# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3 _audit_creation_date ? _audit_creation_method ; Olex2 1.2 (compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety '0.08(C84 H28 Co8 Gd4 N12 O72)' _chemical_formula_sum 'C7 H2.33 Co0.66 Gd0.33 N O6' _chemical_formula_weight 287.22 _chemical_melting_point ? 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system hexagonal _space_group_IT_number 192 _space_group_name_H-M_alt 'P 6/m c c' _space_group_name_Hall '-P 6 2c' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-y, x-y, z' 3 '-x+y, -x, z' 4 '-x, -y, z' 5 'y, -x+y, z' 6 'x-y, x, z' 7 'y, x, -z+1/2' 8 'x-y, -y, -z+1/2' 9 '-x, -x+y, -z+1/2' 10 '-y, -x, -z+1/2' 11 '-x+y, y, -z+1/2' 12 'x, x-y, -z+1/2' 13 '-x, -y, -z' 14 'y, -x+y, -z' 15 'x-y, x, -z' 16 'x, y, -z' 17 '-y, x-y, -z' 18 '-x+y, -x, -z' 19 '-y, -x, z-1/2' 20 '-x+y, y, z-1/2' 21 'x, x-y, z-1/2' 22 'y, x, z-1/2' 23 'x-y, -y, z-1/2' 24 '-x, -x+y, z-1/2' _cell_length_a 15.3945(12) _cell_length_b 15.3945(12) _cell_length_c 14.6706(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3011.0(4) _cell_formula_units_Z 12 _cell_measurement_reflns_used ? _cell_measurement_temperature 413 _cell_measurement_theta_max ? _cell_measurement_theta_min ? _exptl_absorpt_coefficient_mu 3.117 _exptl_absorpt_correction_T_min 0.24481 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ? _exptl_crystal_colour violet _exptl_crystal_density_diffrn 1.897 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description ? _exptl_crystal_F_000 1623 _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_unetI/netI 0.1013 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 929 _diffrn_reflns_theta_full 25.01 _diffrn_reflns_theta_max 25.01 _diffrn_reflns_theta_min 3.06 _diffrn_ambient_temperature 413 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 308 _reflns_number_total 929 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 0.686 _refine_diff_density_min -0.648 _refine_diff_density_rms 0.142 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.903 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 59 _refine_ls_number_reflns 929 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1999 _refine_ls_R_factor_gt 0.0923 _refine_ls_restrained_S_all 0.897 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1335P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2426 _refine_ls_wR_factor_ref 0.2849 _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. ISOR 0.005 0.01 C8 C5 ISOR 0.005 0.01 O4 ISOR 0.005 0.01 O1 EADP O3 C6 O2 EADP C8 O4 ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Gd1 Gd 0.6667 0.3333 0.2500 0.1095(12) Uani 1 6 d S . . Co3 Co 0.5000 0.5000 0.0000 0.159(3) Uani 1 4 d S . . C4 C 0.4202(18) 0.2691(16) 0.1896(14) 0.141(7) Uani 1 1 d . . . C5 C 0.3181(19) 0.2159(18) 0.1904(17) 0.170(9) Uani 1 1 d U . . H5 H 0.2906 0.2314 0.1468 0.203 Uiso 1 1 d . . . C6 C 0.493(3) 0.354(2) 0.1408(15) 0.163(4) Uani 1 1 d . . . N7 N 0.4790(17) 0.2395(9) 0.2500 0.130(7) Uani 1 2 d S . . C8 C 0.286(3) 0.1431(16) 0.2500 0.200(6) Uani 1 2 d SU . . O1 O 0.3464(14) 0.4805(14) 0.0000 0.185(8) Uani 1 2 d SU . . H1 H 0.3123 0.4133 0.0000 0.294 Uiso 0.33 2 d SP . . O2 O 0.5884(12) 0.3882(11) 0.1435(9) 0.163(4) Uani 1 1 d . . . O3 O 0.4499(10) 0.3915(12) 0.0966(8) 0.163(4) Uani 1 1 d . . . Co1 Co 0.0000 0.0000 0.2500 0.12(2) Uani 0.13 12 d SP . . O4 O 0.1690(19) 0.0845(10) 0.2500 0.200(6) Uani 1 2 d SU . . 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 Gd1 0.1265(15) 0.1265(15) 0.0756(13) 0.000 0.000 0.0632(8) Co3 0.218(7) 0.224(7) 0.110(4) 0.000 0.000 0.167(6) C4 0.15(2) 0.121(18) 0.151(18) -0.028(16) 0.022(16) 0.062(16) C5 0.171(9) 0.172(10) 0.170(10) -0.003(5) 0.000(5) 0.089(6) C6 0.178(10) 0.220(10) 0.128(6) 0.009(6) -0.012(7) 0.127(9) N7 0.129(18) 0.130(14) 0.131(17) -0.035(14) 0.000 0.065(9) C8 0.200(6) 0.196(6) 0.205(7) -0.005(3) 0.000 0.100(3) O1 0.189(12) 0.198(11) 0.164(11) 0.000 0.000 0.094(8) O2 0.178(10) 0.220(10) 0.128(6) 0.009(6) -0.012(7) 0.127(9) O3 0.178(10) 0.220(10) 0.128(6) 0.009(6) -0.012(7) 0.127(9) Co1 0.15(3) 0.15(3) 0.06(3) 0.000 0.000 0.074(16) O4 0.200(6) 0.196(6) 0.205(7) -0.005(3) 0.000 0.100(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 N7 2.50(2) 2_655 ? Gd1 N7 2.50(2) . ? Gd1 N7 2.50(2) 3_665 ? Gd1 O2 2.372(14) . ? Gd1 O2 2.372(14) 10_665 ? Gd1 O2 2.371(14) 11_655 ? Gd1 O2 2.371(14) 2_655 ? Gd1 O2 2.371(14) 12 ? Gd1 O2 2.371(14) 3_665 ? Co3 O1 2.23(2) . ? Co3 O1 2.23(2) 13_665 ? Co3 O3 2.026(14) 16 ? Co3 O3 2.026(14) 4_665 ? Co3 O3 2.026(14) 13_665 ? Co3 O3 2.026(14) . ? C4 C5 1.36(3) . ? C4 C6 1.42(3) . ? C4 N7 1.49(2) . ? C5 C8 1.31(3) . ? C6 O2 1.29(3) . ? C6 O3 1.25(2) . ? N7 C4 1.49(2) 12 ? C8 C5 1.31(3) 12 ? C8 O4 1.56(4) . ? Co1 O4 2.25(3) 3 ? Co1 O4 2.25(3) 2 ? Co1 O4 2.25(3) 5 ? Co1 O4 2.25(3) . ? Co1 O4 2.25(3) 6 ? Co1 O4 2.25(3) 4 ? 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 N7 Gd1 N7 120.017(1) 2_655 . ? N7 Gd1 N7 120.018(2) 2_655 3_665 ? N7 Gd1 N7 119.965(1) . 3_665 ? O2 Gd1 N7 72.0(4) 2_655 . ? O2 Gd1 N7 138.5(3) 3_665 . ? O2 Gd1 N7 63.9(4) 12 . ? O2 Gd1 N7 72.0(4) 12 2_655 ? O2 Gd1 N7 138.5(3) 10_665 2_655 ? O2 Gd1 N7 138.5(3) . 2_655 ? O2 Gd1 N7 138.5(3) 11_655 . ? O2 Gd1 N7 72.0(4) 10_665 . ? O2 Gd1 N7 138.5(3) 12 3_665 ? O2 Gd1 N7 63.9(4) 10_665 3_665 ? O2 Gd1 N7 72.0(4) . 3_665 ? O2 Gd1 N7 63.9(4) 3_665 3_665 ? O2 Gd1 N7 63.9(4) . . ? O2 Gd1 N7 72.0(4) 11_655 3_665 ? O2 Gd1 N7 138.5(3) 2_655 3_665 ? O2 Gd1 N7 63.9(4) 11_655 2_655 ? O2 Gd1 N7 63.9(4) 2_655 2_655 ? O2 Gd1 N7 72.0(4) 3_665 2_655 ? O2 Gd1 O2 83.1(7) 2_655 12 ? O2 Gd1 O2 144.1(7) 3_665 12 ? O2 Gd1 O2 81.3(5) 11_655 10_665 ? O2 Gd1 O2 81.3(5) 11_655 12 ? O2 Gd1 O2 127.8(8) 11_655 2_655 ? O2 Gd1 O2 83.1(7) 11_655 3_665 ? O2 Gd1 O2 81.3(5) 2_655 3_665 ? O2 Gd1 O2 144.0(7) 2_655 10_665 ? O2 Gd1 O2 81.3(5) 3_665 . ? O2 Gd1 O2 127.8(8) 12 . ? O2 Gd1 O2 83.0(7) 10_665 . ? O2 Gd1 O2 81.3(5) 2_655 . ? O2 Gd1 O2 127.8(8) 3_665 10_665 ? O2 Gd1 O2 81.3(5) 12 10_665 ? O2 Gd1 O2 144.0(7) 11_655 . ? O1 Co3 O1 179.999(1) . 13_665 ? O3 Co3 O1 93.0(5) 13_665 . ? O3 Co3 O1 87.0(5) 16 . ? O3 Co3 O1 93.0(5) 4_665 . ? O3 Co3 O1 87.0(5) . . ? O3 Co3 O1 87.0(5) 13_665 13_665 ? O3 Co3 O1 93.0(5) . 13_665 ? O3 Co3 O1 87.0(5) 4_665 13_665 ? O3 Co3 O1 93.0(5) 16 13_665 ? O3 Co3 O3 91.3(8) 4_665 . ? O3 Co3 O3 88.7(8) 16 . ? O3 Co3 O3 180.0(9) 16 4_665 ? O3 Co3 O3 180.0(8) . 13_665 ? O3 Co3 O3 88.7(8) 4_665 13_665 ? O3 Co3 O3 91.3(8) 16 13_665 ? C5 C4 C6 134(3) . . ? C5 C4 N7 120(2) . . ? C6 C4 N7 105(2) . . ? C8 C5 C4 110(3) . . ? O2 C6 C4 125(3) . . ? O3 C6 C4 109(3) . . ? O3 C6 O2 126(3) . . ? C4 N7 Gd1 121.7(13) 12 . ? C4 N7 Gd1 121.7(13) . . ? C4 N7 C4 117(3) 12 . ? C5 C8 C5 142(5) . 12 ? C5 C8 O4 109(2) 12 . ? C5 C8 O4 109(2) . . ? C6 O2 Gd1 123.6(16) . . ? C6 O3 Co3 132(2) . . ? O4 Co1 O4 60.0 . 5 ? O4 Co1 O4 120.000(1) 3 2 ? O4 Co1 O4 60.0 4 2 ? O4 Co1 O4 120.000(1) 6 5 ? O4 Co1 O4 180.000(1) 2 5 ? O4 Co1 O4 60.0 3 5 ? O4 Co1 O4 120.000(1) 4 5 ? O4 Co1 O4 60.0 6 2 ? O4 Co1 O4 120.000(2) 6 4 ? O4 Co1 O4 180.0(15) . 4 ? O4 Co1 O4 60.000(1) . 6 ? O4 Co1 O4 120.000(1) . 3 ? O4 Co1 O4 120.000(1) . 2 ? O4 Co1 O4 60.0 4 3 ? O4 Co1 O4 180.000(1) 6 3 ? C8 O4 Co1 180.000(2) . . ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 202 37 ' ' 2 0.000 0.000 0.500 202 39 ' ' _platon_squeeze_details ; Two Co2+ ions are highly disordered. Therefore, the SQUEEZE routine of PLATON was applied. The final formula was calculated from the TGA combined with elemental analysis data. ; # start Validation Reply Form _vrf_CHEMW03_ALERT_2_C ; PROBLEM: The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.99 <> 1.01 RESPONSE: This is a consequence of the use of SQUEEZE. The solvent is included in formula, but is not in the model. ; _vrf_PLAT041_ALERT_1_C ; PROBLEM: Calc. and Reported SumFormula Differ RESPONSE: This is a consequence of the use of SQUEEZE. The solvent is included in formula, but is not in the model. ; # end Validation Reply Form _database_code_depnum_ccdc_archive 'CCDC 958890' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 _audit_creation_date 2013-11-01 _audit_creation_method ; Olex2 1.2 (compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety '0.5(C84 H36 Co6 Gd4 N12 O72), Co1 H 12 O6, 3(H4 O2)' _chemical_formula_sum 'C42 H42 Co4 Gd2 N6 O48' _chemical_formula_weight 1949.03 _chemical_melting_point ? 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system hexagonal _space_group_IT_number 192 _space_group_name_H-M_alt 'P 6/m c c' _space_group_name_Hall '-P 6 2c' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 'x-y, x, z' 3 '-y, x-y, z' 4 '-x, -y, z' 5 '-x+y, -x, z' 6 'y, -x+y, z' 7 'x-y, -y, -z+1/2' 8 '-x, -x+y, -z+1/2' 9 'y, x, -z+1/2' 10 '-y, -x, -z+1/2' 11 '-x+y, y, -z+1/2' 12 'x, x-y, -z+1/2' 13 '-x, -y, -z' 14 '-x+y, -x, -z' 15 'y, -x+y, -z' 16 'x, y, -z' 17 'x-y, x, -z' 18 '-y, x-y, -z' 19 '-x+y, y, z-1/2' 20 'x, x-y, z-1/2' 21 '-y, -x, z-1/2' 22 'y, x, z-1/2' 23 'x-y, -y, z-1/2' 24 '-x, -x+y, z-1/2' _cell_length_a 15.7215(8) _cell_length_b 15.7215(8) _cell_length_c 14.9689(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3204.1(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 2754 _cell_measurement_temperature 120 _cell_measurement_theta_max 28.9329 _cell_measurement_theta_min 2.5859 _exptl_absorpt_coefficient_mu 3.171 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.91008 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.36.21 Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour pink _exptl_crystal_density_diffrn 2.007 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 1864 _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_unetI/netI 0.0396 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 6658 _diffrn_reflns_theta_full 25.01 _diffrn_reflns_theta_max 25.01 _diffrn_reflns_theta_min 2.59 _diffrn_ambient_temperature 120 _diffrn_detector_area_resol_mean 16.2116 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0028205000 _diffrn_orient_matrix_UB_12 -0.0267617000 _diffrn_orient_matrix_UB_13 -0.0369684000 _diffrn_orient_matrix_UB_21 0.0393783000 _diffrn_orient_matrix_UB_22 -0.0022083000 _diffrn_orient_matrix_UB_23 0.0207224000 _diffrn_orient_matrix_UB_31 -0.0340140000 _diffrn_orient_matrix_UB_32 -0.0446509000 _diffrn_orient_matrix_UB_33 0.0211179000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'SuperNova (Mo) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 672 _reflns_number_total 994 _reflns_odcompleteness_completeness 99.78 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELX, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELX, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.825 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.095 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 116 _refine_ls_number_reflns 994 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.0503 _refine_ls_R_factor_gt 0.0265 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.0656 _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. DFIX 1.35 C6 C3 DFIX 1.4 C3 C6 ISOR 0.01 0.02 O5 O5' ISOR 0.005 0.01 O7 C6 ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Gd1 Gd 0.6667 0.3333 0.2500 0.00770(17) Uani 1 6 d S . . Co1 Co 0.5000 0.0000 0.0000 0.0118(3) Uani 1 4 d S . . O4 O 0.5147(4) -0.1295(4) 0.0000 0.0146(12) Uani 1 2 d S . . H4 H 0.477(7) -0.170(7) -0.039(5) 0.022 Uiso 0.50 1 d P . . O1 O 0.6108(3) 0.1988(2) 0.14131(17) 0.0147(8) Uani 1 1 d . . . N1 N 0.75811(17) 0.24189(17) 0.2500 0.0132(11) Uani 1 2 d S . . O2 O 0.6089(3) 0.0619(2) 0.0954(2) 0.0220(9) Uani 1 1 d . . . C3 C 0.7781(4) 0.1115(4) 0.1956(4) 0.0272(14) Uani 1 1 d D . . H3 H 0.7481 0.0477 0.1654 0.033 Uiso 1 1 calc R . . C4B C 0.7300(3) 0.1634(3) 0.1983(3) 0.0121(11) Uani 1 1 d . . . C5 C 0.6426(4) 0.1385(4) 0.1399(3) 0.0146(12) Uani 1 1 d . . . C6 C 0.8654(10) 0.1475(10) 0.2327(6) 0.018(3) Uani 0.50 1 d PDU . . Co2 Co 1.0000 1.0000 0.0000 0.0157(5) Uani 1 12 d S . . O6 O 0.7252(12) 0.9659(10) 0.0000 0.040(4) Uani 0.50 2 d SP . . O5 O 0.9321(15) 0.8940(11) 0.1010(9) 0.048(5) Uani 0.25 1 d PU . . O5' O 0.8595(13) 0.8961(13) 0.0365(10) 0.065(7) Uani 0.25 1 d PU . . O6' O 0.7009(13) 0.9003(14) 0.0000 0.067(6) Uani 0.50 2 d SP . . O7 O 0.9158(8) 0.1004(7) 0.2196(4) 0.032(2) Uani 0.50 1 d PU . . 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 Gd1 0.0078(2) 0.0078(2) 0.0075(2) 0.000 0.000 0.00390(11) Co1 0.0198(10) 0.0081(6) 0.0065(5) 0.000 0.000 0.0063(9) O4 0.019(3) 0.012(3) 0.012(2) 0.000 0.000 0.007(3) O1 0.019(3) 0.0150(17) 0.0121(14) -0.0037(11) -0.0043(15) 0.0097(19) N1 0.016(2) 0.016(2) 0.012(2) 0.002(3) 0.002(3) 0.011(2) O2 0.036(3) 0.013(2) 0.0195(17) -0.0102(16) -0.0129(17) 0.0150(19) C3 0.012(3) 0.011(3) 0.058(4) -0.015(3) -0.004(3) 0.005(3) C4B 0.012(3) 0.006(3) 0.016(3) -0.002(2) 0.005(2) 0.002(2) C5 0.016(3) 0.018(3) 0.009(2) 0.003(2) 0.002(2) 0.008(3) C6 0.017(5) 0.011(5) 0.022(6) 0.006(4) 0.009(4) 0.005(4) Co2 0.0152(7) 0.0152(7) 0.0166(10) 0.000 0.000 0.0076(4) O6 0.041(9) 0.027(9) 0.053(8) 0.000 0.000 0.018(8) O5 0.066(10) 0.041(8) 0.048(7) 0.021(6) 0.039(7) 0.035(7) O5' 0.042(9) 0.048(10) 0.080(10) -0.004(7) 0.028(7) 0.003(7) O6' 0.039(10) 0.110(17) 0.049(9) 0.000 0.000 0.035(13) O7 0.026(4) 0.021(4) 0.059(4) -0.010(3) 0.000(3) 0.019(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O1 2.456(3) 3_655 ? Gd1 O1 2.456(3) 12 ? Gd1 O1 2.456(3) 5_665 ? Gd1 O1 2.456(3) 11_655 ? Gd1 O1 2.456(3) . ? Gd1 O1 2.456(3) 10_665 ? Gd1 N1 2.490(5) 5_665 ? Gd1 N1 2.490(5) 3_655 ? Gd1 N1 2.490(5) . ? Co1 O4 2.160(5) 13_655 ? Co1 O4 2.160(5) . ? Co1 O2 2.062(3) . ? Co1 O2 2.062(3) 13_655 ? Co1 O2 2.062(3) 4_655 ? Co1 O2 2.062(3) 16 ? O1 C5 1.274(6) . ? N1 C4B 1.331(5) . ? N1 C4B 1.331(5) 10_665 ? O2 C5 1.240(5) . ? C3 C4B 1.362(7) . ? C3 C6 1.493(13) 10_665 ? C3 C6 1.317(11) . ? C4B C5 1.506(6) . ? C6 C3 1.493(13) 10_665 ? C6 C6 0.557(19) 10_665 ? C6 O7 1.524(10) 10_665 ? C6 O7 1.341(10) . ? Co2 O5' 2.059(17) 13_775 ? Co2 O5' 2.059(17) 4_775 ? Co2 O5' 2.059(17) 6_565 ? Co2 O5' 2.059(17) 16 ? Co2 O5' 2.059(17) 14_675 ? Co2 O5' 2.059(17) 5_675 ? Co2 O5' 2.059(17) 17_655 ? Co2 O5' 2.059(17) 18_765 ? Co2 O5' 2.059(17) 3_765 ? Co2 O5' 2.059(17) 15_565 ? Co2 O5' 2.059(17) . ? Co2 O5' 2.059(17) 2_655 ? O6 O6' 0.903(19) . ? O5 O5 1.462(15) 2_655 ? O5 O5 1.462(15) 6_565 ? O5 O5' 1.51(2) . ? O5 O5' 1.32(2) 2_655 ? O5' O5 1.32(2) 6_565 ? O5' O5' 1.09(3) 16 ? O7 C6 1.524(10) 10_665 ? O7 O7 0.945(12) 10_665 ? 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 Gd1 O1 128.29(17) 11_655 5_665 ? O1 Gd1 O1 128.29(17) 3_655 12 ? O1 Gd1 O1 80.91(10) 10_665 12 ? O1 Gd1 O1 80.91(10) . 5_665 ? O1 Gd1 O1 83.57(13) 12 5_665 ? O1 Gd1 O1 80.91(10) 3_655 5_665 ? O1 Gd1 O1 143.94(17) 10_665 5_665 ? O1 Gd1 O1 143.94(17) . 12 ? O1 Gd1 O1 128.29(17) . 10_665 ? O1 Gd1 O1 80.91(10) 11_655 10_665 ? O1 Gd1 O1 83.57(13) 11_655 . ? O1 Gd1 O1 143.94(17) 11_655 3_655 ? O1 Gd1 O1 80.91(10) 11_655 12 ? O1 Gd1 O1 83.57(13) 10_665 3_655 ? O1 Gd1 O1 80.91(10) . 3_655 ? O1 Gd1 N1 71.97(8) 5_665 3_655 ? O1 Gd1 N1 64.14(8) 11_655 5_665 ? O1 Gd1 N1 64.14(9) 12 3_655 ? O1 Gd1 N1 64.14(8) 3_655 3_655 ? O1 Gd1 N1 71.97(8) . 5_665 ? O1 Gd1 N1 64.14(9) 5_665 5_665 ? O1 Gd1 N1 71.97(8) 12 5_665 ? O1 Gd1 N1 138.21(7) 3_655 5_665 ? O1 Gd1 N1 138.21(7) 10_665 5_665 ? O1 Gd1 N1 138.21(7) 12 . ? O1 Gd1 N1 71.97(8) 3_655 . ? O1 Gd1 N1 64.14(8) 10_665 . ? O1 Gd1 N1 64.14(8) . . ? O1 Gd1 N1 71.97(8) 11_655 . ? O1 Gd1 N1 71.97(8) 10_665 3_655 ? O1 Gd1 N1 138.21(7) . 3_655 ? O1 Gd1 N1 138.21(7) 11_655 3_655 ? O1 Gd1 N1 138.21(7) 5_665 . ? N1 Gd1 N1 120.0 3_655 5_665 ? N1 Gd1 N1 120.0 . 5_665 ? N1 Gd1 N1 120.000(1) . 3_655 ? O4 Co1 O4 180.0 13_655 . ? O2 Co1 O4 90.58(14) . 13_655 ? O2 Co1 O4 89.42(14) 13_655 13_655 ? O2 Co1 O4 89.42(14) 4_655 13_655 ? O2 Co1 O4 90.58(14) 16 13_655 ? O2 Co1 O4 89.42(14) . . ? O2 Co1 O4 89.42(14) 16 . ? O2 Co1 O4 90.58(14) 4_655 . ? O2 Co1 O4 90.58(14) 13_655 . ? O2 Co1 O2 180.0 4_655 16 ? O2 Co1 O2 92.36(19) 13_655 16 ? O2 Co1 O2 87.64(19) 13_655 4_655 ? O2 Co1 O2 87.64(19) 16 . ? O2 Co1 O2 92.36(19) 4_655 . ? O2 Co1 O2 180.00(19) 13_655 . ? C5 O1 Gd1 123.2(3) . . ? C4B N1 Gd1 121.0(3) . . ? C4B N1 Gd1 121.0(3) 10_665 . ? C4B N1 C4B 118.0(5) 10_665 . ? C5 O2 Co1 132.9(3) . . ? C4B C3 C6 115.8(6) . 10_665 ? C6 C3 C4B 120.1(6) . . ? C6 C3 C6 21.7(9) . 10_665 ? N1 C4B C3 123.1(5) . . ? N1 C4B C5 114.5(4) . . ? C3 C4B C5 122.3(4) . . ? O1 C5 C4B 116.3(4) . . ? O2 C5 O1 126.6(5) . . ? O2 C5 C4B 117.1(5) . . ? C3 C6 C3 115.6(7) . 10_665 ? C3 C6 O7 123.3(12) . 10_665 ? C3 C6 O7 98.5(6) 10_665 10_665 ? C3 C6 O7 118.6(10) . . ? C6 C6 C3 97(3) 10_665 . ? C6 C6 C3 61(2) 10_665 10_665 ? C6 C6 O7 98.2(5) 10_665 . ? C6 C6 O7 60.6(4) 10_665 10_665 ? O7 C6 C3 123.9(9) . 10_665 ? O7 C6 O7 37.8(5) . 10_665 ? O5' Co2 O5' 57.65(13) 4_775 5_675 ? O5' Co2 O5' 66.8(4) 13_775 5_675 ? O5' Co2 O5' 57.64(13) 6_565 5_675 ? O5' Co2 O5' 66.8(4) 15_565 5_675 ? O5' Co2 O5' 180.0(10) 2_655 14_675 ? O5' Co2 O5' 149.2(9) 17_655 14_675 ? O5' Co2 O5' 113.2(4) 18_765 14_675 ? O5' Co2 O5' 122.36(14) 3_765 14_675 ? O5' Co2 O5' 113.2(4) 3_765 5_675 ? O5' Co2 O5' 30.8(9) 4_775 13_775 ? O5' Co2 O5' 122.36(13) 6_565 13_775 ? O5' Co2 O5' 113.2(4) 15_565 13_775 ? O5' Co2 O5' 113.2(4) . 5_675 ? O5' Co2 O5' 149.2(9) 2_655 5_675 ? O5' Co2 O5' 180.0(10) 17_655 5_675 ? O5' Co2 O5' 122.36(14) 18_765 5_675 ? O5' Co2 O5' 122.35(14) . 14_675 ? O5' Co2 O5' 66.8(4) 6_565 16 ? O5' Co2 O5' 57.64(13) 15_565 16 ? O5' Co2 O5' 30.8(9) . 16 ? O5' Co2 O5' 66.8(4) 2_655 16 ? O5' Co2 O5' 113.2(4) 14_675 16 ? O5' Co2 O5' 122.35(14) 5_675 16 ? O5' Co2 O5' 149.2(9) 13_775 16 ? O5' Co2 O5' 179.998(2) 4_775 16 ? O5' Co2 O5' 57.65(13) 13_775 14_675 ? O5' Co2 O5' 66.8(4) 4_775 14_675 ? O5' Co2 O5' 66.8(4) 6_565 14_675 ? O5' Co2 O5' 57.64(13) 15_565 14_675 ? O5' Co2 O5' 57.65(14) 17_655 16 ? O5' Co2 O5' 113.2(4) 18_765 16 ? O5' Co2 O5' 122.36(13) 3_765 16 ? O5' Co2 O5' 30.8(9) 5_675 14_675 ? O5' Co2 O5' 149.2(9) 18_765 15_565 ? O5' Co2 O5' 179.999(3) 3_765 15_565 ? O5' Co2 O5' 57.65(14) 2_655 . ? O5' Co2 O5' 66.8(4) 17_655 . ? O5' Co2 O5' 149.2(9) 3_765 6_565 ? O5' Co2 O5' 66.8(4) . 15_565 ? O5' Co2 O5' 122.36(14) 2_655 15_565 ? O5' Co2 O5' 113.2(4) 17_655 15_565 ? O5' Co2 O5' 57.64(13) 3_765 2_655 ? O5' Co2 O5' 57.64(13) 18_765 17_655 ? O5' Co2 O5' 66.8(4) 3_765 17_655 ? O5' Co2 O5' 30.8(9) 3_765 18_765 ? O5' Co2 O5' 122.36(13) 18_765 . ? O5' Co2 O5' 113.2(4) 3_765 . ? O5' Co2 O5' 30.8(9) 17_655 2_655 ? O5' Co2 O5' 66.8(4) 18_765 2_655 ? O5' Co2 O5' 179.999(3) 18_765 6_565 ? O5' Co2 O5' 66.8(4) 3_765 13_775 ? O5' Co2 O5' 113.2(4) 6_565 4_775 ? O5' Co2 O5' 122.36(13) 15_565 4_775 ? O5' Co2 O5' 149.2(9) . 4_775 ? O5' Co2 O5' 179.997(2) . 13_775 ? O5' Co2 O5' 122.35(14) 2_655 13_775 ? O5' Co2 O5' 113.2(4) 17_655 13_775 ? O5' Co2 O5' 57.64(13) 18_765 13_775 ? O5' Co2 O5' 30.8(9) 15_565 6_565 ? O5' Co2 O5' 57.64(13) . 6_565 ? O5' Co2 O5' 113.2(4) 2_655 6_565 ? O5' Co2 O5' 122.36(14) 17_655 6_565 ? O5' Co2 O5' 113.2(4) 2_655 4_775 ? O5' Co2 O5' 122.35(14) 17_655 4_775 ? O5' Co2 O5' 57.64(13) 3_765 4_775 ? O5' Co2 O5' 66.8(4) 18_765 4_775 ? O5 O5 Co2 69.67(16) 6_565 . ? O5 O5 Co2 69.67(16) 2_655 . ? O5 O5 O5 119.999(13) 6_565 2_655 ? O5 O5 O5' 135.3(8) 2_655 . ? O5 O5 O5' 52.6(11) 6_565 . ? O5' O5 Co2 67.2(9) . . ? O5' O5 Co2 69.7(10) 2_655 . ? O5' O5 O5 132.4(10) 2_655 6_565 ? O5' O5 O5 65.5(14) 2_655 2_655 ? O5' O5 O5' 88.9(11) 2_655 . ? O5 O5' Co2 73.4(11) 6_565 . ? O5 O5' Co2 70.3(10) . . ? O5 O5' O5 61.9(12) 6_565 . ? O5' O5' Co2 74.6(4) 16 . ? O5' O5' O5 137.2(10) 16 6_565 ? O5' O5' O5 129.8(8) 16 . ? C6 O7 C6 21.2(7) . 10_665 ? O7 O7 C6 60.5(4) 10_665 10_665 ? O7 O7 C6 81.6(5) 10_665 . ? # start Validation Reply Form _vrf_PLAT041_ALERT_1_C ; PROBLEM: Check Calc. and Reported SumFormula RESPONSE: Becuse it is difficult to lacate H atoms on guest water molecules, such H atoms is included in formula, but is not in the model. ; _vrf_CHEMW03_ALERT_2_C ; PROBLEM: The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.99 <> 1.01 RESPONSE: Becuse it is difficult to lacate H atoms on guest water molecules, such H atoms is included in formula, but is not in the model. ; # end Validation Reply Form _database_code_depnum_ccdc_archive 'CCDC 958891' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 _audit_creation_date 2013-11-01 _audit_creation_method ; Olex2 1.2 (compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety '0.5(C84 H36 Co6 Gd4 N12 O72), Co1 H8 O4, 12(H0.5 O0.25)' _chemical_formula_sum 'C42 H32 Co4 Gd2 N6 O43' _chemical_formula_weight 1858.95 _chemical_melting_point ? 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system hexagonal _space_group_IT_number 192 _space_group_name_H-M_alt 'P 6/m c c' _space_group_name_Hall '-P 6 2c' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 'x-y, x, z' 3 '-y, x-y, z' 4 '-x, -y, z' 5 '-x+y, -x, z' 6 'y, -x+y, z' 7 'x-y, -y, -z+1/2' 8 '-x, -x+y, -z+1/2' 9 'y, x, -z+1/2' 10 '-y, -x, -z+1/2' 11 '-x+y, y, -z+1/2' 12 'x, x-y, -z+1/2' 13 '-x, -y, -z' 14 '-x+y, -x, -z' 15 'y, -x+y, -z' 16 'x, y, -z' 17 'x-y, x, -z' 18 '-y, x-y, -z' 19 '-x+y, y, z-1/2' 20 'x, x-y, z-1/2' 21 '-y, -x, z-1/2' 22 'y, x, z-1/2' 23 'x-y, -y, z-1/2' 24 '-x, -x+y, z-1/2' _cell_length_a 15.7818(13) _cell_length_b 15.7818(13) _cell_length_c 15.0060(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3236.8(4) _cell_formula_units_Z 2 _cell_measurement_reflns_used 1013 _cell_measurement_temperature 369 _cell_measurement_theta_max 29.0545 _cell_measurement_theta_min 3.0910 _exptl_absorpt_coefficient_mu 3.130 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.25863 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'light violet' _exptl_crystal_density_diffrn 1.907 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 1784 _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_unetI/netI 0.0457 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 2535 _diffrn_reflns_theta_full 23.99 _diffrn_reflns_theta_max 23.99 _diffrn_reflns_theta_min 3.10 _diffrn_ambient_temperature 369 _diffrn_detector_area_resol_mean 16.2116 _diffrn_measured_fraction_theta_full 0.9192 _diffrn_measured_fraction_theta_max 0.9412 _diffrn_measurement_device_type 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0513410000 _diffrn_orient_matrix_UB_12 0.0286569000 _diffrn_orient_matrix_UB_13 0.0061192000 _diffrn_orient_matrix_UB_21 0.0018904000 _diffrn_orient_matrix_UB_22 -0.0426660000 _diffrn_orient_matrix_UB_23 0.0113403000 _diffrn_orient_matrix_UB_31 0.0073677000 _diffrn_orient_matrix_UB_32 -0.0067870000 _diffrn_orient_matrix_UB_33 -0.0454670000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'SuperNova (Mo) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 649 _reflns_number_total 844 _reflns_odcompleteness_completeness 91.92 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELX, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELX, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 1.013 _refine_diff_density_min -2.200 _refine_diff_density_rms 0.152 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 112 _refine_ls_number_reflns 844 _refine_ls_number_restraints 45 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0477 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+32.5500P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1245 _refine_ls_wR_factor_ref 0.1360 _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. EQIV $1 +X,+Y,1-Z DFIX 0.85 H O4 DFIX 2.8 H Co1 DFIX 1.2 H H_$1 ISOR 0.005 0.01 O3 C8 C5 ISOR 0.005 0.01 O6' O6 ISOR 0.01 0.02 O5 O5' ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Gd1 Gd 0.6667 0.3333 0.2500 0.0169(4) Uani 1 6 d S . . Co1 Co 0.5000 0.5000 0.5000 0.0221(6) Uani 1 4 d SD . . O4 O 0.4853(7) 0.3556(7) 0.5000 0.030(2) Uani 1 2 d SD . . H H 0.504(6) 0.330(4) 0.5399(7) 0.046 Uiso 0.50 1 d PD . . O1 O 0.6111(5) 0.4121(5) 0.3584(4) 0.0312(16) Uani 1 1 d . . . O2 O 0.6086(5) 0.5460(5) 0.4045(4) 0.0389(17) Uani 1 1 d . . . C4 C 0.7304(7) 0.5673(7) 0.3017(6) 0.027(2) Uani 1 1 d . . . C5 C 0.7776(7) 0.6658(7) 0.3034(7) 0.040(3) Uani 1 1 d U . . H5 H 0.7560 0.6987 0.3400 0.047 Uiso 1 1 calc R . . C6 C 0.6428(7) 0.5046(7) 0.3596(5) 0.026(2) Uani 1 1 d . . . N7 N 0.7578(4) 0.5156(7) 0.2500 0.023(2) Uani 1 2 d S . . C8 C 0.8584(6) 0.7168(12) 0.2500 0.053(4) Uani 1 2 d SU . . Co2 Co 1.0000 1.0000 0.5000 0.0348(11) Uani 1 12 d S . . O3 O 0.9159(12) 0.8163(10) 0.2802(8) 0.045(4) Uani 0.50 1 d PU . . O6 O 0.901(4) 0.702(3) 0.5000 0.029(11) Uani 0.20 2 d SPU . . O6' O 0.957(2) 0.721(2) 0.5000 0.030(7) Uani 0.30 2 d SPU . . O5' O 0.887(3) 0.929(3) 0.403(3) 0.040(9) Uani 0.17 1 d PU . . O5 O 0.894(3) 0.860(3) 0.470(3) 0.061(14) Uani 0.17 1 d PU . . 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 Gd1 0.0176(5) 0.0176(5) 0.0156(5) 0.000 0.000 0.0088(2) Co1 0.0329(15) 0.0296(14) 0.0138(9) 0.000 0.000 0.0231(12) O4 0.043(6) 0.031(5) 0.023(4) 0.000 0.000 0.023(5) O1 0.043(4) 0.030(4) 0.026(3) 0.001(3) 0.010(3) 0.022(3) O2 0.056(5) 0.035(4) 0.036(3) 0.002(3) 0.017(3) 0.030(4) C4 0.025(5) 0.028(5) 0.033(5) -0.002(4) 0.000(4) 0.018(5) C5 0.033(4) 0.036(4) 0.053(4) -0.006(4) 0.004(3) 0.020(4) C6 0.031(5) 0.028(6) 0.020(4) 0.000(4) 0.001(4) 0.016(5) N7 0.023(4) 0.021(6) 0.024(4) 0.000 0.005(4) 0.010(3) C8 0.046(5) 0.047(5) 0.067(6) 0.000 0.004(4) 0.023(3) Co2 0.0337(17) 0.0337(17) 0.037(2) 0.000 0.000 0.0168(8) O3 0.043(5) 0.040(5) 0.058(6) -0.004(4) 0.004(5) 0.025(4) O6 0.033(14) 0.021(14) 0.034(14) 0.000 0.000 0.015(10) O6' 0.032(11) 0.020(11) 0.037(10) 0.000 0.000 0.014(8) O5' 0.031(12) 0.050(13) 0.049(12) -0.016(9) -0.012(9) 0.028(9) O5 0.061(16) 0.049(16) 0.061(17) -0.015(9) 0.001(9) 0.020(11) _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 Gd1 O1 2.459(6) 3_655 ? Gd1 O1 2.459(6) 10_665 ? Gd1 O1 2.459(6) . ? Gd1 O1 2.459(6) 5_665 ? Gd1 O1 2.459(6) 11_655 ? Gd1 O1 2.459(6) 12 ? Gd1 N7 2.491(10) . ? Gd1 N7 2.491(10) 3_655 ? Gd1 N7 2.491(10) 5_665 ? Co1 O4 2.172(9) . ? Co1 O4 2.172(9) 13_666 ? Co1 O2 2.067(6) 16_556 ? Co1 O2 2.067(6) . ? Co1 O2 2.067(6) 4_665 ? Co1 O2 2.067(6) 13_666 ? O1 C6 1.285(11) . ? O2 C6 1.236(10) . ? C4 C5 1.346(13) . ? C4 C6 1.508(12) . ? C4 N7 1.345(10) . ? C5 C8 1.374(13) . ? N7 C4 1.345(10) 11_655 ? C8 C5 1.374(13) 11_655 ? C8 O3 1.44(2) . ? C8 O3 1.44(2) 11_655 ? Co2 O5 2.05(4) 18_766 ? Co2 O5 2.05(4) 4_775 ? Co2 O5 2.05(4) 13_776 ? Co2 O5 2.05(4) 15_566 ? Co2 O5 2.05(4) 6_565 ? Co2 O5 2.05(4) 3_765 ? Co2 O5 2.05(4) 14_676 ? Co2 O5 2.05(4) 17_656 ? Co2 O5 2.05(4) 2_655 ? Co2 O5 2.05(4) . ? Co2 O5 2.05(4) 16_556 ? Co2 O5 2.05(4) 5_675 ? O3 O3 0.94(2) 11_655 ? O6 O6' 0.77(5) . ? O5' O5' 1.56(4) 6_565 ? O5' O5' 1.56(4) 2_655 ? O5' O5 1.33(5) 6_565 ? O5' O5 1.53(6) . ? O5 O5' 1.33(5) 2_655 ? O5 O5 0.90(8) 16_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 O1 Gd1 O1 81.0(2) 5_665 . ? O1 Gd1 O1 128.1(3) 3_655 10_665 ? O1 Gd1 O1 81.0(2) 12 10_665 ? O1 Gd1 O1 128.1(3) 11_655 . ? O1 Gd1 O1 83.5(3) 10_665 . ? O1 Gd1 O1 81.0(2) 3_655 . ? O1 Gd1 O1 144.0(3) 12 . ? O1 Gd1 O1 81.0(2) 11_655 10_665 ? O1 Gd1 O1 81.0(2) 11_655 12 ? O1 Gd1 O1 128.1(3) 5_665 12 ? O1 Gd1 O1 83.5(3) 5_665 11_655 ? O1 Gd1 O1 81.0(2) 5_665 3_655 ? O1 Gd1 O1 144.0(3) 5_665 10_665 ? O1 Gd1 O1 83.5(3) 12 3_655 ? O1 Gd1 O1 144.0(3) 11_655 3_655 ? O1 Gd1 N7 72.01(15) . 3_655 ? O1 Gd1 N7 72.01(15) 5_665 . ? O1 Gd1 N7 64.05(15) 10_665 3_655 ? O1 Gd1 N7 64.05(15) 3_655 3_655 ? O1 Gd1 N7 64.05(15) 11_655 . ? O1 Gd1 N7 64.05(15) . . ? O1 Gd1 N7 72.01(15) 10_665 . ? O1 Gd1 N7 138.27(14) 3_655 . ? O1 Gd1 N7 138.27(14) 12 . ? O1 Gd1 N7 138.27(14) 10_665 5_665 ? O1 Gd1 N7 72.01(15) 3_655 5_665 ? O1 Gd1 N7 64.05(15) 12 5_665 ? O1 Gd1 N7 72.02(15) 11_655 5_665 ? O1 Gd1 N7 64.05(15) 5_665 5_665 ? O1 Gd1 N7 72.01(15) 12 3_655 ? O1 Gd1 N7 138.27(14) 11_655 3_655 ? O1 Gd1 N7 138.27(14) 5_665 3_655 ? O1 Gd1 N7 138.27(14) . 5_665 ? N7 Gd1 N7 120.0 3_655 . ? N7 Gd1 N7 120.000(1) 5_665 . ? N7 Gd1 N7 120.0 5_665 3_655 ? O4 Co1 O4 180.000(2) . 13_666 ? O2 Co1 O4 89.8(2) . 13_666 ? O2 Co1 O4 90.2(2) 16_556 . ? O2 Co1 O4 89.8(2) 13_666 . ? O2 Co1 O4 89.8(2) 16_556 13_666 ? O2 Co1 O4 90.2(2) 13_666 13_666 ? O2 Co1 O4 90.2(2) 4_665 13_666 ? O2 Co1 O4 89.8(2) 4_665 . ? O2 Co1 O4 90.2(2) . . ? O2 Co1 O2 87.8(4) 4_665 13_666 ? O2 Co1 O2 179.999(1) . 13_666 ? O2 Co1 O2 92.2(4) . 4_665 ? O2 Co1 O2 92.2(4) 13_666 16_556 ? O2 Co1 O2 179.998(1) 4_665 16_556 ? O2 Co1 O2 87.8(4) . 16_556 ? C6 O1 Gd1 123.3(5) . . ? C6 O2 Co1 134.2(6) . . ? C5 C4 C6 122.9(9) . . ? N7 C4 C5 123.4(9) . . ? N7 C4 C6 113.6(8) . . ? C4 C5 C8 118.8(11) . . ? O1 C6 C4 116.5(8) . . ? O2 C6 O1 125.7(9) . . ? O2 C6 C4 117.8(9) . . ? C4 N7 Gd1 121.7(5) 11_655 . ? C4 N7 Gd1 121.7(5) . . ? C4 N7 C4 116.6(11) 11_655 . ? C5 C8 C5 119.1(15) 11_655 . ? C5 C8 O3 110.5(9) . . ? C5 C8 O3 127.5(10) 11_655 . ? C5 C8 O3 127.5(10) . 11_655 ? C5 C8 O3 110.5(9) 11_655 11_655 ? O3 C8 O3 38.1(11) 11_655 . ? O5 Co2 O5 25(2) 18_766 3_765 ? O5 Co2 O5 58.4(3) 4_775 3_765 ? O5 Co2 O5 64.7(8) 13_776 3_765 ? O5 Co2 O5 115.3(8) . 3_765 ? O5 Co2 O5 58.4(3) 5_675 6_565 ? O5 Co2 O5 64.7(8) 14_676 6_565 ? O5 Co2 O5 121.6(3) 17_656 6_565 ? O5 Co2 O5 115.3(8) 2_655 6_565 ? O5 Co2 O5 58.4(3) 2_655 3_765 ? O5 Co2 O5 64.7(8) 4_775 18_766 ? O5 Co2 O5 58.4(3) 13_776 18_766 ? O5 Co2 O5 121.6(3) . 18_766 ? O5 Co2 O5 121.6(3) 16_556 3_765 ? O5 Co2 O5 115.3(8) 5_675 3_765 ? O5 Co2 O5 121.6(3) 14_676 3_765 ? O5 Co2 O5 64.7(8) 17_656 3_765 ? O5 Co2 O5 64.7(8) 16_556 6_565 ? O5 Co2 O5 115.3(8) 13_776 15_566 ? O5 Co2 O5 64.7(8) . 15_566 ? O5 Co2 O5 58.4(3) 16_556 15_566 ? O5 Co2 O5 64.7(8) 5_675 15_566 ? O5 Co2 O5 25(2) 6_565 15_566 ? O5 Co2 O5 179.998(3) 3_765 15_566 ? O5 Co2 O5 155(2) 18_766 15_566 ? O5 Co2 O5 121.6(3) 4_775 15_566 ? O5 Co2 O5 179.998(3) 18_766 6_565 ? O5 Co2 O5 115.3(8) 4_775 6_565 ? O5 Co2 O5 121.6(3) 13_776 6_565 ? O5 Co2 O5 58.4(3) . 6_565 ? O5 Co2 O5 58.4(3) 14_676 15_566 ? O5 Co2 O5 115.3(8) 17_656 15_566 ? O5 Co2 O5 121.6(3) 2_655 15_566 ? O5 Co2 O5 155(2) 3_765 6_565 ? O5 Co2 O5 64.7(8) 17_656 . ? O5 Co2 O5 58.4(3) 2_655 . ? O5 Co2 O5 121.6(3) 5_675 16_556 ? O5 Co2 O5 115.3(8) 14_676 16_556 ? O5 Co2 O5 121.6(3) 2_655 13_776 ? O5 Co2 O5 25(2) 16_556 . ? O5 Co2 O5 115.3(8) 5_675 . ? O5 Co2 O5 121.6(3) 14_676 . ? O5 Co2 O5 155(2) 2_655 5_675 ? O5 Co2 O5 155(2) 17_656 14_676 ? O5 Co2 O5 180.00(2) 2_655 14_676 ? O5 Co2 O5 25(2) 2_655 17_656 ? O5 Co2 O5 58.4(3) 17_656 16_556 ? O5 Co2 O5 64.7(8) 2_655 16_556 ? O5 Co2 O5 25(2) 14_676 5_675 ? O5 Co2 O5 180.00(2) 17_656 5_675 ? O5 Co2 O5 115.3(8) 17_656 13_776 ? O5 Co2 O5 64.7(8) 2_655 18_766 ? O5 Co2 O5 25(2) 13_776 4_775 ? O5 Co2 O5 155(2) . 4_775 ? O5 Co2 O5 179.999(8) 16_556 4_775 ? O5 Co2 O5 115.3(8) 16_556 18_766 ? O5 Co2 O5 121.6(3) 5_675 18_766 ? O5 Co2 O5 115.3(8) 14_676 18_766 ? O5 Co2 O5 58.4(3) 17_656 18_766 ? O5 Co2 O5 180(2) . 13_776 ? O5 Co2 O5 155(2) 16_556 13_776 ? O5 Co2 O5 64.7(8) 5_675 13_776 ? O5 Co2 O5 58.4(3) 14_676 13_776 ? O5 Co2 O5 58.4(3) 5_675 4_775 ? O5 Co2 O5 64.7(8) 14_676 4_775 ? O5 Co2 O5 121.6(3) 17_656 4_775 ? O5 Co2 O5 115.3(8) 2_655 4_775 ? O3 O3 C8 70.9(5) 11_655 . ? O5' O5' Co2 68.6(4) 6_565 . ? O5' O5' Co2 68.6(4) 2_655 . ? O5' O5' O5' 120.00(4) 6_565 2_655 ? O5 O5' Co2 68(2) 6_565 . ? O5 O5' Co2 66(2) . . ? O5 O5' O5' 63(3) 6_565 6_565 ? O5 O5' O5' 133(2) . 6_565 ? O5 O5' O5' 130(2) 6_565 2_655 ? O5 O5' O5' 51(2) . 2_655 ? O5 O5' O5 88(3) 6_565 . ? O5' O5 Co2 75(3) 2_655 . ? O5' O5 Co2 72(2) . . ? O5' O5 O5' 66(3) 2_655 . ? O5 O5 Co2 77.3(11) 16_556 . ? O5 O5 O5' 131(2) 16_556 . ? O5 O5 O5' 139(2) 16_556 2_655 ? # start Validation Reply Form _vrf_PLAT041_ALERT_1_C ; PROBLEM: Check Calc. and Reported SumFormula RESPONSE: Becuse it is difficult to lacate H atoms on guest water molecules, such H atoms is included in formula, but is not in the model. ; # end Validation Reply Form _database_code_depnum_ccdc_archive 'CCDC 958892' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_[Gd(H2CAM)3]_5.25H2O _audit_creation_date 2013-11-01 _audit_creation_method ; Olex2 1.2 (compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C21 H12 Gd N3 O15, 5.25(H2 O)' _chemical_formula_sum 'C21 H22.5 Gd N3 O20.25' _chemical_formula_weight 798.16 _chemical_absolute_configuration ad _chemical_melting_point ? 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' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system trigonal _space_group_IT_number 144 _space_group_name_H-M_alt 'P 31' _space_group_name_Hall 'P 31' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-y, x-y, z+1/3' 3 '-x+y, -x, z+2/3' _cell_length_a 13.9410(9) _cell_length_b 13.9410(9) _cell_length_c 21.8405(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3676.0(4) _cell_formula_units_Z 3 _cell_measurement_reflns_used ? _cell_measurement_temperature 293(2) _cell_measurement_theta_max ? _cell_measurement_theta_min ? _exptl_absorpt_coefficient_mu 1.406 _exptl_absorpt_correction_T_max 0.7663 _exptl_absorpt_correction_T_min 0.7663 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ? _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.082 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1228 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0890 _diffrn_reflns_av_unetI/netI 0.0987 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 20433 _diffrn_reflns_theta_full 25.01 _diffrn_reflns_theta_max 25.01 _diffrn_reflns_theta_min 3.07 _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71075 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 7002 _reflns_number_total 8359 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELX, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 0.802 _refine_diff_density_min -1.199 _refine_diff_density_rms 0.130 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.06(2) _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 319 _refine_ls_number_reflns 8359 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0805 _refine_ls_R_factor_gt 0.0688 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0956P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1646 _refine_ls_wR_factor_ref 0.1714 _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. ISOR 0.005 0.01 O3 O7 ISOR 0.005 0.01 O4 EADP O3BA C5DA C6DA C9CA C1DA N0AA C4BA EADP O9AA C5CA C3CA C8BA N1AA C9BA C4CA EADP O2BA O8AA C0DA EADP O7AA C7BA O6AA EADP O0BA C5BA O5AA EADP O6 O3 EADP O8 O5 EADP O10 O2 ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Gd1 Gd -0.70135(4) -0.03160(4) -0.03906(3) 0.03746(16) Uani 1 1 d . . . N N -0.6892(7) 0.1520(7) -0.0197(4) 0.0404(19) Uani 1 1 d . . . O O -0.7370(7) -0.1569(7) -0.1256(3) 0.054(2) Uani 1 1 d . . . O0AA O -0.8228(6) -0.0615(7) 0.0493(4) 0.0480(19) Uani 1 1 d . . . O1AA O -0.9735(7) -0.1650(7) 0.1045(4) 0.058(2) Uani 1 1 d . . . O2AA O -0.8450(8) -0.3181(8) -0.1726(5) 0.095(4) Uani 1 1 d . . . O3AA O -0.8334(7) -0.0021(7) -0.0929(4) 0.059(2) Uani 1 1 d . . . C5AA C -0.8366(11) 0.0876(12) -0.0942(5) 0.054(3) Uani 1 1 d . . . C6AA C -0.8226(11) -0.2540(12) -0.1305(7) 0.063(4) Uani 1 1 d . . . C7AA C -0.9142(8) -0.1508(9) 0.0587(5) 0.036(2) Uani 1 1 d . . . O4AA O -0.9032(9) 0.1013(8) -0.1255(5) 0.085(3) Uani 1 1 d . . . O5AA O -0.5634(7) 0.0915(7) 0.0371(4) 0.0576(13) Uani 1 1 d . . . O6AA O -0.5837(8) 0.1019(8) -0.1183(4) 0.0722(17) Uani 1 1 d . . . N0AA N -0.5215(10) -0.0249(10) -0.0612(5) 0.0735(14) Uani 1 1 d . . . N1AA N -0.8821(8) -0.2123(8) -0.0362(5) 0.0605(11) Uani 1 1 d . . . C3BA C -0.7564(9) 0.1781(9) -0.0528(5) 0.046(3) Uani 1 1 d . . . C4BA C -0.4604(13) 0.0366(14) -0.1073(7) 0.0735(14) Uani 1 1 d . . . C5BA C -0.5416(11) 0.1904(12) 0.0456(6) 0.0576(13) Uani 1 1 d . . . O7AA O -0.4370(8) 0.1725(7) -0.1808(4) 0.0722(17) Uani 1 1 d . . . C7BA C -0.5002(13) 0.1064(12) -0.1379(7) 0.0722(17) Uani 1 1 d . . . C8BA C -0.9518(11) -0.2390(10) 0.0135(6) 0.0605(11) Uani 1 1 d . . . C9BA C -0.9101(10) -0.2873(10) -0.0823(6) 0.0605(11) Uani 1 1 d . . . O8AA O -0.6659(8) -0.1590(8) 0.0163(4) 0.0702(16) Uani 1 1 d . . . O9AA O -1.1696(7) -0.5133(6) -0.0293(4) 0.0605(11) Uani 1 1 d . . . H9AA H -1.1583 -0.5623 -0.0418 0.091 Uiso 1 1 calc R . . O0BA O -0.4679(6) 0.2576(7) 0.0818(4) 0.0576(13) Uani 1 1 d . . . C3CA C -1.0461(10) -0.3359(9) 0.0173(6) 0.0605(11) Uani 1 1 d . . . H3CA H -1.0938 -0.3500 0.0502 0.073 Uiso 1 1 calc R . . C4CA C -1.0024(10) -0.3866(10) -0.0825(6) 0.0605(11) Uani 1 1 d . . . H4CA H -1.0209 -0.4347 -0.1156 0.073 Uiso 1 1 calc R . . C5CA C -1.0729(10) -0.4159(10) -0.0279(6) 0.0605(11) Uani 1 1 d . . . C6CA C -0.7454(10) 0.2821(9) -0.0508(6) 0.056(3) Uani 1 1 d . . . H6CA H -0.7949 0.2968 -0.0715 0.067 Uiso 1 1 calc R . . O1BA O -0.6447(9) 0.4689(8) -0.0154(6) 0.087(3) Uani 1 1 d . . . H1BA H -0.5799 0.5155 -0.0220 0.131 Uiso 1 1 calc R . . O2BA O -0.5560(8) -0.2268(8) 0.0443(4) 0.0702(16) Uani 1 1 d . . . C9CA C -0.4024(11) -0.1014(12) -0.0498(6) 0.0735(14) Uani 1 1 d . . . H9CA H -0.3861 -0.1491 -0.0283 0.088 Uiso 1 1 calc R . . C0DA C -0.5808(12) -0.1686(13) 0.0125(7) 0.0702(16) Uani 1 1 d . . . C1DA C -0.4999(12) -0.0939(13) -0.0338(7) 0.0735(14) Uani 1 1 d . . . C2DA C -0.5924(10) 0.3367(9) 0.0176(7) 0.061(3) Uani 1 1 d . . . H2DA H -0.5366 0.3885 0.0427 0.074 Uiso 1 1 calc R . . C3DA C -0.6561(10) 0.3667(10) -0.0162(7) 0.066(4) Uani 1 1 d . . . C4DA C -0.6114(10) 0.2274(10) 0.0144(5) 0.048(3) Uani 1 1 d . . . C5DA C -0.3349(12) -0.0385(13) -0.0963(6) 0.0735(14) Uani 1 1 d . . . C6DA C -0.3645(12) 0.0302(13) -0.1266(7) 0.0735(14) Uani 1 1 d . . . H6DA H -0.3225 0.0725 -0.1596 0.088 Uiso 1 1 calc R . . O3BA O -0.2482(8) -0.0444(8) -0.1130(4) 0.0735(14) Uani 1 1 d . . . H3BA H -0.1919 0.0134 -0.1040 0.110 Uiso 1 1 calc R . . O1 O -0.2757(8) 0.4629(8) 0.0750(5) 0.039(3) Uani 0.60 1 d P . . O2 O -0.4900(13) 0.3344(14) -0.2044(7) 0.058(4) Uani 0.50 1 d P . . O3 O -1.0399(11) -0.0965(11) -0.1795(7) 0.045(3) Uani 0.50 1 d PU . . O5 O -0.6434(14) -0.2635(14) -0.2287(6) 0.058(3) Uani 0.50 1 d P . . O7 O -0.4497(11) 0.6097(11) 0.0346(7) 0.051(4) Uani 0.50 1 d PU . . O6 O -1.0926(17) -0.1704(17) -0.1250(10) 0.045(3) Uani 0.33 1 d P . . O8 O -0.562(2) -0.251(2) -0.1769(9) 0.058(3) Uani 0.33 1 d P . . O10 O -0.510(2) 0.3954(18) -0.1545(11) 0.058(4) Uani 0.33 1 d P . . O4 O -0.3494(13) 0.6847(14) 0.1137(9) 0.047(5) Uani 0.40 1 d PU . . 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 Gd1 0.0383(3) 0.0350(3) 0.0397(2) -0.0003(2) -0.0004(2) 0.0188(2) N 0.050(5) 0.032(4) 0.038(5) -0.003(4) -0.006(4) 0.019(4) O 0.063(5) 0.062(5) 0.036(4) -0.006(4) 0.012(4) 0.031(5) O0AA 0.044(4) 0.051(5) 0.049(4) -0.015(4) 0.004(4) 0.024(4) O1AA 0.050(5) 0.065(5) 0.047(5) -0.016(4) -0.009(4) 0.021(4) O2AA 0.073(6) 0.063(6) 0.115(8) -0.064(6) 0.027(6) 0.008(5) O3AA 0.069(5) 0.056(5) 0.066(5) -0.020(4) -0.016(4) 0.042(4) C5AA 0.058(8) 0.074(9) 0.036(6) -0.016(6) -0.023(6) 0.038(7) C6AA 0.044(7) 0.055(8) 0.073(9) -0.003(7) 0.003(7) 0.011(6) C7AA 0.027(5) 0.055(7) 0.033(5) 0.003(5) 0.013(4) 0.027(5) O4AA 0.090(7) 0.068(6) 0.108(8) -0.009(6) -0.044(7) 0.048(6) O5AA 0.045(3) 0.058(3) 0.067(3) -0.011(3) -0.021(2) 0.025(3) O6AA 0.080(4) 0.066(4) 0.084(4) 0.041(3) 0.037(3) 0.046(3) N0AA 0.075(3) 0.093(4) 0.076(3) 0.024(3) 0.016(3) 0.059(3) N1AA 0.058(3) 0.043(2) 0.069(3) -0.009(2) -0.002(2) 0.0168(19) C3BA 0.043(6) 0.051(6) 0.040(6) -0.010(5) -0.001(5) 0.019(5) C4BA 0.075(3) 0.093(4) 0.076(3) 0.024(3) 0.016(3) 0.059(3) C5BA 0.045(3) 0.058(3) 0.067(3) -0.011(3) -0.021(2) 0.025(3) O7AA 0.080(4) 0.066(4) 0.084(4) 0.041(3) 0.037(3) 0.046(3) C7BA 0.080(4) 0.066(4) 0.084(4) 0.041(3) 0.037(3) 0.046(3) C8BA 0.058(3) 0.043(2) 0.069(3) -0.009(2) -0.002(2) 0.0168(19) C9BA 0.058(3) 0.043(2) 0.069(3) -0.009(2) -0.002(2) 0.0168(19) O8AA 0.079(4) 0.083(4) 0.075(4) 0.030(3) 0.020(3) 0.060(3) O9AA 0.058(3) 0.043(2) 0.069(3) -0.009(2) -0.002(2) 0.0168(19) O0BA 0.045(3) 0.058(3) 0.067(3) -0.011(3) -0.021(2) 0.025(3) C3CA 0.058(3) 0.043(2) 0.069(3) -0.009(2) -0.002(2) 0.0168(19) C4CA 0.058(3) 0.043(2) 0.069(3) -0.009(2) -0.002(2) 0.0168(19) C5CA 0.058(3) 0.043(2) 0.069(3) -0.009(2) -0.002(2) 0.0168(19) C6CA 0.054(7) 0.044(6) 0.078(8) -0.017(6) -0.017(6) 0.031(6) O1BA 0.096(8) 0.066(6) 0.107(8) -0.015(6) -0.024(7) 0.047(6) O2BA 0.079(4) 0.083(4) 0.075(4) 0.030(3) 0.020(3) 0.060(3) C9CA 0.075(3) 0.093(4) 0.076(3) 0.024(3) 0.016(3) 0.059(3) C0DA 0.079(4) 0.083(4) 0.075(4) 0.030(3) 0.020(3) 0.060(3) C1DA 0.075(3) 0.093(4) 0.076(3) 0.024(3) 0.016(3) 0.059(3) C2DA 0.049(7) 0.038(6) 0.093(10) -0.022(6) -0.005(7) 0.019(5) C3DA 0.061(8) 0.054(7) 0.102(10) -0.011(7) -0.021(7) 0.043(7) C4DA 0.046(7) 0.052(7) 0.048(6) 0.000(6) -0.013(5) 0.028(6) C5DA 0.075(3) 0.093(4) 0.076(3) 0.024(3) 0.016(3) 0.059(3) C6DA 0.075(3) 0.093(4) 0.076(3) 0.024(3) 0.016(3) 0.059(3) O3BA 0.075(3) 0.093(4) 0.076(3) 0.024(3) 0.016(3) 0.059(3) O1 0.022(5) 0.023(5) 0.065(7) 0.009(5) -0.003(5) 0.006(4) O2 0.074(9) 0.045(7) 0.063(8) 0.023(6) 0.043(8) 0.036(7) O3 0.042(5) 0.045(6) 0.058(6) -0.013(5) -0.020(5) 0.029(5) O5 0.069(9) 0.075(9) 0.036(6) -0.015(6) 0.003(6) 0.041(8) O7 0.036(6) 0.033(6) 0.083(8) 0.007(6) -0.004(6) 0.017(5) O6 0.042(5) 0.045(6) 0.058(6) -0.013(5) -0.020(5) 0.029(5) O8 0.069(9) 0.075(9) 0.036(6) -0.015(6) 0.003(6) 0.041(8) O10 0.074(9) 0.045(7) 0.063(8) 0.023(6) 0.043(8) 0.036(7) O4 0.038(7) 0.045(7) 0.061(10) -0.013(6) 0.010(6) 0.022(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 Gd1 N 2.515(8) . ? Gd1 O 2.450(8) . ? Gd1 O0AA 2.462(7) . ? Gd1 O3AA 2.387(8) . ? Gd1 O5AA 2.472(8) . ? Gd1 O6AA 2.470(8) . ? Gd1 N0AA 2.509(11) . ? Gd1 N1AA 2.520(9) . ? Gd1 O8AA 2.395(8) . ? N C3BA 1.368(14) . ? N C4DA 1.303(14) . ? O C6AA 1.286(15) . ? O0AA C7AA 1.277(13) . ? O1AA C7AA 1.249(12) . ? O2AA C6AA 1.210(16) . ? O3AA C5AA 1.274(15) . ? C5AA O4AA 1.242(14) . ? C5AA C3BA 1.499(16) . ? C6AA C9BA 1.498(19) . ? C7AA C8BA 1.455(16) . ? O5AA C5BA 1.268(17) . ? O6AA C7BA 1.211(16) . ? N0AA C4BA 1.320(18) . ? N0AA C1DA 1.289(17) . ? N1AA C8BA 1.377(16) . ? N1AA C9BA 1.361(15) . ? C3BA C6CA 1.381(15) . ? C4BA C7BA 1.498(19) . ? C4BA C6DA 1.446(19) . ? C5BA O0BA 1.262(14) . ? C5BA C4DA 1.476(17) . ? O7AA C7BA 1.301(15) . ? C8BA C3CA 1.335(17) . ? C9BA C4CA 1.338(16) . ? O8AA C0DA 1.261(15) . ? O9AA C5CA 1.353(14) . ? C3CA C5CA 1.394(17) . ? C4CA C5CA 1.468(18) . ? C6CA C3DA 1.429(17) . ? O1BA C3DA 1.353(14) . ? O2BA C0DA 1.241(14) . ? C9CA C1DA 1.457(18) . ? C9CA C5DA 1.363(18) . ? C0DA C1DA 1.486(19) . ? C2DA C3DA 1.371(17) . ? C2DA C4DA 1.412(16) . ? C5DA C6DA 1.386(18) . ? C5DA O3BA 1.304(15) . ? O2 O10 1.49(3) . ? O3 O6 1.50(3) . ? O5 O8 1.55(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 N Gd1 N1AA 122.5(3) . . ? O Gd1 N 137.9(3) . . ? O Gd1 O0AA 127.4(2) . . ? O Gd1 O5AA 145.5(3) . . ? O Gd1 O6AA 79.5(3) . . ? O Gd1 N0AA 73.8(4) . . ? O Gd1 N1AA 64.0(3) . . ? O0AA Gd1 N 74.4(3) . . ? O0AA Gd1 O5AA 79.7(3) . . ? O0AA Gd1 O6AA 145.0(3) . . ? O0AA Gd1 N0AA 138.4(3) . . ? O0AA Gd1 N1AA 63.4(3) . . ? O3AA Gd1 N 64.7(3) . . ? O3AA Gd1 O 81.0(3) . . ? O3AA Gd1 O0AA 83.8(3) . . ? O3AA Gd1 O5AA 127.7(3) . . ? O3AA Gd1 O6AA 78.7(3) . . ? O3AA Gd1 N0AA 137.8(3) . . ? O3AA Gd1 N1AA 73.3(3) . . ? O3AA Gd1 O8AA 147.1(3) . . ? O5AA Gd1 N 63.1(3) . . ? O5AA Gd1 N0AA 71.8(4) . . ? O5AA Gd1 N1AA 136.0(3) . . ? O6AA Gd1 N 70.7(3) . . ? O6AA Gd1 O5AA 87.5(3) . . ? O6AA Gd1 N0AA 64.0(3) . . ? O6AA Gd1 N1AA 136.6(4) . . ? N0AA Gd1 N 115.9(3) . . ? N0AA Gd1 N1AA 121.5(4) . . ? O8AA Gd1 N 137.4(3) . . ? O8AA Gd1 O 84.5(3) . . ? O8AA Gd1 O0AA 81.8(3) . . ? O8AA Gd1 O5AA 78.3(3) . . ? O8AA Gd1 O6AA 127.4(3) . . ? O8AA Gd1 N0AA 63.4(3) . . ? O8AA Gd1 N1AA 73.7(4) . . ? C3BA N Gd1 118.4(6) . . ? C4DA N Gd1 121.5(7) . . ? C4DA N C3BA 119.5(9) . . ? C6AA O Gd1 124.4(8) . . ? C7AA O0AA Gd1 123.9(6) . . ? C5AA O3AA Gd1 126.1(7) . . ? O3AA C5AA C3BA 115.8(10) . . ? O4AA C5AA O3AA 124.0(11) . . ? O4AA C5AA C3BA 120.2(12) . . ? O C6AA C9BA 116.8(12) . . ? O2AA C6AA O 126.9(13) . . ? O2AA C6AA C9BA 115.9(11) . . ? O0AA C7AA C8BA 118.5(9) . . ? O1AA C7AA O0AA 122.8(10) . . ? O1AA C7AA C8BA 118.7(10) . . ? C5BA O5AA Gd1 122.3(8) . . ? C7BA O6AA Gd1 123.0(8) . . ? C4BA N0AA Gd1 118.7(9) . . ? C1DA N0AA Gd1 119.0(9) . . ? C1DA N0AA C4BA 121.5(12) . . ? C8BA N1AA Gd1 120.5(7) . . ? C9BA N1AA Gd1 120.6(8) . . ? C9BA N1AA C8BA 118.8(10) . . ? N C3BA C5AA 114.6(10) . . ? N C3BA C6CA 122.1(10) . . ? C6CA C3BA C5AA 123.2(11) . . ? N0AA C4BA C7BA 115.7(12) . . ? N0AA C4BA C6DA 119.9(12) . . ? C6DA C4BA C7BA 124.4(12) . . ? O5AA C5BA C4DA 118.1(11) . . ? O0BA C5BA O5AA 124.2(12) . . ? O0BA C5BA C4DA 117.7(12) . . ? O6AA C7BA C4BA 117.9(11) . . ? O6AA C7BA O7AA 125.8(12) . . ? O7AA C7BA C4BA 116.2(12) . . ? N1AA C8BA C7AA 113.5(10) . . ? C3CA C8BA C7AA 124.6(12) . . ? C3CA C8BA N1AA 121.9(11) . . ? N1AA C9BA C6AA 113.9(11) . . ? C4CA C9BA C6AA 122.0(11) . . ? C4CA C9BA N1AA 123.8(12) . . ? C0DA O8AA Gd1 126.9(8) . . ? C8BA C3CA C5CA 119.9(13) . . ? C9BA C4CA C5CA 116.6(11) . . ? O9AA C5CA C3CA 123.5(12) . . ? O9AA C5CA C4CA 117.0(10) . . ? C3CA C5CA C4CA 118.6(11) . . ? C3BA C6CA C3DA 118.5(10) . . ? C5DA C9CA C1DA 120.0(12) . . ? O8AA C0DA C1DA 113.3(11) . . ? O2BA C0DA O8AA 128.2(13) . . ? O2BA C0DA C1DA 118.4(12) . . ? N0AA C1DA C9CA 121.1(12) . . ? N0AA C1DA C0DA 117.4(12) . . ? C9CA C1DA C0DA 121.5(12) . . ? C3DA C2DA C4DA 120.2(11) . . ? O1BA C3DA C6CA 118.1(10) . . ? O1BA C3DA C2DA 124.1(12) . . ? C2DA C3DA C6CA 117.6(10) . . ? N C4DA C5BA 114.3(11) . . ? N C4DA C2DA 122.0(10) . . ? C2DA C4DA C5BA 123.6(11) . . ? C9CA C5DA C6DA 116.8(12) . . ? O3BA C5DA C9CA 122.1(12) . . ? O3BA C5DA C6DA 121.0(12) . . ? C5DA C6DA C4BA 120.5(13) . . ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.331 0.552 0.925 1477 386 ' ' _platon_squeeze_details ; One point two five water molecules are highly disordered. Therefore, the SQUEEZE routine of PLATON was applied. The final formula was calculated from the elemental analysis data. ; # start Validation Reply Form _vrf_CHEMW03_ALERT_2_C ; PROBLEM: The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.99 <> 1.01 RESPONSE: This is a consequence of the use of SQUEEZE. The solvent is included in formula, but is not in the model. ; _vrf_PLAT041_ALERT_1_C ; PROBLEM: Calc. and Reported SumFormula Differ RESPONSE: This is a consequence of the use of SQUEEZE. The solvent is included in formula, but is not in the model. ; _vrf_PLAT068_ALERT_1_C ; PROBLEM: Reported F000 Differs from Calcd RESPONSE: This is a consequence of the use of SQUEEZE. The solvent is included in formula, but is not in the model. ; # end Validation Reply Form _database_code_depnum_ccdc_archive 'CCDC 937632'