# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 #start Validation Reply Form _vrf_PLAT306_1 ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O18 RESPONSE: The hydrogen atoms belonging to the water molecule could not be located unambiguously using the difference Fourier maps or potential hydrogen bonds and were therefore not added to the model. ; _chemical_formula_moiety '(Cu1 Cl1 C6 O11 H4, Co1 N6 H18)' _chemical_formula_sum 'C6 H22 Cl1 Co1 Cu1 N6 O11' _chemical_formula_weight 512.21 _chemical_absolute_configuration . _chemical_compound_source ? 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 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 C 4.2.6.8 and 6.1.1.4' Co 0.3494 0.9721 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692 1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,-y,-z 3 -x,y+1/2,-z+1/2 4 x,-y+1/2,z+1/2 _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall '-P 2ybc' _cell_length_a 13.2165(13) _cell_length_b 9.0119(10) _cell_length_c 14.5162(16) _cell_angle_alpha 90 _cell_angle_beta 91.457(12) _cell_angle_gamma 90 _cell_volume 1728.4(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 8000 _cell_measurement_temperature 293 _cell_measurement_theta_max 26.005 _cell_measurement_theta_min 2.661 _exptl_absorpt_coefficient_mu 2.413 _exptl_absorpt_correction_T_max 0.89 _exptl_absorpt_correction_T_min 0.51 # Sheldrick geometric approximatio 0.62 0.89 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.968 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description platelet # Non-dispersive F(000): _exptl_crystal_F_000 1044 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _diffrn_reflns_av_R_equivalents 0.053 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_number 24359 _diffrn_reflns_theta_full 25.224 _diffrn_reflns_theta_max 26.005 # Number of reflections with Friedels Law is 3500 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 3399 _diffrn_reflns_theta_min 2.661 _diffrn_ambient_temperature 293 _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.968 _diffrn_measurement_device 'one-circle diffractometer ' _diffrn_measurement_device_type 'STOE IPDS 1' _diffrn_measurement_method '\f scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number 0 _reflns_limit_h_min -16 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 11 _reflns_limit_l_min 0 _reflns_limit_l_max 17 _reflns_number_gt 2363 _reflns_number_total 3278 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _computing_cell_refinement 'X-area (STOE)' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'X-area (STOE)' _computing_data_reduction 'X-area (STOE)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_structure_solution 'Sir2004 (Burla et al., 2005)' _refine_diff_density_max 0.59 _refine_diff_density_min -0.63 _refine_ls_extinction_method None _refine_ls_goodness_of_fit_ref 1.1777 _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, _refine_ls_matrix_type full _refine_ls_number_parameters 235 _refine_ls_number_reflns 2715 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0400 _refine_ls_R_factor_gt 0.0298 _refine_ls_shift/su_max 0.008639 _refine_ls_shift/su_mean 0.000856 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 16.0 20.0 8.09 ; # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.0633 _refine_ls_wR_factor_gt 0.0580 _refine_ls_wR_factor_ref 0.0603 # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct #heavy,direct,difmap,geom # 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_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Cu1 Cu 0.26931(3) 0.28649(4) 0.22119(3) 0.0292 1.0000 Uani . . . . . . . O2 O 0.16508(18) 0.3797(3) 0.29294(19) 0.0343 1.0000 Uani . . . . . . . C3 C 0.0824(2) 0.3217(4) 0.3185(2) 0.0219 1.0000 Uani . . . . . . . O4 O 0.02857(18) 0.3794(3) 0.37662(17) 0.0330 1.0000 Uani . . . . . . . C5 C 0.0492(2) 0.1781(4) 0.2713(2) 0.0244 1.0000 Uani . . . . . . . O6 O -0.04268(18) 0.1288(3) 0.3061(2) 0.0421 1.0000 Uani . . . . . . . C7 C 0.1309(2) 0.0564(4) 0.2775(2) 0.0226 1.0000 Uani . . . . . . . O8 O 0.21637(18) 0.0873(3) 0.24518(19) 0.0332 1.0000 Uani . . . . . . . O9 O 0.33500(17) 0.4785(3) 0.19854(18) 0.0300 1.0000 Uani . . . . . . . C10 C 0.4285(3) 0.4942(4) 0.1830(2) 0.0252 1.0000 Uani . . . . . . . O11 O 0.46436(19) 0.6024(3) 0.14184(19) 0.0353 1.0000 Uani . . . . . . . C12 C 0.4997(2) 0.3717(4) 0.2185(2) 0.0226 1.0000 Uani . . . . . . . O13 O 0.60315(17) 0.4034(3) 0.20730(18) 0.0325 1.0000 Uani . . . . . . . C14 C 0.4747(2) 0.2252(4) 0.1696(2) 0.0245 1.0000 Uani . . . . . . . O15 O 0.54142(18) 0.1570(3) 0.13001(19) 0.0375 1.0000 Uani . . . . . . . O16 O 0.38363(17) 0.1768(3) 0.17476(18) 0.0310 1.0000 Uani . . . . . . . O18 O 0.3576(3) 0.2636(4) 0.4104(3) 0.0769 1.0000 Uani . . . . . . . H8 H 0.6141 0.5008 0.2218 0.0500 1.0000 Uiso R . . . . . . H12 H 0.4841 0.3576 0.2804 0.0500 1.0000 Uiso R . . . . . . H18 H -0.0431 0.0333 0.3102 0.0500 1.0000 Uiso R . . . . . . O21 O 0.10693(19) -0.0654(3) 0.30854(18) 0.0339 1.0000 Uani . . . . . . . H22 H 0.0424 0.2019 0.2082 0.0500 1.0000 Uiso R . . . . . . Cl1 Cl 0.16924(9) 0.33813(11) 0.05270(8) 0.0470 1.0000 Uani . . . . . . . Co19 Co 0.23221(3) 0.69312(5) 0.50965(3) 0.0176 1.0000 Uani . . . . . . . N20 N 0.1491(2) 0.5174(3) 0.5288(2) 0.0299 1.0000 Uani . . . . . . . N21 N 0.1067(2) 0.8106(3) 0.49553(19) 0.0273 1.0000 Uani . . . . . . . N22 N 0.3134(2) 0.8726(3) 0.4897(2) 0.0285 1.0000 Uani . . . . . . . N23 N 0.3556(2) 0.5718(4) 0.5274(2) 0.0384 1.0000 Uani . . . . . . . N24 N 0.2321(2) 0.7314(3) 0.64297(18) 0.0257 1.0000 Uani . . . . . . . N25 N 0.2348(2) 0.6606(3) 0.37603(18) 0.0248 1.0000 Uani . . . . . . . H25 H 0.1847 0.4415 0.5527 0.0500 1.0000 Uiso R . . . . . . H26 H 0.1008 0.5408 0.5684 0.0500 1.0000 Uiso R . . . . . . H27 H 0.1187 0.4861 0.4760 0.0500 1.0000 Uiso R . . . . . . H29 H 0.2588 0.6536 0.6714 0.0500 1.0000 Uiso R . . . . . . H30 H 0.2692 0.8114 0.6571 0.0500 1.0000 Uiso R . . . . . . H31 H 0.1700 0.7464 0.6658 0.0500 1.0000 Uiso R . . . . . . H33 H 0.0553 0.7776 0.5278 0.0500 1.0000 Uiso R . . . . . . H34 H 0.0862 0.8149 0.4356 0.0500 1.0000 Uiso R . . . . . . H35 H 0.1203 0.9046 0.5134 0.0500 1.0000 Uiso R . . . . . . H37 H 0.3397 0.8763 0.4332 0.0500 1.0000 Uiso R . . . . . . H38 H 0.2783 0.9569 0.4984 0.0500 1.0000 Uiso R . . . . . . H39 H 0.3651 0.8710 0.5314 0.0500 1.0000 Uiso R . . . . . . H41 H 0.2007 0.7324 0.3456 0.0500 1.0000 Uiso R . . . . . . H42 H 0.2077 0.5734 0.3596 0.0500 1.0000 Uiso R . . . . . . H43 H 0.2989 0.6619 0.3553 0.0500 1.0000 Uiso R . . . . . . H45 H 0.4107 0.6299 0.5316 0.0500 1.0000 Uiso R . . . . . . H46 H 0.3530 0.5173 0.5780 0.0500 1.0000 Uiso R . . . . . . H47 H 0.3639 0.5109 0.4789 0.0500 1.0000 Uiso 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 Cu1 0.0197(2) 0.0168(2) 0.0516(3) -0.00553(19) 0.01186(18) -0.00011(16) O2 0.0277(13) 0.0190(12) 0.0569(17) -0.0091(11) 0.0158(12) -0.0018(10) C3 0.0193(16) 0.0199(16) 0.0267(16) 0.0006(13) 0.0012(13) 0.0047(12) O4 0.0308(13) 0.0325(14) 0.0362(14) -0.0109(11) 0.0094(11) -0.0003(11) C5 0.0197(16) 0.0229(17) 0.0306(17) -0.0019(14) 0.0034(13) 0.0013(13) O6 0.0245(13) 0.0255(13) 0.077(2) -0.0109(13) 0.0167(13) -0.0048(11) C7 0.0265(17) 0.0183(16) 0.0232(16) -0.0035(13) 0.0024(13) 0.0008(13) O8 0.0249(13) 0.0184(12) 0.0570(17) 0.0026(11) 0.0132(12) 0.0025(10) O9 0.0195(12) 0.0199(12) 0.0508(15) 0.0005(11) 0.0020(11) 0.0015(9) C10 0.0249(18) 0.0208(16) 0.0297(18) -0.0038(14) -0.0028(14) 0.0001(13) O11 0.0312(14) 0.0262(13) 0.0483(16) 0.0086(12) -0.0044(12) -0.0067(11) C12 0.0192(16) 0.0195(16) 0.0291(17) -0.0013(13) 0.0018(13) 0.0004(12) O13 0.0165(12) 0.0263(13) 0.0545(16) -0.0054(12) -0.0013(11) -0.0021(10) C14 0.0177(16) 0.0237(17) 0.0323(18) -0.0005(14) 0.0040(13) 0.0011(13) O15 0.0242(13) 0.0350(15) 0.0538(17) -0.0164(13) 0.0126(12) 0.0006(11) O16 0.0191(12) 0.0235(13) 0.0509(15) -0.0111(11) 0.0075(11) -0.0011(9) O18 0.073(2) 0.051(2) 0.108(3) 0.000(2) 0.022(2) 0.0059(19) O21 0.0395(15) 0.0209(13) 0.0418(15) 0.0055(11) 0.0087(12) -0.0006(11) Cl1 0.0563(6) 0.0263(5) 0.0578(6) 0.0054(4) -0.0119(5) -0.0086(4) Co19 0.0174(2) 0.0159(2) 0.0195(2) 0.00064(16) 0.00169(15) -0.00027(16) N20 0.0316(16) 0.0218(15) 0.0367(17) 0.0012(13) 0.0085(13) -0.0030(12) N21 0.0237(15) 0.0291(15) 0.0293(15) 0.0018(12) 0.0037(12) 0.0033(12) N22 0.0292(16) 0.0270(15) 0.0296(15) -0.0020(12) 0.0043(12) -0.0079(12) N23 0.0305(17) 0.044(2) 0.0406(18) 0.0157(16) 0.0086(14) 0.0119(15) N24 0.0255(15) 0.0282(15) 0.0235(14) 0.0008(12) 0.0013(11) -0.0028(12) N25 0.0270(15) 0.0222(14) 0.0254(14) -0.0030(11) 0.0037(11) -0.0022(11) 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 Cu1 . O2 . 1.939(2) yes Cu1 . O8 . 1.961(2) yes Cu1 . O9 . 1.967(2) yes Cu1 . O16 . 1.941(2) yes Cu1 . Cl1 . 2.7899(12) yes O2 . C3 . 1.275(4) yes C3 . O4 . 1.232(4) yes C3 . C5 . 1.523(4) yes C5 . O6 . 1.399(4) yes C5 . C7 . 1.541(4) yes C5 . H22 . 0.942 no O6 . H18 . 0.862 no C7 . O8 . 1.265(4) yes C7 . O21 . 1.231(4) yes O9 . C10 . 1.270(4) yes C10 . O11 . 1.244(4) yes C10 . C12 . 1.531(4) yes C12 . O13 . 1.411(4) yes C12 . C14 . 1.531(4) yes C12 . H12 . 0.935 no O13 . H8 . 0.913 no C14 . O15 . 1.229(4) yes C14 . O16 . 1.284(4) yes Co19 . N20 . 1.951(3) yes Co19 . N21 . 1.974(3) yes Co19 . N22 . 1.966(3) yes Co19 . N23 . 1.974(3) yes Co19 . N24 . 1.966(3) yes Co19 . N25 . 1.963(3) yes N20 . H25 . 0.895 no N20 . H26 . 0.896 no N20 . H27 . 0.901 no N21 . H33 . 0.888 no N21 . H34 . 0.906 no N21 . H35 . 0.902 no N22 . H37 . 0.899 no N22 . H38 . 0.901 no N22 . H39 . 0.902 no N23 . H45 . 0.897 no N23 . H46 . 0.885 no N23 . H47 . 0.902 no N24 . H29 . 0.883 no N24 . H30 . 0.893 no N24 . H31 . 0.903 no N25 . H41 . 0.898 no N25 . H42 . 0.894 no N25 . H43 . 0.906 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 O2 . Cu1 . O8 . 92.26(10) yes O2 . Cu1 . O9 . 91.80(10) yes O2 . Cu1 . O16 . 167.70(12) yes O2 . Cu1 . Cl1 . 94.08(9) yes O8 . Cu1 . O9 . 174.72(10) yes O8 . Cu1 . O16 . 83.09(10) yes O8 . Cu1 . Cl1 . 98.34(9) yes O9 . Cu1 . O16 . 92.25(10) yes O9 . Cu1 . Cl1 . 84.73(8) yes O16 . Cu1 . Cl1 . 97.84(8) yes Cu1 . O2 . C3 . 127.2(2) yes O2 . C3 . O4 . 122.7(3) yes O2 . C3 . C5 . 117.2(3) yes O4 . C3 . C5 . 120.1(3) yes C3 . C5 . O6 . 110.5(3) yes C3 . C5 . C7 . 112.6(3) yes C3 . C5 . H22 . 105.3 no O6 . C5 . C7 . 111.5(3) yes O6 . C5 . H22 . 111.2 no C7 . C5 . H22 . 105.5 no C5 . O6 . H18 . 110.4 no C5 . C7 . O8 . 116.9(3) yes C5 . C7 . O21 . 118.0(3) yes O8 . C7 . O21 . 125.0(3) yes C7 . O8 . Cu1 . 126.4(2) yes Cu1 . O9 . C10 . 124.3(2) yes O9 . C10 . O11 . 123.9(3) yes O9 . C10 . C12 . 116.9(3) yes O11 . C10 . C12 . 119.3(3) yes C10 . C12 . O13 . 113.8(3) yes C10 . C12 . C14 . 110.0(3) yes C10 . C12 . H12 . 105.8 no O13 . C12 . C14 . 108.7(3) yes O13 . C12 . H12 . 112.1 no C14 . C12 . H12 . 106.2 no C12 . O13 . H8 . 108.5 no C12 . C14 . O15 . 119.9(3) yes C12 . C14 . O16 . 117.2(3) yes O15 . C14 . O16 . 122.8(3) yes C14 . O16 . Cu1 . 125.9(2) yes N20 . Co19 . N21 . 88.62(12) yes N20 . Co19 . N22 . 178.80(13) yes N20 . Co19 . N23 . 89.88(14) yes N20 . Co19 . N24 . 89.32(12) yes N20 . Co19 . N25 . 92.49(12) yes N21 . Co19 . N22 . 90.20(13) yes N21 . Co19 . N23 . 177.98(12) yes N21 . Co19 . N24 . 89.22(12) yes N21 . Co19 . N25 . 90.75(12) yes N22 . Co19 . N23 . 91.31(14) yes N22 . Co19 . N24 . 90.85(12) yes N22 . Co19 . N25 . 87.34(12) yes N23 . Co19 . N24 . 89.41(13) yes N23 . Co19 . N25 . 90.66(13) yes N24 . Co19 . N25 . 178.19(12) yes Co19 . N20 . H25 . 112.5 no Co19 . N20 . H26 . 108.3 no Co19 . N20 . H27 . 111.9 no H25 . N20 . H26 . 107.9 no H25 . N20 . H27 . 108.1 no H26 . N20 . H27 . 108.0 no Co19 . N21 . H33 . 114.7 no Co19 . N21 . H34 . 110.7 no Co19 . N21 . H35 . 108.3 no H33 . N21 . H34 . 107.9 no H33 . N21 . H35 . 108.2 no H34 . N21 . H35 . 106.8 no Co19 . N22 . H37 . 113.0 no Co19 . N22 . H38 . 112.9 no Co19 . N22 . H39 . 107.2 no H37 . N22 . H38 . 108.0 no H37 . N22 . H39 . 107.9 no H38 . N22 . H39 . 107.6 no Co19 . N23 . H45 . 110.6 no Co19 . N23 . H46 . 111.5 no Co19 . N23 . H47 . 110.6 no H45 . N23 . H46 . 108.4 no H45 . N23 . H47 . 107.0 no H46 . N23 . H47 . 108.5 no Co19 . N24 . H29 . 108.1 no Co19 . N24 . H30 . 110.8 no Co19 . N24 . H31 . 114.2 no H29 . N24 . H30 . 108.8 no H29 . N24 . H31 . 107.7 no H30 . N24 . H31 . 107.1 no Co19 . N25 . H41 . 110.9 no Co19 . N25 . H42 . 112.2 no Co19 . N25 . H43 . 111.5 no H41 . N25 . H42 . 108.0 no H41 . N25 . H43 . 106.8 no H42 . N25 . H43 . 107.2 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag O13 . H8 . O16 3_655 149 0.91 2.18 3.002(5) yes O6 . H18 . O2 3_545 120 0.86 2.58 3.099(5) yes N20 . H26 . O4 2_566 163 0.90 2.04 2.904(5) yes N20 . H27 . O4 . 165 0.90 2.08 2.964(5) yes N24 . H29 . O8 4_555 143 0.88 2.49 3.242(5) yes N24 . H29 . O13 2_666 139 0.88 2.56 3.271(5) yes N24 . H30 . O9 4_565 170 0.89 2.16 3.046(5) yes N24 . H31 . O6 2_566 155 0.90 2.07 2.915(5) yes N21 . H33 . O4 2_566 157 0.89 2.29 3.121(5) yes N21 . H34 . O21 1_565 143 0.91 2.16 2.935(5) yes N22 . H37 . O13 3_655 175 0.90 2.21 3.103(5) yes N22 . H39 . O11 4_565 168 0.90 2.06 2.948(5) yes N25 . H41 . O21 1_565 164 0.90 2.26 3.135(5) yes N25 . H42 . O2 . 166 0.89 2.07 2.942(5) yes N25 . H43 . O15 3_655 155 0.91 2.12 2.961(5) yes N23 . H46 . O16 4_555 158 0.89 2.27 3.113(5) yes N23 . H47 . O18 . 151 0.90 2.44 3.257(5) yes _database_code_depnum_ccdc_archive 'CCDC 947966' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C9 H13 Cu3 O20 Rb3' _chemical_formula_sum 'C9 H13 Cu3 O20 Rb3' _chemical_formula_weight 888.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rb Rb -0.4688 1.6079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 9.7676(4) _cell_length_b 8.5338(3) _cell_length_c 25.7855(7) _cell_angle_alpha 90.00 _cell_angle_beta 94.527(3) _cell_angle_gamma 90.00 _cell_volume 2142.63(12) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 3641 _cell_measurement_theta_min 3.4359 _cell_measurement_theta_max 73.0965 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.1534 _exptl_crystal_size_mid 0.0858 _exptl_crystal_size_min 0.0518 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.753 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1700 _exptl_absorpt_coefficient_mu 12.640 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.311 _exptl_absorpt_correction_T_max 0.617 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4679 _diffrn_reflns_number 7668 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0351 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 73.25 _reflns_number_total 4174 _reflns_number_gt 3715 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_structure_solution 'SIR97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP 3 (Farrugia, 1997)' _computing_publication_material ShelX_Acta _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. Disorder and H atoms of water molecules: One water molecule O(16)H2 is disordered between two positions A and B (refined occupancies around 0.5/0.5) and refined with constrains on Uiso. H atoms of this disordered water molecule as well as those of O(3)H2 water molecule cannot be located from the difference Fourier map. Positions of these hydrogen atoms were calculated to form realistic hydrogen bonds and then were refined with a riding model (AFIX 3). ; _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^)+(0.0633P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4174 _refine_ls_number_parameters 318 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.1208 _refine_ls_wR_factor_gt 0.1163 _refine_ls_goodness_of_fit_ref 1.291 _refine_ls_restrained_S_all 1.301 _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 Rb1 Rb 0.25070(5) 0.70835(6) 0.737786(19) 0.02915(15) Uani 1 1 d . . . Rb2 Rb 0.65174(6) 0.20511(6) 0.60738(2) 0.03743(16) Uani 1 1 d . . . Rb3 Rb 0.30257(5) 0.16231(6) 0.505155(18) 0.02684(15) Uani 1 1 d . . . Cu1 Cu 0.30182(7) 0.40056(8) 0.62592(3) 0.02160(18) Uani 1 1 d . . . Cu2 Cu 0.12124(8) 0.73178(10) 0.60502(3) 0.02644(19) Uani 1 1 d . A . Cu3 Cu -0.00463(7) 0.41887(8) 0.66984(3) 0.02293(18) Uani 1 1 d . . . O1 O 0.4358(4) 0.4181(4) 0.57533(14) 0.0271(7) Uani 1 1 d . . . O1W O 0.4185(4) 0.4659(5) 0.79806(16) 0.0377(9) Uani 1 1 d D . . H1WA H 0.4919 0.4582 0.8070 0.057 Uiso 1 1 d RD . . H1WB H 0.3693 0.3792 0.8088 0.057 Uiso 1 1 d RD . . O2 O 0.5909(4) 0.5889(5) 0.55181(15) 0.0325(8) Uani 1 1 d . . . O2W O 0.5070(4) 0.3859(5) 0.69779(16) 0.0365(9) Uani 1 1 d . . . H2WA H 0.4659 0.3967 0.7213 0.055 Uiso 1 1 d R . . H2WB H 0.5493 0.4623 0.6942 0.055 Uiso 1 1 d R . . O3 O 0.2939(3) 0.6286(4) 0.62214(12) 0.0208(6) Uani 1 1 d . . . O3W O 0.1770(6) 0.5074(9) 0.4800(2) 0.0739(19) Uani 1 1 d . A . H3WA H 0.1236 0.4790 0.4527 0.111 Uiso 1 1 d R . . H3WB H 0.2550 0.5183 0.4680 0.111 Uiso 1 1 d R . . O4 O 0.2076(4) 0.8237(5) 0.54828(14) 0.0306(8) Uani 1 1 d . . . O5 O 0.4071(4) 0.8444(5) 0.51346(16) 0.0339(9) Uani 1 1 d . . . O6 O -0.0433(4) 0.8462(6) 0.58586(16) 0.0409(10) Uani 1 1 d . . . O7 O -0.2492(4) 0.9004(4) 0.61079(15) 0.0308(8) Uani 1 1 d . . . O8 O 0.0204(4) 0.6430(4) 0.65903(13) 0.0226(7) Uani 1 1 d . . . O9 O -0.1980(4) 0.4623(4) 0.65764(14) 0.0280(7) Uani 1 1 d . . . O10 O -0.3392(4) 0.6519(4) 0.67798(14) 0.0268(7) Uani 1 1 d . . . O11 O -0.0461(4) 0.2046(4) 0.68640(16) 0.0293(8) Uani 1 1 d . . . O12 O 0.0520(4) 0.0034(4) 0.73006(15) 0.0317(8) Uani 1 1 d . . . O13 O 0.1851(3) 0.3611(4) 0.68170(12) 0.0217(7) Uani 1 1 d . . . O14 O 0.3186(4) 0.1739(4) 0.62107(14) 0.0271(8) Uani 1 1 d . . . O15 O 0.2975(5) -0.0375(5) 0.66947(16) 0.0364(9) Uani 1 1 d . . . O16A O 0.9341(10) 0.1585(12) 0.5501(4) 0.0442(15) Uiso 0.509(10) 1 d P A 1 H16A H 0.8875 0.1605 0.5217 0.066 Uiso 0.509(10) 1 d PR A 1 H16B H 0.9397 0.0632 0.5625 0.066 Uiso 0.509(10) 1 d PR A 1 O16B O 0.9948(11) 0.1296(13) 0.5358(4) 0.0442(15) Uiso 0.491(10) 1 d P . 2 H16C H 0.9766 0.0296 0.5539 0.066 Uiso 0.491(10) 1 d PR A 2 H16D H 0.9262 0.1333 0.5053 0.066 Uiso 0.491(10) 1 d PR A 2 C19 C -0.2264(5) 0.6050(6) 0.66610(17) 0.0218(9) Uani 1 1 d . A . C22 C -0.1068(5) 0.7215(5) 0.66297(18) 0.0213(9) Uani 1 1 d . A . H22 H -0.0994 0.7853 0.6956 0.026 Uiso 1 1 calc R . . C27 C 0.0587(5) 0.1257(6) 0.70595(19) 0.0241(10) Uani 1 1 d . . . C28 C -0.1406(5) 0.8325(6) 0.6169(2) 0.0252(10) Uani 1 1 d . . . C29 C 0.1981(5) 0.2026(5) 0.69817(19) 0.0213(9) Uani 1 1 d . A . H29 H 0.2535 0.2014 0.7325 0.026 Uiso 1 1 calc R . . C30 C 0.3963(5) 0.6883(5) 0.59167(19) 0.0210(9) Uani 1 1 d . . . H30 H 0.4589 0.7556 0.6148 0.025 Uiso 1 1 calc R . . C33 C 0.4827(5) 0.5569(6) 0.57078(18) 0.0224(9) Uani 1 1 d . . . C34 C 0.2751(5) 0.1025(6) 0.65990(19) 0.0240(10) Uani 1 1 d . . . C35 C 0.3350(5) 0.7920(6) 0.5466(2) 0.0244(10) Uani 1 1 d . . . O4W O 0.0835(5) 0.4086(6) 0.56797(19) 0.0498(12) Uani 1 1 d . . . H4WA H 0.1000 0.4475 0.5343 0.060 Uiso 1 1 d R . . H4WB H 0.0120 0.3543 0.5720 0.060 Uiso 1 1 d 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 Rb1 0.0354(3) 0.0282(3) 0.0237(2) 0.00425(19) 0.00157(18) -0.0011(2) Rb2 0.0483(3) 0.0218(3) 0.0408(3) -0.0054(2) -0.0056(2) 0.0079(2) Rb3 0.0356(3) 0.0214(3) 0.0241(2) 0.00215(17) 0.00568(18) 0.00016(19) Cu1 0.0322(4) 0.0122(3) 0.0215(3) 0.0014(3) 0.0093(3) 0.0016(3) Cu2 0.0282(4) 0.0294(4) 0.0225(4) 0.0093(3) 0.0072(3) 0.0067(3) Cu3 0.0255(4) 0.0145(3) 0.0288(4) 0.0001(3) 0.0023(3) 0.0014(3) O1 0.0392(19) 0.0180(17) 0.0255(16) 0.0014(14) 0.0117(14) 0.0035(15) O1W 0.036(2) 0.037(2) 0.041(2) 0.0113(19) 0.0048(16) -0.0055(18) O2 0.0355(19) 0.029(2) 0.035(2) 0.0061(16) 0.0135(15) 0.0017(16) O2W 0.043(2) 0.031(2) 0.036(2) -0.0024(17) 0.0072(16) -0.0060(18) O3 0.0292(16) 0.0123(15) 0.0216(15) 0.0028(12) 0.0059(12) 0.0024(13) O3W 0.054(3) 0.103(5) 0.068(4) 0.010(4) 0.019(3) 0.031(3) O4 0.0300(18) 0.038(2) 0.0238(17) 0.0109(16) 0.0040(13) 0.0069(16) O5 0.0356(19) 0.028(2) 0.040(2) 0.0171(17) 0.0123(16) 0.0039(17) O6 0.040(2) 0.048(3) 0.036(2) 0.0246(19) 0.0125(17) 0.018(2) O7 0.0348(19) 0.0217(18) 0.0360(19) 0.0051(15) 0.0029(15) 0.0077(16) O8 0.0289(16) 0.0148(16) 0.0243(16) 0.0041(13) 0.0025(12) 0.0060(14) O9 0.0254(16) 0.0217(18) 0.0360(19) -0.0039(15) -0.0031(13) 0.0030(14) O10 0.0274(17) 0.0254(18) 0.0282(17) 0.0008(15) 0.0051(13) 0.0035(15) O11 0.0294(18) 0.0159(17) 0.043(2) -0.0031(15) 0.0058(15) 0.0000(14) O12 0.044(2) 0.0185(17) 0.0337(18) 0.0037(16) 0.0113(16) -0.0048(16) O13 0.0292(16) 0.0128(15) 0.0237(16) 0.0013(13) 0.0051(12) 0.0023(13) O14 0.044(2) 0.0147(16) 0.0243(17) 0.0037(13) 0.0133(14) 0.0021(15) O15 0.052(2) 0.0177(18) 0.042(2) 0.0080(16) 0.0166(18) 0.0083(18) C19 0.028(2) 0.020(2) 0.017(2) 0.0035(17) 0.0003(16) -0.0056(19) C22 0.026(2) 0.015(2) 0.023(2) -0.0013(17) 0.0047(17) -0.0009(18) C27 0.035(3) 0.015(2) 0.024(2) -0.0035(19) 0.0084(18) -0.005(2) C28 0.027(2) 0.018(2) 0.031(2) 0.001(2) 0.0021(18) 0.0032(19) C29 0.030(2) 0.013(2) 0.022(2) 0.0035(17) 0.0049(17) 0.0011(18) C30 0.027(2) 0.012(2) 0.025(2) 0.0036(18) 0.0050(17) -0.0013(17) C33 0.028(2) 0.019(2) 0.020(2) 0.0011(18) 0.0028(17) 0.0019(19) C34 0.033(2) 0.015(2) 0.024(2) -0.0017(18) 0.0029(18) -0.0013(19) C35 0.034(2) 0.015(2) 0.025(2) 0.0019(18) 0.0062(19) 0.0003(19) O4W 0.058(3) 0.049(3) 0.041(2) -0.007(2) -0.008(2) 0.004(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 Rb1 O15 2.854(4) 1_565 ? Rb1 O11 2.904(4) 2_556 ? Rb1 O8 2.962(4) . ? Rb1 O1W 2.997(4) . ? Rb1 O3 3.120(3) . ? Rb1 O2W 3.168(4) 2_656 ? Rb1 O12 3.175(4) 1_565 ? Rb1 O13 3.337(3) . ? Rb1 C27 3.525(5) 2_556 ? Rb1 O9 3.529(4) 2_556 ? Rb1 Cu2 3.5602(9) . ? Rb1 O12 3.588(4) 2_556 ? Rb2 O7 2.773(4) 1_645 ? Rb2 O1 2.857(4) . ? Rb2 O9 2.890(4) 1_655 ? Rb2 O5 3.152(4) 3_666 ? Rb2 O2W 3.215(4) . ? Rb2 O16A 3.254(11) . ? Rb2 O1W 3.293(4) 2_646 ? Rb2 O14 3.311(4) . ? Rb2 O11 3.452(4) 1_655 ? Rb2 C33 3.519(5) . ? Rb2 O2 3.605(4) . ? Rb2 Cu1 3.8666(9) . ? Rb3 O2 2.826(4) 3_666 ? Rb3 O5 2.901(4) 1_545 ? Rb3 O5 2.914(4) 3_666 ? Rb3 O14 2.982(4) . ? Rb3 O7 3.042(4) 3_566 ? Rb3 O1 3.060(4) . ? Rb3 O16B 3.180(11) 1_455 ? Rb3 O3W 3.236(7) . ? Rb3 O4 3.257(4) 1_545 ? Rb3 O6 3.315(5) 3_566 ? Rb3 C35 3.344(5) 1_545 ? Rb3 C28 3.409(5) 3_566 ? Rb3 H3WB 3.2086 . ? Rb3 H4WA 3.2622 . ? Cu1 O1 1.925(3) . ? Cu1 O13 1.934(3) . ? Cu1 O14 1.946(4) . ? Cu1 O3 1.950(3) . ? Cu2 O6 1.912(4) . ? Cu2 O4 1.914(4) . ? Cu2 O3 1.923(3) . ? Cu2 O8 1.923(3) . ? Cu3 O13 1.919(3) . ? Cu3 O9 1.926(4) . ? Cu3 O11 1.928(4) . ? Cu3 O8 1.951(4) . ? Cu3 Rb1 3.9472(9) 2_546 ? Cu3 Rb2 4.0415(10) 1_455 ? O1 C33 1.279(6) . ? O1W Rb2 3.294(4) 2_656 ? O1W H1WA 0.7389 . ? O1W H1WB 0.9357 . ? O2 C33 1.230(6) . ? O2 Rb3 2.826(4) 3_666 ? O2W Rb1 3.168(4) 2_646 ? O2W H2WA 0.7580 . ? O2W H2WB 0.7813 . ? O3 C30 1.414(5) . ? O3W H3WA 0.8763 . ? O3W H3WB 0.8494 . ? O4 C35 1.277(7) . ? O4 Rb3 3.257(4) 1_565 ? O5 C35 1.234(6) . ? O5 Rb3 2.901(4) 1_565 ? O5 Rb3 2.914(4) 3_666 ? O5 Rb2 3.152(4) 3_666 ? O6 C28 1.295(7) . ? O6 Rb3 3.315(5) 3_566 ? O7 C28 1.208(7) . ? O7 Rb2 2.773(4) 1_465 ? O7 Rb3 3.041(4) 3_566 ? O8 C22 1.422(6) . ? O9 C19 1.271(6) . ? O9 Rb2 2.890(4) 1_455 ? O9 Rb1 3.529(4) 2_546 ? O10 C19 1.234(6) . ? O11 C27 1.293(7) . ? O11 Rb1 2.904(4) 2_546 ? O11 Rb2 3.452(4) 1_455 ? O12 C27 1.219(6) . ? O12 Rb1 3.175(4) 1_545 ? O12 Rb1 3.588(4) 2_546 ? O13 C29 1.420(6) . ? O14 C34 1.273(6) . ? O15 C34 1.236(7) . ? O15 Rb1 2.854(4) 1_545 ? O16A H16A 0.8319 . ? O16A H16B 0.8741 . ? O16A H16C 1.1765 . ? O16A H16D 1.1722 . ? O16B Rb3 3.180(10) 1_655 ? O16B H16A 1.1140 . ? O16B H16B 1.0694 . ? O16B H16C 0.9951 . ? O16B H16D 0.9934 . ? C19 C22 1.541(6) . ? C22 C28 1.535(7) . ? C22 H22 1.0000 . ? C27 C29 1.540(7) . ? C27 Rb1 3.525(5) 2_546 ? C28 Rb3 3.409(5) 3_566 ? C29 C34 1.545(7) . ? C29 H29 1.0000 . ? C30 C33 1.527(7) . ? C30 C35 1.543(7) . ? C30 H30 1.0000 . ? C35 Rb3 3.344(5) 1_565 ? O4W H4WA 0.9545 . ? O4W H4WB 0.8512 . ? 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 O15 Rb1 O11 125.19(11) 1_565 2_556 ? O15 Rb1 O8 82.52(12) 1_565 . ? O11 Rb1 O8 86.20(10) 2_556 . ? O15 Rb1 O1W 137.49(12) 1_565 . ? O11 Rb1 O1W 91.17(11) 2_556 . ? O8 Rb1 O1W 125.47(11) . . ? O15 Rb1 O3 62.31(10) 1_565 . ? O11 Rb1 O3 142.50(10) 2_556 . ? O8 Rb1 O3 57.07(9) . . ? O1W Rb1 O3 103.62(10) . . ? O15 Rb1 O2W 79.09(12) 1_565 2_656 ? O11 Rb1 O2W 100.23(11) 2_556 2_656 ? O8 Rb1 O2W 160.92(10) . 2_656 ? O1W Rb1 O2W 72.71(11) . 2_656 ? O3 Rb1 O2W 116.98(10) . 2_656 ? O15 Rb1 O12 59.04(10) 1_565 1_565 ? O11 Rb1 O12 66.51(10) 2_556 1_565 ? O8 Rb1 O12 71.28(10) . 1_565 ? O1W Rb1 O12 152.43(11) . 1_565 ? O3 Rb1 O12 103.95(9) . 1_565 ? O2W Rb1 O12 94.67(11) 2_656 1_565 ? O15 Rb1 O13 116.23(10) 1_565 . ? O11 Rb1 O13 99.39(9) 2_556 . ? O8 Rb1 O13 54.99(9) . . ? O1W Rb1 O13 71.95(10) . . ? O3 Rb1 O13 55.11(8) . . ? O2W Rb1 O13 139.62(10) 2_656 . ? O12 Rb1 O13 125.55(10) 1_565 . ? O15 Rb1 C27 126.19(12) 1_565 2_556 ? O11 Rb1 C27 20.43(12) 2_556 2_556 ? O8 Rb1 C27 67.37(11) . 2_556 ? O1W Rb1 C27 95.73(11) . 2_556 ? O3 Rb1 C27 122.34(11) . 2_556 ? O2W Rb1 C27 120.61(11) 2_656 2_556 ? O12 Rb1 C27 69.21(11) 1_565 2_556 ? O13 Rb1 C27 81.90(10) . 2_556 ? O15 Rb1 O9 92.57(10) 1_565 2_556 ? O11 Rb1 O9 48.92(10) 2_556 2_556 ? O8 Rb1 O9 119.40(9) . 2_556 ? O1W Rb1 O9 97.73(10) . 2_556 ? O3 Rb1 O9 154.59(9) . 2_556 ? O2W Rb1 O9 56.87(9) 2_656 2_556 ? O12 Rb1 O9 55.65(9) 1_565 2_556 ? O13 Rb1 O9 147.35(8) . 2_556 ? C27 Rb1 O9 68.10(10) 2_556 2_556 ? O15 Rb1 Cu2 54.96(9) 1_565 . ? O11 Rb1 Cu2 115.91(8) 2_556 . ? O8 Rb1 Cu2 32.69(7) . . ? O1W Rb1 Cu2 132.51(9) . . ? O3 Rb1 Cu2 32.62(6) . . ? O2W Rb1 Cu2 132.17(8) 2_656 . ? O12 Rb1 Cu2 74.11(7) 1_565 . ? O13 Rb1 Cu2 65.90(6) . . ? C27 Rb1 Cu2 98.98(8) 2_556 . ? O9 Rb1 Cu2 129.65(6) 2_556 . ? O15 Rb1 O12 133.49(12) 1_565 2_556 ? O11 Rb1 O12 38.34(10) 2_556 2_556 ? O8 Rb1 O12 58.11(9) . 2_556 ? O1W Rb1 O12 88.31(10) . 2_556 ? O3 Rb1 O12 106.90(9) . 2_556 ? O2W Rb1 O12 135.00(10) 2_656 2_556 ? O12 Rb1 O12 83.71(4) 1_565 2_556 ? O13 Rb1 O12 62.21(8) . 2_556 ? C27 Rb1 O12 19.71(10) 2_556 2_556 ? O9 Rb1 O12 87.16(8) 2_556 2_556 ? Cu2 Rb1 O12 90.74(7) . 2_556 ? O7 Rb2 O1 148.59(12) 1_645 . ? O7 Rb2 O9 122.31(11) 1_645 1_655 ? O1 Rb2 O9 89.06(11) . 1_655 ? O7 Rb2 O5 86.65(11) 1_645 3_666 ? O1 Rb2 O5 74.13(10) . 3_666 ? O9 Rb2 O5 126.27(11) 1_655 3_666 ? O7 Rb2 O2W 126.81(11) 1_645 . ? O1 Rb2 O2W 63.10(10) . . ? O9 Rb2 O2W 63.07(10) 1_655 . ? O5 Rb2 O2W 136.46(11) 3_666 . ? O7 Rb2 O16A 66.0(2) 1_645 . ? O1 Rb2 O16A 125.41(19) . . ? O9 Rb2 O16A 82.99(19) 1_655 . ? O5 Rb2 O16A 68.28(18) 3_666 . ? O2W Rb2 O16A 145.57(19) . . ? O7 Rb2 O1W 59.20(11) 1_645 2_646 ? O1 Rb2 O1W 114.61(10) . 2_646 ? O9 Rb2 O1W 105.48(11) 1_655 2_646 ? O5 Rb2 O1W 128.05(10) 3_666 2_646 ? O2W Rb2 O1W 68.37(10) . 2_646 ? O16A Rb2 O1W 119.58(19) . 2_646 ? O7 Rb2 O14 105.33(10) 1_645 . ? O1 Rb2 O14 51.15(10) . . ? O9 Rb2 O14 118.80(10) 1_655 . ? O5 Rb2 O14 89.46(10) 3_666 . ? O2W Rb2 O14 57.93(10) . . ? O16A Rb2 O14 156.03(18) . . ? O1W Rb2 O14 66.88(10) 2_646 . ? O7 Rb2 O11 72.55(10) 1_645 1_655 ? O1 Rb2 O11 138.51(10) . 1_655 ? O9 Rb2 O11 49.91(9) 1_655 1_655 ? O5 Rb2 O11 131.61(10) 3_666 1_655 ? O2W Rb2 O11 88.69(10) . 1_655 ? O16A Rb2 O11 63.38(18) . 1_655 ? O1W Rb2 O11 77.32(10) 2_646 1_655 ? O14 Rb2 O11 137.61(9) . 1_655 ? O7 Rb2 C33 164.47(12) 1_645 . ? O1 Rb2 C33 19.86(11) . . ? O9 Rb2 C33 71.52(11) 1_655 . ? O5 Rb2 C33 78.71(11) 3_666 . ? O2W Rb2 C33 63.97(11) . . ? O16A Rb2 C33 112.29(19) . . ? O1W Rb2 C33 127.34(10) 2_646 . ? O14 Rb2 C33 69.70(10) . . ? O11 Rb2 C33 121.38(10) 1_655 . ? O7 Rb2 O2 155.57(10) 1_645 . ? O1 Rb2 O2 38.02(10) . . ? O9 Rb2 O2 63.26(10) 1_655 . ? O5 Rb2 O2 73.59(10) 3_666 . ? O2W Rb2 O2 77.53(10) . . ? O16A Rb2 O2 92.85(19) . . ? O1W Rb2 O2 145.07(9) 2_646 . ? O14 Rb2 O2 89.02(9) . . ? O11 Rb2 O2 110.01(9) 1_655 . ? C33 Rb2 O2 19.84(10) . . ? O7 Rb2 Cu1 135.24(9) 1_645 . ? O1 Rb2 Cu1 28.55(7) . . ? O9 Rb2 Cu1 92.26(7) 1_655 . ? O5 Rb2 Cu1 94.94(7) 3_666 . ? O2W Rb2 Cu1 42.24(8) . . ? O16A Rb2 Cu1 153.90(17) . . ? O1W Rb2 Cu1 86.45(7) 2_646 . ? O14 Rb2 Cu1 30.21(6) . . ? O11 Rb2 Cu1 130.59(7) 1_655 . ? C33 Rb2 Cu1 42.65(8) . . ? O2 Rb2 Cu1 62.47(6) . . ? O2 Rb3 O5 126.80(11) 3_666 1_545 ? O2 Rb3 O5 61.72(11) 3_666 3_666 ? O5 Rb3 O5 69.66(13) 1_545 3_666 ? O2 Rb3 O14 120.23(11) 3_666 . ? O5 Rb3 O14 88.09(11) 1_545 . ? O5 Rb3 O14 101.00(11) 3_666 . ? O2 Rb3 O7 70.30(11) 3_666 3_566 ? O5 Rb3 O7 86.55(11) 1_545 3_566 ? O5 Rb3 O7 85.88(11) 3_666 3_566 ? O14 Rb3 O7 169.23(11) . 3_566 ? O2 Rb3 O1 67.33(10) 3_666 . ? O5 Rb3 O1 119.53(11) 1_545 . ? O5 Rb3 O1 74.77(11) 3_666 . ? O14 Rb3 O1 52.94(10) . . ? O7 Rb3 O1 137.63(10) 3_566 . ? O2 Rb3 O16B 126.1(2) 3_666 1_455 ? O5 Rb3 O16B 103.5(2) 1_545 1_455 ? O5 Rb3 O16B 172.1(2) 3_666 1_455 ? O14 Rb3 O16B 74.32(19) . 1_455 ? O7 Rb3 O16B 97.88(19) 3_566 1_455 ? O1 Rb3 O16B 106.4(2) . 1_455 ? O2 Rb3 O3W 50.32(13) 3_666 . ? O5 Rb3 O3W 172.55(15) 1_545 . ? O5 Rb3 O3W 110.07(14) 3_666 . ? O14 Rb3 O3W 99.20(13) . . ? O7 Rb3 O3W 86.01(13) 3_566 . ? O1 Rb3 O3W 66.80(15) . . ? O16B Rb3 O3W 77.2(2) 1_455 . ? O2 Rb3 O4 165.98(11) 3_666 1_545 ? O5 Rb3 O4 41.68(10) 1_545 1_545 ? O5 Rb3 O4 110.23(10) 3_666 1_545 ? O14 Rb3 O4 71.41(10) . 1_545 ? O7 Rb3 O4 98.52(10) 3_566 1_545 ? O1 Rb3 O4 123.39(10) . 1_545 ? O16B Rb3 O4 62.4(2) 1_455 1_545 ? O3W Rb3 O4 139.66(13) . 1_545 ? O2 Rb3 O6 86.59(11) 3_666 3_566 ? O5 Rb3 O6 106.06(12) 1_545 3_566 ? O5 Rb3 O6 125.60(11) 3_666 3_566 ? O14 Rb3 O6 133.40(10) . 3_566 ? O7 Rb3 O6 40.38(10) 3_566 3_566 ? O1 Rb3 O6 134.41(11) . 3_566 ? O16B Rb3 O6 59.33(18) 1_455 3_566 ? O3W Rb3 O6 67.78(15) . 3_566 ? O4 Rb3 O6 90.00(11) 1_545 3_566 ? O2 Rb3 C35 147.87(12) 3_666 1_545 ? O5 Rb3 C35 21.32(12) 1_545 1_545 ? O5 Rb3 C35 88.01(12) 3_666 1_545 ? O14 Rb3 C35 73.42(11) . 1_545 ? O7 Rb3 C35 98.78(11) 3_566 1_545 ? O1 Rb3 C35 117.40(11) . 1_545 ? O16B Rb3 C35 84.5(2) 1_455 1_545 ? O3W Rb3 C35 161.65(14) . 1_545 ? O4 Rb3 C35 22.26(12) 1_545 1_545 ? O6 Rb3 C35 104.69(13) 3_566 1_545 ? O2 Rb3 C28 70.94(12) 3_666 3_566 ? O5 Rb3 C28 102.43(12) 1_545 3_566 ? O5 Rb3 C28 103.58(12) 3_666 3_566 ? O14 Rb3 C28 155.32(12) . 3_566 ? O7 Rb3 C28 20.59(11) 3_566 3_566 ? O1 Rb3 C28 132.95(11) . 3_566 ? O16B Rb3 C28 81.49(19) 1_455 3_566 ? O3W Rb3 C28 70.26(15) . 3_566 ? O4 Rb3 C28 101.70(11) 1_545 3_566 ? O6 Rb3 C28 22.16(11) 3_566 3_566 ? C35 Rb3 C28 109.44(12) 1_545 3_566 ? O2 Rb3 H3WB 35.3 3_666 . ? O5 Rb3 H3WB 161.7 1_545 . ? O5 Rb3 H3WB 95.1 3_666 . ? O14 Rb3 H3WB 105.2 . . ? O7 Rb3 H3WB 82.1 3_566 . ? O1 Rb3 H3WB 63.0 . . ? O16B Rb3 H3WB 92.3 1_455 . ? O3W Rb3 H3WB 15.1 . . ? O4 Rb3 H3WB 154.6 1_545 . ? O6 Rb3 H3WB 74.0 3_566 . ? C35 Rb3 H3WB 176.8 1_545 . ? C28 Rb3 H3WB 70.5 3_566 . ? O2 Rb3 H4WA 79.3 3_666 . ? O5 Rb3 H4WA 153.8 1_545 . ? O5 Rb3 H4WA 132.0 3_666 . ? O14 Rb3 H4WA 74.3 . . ? O7 Rb3 H4WA 107.3 3_566 . ? O1 Rb3 H4WA 64.5 . . ? O16B Rb3 H4WA 53.5 1_455 . ? O3W Rb3 H4WA 30.7 . . ? O4 Rb3 H4WA 112.9 1_545 . ? O6 Rb3 H4WA 74.7 3_566 . ? C35 Rb3 H4WA 132.5 1_545 . ? C28 Rb3 H4WA 87.6 3_566 . ? H3WB Rb3 H4WA 44.5 . . ? O1 Cu1 O13 171.71(15) . . ? O1 Cu1 O14 88.19(15) . . ? O13 Cu1 O14 86.13(15) . . ? O1 Cu1 O3 85.11(15) . . ? O13 Cu1 O3 100.82(14) . . ? O14 Cu1 O3 172.77(14) . . ? O1 Cu1 Rb3 55.17(12) . . ? O13 Cu1 Rb3 124.59(11) . . ? O14 Cu1 Rb3 52.93(11) . . ? O3 Cu1 Rb3 120.43(10) . . ? O1 Cu1 Rb2 45.17(11) . . ? O13 Cu1 Rb2 126.55(10) . . ? O14 Cu1 Rb2 58.90(12) . . ? O3 Cu1 Rb2 117.14(10) . . ? Rb3 Cu1 Rb2 66.454(16) . . ? O1 Cu1 Rb1 124.98(12) . . ? O13 Cu1 Rb1 57.21(10) . . ? O14 Cu1 Rb1 136.21(11) . . ? O3 Cu1 Rb1 50.79(9) . . ? Rb3 Cu1 Rb1 168.71(2) . . ? Rb2 Cu1 Rb1 122.65(2) . . ? O6 Cu2 O4 90.31(17) . . ? O6 Cu2 O3 175.89(18) . . ? O4 Cu2 O3 86.07(15) . . ? O6 Cu2 O8 85.43(16) . . ? O4 Cu2 O8 175.37(15) . . ? O3 Cu2 O8 98.25(14) . . ? O6 Cu2 Rb1 120.31(14) . . ? O4 Cu2 Rb1 127.86(12) . . ? O3 Cu2 Rb1 60.99(10) . . ? O8 Cu2 Rb1 56.28(11) . . ? O13 Cu3 O9 176.22(16) . . ? O13 Cu3 O11 86.46(15) . . ? O9 Cu3 O11 89.91(16) . . ? O13 Cu3 O8 98.29(15) . . ? O9 Cu3 O8 85.43(16) . . ? O11 Cu3 O8 172.89(16) . . ? O13 Cu3 Rb1 60.49(10) . . ? O9 Cu3 Rb1 123.00(11) . . ? O11 Cu3 Rb1 130.57(12) . . ? O8 Cu3 Rb1 49.41(10) . . ? O13 Cu3 Rb1 114.42(10) . 2_546 ? O9 Cu3 Rb1 63.28(12) . 2_546 ? O11 Cu3 Rb1 44.45(11) . 2_546 ? O8 Cu3 Rb1 128.44(10) . 2_546 ? Rb1 Cu3 Rb1 114.999(19) . 2_546 ? O13 Cu3 Rb2 135.14(11) . 1_455 ? O9 Cu3 Rb2 41.33(11) . 1_455 ? O11 Cu3 Rb2 58.52(12) . 1_455 ? O8 Cu3 Rb2 119.68(11) . 1_455 ? Rb1 Cu3 Rb2 164.29(2) . 1_455 ? Rb1 Cu3 Rb2 60.594(15) 2_546 1_455 ? C33 O1 Cu1 113.7(3) . . ? C33 O1 Rb2 110.8(3) . . ? Cu1 O1 Rb2 106.28(15) . . ? C33 O1 Rb3 138.2(3) . . ? Cu1 O1 Rb3 93.73(14) . . ? Rb2 O1 Rb3 89.26(10) . . ? Rb1 O1W Rb2 79.55(10) . 2_656 ? Rb1 O1W H1WA 134.5 . . ? Rb2 O1W H1WA 94.4 2_656 . ? Rb1 O1W H1WB 115.2 . . ? Rb2 O1W H1WB 97.5 2_656 . ? H1WA O1W H1WB 110.2 . . ? C33 O2 Rb3 137.4(3) . 3_666 ? C33 O2 Rb2 76.1(3) . . ? Rb3 O2 Rb2 146.41(13) 3_666 . ? Rb1 O2W Rb2 78.32(10) 2_646 . ? Rb1 O2W H2WA 93.5 2_646 . ? Rb2 O2W H2WA 158.2 . . ? Rb1 O2W H2WB 94.7 2_646 . ? Rb2 O2W H2WB 92.7 . . ? H2WA O2W H2WB 108.2 . . ? C30 O3 Cu2 110.7(3) . . ? C30 O3 Cu1 111.1(3) . . ? Cu2 O3 Cu1 119.92(18) . . ? C30 O3 Rb1 127.4(3) . . ? Cu2 O3 Rb1 86.40(11) . . ? Cu1 O3 Rb1 100.24(12) . . ? Rb3 O3W H3WA 95.8 . . ? Rb3 O3W H3WB 80.6 . . ? H3WA O3W H3WB 103.4 . . ? C35 O4 Cu2 115.3(3) . . ? C35 O4 Rb3 82.7(3) . 1_565 ? Cu2 O4 Rb3 141.18(19) . 1_565 ? C35 O5 Rb3 100.0(3) . 1_565 ? C35 O5 Rb3 136.3(4) . 3_666 ? Rb3 O5 Rb3 110.34(13) 1_565 3_666 ? C35 O5 Rb2 124.5(4) . 3_666 ? Rb3 O5 Rb2 90.96(10) 1_565 3_666 ? Rb3 O5 Rb2 86.47(10) 3_666 3_666 ? C28 O6 Cu2 115.9(3) . . ? C28 O6 Rb3 83.0(3) . 3_566 ? Cu2 O6 Rb3 138.7(2) . 3_566 ? C28 O7 Rb2 139.0(4) . 1_465 ? C28 O7 Rb3 97.1(3) . 3_566 ? Rb2 O7 Rb3 95.83(11) 1_465 3_566 ? C22 O8 Cu2 111.5(3) . . ? C22 O8 Cu3 109.3(3) . . ? Cu2 O8 Cu3 124.52(18) . . ? C22 O8 Rb1 118.9(3) . . ? Cu2 O8 Rb1 91.02(13) . . ? Cu3 O8 Rb1 100.58(13) . . ? C19 O9 Cu3 112.4(3) . . ? C19 O9 Rb2 134.0(3) . 1_455 ? Cu3 O9 Rb2 112.56(15) . 1_455 ? C19 O9 Rb1 114.2(3) . 2_546 ? Cu3 O9 Rb1 87.54(13) . 2_546 ? Rb2 O9 Rb1 77.09(9) 1_455 2_546 ? C27 O11 Cu3 114.0(3) . . ? C27 O11 Rb1 108.0(3) . 2_546 ? Cu3 O11 Rb1 107.83(15) . 2_546 ? C27 O11 Rb2 147.6(3) . 1_455 ? Cu3 O11 Rb2 93.03(14) . 1_455 ? Rb1 O11 Rb2 78.21(9) 2_546 1_455 ? C27 O12 Rb1 130.8(3) . 1_545 ? C27 O12 Rb1 77.2(3) . 2_546 ? Rb1 O12 Rb1 151.96(12) 1_545 2_546 ? C29 O13 Cu3 110.8(3) . . ? C29 O13 Cu1 110.1(3) . . ? Cu3 O13 Cu1 117.08(17) . . ? C29 O13 Rb1 135.0(3) . . ? Cu3 O13 Rb1 89.48(12) . . ? Cu1 O13 Rb1 93.64(12) . . ? C34 O14 Cu1 113.0(3) . . ? C34 O14 Rb3 141.1(3) . . ? Cu1 O14 Rb3 95.70(13) . . ? C34 O14 Rb2 120.9(3) . . ? Cu1 O14 Rb2 90.89(13) . . ? Rb3 O14 Rb2 82.54(9) . . ? C34 O15 Rb1 145.4(4) . 1_545 ? Rb2 O16A H16A 88.4 . . ? Rb2 O16A H16B 88.7 . . ? H16A O16A H16B 110.9 . . ? Rb2 O16A H16C 112.5 . . ? Rb2 O16A H16D 118.5 . . ? Rb3 O16B H16A 141.4 1_655 . ? Rb3 O16B H16B 137.7 1_655 . ? Rb3 O16B H16C 113.5 1_655 . ? Rb3 O16B H16D 113.0 1_655 . ? H16C O16B H16D 105.3 . . ? O10 C19 O9 124.3(5) . . ? O10 C19 C22 120.0(4) . . ? O9 C19 C22 115.6(4) . . ? O8 C22 C28 111.8(4) . . ? O8 C22 C19 111.7(4) . . ? C28 C22 C19 108.7(4) . . ? O8 C22 H22 108.2 . . ? C28 C22 H22 108.2 . . ? C19 C22 H22 108.2 . . ? O12 C27 O11 124.9(5) . . ? O12 C27 C29 121.0(5) . . ? O11 C27 C29 114.1(4) . . ? O12 C27 Rb1 83.1(3) . 2_546 ? O11 C27 Rb1 51.6(2) . 2_546 ? C29 C27 Rb1 139.9(3) . 2_546 ? O7 C28 O6 123.8(5) . . ? O7 C28 C22 122.0(5) . . ? O6 C28 C22 114.2(4) . . ? O7 C28 Rb3 62.3(3) . 3_566 ? O6 C28 Rb3 74.8(3) . 3_566 ? C22 C28 Rb3 141.1(3) . 3_566 ? O13 C29 C27 112.7(4) . . ? O13 C29 C34 111.9(4) . . ? C27 C29 C34 109.2(4) . . ? O13 C29 H29 107.6 . . ? C27 C29 H29 107.6 . . ? C34 C29 H29 107.6 . . ? O3 C30 C33 111.5(4) . . ? O3 C30 C35 112.0(4) . . ? C33 C30 C35 110.4(4) . . ? O3 C30 H30 107.6 . . ? C33 C30 H30 107.6 . . ? C35 C30 H30 107.6 . . ? O2 C33 O1 124.6(5) . . ? O2 C33 C30 119.6(5) . . ? O1 C33 C30 115.9(4) . . ? O2 C33 Rb2 84.0(3) . . ? O1 C33 Rb2 49.4(2) . . ? C30 C33 Rb2 142.4(3) . . ? O15 C34 O14 123.7(5) . . ? O15 C34 C29 119.6(5) . . ? O14 C34 C29 116.6(4) . . ? O5 C35 O4 123.8(5) . . ? O5 C35 C30 121.4(5) . . ? O4 C35 C30 114.7(4) . . ? O5 C35 Rb3 58.7(3) . 1_565 ? O4 C35 Rb3 75.1(3) . 1_565 ? C30 C35 Rb3 143.5(3) . 1_565 ? Rb3 O4W H4WA 68.5 . . ? Rb3 O4W H4WB 105.5 . . ? H4WA O4W H4WB 119.9 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA O15 0.74 2.10 2.834(6) 173.7 2_656 O1W H1WB O10 0.94 2.00 2.870(6) 154.9 2_546 O1W H1WB O7 0.94 2.47 3.030(5) 118.6 2_546 O2W H2WA O1W 0.76 2.15 2.873(6) 159.1 . O2W H2WB O10 0.78 2.01 2.791(6) 174.6 1_655 O3W H3WA O4W 0.88 2.26 2.832(8) 122.4 3_566 O3W H3WB O2 0.85 1.87 2.604(7) 144.2 3_666 O16A H16A O4 0.83 1.97 2.797(10) 174.3 3_666 O16A H16B O6 0.87 1.95 2.823(11) 176.2 1_645 O16A H16B O7 0.87 2.69 3.309(11) 128.6 1_645 O16B H16C O6 1.00 1.79 2.780(11) 175.8 1_645 O16B H16D O4 0.99 1.86 2.845(10) 169.9 3_666 O4W H4WA O3W 0.95 1.72 2.649(8) 163.7 . O4W H4WB O16A 0.85 1.90 2.606(11) 139.0 1_455 O4W H4WB O16B 0.85 2.13 2.644(12) 118.3 1_455 _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 66.97 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.316 _refine_diff_density_min -1.105 _refine_diff_density_rms 0.153 _database_code_depnum_ccdc_archive 'CCDC 947967' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C9 H4 Cu3 O19 Rb3, H2 O' _chemical_formula_sum 'C9 H6 Cu3 O20 Rb3' _chemical_formula_weight 881.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rb Rb -0.4688 1.6079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5543(3) _cell_length_b 11.2377(4) _cell_length_c 12.8604(5) _cell_angle_alpha 74.196(4) _cell_angle_beta 88.056(3) _cell_angle_gamma 69.815(3) _cell_volume 1114.02(7) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 7686 _cell_measurement_theta_min 3.5768 _cell_measurement_theta_max 73.1781 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.5870 _exptl_crystal_size_mid 0.2741 _exptl_crystal_size_min 0.0328 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.627 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 836 _exptl_absorpt_coefficient_mu 12.155 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.072 _exptl_absorpt_correction_T_max 0.679 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4679 _diffrn_reflns_number 12132 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_unetI/netI 0.0336 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 73.34 _reflns_number_total 4363 _reflns_number_gt 4007 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_structure_solution 'SIR97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep 3 (Farrugia, 1997)' _computing_publication_material ShelX_Acta _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^)+(0.1015P)^2^+7.6352P] 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 4363 _refine_ls_number_parameters 320 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0605 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1666 _refine_ls_wR_factor_gt 0.1629 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 Rb1 Rb -0.46385(8) 0.52083(6) 0.18055(5) 0.02725(19) Uani 1 1 d . . . Rb2 Rb 0.36652(10) 0.20044(8) 0.39530(6) 0.0440(2) Uani 1 1 d . . . Rb3 Rb 1.11571(9) 0.04240(8) 0.20746(9) 0.0512(3) Uani 1 1 d . . . Cu1 Cu 0.33522(10) 0.28432(9) 0.08290(7) 0.0204(2) Uani 1 1 d . . . Cu2 Cu 0.50005(11) 0.12596(8) -0.10524(7) 0.0203(2) Uani 1 1 d . . . Cu3 Cu 0.09859(11) 0.30651(9) -0.14900(7) 0.0219(2) Uani 1 1 d . . . O1 O 0.5108(5) 0.2522(4) 0.1866(4) 0.0246(9) Uani 1 1 d . . . O2 O 0.7849(6) 0.1718(7) 0.2162(5) 0.0466(15) Uani 1 1 d . . . O3 O 0.5125(5) 0.2257(4) -0.0083(3) 0.0203(8) Uani 1 1 d . . . O3W O 0.1429(16) 0.0462(16) 0.4438(15) 0.145(5) Uani 1 1 d . . . O4 O 0.8770(6) -0.0511(5) 0.1139(4) 0.0347(11) Uani 1 1 d . . . O4W O 0.2874(13) 0.4815(10) 0.3749(8) 0.097(3) Uani 1 1 d . . . O5 O 0.6824(5) -0.0154(4) -0.0123(4) 0.0233(9) Uani 1 1 d . . . O5W O 1.2877(8) -0.2330(7) 0.2324(8) 0.072(2) Uani 1 1 d . . . O6 O 0.1643(6) 0.3102(5) 0.1867(4) 0.0271(10) Uani 1 1 d . . . O7 O -0.1017(6) 0.4278(5) 0.1964(4) 0.0300(10) Uani 1 1 d . . . O8 O 0.1451(5) 0.3396(4) -0.0169(3) 0.0204(8) Uani 1 1 d . . . O9 O -0.1267(6) 0.3600(5) -0.1065(4) 0.0260(9) Uani 1 1 d . . . O10 O -0.2960(5) 0.4744(4) -0.0062(4) 0.0241(9) Uani 1 1 d . . . O11 O 0.0259(6) 0.3136(5) -0.2920(4) 0.0312(10) Uani 1 1 d . . . O12 O 0.1230(8) 0.2864(9) -0.4498(5) 0.075(3) Uani 1 1 d . . . O13 O 0.3193(5) 0.2636(4) -0.2003(3) 0.0231(9) Uani 1 1 d . . . O14 O 0.5126(6) 0.0285(5) -0.2102(4) 0.0258(9) Uani 1 1 d . . . O15 O 0.4335(9) 0.0590(6) -0.3800(5) 0.0512(16) Uani 1 1 d . . . C1 C 0.6570(8) 0.1964(6) 0.1596(6) 0.0262(13) Uani 1 1 d . . . C2 C 0.6713(7) 0.1685(6) 0.0497(5) 0.0220(12) Uani 1 1 d . . . H2 H 0.7445 0.2147 0.0079 0.026 Uiso 1 1 calc R . . C3 C 0.7523(7) 0.0229(6) 0.0542(5) 0.0226(12) Uani 1 1 d . . . C4 C 0.0177(7) 0.3839(6) 0.1450(5) 0.0201(12) Uani 1 1 d . . . C5 C 0.0044(7) 0.4232(6) 0.0189(5) 0.0195(11) Uani 1 1 d . . . C6 C -0.1539(7) 0.4190(6) -0.0318(5) 0.0195(12) Uani 1 1 d . . . C7 C 0.1454(10) 0.2833(8) -0.3539(6) 0.0381(18) Uani 1 1 d . . . C8 C 0.3225(8) 0.2424(7) -0.3035(5) 0.0280(14) Uani 1 1 d . . . H8 H 0.3778 0.3005 -0.3511 0.034 Uiso 1 1 calc R . . C9 C 0.4281(9) 0.0982(7) -0.2995(6) 0.0305(14) Uani 1 1 d . . . O1W O -0.1553(9) 0.4065(9) 0.4115(5) 0.065(2) Uani 1 1 d G . . H1 H -0.1428 0.4479 0.3457 0.098 Uiso 1 1 d G . . H1W H -0.0592 0.3706 0.4483 0.098 Uiso 1 1 d G . . O2W O 0.7021(15) 0.2076(16) 0.4159(9) 0.128(5) Uani 1 1 d . . . H2WA H 0.7136 0.2305 0.4747 0.192 Uiso 1 1 d R . . H2WB H 0.7768 0.1291 0.4205 0.192 Uiso 1 1 d 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 Rb1 0.0212(3) 0.0225(3) 0.0364(4) -0.0074(3) 0.0038(2) -0.0064(3) Rb2 0.0386(5) 0.0476(5) 0.0322(4) -0.0072(3) 0.0043(3) -0.0016(4) Rb3 0.0171(4) 0.0405(5) 0.0947(7) -0.0242(4) 0.0055(4) -0.0043(3) Cu1 0.0086(4) 0.0199(5) 0.0273(5) -0.0046(3) -0.0004(3) 0.0005(3) Cu2 0.0127(5) 0.0147(4) 0.0282(5) -0.0042(3) -0.0006(3) 0.0006(3) Cu3 0.0110(4) 0.0252(5) 0.0268(5) -0.0085(4) 0.0008(3) -0.0021(4) O1 0.013(2) 0.025(2) 0.032(2) -0.0065(18) -0.0004(17) -0.0025(18) O2 0.012(2) 0.068(4) 0.058(3) -0.032(3) -0.008(2) 0.000(2) O3 0.0091(19) 0.0151(19) 0.032(2) -0.0048(16) -0.0018(16) 0.0009(15) O3W 0.081(8) 0.151(13) 0.215(16) -0.067(12) 0.034(9) -0.045(9) O4 0.019(2) 0.027(2) 0.048(3) -0.005(2) -0.015(2) 0.002(2) O4W 0.085(7) 0.075(6) 0.091(6) -0.017(5) -0.028(5) 0.022(5) O5 0.011(2) 0.019(2) 0.036(2) -0.0069(17) -0.0008(17) 0.0005(16) O5W 0.033(3) 0.046(4) 0.149(8) -0.041(4) 0.017(4) -0.019(3) O6 0.014(2) 0.032(2) 0.026(2) -0.0023(18) -0.0013(17) -0.0002(18) O7 0.012(2) 0.037(3) 0.030(2) -0.005(2) 0.0014(17) 0.0013(19) O8 0.0076(19) 0.020(2) 0.029(2) -0.0075(17) -0.0003(15) 0.0013(16) O9 0.017(2) 0.032(2) 0.034(2) -0.0154(19) 0.0042(18) -0.0104(19) O10 0.010(2) 0.023(2) 0.038(2) -0.0095(18) 0.0022(17) -0.0032(17) O11 0.019(2) 0.037(3) 0.031(2) -0.013(2) -0.0014(18) 0.002(2) O12 0.034(3) 0.127(7) 0.035(3) -0.036(4) -0.007(3) 0.020(4) O13 0.012(2) 0.022(2) 0.028(2) -0.0053(17) 0.0014(16) 0.0011(17) O14 0.016(2) 0.026(2) 0.032(2) -0.0102(18) 0.0008(17) -0.0023(18) O15 0.063(4) 0.040(3) 0.034(3) -0.016(2) -0.003(3) 0.006(3) C1 0.009(3) 0.022(3) 0.041(3) -0.005(3) -0.005(2) 0.001(2) C2 0.010(3) 0.019(3) 0.033(3) -0.005(2) 0.003(2) -0.003(2) C3 0.009(3) 0.021(3) 0.035(3) -0.008(2) 0.006(2) -0.003(2) C4 0.014(3) 0.014(3) 0.031(3) -0.006(2) 0.003(2) -0.004(2) C5 0.009(3) 0.015(3) 0.030(3) -0.003(2) 0.000(2) -0.001(2) C6 0.012(3) 0.014(3) 0.030(3) -0.003(2) 0.001(2) -0.003(2) C7 0.026(4) 0.047(4) 0.025(3) -0.012(3) -0.003(3) 0.010(3) C8 0.021(3) 0.027(3) 0.027(3) -0.006(3) 0.007(3) 0.001(3) C9 0.024(3) 0.031(4) 0.032(3) -0.008(3) 0.008(3) -0.005(3) O1W 0.045(4) 0.094(6) 0.043(3) -0.013(4) 0.001(3) -0.012(4) O2W 0.105(9) 0.209(15) 0.079(7) -0.072(8) 0.007(6) -0.043(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rb1 O10 2.834(5) . ? Rb1 O7 2.902(5) . ? Rb1 O3 3.000(4) 2_565 ? Rb1 O10 3.069(4) 2_465 ? Rb1 O5W 3.077(7) 1_365 ? Rb1 O1 3.081(4) 1_455 ? Rb1 O13 3.144(4) 2_565 ? Rb1 O4W 3.265(12) 1_455 ? Rb1 O9 3.356(4) 2_465 ? Rb1 H1 3.2591 . ? Rb2 O15 2.862(6) 1_556 ? Rb2 O15 2.883(6) 2_655 ? Rb2 O1 2.914(5) . ? Rb2 O2W 2.922(12) . ? Rb2 O4W 2.931(10) . ? Rb2 O12 2.935(6) 1_556 ? Rb2 O3W 2.945(14) . ? Rb2 O6 2.958(4) . ? Rb3 O2 2.713(5) . ? Rb3 O5W 2.863(7) . ? Rb3 O14 2.998(5) 2_755 ? Rb3 O4 3.010(5) . ? Rb3 O5 3.022(5) 2_755 ? Rb3 O3W 3.070(18) 1_655 ? Rb3 O6 3.117(5) 1_655 ? Cu1 O1 1.914(4) . ? Cu1 O8 1.921(4) . ? Cu1 O3 1.929(4) . ? Cu1 O6 1.947(5) . ? Cu2 O3 1.917(4) . ? Cu2 O13 1.930(4) . ? Cu2 O14 1.935(5) . ? Cu2 O5 1.941(4) . ? Cu3 O8 1.917(4) . ? Cu3 O9 1.919(5) . ? Cu3 O13 1.922(4) . ? Cu3 O11 1.933(5) . ? O1 C1 1.274(8) . ? O1 Rb1 3.081(4) 1_655 ? O2 C1 1.241(8) . ? O3 C2 1.421(7) . ? O3 Rb1 3.000(4) 2_565 ? O3W Rb3 3.070(18) 1_455 ? O4 C3 1.231(8) . ? O4W Rb1 3.265(12) 1_655 ? O5 C3 1.299(8) . ? O5 Rb3 3.022(5) 2_755 ? O5W Rb1 3.077(7) 1_745 ? O6 C4 1.278(8) . ? O6 Rb3 3.117(5) 1_455 ? O7 C4 1.227(8) . ? O8 C5 1.401(7) . ? O9 C6 1.281(8) . ? O9 Rb1 3.356(4) 2_465 ? O10 C6 1.239(8) . ? O10 Rb1 3.069(4) 2_465 ? O11 C7 1.283(9) . ? O12 C7 1.244(9) . ? O12 Rb2 2.935(6) 1_554 ? O13 C8 1.408(8) . ? O13 Rb1 3.144(4) 2_565 ? O14 C9 1.277(8) . ? O14 Rb3 2.998(5) 2_755 ? O15 C9 1.224(9) . ? O15 Rb2 2.862(6) 1_554 ? O15 Rb2 2.883(6) 2_655 ? C1 C2 1.522(9) . ? C2 C3 1.526(8) . ? C2 H2 1.0000 . ? C4 C5 1.558(8) . ? C5 C6 1.544(8) . ? C5 C5 1.636(11) 2_565 ? C7 C8 1.533(10) . ? C8 C9 1.547(9) . ? C8 H8 1.0000 . ? O1W H1 0.8701 . ? O1W H1W 0.8700 . ? O2W H2WA 0.8801 . ? O2W H2WB 0.8803 . ? 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 O10 Rb1 O7 62.16(13) . . ? O10 Rb1 O3 68.62(12) . 2_565 ? O7 Rb1 O3 96.40(12) . 2_565 ? O10 Rb1 O10 68.80(13) . 2_465 ? O7 Rb1 O10 129.67(13) . 2_465 ? O3 Rb1 O10 75.13(11) 2_565 2_465 ? O10 Rb1 O5W 133.9(2) . 1_365 ? O7 Rb1 O5W 128.83(16) . 1_365 ? O3 Rb1 O5W 65.71(19) 2_565 1_365 ? O10 Rb1 O5W 93.31(18) 2_465 1_365 ? O10 Rb1 O1 79.39(12) . 1_455 ? O7 Rb1 O1 95.33(13) . 1_455 ? O3 Rb1 O1 135.24(12) 2_565 1_455 ? O10 Rb1 O1 64.30(11) 2_465 1_455 ? O5W Rb1 O1 131.92(14) 1_365 1_455 ? O10 Rb1 O13 95.34(12) . 2_565 ? O7 Rb1 O13 66.83(13) . 2_565 ? O3 Rb1 O13 55.60(11) 2_565 2_565 ? O10 Rb1 O13 130.45(11) 2_465 2_565 ? O5W Rb1 O13 63.70(14) 1_365 2_565 ? O1 Rb1 O13 161.53(11) 1_455 2_565 ? O10 Rb1 O4W 155.7(2) . 1_455 ? O7 Rb1 O4W 127.85(18) . 1_455 ? O3 Rb1 O4W 124.93(18) 2_565 1_455 ? O10 Rb1 O4W 93.9(2) 2_465 1_455 ? O5W Rb1 O4W 61.2(2) 1_365 1_455 ? O1 Rb1 O4W 77.7(2) 1_455 1_455 ? O13 Rb1 O4W 108.9(2) 2_565 1_455 ? O10 Rb1 O9 106.17(12) . 2_465 ? O7 Rb1 O9 168.04(12) . 2_465 ? O3 Rb1 O9 75.76(11) 2_565 2_465 ? O10 Rb1 O9 40.02(11) 2_465 2_465 ? O5W Rb1 O9 56.46(16) 1_365 2_465 ? O1 Rb1 O9 84.46(11) 1_455 2_465 ? O13 Rb1 O9 113.99(11) 2_565 2_465 ? O4W Rb1 O9 63.84(17) 1_455 2_465 ? O10 Rb1 C1 63.99(14) . 1_455 ? O7 Rb1 C1 75.56(15) . 1_455 ? O3 Rb1 C1 129.89(14) 2_565 1_455 ? O10 Rb1 C1 73.58(13) 2_465 1_455 ? O5W Rb1 C1 152.89(16) 1_365 1_455 ? O1 Rb1 C1 20.99(13) 1_455 1_455 ? O13 Rb1 C1 142.33(13) 2_565 1_455 ? O4W Rb1 C1 95.4(2) 1_455 1_455 ? O9 Rb1 C1 102.33(13) 2_465 1_455 ? O10 Rb1 C6 87.35(13) . 2_465 ? O7 Rb1 C6 148.94(14) . 2_465 ? O3 Rb1 C6 76.13(12) 2_565 2_465 ? O10 Rb1 C6 19.33(13) 2_465 2_465 ? O5W Rb1 C6 76.06(18) 1_365 2_465 ? O1 Rb1 C6 71.82(12) 1_455 2_465 ? O13 Rb1 C6 125.97(12) 2_565 2_465 ? O4W Rb1 C6 78.08(19) 1_455 2_465 ? O9 Rb1 C6 20.82(12) 2_465 2_465 ? C1 Rb1 C6 86.22(14) 1_455 2_465 ? O10 Rb1 Cu2 93.52(9) . 2_565 ? O7 Rb1 Cu2 92.97(10) . 2_565 ? O3 Rb1 Cu2 30.80(8) 2_565 2_565 ? O10 Rb1 Cu2 100.82(9) 2_465 2_565 ? O5W Rb1 Cu2 46.83(14) 1_365 2_565 ? O1 Rb1 Cu2 164.96(8) 1_455 2_565 ? O13 Rb1 Cu2 31.21(8) 2_565 2_565 ? O4W Rb1 Cu2 106.83(18) 1_455 2_565 ? O9 Rb1 Cu2 84.84(8) 2_465 2_565 ? C1 Rb1 Cu2 157.46(12) 1_455 2_565 ? C6 Rb1 Cu2 94.78(9) 2_465 2_565 ? O10 Rb1 H1 99.4 . . ? O7 Rb1 H1 37.3 . . ? O3 Rb1 H1 110.7 2_565 . ? O10 Rb1 H1 164.6 2_465 . ? O5W Rb1 H1 102.1 1_365 . ? O1 Rb1 H1 104.6 1_455 . ? O13 Rb1 H1 58.5 2_565 . ? O4W Rb1 H1 93.9 1_455 . ? O9 Rb1 H1 154.0 2_465 . ? C1 Rb1 H1 92.4 1_455 . ? C6 Rb1 H1 171.7 2_465 . ? Cu2 Rb1 H1 89.6 2_565 . ? O15 Rb2 O15 79.64(17) 1_556 2_655 ? O15 Rb2 O1 145.23(16) 1_556 . ? O15 Rb2 O1 76.33(16) 2_655 . ? O15 Rb2 O2W 83.4(3) 1_556 . ? O15 Rb2 O2W 79.3(3) 2_655 . ? O1 Rb2 O2W 67.8(2) . . ? O15 Rb2 O4W 108.4(2) 1_556 . ? O15 Rb2 O4W 156.4(3) 2_655 . ? O1 Rb2 O4W 85.9(2) . . ? O2W Rb2 O4W 79.6(4) . . ? O15 Rb2 O12 60.83(19) 1_556 1_556 ? O15 Rb2 O12 131.5(2) 2_655 1_556 ? O1 Rb2 O12 151.0(2) . 1_556 ? O2W Rb2 O12 119.2(3) . 1_556 ? O4W Rb2 O12 69.2(3) . 1_556 ? O15 Rb2 O3W 73.7(4) 1_556 . ? O15 Rb2 O3W 75.0(3) 2_655 . ? O1 Rb2 O3W 122.4(3) . . ? O2W Rb2 O3W 148.1(4) . . ? O4W Rb2 O3W 128.4(4) . . ? O12 Rb2 O3W 68.2(4) 1_556 . ? O15 Rb2 O6 153.89(18) 1_556 . ? O15 Rb2 O6 101.08(15) 2_655 . ? O1 Rb2 O6 57.11(12) . . ? O2W Rb2 O6 122.6(2) . . ? O4W Rb2 O6 81.5(2) . . ? O12 Rb2 O6 103.15(15) 1_556 . ? O3W Rb2 O6 81.2(4) . . ? O15 Rb2 C9 94.34(16) 1_556 2_655 ? O15 Rb2 C9 15.51(16) 2_655 2_655 ? O1 Rb2 C9 65.55(14) . 2_655 ? O2W Rb2 C9 85.8(3) . 2_655 ? O4W Rb2 C9 151.2(2) . 2_655 ? O12 Rb2 C9 139.3(2) 1_556 2_655 ? O3W Rb2 C9 74.3(3) . 2_655 ? O6 Rb2 C9 85.70(15) . 2_655 ? O15 Rb2 Cu1 162.58(12) 1_556 . ? O15 Rb2 Cu1 83.20(11) 2_655 . ? O1 Rb2 Cu1 28.66(8) . . ? O2W Rb2 Cu1 96.3(2) . . ? O4W Rb2 Cu1 88.63(19) . . ? O12 Rb2 Cu1 131.93(13) 1_556 . ? O3W Rb2 Cu1 99.0(4) . . ? O6 Rb2 Cu1 29.52(9) . . ? C9 Rb2 Cu1 68.32(11) 2_655 . ? O15 Rb2 Rb3 114.55(14) 1_556 1_455 ? O15 Rb2 Rb3 66.60(14) 2_655 1_455 ? O1 Rb2 Rb3 78.03(9) . 1_455 ? O2W Rb2 Rb3 136.4(2) . 1_455 ? O4W Rb2 Rb3 125.08(18) . 1_455 ? O12 Rb2 Rb3 103.91(17) 1_556 1_455 ? O3W Rb2 Rb3 44.8(3) . 1_455 ? O6 Rb2 Rb3 45.78(10) . 1_455 ? C9 Rb2 Rb3 54.90(11) 2_655 1_455 ? Cu1 Rb2 Rb3 54.71(2) . 1_455 ? O15 Rb2 Rb2 40.00(11) 1_556 2_656 ? O15 Rb2 Rb2 39.64(11) 2_655 2_656 ? O1 Rb2 Rb2 112.23(9) . 2_656 ? O2W Rb2 Rb2 78.7(3) . 2_656 ? O4W Rb2 Rb2 143.41(18) . 2_656 ? O12 Rb2 Rb2 96.72(17) 1_556 2_656 ? O3W Rb2 Rb2 69.4(3) . 2_656 ? O6 Rb2 Rb2 135.06(10) . 2_656 ? C9 Rb2 Rb2 54.51(11) 2_655 2_656 ? Cu1 Rb2 Rb2 122.78(3) . 2_656 ? Rb3 Rb2 Rb2 90.57(3) 1_455 2_656 ? O2 Rb3 O5W 128.7(2) . . ? O2 Rb3 O14 163.02(16) . 2_755 ? O5W Rb3 O14 67.45(15) . 2_755 ? O2 Rb3 O4 62.93(16) . . ? O5W Rb3 O4 74.17(17) . . ? O14 Rb3 O4 133.14(13) 2_755 . ? O2 Rb3 O5 129.40(16) . 2_755 ? O5W Rb3 O5 72.1(2) . 2_755 ? O14 Rb3 O5 55.66(12) 2_755 2_755 ? O4 Rb3 O5 87.99(14) . 2_755 ? O2 Rb3 O3W 84.9(3) . 1_655 ? O5W Rb3 O3W 99.5(4) . 1_655 ? O14 Rb3 O3W 87.1(2) 2_755 1_655 ? O4 Rb3 O3W 125.7(3) . 1_655 ? O5 Rb3 O3W 142.5(2) 2_755 1_655 ? O2 Rb3 O6 86.93(16) . 1_655 ? O5W Rb3 O6 144.07(15) . 1_655 ? O14 Rb3 O6 76.64(12) 2_755 1_655 ? O4 Rb3 O6 137.07(13) . 1_655 ? O5 Rb3 O6 89.16(12) 2_755 1_655 ? O3W Rb3 O6 76.8(3) 1_655 1_655 ? O2 Rb3 C4 67.91(18) . 1_655 ? O5W Rb3 C4 162.85(17) . 1_655 ? O14 Rb3 C4 96.51(13) 2_755 1_655 ? O4 Rb3 C4 116.49(13) . 1_655 ? O5 Rb3 C4 94.11(13) 2_755 1_655 ? O3W Rb3 C4 85.2(3) 1_655 1_655 ? O6 Rb3 C4 21.30(13) 1_655 1_655 ? O2 Rb3 Cu2 159.87(12) . 2_755 ? O5W Rb3 Cu2 49.22(15) . 2_755 ? O14 Rb3 Cu2 32.63(9) 2_755 2_755 ? O4 Rb3 Cu2 100.93(11) . 2_755 ? O5 Rb3 Cu2 32.73(8) 2_755 2_755 ? O3W Rb3 Cu2 115.1(2) 1_655 2_755 ? O6 Rb3 Cu2 99.38(9) 1_655 2_755 ? C4 Rb3 Cu2 113.86(10) 1_655 2_755 ? O2 Rb3 C3 115.94(16) . 2_755 ? O5W Rb3 C3 68.4(2) . 2_755 ? O14 Rb3 C3 72.65(13) 2_755 2_755 ? O4 Rb3 C3 68.86(14) . 2_755 ? O5 Rb3 C3 19.14(12) 2_755 2_755 ? O3W Rb3 C3 159.1(3) 1_655 2_755 ? O6 Rb3 C3 102.72(13) 1_655 2_755 ? C4 Rb3 C3 101.82(14) 1_655 2_755 ? Cu2 Rb3 C3 44.09(10) 2_755 2_755 ? O2 Rb3 C1 13.70(16) . . ? O5W Rb3 C1 122.34(17) . . ? O14 Rb3 C1 167.45(14) 2_755 . ? O4 Rb3 C1 51.36(14) . . ? O5 Rb3 C1 117.45(14) 2_755 . ? O3W Rb3 C1 98.2(3) 1_655 . ? O6 Rb3 C1 93.41(13) 1_655 . ? C4 Rb3 C1 72.75(14) 1_655 . ? Cu2 Rb3 C1 146.27(11) 2_755 . ? C3 Rb3 C1 102.69(15) 2_755 . ? O2 Rb3 Cu1 110.71(15) . 1_655 ? O5W Rb3 Cu1 118.95(14) . 1_655 ? O14 Rb3 Cu1 55.70(9) 2_755 1_655 ? O4 Rb3 Cu1 132.75(11) . 1_655 ? O5 Rb3 Cu1 59.18(8) 2_755 1_655 ? O3W Rb3 Cu1 98.2(3) 1_655 1_655 ? O6 Rb3 Cu1 30.73(8) 1_655 1_655 ? C4 Rb3 Cu1 43.89(10) 1_655 1_655 ? Cu2 Rb3 Cu1 70.36(2) 2_755 1_655 ? C3 Rb3 Cu1 74.92(10) 2_755 1_655 ? C1 Rb3 Cu1 112.05(10) . 1_655 ? O1 Cu1 O8 172.11(19) . . ? O1 Cu1 O3 85.23(18) . . ? O8 Cu1 O3 100.02(18) . . ? O1 Cu1 O6 93.28(19) . . ? O8 Cu1 O6 82.59(18) . . ? O3 Cu1 O6 169.81(19) . . ? O1 Cu1 Rb3 106.18(14) . 1_455 ? O8 Cu1 Rb3 76.96(13) . 1_455 ? O3 Cu1 Rb3 115.85(13) . 1_455 ? O6 Cu1 Rb3 54.91(15) . 1_455 ? O1 Cu1 Rb1 102.94(14) . 2_565 ? O8 Cu1 Rb1 76.50(13) . 2_565 ? O3 Cu1 Rb1 49.91(12) . 2_565 ? O6 Cu1 Rb1 139.95(14) . 2_565 ? Rb3 Cu1 Rb1 146.14(3) 1_455 2_565 ? O1 Cu1 Rb2 46.89(13) . . ? O8 Cu1 Rb2 130.45(13) . . ? O3 Cu1 Rb2 126.78(13) . . ? O6 Cu1 Rb2 48.47(13) . . ? Rb3 Cu1 Rb2 69.14(3) 1_455 . ? Rb1 Cu1 Rb2 144.67(3) 2_565 . ? O1 Cu1 Rb1 45.93(14) . 1_655 ? O8 Cu1 Rb1 127.13(13) . 1_655 ? O3 Cu1 Rb1 95.05(12) . 1_655 ? O6 Cu1 Rb1 91.09(15) . 1_655 ? Rb3 Cu1 Rb1 137.96(3) 1_455 1_655 ? Rb1 Cu1 Rb1 75.63(2) 2_565 1_655 ? Rb2 Cu1 Rb1 69.56(2) . 1_655 ? O3 Cu2 O13 96.41(18) . . ? O3 Cu2 O14 172.86(19) . . ? O13 Cu2 O14 85.50(19) . . ? O3 Cu2 O5 85.13(18) . . ? O13 Cu2 O5 178.46(19) . . ? O14 Cu2 O5 92.95(19) . . ? O3 Cu2 Rb3 116.94(13) . 2_755 ? O13 Cu2 Rb3 121.59(13) . 2_755 ? O14 Cu2 Rb3 56.65(13) . 2_755 ? O5 Cu2 Rb3 57.36(13) . 2_755 ? O3 Cu2 Rb1 53.25(12) . 2_565 ? O13 Cu2 Rb1 57.57(13) . 2_565 ? O14 Cu2 Rb1 123.41(14) . 2_565 ? O5 Cu2 Rb1 123.53(13) . 2_565 ? Rb3 Cu2 Rb1 105.48(3) 2_755 2_565 ? O8 Cu3 O9 82.98(18) . . ? O8 Cu3 O13 98.78(18) . . ? O9 Cu3 O13 176.0(2) . . ? O8 Cu3 O11 167.7(2) . . ? O9 Cu3 O11 91.9(2) . . ? O13 Cu3 O11 85.7(2) . . ? O8 Cu3 Rb1 68.13(13) . 2_565 ? O9 Cu3 Rb1 132.61(14) . 2_565 ? O13 Cu3 Rb1 45.77(13) . 2_565 ? O11 Cu3 Rb1 108.38(16) . 2_565 ? C1 O1 Cu1 114.4(4) . . ? C1 O1 Rb2 129.6(4) . . ? Cu1 O1 Rb2 104.46(17) . . ? C1 O1 Rb1 99.0(4) . 1_655 ? Cu1 O1 Rb1 107.55(18) . 1_655 ? Rb2 O1 Rb1 98.43(13) . 1_655 ? C1 O2 Rb3 135.1(5) . . ? C2 O3 Cu2 109.8(3) . . ? C2 O3 Cu1 111.8(4) . . ? Cu2 O3 Cu1 122.7(2) . . ? C2 O3 Rb1 114.5(3) . 2_565 ? Cu2 O3 Rb1 95.95(16) . 2_565 ? Cu1 O3 Rb1 100.63(16) . 2_565 ? Rb2 O3W Rb3 92.6(4) . 1_455 ? C3 O4 Rb3 124.0(4) . . ? Rb2 O4W Rb1 94.1(3) . 1_655 ? C3 O5 Cu2 113.8(4) . . ? C3 O5 Rb3 111.1(3) . 2_755 ? Cu2 O5 Rb3 89.91(16) . 2_755 ? Rb3 O5W Rb1 157.0(3) . 1_745 ? C4 O6 Cu1 114.8(4) . . ? C4 O6 Rb2 141.6(4) . . ? Cu1 O6 Rb2 102.01(17) . . ? C4 O6 Rb3 96.3(4) . 1_455 ? Cu1 O6 Rb3 94.35(18) . 1_455 ? Rb2 O6 Rb3 91.37(12) . 1_455 ? C4 O7 Rb1 140.5(4) . . ? C5 O8 Cu3 112.9(3) . . ? C5 O8 Cu1 110.5(4) . . ? Cu3 O8 Cu1 136.6(2) . . ? C6 O9 Cu3 115.9(4) . . ? C6 O9 Rb1 90.6(3) . 2_465 ? Cu3 O9 Rb1 148.0(2) . 2_465 ? C6 O10 Rb1 139.6(4) . . ? C6 O10 Rb1 105.6(4) . 2_465 ? Rb1 O10 Rb1 111.20(13) . 2_465 ? C7 O11 Cu3 114.0(4) . . ? C7 O12 Rb2 130.0(5) . 1_554 ? C8 O13 Cu3 112.0(4) . . ? C8 O13 Cu2 110.3(4) . . ? Cu3 O13 Cu2 118.2(2) . . ? C8 O13 Rb1 115.5(4) . 2_565 ? Cu3 O13 Rb1 108.25(17) . 2_565 ? Cu2 O13 Rb1 91.21(16) . 2_565 ? C9 O14 Cu2 113.9(4) . . ? C9 O14 Rb3 117.6(4) . 2_755 ? Cu2 O14 Rb3 90.73(16) . 2_755 ? C9 O15 Rb2 130.8(5) . 1_554 ? C9 O15 Rb2 125.4(5) . 2_655 ? Rb2 O15 Rb2 100.36(17) 1_554 2_655 ? O2 C1 O1 122.7(7) . . ? O2 C1 C2 120.0(6) . . ? O1 C1 C2 117.2(5) . . ? O2 C1 Rb1 87.2(4) . 1_655 ? O1 C1 Rb1 60.0(3) . 1_655 ? C2 C1 Rb1 121.1(4) . 1_655 ? O2 C1 Rb3 31.2(3) . . ? O1 C1 Rb3 153.6(5) . . ? C2 C1 Rb3 89.1(3) . . ? Rb1 C1 Rb3 108.63(17) 1_655 . ? O3 C2 C1 110.0(5) . . ? O3 C2 C3 111.5(5) . . ? C1 C2 C3 114.5(5) . . ? O3 C2 H2 106.8 . . ? C1 C2 H2 106.8 . . ? C3 C2 H2 106.8 . . ? O4 C3 O5 122.8(6) . . ? O4 C3 C2 122.5(6) . . ? O5 C3 C2 114.6(5) . . ? O4 C3 Rb3 100.7(4) . 2_755 ? O5 C3 Rb3 49.7(3) . 2_755 ? C2 C3 Rb3 115.0(4) . 2_755 ? O7 C4 O6 124.9(6) . . ? O7 C4 C5 121.4(5) . . ? O6 C4 C5 113.5(5) . . ? O7 C4 Rb3 107.8(4) . 1_455 ? O6 C4 Rb3 62.4(3) . 1_455 ? C5 C4 Rb3 101.3(3) . 1_455 ? O8 C5 C6 108.8(5) . . ? O8 C5 C4 109.0(5) . . ? C6 C5 C4 114.8(5) . . ? O8 C5 C5 112.0(6) . 2_565 ? C6 C5 C5 107.1(5) . 2_565 ? C4 C5 C5 105.1(6) . 2_565 ? O10 C6 O9 123.0(5) . . ? O10 C6 C5 122.5(5) . . ? O9 C6 C5 114.4(5) . . ? O10 C6 Rb1 55.1(3) . 2_465 ? O9 C6 Rb1 68.6(3) . 2_465 ? C5 C6 Rb1 168.1(4) . 2_465 ? O12 C7 O11 123.4(7) . . ? O12 C7 C8 120.4(7) . . ? O11 C7 C8 116.2(6) . . ? O13 C8 C7 111.3(5) . . ? O13 C8 C9 111.4(5) . . ? C7 C8 C9 111.9(6) . . ? O13 C8 H8 107.3 . . ? C7 C8 H8 107.3 . . ? C9 C8 H8 107.3 . . ? O15 C9 O14 123.9(7) . . ? O15 C9 C8 120.4(6) . . ? O14 C9 C8 115.5(6) . . ? O15 C9 Rb2 39.0(4) . 2_655 ? O14 C9 Rb2 84.9(4) . 2_655 ? C8 C9 Rb2 159.3(4) . 2_655 ? H1 O1W H1W 109.5 . . ? Rb2 O2W H2WA 109.8 . . ? Rb2 O2W H2WB 109.8 . . ? H2WA O2W H2WB 109.1 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 66.97 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.829 _refine_diff_density_min -1.847 _refine_diff_density_rms 0.217 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1 O7 0.87 2.00 2.748(8) 143.4 . O1W H1W O12 0.87 1.87 2.726(9) 169.0 1_556 O2W H2WB O3W 0.88 2.16 2.81(2) 130.1 2_656 #==END==# _database_code_depnum_ccdc_archive 'CCDC 947968'