# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Partha Mukherjee' 'Oindrila Sengupta' _publ_contact_author_name 'Partha Mukherjee' _publ_contact_author_email PSM@IPC.IISC.ERNET.IN _publ_section_title ; Three components assembly of a metal-inorganic 3D Co(II) polymer containing bridging hydrazine ; # Attachment 'Dalton.cif' data_Comp_1 _database_code_depnum_ccdc_archive 'CCDC 727114' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Department of Chemistry University of Anywhere Sometown Somewhere, UK ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H8 Co3 N22' _chemical_formula_weight 493.07 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.8472(8) _cell_length_b 7.1125(6) _cell_length_c 10.5241(8) _cell_angle_alpha 90.00 _cell_angle_beta 98.4390(10) _cell_angle_gamma 90.00 _cell_volume 729.11(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.246 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 486 _exptl_absorpt_coefficient_mu 3.420 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.4075 _exptl_absorpt_correction_T_max 0.5337 _exptl_absorpt_process_details ? _exptl_special_details ; Department of Chemistry University of Anywhere Sometown Somewhere, UK ; _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6077 _diffrn_reflns_av_R_equivalents 0.0194 _diffrn_reflns_av_sigmaI/netI 0.0190 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 28.34 _reflns_number_total 1746 _reflns_number_gt 1639 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2\s(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^)+(0.0275P)^2^+0.0393P] 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 1746 _refine_ls_number_parameters 131 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0215 _refine_ls_R_factor_gt 0.0195 _refine_ls_wR_factor_ref 0.0479 _refine_ls_wR_factor_gt 0.0470 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _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 0.623864(19) 0.04874(3) 0.921009(19) 0.01491(7) Uani 1 1 d . . . Co2 Co 1.0000 0.0000 1.0000 0.01482(8) Uani 1 2 d S . . N1 N 0.44717(13) 0.17568(18) 0.97797(13) 0.0226(3) Uani 1 1 d . . . N2 N 0.38541(13) 0.31141(18) 0.93371(13) 0.0212(3) Uani 1 1 d . . . N3 N 0.32664(18) 0.4407(2) 0.89105(18) 0.0412(4) Uani 1 1 d . . . N4 N 0.74746(13) 0.15503(19) 1.08862(12) 0.0188(3) Uani 1 1 d . . . H4A H 0.7042(19) 0.248(3) 1.1165(17) 0.025(5) Uiso 1 1 d . . . H4B H 0.7647(19) 0.060(3) 1.1496(19) 0.024(5) Uiso 1 1 d . . . N5 N 0.88023(13) 0.22394(19) 1.06329(13) 0.0192(3) Uani 1 1 d . . . H5A H 0.920(2) 0.291(3) 1.1285(19) 0.029(5) Uiso 1 1 d . . . H5B H 0.8640(19) 0.305(3) 1.0018(18) 0.024(5) Uiso 1 1 d . . . N6 N 0.81233(13) -0.08451(19) 0.88168(12) 0.0214(3) Uani 1 1 d . . . N7 N 0.81899(12) -0.14163(17) 0.77613(12) 0.0178(3) Uani 1 1 d . . . N9 N 0.51624(15) -0.03965(19) 0.74067(14) 0.0271(3) Uani 1 1 d . . . N10 N 0.48328(13) -0.18892(18) 0.69867(12) 0.0196(3) Uani 1 1 d . . . N11 N 0.44646(15) -0.3352(2) 0.65578(13) 0.0280(3) Uani 1 1 d . . . N8 N 0.82528(14) -0.1938(2) 0.67344(13) 0.0277(3) Uani 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 0.01246(12) 0.01657(11) 0.01596(12) 0.00050(7) 0.00298(8) -0.00013(7) Co2 0.01252(15) 0.01623(15) 0.01518(15) -0.00103(10) 0.00032(11) 0.00082(10) N1 0.0182(6) 0.0183(6) 0.0331(7) 0.0073(5) 0.0100(6) 0.0038(5) N2 0.0208(6) 0.0182(6) 0.0249(7) -0.0007(5) 0.0044(5) -0.0008(5) N3 0.0445(10) 0.0263(8) 0.0515(11) 0.0089(7) 0.0024(8) 0.0122(7) N4 0.0172(6) 0.0208(6) 0.0189(6) -0.0012(5) 0.0045(5) 0.0024(5) N5 0.0153(6) 0.0185(6) 0.0225(7) -0.0031(5) -0.0011(5) -0.0006(5) N6 0.0137(6) 0.0302(7) 0.0199(7) -0.0075(5) 0.0013(5) 0.0022(5) N7 0.0114(6) 0.0208(6) 0.0206(6) -0.0039(5) -0.0005(5) 0.0031(5) N9 0.0281(8) 0.0234(7) 0.0268(8) -0.0015(5) -0.0061(6) -0.0012(6) N10 0.0167(6) 0.0258(7) 0.0163(6) 0.0000(5) 0.0026(5) 0.0020(5) N11 0.0307(8) 0.0257(7) 0.0286(8) -0.0068(6) 0.0081(6) -0.0043(6) N8 0.0287(8) 0.0322(8) 0.0220(7) -0.0078(6) 0.0027(6) 0.0072(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N1 2.0942(13) 3_657 ? Co1 N1 2.1232(13) . ? Co1 N9 2.1284(14) . ? Co1 N4 2.1293(13) . ? Co1 N8 2.1768(14) 2_656 ? Co1 N6 2.1770(12) . ? Co2 N11 2.1432(14) 2_656 ? Co2 N11 2.1432(14) 4_656 ? Co2 N5 2.1453(13) . ? Co2 N5 2.1453(13) 3_757 ? Co2 N6 2.1567(13) 3_757 ? Co2 N6 2.1567(13) . ? N1 N2 1.1982(18) . ? N1 Co1 2.0942(13) 3_657 ? N2 N3 1.1426(19) . ? N4 N5 1.4570(18) . ? N4 H4A 0.86(2) . ? N4 H4B 0.93(2) . ? N5 H5A 0.88(2) . ? N5 H5B 0.86(2) . ? N6 N7 1.1936(17) . ? N7 N8 1.1529(17) . ? N9 N10 1.1772(19) . ? N10 N11 1.1703(19) . ? N11 Co2 2.1432(14) 2_646 ? N8 Co1 2.1768(13) 2_646 ? 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 Co1 N1 80.34(5) 3_657 . ? N1 Co1 N9 93.89(6) 3_657 . ? N1 Co1 N9 93.21(6) . . ? N1 Co1 N4 92.46(5) 3_657 . ? N1 Co1 N4 90.44(5) . . ? N9 Co1 N4 173.13(5) . . ? N1 Co1 N8 171.65(5) 3_657 2_656 ? N1 Co1 N8 91.38(5) . 2_656 ? N9 Co1 N8 87.66(5) . 2_656 ? N4 Co1 N8 86.43(5) . 2_656 ? N1 Co1 N6 97.02(5) 3_657 . ? N1 Co1 N6 174.62(5) . . ? N9 Co1 N6 91.64(5) . . ? N4 Co1 N6 84.98(5) . . ? N8 Co1 N6 91.13(5) 2_656 . ? N11 Co2 N11 180.0 2_656 4_656 ? N11 Co2 N5 92.27(5) 2_656 . ? N11 Co2 N5 87.73(5) 4_656 . ? N11 Co2 N5 87.73(5) 2_656 3_757 ? N11 Co2 N5 92.27(5) 4_656 3_757 ? N5 Co2 N5 180.000(1) . 3_757 ? N11 Co2 N6 90.18(5) 2_656 3_757 ? N11 Co2 N6 89.82(5) 4_656 3_757 ? N5 Co2 N6 94.44(5) . 3_757 ? N5 Co2 N6 85.56(5) 3_757 3_757 ? N11 Co2 N6 89.82(5) 2_656 . ? N11 Co2 N6 90.18(5) 4_656 . ? N5 Co2 N6 85.56(5) . . ? N5 Co2 N6 94.44(5) 3_757 . ? N6 Co2 N6 180.0 3_757 . ? N2 N1 Co1 128.55(11) . 3_657 ? N2 N1 Co1 128.54(11) . . ? Co1 N1 Co1 99.66(5) 3_657 . ? N3 N2 N1 179.74(19) . . ? N5 N4 Co1 112.77(9) . . ? N5 N4 H4A 107.9(13) . . ? Co1 N4 H4A 107.7(12) . . ? N5 N4 H4B 107.0(12) . . ? Co1 N4 H4B 109.8(12) . . ? H4A N4 H4B 111.7(16) . . ? N4 N5 Co2 110.85(9) . . ? N4 N5 H5A 110.1(12) . . ? Co2 N5 H5A 116.6(12) . . ? N4 N5 H5B 106.8(12) . . ? Co2 N5 H5B 108.3(12) . . ? H5A N5 H5B 103.5(18) . . ? N7 N6 Co2 118.21(10) . . ? N7 N6 Co1 119.33(10) . . ? Co2 N6 Co1 116.81(6) . . ? N8 N7 N6 178.87(16) . . ? N10 N9 Co1 132.46(12) . . ? N11 N10 N9 177.92(16) . . ? N10 N11 Co2 133.17(12) . 2_646 ? N7 N8 Co1 138.28(12) . 2_646 ? 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 N4 H4A N3 0.86(2) 2.24(2) 2.982(2) 145.0(16) 3_667 N4 H4B N11 0.93(2) 2.395(19) 3.0179(19) 124.3(15) 4_656 N4 H4B N3 0.93(2) 2.52(2) 3.236(2) 133.6(14) 4_666 N5 H5A N9 0.88(2) 2.26(2) 3.0963(19) 159.8(17) 4_666 N5 H5B N8 0.86(2) 2.422(19) 3.0274(19) 127.5(15) 2_656 _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.380 _refine_diff_density_min -0.263 _refine_diff_density_rms 0.070