# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Yan Xing' _publ_contact_author_email XINGYAN69CN@YAHOO.COM.CN _publ_section_title ; Chirality and Magnetism of an Open-framework Cobalt Phosphite Containing Helical Channels from Achiral Materials ; loop_ _publ_author_name 'Yan Xing' 'Xianchun Liu' 'Xizheng Liu' 'Kuizhan Shaoa' 'Zhongmin Su' ; Xinlong Wang ; 'Hongbin Xu' data_Xing _database_code_depnum_ccdc_archive 'CCDC 723093' #TrackingRef 'Co_xing1_723093.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'Co H2 O6 P2, C6 H14 N2' _chemical_formula_sum 'C6 H16 Co N2 O6 P2' _chemical_formula_weight 333.08 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' 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' P P 0.1023 0.0942 '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 orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' 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' _cell_length_a 10.1040(4) _cell_length_b 10.8100(5) _cell_length_c 10.9930(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1200.70(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1387 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 26.07 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.843 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 684 _exptl_absorpt_coefficient_mu 1.713 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7149 _exptl_absorpt_correction_T_max 0.7711 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 6673 _diffrn_reflns_av_R_equivalents 0.0180 _diffrn_reflns_av_sigmaI/netI 0.0267 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 26.07 _reflns_number_total 2368 _reflns_number_gt 2272 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT software (Bruker, 1999)' _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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^)+(0.0384P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.034(14) _refine_ls_number_reflns 2368 _refine_ls_number_parameters 168 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0221 _refine_ls_R_factor_gt 0.0209 _refine_ls_wR_factor_ref 0.0608 _refine_ls_wR_factor_gt 0.0603 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _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 C1 C 0.4931(3) -0.3266(3) -0.1626(2) 0.0347(6) Uani 1 1 d . . . H1A H 0.4686 -0.2499 -0.2025 0.042 Uiso 1 1 calc R . . H1B H 0.5860 -0.3423 -0.1786 0.042 Uiso 1 1 calc R . . C2 C 0.4279(3) -0.5422(2) -0.1317(2) 0.0302(5) Uani 1 1 d . . . H2A H 0.5213 -0.5594 -0.1204 0.036 Uiso 1 1 calc R . . H2B H 0.3871 -0.6136 -0.1697 0.036 Uiso 1 1 calc R . . C3 C 0.2369(2) -0.3407(2) -0.0817(2) 0.0319(6) Uani 1 1 d . . . H3A H 0.2326 -0.2511 -0.0843 0.038 Uiso 1 1 calc R . . H3B H 0.1519 -0.3719 -0.0545 0.038 Uiso 1 1 calc R . . C4 C 0.4697(2) -0.3164(2) -0.0275(2) 0.0327(6) Uani 1 1 d . . . H4C H 0.5426 -0.3540 0.0165 0.039 Uiso 1 1 calc R . . H4D H 0.4643 -0.2300 -0.0040 0.039 Uiso 1 1 calc R . . C5 C 0.3622(2) -0.5162(2) -0.0081(2) 0.0301(5) Uani 1 1 d . . . H5A H 0.2775 -0.5582 -0.0033 0.036 Uiso 1 1 calc R . . H5B H 0.4180 -0.5462 0.0574 0.036 Uiso 1 1 calc R . . C6 C 0.2690(2) -0.3916(2) -0.2080(3) 0.0312(5) Uani 1 1 d . . . H6C H 0.2123 -0.4617 -0.2260 0.037 Uiso 1 1 calc R . . H6D H 0.2536 -0.3284 -0.2690 0.037 Uiso 1 1 calc R . . N1 N 0.41075(18) -0.43076(18) -0.2103(2) 0.0257(4) Uani 1 1 d . . . N2 N 0.34306(19) -0.38095(18) 0.00329(19) 0.0264(4) Uani 1 1 d . . . O1 O 0.20019(18) 0.02758(18) 0.54562(15) 0.0371(5) Uani 1 1 d . . . O2 O 0.5534(2) -0.34242(17) 0.2682(2) 0.0460(5) Uani 1 1 d . . . O3 O 0.30965(18) -0.30847(19) 0.22555(17) 0.0373(4) Uani 1 1 d . . . O4 O 0.19918(16) 0.02642(18) 0.31719(15) 0.0334(4) Uani 1 1 d . . . O5 O -0.00834(16) -0.0241(2) 0.42845(15) 0.0391(5) Uani 1 1 d . . . O6 O 0.46362(16) -0.13166(15) 0.2761(2) 0.0369(4) Uani 1 1 d . . . P1 P 0.14181(6) -0.02975(5) 0.43213(5) 0.02426(14) Uani 1 1 d D . . P2 P 0.43154(6) -0.26680(5) 0.29475(6) 0.02442(13) Uani 1 1 d D . . Co1 Co 0.35445(3) 0.00184(3) 0.21405(3) 0.02118(9) Uani 1 1 d . . . H1 H 0.168(3) -0.1531(10) 0.434(2) 0.032 Uiso 1 1 d D . . H1N H 0.437(3) -0.454(3) -0.302(3) 0.048(9) Uiso 1 1 d . . . H2 H 0.405(3) -0.277(4) 0.4166(11) 0.072 Uiso 1 1 d D . . H2N H 0.327(3) -0.360(3) 0.080(3) 0.056(10) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0301(13) 0.0383(14) 0.0356(14) -0.0011(12) 0.0076(12) -0.0089(11) C2 0.0315(12) 0.0271(12) 0.0322(13) -0.0035(10) 0.0003(11) 0.0058(10) C3 0.0244(12) 0.0320(13) 0.0392(15) -0.0021(12) 0.0001(11) 0.0041(9) C4 0.0277(12) 0.0348(13) 0.0358(14) -0.0088(11) 0.0001(11) -0.0090(11) C5 0.0344(11) 0.0286(12) 0.0273(11) 0.0024(10) -0.0001(11) -0.0004(12) C6 0.0265(11) 0.0373(13) 0.0296(12) 0.0002(12) -0.0060(11) 0.0052(10) N1 0.0249(9) 0.0317(10) 0.0204(9) -0.0030(9) 0.0021(9) 0.0003(8) N2 0.0265(10) 0.0298(10) 0.0229(10) -0.0055(8) 0.0029(10) -0.0013(9) O1 0.0411(10) 0.0511(12) 0.0191(8) -0.0019(8) -0.0018(7) -0.0142(9) O2 0.0477(11) 0.0269(9) 0.0633(14) 0.0056(10) 0.0122(11) 0.0137(8) O3 0.0352(9) 0.0450(10) 0.0315(10) -0.0118(9) 0.0076(8) -0.0142(8) O4 0.0306(8) 0.0474(11) 0.0222(9) 0.0020(8) 0.0077(7) 0.0022(8) O5 0.0246(8) 0.0688(14) 0.0240(8) -0.0034(10) 0.0032(7) -0.0055(9) O6 0.0342(9) 0.0204(8) 0.0559(12) -0.0007(9) -0.0132(9) 0.0015(8) P1 0.0270(3) 0.0293(3) 0.0164(3) -0.0010(2) 0.0006(3) -0.0016(2) P2 0.0301(3) 0.0196(3) 0.0236(3) -0.0009(2) 0.0023(3) 0.0021(2) Co1 0.02211(14) 0.02190(15) 0.01953(15) -0.00003(13) 0.00067(12) -0.00081(13) _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 C1 N1 1.495(3) . ? C1 C4 1.508(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N1 1.493(3) . ? C2 C5 1.538(3) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N2 1.487(3) . ? C3 C6 1.528(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N2 1.497(3) . ? C4 H4C 0.9700 . ? C4 H4D 0.9700 . ? C5 N2 1.480(3) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N1 1.494(3) . ? C6 H6C 0.9700 . ? C6 H6D 0.9700 . ? N1 H1N 1.07(3) . ? N2 H2N 0.89(4) . ? O1 P1 1.5128(18) . ? O1 Co1 1.9581(17) 2 ? O2 P2 1.5066(19) . ? O2 Co1 1.9337(18) 4_645 ? O3 P2 1.5160(19) . ? O4 P1 1.5170(17) . ? O4 Co1 1.9538(16) . ? O5 P1 1.5189(17) . ? O6 P2 1.5104(17) . ? O6 Co1 1.9403(17) . ? P1 H1 1.360(10) . ? P2 H2 1.371(10) . ? Co1 O2 1.9337(18) 4_655 ? Co1 O1 1.9581(17) 2_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 N1 C1 C4 108.3(2) . . ? N1 C1 H1A 110.0 . . ? C4 C1 H1A 110.0 . . ? N1 C1 H1B 110.0 . . ? C4 C1 H1B 110.0 . . ? H1A C1 H1B 108.4 . . ? N1 C2 C5 108.31(18) . . ? N1 C2 H2A 110.0 . . ? C5 C2 H2A 110.0 . . ? N1 C2 H2B 110.0 . . ? C5 C2 H2B 110.0 . . ? H2A C2 H2B 108.4 . . ? N2 C3 C6 108.25(19) . . ? N2 C3 H3A 110.0 . . ? C6 C3 H3A 110.0 . . ? N2 C3 H3B 110.0 . . ? C6 C3 H3B 110.0 . . ? H3A C3 H3B 108.4 . . ? N2 C4 C1 108.8(2) . . ? N2 C4 H4C 109.9 . . ? C1 C4 H4C 109.9 . . ? N2 C4 H4D 109.9 . . ? C1 C4 H4D 109.9 . . ? H4C C4 H4D 108.3 . . ? N2 C5 C2 108.14(19) . . ? N2 C5 H5A 110.1 . . ? C2 C5 H5A 110.1 . . ? N2 C5 H5B 110.1 . . ? C2 C5 H5B 110.1 . . ? H5A C5 H5B 108.4 . . ? N1 C6 C3 108.7(2) . . ? N1 C6 H6C 110.0 . . ? C3 C6 H6C 110.0 . . ? N1 C6 H6D 110.0 . . ? C3 C6 H6D 110.0 . . ? H6C C6 H6D 108.3 . . ? C2 N1 C6 109.30(18) . . ? C2 N1 C1 109.86(19) . . ? C6 N1 C1 108.3(2) . . ? C2 N1 H1N 109.0(17) . . ? C6 N1 H1N 108.6(17) . . ? C1 N1 H1N 111.8(16) . . ? C5 N2 C3 109.25(19) . . ? C5 N2 C4 109.28(18) . . ? C3 N2 C4 109.8(2) . . ? C5 N2 H2N 111(2) . . ? C3 N2 H2N 113(2) . . ? C4 N2 H2N 105(2) . . ? P1 O1 Co1 127.11(11) . 2 ? P2 O2 Co1 147.82(13) . 4_645 ? P1 O4 Co1 137.37(11) . . ? P2 O6 Co1 130.17(11) . . ? O1 P1 O4 111.96(10) . . ? O1 P1 O5 113.26(11) . . ? O4 P1 O5 110.08(10) . . ? O1 P1 H1 108.2(11) . . ? O4 P1 H1 109.4(11) . . ? O5 P1 H1 103.5(11) . . ? O2 P2 O6 108.85(11) . . ? O2 P2 O3 113.91(12) . . ? O6 P2 O3 113.18(11) . . ? O2 P2 H2 107.7(15) . . ? O6 P2 H2 104.8(16) . . ? O3 P2 H2 107.8(15) . . ? O2 Co1 O6 109.77(8) 4_655 . ? O2 Co1 O4 102.10(8) 4_655 . ? O6 Co1 O4 110.71(8) . . ? O2 Co1 O1 111.88(9) 4_655 2_554 ? O6 Co1 O1 111.83(9) . 2_554 ? O4 Co1 O1 110.15(7) . 2_554 ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C4 N2 -19.2(3) . . . . ? N1 C2 C5 N2 -17.4(3) . . . . ? N2 C3 C6 N1 -16.2(3) . . . . ? C5 C2 N1 C6 -49.3(3) . . . . ? C5 C2 N1 C1 69.4(2) . . . . ? C3 C6 N1 C2 69.2(2) . . . . ? C3 C6 N1 C1 -50.5(3) . . . . ? C4 C1 N1 C2 -47.8(3) . . . . ? C4 C1 N1 C6 71.5(3) . . . . ? C2 C5 N2 C3 71.0(2) . . . . ? C2 C5 N2 C4 -49.2(3) . . . . ? C6 C3 N2 C5 -51.1(2) . . . . ? C6 C3 N2 C4 68.7(2) . . . . ? C1 C4 N2 C5 71.6(3) . . . . ? C1 C4 N2 C3 -48.2(3) . . . . ? Co1 O1 P1 O4 173.41(13) 2 . . . ? Co1 O1 P1 O5 48.22(18) 2 . . . ? Co1 O4 P1 O1 85.07(19) . . . . ? Co1 O4 P1 O5 -148.01(16) . . . . ? Co1 O2 P2 O6 161.8(3) 4_645 . . . ? Co1 O2 P2 O3 -70.8(3) 4_645 . . . ? Co1 O6 P2 O2 144.91(17) . . . . ? Co1 O6 P2 O3 17.2(2) . . . . ? P2 O6 Co1 O2 172.85(15) . . . 4_655 ? P2 O6 Co1 O4 60.88(19) . . . . ? P2 O6 Co1 O1 -62.36(19) . . . 2_554 ? P1 O4 Co1 O2 -116.36(18) . . . 4_655 ? P1 O4 Co1 O6 0.4(2) . . . . ? P1 O4 Co1 O1 124.64(16) . . . 2_554 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2N O3 0.89(4) 1.70(4) 2.588(3) 174(3) . N1 H1N O5 1.07(3) 1.52(3) 2.580(3) 172(3) 3_545 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.607 _refine_diff_density_min -0.300 _refine_diff_density_rms 0.053 # Attachment 'Co_xing2_723094.cif' data_Xing2 _database_code_depnum_ccdc_archive 'CCDC 723094' #TrackingRef 'Co_xing2_723094.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'Co H2 O6 P2, C6 H14 N2' _chemical_formula_sum 'C6 H16 Co N2 O6 P2' _chemical_formula_weight 333.08 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' 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' P P 0.1023 0.0942 '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 orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' 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' _cell_length_a 10.100(5) _cell_length_b 10.796(5) _cell_length_c 10.982(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 90.000(5) _cell_volume 1197.5(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1384 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 26.08 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.848 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 684 _exptl_absorpt_coefficient_mu 1.718 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5846 _exptl_absorpt_correction_T_max 0.7473 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 6670 _diffrn_reflns_av_R_equivalents 0.0180 _diffrn_reflns_av_sigmaI/netI 0.0267 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 26.08 _reflns_number_total 2375 _reflns_number_gt 2255 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT software (Bruker, 1999)' _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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^)+(0.0460P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.031(15) _refine_ls_number_reflns 2375 _refine_ls_number_parameters 168 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0251 _refine_ls_R_factor_gt 0.0237 _refine_ls_wR_factor_ref 0.0684 _refine_ls_wR_factor_gt 0.0676 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.35434(3) 0.00172(3) 0.28591(3) 0.02088(10) Uani 1 1 d . . . P1 P 0.35797(7) 0.02994(6) 0.56779(6) 0.02417(16) Uani 1 1 d D . . P2 P 0.43194(7) -0.26685(6) 0.20513(6) 0.02401(15) Uani 1 1 d D . . O4 O 0.46394(18) -0.13159(18) 0.2243(2) 0.0365(5) Uani 1 1 d . . . O1 O 0.30092(18) -0.0267(2) 0.68262(16) 0.0331(5) Uani 1 1 d . . . O2 O 0.50788(19) 0.0247(2) 0.57124(17) 0.0393(5) Uani 1 1 d . . . O5 O 0.3098(2) -0.3087(2) 0.27417(19) 0.0365(5) Uani 1 1 d . . . O6 O 0.5533(2) -0.3425(2) 0.2319(2) 0.0453(6) Uani 1 1 d . . . N2 N 0.3433(2) -0.3811(2) 0.4968(2) 0.0258(5) Uani 1 1 d . . . O3 O 0.2997(2) -0.0279(2) 0.45440(17) 0.0371(5) Uani 1 1 d . . . N1 N 0.4107(2) -0.4305(2) 0.7104(2) 0.0253(5) Uani 1 1 d . . . C6 C 0.2371(3) -0.3408(3) 0.5815(3) 0.0315(6) Uani 1 1 d . . . H6A H 0.1521 -0.3721 0.5542 0.038 Uiso 1 1 calc R . . H6B H 0.2327 -0.2510 0.5839 0.038 Uiso 1 1 calc R . . C5 C 0.3626(3) -0.5160(2) 0.5080(2) 0.0295(5) Uani 1 1 d . . . H5A H 0.4185 -0.5459 0.4425 0.035 Uiso 1 1 calc R . . H5B H 0.2780 -0.5582 0.5032 0.035 Uiso 1 1 calc R . . C4 C 0.4700(3) -0.3165(3) 0.5273(3) 0.0323(7) Uani 1 1 d . . . H4A H 0.4646 -0.2300 0.5037 0.039 Uiso 1 1 calc R . . H4B H 0.5428 -0.3543 0.4834 0.039 Uiso 1 1 calc R . . C1 C 0.4930(3) -0.3266(3) 0.6623(3) 0.0335(7) Uani 1 1 d . . . H1A H 0.5859 -0.3424 0.6784 0.040 Uiso 1 1 calc R . . H1B H 0.4685 -0.2497 0.7021 0.040 Uiso 1 1 calc R . . C3 C 0.2693(3) -0.3916(3) 0.7079(3) 0.0311(6) Uani 1 1 d . . . H3A H 0.2538 -0.3283 0.7689 0.037 Uiso 1 1 calc R . . H3B H 0.2127 -0.4618 0.7259 0.037 Uiso 1 1 calc R . . C2 C 0.4284(3) -0.5419(3) 0.6317(3) 0.0292(6) Uani 1 1 d . . . H2A H 0.3878 -0.6136 0.6697 0.035 Uiso 1 1 calc R . . H2B H 0.5219 -0.5590 0.6205 0.035 Uiso 1 1 calc R . . H1 H 0.332(3) 0.1599(17) 0.567(3) 0.044 Uiso 1 1 d D . . H2N H 0.331(4) -0.361(3) 0.422(4) 0.051(11) Uiso 1 1 d . . . H1N H 0.434(4) -0.454(4) 0.795(4) 0.055(11) Uiso 1 1 d . . . H2 H 0.404(4) -0.275(4) 0.0781(19) 0.083 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.02188(16) 0.02055(17) 0.02022(17) 0.00015(15) -0.00074(12) -0.00079(15) P1 0.0272(3) 0.0279(4) 0.0174(3) -0.0007(3) 0.0009(3) -0.0020(3) P2 0.0298(3) 0.0183(3) 0.0240(3) 0.0008(3) -0.0019(3) 0.0021(3) O4 0.0328(10) 0.0196(10) 0.0570(14) 0.0021(10) 0.0128(10) 0.0015(8) O1 0.0298(10) 0.0464(13) 0.0231(10) 0.0015(9) 0.0066(7) 0.0027(9) O2 0.0254(10) 0.0682(17) 0.0244(10) -0.0035(11) 0.0038(7) -0.0067(10) O5 0.0341(10) 0.0425(12) 0.0330(11) 0.0105(10) -0.0069(8) -0.0137(9) O6 0.0471(13) 0.0248(11) 0.0639(16) -0.0066(11) -0.0116(12) 0.0134(9) N2 0.0261(11) 0.0280(12) 0.0231(11) 0.0048(9) -0.0035(10) -0.0008(10) O3 0.0409(11) 0.0501(14) 0.0201(10) -0.0021(9) -0.0004(8) -0.0148(10) N1 0.0240(11) 0.0307(12) 0.0214(11) 0.0024(10) -0.0022(9) 0.0003(9) C6 0.0235(13) 0.0313(15) 0.0396(16) 0.0042(13) 0.0000(12) 0.0041(11) C5 0.0329(13) 0.0284(14) 0.0273(13) -0.0032(11) 0.0005(11) 0.0003(13) C4 0.0280(14) 0.0328(15) 0.0362(16) 0.0072(12) 0.0001(11) -0.0100(12) C1 0.0290(15) 0.0348(16) 0.0366(16) 0.0005(13) -0.0080(12) -0.0071(12) C3 0.0257(12) 0.0357(15) 0.0319(14) -0.0003(14) 0.0051(12) 0.0061(11) C2 0.0314(13) 0.0264(14) 0.0300(14) 0.0033(11) -0.0019(12) 0.0064(12) _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 O6 1.933(2) 4_655 ? Co1 O4 1.938(2) . ? Co1 O1 1.9540(19) 2_554 ? Co1 O3 1.957(2) . ? P1 O3 1.513(2) . ? P1 O1 1.515(2) . ? P1 O2 1.516(2) . ? P1 H1 1.427(17) . ? P2 O6 1.502(2) . ? P2 O4 1.510(2) . ? P2 O5 1.517(2) . ? P2 H2 1.426(19) . ? O1 Co1 1.9540(19) 2 ? O6 Co1 1.933(2) 4_645 ? N2 C5 1.474(3) . ? N2 C6 1.485(4) . ? N2 C4 1.495(4) . ? N2 H2N 0.86(4) . ? N1 C3 1.489(3) . ? N1 C2 1.492(4) . ? N1 C1 1.492(4) . ? N1 H1N 0.99(4) . ? C6 C3 1.528(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C5 C2 1.538(4) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C4 C1 1.505(4) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? 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 O6 Co1 O4 109.57(10) 4_655 . ? O6 Co1 O1 102.05(10) 4_655 2_554 ? O4 Co1 O1 110.99(9) . 2_554 ? O6 Co1 O3 111.97(10) 4_655 . ? O4 Co1 O3 111.71(10) . . ? O1 Co1 O3 110.17(9) 2_554 . ? O3 P1 O1 111.74(12) . . ? O3 P1 O2 113.21(12) . . ? O1 P1 O2 110.12(12) . . ? O3 P1 H1 109.4(14) . . ? O1 P1 H1 109.4(14) . . ? O2 P1 H1 102.6(13) . . ? O6 P2 O4 108.91(13) . . ? O6 P2 O5 113.80(14) . . ? O4 P2 O5 113.12(13) . . ? O6 P2 H2 108.5(18) . . ? O4 P2 H2 104.0(19) . . ? O5 P2 H2 108.0(17) . . ? P2 O4 Co1 130.13(12) . . ? P1 O1 Co1 137.11(13) . 2 ? P2 O6 Co1 147.92(15) . 4_645 ? C5 N2 C6 109.5(2) . . ? C5 N2 C4 109.3(2) . . ? C6 N2 C4 109.9(2) . . ? C5 N2 H2N 111(2) . . ? C6 N2 H2N 115(2) . . ? C4 N2 H2N 103(2) . . ? P1 O3 Co1 126.93(13) . . ? C3 N1 C2 109.4(2) . . ? C3 N1 C1 108.4(2) . . ? C2 N1 C1 109.5(2) . . ? C3 N1 H1N 109(2) . . ? C2 N1 H1N 108(2) . . ? C1 N1 H1N 113(2) . . ? N2 C6 C3 108.0(2) . . ? N2 C6 H6A 110.1 . . ? C3 C6 H6A 110.1 . . ? N2 C6 H6B 110.1 . . ? C3 C6 H6B 110.1 . . ? H6A C6 H6B 108.4 . . ? N2 C5 C2 108.1(2) . . ? N2 C5 H5A 110.1 . . ? C2 C5 H5A 110.1 . . ? N2 C5 H5B 110.1 . . ? C2 C5 H5B 110.1 . . ? H5A C5 H5B 108.4 . . ? N2 C4 C1 108.6(2) . . ? N2 C4 H4A 110.0 . . ? C1 C4 H4A 110.0 . . ? N2 C4 H4B 110.0 . . ? C1 C4 H4B 110.0 . . ? H4A C4 H4B 108.4 . . ? N1 C1 C4 108.5(2) . . ? N1 C1 H1A 110.0 . . ? C4 C1 H1A 110.0 . . ? N1 C1 H1B 110.0 . . ? C4 C1 H1B 110.0 . . ? H1A C1 H1B 108.4 . . ? N1 C3 C6 108.8(2) . . ? N1 C3 H3A 109.9 . . ? C6 C3 H3A 109.9 . . ? N1 C3 H3B 109.9 . . ? C6 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? N1 C2 C5 108.2(2) . . ? N1 C2 H2A 110.1 . . ? C5 C2 H2A 110.1 . . ? N1 C2 H2B 110.1 . . ? C5 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 P2 O4 Co1 -145.07(19) . . . . ? O5 P2 O4 Co1 -17.5(2) . . . . ? O6 Co1 O4 P2 -172.58(17) 4_655 . . . ? O1 Co1 O4 P2 -60.6(2) 2_554 . . . ? O3 Co1 O4 P2 62.8(2) . . . . ? O3 P1 O1 Co1 -85.6(2) . . . 2 ? O2 P1 O1 Co1 147.73(18) . . . 2 ? O4 P2 O6 Co1 -161.8(3) . . . 4_645 ? O5 P2 O6 Co1 71.0(4) . . . 4_645 ? O1 P1 O3 Co1 -173.31(14) . . . . ? O2 P1 O3 Co1 -48.3(2) . . . . ? O6 Co1 O3 P1 -21.7(2) 4_655 . . . ? O4 Co1 O3 P1 101.62(18) . . . . ? O1 Co1 O3 P1 -134.53(16) 2_554 . . . ? C5 N2 C6 C3 51.2(3) . . . . ? C4 N2 C6 C3 -68.8(3) . . . . ? C6 N2 C5 C2 -71.1(3) . . . . ? C4 N2 C5 C2 49.3(3) . . . . ? C5 N2 C4 C1 -71.8(3) . . . . ? C6 N2 C4 C1 48.3(3) . . . . ? C3 N1 C1 C4 -71.4(3) . . . . ? C2 N1 C1 C4 47.8(3) . . . . ? N2 C4 C1 N1 19.1(3) . . . . ? C2 N1 C3 C6 -69.1(3) . . . . ? C1 N1 C3 C6 50.2(3) . . . . ? N2 C6 C3 N1 16.3(3) . . . . ? C3 N1 C2 C5 49.1(3) . . . . ? C1 N1 C2 C5 -69.5(3) . . . . ? N2 C5 C2 N1 17.5(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1N O2 0.99(4) 1.60(4) 2.581(3) 170(3) 4_646 N2 H2N O5 0.86(4) 1.73(4) 2.589(3) 176(4) . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.08 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.868 _refine_diff_density_min -0.345 _refine_diff_density_rms 0.063