# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name 'M Schroder' 'Alexander J. Blake' 'Marina Felloni' 'Peter Hubberstey' 'Simon J Teat' 'Claire Wilson' _publ_contact_author_name 'M Schroder' _publ_contact_author_email M.SCHRODER@NOTTINGHAM.AC.UK _publ_section_title ; Transition Metal Dipicolinates as Designer T-shaped Building Blocks ; # Attachment 'CIF_1_COPYDM.CIF' data_COPYDM_Complex_1 _database_code_depnum_ccdc_archive 'CCDC 742523' _audit_creation_method SHELXL _chemical_name_systematic ; Cobalt(II) dipicolinate water solvate dimethylsulfoxide bis-solvate ; _chemical_name_common Co(II)(dipic)(H2O)(dmso)2 _chemical_formula_moiety 'C11 H17 Co N O7 S2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C11 H17 Co N O7 S2' _chemical_formula_weight 398.31 _chemical_melting_point ? _chemical_compound_source 'diffusion of ether in mother liquor' 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' S S 0.1246 0.1234 '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 C2/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 9.8087(14) _cell_length_b 11.592(2) _cell_length_c 14.463(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.865(12) _cell_angle_gamma 90.00 _cell_volume 1596.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 39 _cell_measurement_theta_min 13 _cell_measurement_theta_max 17 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.657 _exptl_crystal_density_method ? _exptl_crystal_F_000 820 _exptl_absorpt_coefficient_mu 1.367 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.544 _exptl_absorpt_correction_T_max 0.648 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Stoe Stadi-4 four-circle' _diffrn_measurement_method omega-theta _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'random variation +/- 2.1' _diffrn_reflns_number 3021 _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_av_sigmaI/netI 0.042 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 26.02 _reflns_number_total 1579 _reflns_number_observed 1461 _reflns_observed_criterion I>2sigma(I) _computing_data_collection 'STADI-4 (Stoe & Cie, 1997a)' _computing_cell_refinement STADI-4 _computing_data_reduction 'X-RED version 1.09 (Stoe & Cie, 1997b)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008); SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL93 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1994)' _computing_publication_material 'SHELXL93; PLATON (Spek, 2003)' _refine_special_details ; ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_DETAILS 'calc w=1/[\s^2^(Fo^2^)+(0.0231P)^2^+1.9438P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary 'difference Fourier methods' _atom_sites_solution_hydrogens ; aromatic Hs placed geometrically; water Hs from q-peaks list; dmso Hs from delta F synthesis ; _refine_ls_hydrogen_treatment ; aromatic Hs refined by riding model; water Hs refined with restraints; dmso Hs refined as rigid rotators ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1573 _refine_ls_number_parameters 136 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0291 _refine_ls_R_factor_obs 0.0257 _refine_ls_wR_factor_all 0.0671 _refine_ls_wR_factor_obs 0.0640 _refine_ls_goodness_of_fit_all 1.083 _refine_ls_goodness_of_fit_obs 1.099 _refine_ls_restrained_S_all 1.106 _refine_ls_restrained_S_obs 1.099 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co Co 0.5000 0.17824(3) 0.7500 0.01438(12) Uani 1 d S . N1 N 0.5000 0.3538(2) 0.7500 0.0148(4) Uani 1 d S . O1R O 0.64022(14) 0.17244(11) 0.88938(9) 0.0199(3) Uani 1 d . . S1R S 0.58942(5) 0.10144(4) 0.96324(3) 0.02309(14) Uani 1 d . . C1R C 0.5455(3) 0.2028(2) 1.0443(2) 0.0351(5) Uani 1 d . . H1R1 H 0.5199 0.1622 1.0955 0.053 Uiso 1 calc R . H1R2 H 0.4680 0.2494 1.0115 0.053 Uiso 1 calc R . H1R3 H 0.6251 0.2513 1.0695 0.053 Uiso 1 calc R . O1S O 0.5000 0.0054(2) 0.7500 0.0256(4) Uani 1 d SD . H1SA H 0.4366(21) -0.0354(20) 0.7212(18) 0.038 Uiso 1 d D . C2R C 0.7445(3) 0.0420(2) 1.0383(2) 0.0341(5) Uani 1 d . . H2R1 H 0.7202 -0.0012 1.0887 0.051 Uiso 1 calc R . H2R2 H 0.8075 0.1033 1.0651 0.051 Uiso 1 calc R . H2R3 H 0.7892 -0.0080 1.0016 0.051 Uiso 1 calc R . C2 C 0.4025(2) 0.40951(15) 0.78281(12) 0.0161(4) Uani 1 d . . O3 O 0.32962(14) 0.22166(11) 0.81086(10) 0.0205(3) Uani 1 d . . C3 C 0.3989(2) 0.5294(2) 0.78428(13) 0.0205(4) Uani 1 d . . H3 H 0.3312 0.5685 0.80741 0.025 Uiso 1 calc R . O4 O 0.20209(14) 0.36937(12) 0.84397(10) 0.0247(3) Uani 1 d . . C4 C 0.5000 0.5893(2) 0.7500 0.0239(6) Uani 1 d S . H4 H 0.5000 0.6695 0.7500 0.029 Uiso 1 calc SR . C8 C 0.3019(2) 0.3275(2) 0.81531(12) 0.0172(4) Uani 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 Co 0.0153(2) 0.0118(2) 0.0154(2) 0.000 0.00231(12) 0.000 N1 0.0158(10) 0.0147(10) 0.0125(9) 0.000 0.0005(8) 0.000 O1R 0.0205(6) 0.0218(7) 0.0159(6) 0.0023(5) 0.0014(5) -0.0053(5) S1R 0.0271(3) 0.0253(3) 0.0149(2) 0.0017(2) 0.0012(2) -0.0116(2) C1R 0.0384(12) 0.0439(13) 0.0272(11) -0.0080(9) 0.0161(9) -0.0147(10) O1S 0.0261(11) 0.0139(9) 0.0296(11) 0.000 -0.0073(8) 0.000 C2R 0.0412(13) 0.0338(11) 0.0204(10) 0.0069(8) -0.0062(9) -0.0046(10) C2 0.0163(8) 0.0170(8) 0.0131(8) -0.0008(6) 0.0001(7) 0.0012(7) O3 0.0197(6) 0.0165(6) 0.0266(7) -0.0013(5) 0.0085(5) -0.0019(5) C3 0.0217(9) 0.0173(9) 0.0216(9) -0.0015(7) 0.0034(7) 0.0044(7) O4 0.0221(7) 0.0263(7) 0.0280(7) 0.0036(6) 0.0108(6) 0.0059(6) C4 0.0284(14) 0.0140(12) 0.0275(14) 0.000 0.0030(11) 0.000 C8 0.0161(8) 0.0207(9) 0.0133(8) 0.0001(6) 0.0003(6) 0.0019(7) _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 Co O1S 2.003(2) . y Co N1 2.035(2) . y Co O3 2.1275(13) . y Co O3 2.1275(13) 2_656 n Co O1R 2.1519(13) . y Co O1R 2.1519(13) 2_656 n N1 C2 1.332(2) 2_656 ? N1 C2 1.332(2) . ? O1R S1R 1.5238(13) . ? S1R C2R 1.782(2) . ? S1R C1R 1.784(2) . ? C2 C3 1.391(3) . ? C2 C8 1.524(3) . ? O3 C8 1.262(2) . ? C3 C4 1.395(2) . ? O4 C8 1.249(2) . ? C4 C3 1.395(2) 2_656 ? 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 O1S Co N1 180 . . y O1S Co O3 103.69(3) . . y N1 Co O3 76.31(3) . . y O1S Co O3 103.69(3) . 2_656 y N1 Co O3 76.31(3) . 2_656 y O3 Co O3 152.63(7) . 2_656 y O1S Co O1R 88.21(3) . . y N1 Co O1R 91.79(3) . . y O3 Co O1R 90.51(5) . . y O3 Co O1R 90.34(5) 2_656 . y O1S Co O1R 88.21(3) . 2_656 y N1 Co O1R 91.79(3) . 2_656 y O3 Co O1R 90.34(5) . 2_656 y O3 Co O1R 90.51(5) 2_656 2_656 y O1R Co O1R 176.42(7) . 2_656 y C2 N1 C2 122.0(2) 2_656 . ? C2 N1 Co 119.01(10) 2_656 . y C2 N1 Co 119.01(10) . . y S1R O1R Co 115.51(7) . . y O1R S1R C2R 105.14(10) . . ? O1R S1R C1R 106.01(9) . . ? C2R S1R C1R 99.16(12) . . ? N1 C2 C3 120.9(2) . . ? N1 C2 C8 112.40(15) . . ? C3 C2 C8 126.7(2) . . ? C8 O3 Co 116.85(11) . . y C2 C3 C4 118.0(2) . . ? C3 C4 C3 120.3(2) . 2_656 ? O4 C8 O3 126.2(2) . . ? O4 C8 C2 118.5(2) . . ? O3 C8 C2 115.3(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 C2 N1 C2 C3 -0.13(12) 2_656 . . . ? C2 N1 C2 C8 179.3(2) 2_656 . . . ? N1 C2 C3 C4 0.3(2) . . . . ? C8 C2 C3 C4 -179.13(14) . . . . ? C2 C3 C4 C3 -0.13(11) . . . 2_656 ? N1 C2 C8 O4 -177.11(14) . . . . ? C3 C2 C8 O4 2.3(3) . . . . ? N1 C2 C8 O3 3.4(2) . . . . ? C3 C2 C8 O3 -177.2(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.36 _refine_diff_density_min -0.32 _refine_diff_density_rms 0.07 #=== END of CIF # Attachment 'CIF_2_PC44CO.CIF' data_PC44CO_Complex_2 _database_code_depnum_ccdc_archive 'CCDC 742524' _refine_special_details ; Data shows non-merohedral twinning which was treated by creating an hklf5 format file. The twin law corresponds to a 180 degree rotation about the 0 0 -1 reciprocal lattice vector and the BASF refined to 0.424(3). ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Co(II)(dipic)(bipy)](MeOH)(H2O)' _chemical_melting_point ? _chemical_formula_moiety 'C17 H11 Co N3 O4, C H4 O, H2 O' _chemical_formula_sum 'C18 H17 Co N3 O6' _chemical_formula_weight 430.28 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' 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 'P 21/n' 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 11.294(2) _cell_length_b 10.135(2) _cell_length_c 15.520(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.32(3) _cell_angle_gamma 90.00 _cell_volume 1757.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3144 _cell_measurement_theta_min 3.8 _cell_measurement_theta_max 27.6 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.626 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 884 _exptl_absorpt_coefficient_mu 1.020 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.77 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'Bruker SAINT v6.02a' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.6861 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method 'w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5282 _diffrn_reflns_av_R_equivalents 0.033 _diffrn_reflns_av_sigmaI/netI 0.069 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.84 _diffrn_reflns_theta_max 27.62 _reflns_number_total 3348 _reflns_number_gt 4391 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Bruker SMART v5.624 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT v6.02A (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL/PC v5.1 (Sheldrick, 2008)' _computing_publication_material 'SHELXL97; PLATON (Spek, 2003)' _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^)+13.42P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary 'difference Fourier method' _atom_sites_solution_hydrogens 'geometrically placed' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5168 _refine_ls_number_parameters 244 _refine_ls_number_restraints 74 _refine_ls_R_factor_all 0.0834 _refine_ls_R_factor_gt 0.0734 _refine_ls_wR_factor_ref 0.197 _refine_ls_wR_factor_gt 0.192 _refine_ls_goodness_of_fit_ref 1.17 _refine_ls_restrained_S_all 1.16 _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 Co Co -0.74552(7) 0.76029(6) -1.31340(5) 0.0102(2) Uani 1 1 d U . . N1 N -0.7841(4) 0.6418(4) -1.4209(3) 0.0131(9) Uani 1 1 d U . . C2 C -0.7967(5) 0.6974(5) -1.4991(3) 0.0149(12) Uani 1 1 d U . . C3 C -0.8358(7) 0.6276(5) -1.5738(4) 0.0258(15) Uani 1 1 d U . . H3 H -0.8441 0.6677 -1.6282 0.031 Uiso 1 1 calc R . . C4 C -0.8624(8) 0.4955(6) -1.5650(4) 0.0348(18) Uani 1 1 d U . . H4 H -0.8930 0.4468 -1.6139 0.042 Uiso 1 1 calc R . . C5 C -0.8439(6) 0.4350(5) -1.4844(4) 0.0248(15) Uani 1 1 d U . . H5 H -0.8578 0.3453 -1.4783 0.030 Uiso 1 1 calc R . . C6 C -0.8038(5) 0.5139(5) -1.4126(3) 0.0136(11) Uani 1 1 d U . . C7 C -0.7644(5) 0.8430(5) -1.4962(4) 0.0152(11) Uani 1 1 d U . . O1 O -0.7474(4) 0.8982(4) -1.5623(3) 0.0221(9) Uani 1 1 d U . . O2 O -0.7555(3) 0.8924(3) -1.4197(2) 0.0118(8) Uani 1 1 d U . . C8 C -0.7807(5) 0.4695(4) -1.3195(3) 0.0114(11) Uani 1 1 d U . . O3 O -0.7916(3) 0.3480(3) -1.3050(2) 0.0138(8) Uani 1 1 d U . . O4 O -0.7509(4) 0.5566(3) -1.2644(2) 0.0130(8) Uani 1 1 d U . . N1L N -0.9290(5) 0.7779(5) -1.3018(3) 0.0181(10) Uani 1 1 d U . . C2L C -0.9764(6) 0.7252(5) -1.2353(4) 0.0188(12) Uani 1 1 d U . . H2L H -0.9246 0.6891 -1.1893 0.023 Uiso 1 1 calc R . . C3L C -1.0985(5) 0.7214(5) -1.2309(4) 0.0196(12) Uani 1 1 d U . . H3L H -1.1269 0.6838 -1.1831 0.023 Uiso 1 1 calc R . . C4L C -1.1771(5) 0.7745(5) -1.2989(3) 0.0132(10) Uani 1 1 d U . . C5L C -1.1299(5) 0.8322(5) -1.3665(4) 0.0138(11) Uani 1 1 d U . . H5L H -1.1801 0.8721 -1.4119 0.017 Uiso 1 1 calc R . . C6L C -1.0077(5) 0.8308(5) -1.3671(4) 0.0143(11) Uani 1 1 d U . . H6L H -0.9779 0.8679 -1.4144 0.017 Uiso 1 1 calc R . . C7L C -1.3078(5) 0.7669(5) -1.3014(4) 0.0156(11) Uani 1 1 d U . . C8L C -1.3626(5) 0.6625(5) -1.2657(4) 0.0182(12) Uani 1 1 d U . . H8L H -1.3167 0.5946 -1.2378 0.022 Uiso 1 1 calc R . . C9L C -1.4850(5) 0.6596(5) -1.2716(4) 0.0168(12) Uani 1 1 d U . . H9L H -1.5196 0.5882 -1.2471 0.020 Uiso 1 1 calc R . . N10L N -1.5563(5) 0.7515(5) -1.3097(3) 0.0217(11) Uani 1 1 d U . . C11L C -1.5028(6) 0.8558(5) -1.3437(4) 0.0234(14) Uani 1 1 d U . . H11L H -1.5507 0.9239 -1.3694 0.028 Uiso 1 1 calc R . . C12L C -1.3811(5) 0.8646(5) -1.3416(4) 0.0225(13) Uani 1 1 d U . . H12L H -1.3481 0.9361 -1.3672 0.027 Uiso 1 1 calc R . . O1W O -0.8832(5) 0.1316(4) -1.4238(3) 0.0373(13) Uani 1 1 d . . . O1M O -0.9684(16) 0.8327(16) -1.0105(11) 0.092(5) Uiso 0.50 1 d PDU . . C1M C -1.005(3) 0.952(2) -1.0461(18) 0.118(10) Uiso 0.50 1 d PDU . . 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 Co 0.0063(4) 0.0099(3) 0.0145(4) -0.0014(3) 0.0016(3) -0.0013(3) N1 0.011(3) 0.0121(19) 0.017(2) 0.0010(15) 0.003(2) 0.0043(16) C2 0.015(4) 0.016(2) 0.015(3) -0.0003(17) 0.006(3) -0.0006(19) C3 0.041(5) 0.021(3) 0.015(3) 0.000(2) 0.005(3) -0.006(2) C4 0.067(6) 0.019(3) 0.017(3) -0.003(2) 0.001(3) -0.005(3) C5 0.041(5) 0.011(2) 0.021(3) -0.0037(19) 0.001(3) -0.003(2) C6 0.010(3) 0.015(2) 0.015(2) -0.0004(17) 0.001(2) 0.0009(19) C7 0.009(3) 0.014(2) 0.024(3) 0.0016(18) 0.008(3) -0.0004(18) O1 0.029(3) 0.0185(19) 0.020(2) 0.0054(15) 0.007(2) -0.0009(16) O2 0.008(2) 0.0114(16) 0.0161(19) -0.0009(12) 0.0021(16) -0.0022(13) C8 0.005(3) 0.010(2) 0.020(3) -0.0017(17) 0.005(2) 0.0023(16) O3 0.011(2) 0.0110(16) 0.0183(19) 0.0038(13) -0.0014(18) -0.0016(12) O4 0.012(2) 0.0154(16) 0.0106(18) -0.0005(12) -0.0020(17) -0.0012(13) N1L 0.006(3) 0.028(2) 0.020(3) -0.0006(18) 0.000(2) -0.0027(17) C2L 0.012(3) 0.025(3) 0.019(3) 0.002(2) 0.001(3) 0.006(2) C3L 0.011(3) 0.026(3) 0.023(3) 0.003(2) 0.006(3) 0.001(2) C4L 0.008(3) 0.013(2) 0.019(3) -0.0048(18) 0.001(2) 0.0016(17) C5L 0.003(3) 0.018(3) 0.020(3) 0.0058(19) -0.001(2) 0.0038(18) C6L 0.005(3) 0.021(3) 0.016(3) 0.0002(19) 0.000(2) -0.0051(19) C7L 0.011(3) 0.016(2) 0.019(3) -0.0026(19) 0.002(2) -0.0016(18) C8L 0.010(3) 0.022(3) 0.024(3) 0.002(2) 0.004(3) -0.004(2) C9L 0.011(3) 0.019(3) 0.021(3) 0.0011(19) 0.003(3) -0.004(2) N10L 0.010(3) 0.026(2) 0.030(3) 0.003(2) 0.006(2) -0.0029(19) C11L 0.010(3) 0.015(3) 0.045(4) 0.007(2) 0.004(3) 0.002(2) C12L 0.002(3) 0.016(3) 0.050(4) 0.009(2) 0.005(3) -0.0001(19) O1W 0.055(4) 0.029(2) 0.025(2) 0.0034(18) -0.008(3) 0.006(2) _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 Co O3 2.029(4) 2_352 ? Co N1 2.051(4) . ? Co N1L 2.113(5) . ? Co O2 2.115(3) . ? Co N10L 2.131(5) 1_655 ? Co O4 2.204(3) . ? N1 C6 1.325(6) . ? N1 C2 1.326(7) . ? C2 C3 1.376(8) . ? C2 C7 1.519(7) . ? C3 C4 1.383(8) . ? C4 C5 1.381(8) . ? C5 C6 1.393(7) . ? C6 C8 1.500(7) . ? C7 O1 1.207(6) . ? C7 O2 1.279(6) . ? C8 O4 1.240(6) . ? C8 O3 1.262(6) . ? N1L C2L 1.341(7) . ? N1L C6L 1.357(7) . ? C2L C3L 1.391(8) . ? C3L C4L 1.386(8) . ? C4L C5L 1.376(7) . ? C4L C7L 1.473(8) . ? C5L C6L 1.381(8) . ? C7L C12L 1.381(8) . ? C7L C8L 1.381(7) . ? C8L C9L 1.373(8) . ? C9L N10L 1.315(7) . ? N10L C11L 1.361(7) . ? C11L C12L 1.374(8) . ? O1M C1M 1.370(10) . ? 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 Co N1 170.00(15) 2_352 . ? O3 Co N1L 87.85(18) 2_352 . ? N1 Co N1L 91.35(19) . . ? O3 Co O2 114.20(14) 2_352 . ? N1 Co O2 75.80(14) . . ? N1L Co O2 94.07(17) . . ? O3 Co N10L 85.35(18) 2_352 1_655 ? N1 Co N10L 95.25(19) . 1_655 ? N1L Co N10L 173.2(2) . 1_655 ? O2 Co N10L 89.27(17) . 1_655 ? O3 Co O4 96.34(13) 2_352 . ? N1 Co O4 73.68(15) . . ? N1L Co O4 88.48(16) . . ? O2 Co O4 149.42(13) . . ? N10L Co O4 91.68(17) 1_655 . ? C6 N1 C2 120.5(5) . . ? C6 N1 Co 120.8(3) . . ? C2 N1 Co 118.5(3) . . ? N1 C2 C3 122.1(5) . . ? N1 C2 C7 113.1(5) . . ? C3 C2 C7 124.8(5) . . ? C2 C3 C4 117.5(5) . . ? C5 C4 C3 120.9(6) . . ? C4 C5 C6 117.3(5) . . ? N1 C6 C5 121.6(5) . . ? N1 C6 C8 112.3(4) . . ? C5 C6 C8 126.1(5) . . ? O1 C7 O2 127.3(5) . . ? O1 C7 C2 119.5(5) . . ? O2 C7 C2 113.1(4) . . ? C7 O2 Co 117.7(3) . . ? O4 C8 O3 126.5(5) . . ? O4 C8 C6 116.3(4) . . ? O3 C8 C6 117.2(4) . . ? C8 O3 Co 125.2(3) . 2_342 ? C8 O4 Co 116.5(3) . . ? C2L N1L C6L 116.1(5) . . ? C2L N1L Co 122.5(4) . . ? C6L N1L Co 121.0(3) . . ? N1L C2L C3L 123.9(6) . . ? C4L C3L C2L 118.8(5) . . ? C5L C4L C3L 118.0(5) . . ? C5L C4L C7L 120.0(5) . . ? C3L C4L C7L 121.9(5) . . ? C4L C5L C6L 119.9(5) . . ? N1L C6L C5L 123.1(5) . . ? C12L C7L C8L 117.2(5) . . ? C12L C7L C4L 120.5(5) . . ? C8L C7L C4L 122.3(5) . . ? C9L C8L C7L 119.7(5) . . ? N10L C9L C8L 124.1(5) . . ? C9L N10L C11L 116.5(5) . . ? C9L N10L Co 126.1(4) . 1_455 ? C11L N10L Co 117.2(4) . 1_455 ? N10L C11L C12L 122.7(5) . . ? C11L C12L C7L 119.8(5) . . ? _diffrn_measured_fraction_theta_max 0.737 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.745 _refine_diff_density_max 1.45 _refine_diff_density_min -0.87 _refine_diff_density_rms 0.20 #===END of CIF # Attachment 'CIF_3_COBPHY.CIF' data_COBPHY_Complex_3 _database_code_depnum_ccdc_archive 'CCDC 742525' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Co(II) dipic 0.5(4,4-bipy) 2(H2O)] 2(H2O)' _chemical_melting_point ? _chemical_formula_moiety 'C12 H11 N2 O6 Co, 2(H2 O)' _chemical_formula_sum 'C12 H15 Co N2 O8' _chemical_formula_weight 374.19 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' 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.5281(9) _cell_length_b 20.152(2) _cell_length_c 7.3501(6) _cell_angle_alpha 90.00 _cell_angle_beta 107.5390(10) _cell_angle_gamma 90.00 _cell_volume 1486.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4057 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 28.2 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.672 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 1.199 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.892 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'SADABS (Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time 5 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6885 _diffrn_reflns_av_R_equivalents 0.0158 _diffrn_reflns_av_sigmaI/netI 0.0228 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 28.56 _reflns_number_total 3424 _reflns_number_gt 2921 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART version 5.624 (Bruker, 1998)' _computing_cell_refinement 'SAINT version 6.02A (Bruker, 2001)' _computing_data_reduction 'SAINT; SHELXTL (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics SHELXTL _computing_publication_material 'SHELXL97; PLATON (Spek, 2003)' _refine_special_details ; ; _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^)+(0.0402P)^2^+0.4914P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary 'difference Fourier method' _atom_sites_solution_hydrogens 'water Hs located from difmap, others geometrically placed' _refine_ls_hydrogen_treatment 'water Hs refined with restraints, others with riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3321 _refine_ls_number_parameters 232 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0715 _refine_ls_wR_factor_gt 0.0692 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 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 Co Co 0.56804(2) 0.893393(11) 0.19631(3) 0.01504(8) Uani 1 1 d . . . O1W O 0.47496(12) 0.90830(6) -0.10181(17) 0.0194(2) Uani 1 1 d D . . H1WA H 0.482(2) 0.8759(7) -0.164(3) 0.029 Uiso 1 1 d D . . H1WB H 0.503(2) 0.9404(7) -0.145(3) 0.029 Uiso 1 1 d D . . O2W O 0.66749(12) 0.88378(6) 0.49309(17) 0.0184(2) Uani 1 1 d D . . H2WA H 0.676(2) 0.9208(6) 0.543(3) 0.028 Uiso 1 1 d D . . H2WB H 0.6275(19) 0.8598(8) 0.546(3) 0.028 Uiso 1 1 d D . . N1 N 0.40372(13) 0.84874(7) 0.23093(18) 0.0145(3) Uani 1 1 d . . . C2 C 0.39003(15) 0.78342(8) 0.2125(2) 0.0156(3) Uani 1 1 d . . . C3 C 0.27775(16) 0.75172(8) 0.2331(2) 0.0189(3) Uani 1 1 d . . . H3A H 0.2673 0.7050 0.2189 0.023 Uiso 1 1 calc R . . C4 C 0.18109(16) 0.79075(9) 0.2754(2) 0.0218(4) Uani 1 1 d . . . H4A H 0.1023 0.7707 0.2873 0.026 Uiso 1 1 calc R . . C5 C 0.19925(15) 0.85876(9) 0.3000(2) 0.0198(3) Uani 1 1 d . . . H5A H 0.1350 0.8855 0.3325 0.024 Uiso 1 1 calc R . . C6 C 0.31375(15) 0.88673(8) 0.2760(2) 0.0161(3) Uani 1 1 d . . . C7 C 0.50736(16) 0.75004(8) 0.1698(2) 0.0162(3) Uani 1 1 d . . . O1 O 0.51001(12) 0.68859(6) 0.16045(16) 0.0201(2) Uani 1 1 d . . . O2 O 0.59515(11) 0.78938(6) 0.14481(17) 0.0192(2) Uani 1 1 d . . . C8 C 0.35153(15) 0.95960(8) 0.2981(2) 0.0160(3) Uani 1 1 d . . . O3 O 0.28038(11) 0.99689(6) 0.36027(17) 0.0217(3) Uani 1 1 d . . . O4 O 0.45448(11) 0.97587(6) 0.25066(16) 0.0191(2) Uani 1 1 d . . . N1L N 0.74186(13) 0.93064(7) 0.15736(19) 0.0186(3) Uani 1 1 d . . . C2L C 0.79419(18) 0.98955(9) 0.2202(3) 0.0260(4) Uani 1 1 d . . . H2L H 0.7604 1.0128 0.3081 0.031 Uiso 1 1 calc R . . C3L C 0.89565(18) 1.01861(10) 0.1636(3) 0.0273(4) Uani 1 1 d . . . H3L H 0.9292 1.0610 0.2108 0.033 Uiso 1 1 calc R . . C4L C 0.94801(15) 0.98481(9) 0.0363(2) 0.0184(3) Uani 1 1 d . . . C5L C 0.89726(17) 0.92202(9) -0.0214(2) 0.0215(3) Uani 1 1 d . . . H5L H 0.9330 0.8963 -0.1027 0.026 Uiso 1 1 calc R . . C6L C 0.79486(17) 0.89692(9) 0.0394(3) 0.0218(4) Uani 1 1 d . . . H6L H 0.7605 0.8542 -0.0036 0.026 Uiso 1 1 calc R . . O1R O 0.85848(14) 0.74135(8) 0.3086(2) 0.0379(3) Uani 1 1 d D . . H1RA H 0.7811(13) 0.7537(13) 0.255(3) 0.057 Uiso 1 1 d D . . H1RB H 0.878(2) 0.7216(13) 0.222(3) 0.057 Uiso 1 1 d D . . O1T O 0.94700(15) 0.84254(9) 0.5611(2) 0.0437(4) Uani 1 1 d D . . H1TA H 0.933(3) 0.8132(11) 0.477(3) 0.066 Uiso 1 1 d D . . H1TB H 0.8802(19) 0.8659(12) 0.538(4) 0.066 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 Co 0.01410(12) 0.01408(13) 0.01997(12) 0.00009(8) 0.00972(9) -0.00147(8) O1W 0.0248(6) 0.0148(6) 0.0214(6) 0.0001(5) 0.0113(5) -0.0016(5) O2W 0.0204(6) 0.0161(6) 0.0211(6) -0.0004(5) 0.0100(5) -0.0018(5) N1 0.0149(6) 0.0144(7) 0.0152(6) -0.0002(5) 0.0063(5) -0.0012(5) C2 0.0175(7) 0.0157(8) 0.0142(7) 0.0005(6) 0.0057(6) -0.0002(6) C3 0.0222(8) 0.0153(8) 0.0202(8) -0.0022(6) 0.0079(6) -0.0057(6) C4 0.0164(8) 0.0251(10) 0.0262(8) -0.0008(7) 0.0099(6) -0.0059(6) C5 0.0136(7) 0.0250(9) 0.0225(8) -0.0002(7) 0.0083(6) 0.0008(6) C6 0.0153(7) 0.0176(8) 0.0154(7) 0.0004(6) 0.0049(6) 0.0004(6) C7 0.0193(8) 0.0168(9) 0.0133(7) 0.0004(6) 0.0063(6) 0.0010(6) O1 0.0273(6) 0.0144(6) 0.0218(6) -0.0009(5) 0.0122(5) 0.0007(5) O2 0.0184(5) 0.0170(6) 0.0266(6) 0.0003(5) 0.0133(5) -0.0005(4) C8 0.0168(7) 0.0153(8) 0.0156(7) 0.0000(6) 0.0044(6) 0.0007(6) O3 0.0191(6) 0.0199(6) 0.0281(6) -0.0045(5) 0.0104(5) 0.0019(5) O4 0.0199(6) 0.0162(6) 0.0244(6) 0.0014(5) 0.0114(5) -0.0001(4) N1L 0.0170(7) 0.0207(8) 0.0212(7) 0.0011(6) 0.0103(5) -0.0027(5) C2L 0.0252(9) 0.0292(10) 0.0303(9) -0.0076(8) 0.0184(7) -0.0073(7) C3L 0.0278(9) 0.0270(10) 0.0335(10) -0.0084(8) 0.0190(8) -0.0107(7) C4L 0.0140(7) 0.0232(9) 0.0191(7) 0.0009(6) 0.0065(6) -0.0020(6) C5L 0.0212(8) 0.0228(9) 0.0244(8) 0.0007(7) 0.0128(7) -0.0003(7) C6L 0.0211(8) 0.0194(9) 0.0280(9) -0.0007(7) 0.0122(7) -0.0028(7) O1R 0.0264(7) 0.0380(9) 0.0481(9) -0.0008(7) 0.0093(6) 0.0029(6) O1T 0.0355(9) 0.0435(10) 0.0486(9) -0.0077(8) 0.0075(7) 0.0064(7) _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 Co N1 2.0329(13) . y Co N1L 2.0760(13) . y Co O2W 2.1250(12) . y Co O1W 2.1349(12) . y Co O4 2.1539(12) . y Co O2 2.1640(12) . y N1 C2 1.327(2) . ? N1 C6 1.335(2) . ? C2 C3 1.392(2) . ? C2 C7 1.520(2) . ? C3 C4 1.393(2) . ? C4 C5 1.388(3) . ? C5 C6 1.389(2) . ? C6 C8 1.517(2) . ? C7 O1 1.241(2) . ? C7 O2 1.2725(19) . ? C8 O3 1.2414(19) . ? C8 O4 1.2773(19) . ? N1L C2L 1.332(2) . ? N1L C6L 1.348(2) . ? C2L C3L 1.387(2) . ? C3L C4L 1.397(2) . ? C4L C5L 1.389(2) . ? C4L C4L 1.487(3) 3_775 ? C5L C6L 1.381(2) . ? 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 Co N1L 174.91(6) . . y N1 Co O2W 90.33(5) . . y N1L Co O2W 89.57(5) . . y N1 Co O1W 92.64(5) . . y N1L Co O1W 87.63(5) . . y O2W Co O1W 176.57(5) . . y N1 Co O4 77.14(5) . . y N1L Co O4 107.95(5) . . y O2W Co O4 90.53(4) . . y O1W Co O4 88.45(5) . . y N1 Co O2 75.83(5) . . y N1L Co O2 99.08(5) . . y O2W Co O2 92.36(5) . . y O1W Co O2 90.04(5) . . y O4 Co O2 152.83(4) . . y C2 N1 C6 122.07(14) . . ? C2 N1 Co 119.78(11) . . y C6 N1 Co 118.13(11) . . y N1 C2 C3 120.93(15) . . ? N1 C2 C7 112.96(13) . . ? C3 C2 C7 126.10(15) . . ? C2 C3 C4 117.82(15) . . ? C5 C4 C3 120.35(15) . . ? C4 C5 C6 118.34(15) . . ? N1 C6 C5 120.43(15) . . ? N1 C6 C8 113.49(14) . . ? C5 C6 C8 126.07(15) . . ? O1 C7 O2 125.75(15) . . ? O1 C7 C2 119.10(14) . . ? O2 C7 C2 115.15(14) . . ? C7 O2 Co 116.00(10) . . y O3 C8 O4 126.94(16) . . ? O3 C8 C6 117.21(14) . . ? O4 C8 C6 115.85(14) . . ? C8 O4 Co 114.62(10) . . y C2L N1L C6L 117.66(14) . . ? C2L N1L Co 124.36(11) . . y C6L N1L Co 117.36(11) . . y N1L C2L C3L 123.22(16) . . ? C2L C3L C4L 119.31(17) . . ? C5L C4L C3L 117.08(15) . . ? C5L C4L C4L 121.49(19) . 3_775 ? C3L C4L C4L 121.42(19) . 3_775 ? C6L C5L C4L 120.05(15) . . ? N1L C6L C5L 122.56(16) . . ? _diffrn_measured_fraction_theta_max 0.876 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 0.440 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.060 # Attachment 'CIF_4_BPCODP.CIF' data_BPCODP_Complex_4 _database_code_depnum_ccdc_archive 'CCDC 742526' _refine_special_details ; one oxygen of a water molecule is half occupied, and its H atom has not been found ; _audit_creation_method SHELXL97 _chemical_name_systematic ; ? ; _chemical_name_common "[Co(II)(H2O)(dipic)(4,4'-bipy)](H2O)" _chemical_melting_point ? _chemical_formula_moiety 'C24 H22 Co2 N4 O12, 3(H2 O)' _chemical_formula_sum 'C24 H28 Co2 N4 O15' _chemical_formula_weight 730.36 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' 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 C2/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 25.230(2) _cell_length_b 10.5470(9) _cell_length_c 10.9426(9) _cell_angle_alpha 90 _cell_angle_beta 109.021(1) _cell_angle_gamma 90 _cell_volume 2752.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5346 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 27.95 _exptl_crystal_description tablet _exptl_crystal_colour purple _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.762 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 1.290 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.919 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Bruker SADABS v2.03 (Bruker, 2001)' _exptl_special_details ; half occupied oxygen of a water molecule ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 11764 _diffrn_reflns_av_R_equivalents 0.020 _diffrn_reflns_av_sigmaI/netI 0.019 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 28.11 _reflns_number_total 3319 _reflns_number_gt 2852 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.02a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97; PLATON (Spek, 2002)' _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^)+(0.039P)^2^+5.326P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary 'difference Fourier method' _atom_sites_solution_hydrogens ; aromatic hydrogens geometrically placed, water hydrogens located from delta-F synthesis ; _refine_ls_hydrogen_treatment ; aromatic hydrogens refined with riding model, water hydrogens refined with restraints ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3152 _refine_ls_number_parameters 222 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0355 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0790 _refine_ls_wR_factor_gt 0.0766 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.053 _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 Co Co 0.357971(10) 0.72504(2) 0.09260(2) 0.01522(9) Uani 1 1 d . . . O1V O 0.30231(6) 0.75114(14) 0.19693(14) 0.0212(3) Uani 1 1 d D . . H1VA H 0.2711(6) 0.721(2) 0.169(2) 0.032 Uiso 1 1 d D . . H1VB H 0.3041(10) 0.8130(17) 0.242(2) 0.032 Uiso 1 1 d D . . O1W O 0.41125(6) 0.67967(15) -0.01356(15) 0.0254(3) Uani 1 1 d D . . H1WA H 0.4410(7) 0.718(2) 0.007(3) 0.038 Uiso 1 1 d D . . H1WB H 0.4175(10) 0.6049(10) -0.018(3) 0.038 Uiso 1 1 d D . . N1 N 0.38901(6) 0.90230(15) 0.13557(15) 0.0155(3) Uani 1 1 d . . . C2 C 0.36798(7) 0.99576(17) 0.05176(18) 0.0162(4) Uani 1 1 d . . . C3 C 0.38563(8) 1.12035(18) 0.0820(2) 0.0203(4) Uani 1 1 d . . . H3 H 0.3723 1.1865 0.0207 0.024 Uiso 1 1 calc R . . C4 C 0.42325(9) 1.14535(19) 0.2038(2) 0.0249(4) Uani 1 1 d . . . H4 H 0.4344 1.2302 0.2282 0.030 Uiso 1 1 calc R . . C5 C 0.44478(8) 1.04705(19) 0.29078(19) 0.0221(4) Uani 1 1 d . . . H5 H 0.4705 1.0631 0.3746 0.027 Uiso 1 1 calc R . . C6 C 0.42735(8) 0.92473(18) 0.25057(17) 0.0169(4) Uani 1 1 d . . . C7 C 0.32380(8) 0.95242(18) -0.07216(17) 0.0171(4) Uani 1 1 d . . . O1 O 0.30618(6) 1.03016(13) -0.16054(13) 0.0238(3) Uani 1 1 d . . . O2 O 0.30815(6) 0.83683(13) -0.07366(13) 0.0197(3) Uani 1 1 d . . . C8 C 0.44972(8) 0.80495(19) 0.32603(19) 0.0198(4) Uani 1 1 d . . . O3 O 0.48907(6) 0.81329(15) 0.42872(14) 0.0281(3) Uani 1 1 d . . . O4 O 0.42579(6) 0.70181(13) 0.27448(14) 0.0220(3) Uani 1 1 d . . . N1L N 0.32339(7) 0.54362(15) 0.05805(15) 0.0172(3) Uani 1 1 d . . . C2L C 0.33034(8) 0.45792(18) 0.15335(18) 0.0191(4) Uani 1 1 d . . . H2L H 0.3550 0.4779 0.2372 0.023 Uiso 1 1 calc R . . C3L C 0.30308(8) 0.34215(18) 0.13437(18) 0.0180(4) Uani 1 1 d . . . H3L H 0.3097 0.2840 0.2041 0.022 Uiso 1 1 calc R . . C4L C 0.26585(7) 0.31081(17) 0.01259(17) 0.0154(3) Uani 1 1 d . . . C5L C 0.25933(8) 0.39922(17) -0.08547(18) 0.0178(4) Uani 1 1 d . . . H5L H 0.2347 0.3822 -0.1702 0.021 Uiso 1 1 calc R . . C6L C 0.28870(8) 0.51182(18) -0.05920(18) 0.0184(4) Uani 1 1 d . . . H6L H 0.2841 0.5700 -0.1281 0.022 Uiso 1 1 calc R . . O1R O 0.5000 0.5040(3) 0.2500 0.0479(7) Uani 1 2 d S . . O1P O 0.57068(10) 0.4285(2) 0.4935(2) 0.0568(6) Uani 1 1 d D . . H1PA H 0.5422(10) 0.427(4) 0.425(2) 0.085 Uiso 1 1 d D . . H1PB H 0.5573(14) 0.415(4) 0.553(2) 0.085 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 Co 0.01634(14) 0.01189(14) 0.01617(14) -0.00061(9) 0.00359(10) -0.00261(9) O1V 0.0203(7) 0.0185(7) 0.0258(7) -0.0068(6) 0.0091(6) -0.0051(5) O1W 0.0243(7) 0.0241(7) 0.0297(8) -0.0045(6) 0.0115(6) -0.0042(6) N1 0.0141(7) 0.0154(7) 0.0163(7) -0.0010(6) 0.0040(6) -0.0009(6) C2 0.0156(8) 0.0150(8) 0.0182(9) 0.0004(7) 0.0058(7) -0.0010(7) C3 0.0190(9) 0.0142(9) 0.0276(10) 0.0002(7) 0.0076(8) 0.0003(7) C4 0.0226(10) 0.0156(9) 0.0345(11) -0.0066(8) 0.0066(9) -0.0030(8) C5 0.0171(9) 0.0227(10) 0.0229(10) -0.0077(8) 0.0015(8) -0.0026(7) C6 0.0148(8) 0.0186(9) 0.0167(9) -0.0019(7) 0.0045(7) 0.0000(7) C7 0.0161(8) 0.0192(9) 0.0161(8) -0.0004(7) 0.0053(7) 0.0013(7) O1 0.0274(7) 0.0210(7) 0.0194(7) 0.0048(5) 0.0026(6) 0.0018(6) O2 0.0199(7) 0.0171(7) 0.0184(7) -0.0001(5) 0.0011(5) -0.0036(5) C8 0.0187(9) 0.0226(9) 0.0185(9) 0.0010(7) 0.0068(7) 0.0036(7) O3 0.0247(7) 0.0310(8) 0.0207(7) -0.0034(6) -0.0035(6) 0.0069(6) O4 0.0223(7) 0.0179(7) 0.0225(7) 0.0028(5) 0.0026(6) -0.0007(5) N1L 0.0200(8) 0.0133(7) 0.0191(8) -0.0010(6) 0.0074(6) -0.0015(6) C2L 0.0215(9) 0.0172(9) 0.0170(9) -0.0018(7) 0.0043(7) -0.0023(7) C3L 0.0218(9) 0.0155(9) 0.0163(9) 0.0007(7) 0.0057(7) -0.0012(7) C4L 0.0164(8) 0.0133(8) 0.0180(9) -0.0019(7) 0.0077(7) -0.0004(7) C5L 0.0218(9) 0.0149(9) 0.0160(8) -0.0014(7) 0.0053(7) -0.0019(7) C6L 0.0236(9) 0.0142(8) 0.0177(9) 0.0018(7) 0.0073(7) -0.0004(7) O1R 0.0488(16) 0.0344(14) 0.0613(18) 0.000 0.0192(14) 0.000 O1P 0.0735(15) 0.0364(11) 0.0734(15) 0.0178(11) 0.0416(12) -0.0009(10) _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 Co N1 2.0223(15) . y Co N1L 2.0858(16) . y Co O1V 2.0968(14) . y Co O1W 2.0984(15) . y Co O2 2.1885(13) . y Co O4 2.1746(14) . y N1 C2 1.333(2) . ? N1 C6 1.335(2) . ? C2 C3 1.392(3) . ? C2 C7 1.518(3) . ? C3 C4 1.387(3) . ? C4 C5 1.392(3) . ? C5 C6 1.388(3) . ? C6 C8 1.514(3) . ? C7 O1 1.235(2) . ? C7 O2 1.280(2) . ? C8 O3 1.236(2) . ? C8 O4 1.282(2) . ? N1L C6L 1.339(2) . ? N1L C2L 1.348(2) . ? C2L C3L 1.383(3) . ? C3L C4L 1.397(3) . ? C4L C5L 1.390(3) . ? C4L C4L 1.489(3) 7 ? C5L C6L 1.380(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 N1 Co N1L 176.08(6) . . y N1 Co O1V 91.68(6) . . y N1L Co O1V 84.51(6) . . y N1 Co O1W 94.02(6) . . y N1L Co O1W 89.78(6) . . y O1V Co O1W 174.23(6) . . y N1 Co O4 76.22(6) . . y N1L Co O4 102.73(6) . . y O1V Co O4 89.05(6) . . y O1W Co O4 91.49(6) . . y N1 Co O2 76.66(6) . . y N1L Co O2 104.51(6) . . y O1V Co O2 94.40(6) . . y O1W Co O2 87.74(6) . . y O4 Co O2 152.74(5) . . y C2 N1 C6 121.42(16) . . ? C2 N1 Co 119.11(12) . . y C6 N1 Co 119.32(13) . . y N1 C2 C3 120.65(17) . . ? N1 C2 C7 113.80(16) . . ? C3 C2 C7 125.53(17) . . ? C4 C3 C2 118.25(18) . . ? C3 C4 C5 120.51(18) . . ? C6 C5 C4 117.58(18) . . ? N1 C6 C5 121.40(17) . . ? N1 C6 C8 113.15(16) . . ? C5 C6 C8 125.42(17) . . ? O1 C7 O2 126.27(17) . . ? O1 C7 C2 118.14(17) . . ? O2 C7 C2 115.59(16) . . ? C7 O2 Co 114.28(11) . . y O3 C8 O4 125.71(19) . . ? O3 C8 C6 118.85(18) . . ? O4 C8 C6 115.43(16) . . ? C8 O4 Co 115.11(12) . . y C6L N1L C2L 116.94(16) . . ? C6L N1L Co 120.51(12) . . y C2L N1L Co 122.27(12) . . y N1L C2L C3L 122.88(17) . . ? C2L C3L C4L 119.92(17) . . ? C5L C4L C3L 116.82(16) . . ? C5L C4L C4L 120.9(2) . 7 ? C3L C4L C4L 122.3(2) . 7 ? C6L C5L C4L 119.74(17) . . ? N1L C6L C5L 123.66(17) . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.55 _refine_diff_density_min -0.38 _refine_diff_density_rms 0.07 #===END of CIF # Attachment 'CIF_5_BPCOPC.CIF' data_BPCOPC_Complex_5 _database_code_depnum_ccdc_archive 'CCDC 742527' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Co(II) dipicolinate 4,4-bipyridyl complex tris hydrated ; _chemical_name_common '[dipicolinate Co(II) 4,4-bipy)] hydrated' _chemical_melting_point ? _chemical_formula_moiety 'C17 H11 Co(II) N3 O4, 3(H2 O)' _chemical_formula_sum 'C17 H17 Co N3 O7' _chemical_formula_weight 434.27 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' 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 P2(1)/n 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 11.3573(7) _cell_length_b 10.2450(7) _cell_length_c 15.6754(13) _cell_angle_alpha 90.00 _cell_angle_beta 99.498(2) _cell_angle_gamma 90.00 _cell_volume 1798.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 33012 _cell_measurement_theta_min 2.9 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 1.001 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.835 _exptl_absorpt_correction_T_max 0.886 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995)' _exptl_special_details ; oxygen atom of a water molecule split in 3 sites with 25%, 25% and 50% occupancies ; _diffrn_ambient_temperature 120(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 KappaCCD area detector' _diffrn_measurement_method 'phi and omega scans to fill Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% 0 _diffrn_reflns_number 25068 _diffrn_reflns_av_R_equivalents 0.132 _diffrn_reflns_av_sigmaI/netI 0.114 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4054 _reflns_number_gt 2425 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1999); DENZO (Otwinowski and Minor, 1997)' _computing_cell_refinement 'COLLECT; DENZO' _computing_data_reduction 'COLLECT; DENZO; SORTAV' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL/PC version 5.03 (Sheldrick, 2008)' _computing_publication_material 'SHELXL97; PLATON (Spek, 2003)' _refine_special_details ; ; _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^)+(0.0204P)^2^+15.7300P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary 'difference Fourier method' _atom_sites_solution_hydrogens 'geometrically placed, H2O not located' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0019(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4054 _refine_ls_number_parameters 259 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.148 _refine_ls_R_factor_gt 0.0834 _refine_ls_wR_factor_ref 0.204 _refine_ls_wR_factor_gt 0.181 _refine_ls_goodness_of_fit_ref 1.18 _refine_ls_restrained_S_all 1.18 _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 Co Co 1.25383(8) 0.75483(10) 0.69027(6) 0.0179(3) Uani 1 1 d . . . N1 N 1.2140(5) 0.6416(5) 0.5796(4) 0.0178(12) Uani 1 1 d . . . C2 C 1.1939(6) 0.5123(7) 0.5850(5) 0.0210(15) Uani 1 1 d . . . C3 C 1.1537(7) 0.4376(7) 0.5126(4) 0.0261(16) Uani 1 1 d . . . H3 H 1.1387 0.3469 0.5173 0.031 Uiso 1 1 calc R . . C4 C 1.1360(8) 0.4999(8) 0.4323(5) 0.0324(18) Uani 1 1 d . . . H4 H 1.1068 0.4518 0.3814 0.039 Uiso 1 1 calc R . . C5 C 1.1609(7) 0.6311(7) 0.4268(5) 0.0279(17) Uani 1 1 d . . . H5 H 1.1516 0.6737 0.3722 0.034 Uiso 1 1 calc R . . C6 C 1.1997(6) 0.6995(7) 0.5024(5) 0.0212(15) Uani 1 1 d . . . C7 C 1.2189(6) 0.4660(7) 0.6785(4) 0.0182(15) Uani 1 1 d . . . O1 O 1.2080(4) 0.3454(4) 0.6918(3) 0.0199(11) Uani 1 1 d . . . O2 O 1.2498(4) 0.5517(5) 0.7352(3) 0.0206(11) Uani 1 1 d . . . C8 C 1.2314(6) 0.8432(7) 0.5090(5) 0.0222(16) Uani 1 1 d . . . O3 O 1.2466(5) 0.9033(5) 0.4430(3) 0.0306(12) Uani 1 1 d . . . O4 O 1.2420(4) 0.8908(5) 0.5857(3) 0.0213(11) Uani 1 1 d . . . N1L N 1.0678(5) 0.7708(5) 0.6985(3) 0.0204(13) Uani 1 1 d . . . C2L C 0.9885(6) 0.8259(6) 0.6366(5) 0.0220(15) Uani 1 1 d . . . H2L H 1.0172 0.8670 0.5897 0.026 Uiso 1 1 calc R . . C3L C 0.8675(6) 0.8262(6) 0.6371(4) 0.0198(15) Uani 1 1 d . . . H3L H 0.8150 0.8667 0.5912 0.024 Uiso 1 1 calc R . . C4L C 0.8219(5) 0.7672(6) 0.7049(4) 0.0134(13) Uani 1 1 d . . . C5L C 0.9064(6) 0.7155(7) 0.7728(4) 0.0209(16) Uani 1 1 d . . . H5L H 0.8804 0.6779 0.8219 0.025 Uiso 1 1 calc R . . C6L C 1.0262(6) 0.7195(7) 0.7681(4) 0.0221(16) Uani 1 1 d . . . H6L H 1.0818 0.6855 0.8148 0.027 Uiso 1 1 calc R . . C7L C 0.6936(5) 0.7607(6) 0.7035(4) 0.0149(13) Uani 1 1 d . . . C8L C 0.6180(6) 0.8638(7) 0.6729(5) 0.0226(16) Uani 1 1 d . . . H8L H 0.6498 0.9418 0.6531 0.027 Uiso 1 1 calc R . . C9L C 0.4976(6) 0.8520(7) 0.6716(5) 0.0276(17) Uani 1 1 d . . . H9L H 0.4485 0.9241 0.6509 0.033 Uiso 1 1 calc R . . N10L N 0.4450(5) 0.7473(5) 0.6972(3) 0.0181(11) Uani 1 1 d . . . C11L C 0.5161(6) 0.6480(7) 0.7302(5) 0.0248(16) Uani 1 1 d . . . H11 H 0.4808 0.5729 0.7511 0.030 Uiso 1 1 calc R . . C12L C 0.6381(6) 0.6519(7) 0.7345(4) 0.0206(15) Uani 1 1 d . . . H12 H 0.6853 0.5802 0.7587 0.025 Uiso 1 1 calc R . . O1W O 1.1162(6) 0.1315(6) 0.5737(4) 0.0516(18) Uani 1 1 d . . . O1R O 1.0681(7) 0.5920(8) 0.9629(4) 0.073(2) Uani 1 1 d . . . O1S O 0.9813(15) 0.1371(15) 0.0130(11) 0.063(5) Uani 0.50 1 d P . . O1T O 1.0000 0.0000 0.0000 0.067(6) Uiso 0.50 2 d SP . . O1U O 0.988(2) 0.082(3) 0.0061(16) 0.026(6) Uiso 0.25 1 d P . . 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 Co 0.0183(5) 0.0160(5) 0.0191(5) -0.0007(4) 0.0022(3) -0.0006(4) N1 0.017(3) 0.016(3) 0.020(3) 0.002(2) 0.003(2) 0.002(2) C2 0.023(4) 0.015(3) 0.024(4) 0.002(3) 0.003(3) 0.003(3) C3 0.036(4) 0.018(4) 0.023(4) 0.001(3) 0.000(3) -0.003(3) C4 0.050(5) 0.025(4) 0.021(4) -0.003(3) 0.002(3) -0.002(4) C5 0.045(5) 0.024(4) 0.015(4) 0.006(3) 0.002(3) 0.005(3) C6 0.023(4) 0.017(3) 0.025(4) 0.002(3) 0.006(3) 0.001(3) C7 0.012(3) 0.018(4) 0.025(4) 0.002(3) 0.002(3) 0.001(3) O1 0.024(3) 0.014(2) 0.020(3) 0.0022(19) 0.001(2) -0.0017(19) O2 0.023(3) 0.020(3) 0.018(3) -0.001(2) 0.0026(19) 0.002(2) C8 0.017(4) 0.024(4) 0.025(4) 0.002(3) 0.004(3) 0.004(3) O3 0.045(3) 0.020(3) 0.028(3) 0.005(2) 0.010(2) -0.002(2) O4 0.023(3) 0.019(3) 0.022(3) -0.001(2) 0.003(2) -0.003(2) N1L 0.026(3) 0.019(3) 0.016(3) -0.002(2) 0.003(2) 0.007(2) C2L 0.029(4) 0.013(3) 0.024(4) 0.004(3) 0.003(3) -0.003(3) C3L 0.022(4) 0.012(3) 0.024(4) 0.002(3) -0.002(3) 0.001(3) C4L 0.020(3) 0.004(3) 0.017(3) -0.002(3) 0.005(2) 0.000(2) C5L 0.019(4) 0.023(4) 0.020(4) 0.002(3) 0.004(3) -0.001(3) C6L 0.024(4) 0.022(4) 0.021(4) -0.001(3) 0.003(3) 0.000(3) C7L 0.022(3) 0.010(3) 0.011(3) -0.004(3) -0.002(2) 0.000(3) C8L 0.017(4) 0.019(4) 0.032(4) 0.000(3) 0.007(3) -0.002(3) C9L 0.023(4) 0.019(4) 0.039(5) -0.001(3) 0.001(3) 0.001(3) N10L 0.031(3) 0.006(2) 0.017(3) -0.001(2) 0.003(2) -0.006(3) C11L 0.023(4) 0.026(4) 0.025(4) 0.003(3) 0.006(3) -0.007(3) C12L 0.018(4) 0.022(4) 0.021(4) 0.003(3) 0.002(3) 0.000(3) O1W 0.086(5) 0.031(4) 0.032(3) -0.003(3) -0.007(3) 0.002(3) O1R 0.100(6) 0.076(5) 0.042(4) -0.005(4) 0.007(4) 0.040(5) O1S 0.084(12) 0.025(8) 0.075(11) -0.030(8) 0.004(8) 0.007(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 Co O1 2.050(5) 2_756 y Co N1 2.074(6) . y Co O4 2.138(5) . y Co N1L 2.145(6) . y Co N10L 2.157(5) 1_655 y Co O2 2.200(5) . y N1 C6 1.333(9) . ? N1 C2 1.349(9) . ? C2 C3 1.383(10) . ? C2 C7 1.523(9) . ? C3 C4 1.395(10) . ? C4 C5 1.380(11) . ? C5 C6 1.385(10) . ? C6 C8 1.515(10) . ? C7 O2 1.258(8) . ? C7 O1 1.262(8) . ? C8 O3 1.240(8) . ? C8 O4 1.285(8) . ? N1L C2L 1.336(8) . ? N1L C6L 1.362(9) . ? C2L C3L 1.375(10) . ? C3L C4L 1.395(9) . ? C4L C5L 1.414(9) . ? C4L C7L 1.455(9) . ? C5L C6L 1.376(10) . ? C7L C8L 1.396(9) . ? C7L C12L 1.406(9) . ? C8L C9L 1.369(10) . ? C9L N10L 1.322(9) . ? N10L C11L 1.348(9) . ? C11L C12L 1.377(10) . ? 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 Co N1 172.8(2) 2_756 . y O1 Co O4 111.93(19) 2_756 . y N1 Co O4 75.3(2) . . y O1 Co N1L 88.56(19) 2_756 . y N1 Co N1L 90.7(2) . . y O4 Co N1L 93.39(19) . . y O1 Co N10L 84.79(19) 2_756 1_655 y N1 Co N10L 95.8(2) . 1_655 y O4 Co N10L 89.83(19) . 1_655 y O1 Co O2 98.73(18) 2_756 . y N1 Co O2 74.09(19) . . y O4 Co O2 149.30(18) . . y N1L Co O2 88.8(2) . . y N10L Co O2 91.38(19) 1_655 . y C6 N1 C2 119.8(6) . . ? C6 N1 Co 119.2(5) . . y C2 N1 Co 120.8(5) . . y N1 C2 C3 121.9(6) . . ? N1 C2 C7 111.1(6) . . ? C3 C2 C7 127.0(6) . . ? C2 C3 C4 117.7(7) . . ? C5 C4 C3 120.2(7) . . ? C4 C5 C6 118.6(7) . . ? N1 C6 C5 121.7(6) . . ? N1 C6 C8 112.2(6) . . ? C5 C6 C8 126.0(7) . . ? O2 C7 O1 126.2(6) . . ? O2 C7 C2 116.7(6) . . ? O1 C7 C2 117.1(6) . . ? C7 O1 Co 125.4(4) . 2_746 y C7 O2 Co 116.9(4) . . y O3 C8 O4 126.0(7) . . ? O3 C8 C6 119.3(7) . . ? O4 C8 C6 114.6(6) . . ? C8 O4 Co 117.0(4) . . y C2L N1L C6L 117.6(6) . . ? C2L N1L Co 122.7(5) . . y C6L N1L Co 119.6(4) . . y N1L C2L C3L 123.4(7) . . ? C2L C3L C4L 120.0(6) . . ? C3L C4L C5L 116.4(6) . . ? C3L C4L C7L 120.4(6) . . ? C5L C4L C7L 123.2(6) . . ? C6L C5L C4L 120.2(6) . . ? N1L C6L C5L 122.1(6) . . ? C8L C7L C12L 115.7(6) . . ? C8L C7L C4L 121.9(6) . . ? C12L C7L C4L 122.4(6) . . ? C9L C8L C7L 119.6(7) . . ? N10L C9L C8L 124.6(7) . . ? C9L N10L C11L 117.2(6) . . ? C9L N10L Co 117.2(5) . 1_455 y C11L N10L Co 125.5(5) . 1_455 y N10L C11L C12L 122.1(7) . . ? C11L C12L C7L 120.7(6) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.808 _refine_diff_density_min -0.600 _refine_diff_density_rms 0.130 # Attachment 'CIF_6_CO44PC.CIF' data_CO44PC_Complex_6 _database_code_depnum_ccdc_archive 'CCDC 742528' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Co(II)(dipic)(4,4-bipy)]2(H2O)0.5(dmso)' _chemical_melting_point ? _chemical_formula_moiety 'C17 H11 Co(II) N3 O4, H4 O2, C H3 O0.5 S0.5' _chemical_formula_sum 'C18 H18 Co N3 O6.50 S0.50' _chemical_formula_weight 455.31 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.445(5) _cell_length_b 16.353(7) _cell_length_c 10.250(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.065(5) _cell_angle_gamma 90.00 _cell_volume 1918.4(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 942 _cell_measurement_theta_min 2.95 _cell_measurement_theta_max 26.45 _exptl_crystal_description column _exptl_crystal_colour orange _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 908 _exptl_absorpt_coefficient_mu 0.992 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; 'Twinned crystal, appears as orthorombic; merohedral twin, twin law (1 0 0, 0 -1 0, 0 0 -1); refines to 0.53:0.47 for two components, left as 50:50 twin, consistent with good Rint for mmm symmetry, 7.7% compared to 6.9% for 2/m; partially disordered dmso, treated as follows: S and one C are on a common site related by symmetry, 50% in total, divided as 30% and 20%' ; _diffrn_ambient_temperature 150(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 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time 20 _diffrn_standards_decay_% '+/- 2% (not corrected)' _diffrn_reflns_number 11726 _diffrn_reflns_av_R_equivalents 0.069 _diffrn_reflns_av_sigmaI/netI 0.062 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 28.44 _reflns_number_total 4488 _reflns_number_gt 3248 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'SMART version 5.054 (Bruker, 1998)' _computing_cell_refinement SAINT _computing_data_reduction 'SAINT version 6.02A (Bruker, 2001)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL/PC version 5.03 (Sheldrick, 2008)' _computing_publication_material 'SHELXL97; PLATON (Spek, 2003)' _refine_special_details ; ; _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^)+(0.0858P)^2^+2.9158P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary 'difference Fourier method' _atom_sites_solution_hydrogens 'geometrically placed' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4333 _refine_ls_number_parameters 251 _refine_ls_number_restraints 47 _refine_ls_R_factor_all 0.0879 _refine_ls_R_factor_gt 0.0611 _refine_ls_wR_factor_ref 0.161 _refine_ls_wR_factor_gt 0.147 _refine_ls_goodness_of_fit_ref 1.03 _refine_ls_restrained_S_all 1.08 _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 Co Co 0.66486(6) 0.31124(4) 0.75442(8) 0.01699(18) Uani 1 1 d . . . N1 N 0.6589(5) 0.4139(3) 0.6334(4) 0.0159(9) Uani 1 1 d . . . C6 C 0.6569(6) 0.4062(3) 0.5031(5) 0.0205(11) Uani 1 1 d . . . C5 C 0.6495(6) 0.4728(4) 0.4232(5) 0.0264(13) Uani 1 1 d . . . H3 H 0.6479 0.4664 0.3331 0.032 Uiso 1 1 calc R . . C4 C 0.6444(6) 0.5510(4) 0.4786(6) 0.0302(15) Uani 1 1 d . . . H4 H 0.6386 0.5973 0.4264 0.036 Uiso 1 1 calc R . . C3 C 0.6482(6) 0.5574(3) 0.6124(7) 0.0254(14) Uani 1 1 d . . . H5 H 0.6457 0.6087 0.6514 0.030 Uiso 1 1 calc R . . C2 C 0.6557(7) 0.4877(3) 0.6897(6) 0.0219(12) Uani 1 1 d . . . C8 C 0.6608(6) 0.4853(3) 0.8370(5) 0.0224(12) Uani 1 1 d . . . O3 O 0.6628(6) 0.5497(3) 0.8974(4) 0.0394(12) Uani 1 1 d . . . O4 O 0.6676(4) 0.4123(2) 0.8844(4) 0.0213(8) Uani 1 1 d . . . C7 C 0.6622(5) 0.3168(3) 0.4606(5) 0.0172(10) Uani 1 1 d . . . O1 O 0.6644(4) 0.3031(2) 0.3396(3) 0.0185(7) Uani 1 1 d . . . O2 O 0.6621(4) 0.2641(2) 0.5496(4) 0.0207(7) Uani 1 1 d . . . N1L N -0.1464(4) 0.3030(2) 0.7560(5) 0.0272(10) Uiso 1 1 d D . . C2L C -0.0847(9) 0.3302(6) 0.8566(10) 0.029(3) Uiso 0.50 1 d PD A 1 H2L H -0.1255 0.3514 0.9275 0.035 Uiso 0.50 1 calc PR A 1 C2L' C -0.0818(9) 0.3677(6) 0.8068(10) 0.030(3) Uiso 0.50 1 d PD A 2 H2L' H -0.1214 0.4132 0.8388 0.037 Uiso 0.50 1 calc PR A 2 C3L C 0.0361(8) 0.3294(7) 0.8636(10) 0.028(3) Uiso 0.50 1 d PD A 1 H3L H 0.0734 0.3506 0.9368 0.033 Uiso 0.50 1 calc PR A 1 C3L' C 0.0406(8) 0.3673(6) 0.8118(11) 0.023(3) Uiso 0.50 1 d PD A 2 H3L' H 0.0814 0.4116 0.8459 0.028 Uiso 0.50 1 calc PR A 2 C4L C 0.1011(5) 0.2977(3) 0.7637(5) 0.0186(12) Uani 1 1 d D . . C5L C 0.0377(7) 0.2628(7) 0.6580(10) 0.023(3) Uiso 0.50 1 d PD A 1 H5L H 0.0775 0.2384 0.5892 0.027 Uiso 0.50 1 calc PR A 1 C5L' C 0.0339(7) 0.2338(6) 0.7174(11) 0.021(3) Uiso 0.50 1 d PD A 2 H5L' H 0.0701 0.1874 0.6840 0.026 Uiso 0.50 1 calc PR A 2 C6L C -0.0847(8) 0.2652(7) 0.6572(10) 0.022(2) Uiso 0.50 1 d PD A 1 H6L H -0.1252 0.2407 0.5889 0.026 Uiso 0.50 1 calc PR A 1 C6L' C -0.0868(8) 0.2381(6) 0.7204(11) 0.023(3) Uiso 0.50 1 d PD A 2 H6L' H -0.1287 0.1919 0.6955 0.028 Uiso 0.50 1 calc PR A 2 C7L C 0.2305(4) 0.2972(3) 0.7630(8) 0.0171(12) Uani 1 1 d . A . C8L C 0.2919(5) 0.3531(4) 0.8412(6) 0.0240(14) Uani 1 1 d . . . H8L H 0.2514 0.3890 0.8951 0.029 Uiso 1 1 calc R A . C9L C 0.4131(5) 0.3548(4) 0.8378(5) 0.0215(12) Uani 1 1 d . A . H9L H 0.4521 0.3926 0.8898 0.026 Uiso 1 1 calc R . . N10L N 0.4763(3) 0.3045(2) 0.7631(6) 0.0129(9) Uani 1 1 d . . . C11L C 0.4178(5) 0.2491(4) 0.6903(6) 0.0213(12) Uani 1 1 d . A . H11L H 0.4606 0.2124 0.6402 0.026 Uiso 1 1 calc R . . C12L C 0.2965(5) 0.2444(4) 0.6870(6) 0.0228(13) Uani 1 1 d . . . H12L H 0.2598 0.2061 0.6339 0.027 Uiso 1 1 calc R A . O1W O 0.7439(4) 0.4210(3) 1.1386(4) 0.0367(11) Uani 1 1 d . . . O2W O 0.9839(5) 0.0523(3) 0.6018(6) 0.0545(15) Uani 1 1 d . . . S1 S 0.0298(5) 0.4987(4) 0.5816(5) 0.0583(15) Uiso 0.30 1 d PD . 1 S1' S -0.0565(7) 0.5325(4) 0.5355(8) 0.063(3) Uiso 0.20 1 d PD . 2 O1S O -0.0788(10) 0.4894(7) 0.6695(11) 0.057(3) Uiso 0.50 1 d PD . . C1S C 0.0531(13) 0.6070(8) 0.5609(19) 0.068(5) Uiso 0.50 1 d PD . . C2S C 0.0298(5) 0.4987(4) 0.5816(5) 0.0583(15) Uiso 0.30 1 d P . 1 C2S' C -0.0565(7) 0.5325(4) 0.5355(8) 0.063(3) Uiso 0.20 1 d P . 2 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 Co 0.0117(3) 0.0198(3) 0.0194(3) 0.0027(3) -0.0003(5) -0.0005(3) N1 0.013(2) 0.020(2) 0.015(2) -0.0040(17) -0.001(2) 0.002(2) C6 0.014(3) 0.024(3) 0.023(3) 0.001(2) -0.002(3) -0.001(3) C5 0.038(4) 0.026(3) 0.016(3) -0.002(2) 0.001(3) 0.000(3) C4 0.035(4) 0.025(3) 0.031(3) 0.000(2) 0.005(3) 0.006(3) C3 0.032(4) 0.010(3) 0.034(3) 0.001(2) 0.000(3) -0.003(3) C2 0.017(3) 0.020(3) 0.028(3) -0.002(2) 0.002(3) -0.001(3) C8 0.020(3) 0.026(3) 0.022(3) -0.002(2) 0.001(3) -0.003(3) O3 0.062(3) 0.029(2) 0.027(2) -0.0065(19) 0.003(3) 0.003(3) O4 0.022(2) 0.021(2) 0.0207(19) -0.0036(16) -0.002(2) -0.0035(19) C7 0.006(2) 0.025(3) 0.020(2) 0.002(2) 0.001(2) 0.002(2) O1 0.0155(17) 0.0224(18) 0.0175(16) -0.0044(14) 0.0008(18) -0.0019(18) O2 0.0215(18) 0.0172(18) 0.0235(18) 0.0016(15) 0.004(2) 0.0038(18) C4L 0.021(2) 0.025(3) 0.009(3) 0.002(2) 0.003(3) 0.0019(19) C7L 0.009(2) 0.021(3) 0.021(3) 0.002(3) -0.005(3) 0.0003(17) C8L 0.016(3) 0.030(3) 0.026(3) -0.012(3) 0.006(2) -0.001(2) C9L 0.013(3) 0.035(3) 0.017(3) -0.007(3) 0.001(2) -0.007(2) N10L 0.0087(17) 0.0204(19) 0.010(2) 0.0047(19) -0.002(2) -0.0004(14) C11L 0.016(3) 0.018(3) 0.031(3) -0.002(2) 0.002(2) 0.000(2) C12L 0.018(3) 0.019(3) 0.032(3) -0.005(2) 0.001(2) -0.003(2) O1W 0.052(3) 0.038(3) 0.020(2) 0.001(2) 0.000(2) -0.006(2) O2W 0.051(4) 0.051(3) 0.062(4) 0.012(3) 0.002(3) 0.003(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 Co O1 2.063(3) 4_566 y Co N1 2.088(4) . y Co O4 2.123(4) . y Co N10L 2.162(4) . y Co N1L 2.164(5) 1_655 y Co O2 2.236(4) . y N1 C2 1.339(7) . ? N1 C6 1.341(7) . ? C6 C5 1.366(8) . ? C6 C7 1.526(7) . ? C5 C4 1.399(8) . ? C4 C3 1.376(9) . ? C3 C2 1.391(8) . ? C2 C8 1.511(7) . ? C8 O3 1.223(7) . ? C8 O4 1.291(7) . ? C7 O2 1.255(6) . ? C7 O1 1.261(6) . ? N1L C6L' 1.313(8) . ? N1L C2L 1.326(8) . ? N1L C6L 1.382(8) . ? N1L C2L' 1.392(8) . ? C2L C3L 1.385(8) . ? C2L' C3L' 1.401(8) . ? C3L C4L 1.368(7) . ? C3L' C4L 1.419(7) . ? C4L C5L' 1.382(7) . ? C4L C5L 1.423(7) . ? C4L C7L 1.482(6) . ? C5L C6L 1.401(8) . ? C5L' C6L' 1.384(8) . ? C7L C12L 1.387(8) . ? C7L C8L 1.404(8) . ? C8L C9L 1.388(8) . ? C9L N10L 1.337(7) . ? N10L C11L 1.351(7) . ? C11L C12L 1.390(8) . ? S1 O1S 1.544(13) . ? S1 C1S 1.803(12) . ? S1 C2S 1.807(10) 3_566 ? S1' O1S 1.566(13) . ? S1' C1S 1.767(12) . ? S1' C2S' 1.826(11) 3_566 ? 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 Co N1 168.38(15) 4_566 . y O1 Co O4 116.10(15) 4_566 . y N1 Co O4 75.39(13) . . y O1 Co N10L 86.18(17) 4_566 . y N1 Co N10L 91.9(2) . . y O4 Co N10L 91.59(19) . . y O1 Co N1L 86.77(17) 4_566 1_655 y N1 Co N1L 95.0(2) . 1_655 y O4 Co N1L 91.69(18) . 1_655 y N10L Co N1L 172.95(15) . 1_655 y O1 Co O2 94.86(13) 4_566 . y N1 Co O2 73.67(14) . . y O4 Co O2 149.04(14) . . y N10L Co O2 90.45(19) . . y N1L Co O2 89.94(18) 1_655 . y C2 N1 C6 120.9(5) . . ? C2 N1 Co 118.0(4) . . y C6 N1 Co 121.1(4) . . y N1 C6 C5 121.5(5) . . ? N1 C6 C7 111.9(4) . . ? C5 C6 C7 126.5(5) . . ? C6 C5 C4 119.2(5) . . ? C3 C4 C5 118.2(6) . . ? C4 C3 C2 120.4(6) . . ? N1 C2 C3 119.7(5) . . ? N1 C2 C8 113.9(5) . . ? C3 C2 C8 126.4(6) . . ? O3 C8 O4 127.3(5) . . ? O3 C8 C2 118.9(5) . . ? O4 C8 C2 113.8(5) . . ? C8 O4 Co 118.8(3) . . ? O2 C7 O1 126.4(5) . . ? O2 C7 C6 116.7(4) . . ? O1 C7 C6 116.9(4) . . ? C7 O1 Co 125.3(3) . 4_565 y C7 O2 Co 116.5(3) . . y C6L' N1L C2L 102.2(7) . . ? C2L N1L C6L 116.6(7) . . ? C6L' N1L C2L' 116.2(7) . . ? C6L N1L C2L' 110.0(7) . . ? C6L' N1L Co 124.5(5) . 1_455 y C2L N1L Co 121.0(6) . 1_455 y C6L N1L Co 122.2(5) . 1_455 y C2L' N1L Co 119.1(5) . 1_455 y N1L C2L C3L 124.6(10) . . ? N1L C2L' C3L' 122.7(9) . . ? C4L C3L C2L 120.6(10) . . ? C2L' C3L' C4L 118.7(9) . . ? C5L' C4L C3L' 117.0(7) . . ? C3L C4L C5L 116.4(7) . . ? C3L' C4L C5L 109.7(7) . . ? C3L C4L C7L 123.4(7) . . ? C5L' C4L C7L 123.3(6) . . ? C3L' C4L C7L 119.6(6) . . ? C5L C4L C7L 120.2(6) . . ? C6L C5L C4L 120.1(9) . . ? C4L C5L' C6L' 120.6(9) . . ? N1L C6L C5L 121.3(9) . . ? N1L C6L' C5L' 124.5(9) . . ? C12L C7L C8L 117.0(5) . . ? C12L C7L C4L 123.5(5) . . ? C8L C7L C4L 119.5(6) . . ? C9L C8L C7L 119.9(6) . . ? N10L C9L C8L 122.9(5) . . ? C9L N10L C11L 117.4(4) . . ? C9L N10L Co 122.2(4) . . y C11L N10L Co 120.4(4) . . y N10L C11L C12L 123.1(5) . . ? C7L C12L C11L 119.7(5) . . ? O1S S1 C1S 106.5(8) . . ? O1S S1 C2S 103.8(6) . 3_566 ? C1S S1 C2S 85.6(7) . 3_566 ? O1S S1' C1S 107.3(9) . . ? O1S S1' C2S' 101.7(7) . 3_566 ? _diffrn_measured_fraction_theta_max 0.898 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.869 _refine_diff_density_min -0.679 _refine_diff_density_rms 0.119 #=== END of CIF # Attachment 'CIF_7_NIPYCB.CIF' data_NIPYCB_Complex_7 _database_code_depnum_ccdc_archive 'CCDC 742529' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[1.5(4,4-bipy)Ni(picolinate)].DMSO.MeOH' _chemical_formula_moiety 'C25 H24 N4 Ni O6 S' _chemical_formula_sum 'C25 H24 N4 Ni O6 S' _chemical_formula_weight 567.25 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.5299(5) _cell_length_b 18.6015(11) _cell_length_c 16.0248(10) _cell_angle_alpha 90.00 _cell_angle_beta 94.641(2) _cell_angle_gamma 90.00 _cell_volume 2534.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6106 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 28.5 _exptl_crystal_description column _exptl_crystal_colour 'pale green' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.487 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 0.896 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.760 _exptl_absorpt_correction_T_max 0.875 _exptl_absorpt_process_details 'SADABS (Bruker, 1999b)' _exptl_special_details ; disordered solvent molecules (DMSO and MeOH) treated as follows: S in DMSO split in 2 sites with 10% and 90% occupancy. both carbons, the oxygen and the hydrogens are occupied only 90%. Oxygen in MeOH split in 2 sites with 50% occupancy each, no hydrogens located ; _diffrn_ambient_temperature 150(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 'Bruker SMART CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% 0 _diffrn_reflns_number 23586 _diffrn_reflns_av_R_equivalents 0.028 _diffrn_reflns_av_sigmaI/netI 0.022 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 28.83 _reflns_number_total 6027 _reflns_number_gt 5277 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'SMART version 5.054 (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL/PC version 5.03 (Sheldrick, 2008)' _computing_publication_material SHELXL97 _refine_special_details ; ; _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^+3.2707P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary 'difference Fourier methods' _atom_sites_solution_hydrogens 'placed geometrically' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6027 _refine_ls_number_parameters 347 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0465 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.1047 _refine_ls_wR_factor_gt 0.1023 _refine_ls_goodness_of_fit_ref 1.141 _refine_ls_restrained_S_all 1.148 _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 Ni Ni 0.59760(3) 0.790638(14) 0.073031(17) 0.01423(8) Uani 1 1 d . . . N1 N 0.6052(2) 0.89626(10) 0.08499(11) 0.0170(4) Uani 1 1 d . . . C2 C 0.5280(3) 0.92648(12) 0.14475(15) 0.0203(4) Uani 1 1 d . . . C3 C 0.5406(3) 0.99987(13) 0.15986(16) 0.0282(5) Uani 1 1 d . . . H3 H 0.4857 1.0219 0.2023 0.034 Uiso 1 1 calc R . . C4 C 0.6352(4) 1.03991(13) 0.11132(18) 0.0329(6) Uani 1 1 d . . . H4 H 0.6467 1.0901 0.1209 0.039 Uiso 1 1 calc R . . C5 C 0.7137(3) 1.00727(13) 0.04851(17) 0.0291(5) Uani 1 1 d . . . H5 H 0.7778 1.0345 0.0145 0.035 Uiso 1 1 calc R . . C6 C 0.6955(3) 0.93374(12) 0.03719(14) 0.0198(4) Uani 1 1 d . . . C7 C 0.7742(3) 0.88770(12) -0.02527(14) 0.0211(5) Uani 1 1 d . . . O1 O 0.8516(2) 0.91737(10) -0.07715(12) 0.0341(4) Uani 1 1 d . . . O2 O 0.75309(18) 0.81964(8) -0.01766(10) 0.0185(3) Uani 1 1 d . . . C8 C 0.4311(3) 0.87348(13) 0.19109(14) 0.0208(5) Uani 1 1 d . . . O3 O 0.3527(2) 0.89579(10) 0.24636(13) 0.0358(5) Uani 1 1 d . . . O4 O 0.44130(18) 0.80782(8) 0.16625(10) 0.0184(3) Uani 1 1 d . . . N1L N 0.7879(2) 0.77410(10) 0.16493(12) 0.0178(4) Uani 1 1 d . . . C2L C 0.7617(3) 0.76154(16) 0.24462(16) 0.0312(6) Uani 1 1 d . . . H2L H 0.6564 0.7638 0.2597 0.037 Uiso 1 1 calc R . . C3L C 0.8784(3) 0.74552(16) 0.30630(16) 0.0310(6) Uani 1 1 d . . . H3L H 0.8526 0.7366 0.3619 0.037 Uiso 1 1 calc R . . C4L C 1.0338(3) 0.74251(12) 0.28686(14) 0.0184(4) Uani 1 1 d . . . C5L C 1.0611(3) 0.75442(16) 0.20415(16) 0.0311(6) Uani 1 1 d . . . H5L H 1.1652 0.7523 0.1873 0.037 Uiso 1 1 calc R . . C6L C 0.9365(3) 0.76949(16) 0.14586(16) 0.0291(6) Uani 1 1 d . . . H6L H 0.9584 0.7769 0.0893 0.035 Uiso 1 1 calc R . . N7L N 0.4080(2) 0.79119(10) -0.02162(12) 0.0167(4) Uani 1 1 d . . . C8L C 0.4359(3) 0.76938(13) -0.09874(15) 0.0222(5) Uani 1 1 d . . . H8L H 0.5418 0.7605 -0.1101 0.027 Uiso 1 1 calc R . . C9L C 0.3198(3) 0.75913(13) -0.16252(15) 0.0224(5) Uani 1 1 d . . . H9L H 0.3461 0.7437 -0.2162 0.027 Uiso 1 1 calc R . . C10L C 0.1636(3) 0.77159(11) -0.14765(14) 0.0176(4) Uani 1 1 d . . . C11L C 0.1345(3) 0.79588(13) -0.06845(15) 0.0219(5) Uani 1 1 d . . . H11L H 0.0301 0.8067 -0.0559 0.026 Uiso 1 1 calc R . . C12L C 0.2582(3) 0.80432(12) -0.00780(14) 0.0200(4) Uani 1 1 d . . . H12L H 0.2356 0.8202 0.0463 0.024 Uiso 1 1 calc R . . N13L N 0.5853(2) 0.68044(10) 0.05934(12) 0.0199(4) Uani 1 1 d . . . C14L C 0.6690(3) 0.64598(13) 0.00493(17) 0.0267(5) Uani 1 1 d . . . H14L H 0.7530 0.6709 -0.0177 0.032 Uiso 1 1 calc R . . C15L C 0.6394(3) 0.57554(13) -0.02018(18) 0.0293(6) Uani 1 1 d . . . H15L H 0.7005 0.5536 -0.0602 0.035 Uiso 1 1 calc R . . C16L C 0.5200(3) 0.53744(12) 0.01360(15) 0.0221(5) Uani 1 1 d . . . C17L C 0.4392(3) 0.57227(13) 0.07388(17) 0.0292(6) Uani 1 1 d . . . H17L H 0.3605 0.5475 0.1012 0.035 Uiso 1 1 calc R . . C18L C 0.4741(3) 0.64295(13) 0.09374(17) 0.0279(5) Uani 1 1 d . . . H18L H 0.4157 0.6661 0.1341 0.033 Uiso 1 1 calc R . . S1R S 0.95716(10) 1.04159(5) 0.26106(5) 0.0411(2) Uani 0.90 1 d PD A 1 S1R' S 0.9766(18) 0.9695(8) 0.3015(10) 0.090(4) Uiso 0.10 1 d P A 2 O1R O 0.8865(4) 1.0211(2) 0.34114(19) 0.0810(11) Uani 0.90 1 d P . . C1R C 0.9935(4) 0.95966(18) 0.2092(2) 0.0440(8) Uani 0.90 1 d PD . . H1RA H 0.8933 0.9376 0.1889 0.066 Uiso 0.90 1 calc PR A 1 H1RB H 1.0515 0.9268 0.2483 0.066 Uiso 0.90 1 calc PR A 1 H1RC H 1.0559 0.9693 0.1616 0.066 Uiso 0.90 1 calc PR A 1 C2R C 1.1566(4) 1.0643(2) 0.2877(2) 0.0443(8) Uani 0.90 1 d PD . . H2RA H 1.1621 1.1100 0.3181 0.067 Uiso 0.90 1 calc PR A 1 H2RB H 1.2114 1.0690 0.2365 0.067 Uiso 0.90 1 calc PR A 1 H2RC H 1.2067 1.0265 0.3231 0.067 Uiso 0.90 1 calc PR A 1 C1S C 1.1031(6) 0.8967(2) 0.4589(3) 0.0759(13) Uani 1 1 d D . . O1S O 1.0652(6) 0.8610(3) 0.5293(3) 0.0576(13) Uani 0.50 1 d PD B 2 O1S' O 0.9798(6) 0.8799(3) 0.4119(4) 0.0638(14) Uani 0.50 1 d PD B 1 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 Ni 0.01340(14) 0.01411(14) 0.01481(14) -0.00030(10) -0.00104(10) -0.00018(10) N1 0.0164(9) 0.0169(8) 0.0171(9) 0.0003(7) -0.0014(7) 0.0002(7) C2 0.0201(11) 0.0204(11) 0.0202(11) 0.0000(8) -0.0001(9) 0.0018(8) C3 0.0370(15) 0.0209(11) 0.0272(13) -0.0040(9) 0.0066(11) 0.0045(10) C4 0.0473(17) 0.0156(11) 0.0359(15) -0.0007(10) 0.0045(12) 0.0002(10) C5 0.0363(14) 0.0197(11) 0.0318(14) 0.0049(10) 0.0060(11) -0.0033(10) C6 0.0210(11) 0.0194(10) 0.0187(11) 0.0026(8) -0.0010(9) -0.0003(8) C7 0.0198(11) 0.0234(11) 0.0197(11) 0.0015(9) -0.0002(9) 0.0003(9) O1 0.0415(11) 0.0295(10) 0.0337(11) 0.0062(8) 0.0189(9) -0.0012(8) O2 0.0173(8) 0.0206(8) 0.0174(8) -0.0010(6) 0.0009(6) -0.0007(6) C8 0.0196(11) 0.0235(11) 0.0193(11) 0.0019(9) 0.0013(9) 0.0031(9) O3 0.0424(11) 0.0305(10) 0.0372(11) -0.0018(8) 0.0207(9) 0.0050(8) O4 0.0175(8) 0.0192(8) 0.0185(8) 0.0010(6) 0.0011(6) -0.0013(6) N1L 0.0158(9) 0.0183(9) 0.0189(9) 0.0011(7) -0.0009(7) -0.0010(7) C2L 0.0156(11) 0.0524(17) 0.0255(13) 0.0120(12) 0.0011(10) 0.0022(11) C3L 0.0203(12) 0.0527(17) 0.0198(12) 0.0108(11) 0.0003(10) 0.0036(11) C4L 0.0170(11) 0.0200(10) 0.0176(11) 0.0011(8) -0.0014(8) 0.0006(8) C5L 0.0153(11) 0.0544(17) 0.0234(13) 0.0075(12) 0.0002(9) 0.0012(11) C6L 0.0203(12) 0.0502(16) 0.0167(11) 0.0071(10) 0.0000(9) 0.0010(11) N7L 0.0156(9) 0.0172(8) 0.0168(9) -0.0010(7) -0.0012(7) -0.0003(7) C8L 0.0161(11) 0.0287(12) 0.0212(11) -0.0054(9) -0.0011(9) 0.0030(9) C9L 0.0194(11) 0.0280(12) 0.0195(11) -0.0073(9) 0.0001(9) 0.0021(9) C10L 0.0167(10) 0.0168(10) 0.0186(11) -0.0005(8) -0.0021(8) -0.0002(8) C11L 0.0145(10) 0.0315(12) 0.0197(11) -0.0029(9) 0.0008(8) 0.0016(9) C12L 0.0189(11) 0.0249(11) 0.0160(10) -0.0017(8) 0.0011(8) -0.0007(8) N13L 0.0179(9) 0.0166(9) 0.0245(10) 0.0003(7) -0.0022(8) 0.0004(7) C14L 0.0231(12) 0.0197(11) 0.0384(14) -0.0031(10) 0.0091(10) -0.0034(9) C15L 0.0274(13) 0.0207(12) 0.0414(15) -0.0058(10) 0.0121(11) -0.0017(9) C16L 0.0213(11) 0.0170(11) 0.0276(12) -0.0014(9) 0.0011(9) -0.0011(8) C17L 0.0306(13) 0.0219(12) 0.0370(15) -0.0057(10) 0.0136(11) -0.0075(10) C18L 0.0308(13) 0.0222(12) 0.0317(13) -0.0053(10) 0.0099(11) -0.0035(10) S1R 0.0320(4) 0.0528(5) 0.0379(4) -0.0045(4) -0.0005(3) 0.0108(4) O1R 0.0484(18) 0.150(4) 0.0477(18) 0.005(2) 0.0231(14) 0.024(2) C1R 0.0384(19) 0.0366(17) 0.055(2) -0.0006(16) -0.0065(16) -0.0001(14) C2R 0.0398(19) 0.048(2) 0.044(2) -0.0110(16) -0.0052(15) 0.0030(15) C1S 0.101(4) 0.054(2) 0.071(3) -0.007(2) -0.001(3) -0.007(2) O1S 0.059(3) 0.056(3) 0.059(3) 0.005(3) 0.010(3) -0.011(2) O1S' 0.055(3) 0.069(4) 0.068(4) -0.011(3) 0.007(3) -0.013(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 Ni N1 1.9747(18) . Y Ni N13L 2.0632(19) . Y Ni O4 2.1056(16) . Y Ni O2 2.1153(16) . Y Ni N1L 2.1242(19) . Y Ni N7L 2.1257(18) . Y N1 C6 1.327(3) . ? N1 C2 1.330(3) . ? C2 C3 1.389(3) . ? C2 C8 1.518(3) . ? C3 C4 1.383(4) . ? C4 C5 1.393(4) . ? C5 C6 1.387(3) . ? C6 C7 1.515(3) . ? C7 O1 1.233(3) . ? C7 O2 1.286(3) . ? C8 O3 1.225(3) . ? C8 O4 1.290(3) . ? N1L C6L 1.330(3) . ? N1L C2L 1.335(3) . ? C2L C3L 1.377(3) . ? C3L C4L 1.387(3) . ? C4L C5L 1.382(3) . ? C4L C10L 1.485(3) 4_676 ? C5L C6L 1.385(3) . ? N7L C12L 1.337(3) . ? N7L C8L 1.340(3) . ? C8L C9L 1.378(3) . ? C9L C10L 1.392(3) . ? C10L C11L 1.388(3) . ? C10L C4L 1.485(3) 4_475 ? C11L C12L 1.385(3) . ? N13L C18L 1.332(3) . ? N13L C14L 1.335(3) . ? C14L C15L 1.388(3) . ? C15L C16L 1.387(3) . ? C16L C17L 1.391(3) . ? C16L C16L 1.491(4) 3_665 ? C17L C18L 1.380(3) . ? S1R O1R 1.510(3) . ? S1R C2R 1.771(3) . ? S1R C1R 1.776(3) . ? S1R' O1R 1.412(16) . ? S1R' C1R 1.509(16) . ? C1S O1S' 1.282(6) . ? C1S O1S 1.370(6) . ? 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 Ni N13L 178.89(8) . . Y N1 Ni O4 78.34(7) . . Y N13L Ni O4 101.34(7) . . Y N1 Ni O2 78.19(7) . . Y N13L Ni O2 102.10(7) . . Y O4 Ni O2 156.49(6) . . Y N1 Ni N1L 93.41(7) . . Y N13L Ni N1L 87.66(7) . . Y O4 Ni N1L 91.29(7) . . Y O2 Ni N1L 91.53(7) . . Y N1 Ni N7L 94.68(7) . . Y N13L Ni N7L 84.25(7) . . Y O4 Ni N7L 90.96(7) . . Y O2 Ni N7L 89.52(7) . . Y N1L Ni N7L 171.88(7) . . Y C6 N1 C2 122.5(2) . . ? C6 N1 Ni 118.87(15) . . Y C2 N1 Ni 118.42(15) . . Y N1 C2 C3 120.3(2) . . ? N1 C2 C8 113.49(19) . . ? C3 C2 C8 126.2(2) . . ? C4 C3 C2 118.1(2) . . ? C3 C4 C5 120.6(2) . . ? C6 C5 C4 118.0(2) . . ? N1 C6 C5 120.5(2) . . ? N1 C6 C7 113.17(19) . . ? C5 C6 C7 126.4(2) . . ? O1 C7 O2 126.3(2) . . ? O1 C7 C6 118.9(2) . . ? O2 C7 C6 114.9(2) . . ? C7 O2 Ni 114.63(14) . . Y O3 C8 O4 126.8(2) . . ? O3 C8 C2 119.0(2) . . ? O4 C8 C2 114.27(19) . . ? C8 O4 Ni 115.15(14) . . Y C6L N1L C2L 116.4(2) . . ? C6L N1L Ni 122.62(16) . . Y C2L N1L Ni 120.71(16) . . Y N1L C2L C3L 123.9(2) . . ? C2L C3L C4L 119.7(2) . . ? C5L C4L C3L 116.5(2) . . ? C5L C4L C10L 122.2(2) . 4_676 ? C3L C4L C10L 121.3(2) . 4_676 ? C4L C5L C6L 120.0(2) . . ? N1L C6L C5L 123.4(2) . . ? C12L N7L C8L 116.84(19) . . ? C12L N7L Ni 124.39(15) . . Y C8L N7L Ni 118.35(15) . . Y N7L C8L C9L 123.7(2) . . ? C8L C9L C10L 119.4(2) . . ? C11L C10L C9L 117.1(2) . . ? C11L C10L C4L 121.7(2) . 4_475 ? C9L C10L C4L 121.2(2) . 4_475 ? C12L C11L C10L 119.8(2) . . ? N7L C12L C11L 123.2(2) . . ? C18L N13L C14L 117.1(2) . . ? C18L N13L Ni 120.51(16) . . Y C14L N13L Ni 121.42(16) . . Y N13L C14L C15L 123.3(2) . . ? C16L C15L C14L 119.4(2) . . ? C15L C16L C17L 117.0(2) . . ? C15L C16L C16L 121.4(3) . 3_665 ? C17L C16L C16L 121.6(3) . 3_665 ? C18L C17L C16L 119.6(2) . . ? N13L C18L C17L 123.4(2) . . ? O1R S1R C2R 107.28(19) . . ? O1R S1R C1R 106.1(2) . . ? C2R S1R C1R 96.70(17) . . ? O1R S1R' C1R 128.5(11) . . ? S1R' O1R S1R 61.3(6) . . ? S1R' C1R S1R 53.3(6) . . ? O1S' C1S O1S 97.4(5) . . ? _diffrn_measured_fraction_theta_max 0.907 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.592 _refine_diff_density_min -0.353 _refine_diff_density_rms 0.072 #=== END of CIF # Attachment 'CIF_8_NIDPEN.CIF' data_NIDPEN_Complex_8 _database_code_depnum_ccdc_archive 'CCDC 742530' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Ni(II)(dipic)(diazobpe)](H2O)(diazobpe)0.5' _chemical_melting_point ? _chemical_formula_moiety 'C17 H11 Ni N5 O4, 0.5(C10 H8 N4), H2 O' _chemical_formula_sum 'C22 H17 N7 Ni O5' _chemical_formula_weight 518.14 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.1967(7) _cell_length_b 15.8470(8) _cell_length_c 10.6187(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.310(2) _cell_angle_gamma 90.00 _cell_volume 2184.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5646 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 28.94 _exptl_crystal_description block _exptl_crystal_colour amber _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 0.940 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min . _exptl_absorpt_correction_T_max . _exptl_absorpt_process_details . _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.6900 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 15 _diffrn_reflns_number 15706 _diffrn_reflns_av_R_equivalents 0.039 _diffrn_reflns_av_sigmaI/netI 0.049 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 29.51 _reflns_number_total 6009 _reflns_number_gt 4595 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Bruker SMART version 5.624 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.02A (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL/PC v.5.1 (Sheldrick, 2008)' _computing_publication_material 'SHELXL97; PLATON (Spek, 2003)' _refine_special_details ; ; _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^)+(0.0357P)^2^+1.8784P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary 'difference Fourier method' _atom_sites_solution_hydrogens 'aromatic H geometrically placed, water H located from delta-F' _refine_ls_hydrogen_treatment 'aromatic H refined with riding model, water H refined with restraints' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6009 _refine_ls_number_parameters 322 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.0978 _refine_ls_wR_factor_gt 0.0904 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.044 _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 Ni Ni 0.368545(19) 1.316382(16) 0.74045(2) 0.01026(7) Uani 1 1 d . . . N1 N 0.36761(13) 1.41349(10) 0.62027(16) 0.0116(3) Uani 1 1 d . . . C2 C 0.36910(15) 1.40081(12) 0.49598(19) 0.0122(4) Uani 1 1 d . . . C3 C 0.37108(17) 1.46832(13) 0.4131(2) 0.0173(4) Uani 1 1 d . . . H3 H 0.3733 1.4594 0.3252 0.021 Uiso 1 1 calc R . . C4 C 0.36971(19) 1.54945(14) 0.4628(2) 0.0223(5) Uani 1 1 d . . . H4 H 0.3714 1.5968 0.4084 0.027 Uiso 1 1 calc R . . C5 C 0.36594(19) 1.56166(14) 0.5912(2) 0.0204(5) Uani 1 1 d . . . H5 H 0.3635 1.6169 0.6252 0.025 Uiso 1 1 calc R . . C6 C 0.36574(16) 1.49129(13) 0.6687(2) 0.0139(4) Uani 1 1 d . . . C7 C 0.36720(15) 1.30807(12) 0.46035(19) 0.0120(4) Uani 1 1 d . . . O1 O 0.36942(12) 1.29165(9) 0.34431(14) 0.0161(3) Uani 1 1 d . . . O2 O 0.36179(11) 1.25649(9) 0.54944(14) 0.0146(3) Uani 1 1 d . . . C8 C 0.36237(16) 1.49218(13) 0.8115(2) 0.0153(4) Uani 1 1 d . . . O3 O 0.34881(15) 1.55965(10) 0.86327(16) 0.0261(4) Uani 1 1 d . . . O4 O 0.37314(11) 1.41945(9) 0.86522(14) 0.0147(3) Uani 1 1 d . . . N1L N 0.53082(13) 1.30758(11) 0.77129(16) 0.0136(3) Uani 1 1 d . . . C2L C 0.58880(17) 1.36146(15) 0.8513(2) 0.0194(4) Uani 1 1 d . . . H2L H 0.5555 1.3992 0.9002 0.023 Uiso 1 1 calc R . . C3L C 0.69527(17) 1.36435(16) 0.8655(2) 0.0225(5) Uani 1 1 d . . . H3L H 0.7341 1.4024 0.9244 0.027 Uiso 1 1 calc R . . C4L C 0.74403(16) 1.31062(14) 0.7922(2) 0.0176(4) Uani 1 1 d . . . C5L C 0.68548(16) 1.25212(13) 0.7126(2) 0.0168(4) Uani 1 1 d . . . H5L H 0.7173 1.2129 0.6643 0.020 Uiso 1 1 calc R . . C6L C 0.57990(16) 1.25248(12) 0.7055(2) 0.0159(4) Uani 1 1 d . . . H6L H 0.5399 1.2121 0.6520 0.019 Uiso 1 1 calc R . . N7L N 0.85350(14) 1.31791(13) 0.8052(2) 0.0224(4) Uani 1 1 d . . . N8L N 0.88461(14) 1.30399(13) 0.70239(19) 0.0208(4) Uani 1 1 d . . . C9L C 0.99509(17) 1.31095(14) 0.7148(2) 0.0189(4) Uani 1 1 d . . . C10L C 1.06061(17) 1.33671(15) 0.8246(2) 0.0207(5) Uani 1 1 d . . . H10L H 1.0344 1.3531 0.8986 0.025 Uiso 1 1 calc R . . C11L C 1.16496(17) 1.33802(15) 0.8240(2) 0.0204(5) Uani 1 1 d . . . H11L H 1.2100 1.3553 0.8996 0.024 Uiso 1 1 calc R . . N12L N 1.20655(14) 1.31592(12) 0.72107(17) 0.0161(3) Uani 1 1 d . . . C13L C 1.14161(17) 1.29376(16) 0.6146(2) 0.0224(5) Uani 1 1 d . . . H13L H 1.1695 1.2791 0.5411 0.027 Uiso 1 1 calc R . . C14L C 1.03539(18) 1.29111(17) 0.6062(2) 0.0259(5) Uani 1 1 d . . . H14L H 0.9915 1.2762 0.5284 0.031 Uiso 1 1 calc R . . N1B N 1.0424(2) 1.41488(19) 1.1072(3) 0.0508(7) Uani 1 1 d . . . C2B C 0.9458(3) 1.4157(2) 1.1289(3) 0.0553(10) Uani 1 1 d . . . H2B H 0.8924 1.3998 1.0606 0.066 Uiso 1 1 calc R . . C3B C 0.9183(2) 1.4380(2) 1.2442(3) 0.0421(7) Uani 1 1 d . . . H3B H 0.8485 1.4365 1.2554 0.051 Uiso 1 1 calc R . . C4B C 0.9955(2) 1.46248(17) 1.3417(3) 0.0301(6) Uani 1 1 d . . . C5B C 1.0960(2) 1.4624(2) 1.3216(3) 0.0419(7) Uani 1 1 d . . . H5B H 1.1509 1.4786 1.3878 0.050 Uiso 1 1 calc R . . C6B C 1.1148(3) 1.4383(2) 1.2029(3) 0.0491(8) Uani 1 1 d . . . H6B H 1.1841 1.4387 1.1894 0.059 Uiso 1 1 calc R . . N7B N 0.96404(18) 1.48687(16) 1.4594(2) 0.0328(5) Uani 1 1 d . . . O1W O 0.3559(2) 1.07298(12) 0.62066(19) 0.0464(6) Uani 1 1 d D . . H1W H 0.367(3) 1.067(2) 0.5472(17) 0.070 Uiso 1 1 d D . . H2W H 0.361(3) 1.1235(8) 0.636(3) 0.070 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 Ni 0.00943(12) 0.01113(12) 0.01092(12) 0.00094(10) 0.00368(8) 0.00001(10) N1 0.0113(8) 0.0112(8) 0.0129(8) -0.0012(6) 0.0037(6) 0.0006(6) C2 0.0127(9) 0.0120(9) 0.0121(9) -0.0004(7) 0.0028(7) 0.0006(7) C3 0.0228(11) 0.0185(10) 0.0113(9) 0.0015(8) 0.0044(8) 0.0004(8) C4 0.0332(13) 0.0157(10) 0.0179(11) 0.0052(8) 0.0046(9) -0.0009(9) C5 0.0322(13) 0.0117(10) 0.0175(11) -0.0009(8) 0.0048(9) 0.0007(8) C6 0.0152(10) 0.0138(9) 0.0129(9) -0.0021(7) 0.0035(7) 0.0001(7) C7 0.0083(9) 0.0130(9) 0.0149(9) -0.0028(7) 0.0027(7) -0.0007(7) O1 0.0177(8) 0.0170(7) 0.0145(7) -0.0053(6) 0.0055(6) 0.0008(6) O2 0.0165(8) 0.0118(7) 0.0163(7) 0.0009(6) 0.0051(6) 0.0000(5) C8 0.0154(10) 0.0175(10) 0.0133(9) -0.0026(8) 0.0033(8) -0.0005(8) O3 0.0445(11) 0.0184(8) 0.0163(8) -0.0050(6) 0.0079(7) 0.0037(7) O4 0.0164(7) 0.0160(7) 0.0123(7) -0.0001(6) 0.0047(6) -0.0005(6) N1L 0.0123(8) 0.0155(8) 0.0137(8) 0.0038(7) 0.0041(6) 0.0007(6) C2L 0.0132(10) 0.0278(12) 0.0179(10) -0.0051(9) 0.0041(8) 0.0010(8) C3L 0.0146(11) 0.0307(13) 0.0217(11) -0.0094(9) 0.0017(8) -0.0012(9) C4L 0.0094(9) 0.0248(11) 0.0184(10) 0.0016(9) 0.0018(7) 0.0018(8) C5L 0.0139(10) 0.0152(10) 0.0222(11) 0.0013(8) 0.0056(8) 0.0018(8) C6L 0.0150(10) 0.0096(9) 0.0234(11) 0.0008(8) 0.0040(8) 0.0006(7) N7L 0.0112(9) 0.0297(10) 0.0276(10) -0.0041(9) 0.0076(7) -0.0005(8) N8L 0.0124(9) 0.0286(10) 0.0219(9) -0.0010(8) 0.0046(7) -0.0009(7) C9L 0.0129(10) 0.0222(11) 0.0225(11) 0.0013(9) 0.0060(8) 0.0000(8) C10L 0.0148(11) 0.0299(12) 0.0191(11) -0.0029(9) 0.0079(8) -0.0017(9) C11L 0.0151(11) 0.0290(12) 0.0171(10) -0.0015(9) 0.0032(8) -0.0035(8) N12L 0.0138(8) 0.0175(8) 0.0178(9) 0.0019(7) 0.0052(7) -0.0004(7) C13L 0.0146(11) 0.0347(13) 0.0192(11) -0.0069(9) 0.0067(8) -0.0023(9) C14L 0.0137(11) 0.0423(14) 0.0219(12) -0.0086(10) 0.0034(9) -0.0033(10) N1B 0.063(2) 0.0579(18) 0.0325(14) -0.0096(13) 0.0106(13) 0.0074(15) C2B 0.053(2) 0.071(2) 0.0358(17) -0.0163(17) -0.0098(15) 0.0143(18) C3B 0.0307(16) 0.0516(19) 0.0421(17) -0.0140(14) 0.0010(12) 0.0074(13) C4B 0.0315(14) 0.0317(13) 0.0269(13) -0.0046(11) 0.0047(10) 0.0038(11) C5B 0.0325(16) 0.059(2) 0.0352(16) -0.0128(14) 0.0085(12) -0.0065(14) C6B 0.0449(19) 0.062(2) 0.0454(19) -0.0168(16) 0.0205(15) -0.0070(16) N7B 0.0284(12) 0.0399(13) 0.0302(12) -0.0074(10) 0.0052(9) 0.0014(10) O1W 0.102(2) 0.0226(10) 0.0201(10) -0.0006(8) 0.0259(11) -0.0042(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 Ni N1 1.9978(17) . y Ni O1 2.0354(15) 4_586 y Ni O4 2.0971(15) . y Ni N12L 2.1108(18) 1_455 y Ni N1L 2.1123(17) . y Ni O2 2.2267(15) . y N1 C6 1.338(3) . ? N1 C2 1.339(3) . ? C2 C3 1.388(3) . ? C2 C7 1.517(3) . ? C3 C4 1.391(3) . ? C4 C5 1.387(3) . ? C5 C6 1.386(3) . ? C6 C8 1.526(3) . ? C7 O2 1.262(2) . ? C7 O1 1.265(2) . ? C8 O3 1.230(3) . ? C8 O4 1.282(3) . ? N1L C2L 1.343(3) . ? N1L C6L 1.353(3) . ? C2L C3L 1.387(3) . ? C3L C4L 1.388(3) . ? C4L C5L 1.392(3) . ? C4L N7L 1.431(3) . ? C5L C6L 1.382(3) . ? N7L N8L 1.252(3) . ? N8L C9L 1.444(3) . ? C9L C10L 1.383(3) . ? C9L C14L 1.389(3) . ? C10L C11L 1.378(3) . ? C11L N12L 1.354(3) . ? N12L C13L 1.337(3) . ? C13L C14L 1.389(3) . ? N1B C6B 1.317(5) . ? N1B C2B 1.336(5) . ? C2B C3B 1.384(4) . ? C3B C4B 1.372(4) . ? C4B C5B 1.380(4) . ? C4B N7B 1.438(3) . ? C5B C6B 1.382(4) . ? N7B N7B 1.235(5) 3_788 ? 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 Ni O1 173.12(7) . 4_586 y N1 Ni O4 78.45(6) . . y O1 Ni O4 108.42(6) 4_586 . y N1 Ni N12L 92.87(7) . 1_455 y O1 Ni N12L 87.55(7) 4_586 1_455 y O4 Ni N12L 88.77(7) . 1_455 y N1 Ni N1L 92.30(7) . . y O1 Ni N1L 87.32(6) 4_586 . y O4 Ni N1L 92.27(6) . . y N12L Ni N1L 174.83(7) 1_455 . y N1 Ni O2 75.63(6) . . y O1 Ni O2 97.49(6) 4_586 . y O4 Ni O2 154.08(6) . . y N12L Ni O2 92.00(6) 1_455 . y N1L Ni O2 89.27(6) . . y C6 N1 C2 121.44(17) . . ? C6 N1 Ni 117.58(14) . . y C2 N1 Ni 120.98(13) . . y N1 C2 C3 120.97(18) . . ? N1 C2 C7 112.88(17) . . ? C3 C2 C7 126.14(18) . . ? C2 C3 C4 117.96(19) . . ? C5 C4 C3 120.5(2) . . ? C6 C5 C4 118.4(2) . . ? N1 C6 C5 120.77(19) . . ? N1 C6 C8 113.35(18) . . ? C5 C6 C8 125.88(19) . . ? O2 C7 O1 127.70(18) . . ? O2 C7 C2 116.18(17) . . ? O1 C7 C2 116.11(17) . . ? C7 O1 Ni 134.58(14) . 4_585 y C7 O2 Ni 114.10(12) . . y O3 C8 O4 126.6(2) . . ? O3 C8 C6 119.00(19) . . ? O4 C8 C6 114.41(18) . . ? C8 O4 Ni 115.50(13) . . y C2L N1L C6L 117.74(18) . . ? C2L N1L Ni 120.21(14) . . y C6L N1L Ni 121.88(14) . . y N1L C2L C3L 122.8(2) . . ? C2L C3L C4L 118.8(2) . . ? C3L C4L C5L 119.1(2) . . ? C3L C4L N7L 117.2(2) . . ? C5L C4L N7L 123.6(2) . . ? C6L C5L C4L 118.4(2) . . ? N1L C6L C5L 123.1(2) . . ? N8L N7L C4L 112.60(19) . . ? N7L N8L C9L 112.95(19) . . ? C10L C9L C14L 119.5(2) . . ? C10L C9L N8L 124.6(2) . . ? C14L C9L N8L 115.9(2) . . ? C11L C10L C9L 118.4(2) . . ? N12L C11L C10L 123.3(2) . . ? C13L N12L C11L 117.33(19) . . ? C13L N12L Ni 124.61(15) . 1_655 y C11L N12L Ni 118.05(15) . 1_655 y N12L C13L C14L 123.3(2) . . ? C13L C14L C9L 118.1(2) . . ? C6B N1B C2B 116.6(3) . . ? N1B C2B C3B 124.3(3) . . ? C4B C3B C2B 117.6(3) . . ? C3B C4B C5B 119.1(3) . . ? C3B C4B N7B 116.1(2) . . ? C5B C4B N7B 124.7(3) . . ? C4B C5B C6B 118.4(3) . . ? N1B C6B C5B 123.9(3) . . ? N7B N7B C4B 113.1(3) 3_788 . ? _diffrn_measured_fraction_theta_max 0.902 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.07 _refine_diff_density_min -0.52 _refine_diff_density_rms 0.08