 1 H6A2 H 0.3800 0.3734 0.6986 0.048 Uiso 0.496(7) 1 calc PR A 1 C7A C 0.3568(5) 0.3241(7) 0.8649(6) 0.0459(14) Uiso 0.496(7) 1 d P A 1 H7A1 H 0.4155 0.3569 0.9099 0.055 Uiso 0.496(7) 1 calc PR A 1 H7A2 H 0.3030 0.3922 0.8663 0.055 Uiso 0.496(7) 1 calc PR A 1 C8A C 0.3173(5) 0.2001(7) 0.9182(6) 0.0437(13) Uiso 0.496(7) 1 d P A 1 H8A1 H 0.3739 0.1374 0.9305 0.052 Uiso 0.496(7) 1 calc PR A 1 H8A2 H 0.2858 0.2195 0.9938 0.052 Uiso 0.496(7) 1 calc PR A 1 N9A N 0.2415(4) 0.1429(5) 0.8401(4) 0.0355(10) Uiso 0.496(7) 1 d P A 1 H9A H 0.1858 0.1991 0.8402 0.043 Uiso 0.496(7) 1 calc PR A 1 C10A C 0.2022(6) 0.0091(9) 0.8654(7) 0.0597(17) Uiso 0.496(7) 1 d P A 1 H10A H 0.1499 0.0143 0.9266 0.072 Uiso 0.496(7) 1 calc PR A 1 H10B H 0.2585 -0.0468 0.8938 0.072 Uiso 0.496(7) 1 calc PR A 1 C11A C 0.1561(8) -0.0525(10) 0.7582(11) 0.073(2) Uiso 0.496(7) 1 d P A 1 H11A H 0.0941 -0.0047 0.7338 0.087 Uiso 0.496(7) 1 calc PR A 1 H11B H 0.1386 -0.1458 0.7717 0.087 Uiso 0.496(7) 1 calc PR A 1 N12A N 0.2429(6) -0.0393(7) 0.6657(7) 0.0607(18) Uiso 0.496(7) 1 d P A 1 H12A H 0.2174 -0.0557 0.5934 0.073 Uiso 0.496(7) 1 calc PR A 1 H12B H 0.2938 -0.0987 0.6805 0.073 Uiso 0.496(7) 1 calc PR A 1 N6B N 0.3673(5) 0.2614(7) 0.7608(6) 0.0519(15) Uiso 0.504(7) 1 d P A 2 H6B1 H 0.4352 0.2400 0.7605 0.062 Uiso 0.504(7) 1 calc PR A 2 H6B2 H 0.3606 0.3424 0.7268 0.062 Uiso 0.504(7) 1 calc PR A 2 C7B C 0.3298(6) 0.2697(8) 0.8865(7) 0.0531(16) Uiso 0.504(7) 1 d P A 2 H7B1 H 0.3870 0.2914 0.9387 0.064 Uiso 0.504(7) 1 calc PR A 2 H7B2 H 0.2769 0.3383 0.8943 0.064 Uiso 0.504(7) 1 calc PR A 2 C8B C 0.2871(6) 0.1383(8) 0.9153(7) 0.0564(17) Uiso 0.504(7) 1 d P A 2 H8B1 H 0.2510 0.1423 0.9900 0.068 Uiso 0.504(7) 1 calc PR A 2 H8B2 H 0.3428 0.0733 0.9219 0.068 Uiso 0.504(7) 1 calc PR A 2 N9B N 0.2137(4) 0.0972(5) 0.8205(4) 0.0387(11) Uiso 0.504(7) 1 d P A 2 H9B H 0.1594 0.1557 0.8223 0.046 Uiso 0.504(7) 1 calc PR A 2 C10B C 0.1701(7) -0.0370(8) 0.8211(9) 0.0596(19) Uiso 0.504(7) 1 d P A 2 H10C H 0.1118 -0.0411 0.8751 0.072 Uiso 0.504(7) 1 calc PR A 2 H10D H 0.2221 -0.1008 0.8470 0.072 Uiso 0.504(7) 1 calc PR A 2 C11B C 0.1351(7) -0.0711(9) 0.7009(9) 0.067(2) Uiso 0.504(7) 1 d P A 2 H11C H 0.1135 -0.1642 0.6976 0.081 Uiso 0.504(7) 1 calc PR A 2 H11D H 0.0766 -0.0154 0.6789 0.081 Uiso 0.504(7) 1 calc PR A 2 N12B N 0.2196(6) -0.0491(7) 0.6224(7) 0.0580(16) Uiso 0.504(7) 1 d P A 2 H12C H 0.1963 -0.0431 0.5481 0.070 Uiso 0.504(7) 1 calc PR A 2 H12D H 0.2649 -0.1177 0.6266 0.070 Uiso 0.504(7) 1 calc PR A 2 O1 O 0.4046(2) -0.2222(4) 0.8276(3) 0.0791(9) Uani 1 1 d . . . O2 O 0.1114(4) 0.0453(5) 0.4205(5) 0.1323(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.01850(8) 0.02673(10) 0.01587(8) 0.000 0.000 -0.00211(9) C1 0.0323(10) 0.0355(11) 0.0245(9) -0.0012(8) -0.0001(7) -0.0066(8) N1 0.0488(13) 0.0497(13) 0.0381(12) 0.0009(10) 0.0035(10) -0.0217(11) C2 0.0315(10) 0.0570(16) 0.0300(11) 0.0077(11) -0.0025(9) 0.0051(10) N2 0.0406(12) 0.109(3) 0.0516(17) 0.0120(16) -0.0105(12) 0.0212(15) C3 0.0352(10) 0.0542(14) 0.0311(11) 0.0109(11) -0.0075(8) -0.0157(10) N3 0.0593(17) 0.094(2) 0.0448(15) 0.0335(16) -0.0170(13) -0.0347(16) C4 0.0285(9) 0.0383(11) 0.0267(10) -0.0033(8) 0.0008(8) 0.0005(8) N4 0.0374(10) 0.0591(14) 0.0354(11) -0.0118(11) 0.0077(8) 0.0056(10) Cu1 0.04550(18) 0.0556(2) 0.03019(15) 0.00365(14) 0.01157(13) 0.01998(15) O1 0.0528(14) 0.117(2) 0.0674(18) -0.0093(19) 0.0021(14) -0.0179(16) O2 0.150(4) 0.135(4) 0.112(3) -0.019(3) 0.011(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 Mo1 C4 2.149(2) 2_655 ? Mo1 C4 2.149(2) . y Mo1 C1 2.157(2) 2_655 ? Mo1 C1 2.157(2) . y Mo1 C2 2.161(3) 2_655 ? Mo1 C2 2.161(3) . y Mo1 C3 2.162(3) 2_655 ? Mo1 C3 2.162(3) . y C1 N1 1.151(3) . y N1 Cu1 2.291(2) 4_546 y C2 N2 1.149(4) . y C3 N3 1.155(4) . y C4 N4 1.147(3) . y N4 Cu1 1.949(2) . y Cu1 N6B 1.841(7) . y Cu1 N12A 1.885(7) . y Cu1 N9B 2.017(5) . y Cu1 N9A 2.021(5) . y Cu1 N6A 2.165(6) . y Cu1 N12B 2.174(7) . y Cu1 N1 2.291(2) 4_556 y N6A C7A 1.478(9) . ? N6A H6A1 0.9000 . ? N6A H6A2 0.9000 . ? C7A C8A 1.469(9) . ? C7A H7A1 0.9700 . ? C7A H7A2 0.9700 . ? C8A N9A 1.438(8) . ? C8A H8A1 0.9700 . ? C8A H8A2 0.9700 . ? N9A C10A 1.457(10) . ? N9A H9A 0.9100 . ? C10A C11A 1.489(13) . ? C10A H10A 0.9700 . ? C10A H10B 0.9700 . ? C11A N12A 1.541(13) . ? C11A H11A 0.9700 . ? C11A H11B 0.9700 . ? N12A H12A 0.9000 . ? N12A H12B 0.9000 . ? N6B C7B 1.512(10) . ? N6B H6B1 0.9000 . ? N6B H6B2 0.9000 . ? C7B C8B 1.458(11) . ? C7B H7B1 0.9700 . ? C7B H7B2 0.9700 . ? C8B N9B 1.492(9) . ? C8B H8B1 0.9700 . ? C8B H8B2 0.9700 . ? N9B C10B 1.452(9) . ? N9B H9B 0.9100 . ? C10B C11B 1.479(13) . ? C10B H10C 0.9700 . ? C10B H10D 0.9700 . ? C11B N12B 1.424(11) . ? C11B H11C 0.9700 . ? C11B H11D 0.9700 . ? N12B H12C 0.9000 . ? N12B H12D 0.9000 . ? 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 C4 Mo1 C4 77.13(13) 2_655 . ? C4 Mo1 C1 77.00(9) 2_655 2_655 ? C4 Mo1 C1 73.57(9) . 2_655 ? C4 Mo1 C1 73.57(9) 2_655 . ? C4 Mo1 C1 77.00(9) . . ? C1 Mo1 C1 142.10(12) 2_655 . ? C4 Mo1 C2 71.96(10) 2_655 2_655 ? C4 Mo1 C2 141.69(9) . 2_655 ? C1 Mo1 C2 77.83(10) 2_655 2_655 ? C1 Mo1 C2 114.09(11) . 2_655 ? C4 Mo1 C2 141.69(9) 2_655 . ? C4 Mo1 C2 71.96(10) . . ? C1 Mo1 C2 114.09(11) 2_655 . ? C1 Mo1 C2 77.83(10) . . ? C2 Mo1 C2 144.63(15) 2_655 . ? C4 Mo1 C3 115.28(11) 2_655 2_655 ? C4 Mo1 C3 141.74(9) . 2_655 ? C1 Mo1 C3 142.80(9) 2_655 2_655 ? C1 Mo1 C3 72.96(9) . 2_655 ? C2 Mo1 C3 73.79(10) 2_655 2_655 ? C2 Mo1 C3 78.94(11) . 2_655 ? C4 Mo1 C3 141.74(9) 2_655 . ? C4 Mo1 C3 115.28(11) . . ? C1 Mo1 C3 72.96(9) 2_655 . ? C1 Mo1 C3 142.80(9) . . ? C2 Mo1 C3 78.94(11) 2_655 . ? C2 Mo1 C3 73.79(10) . . ? C3 Mo1 C3 78.36(16) 2_655 . ? N1 C1 Mo1 177.1(2) . . ? C1 N1 Cu1 140.7(2) . 4_546 y N2 C2 Mo1 177.4(3) . . ? N3 C3 Mo1 177.9(3) . . ? N4 C4 Mo1 175.1(2) . . ? C4 N4 Cu1 161.5(3) . . y N6B Cu1 N12A 146.6(3) . . ? N6B Cu1 N4 101.1(2) . . y N12A Cu1 N4 97.6(2) . . y N6B Cu1 N9B 86.9(3) . . y N12A Cu1 N9B 70.6(3) . . ? N4 Cu1 N9B 166.81(16) . . y N6B Cu1 N9A 69.2(3) . . ? N12A Cu1 N9A 87.0(3) . . y N4 Cu1 N9A 166.41(16) . . y N9B Cu1 N9A 17.71(15) . . ? N6B Cu1 N6A 11.5(3) . . ? N12A Cu1 N6A 156.0(3) . . y N4 Cu1 N6A 90.87(17) . . y N9B Cu1 N6A 97.9(2) . . ? N9A Cu1 N6A 80.2(2) . . y N6B Cu1 N12B 161.0(3) . . y N12A Cu1 N12B 14.4(3) . . ? N4 Cu1 N12B 90.0(2) . . y N9B Cu1 N12B 79.6(2) . . y N9A Cu1 N12B 97.0(2) . . ? N6A Cu1 N12B 169.8(2) . . ? N6B Cu1 N1 101.6(2) . 4_556 y N12A Cu1 N1 102.5(3) . 4_556 y N4 Cu1 N1 99.26(10) . 4_556 y N9B Cu1 N1 89.27(15) . 4_556 y N9A Cu1 N1 92.18(14) . 4_556 y N6A Cu1 N1 98.23(16) . 4_556 y N12B Cu1 N1 91.7(2) . 4_556 y C7A N6A Cu1 108.1(4) . . ? C7A N6A H6A1 110.1 . . ? Cu1 N6A H6A1 110.1 . . ? C7A N6A H6A2 110.1 . . ? Cu1 N6A H6A2 110.1 . . ? H6A1 N6A H6A2 108.4 . . ? C8A C7A N6A 110.2(5) . . ? C8A C7A H7A1 109.6 . . ? N6A C7A H7A1 109.6 . . ? C8A C7A H7A2 109.6 . . ? N6A C7A H7A2 109.6 . . ? H7A1 C7A H7A2 108.1 . . ? N9A C8A C7A 108.3(5) . . ? N9A C8A H8A1 110.0 . . ? C7A C8A H8A1 110.0 . . ? N9A C8A H8A2 110.0 . . ? C7A C8A H8A2 110.0 . . ? H8A1 C8A H8A2 108.4 . . ? C8A N9A C10A 118.5(5) . . ? C8A N9A Cu1 111.0(4) . . ? C10A N9A Cu1 106.1(4) . . ? C8A N9A H9A 106.9 . . ? C10A N9A H9A 106.9 . . ? Cu1 N9A H9A 106.9 . . ? N9A C10A C11A 110.8(6) . . ? N9A C10A H10A 109.5 . . ? C11A C10A H10A 109.5 . . ? N9A C10A H10B 109.5 . . ? C11A C10A H10B 109.5 . . ? H10A C10A H10B 108.1 . . ? C10A C11A N12A 103.6(8) . . ? C10A C11A H11A 111.0 . . ? N12A C11A H11A 111.0 . . ? C10A C11A H11B 111.0 . . ? N12A C11A H11B 111.0 . . ? H11A C11A H11B 109.0 . . ? C11A N12A Cu1 108.0(6) . . ? C11A N12A H12A 110.1 . . ? Cu1 N12A H12A 110.1 . . ? C11A N12A H12B 110.1 . . ? Cu1 N12A H12B 110.1 . . ? H12A N12A H12B 108.4 . . ? C7B N6B Cu1 112.8(5) . . ? C7B N6B H6B1 109.0 . . ? Cu1 N6B H6B1 109.0 . . ? C7B N6B H6B2 109.0 . . ? Cu1 N6B H6B2 109.0 . . ? H6B1 N6B H6B2 107.8 . . ? C8B C7B N6B 106.5(6) . . ? C8B C7B H7B1 110.4 . . ? N6B C7B H7B1 110.4 . . ? C8B C7B H7B2 110.4 . . ? N6B C7B H7B2 110.4 . . ? H7B1 C7B H7B2 108.6 . . ? C7B C8B N9B 108.9(6) . . ? C7B C8B H8B1 109.9 . . ? N9B C8B H8B1 109.9 . . ? C7B C8B H8B2 109.9 . . ? N9B C8B H8B2 109.9 . . ? H8B1 C8B H8B2 108.3 . . ? C10B N9B C8B 119.7(6) . . ? C10B N9B Cu1 112.7(5) . . ? C8B N9B Cu1 102.4(4) . . ? C10B N9B H9B 107.1 . . ? C8B N9B H9B 107.1 . . ? Cu1 N9B H9B 107.1 . . ? N9B C10B C11B 109.0(7) . . ? N9B C10B H10C 109.9 . . ? C11B C10B H10C 109.9 . . ? N9B C10B H10D 109.9 . . ? C11B C10B H10D 109.9 . . ? H10C C10B H10D 108.3 . . ? N12B C11B C10B 108.2(7) . . ? N12B C11B H11C 110.1 . . ? C10B C11B H11C 110.1 . . ? N12B C11B H11D 110.1 . . ? C10B C11B H11D 110.1 . . ? H11C C11B H11D 108.4 . . ? C11B N12B Cu1 107.9(6) . . ? C11B N12B H12C 110.1 . . ? Cu1 N12B H12C 110.1 . . ? C11B N12B H12D 110.1 . . ? Cu1 N12B H12D 110.1 . . ? H12C N12B H12D 108.4 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 34.95 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.660 _refine_diff_density_min -0.619 _refine_diff_density_rms 0.083