# Electronic Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address 'Xianchun Liu' ; College of Chemistry Northeast Normal University Changchun, 130024 P. R. China ; 'Yan Xing' ; College of Chemistry Northeast Normal University Changchun, 130024 P. R. China ; _publ_contact_author_address ; College of Chemistry Northeast Normal University Changchun, 130024 P. R. China ; _publ_contact_author_email xingy202@nenu.edu.cn _publ_contact_author_phone 86-431-85262135 _publ_contact_author_name 'Yan Xing' _publ_requested_coeditor_name ? #============================================================ # 2. TITLE AND AUTHOR LIST _publ_section_title ; Template Synthesis, Structural Characterization and Magnetic Behavior of One-,Two- and Three Dimensional Cobalt(II) Phosphite ; data_Xing1 _database_code_depnum_ccdc_archive 'CCDC 729332' #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'Co H2 O6 P2, 2(C2 H6 N)' _chemical_formula_sum 'C4 H14 Co N2 O6 P2' _chemical_formula_weight 307.04 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 Monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.783(5) _cell_length_b 7.249(5) _cell_length_c 8.832(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 105.275(5) _cell_angle_gamma 90.000(5) _cell_volume 1098.3(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1282 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 28.22 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.857 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 628 _exptl_absorpt_coefficient_mu 1.864 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6428 _exptl_absorpt_correction_T_max 0.7936 _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 3266 _diffrn_reflns_av_R_equivalents 0.0200 _diffrn_reflns_av_sigmaI/netI 0.0221 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 28.22 _reflns_number_total 1282 _reflns_number_gt 1150 _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^)+(0.0279P)^2^+1.0074P] 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_number_reflns 1282 _refine_ls_number_parameters 97 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0293 _refine_ls_R_factor_gt 0.0250 _refine_ls_wR_factor_ref 0.0636 _refine_ls_wR_factor_gt 0.0621 _refine_ls_goodness_of_fit_ref 1.154 _refine_ls_restrained_S_all 1.154 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.0000 0.08319(5) 0.2500 0.02006(12) Uani 1 2 d S . . P1 P -0.06992(3) -0.25538(7) 0.41168(6) 0.02111(14) Uani 1 1 d . . . O2 O -0.13916(9) -0.3746(2) 0.33471(17) 0.0337(4) Uani 1 1 d . . . O1 O -0.07190(9) -0.0748(2) 0.32466(19) 0.0347(4) Uani 1 1 d . . . O3 O -0.06496(10) -0.2320(2) 0.58403(17) 0.0415(4) Uani 1 1 d . . . C2 C -0.18253(13) -0.2118(3) -0.0563(3) 0.0301(5) Uani 1 1 d . . . N1 N -0.19199(10) -0.3918(2) 0.0175(2) 0.0251(4) Uani 1 1 d . . . C1 C -0.27582(13) -0.4393(3) -0.0059(3) 0.0290(4) Uani 1 1 d . . . H1 H -0.0086(12) -0.339(3) 0.403(2) 0.018(5) Uiso 1 1 d . . . H1NA H -0.1675(14) -0.390(3) 0.117(3) 0.027(6) Uiso 1 1 d . . . H1NB H -0.1654(14) -0.480(3) -0.025(3) 0.033(6) Uiso 1 1 d . . . H2CB H -0.2051(14) -0.227(3) -0.174(3) 0.031(6) Uiso 1 1 d . . . H1CB H -0.2969(14) -0.455(3) -0.114(3) 0.028(6) Uiso 1 1 d . . . H1CA H -0.2794(16) -0.549(4) 0.041(3) 0.039(7) Uiso 1 1 d . . . H2CA H -0.1291(18) -0.181(4) -0.035(3) 0.055(8) 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 Co1 0.0233(2) 0.02112(19) 0.01426(19) 0.000 0.00235(13) 0.000 P1 0.0214(3) 0.0237(3) 0.0170(3) -0.00043(19) 0.00282(18) -0.00361(18) O2 0.0405(9) 0.0387(9) 0.0184(7) -0.0008(6) 0.0016(6) -0.0189(7) O1 0.0328(8) 0.0321(8) 0.0395(9) 0.0099(7) 0.0102(7) -0.0043(6) O3 0.0530(11) 0.0500(10) 0.0189(8) -0.0076(7) 0.0049(7) -0.0235(8) C2 0.0274(11) 0.0347(11) 0.0298(12) 0.0030(9) 0.0104(9) -0.0005(9) N1 0.0263(9) 0.0276(9) 0.0191(9) -0.0027(7) 0.0020(7) 0.0051(7) C1 0.0287(11) 0.0258(10) 0.0301(12) -0.0018(9) 0.0034(9) -0.0034(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O3 1.9377(16) 5_556 ? Co1 O3 1.9377(16) 6 ? Co1 O1 1.9558(16) . ? Co1 O1 1.9558(16) 2 ? P1 O2 1.5115(16) . ? P1 O3 1.5109(18) . ? P1 O1 1.5140(17) . ? P1 H1 1.27(2) . ? O3 Co1 1.9377(16) 5_556 ? C2 N1 1.488(3) . ? C2 C1 1.505(3) 7_445 ? C2 H2CB 1.01(2) . ? C2 H2CA 0.94(3) . ? N1 C1 1.490(3) . ? N1 H1NA 0.87(3) . ? N1 H1NB 0.93(2) . ? C1 C2 1.505(3) 7_445 ? C1 H1CB 0.94(3) . ? C1 H1CA 0.91(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 O3 Co1 O3 112.34(12) 5_556 6 ? O3 Co1 O1 112.54(8) 5_556 . ? O3 Co1 O1 105.58(8) 6 . ? O3 Co1 O1 105.58(8) 5_556 2 ? O3 Co1 O1 112.54(8) 6 2 ? O1 Co1 O1 108.33(10) . 2 ? O2 P1 O3 109.97(9) . . ? O2 P1 O1 111.04(10) . . ? O3 P1 O1 113.70(10) . . ? O2 P1 H1 108.1(9) . . ? O3 P1 H1 106.8(9) . . ? O1 P1 H1 106.9(9) . . ? P1 O1 Co1 138.38(10) . . ? P1 O3 Co1 133.59(10) . 5_556 ? N1 C2 C1 110.79(18) . 7_445 ? N1 C2 H2CB 107.0(13) . . ? C1 C2 H2CB 110.7(14) 7_445 . ? N1 C2 H2CA 109.9(18) . . ? C1 C2 H2CA 108.6(18) 7_445 . ? H2CB C2 H2CA 110(2) . . ? C2 N1 C1 111.47(16) . . ? C2 N1 H1NA 110.0(15) . . ? C1 N1 H1NA 111.2(16) . . ? C2 N1 H1NB 107.0(15) . . ? C1 N1 H1NB 112.5(15) . . ? H1NA N1 H1NB 104(2) . . ? N1 C1 C2 110.58(17) . 7_445 ? N1 C1 H1CB 106.6(14) . . ? C2 C1 H1CB 110.9(14) 7_445 . ? N1 C1 H1CA 109.1(17) . . ? C2 C1 H1CA 111.6(16) 7_445 . ? H1CB C1 H1CA 108(2) . . ? 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 O2 P1 O1 Co1 -135.52(15) . . . . ? O3 P1 O1 Co1 99.83(17) . . . . ? O3 Co1 O1 P1 -78.85(17) 5_556 . . . ? O3 Co1 O1 P1 158.27(15) 6 . . . ? O1 Co1 O1 P1 37.50(13) 2 . . . ? O2 P1 O3 Co1 -173.08(14) . . . 5_556 ? O1 P1 O3 Co1 -47.86(18) . . . 5_556 ? C1 C2 N1 C1 56.4(3) 7_445 . . . ? C2 N1 C1 C2 -56.3(3) . . . 7_445 ? 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 H1NA O2 0.87(3) 1.86(3) 2.713(3) 166(2) . _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.291 _refine_diff_density_min -0.313 _refine_diff_density_rms 0.067 # Attachment 'P -1(2D).cif' data_Xing2 _database_code_depnum_ccdc_archive 'CCDC 729333' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'Co2 H3 O9 P3, C2 H6 N, C2 H8 N' _chemical_formula_sum 'C4 H17 Co2 N2 O9 P3' _chemical_formula_weight 447.97 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 Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.718(5) _cell_length_b 8.840(5) _cell_length_c 12.151(5) _cell_angle_alpha 76.056(5) _cell_angle_beta 77.939(5) _cell_angle_gamma 68.704(5) _cell_volume 742.9(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2907 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 26.07 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.003 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 452 _exptl_absorpt_coefficient_mu 2.595 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5748 _exptl_absorpt_correction_T_max 0.6667 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 4090 _diffrn_reflns_av_R_equivalents 0.0136 _diffrn_reflns_av_sigmaI/netI 0.0260 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 26.07 _reflns_number_total 2907 _reflns_number_gt 2493 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+0.5280P] 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_number_reflns 2907 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0320 _refine_ls_R_factor_gt 0.0253 _refine_ls_wR_factor_ref 0.0666 _refine_ls_wR_factor_gt 0.0636 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 Co2 Co 0.48431(5) 0.26074(4) -0.02077(3) 0.02534(10) Uani 1 1 d . . . Co1 Co 0.47627(5) 0.88194(4) -0.33654(3) 0.02433(10) Uani 1 1 d . . . P3 P 0.31847(9) 0.63715(8) -0.14433(6) 0.02477(15) Uani 1 1 d . . . P2 P 0.83681(9) 0.84808(8) -0.52615(6) 0.02732(15) Uani 1 1 d . . . P1 P 0.68412(9) 0.98006(8) -0.18064(5) 0.02342(15) Uani 1 1 d . . . O9 O 0.3241(3) 0.7083(3) -0.04419(17) 0.0383(5) Uani 1 1 d . . . O8 O 0.4566(3) 0.6707(2) -0.24822(16) 0.0351(4) Uani 1 1 d . . . O7 O 0.7645(3) 1.0060(3) -0.6091(2) 0.0478(6) Uani 1 1 d . . . O6 O 0.6591(3) 1.1315(2) -0.13373(16) 0.0345(4) Uani 1 1 d . . . O5 O 0.6878(3) 0.8298(2) -0.08967(16) 0.0382(5) Uani 1 1 d . . . O4 O 0.9814(3) 0.7131(3) -0.58394(17) 0.0400(5) Uani 1 1 d . . . O3 O 0.3360(3) 0.4573(2) -0.11445(17) 0.0365(5) Uani 1 1 d . . . N2 N 0.6725(3) 0.4765(3) -0.4609(2) 0.0291(5) Uani 1 1 d . . . O2 O 0.6792(3) 0.7892(2) -0.45363(17) 0.0380(5) Uani 1 1 d . . . O1 O 0.5459(3) 1.0182(2) -0.26307(17) 0.0383(5) Uani 1 1 d . . . N1 N 0.9515(3) 0.2760(3) -0.1834(2) 0.0365(5) Uani 1 1 d . . . C4 C 0.4563(4) 0.6128(3) -0.6051(2) 0.0359(6) Uani 1 1 d . . . H4A H 0.4202 0.7193 -0.5825 0.043 Uiso 1 1 calc R . . H4B H 0.4470 0.6319 -0.6860 0.043 Uiso 1 1 calc R . . C3 C 0.6557(4) 0.5150(4) -0.5847(2) 0.0377(7) Uani 1 1 d . . . H3A H 0.6957 0.4130 -0.6140 0.045 Uiso 1 1 calc R . . H3B H 0.7372 0.5778 -0.6256 0.045 Uiso 1 1 calc R . . C2 C 0.9113(5) 0.4509(4) -0.1781(3) 0.0540(9) Uani 1 1 d . . . H2C H 0.8082 0.5188 -0.2195 0.081 Uiso 1 1 calc R . . H2D H 1.0202 0.4823 -0.2118 0.081 Uiso 1 1 calc R . . H2E H 0.8795 0.4653 -0.0997 0.081 Uiso 1 1 calc R . . C1 C 1.1076(5) 0.1614(5) -0.1228(3) 0.0590(10) Uani 1 1 d . . . H1B H 1.1262 0.0506 -0.1299 0.088 Uiso 1 1 calc R . . H1C H 1.0791 0.1704 -0.0433 0.088 Uiso 1 1 calc R . . H1D H 1.2197 0.1882 -0.1554 0.088 Uiso 1 1 calc R . . H1 H 0.858(4) 0.940(3) -0.241(2) 0.025(7) Uiso 1 1 d . . . H3 H 0.148(4) 0.718(3) -0.177(2) 0.026(7) Uiso 1 1 d . . . H2 H 0.924(4) 0.877(3) -0.453(2) 0.026(7) Uiso 1 1 d . . . H2NB H 0.809(5) 0.407(4) -0.449(3) 0.063(11) Uiso 1 1 d . . . H2NA H 0.661(5) 0.570(4) -0.444(3) 0.050(10) Uiso 1 1 d . . . H1NB H 0.988(5) 0.261(5) -0.260(4) 0.072(12) Uiso 1 1 d . . . H1NA H 0.844(5) 0.240(4) -0.157(3) 0.059(11) 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 Co2 0.0322(2) 0.02106(17) 0.02362(19) -0.00369(13) -0.00306(14) -0.01044(14) Co1 0.02796(19) 0.02069(17) 0.02316(18) -0.00469(13) -0.00264(14) -0.00663(14) P3 0.0266(3) 0.0196(3) 0.0285(3) -0.0021(2) -0.0097(3) -0.0061(3) P2 0.0222(3) 0.0298(3) 0.0275(3) -0.0059(3) -0.0041(3) -0.0049(3) P1 0.0265(3) 0.0216(3) 0.0218(3) -0.0059(2) 0.0014(3) -0.0087(3) O9 0.0370(11) 0.0478(12) 0.0396(11) -0.0197(9) -0.0025(9) -0.0189(9) O8 0.0464(12) 0.0258(9) 0.0325(10) -0.0018(8) -0.0019(9) -0.0151(9) O7 0.0327(11) 0.0400(12) 0.0608(15) 0.0107(10) -0.0151(10) -0.0081(9) O6 0.0403(11) 0.0344(10) 0.0354(11) -0.0180(8) 0.0024(9) -0.0167(9) O5 0.0403(11) 0.0361(11) 0.0361(11) 0.0057(9) -0.0065(9) -0.0172(9) O4 0.0270(10) 0.0471(12) 0.0372(11) -0.0151(9) -0.0042(8) 0.0024(9) O3 0.0480(12) 0.0245(9) 0.0388(11) 0.0039(8) -0.0151(9) -0.0152(9) N2 0.0256(11) 0.0270(11) 0.0359(13) -0.0117(10) -0.0098(9) -0.0030(9) O2 0.0390(11) 0.0357(11) 0.0398(11) -0.0166(9) 0.0125(9) -0.0165(9) O1 0.0525(13) 0.0293(10) 0.0374(11) -0.0054(8) -0.0177(10) -0.0124(9) N1 0.0293(12) 0.0465(15) 0.0343(14) -0.0090(11) -0.0020(11) -0.0134(11) C4 0.0415(16) 0.0351(15) 0.0282(14) 0.0021(11) -0.0101(12) -0.0112(13) C3 0.0334(15) 0.0492(17) 0.0308(15) -0.0079(13) 0.0011(12) -0.0166(13) C2 0.058(2) 0.051(2) 0.051(2) -0.0162(16) 0.0069(17) -0.0190(17) C1 0.0447(19) 0.068(2) 0.053(2) -0.0121(18) -0.0167(16) 0.0012(17) _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 Co2 O5 1.928(2) 2_665 ? Co2 O9 1.942(2) 2_665 ? Co2 O3 1.9422(19) . ? Co2 O6 1.9677(19) 1_545 ? Co1 O1 1.930(2) . ? Co1 O7 1.931(2) 2_674 ? Co1 O8 1.958(2) . ? Co1 O2 1.961(2) . ? P3 O3 1.505(2) . ? P3 O9 1.513(2) . ? P3 O8 1.518(2) . ? P3 H3 1.34(3) . ? P2 O7 1.506(2) . ? P2 O4 1.507(2) . ? P2 O2 1.522(2) . ? P2 H2 1.34(3) . ? P1 O5 1.505(2) . ? P1 O1 1.509(2) . ? P1 O6 1.5124(19) . ? P1 H1 1.36(3) . ? O9 Co2 1.942(2) 2_665 ? O7 Co1 1.931(2) 2_674 ? O6 Co2 1.9678(19) 1_565 ? O5 Co2 1.928(2) 2_665 ? N2 C4 1.478(4) 2_664 ? N2 C3 1.483(4) . ? N2 H2NB 1.03(4) . ? N2 H2NA 0.87(4) . ? N1 C1 1.464(4) . ? N1 C2 1.477(4) . ? N1 H1NB 0.94(4) . ? N1 H1NA 0.96(4) . ? C4 N2 1.478(4) 2_664 ? C4 C3 1.506(4) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C2 H2C 0.9600 . ? C2 H2D 0.9600 . ? C2 H2E 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? 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 O5 Co2 O9 114.54(9) 2_665 2_665 ? O5 Co2 O3 107.52(9) 2_665 . ? O9 Co2 O3 114.80(9) 2_665 . ? O5 Co2 O6 120.15(9) 2_665 1_545 ? O9 Co2 O6 95.86(9) 2_665 1_545 ? O3 Co2 O6 103.54(9) . 1_545 ? O1 Co1 O7 112.29(10) . 2_674 ? O1 Co1 O8 118.47(9) . . ? O7 Co1 O8 103.97(9) 2_674 . ? O1 Co1 O2 110.85(10) . . ? O7 Co1 O2 113.97(10) 2_674 . ? O8 Co1 O2 96.37(9) . . ? O3 P3 O9 113.85(12) . . ? O3 P3 O8 111.36(11) . . ? O9 P3 O8 113.06(12) . . ? O3 P3 H3 106.0(11) . . ? O9 P3 H3 106.5(11) . . ? O8 P3 H3 105.3(11) . . ? O7 P2 O4 112.60(13) . . ? O7 P2 O2 112.32(12) . . ? O4 P2 O2 110.97(12) . . ? O7 P2 H2 108.5(11) . . ? O4 P2 H2 106.0(11) . . ? O2 P2 H2 106.0(11) . . ? O5 P1 O1 113.60(11) . . ? O5 P1 O6 113.65(12) . . ? O1 P1 O6 111.03(11) . . ? O5 P1 H1 104.3(11) . . ? O1 P1 H1 107.4(11) . . ? O6 P1 H1 106.2(11) . . ? P3 O9 Co2 136.23(13) . 2_665 ? P3 O8 Co1 129.37(12) . . ? P2 O7 Co1 132.04(13) . 2_674 ? P1 O6 Co2 138.25(12) . 1_565 ? P1 O5 Co2 139.32(13) . 2_665 ? P3 O3 Co2 136.36(12) . . ? C4 N2 C3 111.1(2) 2_664 . ? C4 N2 H2NB 110(2) 2_664 . ? C3 N2 H2NB 109(2) . . ? C4 N2 H2NA 118(2) 2_664 . ? C3 N2 H2NA 105(2) . . ? H2NB N2 H2NA 102(3) . . ? P2 O2 Co1 132.36(12) . . ? P1 O1 Co1 133.15(12) . . ? C1 N1 C2 113.9(3) . . ? C1 N1 H1NB 105(2) . . ? C2 N1 H1NB 109(2) . . ? C1 N1 H1NA 109(2) . . ? C2 N1 H1NA 113(2) . . ? H1NB N1 H1NA 106(3) . . ? N2 C4 C3 110.6(2) 2_664 . ? N2 C4 H4A 109.5 2_664 . ? C3 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 2_664 . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? N2 C3 C4 110.8(2) . . ? N2 C3 H3A 109.5 . . ? C4 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? N1 C2 H2C 109.5 . . ? N1 C2 H2D 109.5 . . ? H2C C2 H2D 109.5 . . ? N1 C2 H2E 109.5 . . ? H2C C2 H2E 109.5 . . ? H2D C2 H2E 109.5 . . ? N1 C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C1 H1D 109.5 . . ? H1B C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 P3 O9 Co2 92.5(2) . . . 2_665 ? O8 P3 O9 Co2 -35.9(2) . . . 2_665 ? O3 P3 O8 Co1 171.47(13) . . . . ? O9 P3 O8 Co1 -58.87(18) . . . . ? O1 Co1 O8 P3 66.20(18) . . . . ? O7 Co1 O8 P3 -59.22(17) 2_674 . . . ? O2 Co1 O8 P3 -175.90(15) . . . . ? O4 P2 O7 Co1 110.40(19) . . . 2_674 ? O2 P2 O7 Co1 -15.8(2) . . . 2_674 ? O5 P1 O6 Co2 -53.6(2) . . . 1_565 ? O1 P1 O6 Co2 75.9(2) . . . 1_565 ? O1 P1 O5 Co2 -50.1(2) . . . 2_665 ? O6 P1 O5 Co2 78.1(2) . . . 2_665 ? O9 P3 O3 Co2 -41.0(2) . . . . ? O8 P3 O3 Co2 88.3(2) . . . . ? O5 Co2 O3 P3 122.64(19) 2_665 . . . ? O9 Co2 O3 P3 -6.1(2) 2_665 . . . ? O6 Co2 O3 P3 -109.21(19) 1_545 . . . ? O7 P2 O2 Co1 -66.0(2) . . . . ? O4 P2 O2 Co1 167.02(15) . . . . ? O1 Co1 O2 P2 -26.5(2) . . . . ? O7 Co1 O2 P2 101.36(18) 2_674 . . . ? O8 Co1 O2 P2 -150.24(17) . . . . ? O5 P1 O1 Co1 -40.6(2) . . . . ? O6 P1 O1 Co1 -170.15(15) . . . . ? O7 Co1 O1 P1 160.37(17) 2_674 . . . ? O8 Co1 O1 P1 39.1(2) . . . . ? O2 Co1 O1 P1 -70.88(19) . . . . ? C4 N2 C3 C4 56.6(3) 2_664 . . . ? N2 C4 C3 N2 -56.3(3) 2_664 . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.07 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.325 _refine_diff_density_min -0.454 _refine_diff_density_rms 0.067 # Attachment 'mc2c(3D).cif' data_Xing3 _database_code_depnum_ccdc_archive 'CCDC 729334' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'Co3 H4 O12 P4, 2(C2 H8 N)' _chemical_formula_sum 'C4 H20 Co3 N2 O12 P4' _chemical_formula_weight 588.89 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 Monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.882(5) _cell_length_b 8.462(5) _cell_length_c 16.096(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 112.563(5) _cell_angle_gamma 90.000(5) _cell_volume 1997.6(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2347 _cell_measurement_theta_min 2.74 _cell_measurement_theta_max 28.56 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.958 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1180 _exptl_absorpt_coefficient_mu 2.835 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.483 _exptl_absorpt_correction_T_max 0.692 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 5936 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 28.56 _reflns_number_total 2347 _reflns_number_gt 1674 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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_number_reflns 2347 _refine_ls_number_parameters 130 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0568 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.1203 _refine_ls_wR_factor_gt 0.0999 _refine_ls_goodness_of_fit_ref 0.805 _refine_ls_restrained_S_all 0.805 _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 0.36390(3) 0.13654(5) -0.52374(3) 0.03276(17) Uani 1 1 d . . . Co2 Co 0.5000 0.12672(8) -0.2500 0.03138(19) Uani 1 2 d S . . P1 P 0.15253(6) 0.13676(11) -0.63666(6) 0.0329(2) Uani 1 1 d . . . P2 P 0.47982(6) -0.12988(10) -0.40078(6) 0.0308(2) Uani 1 1 d . . . O1 O 0.1113(2) 0.2488(4) -0.71534(18) 0.0556(8) Uani 1 1 d . . . O2 O 0.24815(19) 0.0965(4) -0.62433(18) 0.0539(8) Uani 1 1 d . . . O3 O 0.3604(2) 0.3101(4) -0.44642(18) 0.0481(7) Uani 1 1 d . . . O4 O 0.39151(18) -0.0807(3) -0.47636(18) 0.0436(6) Uani 1 1 d . . . O5 O 0.52557(18) 0.0081(4) -0.34059(18) 0.0515(7) Uani 1 1 d . . . O6 O 0.54381(19) -0.2151(3) -0.4346(2) 0.0466(7) Uani 1 1 d . . . N1 N 0.3376(3) -0.2831(4) -0.6358(3) 0.0444(8) Uani 1 1 d . . . H1NB H 0.351(3) -0.215(5) -0.592(3) 0.045(12) Uiso 1 1 d . . . H1NA H 0.352(3) -0.249(6) -0.676(4) 0.065(16) Uiso 1 1 d . . . C1 C 0.2379(4) -0.3061(7) -0.6683(4) 0.0748(15) Uani 1 1 d . . . H1A H 0.2076 -0.2068 -0.6883 0.112 Uiso 1 1 calc R . . H1B H 0.2224 -0.3467 -0.6203 0.112 Uiso 1 1 calc R . . H1C H 0.2188 -0.3798 -0.7174 0.112 Uiso 1 1 calc R . . C2 C 0.3896(4) -0.4296(6) -0.6031(3) 0.0666(14) Uani 1 1 d . . . H2A H 0.4537 -0.4074 -0.5826 0.100 Uiso 1 1 calc R . . H2B H 0.3731 -0.5055 -0.6510 0.100 Uiso 1 1 calc R . . H2C H 0.3760 -0.4716 -0.5542 0.100 Uiso 1 1 calc R . . H1 H 0.110(3) 0.006(5) -0.656(3) 0.054(12) Uiso 1 1 d . . . H2 H 0.458(3) -0.237(5) -0.353(3) 0.051(12) 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 Co1 0.0297(3) 0.0387(3) 0.0316(3) 0.0009(2) 0.0136(2) 0.00805(19) Co2 0.0269(3) 0.0426(4) 0.0238(3) 0.000 0.0088(3) 0.000 P1 0.0314(5) 0.0384(5) 0.0296(5) -0.0040(4) 0.0125(4) 0.0049(4) P2 0.0316(5) 0.0346(5) 0.0316(5) 0.0047(3) 0.0180(4) 0.0049(3) O1 0.0538(18) 0.079(2) 0.0395(15) 0.0137(15) 0.0238(14) 0.0310(16) O2 0.0359(15) 0.083(2) 0.0365(15) -0.0125(15) 0.0069(12) 0.0160(14) O3 0.067(2) 0.0500(16) 0.0388(15) 0.0005(12) 0.0327(14) 0.0114(14) O4 0.0381(15) 0.0411(14) 0.0458(15) 0.0032(12) 0.0097(12) 0.0035(11) O5 0.0416(15) 0.0632(19) 0.0515(17) -0.0181(15) 0.0198(13) 0.0012(14) O6 0.0516(17) 0.0386(15) 0.0674(19) -0.0002(13) 0.0426(15) 0.0047(12) N1 0.056(2) 0.043(2) 0.042(2) -0.0034(16) 0.0273(17) -0.0080(16) C1 0.056(3) 0.083(4) 0.097(4) -0.009(3) 0.043(3) -0.006(3) C2 0.075(4) 0.064(3) 0.057(3) 0.010(2) 0.021(3) 0.016(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 Co1 O3 1.939(3) . ? Co1 O6 1.948(3) 5_654 ? Co1 O2 1.957(3) . ? Co1 O4 1.974(3) . ? Co2 O5 1.937(3) 2_654 ? Co2 O5 1.937(3) . ? Co2 O1 1.947(3) 7_554 ? Co2 O1 1.947(3) 8_556 ? P1 O2 1.494(3) . ? P1 O3 1.498(3) 7_554 ? P1 O1 1.515(3) . ? P1 H1 1.27(4) . ? P2 O6 1.508(3) . ? P2 O5 1.513(3) . ? P2 O4 1.520(3) . ? P2 H2 1.31(4) . ? O1 Co2 1.947(3) 7_554 ? O3 P1 1.498(3) 7_554 ? O6 Co1 1.948(3) 5_654 ? N1 C2 1.471(6) . ? N1 C1 1.478(6) . ? N1 H1NB 0.87(5) . ? N1 H1NA 0.82(5) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Co1 O6 99.96(12) . 5_654 ? O3 Co1 O2 114.40(13) . . ? O6 Co1 O2 111.48(13) 5_654 . ? O3 Co1 O4 120.93(12) . . ? O6 Co1 O4 111.46(12) 5_654 . ? O2 Co1 O4 99.05(13) . . ? O5 Co2 O5 117.59(19) 2_654 . ? O5 Co2 O1 93.80(13) 2_654 7_554 ? O5 Co2 O1 119.62(12) . 7_554 ? O5 Co2 O1 119.62(12) 2_654 8_556 ? O5 Co2 O1 93.80(13) . 8_556 ? O1 Co2 O1 114.5(2) 7_554 8_556 ? O2 P1 O3 115.52(17) . 7_554 ? O2 P1 O1 110.17(18) . . ? O3 P1 O1 113.27(17) 7_554 . ? O2 P1 H1 104.8(18) . . ? O3 P1 H1 103.6(18) 7_554 . ? O1 P1 H1 108.7(18) . . ? O6 P2 O5 112.06(16) . . ? O6 P2 O4 112.63(17) . . ? O5 P2 O4 111.70(16) . . ? O6 P2 H2 104.4(19) . . ? O5 P2 H2 109.1(19) . . ? O4 P2 H2 106.5(19) . . ? P1 O1 Co2 129.16(18) . 7_554 ? P1 O2 Co1 130.89(17) . . ? P1 O3 Co1 148.0(2) 7_554 . ? P2 O4 Co1 124.36(17) . . ? P2 O5 Co2 133.94(18) . . ? P2 O6 Co1 131.42(17) . 5_654 ? C2 N1 C1 113.2(4) . . ? C2 N1 H1NB 110(3) . . ? C1 N1 H1NB 106(3) . . ? C2 N1 H1NA 107(4) . . ? C1 N1 H1NA 111(4) . . ? H1NB N1 H1NA 111(5) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 P1 O1 Co2 -167.0(2) . . . 7_554 ? O3 P1 O1 Co2 -35.9(3) 7_554 . . 7_554 ? O3 P1 O2 Co1 -12.7(4) 7_554 . . . ? O1 P1 O2 Co1 117.2(3) . . . . ? O3 Co1 O2 P1 -22.5(3) . . . . ? O6 Co1 O2 P1 -135.0(3) 5_654 . . . ? O4 Co1 O2 P1 107.5(3) . . . . ? O6 Co1 O3 P1 -146.9(4) 5_654 . . 7_554 ? O2 Co1 O3 P1 93.9(4) . . . 7_554 ? O4 Co1 O3 P1 -24.3(4) . . . 7_554 ? O6 P2 O4 Co1 -102.8(2) . . . . ? O5 P2 O4 Co1 24.3(3) . . . . ? O3 Co1 O4 P2 -60.2(2) . . . . ? O6 Co1 O4 P2 56.6(2) 5_654 . . . ? O2 Co1 O4 P2 174.1(2) . . . . ? O6 P2 O5 Co2 -159.2(2) . . . . ? O4 P2 O5 Co2 73.3(3) . . . . ? O5 Co2 O5 P2 48.0(2) 2_654 . . . ? O1 Co2 O5 P2 -64.5(3) 7_554 . . . ? O1 Co2 O5 P2 174.4(3) 8_556 . . . ? O5 P2 O6 Co1 -40.1(3) . . . 5_654 ? O4 P2 O6 Co1 86.8(3) . . . 5_654 ? 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 H1NB O4 0.87(5) 2.06(5) 2.928(5) 172(4) . N1 H1NA O1 0.82(5) 2.04(5) 2.821(5) 159(5) 4_543 _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 28.56 _diffrn_measured_fraction_theta_full 0.97 _refine_diff_density_max 0.477 _refine_diff_density_min -0.268 _refine_diff_density_rms 0.076