Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Bakalbassis, Evangelos G.' 'Korabik, Maria' 'Michailides, Adonis' 'Mrozinski, Jerzy' 'Raptopoulou, Catherine' 'Skoulika, Stavroula' 'Terzis, Aris' 'Tsaousis, Dimitris' _publ_contact_author_name 'Dr Evangelos G Bakalbassis' _publ_contact_author_address ; Dr Evangelos G Bakalbassis Dept of General & Inorganic Chemistry, Faculty of Chemistry Aristotle University of Thessaloniki PO Box 135 Thessaloniki 54006 GREECE ; #COMPOUND 1 data_shel93_COMPOUND_1 _database_code_CSD 152778 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C6 H12 Cd O6' _chemical_formula_weight 292.56 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cd' 'Cd' -0.8075 1.2024 '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 16.523(7) _cell_length_b 5.585(2) _cell_length_c 11.089(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.53(1) _cell_angle_gamma 90.00 _cell_volume 1018.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 298 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5.4 _cell_measurement_theta_max 11.6 _exptl_crystal_description 'parallelipiped' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.908 _exptl_crystal_density_method ? _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 2.141 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Crystal Logic Dual Goniometer diffractometer' _diffrn_measurement_method theta-2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.5 _diffrn_reflns_number 1143 _diffrn_reflns_av_R_equivalents 0.0109 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.69 _diffrn_reflns_theta_max 26.98 _reflns_number_total 1105 _reflns_number_observed 1042 _reflns_observed_criterion >2sigma(I) _computing_data_collection ; Program COLLECT (UCLA Crystallographic package, C.E.Strouse, 1994) ; _computing_cell_refinement ; Program LEAST (UCLA Crystallographic package, C.E.Strouse, 1994) ; _computing_data_reduction ; Program REDUCE (UCLA Crystallographic package, C.E.Strouse, 1994) ; _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.4426P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1105 _refine_ls_number_parameters 84 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0245 _refine_ls_R_factor_obs 0.0220 _refine_ls_wR_factor_all 0.0580 _refine_ls_wR_factor_obs 0.0561 _refine_ls_goodness_of_fit_all 1.080 _refine_ls_goodness_of_fit_obs 1.078 _refine_ls_restrained_S_all 1.080 _refine_ls_restrained_S_obs 1.078 _refine_ls_shift/esd_max 0.100 _refine_ls_shift/esd_mean 0.006 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cd Cd 0.0000 0.15999(4) 0.2500 0.03067(11) Uani 1 d S . OW O -0.0840(2) -0.1047(4) 0.3222(2) 0.0431(5) Uani 1 d . . O1 O 0.0621(2) 0.2352(5) 0.4432(2) 0.0507(6) Uani 1 d . . O2 O 0.09592(13) 0.4648(4) 0.2970(2) 0.0401(4) Uani 1 d . . C1 C 0.1022(2) 0.4086(6) 0.4074(2) 0.0379(6) Uani 1 d . . C2 C 0.1568(3) 0.5458(9) 0.4986(3) 0.0654(12) Uani 1 d . . C3 C 0.2220(2) 0.6894(7) 0.4501(3) 0.0490(8) Uani 1 d . . H2A H 0.1810(39) 0.4338(128) 0.5661(59) 0.120(21) Uiso 1 d . . H2B H 0.1107(39) 0.6921(115) 0.5157(60) 0.114(23) Uiso 1 d . . H3A H 0.2574(38) 0.5653(119) 0.4117(52) 0.110(19) Uiso 1 d . . H3B H 0.2021(31) 0.8099(86) 0.3933(47) 0.080(16) Uiso 1 d . . HWA H -0.0715(30) -0.1396(74) 0.3931(47) 0.066(14) Uiso 1 d . . HWB H -0.0890(33) -0.2281(104) 0.2936(49) 0.082(17) Uiso 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 Cd 0.0394(2) 0.0265(2) 0.02457(15) 0.000 -0.00516(10) 0.000 OW 0.0623(14) 0.0377(11) 0.0291(10) -0.0006(9) 0.0032(9) -0.0119(10) O1 0.0659(14) 0.0542(13) 0.0303(10) 0.0032(10) -0.0052(9) -0.0288(12) O2 0.0525(11) 0.0365(10) 0.0298(9) 0.0012(8) -0.0042(8) -0.0112(9) C1 0.0403(14) 0.0410(14) 0.0316(13) -0.0041(11) 0.0000(11) -0.0100(12) C2 0.075(2) 0.084(3) 0.0352(15) -0.009(2) 0.000(2) -0.051(2) C3 0.053(2) 0.055(2) 0.038(2) -0.0021(14) -0.0020(14) -0.023(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 Cd OW 2.229(2) . ? Cd OW 2.229(2) 6_556 ? Cd O1 2.323(2) . ? Cd O1 2.323(2) 6_556 ? Cd O2 2.350(2) 6_556 ? Cd O2 2.350(2) . ? Cd C1 2.694(3) 6_556 ? Cd C1 2.694(3) . ? O1 C1 1.259(4) . ? O2 C1 1.258(3) . ? C1 C2 1.500(4) . ? C2 C3 1.484(5) . ? C3 C3 1.531(6) 7_566 ? 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 OW Cd OW 96.92(13) . 6_556 ? OW Cd O1 91.36(8) . . ? OW Cd O1 102.48(10) 6_556 . ? OW Cd O1 102.48(10) . 6_556 ? OW Cd O1 91.36(8) 6_556 6_556 ? O1 Cd O1 159.16(14) . 6_556 ? OW Cd O2 97.48(9) . 6_556 ? OW Cd O2 146.17(8) 6_556 6_556 ? O1 Cd O2 107.60(9) . 6_556 ? O1 Cd O2 55.64(7) 6_556 6_556 ? OW Cd O2 146.17(8) . . ? OW Cd O2 97.48(9) 6_556 . ? O1 Cd O2 55.64(7) . . ? O1 Cd O2 107.60(9) 6_556 . ? O2 Cd O2 87.15(11) 6_556 . ? OW Cd C1 101.61(10) . 6_556 ? OW Cd C1 118.83(9) 6_556 6_556 ? O1 Cd C1 134.27(10) . 6_556 ? O1 Cd C1 27.82(8) 6_556 6_556 ? O2 Cd C1 27.82(8) 6_556 6_556 ? O2 Cd C1 97.91(9) . 6_556 ? OW Cd C1 118.83(9) . . ? OW Cd C1 101.62(10) 6_556 . ? O1 Cd C1 27.82(8) . . ? O1 Cd C1 134.27(10) 6_556 . ? O2 Cd C1 97.91(9) 6_556 . ? O2 Cd C1 27.82(8) . . ? C1 Cd C1 117.95(14) 6_556 . ? C1 O1 Cd 92.7(2) . . ? C1 O2 Cd 91.5(2) . . ? O2 C1 O1 120.2(2) . . ? O2 C1 C2 121.1(3) . . ? O1 C1 C2 118.8(3) . . ? O2 C1 Cd 60.72(14) . . ? O1 C1 Cd 59.46(14) . . ? C2 C1 Cd 177.8(2) . . ? C3 C2 C1 116.2(3) . . ? C2 C3 C3 112.7(4) . 7_566 ? _refine_diff_density_max 0.342 _refine_diff_density_min -0.412 _refine_diff_density_rms 0.089 #===END #COMPOUND 2 data_shel93_COMPOUND_2 _database_code_CSD 152779 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C6 H12 Cu O6' _chemical_formula_weight 243.70 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cu' 'Cu' 0.3201 1.2651 '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 4.929(2) _cell_length_b 11.328(4) _cell_length_c 3.866(1) _cell_angle_alpha 87.09(1) _cell_angle_beta 83.47(1) _cell_angle_gamma 84.31(1) _cell_volume 213.2(1) _cell_formula_units_Z 1 _cell_measurement_temperature 298 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5.3 _cell_measurement_theta_max 11.4 _exptl_crystal_description 'parallelipiped' _exptl_crystal_colour 'blueish' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.898 _exptl_crystal_density_method ? _exptl_crystal_F_000 125 _exptl_absorpt_coefficient_mu 2.557 _exptl_absorpt_correction_type 'psi-scan empirical' _exptl_absorpt_correction_T_min 0.87 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Crystal Logic Dual Goniometer diffractometer' _diffrn_measurement_method 'theta-2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.2 _diffrn_reflns_number 1488 _diffrn_reflns_av_R_equivalents 0.0104 _diffrn_reflns_av_sigmaI/netI 0.0303 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.00 _reflns_number_total 744 _reflns_number_observed 741 _reflns_observed_criterion >2sigma(I) _computing_data_collection ; Program COLLECT (UCLA Crystallographic package, C.E.Strouse, 1994) ; _computing_cell_refinement ; Program LEAST (UCLA Crystallographic package, C.E.Strouse, 1994) ; _computing_data_reduction ; Program REDUCE (UCLA Crystallographic package, C.E.Strouse, 1994) ; _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0195P)^2^+0.0993P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 744 _refine_ls_number_parameters 85 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0200 _refine_ls_R_factor_obs 0.0200 _refine_ls_wR_factor_all 0.0535 _refine_ls_wR_factor_obs 0.0535 _refine_ls_goodness_of_fit_all 1.120 _refine_ls_goodness_of_fit_obs 1.122 _refine_ls_restrained_S_all 1.120 _refine_ls_restrained_S_obs 1.122 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu Cu 0.0000 0.0000 0.0000 0.02585(15) Uani 1 d S . O1 O -0.2941(3) 0.12593(12) 0.0484(4) 0.0293(3) Uani 1 d . . OW O 0.2022(4) 0.07577(14) 0.3252(4) 0.0298(3) Uani 1 d . . O2 O -0.0613(3) 0.24981(13) -0.3091(4) 0.0331(3) Uani 1 d . . C1 C -0.2586(4) 0.2299(2) -0.0946(5) 0.0234(4) Uani 1 d . . C2 C -0.4762(4) 0.3279(2) 0.0164(5) 0.0237(4) Uani 1 d . . C3 C -0.3851(4) 0.4522(2) -0.0521(5) 0.0234(4) Uani 1 d . . HWA H 0.3374(67) 0.0932(26) 0.2523(75) 0.041(8) Uiso 1 d . . HWB H 0.1244(63) 0.1268(27) 0.3962(73) 0.040(8) Uiso 1 d . . H2A H -0.5278(51) 0.3161(22) 0.2604(69) 0.034(6) Uiso 1 d . . H2B H -0.6271(54) 0.3160(22) -0.0967(64) 0.032(6) Uiso 1 d . . H3A H -0.3210(49) 0.4646(21) -0.2915(65) 0.030(6) Uiso 1 d . . H3B H -0.2217(55) 0.4619(22) 0.0646(64) 0.034(6) Uiso 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 Cu 0.0153(2) 0.0118(2) 0.0485(2) -0.00307(13) 0.00248(14) 0.00221(12) O1 0.0189(7) 0.0138(7) 0.0530(9) -0.0027(6) 0.0029(6) 0.0026(5) OW 0.0181(8) 0.0190(8) 0.0502(9) -0.0068(7) 0.0062(6) -0.0007(6) O2 0.0269(8) 0.0240(7) 0.0445(8) -0.0089(6) 0.0128(7) 0.0013(6) C1 0.0190(9) 0.0173(9) 0.0338(10) -0.0074(7) -0.0015(8) 0.0008(7) C2 0.0210(10) 0.0164(9) 0.0316(10) -0.0031(7) 0.0037(8) 0.0029(7) C3 0.0234(10) 0.0159(9) 0.0287(10) -0.0032(7) 0.0035(8) 0.0025(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 Cu O1 1.9305(14) . ? Cu O1 1.9305(14) 2 ? Cu OW 1.968(2) 2 ? Cu OW 1.968(2) . ? O1 C1 1.294(2) . ? O2 C1 1.235(3) . ? C1 C2 1.508(3) . ? C2 C3 1.522(3) . ? C3 C3 1.521(4) 2_465 ? 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 O1 Cu O1 180.0 . 2 ? O1 Cu OW 89.19(7) . 2 ? O1 Cu OW 90.81(7) 2 2 ? O1 Cu OW 90.81(7) . . ? O1 Cu OW 89.19(7) 2 . ? OW Cu OW 180.0 2 . ? C1 O1 Cu 119.85(13) . . ? O2 C1 O1 123.3(2) . . ? O2 C1 C2 121.0(2) . . ? O1 C1 C2 115.7(2) . . ? C1 C2 C3 114.1(2) . . ? C3 C3 C2 112.0(2) 2_465 . ? _refine_diff_density_max 0.303 _refine_diff_density_min -0.440 _refine_diff_density_rms 0.062 #===END #COMPOUND 3 data_shel93_COMPOUND_3 _database_code_CSD 152780 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C12 H26 Cu3 O14' _chemical_formula_weight 584.96 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cu' 'Cu' 0.3201 1.2651 '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 5.727(3) _cell_length_b 7.455(4) _cell_length_c 12.648(6) _cell_angle_alpha 97.70(1) _cell_angle_beta 104.16(1) _cell_angle_gamma 106.43(1) _cell_volume 490.1(4) _cell_formula_units_Z 1 _cell_measurement_temperature 298 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5.3 _cell_measurement_theta_max 10.5 _exptl_crystal_description 'parallelipiped' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.982 _exptl_crystal_density_method ? _exptl_crystal_F_000 297 _exptl_absorpt_coefficient_mu 3.295 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Crystal Logic Dual Goniometer diffractometer' _diffrn_measurement_method 'theta-2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.8 _diffrn_reflns_number 1913 _diffrn_reflns_av_R_equivalents 0.0146 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1722 _reflns_number_observed 1442 _reflns_observed_criterion >2sigma(I) _computing_data_collection ; Program COLLECT (UCLA Crystallographic package, C.E.Strouse, 1994) ; _computing_cell_refinement ; Program LEAST (UCLA Crystallographic package, C.E.Strouse, 1994) ; _computing_data_reduction ; Program REDUCE (UCLA Crystallographic package, C.E.Strouse, 1994) ; _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+1.2606P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1722 _refine_ls_number_parameters 184 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0477 _refine_ls_R_factor_obs 0.0366 _refine_ls_wR_factor_all 0.1006 _refine_ls_wR_factor_obs 0.0896 _refine_ls_goodness_of_fit_all 1.112 _refine_ls_goodness_of_fit_obs 1.095 _refine_ls_restrained_S_all 1.112 _refine_ls_restrained_S_obs 1.095 _refine_ls_shift/esd_max 0.034 _refine_ls_shift/esd_mean 0.002 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.0000 0.5000 0.5000 0.0164(2) Uani 1 d S . Cu2 Cu 0.42239(9) 0.35227(7) 0.39455(4) 0.0183(2) Uani 1 d . . O5 O 0.3017(6) 0.4062(4) 0.5245(2) 0.0178(6) Uani 1 d . . OW1 O 0.1608(7) 0.1051(5) 0.3221(3) 0.0275(8) Uani 1 d . . OW2 O 0.2958(6) 0.7893(5) 0.5003(3) 0.0221(7) Uani 1 d . . O1 O 0.0404(6) 0.5687(5) 0.6579(2) 0.0238(7) Uani 1 d . . O2 O 0.5392(6) 0.3362(5) 0.2625(3) 0.0290(8) Uani 1 d . . C1 C 0.2335(9) 0.6235(6) 0.7406(4) 0.0214(9) Uani 1 d . . C2 C 0.1873(9) 0.6424(8) 0.8538(4) 0.0256(10) Uani 1 d . . C3 C 0.4235(10) 0.7222(8) 0.9547(4) 0.0264(10) Uani 1 d . . C4 C 0.3576(9) 0.7351(8) 1.0642(4) 0.0262(10) Uani 1 d . . C5 C 0.5943(9) 0.8145(8) 1.1654(4) 0.0261(10) Uani 1 d . . C6 C 0.5486(8) 0.8408(6) 1.2776(4) 0.0196(9) Uani 1 d . . O3 O 0.3251(6) 0.8017(5) 1.2838(3) 0.0288(8) Uani 1 d . . O4 O 0.7441(6) 0.9015(5) 1.3644(3) 0.0269(7) Uani 1 d . . HO5 H 0.2792(93) 0.3313(71) 0.5561(41) 0.012 Uiso 1 d . . HW1A H 0.0603(116) 0.0651(79) 0.3536(46) 0.026(15) Uiso 1 d . . HW1B H 0.2094(131) 0.0306(99) 0.2978(56) 0.044(21) Uiso 1 d . . HW2A H 0.2842(90) 0.8894(76) 0.5312(40) 0.014(12) Uiso 1 d . . HW2B H 0.3207(101) 0.7884(76) 0.4483(47) 0.018(15) Uiso 1 d . . H2A H 0.0911(98) 0.7106(73) 0.8514(41) 0.018(13) Uiso 1 d . . H2B H 0.0821(115) 0.5160(88) 0.8532(47) 0.038(15) Uiso 1 d . . H3A H 0.5268(98) 0.6480(72) 0.9569(40) 0.019(12) Uiso 1 d . . H3B H 0.5275(112) 0.8378(87) 0.9515(46) 0.034(15) Uiso 1 d . . H4A H 0.2506(125) 0.8257(91) 1.0650(51) 0.047(17) Uiso 1 d . . H4B H 0.2767(101) 0.6215(82) 1.0739(43) 0.027(14) Uiso 1 d . . H5A H 0.6852(109) 0.9252(83) 1.1596(43) 0.029(14) Uiso 1 d . . H5B H 0.6939(118) 0.7377(89) 1.1650(49) 0.040(16) Uiso 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 Cu1 0.0132(4) 0.0220(4) 0.0118(4) 0.0009(3) 0.0028(3) 0.0042(3) Cu2 0.0145(3) 0.0213(3) 0.0139(3) -0.0005(2) 0.0037(2) 0.0004(2) O5 0.016(2) 0.018(2) 0.019(2) 0.0060(12) 0.0060(12) 0.0035(13) OW1 0.019(2) 0.025(2) 0.032(2) -0.004(2) 0.010(2) 0.0006(15) OW2 0.028(2) 0.020(2) 0.018(2) 0.0043(14) 0.0096(15) 0.0071(14) O1 0.022(2) 0.036(2) 0.0123(14) 0.0013(13) 0.0049(13) 0.0091(14) O2 0.024(2) 0.041(2) 0.014(2) 0.0004(14) 0.0060(13) 0.0009(15) C1 0.023(2) 0.017(2) 0.017(2) 0.003(2) 0.004(2) -0.002(2) C2 0.025(2) 0.032(3) 0.015(2) 0.003(2) 0.006(2) 0.003(2) C3 0.025(2) 0.030(3) 0.022(2) 0.005(2) 0.006(2) 0.006(2) C4 0.026(2) 0.033(3) 0.015(2) 0.003(2) 0.004(2) 0.004(2) C5 0.025(2) 0.034(3) 0.017(2) 0.003(2) 0.006(2) 0.006(2) C6 0.024(2) 0.016(2) 0.019(2) 0.003(2) 0.006(2) 0.007(2) O3 0.024(2) 0.037(2) 0.023(2) 0.0007(14) 0.0094(14) 0.0064(15) O4 0.024(2) 0.032(2) 0.017(2) 0.0015(13) 0.0033(13) 0.0007(14) _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 Cu1 O1 1.933(3) . ? Cu1 O1 1.933(3) 2_566 ? Cu1 O5 2.013(3) 2_566 ? Cu1 O5 2.013(3) . ? Cu1 OW2 2.334(3) 2_566 ? Cu1 OW2 2.334(3) . ? Cu1 Cu2 3.0532(15) 1_455 ? Cu1 Cu2 3.0532(15) 2_666 ? Cu2 O2 1.947(3) . ? Cu2 OW1 1.948(4) . ? Cu2 O5 1.969(3) . ? Cu2 O5 1.972(3) 2_666 ? Cu2 OW2 2.403(4) 2_666 ? Cu2 Cu2 2.986(2) 2_666 ? Cu2 Cu1 3.0532(15) 1_655 ? O5 Cu2 1.972(3) 2_666 ? OW2 Cu2 2.403(3) 2_666 ? O1 C1 1.244(5) . ? O2 C1 1.262(6) 2_666 ? C1 O2 1.262(6) 2_666 ? C1 C2 1.514(6) . ? C2 C3 1.520(7) . ? C3 C4 1.519(6) . ? C4 C5 1.523(6) . ? C5 C6 1.502(6) . ? C6 O3 1.255(6) . ? C6 O4 1.282(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 O1 180.000(1) . 2_566 ? O1 Cu1 O5 86.47(13) . 2_566 ? O1 Cu1 O5 93.53(13) 2_566 2_566 ? O1 Cu1 O5 93.53(13) . . ? O1 Cu1 O5 86.47(13) 2_566 . ? O5 Cu1 O5 179.999(1) 2_566 . ? O1 Cu1 OW2 86.35(14) . 2_566 ? O1 Cu1 OW2 93.65(14) 2_566 2_566 ? O5 Cu1 OW2 84.10(13) 2_566 2_566 ? O5 Cu1 OW2 95.90(13) . 2_566 ? O1 Cu1 OW2 93.65(14) . . ? O1 Cu1 OW2 86.35(14) 2_566 . ? O5 Cu1 OW2 95.90(13) 2_566 . ? O5 Cu1 OW2 84.10(13) . . ? OW2 Cu1 OW2 180.0 2_566 . ? O1 Cu1 Cu2 103.36(10) . 1_455 ? O1 Cu1 Cu2 76.64(10) 2_566 1_455 ? O5 Cu1 Cu2 39.51(9) 2_566 1_455 ? O5 Cu1 Cu2 140.49(9) . 1_455 ? OW2 Cu1 Cu2 50.88(9) 2_566 1_455 ? OW2 Cu1 Cu2 129.12(9) . 1_455 ? O1 Cu1 Cu2 76.64(10) . 2_666 ? O1 Cu1 Cu2 103.36(10) 2_566 2_666 ? O5 Cu1 Cu2 140.49(9) 2_566 2_666 ? O5 Cu1 Cu2 39.51(9) . 2_666 ? OW2 Cu1 Cu2 129.12(9) 2_566 2_666 ? OW2 Cu1 Cu2 50.88(9) . 2_666 ? Cu2 Cu1 Cu2 180.0 1_455 2_666 ? O2 Cu2 OW1 87.6(2) . . ? O2 Cu2 O5 171.42(14) . . ? OW1 Cu2 O5 97.5(2) . . ? O2 Cu2 O5 93.85(14) . 2_666 ? OW1 Cu2 O5 176.05(14) . 2_666 ? O5 Cu2 O5 81.51(13) . 2_666 ? O2 Cu2 OW2 96.55(14) . 2_666 ? OW1 Cu2 OW2 93.05(14) . 2_666 ? O5 Cu2 OW2 90.08(13) . 2_666 ? O5 Cu2 OW2 83.14(13) 2_666 2_666 ? O2 Cu2 Cu2 134.15(11) . 2_666 ? OW1 Cu2 Cu2 138.17(13) . 2_666 ? O5 Cu2 Cu2 40.80(9) . 2_666 ? O5 Cu2 Cu2 40.71(9) 2_666 2_666 ? OW2 Cu2 Cu2 85.53(10) 2_666 2_666 ? O2 Cu2 Cu1 78.76(10) . 1_655 ? OW1 Cu2 Cu1 136.60(12) . 1_655 ? O5 Cu2 Cu1 101.81(9) . 1_655 ? O5 Cu2 Cu1 40.48(9) 2_666 1_655 ? OW2 Cu2 Cu1 48.89(8) 2_666 1_655 ? Cu2 Cu2 Cu1 68.44(2) 2_666 1_655 ? Cu2 O5 Cu2 98.49(13) . 2_666 ? Cu2 O5 Cu1 117.1(2) . . ? Cu2 O5 Cu1 100.01(14) 2_666 . ? Cu1 OW2 Cu2 80.23(11) . 2_666 ? C1 O1 Cu1 131.3(3) . . ? C1 O2 Cu2 127.4(3) 2_666 . ? O1 C1 O2 125.6(4) . 2_666 ? O1 C1 C2 116.2(4) . . ? O2 C1 C2 118.2(4) 2_666 . ? C1 C2 C3 116.2(4) . . ? C4 C3 C2 112.3(4) . . ? C3 C4 C5 112.3(4) . . ? C6 C5 C4 116.3(4) . . ? O3 C6 O4 122.4(4) . . ? O3 C6 C5 120.0(4) . . ? O4 C6 C5 117.6(4) . . ? _refine_diff_density_max 0.655 _refine_diff_density_min -0.822 _refine_diff_density_rms 0.122 #===END #COMPOUND 4 data_shel93_COMPOUND_4 _database_code_CSD 152781 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C6 H16 Ni O8' _chemical_formula_weight 274.90 _chemical_melting_point ? _chemical_compound_source ? 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' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y+1/2, z+1/2' '-x, -y, -z' '-x, y-1/2, -z-1/2' _cell_length_a 4.781(1) _cell_length_b 9.780(2) _cell_length_c 11.648(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.927(8) _cell_angle_gamma 90.00 _cell_volume 538.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 298 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 27 _exptl_crystal_description 'parallelipiped' _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.697 _exptl_crystal_density_method ? _exptl_crystal_F_000 288 _exptl_absorpt_coefficient_mu 2.878 _exptl_absorpt_correction_type 'psi-scan empirical' _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'P21 Nicolet upgraded by Crystal Logic' _diffrn_measurement_method theta-2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.5 _diffrn_reflns_number 1027 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_sigmaI/netI 0.0425 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 5.94 _diffrn_reflns_theta_max 65.00 _reflns_number_total 911 _reflns_number_observed 827 _reflns_observed_criterion >2sigma(I) _computing_data_collection ; Program COLLECT (UCLA Crystallographic package, C.E.Strouse, 1994) ; _computing_cell_refinement ; Program LEAST (UCLA Crystallographic package, C.E.Strouse, 1994) ; _computing_data_reduction ; Program REDUCE (UCLA Crystallographic package, C.E.Strouse, 1994) ; _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0955P)^2^+0.2591P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 911 _refine_ls_number_parameters 102 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0512 _refine_ls_R_factor_obs 0.0476 _refine_ls_wR_factor_all 0.1319 _refine_ls_wR_factor_obs 0.1271 _refine_ls_goodness_of_fit_all 1.080 _refine_ls_goodness_of_fit_obs 1.099 _refine_ls_restrained_S_all 1.080 _refine_ls_restrained_S_obs 1.099 _refine_ls_shift/esd_max 0.011 _refine_ls_shift/esd_mean 0.002 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni Ni 0.0000 0.5000 0.5000 0.0201(3) Uani 1 d S . OW1 O -0.1957(5) 0.3228(2) 0.5398(2) 0.0279(5) Uani 1 d . . OW2 O 0.2547(5) 0.3829(2) 0.4105(2) 0.0291(5) Uani 1 d . . O1 O 0.2998(5) 0.4800(2) 0.6466(2) 0.0284(5) Uani 1 d . . O2 O 0.1195(5) 0.3172(2) 0.7466(2) 0.0369(6) Uani 1 d . . C1 C 0.2964(6) 0.4098(3) 0.7382(2) 0.0251(6) Uani 1 d . . C2 C 0.5170(7) 0.4423(4) 0.8413(3) 0.0344(7) Uani 1 d . . C3 C 0.3893(7) 0.4760(4) 0.9506(3) 0.0291(7) Uani 1 d . . HW1A H -0.1191(80) 0.3073(37) 0.6174(32) 0.035(9) Uiso 1 d . . HW1B H -0.3567(77) 0.3287(36) 0.5400(28) 0.022(8) Uiso 1 d . . HW2A H 0.3670(76) 0.4232(38) 0.3829(30) 0.028(9) Uiso 1 d . . HW2B H 0.1933(96) 0.3218(52) 0.3683(38) 0.052(13) Uiso 1 d . . H2A H 0.6474(89) 0.3510(48) 0.8690(35) 0.053(11) Uiso 1 d . . H2B H 0.6080(99) 0.5172(41) 0.8192(38) 0.042(12) Uiso 1 d . . H3A H 0.2859(73) 0.4084(36) 0.9796(30) 0.031(9) Uiso 1 d . . H3B H 0.2485(93) 0.5506(50) 0.9318(36) 0.050(11) Uiso 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 Ni 0.0236(5) 0.0168(5) 0.0190(5) 0.0009(2) 0.0007(3) -0.0017(2) OW1 0.0291(12) 0.0239(11) 0.0291(12) 0.0021(8) -0.0008(9) -0.0050(8) OW2 0.0300(11) 0.0261(12) 0.0319(11) -0.0056(9) 0.0072(9) -0.0061(9) O1 0.0297(11) 0.0327(11) 0.0216(11) 0.0050(8) 0.0006(9) -0.0051(8) O2 0.0414(12) 0.0365(13) 0.0296(12) 0.0117(9) -0.0043(9) -0.0115(9) C1 0.0274(14) 0.0263(14) 0.0212(13) -0.0002(11) 0.0028(10) 0.0040(11) C2 0.033(2) 0.046(2) 0.0227(15) 0.0000(13) 0.0013(12) -0.0054(14) C3 0.033(2) 0.0283(15) 0.024(2) -0.0020(13) -0.0003(14) 0.0005(14) _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 Ni OW1 2.056(2) 3_566 ? Ni OW1 2.056(2) . ? Ni O1 2.061(2) 3_566 ? Ni O1 2.061(2) . ? Ni OW2 2.067(2) . ? Ni OW2 2.067(2) 3_566 ? O1 C1 1.271(4) . ? O2 C1 1.253(4) . ? C1 C2 1.503(4) . ? C2 C3 1.532(4) . ? C3 C3 1.512(7) 3_667 ? 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 OW1 Ni OW1 180.0 3_566 . ? OW1 Ni O1 90.90(9) 3_566 3_566 ? OW1 Ni O1 89.10(9) . 3_566 ? OW1 Ni O1 89.10(9) 3_566 . ? OW1 Ni O1 90.90(9) . . ? O1 Ni O1 180.0 3_566 . ? OW1 Ni OW2 91.67(9) 3_566 . ? OW1 Ni OW2 88.33(9) . . ? O1 Ni OW2 91.33(9) 3_566 . ? O1 Ni OW2 88.66(9) . . ? OW1 Ni OW2 88.34(9) 3_566 3_566 ? OW1 Ni OW2 91.66(9) . 3_566 ? O1 Ni OW2 88.67(9) 3_566 3_566 ? O1 Ni OW2 91.33(9) . 3_566 ? OW2 Ni OW2 180.0 . 3_566 ? C1 O1 Ni 130.5(2) . . ? O2 C1 O1 123.5(3) . . ? O2 C1 C2 119.3(3) . . ? O1 C1 C2 117.2(3) . . ? C1 C2 C3 112.9(3) . . ? C3 C3 C2 112.2(3) 3_667 . ? _refine_diff_density_max 1.148 _refine_diff_density_min -0.778 _refine_diff_density_rms 0.115 #===END