# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Braga, Dario' 'Cojazzi, Gianna' 'Grepioni, F.' 'Maini, Lucia' _publ_contact_author_name 'Prof Dario Braga' _publ_contact_author_address ; Prof Dario Braga Dipartimento di Chimica G. Ciamician Universita di Bologna Via F. Selmi 2 Bologna 40126 ITALY ; _publ_contact_author_email 'DBRAGA@CIAM.UNIBO.IT' data_1 _database_code_CSD 163618 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Rhodizonic acid dihydrate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H6 O8' _chemical_formula_weight 206.11 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.2163(13) _cell_length_b 9.6120(12) _cell_length_c 12.786(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.796(6) _cell_angle_gamma 90.00 _cell_volume 1377.8(3) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.987 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 0.193 _exptl_absorpt_correction_type 'Bruker absorption correction' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9624 _diffrn_reflns_av_R_equivalents 0.1276 _diffrn_reflns_av_sigmaI/netI 0.1551 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 33.95 _reflns_number_total 2589 _reflns_number_gt 1219 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0731P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0029(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2589 _refine_ls_number_parameters 152 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1436 _refine_ls_R_factor_gt 0.0592 _refine_ls_wR_factor_ref 0.1462 _refine_ls_wR_factor_gt 0.1194 _refine_ls_goodness_of_fit_ref 0.730 _refine_ls_restrained_S_all 0.730 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.54949(15) 0.46317(18) 0.12446(15) 0.0179(4) Uani 1 1 d . . . H1 H 0.578(3) 0.549(3) 0.125(2) 0.017(7) Uiso 1 1 d . . . O2 O 0.41445(16) 0.69842(17) 0.12742(16) 0.0227(4) Uani 1 1 d . . . O3A O 0.21427(17) 0.56870(18) -0.01194(13) 0.0174(4) Uani 1 1 d . . . H31 H 0.140(3) 0.547(4) -0.026(3) 0.044(11) Uiso 1 1 d . . . O3B O 0.17288(16) 0.70215(16) 0.13558(14) 0.0156(4) Uani 1 1 d . . . H32 H 0.216(4) 0.771(4) 0.125(3) 0.067(14) Uiso 1 1 d . . . O4A O 0.18712(17) 0.46878(18) 0.26242(14) 0.0180(4) Uani 1 1 d . . . H41 H 0.156(3) 0.541(4) 0.279(3) 0.047(11) Uiso 1 1 d . . . O4B O 0.05609(15) 0.44396(17) 0.11753(15) 0.0172(4) Uani 1 1 d . . . H42 H 0.038(3) 0.361(4) 0.132(3) 0.049(11) Uiso 1 1 d . . . O5 O 0.19167(15) 0.21210(16) 0.11862(14) 0.0180(4) Uani 1 1 d . . . O6 O 0.43038(16) 0.20778(17) 0.12869(15) 0.0183(4) Uani 1 1 d . . . H6 H 0.506(5) 0.225(5) 0.138(4) 0.11(2) Uiso 1 1 d . . . C1 C 0.4297(2) 0.4567(2) 0.12278(18) 0.0123(5) Uani 1 1 d . . . C2 C 0.3627(2) 0.5878(2) 0.11872(18) 0.0130(5) Uani 1 1 d . . . C3 C 0.2282(2) 0.5815(2) 0.09724(18) 0.0113(4) Uani 1 1 d . . . C4 C 0.1741(2) 0.4556(2) 0.15323(18) 0.0119(4) Uani 1 1 d . . . C5 C 0.2442(2) 0.3225(2) 0.12925(18) 0.0113(4) Uani 1 1 d . . . C6 C 0.3738(2) 0.3312(2) 0.12649(18) 0.0128(5) 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 O1 0.0085(9) 0.0149(8) 0.0304(10) 0.0015(7) 0.0013(7) -0.0012(7) O2 0.0150(10) 0.0132(8) 0.0401(12) 0.0005(8) 0.0017(8) -0.0024(7) O3A 0.0184(10) 0.0218(9) 0.0120(8) 0.0017(7) -0.0025(7) -0.0005(7) O3B 0.0147(9) 0.0089(7) 0.0233(9) -0.0006(6) 0.0037(7) 0.0021(7) O4A 0.0260(11) 0.0151(8) 0.0130(8) -0.0007(6) 0.0038(7) 0.0015(7) O4B 0.0096(9) 0.0128(8) 0.0292(10) 0.0031(7) 0.0005(7) -0.0006(6) O5 0.0140(9) 0.0133(7) 0.0266(10) -0.0017(7) 0.0000(7) -0.0017(7) O6 0.0137(10) 0.0119(7) 0.0296(10) 0.0022(7) 0.0024(8) 0.0037(7) C1 0.0099(11) 0.0141(9) 0.0130(11) -0.0004(8) 0.0003(8) 0.0007(9) C2 0.0139(12) 0.0113(9) 0.0139(11) 0.0004(8) 0.0029(9) -0.0004(8) C3 0.0138(12) 0.0101(9) 0.0099(10) -0.0005(7) 0.0004(8) 0.0017(8) C4 0.0116(11) 0.0099(8) 0.0142(11) 0.0004(8) 0.0013(9) -0.0002(8) C5 0.0125(12) 0.0119(9) 0.0094(10) 0.0019(8) -0.0011(8) 0.0014(8) C6 0.0119(12) 0.0120(10) 0.0146(11) -0.0004(8) 0.0007(9) 0.0010(8) _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 O1 C1 1.344(3) . ? O1 H1 0.88(3) . ? O2 C2 1.214(3) . ? O3A C3 1.405(3) . ? O3A H31 0.87(4) . ? O3B C3 1.410(3) . ? O3B H32 0.84(4) . ? O4A C4 1.405(3) . ? O4A H41 0.81(3) . ? O4B C4 1.391(3) . ? O4B H42 0.85(4) . ? O5 C5 1.219(3) . ? O6 C6 1.346(3) . ? O6 H6 0.87(5) . ? C1 C6 1.361(3) . ? C1 C2 1.467(3) . ? C2 C3 1.527(3) . ? C3 C4 1.541(3) . ? C4 C5 1.538(3) . ? C5 C6 1.457(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 O1 H1 113.7(19) . . ? C3 O3A H31 108(2) . . ? C3 O3B H32 109(3) . . ? C4 O4A H41 108(3) . . ? C4 O4B H42 104(2) . . ? C6 O6 H6 107(3) . . ? O1 C1 C6 120.1(2) . . ? O1 C1 C2 118.13(19) . . ? C6 C1 C2 121.8(2) . . ? O2 C2 C1 120.4(2) . . ? O2 C2 C3 121.2(2) . . ? C1 C2 C3 118.34(19) . . ? O3B C3 O3A 112.42(18) . . ? O3B C3 C2 110.37(18) . . ? O3A C3 C2 105.09(18) . . ? O3B C3 C4 107.49(18) . . ? O3A C3 C4 111.07(18) . . ? C2 C3 C4 110.43(18) . . ? O4B C4 O4A 113.70(18) . . ? O4B C4 C5 110.79(18) . . ? O4A C4 C5 103.59(18) . . ? O4B C4 C3 107.18(18) . . ? O4A C4 C3 111.14(18) . . ? C5 C4 C3 110.47(18) . . ? O5 C5 C6 121.8(2) . . ? O5 C5 C4 119.8(2) . . ? C6 C5 C4 118.26(19) . . ? O6 C6 C1 124.4(2) . . ? O6 C6 C5 114.76(19) . . ? C1 C6 C5 120.9(2) . . ? _diffrn_measured_fraction_theta_max 0.923 _diffrn_reflns_theta_full 33.95 _diffrn_measured_fraction_theta_full 0.923 _refine_diff_density_max 0.526 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.091 data_3 _database_code_CSD 163619 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Rubidium rhodizonate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 O6 Rb2' _chemical_formula_weight 339.00 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rb' 'Rb' -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/m 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' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 12.522(4) _cell_length_b 8.354(4) _cell_length_c 3.761(3) _cell_angle_alpha 90.0 _cell_angle_beta 96.93(5) _cell_angle_gamma 90.0 _cell_volume 390.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour green _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.883 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 316 _exptl_absorpt_coefficient_mu 12.528 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.17 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1001 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0718 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 27.95 _reflns_number_total 501 _reflns_number_gt 399 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0720P)^2^+0.1776P] 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 0.000(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 501 _refine_ls_number_parameters 36 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0545 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.1061 _refine_ls_wR_factor_gt 0.1006 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.003 _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 Rb1 Rb 0.16195(5) 0.5000 0.0822(2) 0.0266(3) Uani 1 2 d S . . O1 O 0.0000 0.3267(7) 0.5000 0.0307(12) Uani 1 2 d S . . O2 O 0.1653(3) 0.1606(5) 0.2594(12) 0.0331(9) Uani 1 1 d . . . C1 C 0.0000 0.1768(9) 0.5000 0.0198(13) Uani 1 2 d S . . C2 C 0.0889(3) 0.0879(5) 0.3714(12) 0.0194(10) 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 Rb1 0.0267(4) 0.0263(4) 0.0266(5) 0.000 0.0030(3) 0.000 O1 0.036(3) 0.022(3) 0.035(3) 0.000 0.006(2) 0.000 O2 0.0324(18) 0.026(2) 0.043(2) 0.002(2) 0.0111(16) -0.0046(16) C1 0.020(3) 0.020(3) 0.018(3) 0.000 -0.003(2) 0.000 C2 0.0203(19) 0.023(2) 0.015(2) -0.0026(19) -0.0007(17) -0.0017(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rb1 O2 2.909(4) . ? Rb1 O2 2.914(4) 6_565 ? Rb1 O2 2.965(4) 4 ? Rb1 O2 2.968(4) 7 ? Rb1 O1 3.072(3) . ? Rb1 O1 3.075(3) 5_566 ? Rb1 O1 3.147(3) 5_565 ? Rb1 O1 3.155(3) 1_554 ? Rb1 O2 3.360(5) 7_556 ? Rb1 O2 3.368(5) 4_556 ? Rb1 C2 3.596(5) 7_556 ? Rb1 C2 3.600(5) 4_556 ? O1 C1 1.252(9) . ? O1 Rb1 3.075(3) 5_566 ? O1 Rb1 3.147(3) 5_565 ? O1 Rb1 3.155(3) 1_556 ? O2 C2 1.248(6) . ? O2 Rb1 2.968(4) 7 ? O2 Rb1 3.360(5) 7_556 ? C1 C2 1.468(5) 2_556 ? C1 C2 1.468(5) . ? C2 C2 1.469(9) 6 ? C2 Rb1 3.596(5) 7_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Rb1 O2 153.70(18) . 6_565 ? O2 Rb1 O2 123.22(10) . 4 ? O2 Rb1 O2 70.62(13) 6_565 4 ? O2 Rb1 O2 70.54(13) . 7 ? O2 Rb1 O2 123.30(10) 6_565 7 ? O2 Rb1 O2 53.79(16) 4 7 ? O2 Rb1 O1 54.37(12) . . ? O2 Rb1 O1 109.45(13) 6_565 . ? O2 Rb1 O1 174.28(9) 4 . ? O2 Rb1 O1 124.69(13) 7 . ? O2 Rb1 O1 109.56(13) . 5_566 ? O2 Rb1 O1 54.26(12) 6_565 5_566 ? O2 Rb1 O1 124.66(13) 4 5_566 ? O2 Rb1 O1 174.28(9) 7 5_566 ? O1 Rb1 O1 56.19(19) . 5_566 ? O2 Rb1 O1 126.49(14) . 5_565 ? O2 Rb1 O1 72.80(13) 6_565 5_565 ? O2 Rb1 O1 86.25(11) 4 5_565 ? O2 Rb1 O1 110.36(11) 7 5_565 ? O1 Rb1 O1 99.26(10) . 5_565 ? O1 Rb1 O1 74.36(9) 5_566 5_565 ? O2 Rb1 O1 72.54(14) . 1_554 ? O2 Rb1 O1 126.75(14) 6_565 1_554 ? O2 Rb1 O1 110.43(11) 4 1_554 ? O2 Rb1 O1 86.07(11) 7 1_554 ? O1 Rb1 O1 74.30(9) . 1_554 ? O1 Rb1 O1 99.44(10) 5_566 1_554 ? O1 Rb1 O1 54.68(19) 5_565 1_554 ? O2 Rb1 O2 56.98(14) . 7_556 ? O2 Rb1 O2 103.14(10) 6_565 7_556 ? O2 Rb1 O2 93.44(12) 4 7_556 ? O2 Rb1 O2 72.63(10) 7 7_556 ? O1 Rb1 O2 80.95(9) . 7_556 ? O1 Rb1 O2 102.48(9) 5_566 7_556 ? O1 Rb1 O2 175.80(11) 5_565 7_556 ? O1 Rb1 O2 129.13(13) 1_554 7_556 ? O2 Rb1 O2 103.42(10) . 4_556 ? O2 Rb1 O2 56.69(14) 6_565 4_556 ? O2 Rb1 O2 72.54(10) 4 4_556 ? O2 Rb1 O2 93.62(12) 7 4_556 ? O1 Rb1 O2 102.57(9) . 4_556 ? O1 Rb1 O2 80.77(9) 5_566 4_556 ? O1 Rb1 O2 129.11(13) 5_565 4_556 ? O1 Rb1 O2 175.82(11) 1_554 4_556 ? O2 Rb1 O2 47.01(14) 7_556 4_556 ? O2 Rb1 C2 71.65(12) . 7_556 ? O2 Rb1 C2 94.49(12) 6_565 7_556 ? O2 Rb1 C2 73.20(12) 4 7_556 ? O2 Rb1 C2 61.88(12) 7 7_556 ? O1 Rb1 C2 101.16(9) . 7_556 ? O1 Rb1 C2 112.54(9) 5_566 7_556 ? O1 Rb1 C2 158.66(10) 5_565 7_556 ? O1 Rb1 C2 138.07(12) 1_554 7_556 ? O2 Rb1 C2 20.30(9) 7_556 7_556 ? O2 Rb1 C2 39.20(10) 4_556 7_556 ? O2 Rb1 C2 94.75(12) . 4_556 ? O2 Rb1 C2 71.38(12) 6_565 4_556 ? O2 Rb1 C2 61.76(12) 4 4_556 ? O2 Rb1 C2 73.38(12) 7 4_556 ? O1 Rb1 C2 112.66(8) . 4_556 ? O1 Rb1 C2 100.97(9) 5_566 4_556 ? O1 Rb1 C2 138.07(12) 5_565 4_556 ? O1 Rb1 C2 158.68(10) 1_554 4_556 ? O2 Rb1 C2 39.18(10) 7_556 4_556 ? O2 Rb1 C2 20.30(9) 4_556 4_556 ? C2 Rb1 C2 23.56(14) 7_556 4_556 ? C1 O1 Rb1 118.03(10) . . ? C1 O1 Rb1 118.16(10) . 5_566 ? Rb1 O1 Rb1 123.81(19) . 5_566 ? C1 O1 Rb1 117.20(11) . 5_565 ? Rb1 O1 Rb1 80.74(10) . 5_565 ? Rb1 O1 Rb1 74.36(9) 5_566 5_565 ? C1 O1 Rb1 117.48(11) . 1_556 ? Rb1 O1 Rb1 74.30(9) . 1_556 ? Rb1 O1 Rb1 80.56(10) 5_566 1_556 ? Rb1 O1 Rb1 125.32(19) 5_565 1_556 ? C2 O2 Rb1 124.1(3) . . ? C2 O2 Rb1 123.7(3) . 7 ? Rb1 O2 Rb1 109.46(13) . 7 ? C2 O2 Rb1 90.6(3) . 7_556 ? Rb1 O2 Rb1 123.02(14) . 7_556 ? Rb1 O2 Rb1 72.63(10) 7 7_556 ? O1 C1 C2 120.4(3) . 2_556 ? O1 C1 C2 120.4(3) . . ? C2 C1 C2 119.2(6) 2_556 . ? O2 C2 C2 119.1(3) . 6 ? O2 C2 C1 120.5(5) . . ? C2 C2 C1 120.4(3) 6 . ? O2 C2 Rb1 69.1(3) . 7_556 ? C2 C2 Rb1 78.36(9) 6 7_556 ? C1 C2 Rb1 123.6(2) . 7_556 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.95 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.892 _refine_diff_density_min -0.760 _refine_diff_density_rms 0.184