# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Carine Livage-Sahut' _publ_contact_author_email CARINE.LIVAGE@UVSQ.FR _publ_section_title ; Bulk homochirality of a 3-D inorganic framework: Ligand control of inorganic network chirality ; loop_ _publ_author_name 'Carine Livage-Sahut' 'Gerard Ferey' 'Nathalie Guillou' 'Jerome Marrot' 'Philip Pattison' 'Pierre Rabu' #==================================================================== data_4 _database_code_depnum_ccdc_archive 'CCDC 692198' _audit_creation_method SHELXL-97 _chemical_name_systematic ; diaqua tri R-2-methylglutarate di 3-methylglutarate cobalt (II) pentahydrate ; _chemical_name_common ;diaqua tri R-2-methylglutarate di 3-methylglutarate cobalt (ii) pentahydrate ; _chemical_melting_point ? _chemical_formula_moiety 'C30 H54 Co5 O27' _chemical_formula_sum 'C30 H54 Co5 O27' _chemical_formula_weight 1141.38 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M P4(1)32 _symmetry_space_group_name_Hall 'P 4bd 2ab 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' 'y+3/4, x+1/4, -z+1/4' '-y+3/4, -x+3/4, -z+3/4' 'y+1/4, -x+1/4, z+3/4' '-y+1/4, x+3/4, z+1/4' 'x+3/4, z+1/4, -y+1/4' '-x+1/4, z+3/4, y+1/4' '-x+3/4, -z+3/4, -y+3/4' 'x+1/4, -z+1/4, y+3/4' 'z+3/4, y+1/4, -x+1/4' 'z+1/4, -y+1/4, x+3/4' '-z+1/4, y+3/4, x+1/4' '-z+3/4, -y+3/4, -x+3/4' _cell_length_a 16.72680(10) _cell_length_b 16.72680(10) _cell_length_c 16.72680(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4679.92(5) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6855 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 25.31 _exptl_crystal_description parallelepiped _exptl_crystal_colour pink _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.620 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2340 _exptl_absorpt_coefficient_mu 1.821 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8389 _exptl_absorpt_correction_T_max 0.8986 _exptl_absorpt_process_details 'SADABS (Sheldrick, V2.10)' _chemical_absolute_configuration right-L _exptl_special_details ; 'Blessing, Acta Cryst. (1995) A51, 33-38' ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 512x512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 98330 _diffrn_reflns_av_R_equivalents 0.0721 _diffrn_reflns_av_sigmaI/netI 0.0173 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 30.03 _reflns_number_total 2302 _reflns_number_gt 1965 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0871P)^2^+1.8179P] 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 SHELXL _refine_ls_extinction_coef 0.0113(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(4) _refine_ls_number_reflns 2302 _refine_ls_number_parameters 129 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0679 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1515 _refine_ls_wR_factor_gt 0.1285 _refine_ls_goodness_of_fit_ref 1.191 _refine_ls_restrained_S_all 1.191 _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 Co1 Co -0.05853(3) 0.44147(3) 0.05853(3) 0.0388(2) Uani 1 3 d S . . Co2 Co -0.1250 0.56780(3) 0.18220(3) 0.0420(2) Uani 1 2 d S . . O3 O 0.06497(16) 0.43132(17) 0.07019(18) 0.0498(6) Uani 1 1 d . . . O1 O -0.06808(17) 0.45383(16) 0.18413(16) 0.0467(6) Uani 1 1 d . . . O2 O 0.0197(2) 0.3642(2) 0.22694(19) 0.0583(8) Uani 1 1 d . . . O4 O 0.1161(3) 0.5118(3) -0.0160(3) 0.0579(11) Uani 0.67 1 d P . . C1 C -0.0302(3) 0.4180(3) 0.2392(2) 0.0512(9) Uani 1 1 d . . . C2 C -0.0491(4) 0.4384(4) 0.3248(3) 0.0799(18) Uani 1 1 d . . . H2 H -0.0561 0.4964 0.3294 0.096 Uiso 1 1 calc R . . C3 C -0.1250 0.3975(3) 0.3525(3) 0.096(4) Uani 1 2 d S . . H3A H -0.1193 0.3405 0.3439 0.115 Uiso 0.50 1 calc PR . . H3B H -0.1307 0.4061 0.4095 0.115 Uiso 0.50 1 calc PR . . C4 C 0.0065(17) 0.4161(15) 0.3729(14) 0.180(13) Uani 0.50 1 d P . . HM1A H 0.0473 0.4563 0.3748 0.270 Uiso 0.50 1 calc PR . . HM1B H 0.0291 0.3667 0.3543 0.270 Uiso 0.50 1 calc PR . . HM1C H -0.0155 0.4086 0.4253 0.270 Uiso 0.50 1 calc PR . . C5 C 0.1165(6) 0.4758(9) 0.0405(11) 0.142(7) Uani 0.67 1 d P . . C6 C 0.2035(6) 0.4581(10) 0.0488(10) 0.123(5) Uani 0.67 1 d P . . H6A H 0.2314 0.4798 0.0028 0.147 Uiso 0.67 1 calc PR . . H6B H 0.2109 0.4006 0.0482 0.147 Uiso 0.67 1 calc PR . . C7 C 0.2418(7) 0.4918(7) 0.1250 0.106(6) Uani 0.67 2 d SP . . C8 C 0.216(4) 0.563(3) 0.091(5) 0.25(4) Uani 0.33 1 d P . . OW1 O 0.0950(9) 0.5592(8) 0.0506(14) 0.120(7) Uani 0.33 1 d P . . OW2 O 0.193(4) 0.554(4) 0.116(5) 0.32(4) Uiso 0.33 1 d P . . OW3 O 0.189(5) 0.579(5) -0.108(6) 0.20(3) Uiso 0.17 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0388(2) 0.0388(2) 0.0388(2) -0.00420(19) -0.00420(19) 0.00420(19) Co2 0.0435(4) 0.0413(3) 0.0413(3) -0.0094(3) 0.00052(18) 0.00052(18) O3 0.0405(13) 0.0500(14) 0.0590(15) 0.0036(12) -0.0017(12) 0.0009(11) O1 0.0544(15) 0.0463(13) 0.0392(12) -0.0056(10) -0.0011(11) 0.0101(11) O2 0.066(2) 0.0613(18) 0.0476(15) 0.0000(13) 0.0009(13) 0.0233(15) O4 0.053(3) 0.061(3) 0.060(3) 0.011(2) 0.014(2) -0.008(2) C1 0.058(2) 0.054(2) 0.0412(18) -0.0024(16) 0.0000(16) 0.0151(17) C2 0.120(5) 0.082(3) 0.038(2) -0.002(2) -0.003(2) 0.049(3) C3 0.154(10) 0.067(3) 0.067(3) 0.019(4) 0.040(4) 0.040(4) C4 0.26(3) 0.17(2) 0.113(16) -0.004(14) 0.06(2) 0.09(2) C5 0.056(5) 0.148(12) 0.223(17) 0.122(12) -0.024(7) -0.026(6) C6 0.050(5) 0.155(11) 0.164(13) 0.070(10) 0.007(6) -0.007(6) C7 0.082(6) 0.082(6) 0.153(17) 0.015(8) -0.015(8) -0.019(8) C8 0.20(5) 0.14(3) 0.42(11) 0.18(5) 0.02(5) -0.03(3) OW1 0.076(8) 0.058(7) 0.23(2) 0.056(10) -0.049(10) -0.031(6) _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 Co1 O3 2.082(3) 11_455 ? Co1 O3 2.082(3) . ? Co1 O3 2.082(3) 8 ? Co1 O1 2.117(3) 8 ? Co1 O1 2.117(3) 11_455 ? Co1 O1 2.117(3) . ? Co2 O2 2.039(3) 8 ? Co2 O2 2.039(3) 21_455 ? Co2 O3 2.109(3) 8 ? Co2 O3 2.109(3) 21_455 ? Co2 O1 2.131(3) 19_455 ? Co2 O1 2.131(3) . ? O3 C5 1.243(10) . ? O3 Co2 2.109(3) 11_455 ? O1 C1 1.268(5) . ? O2 C1 1.244(5) . ? O2 Co2 2.039(3) 11_455 ? O4 C5 1.120(13) . ? O4 OW1 1.41(2) . ? C1 C2 1.506(6) . ? C2 C4 1.28(3) . ? C2 C3 1.514(8) . ? C2 H2 0.9800 . ? C3 C2 1.514(8) 19_455 ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 HM1A 0.9600 . ? C4 HM1B 0.9600 . ? C4 HM1C 0.9600 . ? C5 OW1 1.45(2) . ? C5 C6 1.492(15) . ? C6 C7 1.534(18) . ? C6 C8 1.90(8) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 OW2 1.33(7) 13_455 ? C7 OW2 1.33(7) . ? C7 C8 1.39(4) 13_455 ? C7 C8 1.39(4) . ? C7 C6 1.534(18) 13_455 ? C8 OW2 0.59(11) . ? OW3 OW3 0.72(17) 14_554 ? 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 O3 Co1 O3 99.57(10) 11_455 . ? O3 Co1 O3 99.57(10) 11_455 8 ? O3 Co1 O3 99.57(10) . 8 ? O3 Co1 O1 79.35(11) 11_455 8 ? O3 Co1 O1 171.00(11) . 8 ? O3 Co1 O1 89.42(11) 8 8 ? O3 Co1 O1 89.42(11) 11_455 11_455 ? O3 Co1 O1 79.35(11) . 11_455 ? O3 Co1 O1 171.00(11) 8 11_455 ? O1 Co1 O1 91.69(12) 8 11_455 ? O3 Co1 O1 171.00(11) 11_455 . ? O3 Co1 O1 89.42(11) . . ? O3 Co1 O1 79.35(11) 8 . ? O1 Co1 O1 91.69(12) 8 . ? O1 Co1 O1 91.69(12) 11_455 . ? O2 Co2 O2 178.9(2) 8 21_455 ? O2 Co2 O3 90.69(12) 8 8 ? O2 Co2 O3 90.00(13) 21_455 8 ? O2 Co2 O3 90.00(13) 8 21_455 ? O2 Co2 O3 90.69(12) 21_455 21_455 ? O3 Co2 O3 103.26(15) 8 21_455 ? O2 Co2 O1 87.75(12) 8 19_455 ? O2 Co2 O1 91.53(12) 21_455 19_455 ? O3 Co2 O1 177.71(11) 8 19_455 ? O3 Co2 O1 78.42(10) 21_455 19_455 ? O2 Co2 O1 91.53(12) 8 . ? O2 Co2 O1 87.75(12) 21_455 . ? O3 Co2 O1 78.42(10) 8 . ? O3 Co2 O1 177.71(11) 21_455 . ? O1 Co2 O1 99.93(15) 19_455 . ? C5 O3 Co1 127.0(5) . . ? C5 O3 Co2 134.2(6) . 11_455 ? Co1 O3 Co2 97.84(11) . 11_455 ? C1 O1 Co1 129.5(2) . . ? C1 O1 Co2 131.1(3) . . ? Co1 O1 Co2 96.09(11) . . ? C1 O2 Co2 132.6(3) . 11_455 ? C5 O4 OW1 68.8(12) . . ? O2 C1 O1 123.9(4) . . ? O2 C1 C2 117.5(4) . . ? O1 C1 C2 118.5(4) . . ? C4 C2 C1 112.2(10) . . ? C4 C2 C3 106.5(13) . . ? C1 C2 C3 111.4(5) . . ? C4 C2 H2 108.9 . . ? C1 C2 H2 108.9 . . ? C3 C2 H2 108.9 . . ? C2 C3 C2 115.3(6) 19_455 . ? C2 C3 H3A 108.5 19_455 . ? C2 C3 H3A 108.5 . . ? C2 C3 H3B 108.5 19_455 . ? C2 C3 H3B 108.5 . . ? H3A C3 H3B 107.5 . . ? C2 C4 HM1A 109.5 . . ? C2 C4 HM1B 109.5 . . ? HM1A C4 HM1B 109.5 . . ? C2 C4 HM1C 109.5 . . ? HM1A C4 HM1C 109.5 . . ? HM1B C4 HM1C 109.5 . . ? O4 C5 O3 130.9(12) . . ? O4 C5 OW1 65.2(11) . . ? O3 C5 OW1 110.9(13) . . ? O4 C5 C6 101.0(10) . . ? O3 C5 C6 121.4(10) . . ? OW1 C5 C6 115.0(12) . . ? C5 C6 C7 114.3(14) . . ? C5 C6 C8 88(2) . . ? C7 C6 C8 46(2) . . ? C5 C6 H6A 108.7 . . ? C7 C6 H6A 108.7 . . ? C8 C6 H6A 84.0 . . ? C5 C6 H6B 108.7 . . ? C7 C6 H6B 108.7 . . ? C8 C6 H6B 154.9 . . ? H6A C6 H6B 107.6 . . ? OW2 C7 OW2 167(7) 13_455 . ? OW2 C7 C8 25(5) 13_455 13_455 ? OW2 C7 C8 145(5) . 13_455 ? OW2 C7 C8 145(5) 13_455 . ? OW2 C7 C8 25(5) . . ? C8 C7 C8 135(5) 13_455 . ? OW2 C7 C6 101(3) 13_455 . ? OW2 C7 C6 86(4) . . ? C8 C7 C6 126(3) 13_455 . ? C8 C7 C6 81(4) . . ? OW2 C7 C6 86(4) 13_455 13_455 ? OW2 C7 C6 101(3) . 13_455 ? C8 C7 C6 81(4) 13_455 13_455 ? C8 C7 C6 126(3) . 13_455 ? C6 C7 C6 112.5(13) . 13_455 ? OW2 C8 C7 72(10) . . ? OW2 C8 C6 87(10) . . ? C7 C8 C6 53(2) . . ? O4 OW1 C5 46.1(9) . . ? C8 OW2 C7 83(10) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.802 _refine_diff_density_min -0.784 _refine_diff_density_rms 0.297 #===END #==================================================================== data_2 _database_code_depnum_ccdc_archive 'CCDC 692199' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Diaqua penta 2-methylglutarate cobalt (II) hydrate ; _chemical_name_common 'Diaqua penta 2-methylglutarate cobalt (ii) hydrate' _chemical_melting_point ? _chemical_formula_moiety 'C30 H52 Co5 O26' _chemical_formula_sum 'C30 H52 Co5 O26' _chemical_formula_weight 1123.37 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M P4(1)32 _symmetry_space_group_name_Hall 'P 4bd 2ab 3' _chemical_absolute_configuration '80% right 20% left' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' 'z, x, y' 'y, z, x' '-z+1/2, -x, y+1/2' '-y, z+1/2, -x+1/2' 'z+1/2, -x+1/2, -y' '-y+1/2, -z, x+1/2' '-z, x+1/2, -y+1/2' 'y+1/2, -z+1/2, -x' '-y+3/4, -x+3/4, -z+3/4' 'y+3/4, x+1/4, -z+1/4' 'y+1/4, -x+1/4, z+3/4' '-y+1/4, x+3/4, z+1/4' '-x+3/4, -z+3/4, -y+3/4' '-z+3/4, -y+3/4, -x+3/4' 'x+3/4, z+1/4, -y+1/4' '-z+1/4, y+3/4, x+1/4' 'x+1/4, -z+1/4, y+3/4' 'z+3/4, y+1/4, -x+1/4' '-x+1/4, z+3/4, y+1/4' 'z+1/4, -y+1/4, x+3/4' _cell_length_a 16.6130(1) _cell_length_b 16.6130(1) _cell_length_c 16.6130(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4585.05(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1561 _cell_measurement_theta_min 1.71 _cell_measurement_theta_max 25.87 _exptl_crystal_description polyhedral _exptl_crystal_colour pink _exptl_crystal_size_max 0.01 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.627 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2300 _exptl_absorpt_coefficient_mu 1.856 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9817 _exptl_absorpt_correction_T_max 0.9817 _exptl_absorpt_process_details 'SADABS (Sheldrick, V2.10)' _exptl_special_details ; 'Blessing, Acta Cryst. (1995) A51, 33-38' ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.70000 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'BM01 at ESFR, Grenoble France' _diffrn_radiation_monochromator Si(111) _diffrn_measurement_device_type MAR345 _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 21639 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_sigmaI/netI 0.0146 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.87 _reflns_number_total 1561 _reflns_number_gt 1557 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'CrysAlis software package' _computing_structure_solution SIR-92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0650P)^2^+12.7165P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.20(5) _refine_ls_number_reflns 1561 _refine_ls_number_parameters 123 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0378 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.1240 _refine_ls_wR_factor_gt 0.1186 _refine_ls_goodness_of_fit_ref 1.184 _refine_ls_restrained_S_all 1.184 _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 Co1 Co 0.19647(3) 0.19647(3) 0.19647(3) 0.0143(3) Uani 1 3 d S . . Co2 Co 0.32441(4) 0.1250 0.07441(4) 0.0159(2) Uani 1 2 d S . . O1 O 0.21110(17) 0.18436(18) 0.07028(18) 0.0175(6) Uani 1 1 d . . . O2 O 0.1229(2) 0.2744(2) 0.02424(19) 0.0233(7) Uani 1 1 d . . . O3 O 0.18267(19) 0.18752(18) 0.32056(18) 0.0204(6) Uani 1 1 d . . . O4 O 0.2706(3) 0.2693(4) 0.3696(4) 0.0352(13) Uani 0.67 1 d P . . C1 C 0.1768(3) 0.2229(3) 0.0135(2) 0.0171(8) Uani 1 1 d . . . C2 C 0.1977(3) 0.2020(3) -0.0721(3) 0.0241(9) Uani 1 1 d . . . H2 H 0.2558 0.1926 -0.0761 0.029 Uiso 1 1 calc R . . C3 C 0.1524(3) 0.1250 -0.0976(3) 0.0270(15) Uani 1 2 d S . . H3A H 0.1608 0.1166 -0.1547 0.032 Uiso 0.50 1 calc PR . . H3B H 0.0953 0.1334 -0.0892 0.032 Uiso 0.50 1 calc PR . . C4 C 0.1742(7) 0.2711(7) -0.1289(6) 0.037(3) Uani 0.50 1 d P . . H4A H 0.1168 0.2781 -0.1279 0.055 Uiso 0.50 1 calc PR . . H4B H 0.1911 0.2584 -0.1827 0.055 Uiso 0.50 1 calc PR . . H4C H 0.1999 0.3198 -0.1116 0.055 Uiso 0.50 1 calc PR . . C5 C 0.2032(9) 0.2381(8) 0.3705(6) 0.078(5) Uani 0.67 1 d P . . C6 C 0.2043(6) 0.2145(4) 0.4599(4) 0.059(3) Uani 0.67 1 d P . . H6 H 0.2051 0.1557 0.4650 0.070 Uiso 0.67 1 calc PR . . C7 C 0.1250(6) 0.2487(4) 0.4987(4) 0.057(4) Uani 0.67 2 d SPR . . H7A H 0.1231 0.3064 0.4898 0.069 Uiso 0.33 1 calc PR . . H7B H 0.1269 0.2398 0.5564 0.069 Uiso 0.33 1 calc PR . . C8 C 0.2703(6) 0.2481(4) 0.5027(4) 0.077(8) Uani 0.33 1 d PR . . H8A H 0.3188 0.2404 0.4723 0.116 Uiso 0.33 1 calc PR . . H8B H 0.2754 0.2219 0.5540 0.116 Uiso 0.33 1 calc PR . . H8C H 0.2614 0.3046 0.5107 0.116 Uiso 0.33 1 calc PR . . OW1 O 0.2007(6) 0.3159(4) 0.3494(4) 0.071(6) Uani 0.33 1 d PR . . OW2 O 0.3807(6) 0.4478(4) 0.6607(4) 0.077(12) Uani 0.17 1 d PR . . OW3 O 0.3456(6) 0.3507(4) 0.4320(4) 0.119(18) Uiso 0.17 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0143(3) 0.0143(3) 0.0143(3) 0.0016(2) 0.0016(2) 0.0016(2) Co2 0.0153(3) 0.0172(4) 0.0153(3) 0.0001(2) 0.0040(3) -0.0001(2) O1 0.0163(14) 0.0206(15) 0.0157(14) 0.0034(12) 0.0020(11) 0.0045(12) O2 0.0235(16) 0.0264(17) 0.0200(16) -0.0008(12) 0.0001(13) 0.0081(13) O3 0.0240(16) 0.0217(15) 0.0154(14) -0.0017(12) 0.0008(12) -0.0018(13) O4 0.031(3) 0.032(3) 0.043(3) -0.020(3) -0.006(3) -0.013(2) C1 0.0148(19) 0.021(2) 0.016(2) -0.0003(16) 0.0024(15) 0.0018(15) C2 0.023(2) 0.035(3) 0.0140(19) 0.0008(18) 0.0028(17) 0.0100(17) C3 0.0204(18) 0.040(4) 0.0204(18) -0.008(2) -0.006(2) 0.008(2) C4 0.031(5) 0.057(7) 0.023(5) 0.015(5) 0.012(4) 0.016(5) C5 0.123(12) 0.082(8) 0.030(5) -0.022(5) 0.021(6) -0.078(9) C6 0.093(9) 0.061(7) 0.022(4) -0.010(4) 0.005(5) -0.027(6) C7 0.110(13) 0.031(4) 0.031(4) -0.010(5) -0.002(6) 0.002(6) C8 0.081(18) 0.10(2) 0.052(13) -0.010(13) -0.034(13) -0.044(16) OW1 0.142(17) 0.021(6) 0.051(8) -0.011(6) 0.049(9) -0.040(8) OW2 0.036(15) 0.09(2) 0.11(3) 0.07(2) -0.019(17) -0.013(16) _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 Co1 O3 2.079(3) 6 ? Co1 O3 2.079(3) . ? Co1 O3 2.079(3) 5 ? Co1 O1 2.120(3) 5 ? Co1 O1 2.120(3) 6 ? Co1 O1 2.120(3) . ? Co2 O2 2.035(3) 21_554 ? Co2 O2 2.035(3) 6 ? Co2 O3 2.110(3) 5 ? Co2 O3 2.110(3) 15_554 ? Co2 O1 2.126(3) 24_554 ? Co2 O1 2.126(3) . ? O1 C1 1.276(5) . ? O2 C1 1.250(5) . ? O2 Co2 2.035(3) 5 ? O3 C5 1.228(10) . ? O3 Co2 2.110(3) 6 ? O4 C5 1.234(13) . ? O4 OW1 1.436(11) . ? C1 C2 1.505(6) . ? C2 C4 1.535(11) . ? C2 C3 1.543(6) . ? C2 H2 0.9800 . ? C3 C2 1.543(6) 24_554 ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 OW1 1.341(16) . ? C5 C6 1.537(13) . ? C6 C8 1.4212 . ? C6 C7 1.5721 . ? C6 H6 0.9800 . ? C7 C6 1.572(15) 23_545 ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? OW3 OW3 1.035(18) 18 ? OW3 OW3 1.243(17) 17 ? 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 O3 Co1 O3 99.93(11) 6 . ? O3 Co1 O3 99.93(11) 6 5 ? O3 Co1 O3 99.93(11) . 5 ? O3 Co1 O1 78.77(11) 6 5 ? O3 Co1 O1 89.61(12) . 5 ? O3 Co1 O1 170.45(12) 5 5 ? O3 Co1 O1 170.45(12) 6 6 ? O3 Co1 O1 78.77(11) . 6 ? O3 Co1 O1 89.61(12) 5 6 ? O1 Co1 O1 91.74(12) 5 6 ? O3 Co1 O1 89.61(12) 6 . ? O3 Co1 O1 170.45(12) . . ? O3 Co1 O1 78.77(11) 5 . ? O1 Co1 O1 91.74(12) 5 . ? O1 Co1 O1 91.74(12) 6 . ? O2 Co2 O2 179.0(2) 21_554 6 ? O2 Co2 O3 90.12(13) 21_554 5 ? O2 Co2 O3 90.47(14) 6 5 ? O2 Co2 O3 90.47(14) 21_554 15_554 ? O2 Co2 O3 90.12(13) 6 15_554 ? O3 Co2 O3 105.07(16) 5 15_554 ? O2 Co2 O1 91.89(13) 21_554 24_554 ? O2 Co2 O1 87.49(13) 6 24_554 ? O3 Co2 O1 176.36(12) 5 24_554 ? O3 Co2 O1 77.95(11) 15_554 24_554 ? O2 Co2 O1 87.49(13) 21_554 . ? O2 Co2 O1 91.89(13) 6 . ? O3 Co2 O1 77.95(11) 5 . ? O3 Co2 O1 176.36(12) 15_554 . ? O1 Co2 O1 99.09(16) 24_554 . ? C1 O1 Co1 129.3(3) . . ? C1 O1 Co2 130.8(3) . . ? Co1 O1 Co2 96.52(12) . . ? C1 O2 Co2 132.9(3) . 5 ? C5 O3 Co1 126.1(6) . . ? C5 O3 Co2 135.6(6) . 6 ? Co1 O3 Co2 98.27(13) . 6 ? C5 O4 OW1 59.7(9) . . ? O2 C1 O1 123.9(4) . . ? O2 C1 C2 117.3(4) . . ? O1 C1 C2 118.7(4) . . ? C1 C2 C4 110.5(5) . . ? C1 C2 C3 109.7(3) . . ? C4 C2 C3 109.1(6) . . ? C1 C2 H2 109.2 . . ? C4 C2 H2 109.2 . . ? C3 C2 H2 109.2 . . ? C2 C3 C2 114.9(5) . 24_554 ? C2 C3 H3A 108.5 . . ? C2 C3 H3A 108.5 24_554 . ? C2 C3 H3B 108.5 . . ? C2 C3 H3B 108.5 24_554 . ? H3A C3 H3B 107.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O3 C5 O4 122.1(11) . . ? O3 C5 OW1 118.3(11) . . ? O4 C5 OW1 67.7(7) . . ? O3 C5 C6 118.8(9) . . ? O4 C5 C6 96.2(10) . . ? OW1 C5 C6 119.9(8) . . ? C8 C6 C5 113.1(5) . . ? C8 C6 C7 107.5 . . ? C5 C6 C7 107.2(7) . . ? C8 C6 H6 109.7 . . ? C5 C6 H6 109.7 . . ? C7 C6 H6 109.7 . . ? C6 C7 C6 113.9(4) . 23_545 ? C6 C7 H7A 108.8 . . ? C6 C7 H7A 108.8 23_545 . ? C6 C7 H7B 108.8 . . ? C6 C7 H7B 108.8 23_545 . ? H7A C7 H7B 107.7 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C5 OW1 O4 52.6(7) . . ? OW3 OW3 OW3 119.68(13) 18 17 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.87 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.611 _refine_diff_density_min -0.407 _refine_diff_density_rms 0.110 #==================================================================== # 4. text _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_experimental ; ; _publ_section_references ; Sheldrick, G.M. (1993). SHELXL-93. Program for crystal structure determination. Univ. of G\"ottingen, Federal Republic of Germany. Sheldrick, G.M. (1997). SHELXS-86. Program for the solution of crystal structures. Univ. of G\"ottingen, Federal Republic of Germany. ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; ; #==================================================================== data_3 _database_code_depnum_ccdc_archive 'CCDC 692200' _audit_creation_method SHELXL-97 _chemical_name_systematic ; diaqua tri S-2-methylglutarate di 3-methylglutarate cobalt (II) pentahydrate ; _chemical_name_common ;diaqua tri S-2-methylglutarate di 3-methylglutarate cobalt (ii) pentahydrate ; _chemical_melting_point ? _chemical_formula_moiety 'C30 H54 Co5 O27' _chemical_formula_sum 'C30 H54 Co5 O27' _chemical_formula_weight 1141.38 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M P4(3)32 _symmetry_space_group_name_Hall 'P 4acd 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' 'y+1/4, x+3/4, -z+3/4' '-y+1/4, -x+1/4, -z+1/4' 'y+3/4, -x+3/4, z+1/4' '-y+3/4, x+1/4, z+3/4' 'x+1/4, z+3/4, -y+3/4' '-x+3/4, z+1/4, y+3/4' '-x+1/4, -z+1/4, -y+1/4' 'x+3/4, -z+3/4, y+1/4' 'z+1/4, y+3/4, -x+3/4' 'z+3/4, -y+3/4, x+1/4' '-z+3/4, y+1/4, x+3/4' '-z+1/4, -y+1/4, -x+1/4' _cell_length_a 16.7176(2) _cell_length_b 16.7176(2) _cell_length_c 16.7176(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4672.21(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3055 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 22.35 _exptl_crystal_description parallelepiped _exptl_crystal_colour pink _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.623 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2340 _exptl_absorpt_coefficient_mu 1.824 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8984 _exptl_absorpt_correction_T_max 0.9644 _exptl_absorpt_process_details 'SADABS (Sheldrick, V2.10)' _chemical_absolute_configuration Left-D _exptl_special_details ; 'Blessing, Acta Cryst. (1995) A51, 33-38' ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 512x512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33850 _diffrn_reflns_av_R_equivalents 0.1193 _diffrn_reflns_av_sigmaI/netI 0.0606 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 30.02 _reflns_number_total 2299 _reflns_number_gt 1467 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0989P)^2^+0.0475P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(6) _refine_ls_number_reflns 2299 _refine_ls_number_parameters 98 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1220 _refine_ls_R_factor_gt 0.0619 _refine_ls_wR_factor_ref 0.1855 _refine_ls_wR_factor_gt 0.1486 _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_restrained_S_all 1.124 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.55816(5) 0.94184(5) 0.05816(5) 0.045(2) Uani 1 3 d S . . Co2 Co 0.43162(5) 0.81838(5) 0.1250 0.048(2) Uani 1 2 d S . . O1 O 0.5680(2) 0.9543(2) 0.1838(2) 0.055(3) Uani 1 1 d . . . O2 O 0.4798(3) 0.8655(3) 0.2268(3) 0.063(3) Uani 1 1 d . . . O3 O 0.4341(2) 0.9322(2) 0.0698(2) 0.056(3) Uani 1 1 d . . . O4 O 0.3848(4) 1.0126(4) -0.0156(4) 0.064(3) Uani 0.67 1 d P . . C1 C 0.5298(4) 0.9196(4) 0.2393(4) 0.056(3) Uani 1 1 d . . . C2 C 0.5486(5) 0.9381(4) 0.3250(4) 0.084(3) Uani 1 1 d . . . H2 H 0.5577 0.9959 0.3286 0.101 Uiso 1 1 calc R . . C3 C 0.6250 0.8970(3) 0.3530(3) 0.096(5) Uani 1 2 d S . . H3A H 0.6306 0.9056 0.4101 0.115 Uiso 0.50 1 calc PR . . H3B H 0.6194 0.8399 0.3444 0.115 Uiso 0.50 1 calc PR . . C4 C 0.4855 0.9205(3) 0.3744(3) 0.148(10) Uiso 0.50 1 d PR . . H1MA H 0.4401 0.9051 0.3428 0.222 Uiso 0.50 1 calc PR . . H2MB H 0.4722 0.9668 0.4057 0.222 Uiso 0.50 1 calc PR . . H3MC H 0.5000 0.8773 0.4093 0.222 Uiso 0.50 1 calc PR . . C5 C 0.3788 0.9755(3) 0.0391(3) 0.158(10) Uani 0.67 1 d PR . . C6 C 0.2933 0.9563(3) 0.0488(3) 0.140(7) Uani 0.67 1 d PR . . H6A H 0.2868 0.8987 0.0502 0.168 Uiso 0.67 1 calc PR . . H6B H 0.2641 0.9764 0.0029 0.168 Uiso 0.67 1 calc PR . . C7 C 0.2577 0.9923(3) 0.1250(3) 0.123(9) Uani 0.67 2 d SPR . . C8 C 0.2666 1.0702(3) 0.1325(3) 0.27(3) Uiso 0.33 1 d PR . . O1W O 0.4049 1.0620(3) 0.0499(3) 0.108(7) Uani 0.33 1 d PR . . O2W O 0.2981 1.0683(3) 0.0828(3) 0.28(2) Uiso 0.33 1 d PR . . O3W O 0.3177 1.0677(3) -0.1250(3) 0.28(3) Uiso 0.33 2 d SPR . . 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 Co1 0.045(2) 0.045(2) 0.045(2) -0.0043(3) 0.0043(3) -0.0043(3) Co2 0.047(2) 0.047(2) 0.050(3) 0.0002(3) 0.0002(3) -0.0097(4) O1 0.058(3) 0.054(3) 0.052(3) -0.0019(18) 0.0020(19) -0.0124(18) O2 0.072(4) 0.068(4) 0.049(3) 0.004(2) -0.0027(19) -0.023(2) O3 0.048(3) 0.057(3) 0.063(3) 0.004(2) 0.0006(18) -0.0015(18) O4 0.057(5) 0.071(5) 0.062(5) 0.019(3) -0.012(3) 0.001(3) C1 0.059(4) 0.054(4) 0.054(4) 0.000(3) -0.001(3) -0.011(3) C2 0.116(7) 0.086(6) 0.049(4) -0.007(3) 0.005(4) -0.051(5) C3 0.155(13) 0.066(5) 0.066(5) 0.015(5) -0.036(6) -0.036(6) C5 0.047(7) 0.181(18) 0.25(2) 0.141(17) 0.004(10) 0.018(9) C6 0.045(7) 0.203(18) 0.172(17) 0.075(14) -0.020(8) 0.002(9) C7 0.090(9) 0.090(9) 0.19(3) 0.032(12) 0.032(12) 0.018(12) O1W 0.084(11) 0.062(10) 0.18(2) 0.039(11) 0.020(12) 0.033(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 Co1 O3 2.090(4) 6_566 ? Co1 O3 2.090(4) 12_664 ? Co1 O3 2.090(4) . ? Co1 O1 2.116(4) . ? Co1 O1 2.116(4) 6_566 ? Co1 O1 2.116(4) 12_664 ? Co2 O2 2.041(4) 14_665 ? Co2 O2 2.041(4) . ? Co2 O3 2.116(4) . ? Co2 O3 2.116(4) 14_665 ? Co2 O1 2.132(4) 21_545 ? Co2 O1 2.132(4) 12_664 ? O1 C1 1.267(7) . ? O1 Co2 2.132(4) 6_566 ? O2 C1 1.249(7) . ? O3 C5 1.280(6) . ? O4 C5 1.110(9) . ? O4 O1W 1.411(7) . ? C1 C2 1.499(9) . ? C2 C4 1.371(8) . ? C2 C3 1.525(9) . ? C2 H2 0.9800 . ? C3 C2 1.525(9) 19_666 ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H1MA 0.9600 . ? C4 H2MB 0.9600 . ? C4 H3MC 0.9600 . ? C5 C6 1.4735 . ? C5 O1W 1.5213 . ? C6 C7 1.5298 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.3166 . ? C7 C8 1.317(4) 14_665 ? C7 C6 1.530(7) 14_665 ? C7 O2W 1.6024 . ? C7 O2W 1.602(9) 14_665 ? C8 O2W 0.9842 . ? 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 O3 Co1 O3 99.30(14) 6_566 12_664 ? O3 Co1 O3 99.30(14) 6_566 . ? O3 Co1 O3 99.30(14) 12_664 . ? O3 Co1 O1 79.56(15) 6_566 . ? O3 Co1 O1 171.14(16) 12_664 . ? O3 Co1 O1 89.55(15) . . ? O3 Co1 O1 89.55(15) 6_566 6_566 ? O3 Co1 O1 79.56(15) 12_664 6_566 ? O3 Co1 O1 171.14(16) . 6_566 ? O1 Co1 O1 91.62(16) . 6_566 ? O3 Co1 O1 171.14(16) 6_566 12_664 ? O3 Co1 O1 89.55(15) 12_664 12_664 ? O3 Co1 O1 79.56(15) . 12_664 ? O1 Co1 O1 91.62(16) . 12_664 ? O1 Co1 O1 91.62(16) 6_566 12_664 ? O2 Co2 O2 179.3(3) 14_665 . ? O2 Co2 O3 89.92(17) 14_665 . ? O2 Co2 O3 90.52(16) . . ? O2 Co2 O3 90.52(16) 14_665 14_665 ? O2 Co2 O3 89.92(18) . 14_665 ? O3 Co2 O3 103.0(2) . 14_665 ? O2 Co2 O1 91.51(17) 14_665 21_545 ? O2 Co2 O1 88.03(16) . 21_545 ? O3 Co2 O1 177.83(17) . 21_545 ? O3 Co2 O1 78.63(14) 14_665 21_545 ? O2 Co2 O1 88.03(16) 14_665 12_664 ? O2 Co2 O1 91.51(17) . 12_664 ? O3 Co2 O1 78.63(15) . 12_664 ? O3 Co2 O1 177.83(17) 14_665 12_664 ? O1 Co2 O1 99.8(2) 21_545 12_664 ? C1 O1 Co1 130.0(4) . . ? C1 O1 Co2 130.3(4) . 6_566 ? Co1 O1 Co2 96.09(16) . 6_566 ? C1 O2 Co2 133.1(4) . . ? C5 O3 Co1 129.5(3) . . ? C5 O3 Co2 132.0(3) . . ? Co1 O3 Co2 97.40(16) . . ? C5 O4 O1W 73.1(4) . . ? O2 C1 O1 123.1(6) . . ? O2 C1 C2 116.7(6) . . ? O1 C1 C2 120.0(5) . . ? C4 C2 C1 111.8(5) . . ? C4 C2 C3 111.3(6) . . ? C1 C2 C3 112.1(6) . . ? C4 C2 H2 107.1 . . ? C1 C2 H2 107.1 . . ? C3 C2 H2 107.1 . . ? C2 C3 C2 115.2(6) 19_666 . ? C2 C3 H3A 108.5 19_666 . ? C2 C3 H3A 108.5 . . ? C2 C3 H3B 108.5 19_666 . ? C2 C3 H3B 108.5 . . ? H3A C3 H3B 107.5 . . ? C2 C4 H1MA 109.5 . . ? C2 C4 H2MB 109.5 . . ? H1MA C4 H2MB 109.5 . . ? C2 C4 H3MC 109.5 . . ? H1MA C4 H3MC 109.5 . . ? H2MB C4 H3MC 109.5 . . ? O4 C5 O3 125.5(4) . . ? O4 C5 C6 107.5(3) . . ? O3 C5 C6 122.2(3) . . ? O4 C5 O1W 62.6(4) . . ? O3 C5 O1W 106.4(2) . . ? C6 C5 O1W 118.1 . . ? C5 C6 C7 112.5 . . ? C5 C6 H6A 109.1 . . ? C7 C6 H6A 109.1 . . ? C5 C6 H6B 109.1 . . ? C7 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? C8 C7 C8 103.45(13) . 14_665 ? C8 C7 C6 115.1 . . ? C8 C7 C6 105.1(3) 14_665 . ? C8 C7 C6 105.14(8) . 14_665 ? C8 C7 C6 115.1(7) 14_665 14_665 ? C6 C7 C6 112.82(18) . 14_665 ? C8 C7 O2W 37.8 . . ? C8 C7 O2W 117.7(4) 14_665 . ? C6 C7 O2W 77.4 . . ? C6 C7 O2W 120.6(2) 14_665 . ? C8 C7 O2W 117.7 . 14_665 ? C8 C7 O2W 37.8(2) 14_665 14_665 ? C6 C7 O2W 120.63(11) . 14_665 ? C6 C7 O2W 77.4(5) 14_665 14_665 ? O2W C7 O2W 149.56(9) . 14_665 ? O2W C8 C7 87.0 . . ? O4 O1W C5 44.3(4) . . ? C8 O2W C7 55.1 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.206 _refine_diff_density_min -0.183 _refine_diff_density_rms 0.081 #==================================================================== # 4. text _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_experimental ; ; _publ_section_references ; Sheldrick, G.M. (1993). SHELXL-93. Program for crystal structure determination. Univ. of G\"ottingen, Federal Republic of Germany. Sheldrick, G.M. (1997). SHELXS-86. Program for the solution of crystal structures. Univ. of G\"ottingen, Federal Republic of Germany. ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; ; data_1 _database_code_depnum_ccdc_archive 'CCDC 729897' #======================================================================== # 5. CHEMICAL DATA _audit_creation_method FullProf.2k _chemical_name_systematic ; diaqua penta 2-methylglutarate nickel (II) pentahydrate ; _chemical_name_common 'diaqua penta 2-methylglutarate nickel (ii) pentahydrate' _chemical_formula_moiety 'C30 H54 Ni5 O27' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'C30 H54 Ni5 O27' _chemical_formula_weight 1140.44 _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products loop_ _atom_type_symbol _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_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source ni 12.83760 3.87850 7.29200 0.25650 4.44380 12.17630 2.38000 66.34210 1.03410 -2.95600 0.50900 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 o 3.04850 13.27710 2.28680 5.70110 1.54630 0.32390 0.86700 32.90890 0.25080 0.04700 0.03200 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 c 2.31000 20.84390 1.02000 10.20750 1.58860 0.56870 0.86500 51.65120 0.21560 0.01700 0.00900 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 #======================================================================== # 6. POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M 'P 41 3 2' _symmetry_space_group_name_Hall 'P 4bd 2ab 3' loop_ _symmetry_equiv_pos_as_xyz #<--must include 'x,y,z' x,y,z x+1/2,-y+1/2,-z -x,y+1/2,-z+1/2 -x+1/2,-y,z+1/2 y,z,x -y+1/2,-z,x+1/2 y+1/2,-z+1/2,-x -y,z+1/2,-x+1/2 z,x,y -z,x+1/2,-y+1/2 -z+1/2,-x,y+1/2 z+1/2,-x+1/2,-y y+3/4,x+1/4,-z+1/4 -y+1/4,x+3/4,z+1/4 y+1/4,-x+1/4,z+3/4 -y+3/4,-x+3/4,-z+3/4 z+3/4,y+1/4,-x+1/4 -z+3/4,-y+3/4,-x+3/4 -z+1/4,y+3/4,x+1/4 z+1/4,-y+1/4,x+3/4 x+3/4,z+1/4,-y+1/4 x+1/4,-z+1/4,y+3/4 -x+3/4,-z+3/4,-y+3/4 -x+1/4,z+3/4,y+1/4 _cell_length_a 16.5347(3) _cell_length_b 16.5347(3) _cell_length_c 16.5347(3) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 4520.53(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293 _cell_special_details 'reflection Bragg-Brentano geom' _pd_spec_mount_mode 'flat sheet' _pd_spec_shape ? _pd_char_colour green #======================================================================== # 7. EXPERIMENTAL DATA _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.5405981 _diffrn_source 'X-ray tube' _diffrn_radiation_type "'Cu Kalpha1" _diffrn_source_target Cu _diffrn_radiation_monochromator Ge(111) _diffrn_measurement_device_type 'Bruker D8 Advance' # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 4501 _pd_meas_2theta_range_min 5.00000 _pd_meas_2theta_range_max 95.00000 _pd_meas_2theta_range_inc 0.020000 #======================================================================== # REFINEMENT DATA _pd_proc_ls_special_details ; ? ; # The next three items are given as text. _pd_proc_ls_profile_function Pseudo-Voigt _pd_proc_ls_background_function 'background points interpolation' _pd_proc_ls_pref_orient_corr 'not refined' # The following profile R-factors are NOT CORRECTED for background # The sum is extended to all non-excluded points. # These are the current CIF standard _pd_proc_ls_prof_R_factor 9.5838 _pd_proc_ls_prof_wR_factor 12.7891 _pd_proc_ls_prof_wR_expected 3.7563 # The following profile R-factors are CORRECTED for background # The sum is extended to all non-excluded points. # These items are not in the current CIF standard, but are defined above _pd_proc_ls_prof_cR_factor 15.1744 _pd_proc_ls_prof_cwR_factor 17.6592 _pd_proc_ls_prof_cwR_expected 5.1868 # The following items are not in the CIF standard, but are defined above _pd_proc_ls_prof_chi2 11.5918 _pd_proc_ls_prof_echi2 11.8023 # Items related to LS refinement _refine_ls_R_I_factor 8.2091 _refine_ls_number_reflns 502 _refine_ls_number_parameters 52 _refine_ls_number_restraints 24 # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 5.0333 _pd_proc_2theta_range_max 95.0333 _pd_proc_2theta_range_inc 0.020000 _pd_proc_wavelength 1.540600 _pd_block_diffractogram_id ? # The id used for the block containing # the powder pattern profile (section 11) # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? # The following items are used to identify the programs used. _computing_structure_solution 'SIRPOW and SHELX' _computing_structure_refinement FULLPROF _computing_molecular_graphics DIAMOND #======================================================================== # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _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 # Not in version 2.0.1 _atom_site_type_symbol Ni1 0.1919(2) 0.1919(2) 0.1919(2) 0.00000 1.00000 Uiso Ni Ni2 0.3198(2) 0.12500 0.0698(2) 0.00000 1.00000 Uiso Ni O1 0.2053(7) 0.1861(7) 0.0668(6) 0.00000 1.00000 Uiso O O2 0.1187(8) 0.2831(6) 0.0262(7) 0.00000 1.00000 Uiso O O3 0.1812(7) 0.1847(6) 0.3219(6) 0.00000 1.00000 Uiso O C1 0.1635(10) 0.2227(9) 0.0078(5) 0.00000 1.00000 Uiso C C2 0.1772(9) 0.2031(5) -0.0843(6) 0.00000 1.00000 Uiso C C3 0.37500 0.1146(7) 0.6354(7) 0.00000 1.00000 Uiso C C4 0.3629(18) 0.358(2) 0.7285(16) 0.00000 0.50000 Uiso C O4 0.2370(10) 0.3024(9) 0.3414(10) 0.00000 0.66667 Uiso O C5 0.1958(14) 0.2451(9) 0.3694(6) 0.00000 0.66667 Uiso C C6 0.2064(6) 0.2310(10) 0.4575(6) 0.00000 0.66667 Uiso C C7 0.12500 0.2585(8) 0.5085(8) 0.00000 0.66667 Uiso C C8 0.2863(18) 0.275(3) 0.479(3) 0.00000 0.33333 Uiso C Ow1 0.268(2) 0.282(2) 0.398(2) 0.00000 0.33333 Uiso O Ow2 0.025(2) 0.261(2) 0.5823(18) 0.00000 0.33333 Uiso O Ow3 0.12500 0.239(2) 0.489(2) 0.00000 0.33333 Uiso O # Note: if the displacement parameters were refined anisotropically # the U matrices should be given as for single-crystal studies. #============================================================================= # DISTANCES AND ANGLES / MOLECULAR GEOMETRY _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag ? ? ? ? ? ? Ni1 O1 . . 2.08(1) . Ni1 O3 . . 2.16(1) . Ni1 O3 . . 2.15(1) . Ni2 O2 . 5 1.92(1) . Ni2 O3 . 9 2.11(1) . Ni2 O1 . . 2.15(1) . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 Ni1 O1 . . 9 93.7(5) . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag ? ? ? ? ? ? ? ? ? ? ? #==================================================================== # 4. text _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_experimental ; ; _publ_section_references ; Sheldrick, G.M. (1993). SHELXL-93. Program for crystal structure determination. Univ. of G\"ottingen, Federal Republic of Germany. Sheldrick, G.M. (1997). SHELXS-86. Program for the solution of crystal structures. Univ. of G\"ottingen, Federal Republic of Germany. ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; ;