# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 1145/239 data_psi _audit_creation_method SHELXL-97 _chemical_name_systematic ; hydrazinium cobalt phosphate ; _chemical_name_common N2H5CoPO _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H6 Co2 N2 O8 P2' _chemical_formula_weight 341.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 5.1393(6) _cell_length_b 6.3630(10) _cell_length_c 11.2930(10) _cell_angle_alpha 95.650(10) _cell_angle_beta 96.874(9) _cell_angle_gamma 92.786(10) _cell_volume 364.18(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 16 _exptl_crystal_description plate _exptl_crystal_colour 'purple' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.118 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 336 _exptl_absorpt_coefficient_mu 5.021 _exptl_absorpt_correction_type 'semiempirical' _exptl_absorpt_correction_T_min 0.23876 _exptl_absorpt_correction_T_max 0.30436 _exptl_absorpt_process_details '3 psi-scans' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method 'omega-2theta' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '2 hours' _diffrn_standards_decay_% -0.1 _diffrn_reflns_number 1395 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 24.98 _reflns_number_total 1270 _reflns_number_gt 1168 _reflns_threshold_expression >2sigma(I) _computing_data_collection CAD4_(Enraf-Nonius,_1977) _computing_cell_refinement CAD4_(Enraf-Nonius,_1977) _computing_data_reduction SDP_Package_(Enraf-Nonius,_1985) _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-V5.1 (Sheldrick, 1995)' _computing_molecular_graphics 'SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXTL (Siemens, 1994)' _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^)+(0.1148P)^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 1270 _refine_ls_number_parameters 127 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0487 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1429 _refine_ls_wR_factor_gt 0.1385 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _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 0.31830(13) 0.27090(10) 0.60149(6) 0.0108(3) Uani 1 1 d . . . Co2 Co 0.77726(12) 0.03681(11) 0.68911(6) 0.0107(3) Uani 1 1 d . . . P1 P 0.3349(3) 0.2145(2) 0.85639(12) 0.0123(4) Uani 1 1 d . . . P2 P -0.2239(2) 0.2378(2) 0.44052(11) 0.0077(4) Uani 1 1 d . . . O1 O 0.0680(7) 0.1868(5) 0.4417(3) 0.0105(8) Uani 1 1 d . . . O2 O 0.5963(7) 0.2503(6) 0.8080(4) 0.0171(8) Uani 1 1 d . . . O3 O 0.2821(7) 0.5784(5) 0.6350(3) 0.0129(8) Uani 1 1 d . . . O4 O 0.7131(7) 0.2883(5) 0.5698(3) 0.0101(8) Uani 1 1 d . . . O5 O 0.1140(7) 0.2076(6) 0.7512(3) 0.0117(8) Uani 1 1 d . . . O6 O 0.4002(7) -0.0444(5) 0.6176(3) 0.0111(8) Uani 1 1 d . . . O7 O 0.2969(8) 0.4008(7) 0.9495(4) 0.0248(10) Uani 1 1 d . . . H7 H 0.4167 0.4087 1.0049 0.037 Uiso 0.50 1 calc PR . . O8 O 0.3176(8) 0.0068(7) 0.9152(4) 0.0246(10) Uani 1 1 d . . . H8 H 0.4351 0.0098 0.9714 0.037 Uiso 0.50 1 calc PR . . N1 N 0.7629(13) -0.2090(9) 0.8063(5) 0.0330(14) Uani 1 1 d . . . H1A H 0.7891 -0.1430 0.8813 0.040 Uiso 1 1 calc R . . H1B H 0.5957 -0.2632 0.7950 0.040 Uiso 1 1 calc R . . N2 N 0.9174(15) -0.3807(10) 0.8075(7) 0.053(2) Uani 1 1 d . . . H2A H 0.8764 -0.4600 0.8641 0.080 Uiso 1 1 calc R . . H2B H 1.0858 -0.3355 0.8229 0.080 Uiso 1 1 calc R . . H2C H 0.8895 -0.4574 0.7364 0.080 Uiso 1 1 calc R . . 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 0.0084(5) 0.0108(5) 0.0138(5) 0.0013(3) 0.0041(3) -0.0006(3) Co2 0.0057(5) 0.0136(5) 0.0130(5) 0.0020(3) 0.0014(3) -0.0012(3) P1 0.0072(7) 0.0182(8) 0.0109(7) 0.0001(6) 0.0013(5) -0.0005(5) P2 0.0052(7) 0.0086(7) 0.0098(7) 0.0010(5) 0.0031(5) -0.0008(5) O1 0.0034(17) 0.0140(18) 0.0141(18) 0.0023(14) 0.0011(13) -0.0008(14) O2 0.0085(19) 0.022(2) 0.020(2) -0.0046(16) 0.0054(15) -0.0025(15) O3 0.0115(18) 0.0101(18) 0.017(2) 0.0011(15) 0.0008(15) -0.0017(14) O4 0.0059(17) 0.0141(18) 0.0103(18) -0.0020(14) 0.0044(14) -0.0015(14) O5 0.0063(17) 0.0177(18) 0.0110(18) 0.0028(15) 0.0009(14) -0.0017(14) O6 0.0074(18) 0.0085(16) 0.0170(19) -0.0002(14) 0.0023(14) -0.0015(13) O7 0.016(2) 0.036(2) 0.019(2) -0.0145(19) 0.0029(17) -0.0016(18) O8 0.020(2) 0.033(2) 0.022(2) 0.0131(19) 0.0016(17) -0.0013(18) N1 0.047(4) 0.030(3) 0.032(3) 0.018(2) 0.021(3) 0.025(3) N2 0.062(5) 0.036(4) 0.081(5) 0.031(4) 0.051(4) 0.030(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 1.978(4) . ? Co1 O6 2.091(3) . ? Co1 O1 2.094(4) . ? Co1 O4 2.102(3) . ? Co1 O5 2.155(4) . ? Co1 Co2 2.9723(10) . ? Co2 O5 2.011(4) 1_655 ? Co2 O6 2.030(3) . ? Co2 O2 2.139(4) . ? Co2 N1 2.150(5) . ? Co2 O1 2.194(4) 2_656 ? Co2 O4 2.204(4) . ? P1 O2 1.525(4) . ? P1 O5 1.537(4) . ? P1 O8 1.540(4) . ? P1 O7 1.541(4) . ? P2 O3 1.534(4) 2_566 ? P2 O6 1.535(3) 2_556 ? P2 O4 1.539(4) 1_455 ? P2 O1 1.549(4) . ? O1 Co2 2.194(4) 2_656 ? O3 P2 1.535(4) 2_566 ? O4 P2 1.539(4) 1_655 ? O5 Co2 2.011(4) 1_455 ? O6 P2 1.535(3) 2_556 ? O7 H7 0.8200 . ? O8 H8 0.8200 . ? N1 N2 1.382(8) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 H2A 0.8900 . ? N2 H2B 0.8900 . ? N2 H2C 0.8900 . ? 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 163.64(15) . . ? O3 Co1 O1 103.81(14) . . ? O6 Co1 O1 91.81(14) . . ? O3 Co1 O4 97.23(14) . . ? O6 Co1 O4 81.31(13) . . ? O1 Co1 O4 111.03(14) . . ? O3 Co1 O5 91.08(15) . . ? O6 Co1 O5 79.03(14) . . ? O1 Co1 O5 109.24(14) . . ? O4 Co1 O5 135.39(14) . . ? O3 Co1 Co2 125.76(11) . . ? O6 Co1 Co2 43.02(9) . . ? O1 Co1 Co2 125.40(10) . . ? O4 Co1 Co2 47.78(10) . . ? O5 Co1 Co2 92.68(10) . . ? O5 Co2 O6 162.06(15) 1_655 . ? O5 Co2 O2 85.91(14) 1_655 . ? O6 Co2 O2 83.15(14) . . ? O5 Co2 N1 104.3(2) 1_655 . ? O6 Co2 N1 90.3(2) . . ? O2 Co2 N1 91.94(17) . . ? O5 Co2 O1 98.25(14) 1_655 2_656 ? O6 Co2 O1 92.33(14) . 2_656 ? O2 Co2 O1 175.39(13) . 2_656 ? N1 Co2 O1 88.95(18) . 2_656 ? O5 Co2 O4 84.22(13) 1_655 . ? O6 Co2 O4 80.25(13) . . ? O2 Co2 O4 82.23(14) . . ? N1 Co2 O4 169.41(19) . . ? O1 Co2 O4 96.17(13) 2_656 . ? O5 Co2 Co1 117.40(11) 1_655 . ? O6 Co2 Co1 44.66(10) . . ? O2 Co2 Co1 58.57(11) . . ? N1 Co2 Co1 124.51(16) . . ? O1 Co2 Co1 117.38(9) 2_656 . ? O4 Co2 Co1 44.93(9) . . ? O2 P1 O5 108.1(2) . . ? O2 P1 O8 112.4(2) . . ? O5 P1 O8 109.2(2) . . ? O2 P1 O7 109.5(2) . . ? O5 P1 O7 108.6(2) . . ? O8 P1 O7 109.0(3) . . ? O3 P2 O6 107.8(2) 2_566 2_556 ? O3 P2 O4 111.7(2) 2_566 1_455 ? O6 P2 O4 108.12(19) 2_556 1_455 ? O3 P2 O1 109.8(2) 2_566 . ? O6 P2 O1 109.47(19) 2_556 . ? O4 P2 O1 110.0(2) 1_455 . ? P2 O1 Co1 117.4(2) . . ? P2 O1 Co2 125.4(2) . 2_656 ? Co1 O1 Co2 115.09(16) . 2_656 ? P1 O2 Co2 127.5(2) . . ? P2 O3 Co1 135.8(2) 2_566 . ? P2 O4 Co1 118.6(2) 1_655 . ? P2 O4 Co2 116.2(2) 1_655 . ? Co1 O4 Co2 87.29(12) . . ? P1 O5 Co2 138.3(2) . 1_455 ? P1 O5 Co1 103.65(18) . . ? Co2 O5 Co1 108.76(16) 1_455 . ? P2 O6 Co2 140.7(2) 2_556 . ? P2 O6 Co1 125.2(2) 2_556 . ? Co2 O6 Co1 92.32(14) . . ? P1 O7 H7 109.5 . . ? P1 O8 H8 109.5 . . ? N2 N1 Co2 126.0(4) . . ? N2 N1 H1A 105.8 . . ? Co2 N1 H1A 105.8 . . ? N2 N1 H1B 105.8 . . ? Co2 N1 H1B 105.8 . . ? H1A N1 H1B 106.2 . . ? N1 N2 H2A 109.5 . . ? N1 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? N1 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.099 _refine_diff_density_min -1.029 _refine_diff_density_rms 0.255