#Supplementary Material (ESI) for Dalton Transactions #This journal is (c) The Royal Society of Chemistry 2001 data_global data_cudppcl _database_code_CSD 164934 #manuscriptidentification_number _journal_coden_Cambridge 186 _publ_contact_author ;Prof Jorunn Sletten Department of Chemistry University of Bergen Allegaten 41 N-5007 Bergen NORWAY ; _publ_contact_author_email Jorunn.Sletten@kj.uib.no # TITLE AND AUTHOR LIST _publ_section_title ; Solid state polymerization causing transition to a ferromagnetic state. Crystal structures and magnetic properties of [Cu2(dpp)(H2O)(dmso)Cl4].dmso and [Cu2(dpp)Cl4](dpp = 2,3-bis(2-pyridyl)pyrazine ; loop_ _publ_author_name _publ_author_address 'Hilde Grove' ; Department of Chemistry University of Bergen Allegaten 41 N-5007 Bergen Norway ; 'Jorunn Sletten' ; Department of Chemistry University of Bergen Allegaten 41 N-5007 Bergen Norway ; 'Miguel Julve' ; Department of Inorganic Chemistry Faculty of Chemistry University of Valencia Dr. Moliner 50 46100 Burjassot (Valencia) Spain ; 'Francesc Lloret' ; Department of Inorganic Chemistry Faculty of Chemistry University of Valencia Dr. Moliner 50 46100 Burjassot (Valencia) Spain ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[Cu2 (C14 H10 N4) (H2 O) (C2 H6 O S) Cl4]. (C2 H6 O S)' _chemical_formula_analytical ? _chemical_formula_sum 'C18 H24 Cl4 Cu2 N4 O3 S2' _chemical_formula_weight 677.41 _chemical_melting_point ? _chemical_compound_source 'synthesized by H. Grove' 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.434(2) _cell_length_b 11.215(2) _cell_length_c 12.8942(15) _cell_angle_alpha 89.639(12) _cell_angle_beta 73.372(11) _cell_angle_gamma 66.079(13) _cell_volume 1311.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15 _cell_measurement_theta_max 25 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.716 _exptl_crystal_density_method ? _exptl_crystal_F_000 684 _exptl_absorpt_coefficient_mu 2.217 _exptl_absorpt_correction_type 'empirical, based on psi-scans' _exptl_absorpt_correction_T_min 0.71361 _exptl_absorpt_correction_T_max 0.81027 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD4' _diffrn_measurement_method 'omega/2theta scan' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '10800 sec' _diffrn_standards_decay_% 7 _diffrn_reflns_number 8258 _diffrn_reflns_av_R_equivalents 0.0195 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 2 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 27.45 _reflns_number_total 6001 _reflns_number_observed 4869 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'EXPRESS CAD4 program' _computing_cell_refinement 'EXPRESS CAD4 program' _computing_data_reduction 'XCAD4' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'XP' _computing_publication_material 'CIFTAB' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 6 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+1.2060P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom for H bound to C, difmap for H bound to O' _refine_ls_hydrogen_treatment 'riding model, for dmso idealised rotating CH3-group' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5995 _refine_ls_number_parameters 302 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_obs 0.0353 _refine_ls_wR_factor_all 0.0861 _refine_ls_wR_factor_obs 0.0776 _refine_ls_goodness_of_fit_all 1.070 _refine_ls_goodness_of_fit_obs 1.084 _refine_ls_restrained_S_all 1.077 _refine_ls_restrained_S_obs 1.084 _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 Cu1 Cu 0.12889(4) 0.49614(3) 0.19194(3) 0.02730(9) Uani 1 d . . Cu2 Cu 0.60779(4) 0.03747(4) -0.25634(3) 0.03100(9) Uani 1 d . . Cl1 Cl -0.06491(8) 0.44216(9) 0.21138(7) 0.0430(2) Uani 1 d . . Cl2 Cl 0.06400(8) 0.70760(8) 0.11844(7) 0.0395(2) Uani 1 d . . Cl3 Cl 0.62824(10) -0.17336(8) -0.26249(6) 0.0424(2) Uani 1 d . . Cl4 Cl 0.75660(10) 0.12822(9) -0.35836(7) 0.0472(2) Uani 1 d . . S1 S -0.08936(11) 0.68950(10) 0.39221(8) 0.0579(3) Uani 1 d . . S2 S 0.3059(2) -0.1378(2) -0.33974(9) 0.0863(5) Uani 1 d . . O1 O 0.0565(2) 0.5677(2) 0.3474(2) 0.0407(5) Uani 1 d . . O2 O 0.4890(3) 0.0845(3) -0.3569(2) 0.0463(6) Uani 1 d . . H21 H 0.4532(3) 0.0362(3) -0.3731(2) 0.056 Uiso 1 d R . H22 H 0.5276(3) 0.1008(3) -0.4107(2) 0.056 Uiso 1 d R . O3 O 0.3901(4) -0.0796(4) -0.4220(2) 0.0890(12) Uani 1 d . . N1 N 0.3353(2) 0.4699(2) 0.1852(2) 0.0267(5) Uani 1 d . . N2 N 0.2513(2) 0.3747(2) 0.0480(2) 0.0246(4) Uani 1 d . . N3 N 0.4323(2) 0.1815(2) -0.1220(2) 0.0267(5) Uani 1 d . . N4 N 0.7016(3) 0.0142(2) -0.1396(2) 0.0297(5) Uani 1 d . . C1 C 0.3649(4) 0.5446(3) 0.2462(3) 0.0371(7) Uani 1 d . . H1 H 0.2885(4) 0.6038(3) 0.3038(3) 0.045 Uiso 1 calc R . C2 C 0.5057(4) 0.5370(3) 0.2267(3) 0.0406(7) Uani 1 d . . H2 H 0.5239(4) 0.5883(3) 0.2720(3) 0.049 Uiso 1 calc R . C3 C 0.6178(3) 0.4532(3) 0.1401(3) 0.0355(7) Uani 1 d . . H3 H 0.7131(3) 0.4469(3) 0.1258(3) 0.043 Uiso 1 calc R . C4 C 0.5875(3) 0.3777(3) 0.0741(2) 0.0297(6) Uani 1 d . . H4 H 0.6610(3) 0.3231(3) 0.0129(2) 0.036 Uiso 1 calc R . C5 C 0.4457(3) 0.3849(2) 0.1009(2) 0.0242(5) Uani 1 d . . C6 C 0.3968(3) 0.3157(3) 0.0344(2) 0.0236(5) Uani 1 d . . C7 C 0.1975(3) 0.3436(3) -0.0241(2) 0.0284(6) Uani 1 d . . H7 H 0.0965(3) 0.3818(3) -0.0136(2) 0.034 Uiso 1 calc R . C8 C 0.2936(3) 0.2530(3) -0.1158(2) 0.0294(6) Uani 1 d . . H8 H 0.2595(3) 0.2431(3) -0.1729(2) 0.035 Uiso 1 calc R . C9 C 0.4853(3) 0.2043(3) -0.0437(2) 0.0244(5) Uani 1 d . . C10 C 0.6311(3) 0.1005(3) -0.0470(2) 0.0257(5) Uani 1 d . . C11 C 0.6891(3) 0.0812(3) 0.0394(2) 0.0300(6) Uani 1 d . . H11 H 0.6375(3) 0.1377(3) 0.1044(2) 0.036 Uiso 1 calc R . C12 C 0.8236(3) -0.0221(3) 0.0282(3) 0.0353(6) Uani 1 d . . H12 H 0.8651(3) -0.0341(3) 0.0846(3) 0.042 Uiso 1 calc R . C13 C 0.8961(3) -0.1073(3) -0.0673(3) 0.0368(7) Uani 1 d . . H13 H 0.9879(3) -0.1766(3) -0.0773(3) 0.044 Uiso 1 calc R . C14 C 0.8292(3) -0.0871(3) -0.1477(2) 0.0361(7) Uani 1 d . . H14 H 0.8754(3) -0.1472(3) -0.2107(2) 0.043 Uiso 1 calc R . C15 C -0.0577(6) 0.7638(6) 0.4984(5) 0.108(2) Uani 1 d . . H51 H -0.0280(44) 0.7010(13) 0.5475(19) 0.130 Uiso 1 calc R . H52 H -0.1468(15) 0.8380(24) 0.5377(22) 0.130 Uiso 1 calc R . H53 H 0.0186(33) 0.7924(37) 0.4674(5) 0.130 Uiso 1 calc R . C16 C -0.2163(4) 0.6342(5) 0.4745(3) 0.0668(12) Uani 1 d . . H61 H -0.1764(14) 0.5857(24) 0.5281(15) 0.080 Uiso 1 calc R . H62 H -0.2341(24) 0.5783(23) 0.4297(5) 0.080 Uiso 1 calc R . H63 H -0.3073(11) 0.7084(5) 0.5105(18) 0.080 Uiso 1 calc R . C17 C 0.3496(9) -0.2928(7) -0.4054(6) 0.128(3) Uani 1 d . . H71 H 0.2841(34) -0.3283(22) -0.3636(21) 0.154 Uiso 1 calc R . H72 H 0.4495(18) -0.3511(15) -0.4115(34) 0.154 Uiso 1 calc R . H73 H 0.3388(52) -0.2836(10) -0.4769(16) 0.154 Uiso 1 calc R . C18 C 0.1221(6) -0.0582(8) -0.3409(5) 0.116(2) Uani 1 d . . H81 H 0.0786(16) 0.0302(15) -0.3052(31) 0.139 Uiso 1 calc R . H82 H 0.0671(13) -0.1049(25) -0.3032(32) 0.139 Uiso 1 calc R . H83 H 0.1203(7) -0.0564(39) -0.4150(5) 0.139 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0238(2) 0.0307(2) 0.0233(2) -0.00396(13) -0.00499(12) -0.00901(13) Cu2 0.0350(2) 0.0330(2) 0.0245(2) -0.00065(14) -0.00990(14) -0.0134(2) Cl1 0.0319(4) 0.0543(5) 0.0414(4) -0.0097(4) -0.0033(3) -0.0220(3) Cl2 0.0352(4) 0.0367(4) 0.0433(4) 0.0100(3) -0.0151(3) -0.0100(3) Cl3 0.0550(5) 0.0367(4) 0.0365(4) 0.0013(3) -0.0070(3) -0.0249(4) Cl4 0.0605(5) 0.0560(5) 0.0401(4) 0.0120(4) -0.0165(4) -0.0387(4) S1 0.0528(5) 0.0510(5) 0.0401(5) -0.0080(4) 0.0091(4) -0.0086(4) S2 0.0904(9) 0.176(2) 0.0409(5) 0.0435(7) -0.0326(6) -0.0956(10) O1 0.0377(12) 0.0490(13) 0.0248(10) -0.0098(9) -0.0032(9) -0.0120(10) O2 0.0491(13) 0.068(2) 0.0302(11) 0.0060(11) -0.0168(10) -0.0292(12) O3 0.111(3) 0.182(4) 0.0384(15) 0.031(2) -0.032(2) -0.119(3) N1 0.0284(11) 0.0243(11) 0.0270(11) 0.0002(9) -0.0087(9) -0.0105(9) N2 0.0252(11) 0.0248(11) 0.0235(11) 0.0008(9) -0.0074(9) -0.0103(9) N3 0.0278(11) 0.0284(12) 0.0221(11) -0.0002(9) -0.0076(9) -0.0100(9) N4 0.0271(11) 0.0297(12) 0.0253(11) -0.0032(9) -0.0055(9) -0.0070(10) C1 0.042(2) 0.034(2) 0.036(2) -0.0047(13) -0.0128(13) -0.0161(13) C2 0.048(2) 0.040(2) 0.046(2) 0.0005(14) -0.022(2) -0.0248(15) C3 0.035(2) 0.038(2) 0.046(2) 0.0118(14) -0.0193(13) -0.0227(13) C4 0.0271(13) 0.0293(14) 0.0325(14) 0.0052(11) -0.0077(11) -0.0129(11) C5 0.0286(13) 0.0214(12) 0.0238(12) 0.0046(10) -0.0106(10) -0.0102(10) C6 0.0244(12) 0.0252(13) 0.0216(12) 0.0028(10) -0.0068(10) -0.0109(10) C7 0.0251(13) 0.0290(14) 0.0296(14) 0.0014(11) -0.0110(11) -0.0082(11) C8 0.0317(14) 0.0342(15) 0.0250(13) 0.0008(11) -0.0113(11) -0.0147(12) C9 0.0244(12) 0.0269(13) 0.0203(12) 0.0035(10) -0.0047(10) -0.0109(11) C10 0.0274(13) 0.0243(13) 0.0217(12) 0.0023(10) -0.0053(10) -0.0091(11) C11 0.0324(14) 0.0292(14) 0.0235(13) 0.0013(11) -0.0085(11) -0.0083(12) C12 0.037(2) 0.036(2) 0.035(2) 0.0102(13) -0.0176(13) -0.0119(13) C13 0.0289(14) 0.032(2) 0.039(2) 0.0035(13) -0.0095(12) -0.0037(12) C14 0.0322(15) 0.032(2) 0.0325(15) -0.0038(12) -0.0040(12) -0.0060(12) C15 0.098(4) 0.116(5) 0.094(4) -0.072(4) 0.042(3) -0.076(4) C16 0.048(2) 0.088(3) 0.053(2) -0.023(2) 0.006(2) -0.030(2) C17 0.170(7) 0.128(6) 0.111(5) 0.069(5) -0.059(5) -0.076(5) C18 0.077(4) 0.202(8) 0.071(4) 0.027(4) -0.011(3) -0.069(5) _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 Cu1 O1 1.974(2) . ? Cu1 N1 2.027(2) . ? Cu1 N2 2.049(2) . ? Cu1 Cl1 2.2844(9) . ? Cu1 Cl2 2.4531(9) . ? Cu2 O2 1.969(2) . ? Cu2 N4 1.981(2) . ? Cu2 N3 2.187(2) . ? Cu2 Cl3 2.2861(9) . ? Cu2 Cl4 2.2962(9) . ? S1 O1 1.529(2) . ? S1 C16 1.766(4) . ? S1 C15 1.782(5) . ? S2 O3 1.499(3) . ? S2 C18 1.762(6) . ? S2 C17 1.762(8) . ? O2 H21 0.83 . ? O2 H22 0.76 . ? N1 C1 1.333(4) . ? N1 C5 1.350(3) . ? N2 C7 1.328(3) . ? N2 C6 1.345(3) . ? N3 C8 1.319(4) . ? N3 C9 1.352(3) . ? N4 C14 1.330(4) . ? N4 C10 1.355(3) . ? C1 C2 1.384(4) . ? C1 H1 0.93 . ? C2 C3 1.369(5) . ? C2 H2 0.93 . ? C3 C4 1.386(4) . ? C3 H3 0.93 . ? C4 C5 1.388(4) . ? C4 H4 0.93 . ? C5 C6 1.476(4) . ? C6 C9 1.406(4) . ? C7 C8 1.394(4) . ? C7 H7 0.93 . ? C8 H8 0.93 . ? C9 C10 1.483(4) . ? C10 C11 1.390(4) . ? C11 C12 1.379(4) . ? C11 H11 0.93 . ? C12 C13 1.378(4) . ? C12 H12 0.93 . ? C13 C14 1.377(4) . ? C13 H13 0.93 . ? C14 H14 0.93 . ? C15 H51 0.96 . ? C15 H52 0.96 . ? C15 H53 0.96 . ? C16 H61 0.96 . ? C16 H62 0.96 . ? C16 H63 0.96 . ? C17 H71 0.96 . ? C17 H72 0.96 . ? C17 H73 0.96 . ? C18 H81 0.96 . ? C18 H82 0.96 . ? C18 H83 0.96 . ? 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 Cu1 N1 89.94(9) . . ? O1 Cu1 N2 161.73(9) . . ? N1 Cu1 N2 78.90(9) . . ? O1 Cu1 Cl1 91.91(7) . . ? N1 Cu1 Cl1 157.54(7) . . ? N2 Cu1 Cl1 93.06(7) . . ? O1 Cu1 Cl2 97.00(8) . . ? N1 Cu1 Cl2 95.64(7) . . ? N2 Cu1 Cl2 98.45(7) . . ? Cl1 Cu1 Cl2 106.33(3) . . ? O2 Cu2 N4 171.01(10) . . ? O2 Cu2 N3 93.59(9) . . ? N4 Cu2 N3 77.50(9) . . ? O2 Cu2 Cl3 92.63(8) . . ? N4 Cu2 Cl3 92.62(8) . . ? N3 Cu2 Cl3 117.79(7) . . ? O2 Cu2 Cl4 89.80(8) . . ? N4 Cu2 Cl4 92.19(8) . . ? N3 Cu2 Cl4 110.52(7) . . ? Cl3 Cu2 Cl4 131.35(4) . . ? O1 S1 C16 106.3(2) . . ? O1 S1 C15 102.0(2) . . ? C16 S1 C15 98.2(2) . . ? O3 S2 C18 105.5(3) . . ? O3 S2 C17 104.9(3) . . ? C18 S2 C17 98.1(4) . . ? S1 O1 Cu1 120.06(14) . . ? Cu2 O2 H21 121.72(8) . . ? Cu2 O2 H22 113.01(7) . . ? H21 O2 H22 105.5 . . ? C1 N1 C5 119.0(2) . . ? C1 N1 Cu1 124.3(2) . . ? C5 N1 Cu1 115.8(2) . . ? C7 N2 C6 120.1(2) . . ? C7 N2 Cu1 125.6(2) . . ? C6 N2 Cu1 114.0(2) . . ? C8 N3 C9 119.7(2) . . ? C8 N3 Cu2 128.4(2) . . ? C9 N3 Cu2 111.4(2) . . ? C14 N4 C10 119.0(2) . . ? C14 N4 Cu2 121.7(2) . . ? C10 N4 Cu2 119.2(2) . . ? N1 C1 C2 122.1(3) . . ? N1 C1 H1 118.9(2) . . ? C2 C1 H1 118.9(2) . . ? C3 C2 C1 119.3(3) . . ? C3 C2 H2 120.3(2) . . ? C1 C2 H2 120.3(2) . . ? C2 C3 C4 119.1(3) . . ? C2 C3 H3 120.5(2) . . ? C4 C3 H3 120.5(2) . . ? C3 C4 C5 118.9(3) . . ? C3 C4 H4 120.5(2) . . ? C5 C4 H4 120.5(2) . . ? N1 C5 C4 121.4(2) . . ? N1 C5 C6 113.8(2) . . ? C4 C5 C6 124.3(2) . . ? N2 C6 C9 118.8(2) . . ? N2 C6 C5 113.6(2) . . ? C9 C6 C5 127.5(2) . . ? N2 C7 C8 119.5(2) . . ? N2 C7 H7 120.3(2) . . ? C8 C7 H7 120.3(2) . . ? N3 C8 C7 120.5(2) . . ? N3 C8 H8 119.75(15) . . ? C7 C8 H8 119.7(2) . . ? N3 C9 C6 118.7(2) . . ? N3 C9 C10 114.2(2) . . ? C6 C9 C10 126.9(2) . . ? N4 C10 C11 120.5(2) . . ? N4 C10 C9 114.5(2) . . ? C11 C10 C9 124.8(2) . . ? C12 C11 C10 119.6(3) . . ? C12 C11 H11 120.2(2) . . ? C10 C11 H11 120.2(2) . . ? C13 C12 C11 119.4(3) . . ? C13 C12 H12 120.3(2) . . ? C11 C12 H12 120.3(2) . . ? C14 C13 C12 118.3(3) . . ? C14 C13 H13 120.9(2) . . ? C12 C13 H13 120.9(2) . . ? N4 C14 C13 123.1(3) . . ? N4 C14 H14 118.4(2) . . ? C13 C14 H14 118.4(2) . . ? S1 C15 H51 109.5(2) . . ? S1 C15 H52 109.5(2) . . ? H51 C15 H52 109.5 . . ? S1 C15 H53 109.5(2) . . ? H51 C15 H53 109.5 . . ? H52 C15 H53 109.5 . . ? S1 C16 H61 109.5(2) . . ? S1 C16 H62 109.47(14) . . ? H61 C16 H62 109.5 . . ? S1 C16 H63 109.5(2) . . ? H61 C16 H63 109.5 . . ? H62 C16 H63 109.5 . . ? S2 C17 H71 109.5(2) . . ? S2 C17 H72 109.5(3) . . ? H71 C17 H72 109.5 . . ? S2 C17 H73 109.5(2) . . ? H71 C17 H73 109.5 . . ? H72 C17 H73 109.5 . . ? S2 C18 H81 109.5(3) . . ? S2 C18 H82 109.5(2) . . ? H81 C18 H82 109.5 . . ? S2 C18 H83 109.5(2) . . ? H81 C18 H83 109.5 . . ? H82 C18 H83 109.5 . . ? _refine_diff_density_max 0.541 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.074 "#===END" data_cudppclpoly _database_code_CSD 164935 #manuscriptidentification_number _journal_coden_Cambridge 186 _publ_contact_author ;Prof Jorunn Sletten Department of Chemistry University of Bergen Allegaten 41 N-5007 Bergen NORWAY ; _publ_contact_author_email Jorunn.Sletten@kj.uib.no # TITLE AND AUTHOR LIST _publ_section_title ; Solid state polymerization causing transition to a ferromagnetic state. Crystal structures and magnetic properties of [Cu2(dpp)(H2O)(dmso)Cl4].dmso and [Cu2(dpp)Cl4] (dpp = 2,3-bis(2-pyridyl)pyrazine ; loop_ _publ_author_name _publ_author_address 'Hilde Grove' ; Department of Chemistry University of Bergen Allegaten 41 N-5007 Bergen Norway ; 'Jorunn Sletten' ; Department of Chemistry University of Bergen Allegaten 41 N-5007 Bergen Norway ; 'Miguel Julve' ; Department of Inorganic Chemistry Faculty of Chemistry University of Valencia Dr. Moliner 50 46100 Burjassot (Valencia) Spain ; 'Francesc Lloret' ; Department of Inorganic Chemistry Faculty of Chemistry University of Valencia Dr. Moliner 50 46100 Burjassot (Valencia) Spain ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural [Cu (C14 H10 N4) Cl4]n _chemical_formula_analytical 'C14 H10 Cl4 Cu2 N4' _chemical_formula_sum 'C14 H10 Cl4 Cu2 N4' _chemical_formula_weight 503.14 _chemical_melting_point ? _chemical_compound_source 'synthesized by H. Grove' 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 '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 15.1964(3) _cell_length_b 15.0813(8) _cell_length_c 7.2346(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.876(3) _cell_angle_gamma 90.00 _cell_volume 1657.15(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 4 _cell_measurement_theta_max 25 _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.017 _exptl_crystal_density_method ? _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 3.215 _exptl_absorpt_correction_type 'semiempirical, SADABS' _exptl_absorpt_correction_T_min 'ratio of min to max absorption 0.813466' _exptl_absorpt_correction_T_max 'see above' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 '2K SMART CCD' _diffrn_measurement_method \w _diffrn_standards_number '50 first frames remeasured at end of data collection' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 11809 _diffrn_reflns_av_R_equivalents 0.0867 _diffrn_reflns_av_sigmaI/netI 0.0993 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 26.99 _reflns_number_total 3630 _reflns_number_observed 2258 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART, version 5.054' _computing_cell_refinement 'SAINT, version 5.00' _computing_data_reduction 'SAINT, version 5.00' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'XP, version 4.3, 1992' _computing_publication_material 'CIFTAB, Sheldrick, 1993' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 31 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0239P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3599 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0997 _refine_ls_R_factor_obs 0.0445 _refine_ls_wR_factor_all 0.1164 _refine_ls_wR_factor_obs 0.0676 _refine_ls_goodness_of_fit_all 0.975 _refine_ls_goodness_of_fit_obs 1.077 _refine_ls_restrained_S_all 1.437 _refine_ls_restrained_S_obs 1.077 _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 Cu1 Cu 0.13187(3) 0.22624(4) 0.13544(8) 0.0201(2) Uani 1 d . . Cu2 Cu 0.47448(3) 0.01641(4) -0.26532(8) 0.0197(2) Uani 1 d . . Cl1 Cl 0.02874(7) 0.26241(8) 0.3495(2) 0.0237(3) Uani 1 d . . Cl2 Cl 0.17900(7) 0.36619(8) 0.1043(2) 0.0243(3) Uani 1 d . . Cl3 Cl 0.58066(7) 0.11163(8) -0.1760(2) 0.0281(3) Uani 1 d . . Cl4 Cl 0.57156(7) -0.08056(8) -0.3856(2) 0.0261(3) Uani 1 d . . N1 N 0.1100(2) 0.0945(2) 0.1598(5) 0.0191(9) Uani 1 d . . N2 N 0.2520(2) 0.1757(2) 0.0511(5) 0.0179(9) Uani 1 d . . N3 N 0.3812(2) 0.0923(2) -0.1423(5) 0.0179(9) Uani 1 d . . N4 N 0.3714(2) -0.0686(2) -0.2722(5) 0.0181(9) Uani 1 d . . C1 C 0.0403(3) 0.0573(3) 0.2390(6) 0.0247(12) Uani 1 d . . H1 H -0.0096(3) 0.0933(3) 0.2605(6) 0.030 Uiso 1 calc R . C2 C 0.0378(3) -0.0303(3) 0.2904(6) 0.0243(12) Uani 1 d . . H2 H -0.0144(3) -0.0557(3) 0.3361(6) 0.029 Uiso 1 calc R . C3 C 0.1131(3) -0.0804(3) 0.2738(6) 0.0242(11) Uani 1 d . . H3 H 0.1151(3) -0.1397(3) 0.3177(6) 0.029 Uiso 1 calc R . C4 C 0.1854(3) -0.0432(3) 0.1927(6) 0.0228(11) Uani 1 d . . H4 H 0.2382(3) -0.0763(3) 0.1822(6) 0.027 Uiso 1 calc R . C5 C 0.1800(3) 0.0422(3) 0.1273(6) 0.0168(10) Uani 1 d . . C6 C 0.2493(3) 0.0869(3) 0.0264(6) 0.0172(10) Uani 1 d . . C7 C 0.3195(3) 0.2211(3) -0.0149(6) 0.0217(11) Uani 1 d . . H7 H 0.3208(3) 0.2838(3) -0.0036(6) 0.026 Uiso 1 calc R . C8 C 0.3876(3) 0.1780(3) -0.0992(6) 0.0213(11) Uani 1 d . . H8 H 0.4395(3) 0.2097(3) -0.1269(6) 0.026 Uiso 1 calc R . C9 C 0.3090(3) 0.0464(3) -0.0945(6) 0.0162(10) Uani 1 d . . C10 C 0.2978(3) -0.0390(3) -0.1916(6) 0.0171(11) Uani 1 d . . C11 C 0.2177(3) -0.0825(3) -0.2167(6) 0.0232(11) Uani 1 d . . H11 H 0.1656(3) -0.0586(3) -0.1677(6) 0.028 Uiso 1 calc R . C12 C 0.2154(3) -0.1612(3) -0.3144(6) 0.0230(11) Uani 1 d . . H12 H 0.1616(3) -0.1929(3) -0.3297(6) 0.028 Uiso 1 calc R . C13 C 0.2900(3) -0.1937(3) -0.3887(6) 0.0240(12) Uani 1 d . . H13 H 0.2892(3) -0.2483(3) -0.4541(6) 0.029 Uiso 1 calc R . C14 C 0.3676(3) -0.1448(3) -0.3667(6) 0.0250(12) Uani 1 d . . H14 H 0.4196(3) -0.1665(3) -0.4206(6) 0.030 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0179(3) 0.0188(3) 0.0239(3) -0.0025(3) 0.0042(3) 0.0008(3) Cu2 0.0165(3) 0.0223(3) 0.0206(3) -0.0016(3) 0.0043(2) 0.0030(3) Cl1 0.0226(6) 0.0268(7) 0.0216(6) -0.0022(5) 0.0025(5) 0.0061(5) Cl2 0.0224(6) 0.0198(7) 0.0306(7) -0.0024(6) -0.0002(5) -0.0002(5) Cl3 0.0176(6) 0.0345(8) 0.0323(7) -0.0047(6) 0.0012(5) 0.0005(5) Cl4 0.0237(6) 0.0279(7) 0.0272(7) -0.0009(6) 0.0069(5) 0.0093(6) N1 0.014(2) 0.024(2) 0.019(2) -0.003(2) 0.002(2) 0.002(2) N2 0.016(2) 0.019(2) 0.019(2) 0.000(2) 0.003(2) 0.000(2) N3 0.015(2) 0.018(2) 0.020(2) 0.002(2) 0.003(2) 0.000(2) N4 0.021(2) 0.016(2) 0.017(2) 0.000(2) 0.003(2) 0.004(2) C1 0.020(3) 0.027(3) 0.027(3) -0.007(2) 0.005(2) 0.003(2) C2 0.018(3) 0.029(3) 0.026(3) -0.008(2) 0.008(2) -0.009(2) C3 0.030(3) 0.020(3) 0.023(3) 0.002(2) 0.000(2) -0.004(2) C4 0.018(2) 0.028(3) 0.023(3) -0.003(2) 0.003(2) 0.002(2) C5 0.016(2) 0.020(3) 0.014(2) -0.002(2) 0.001(2) 0.003(2) C6 0.012(2) 0.021(3) 0.018(3) 0.001(2) -0.002(2) 0.002(2) C7 0.023(3) 0.013(3) 0.029(3) 0.002(2) 0.001(2) -0.007(2) C8 0.019(2) 0.020(3) 0.026(3) 0.000(2) 0.004(2) -0.002(2) C9 0.013(2) 0.018(3) 0.017(3) 0.003(2) -0.002(2) -0.001(2) C10 0.019(2) 0.018(3) 0.014(2) 0.001(2) -0.002(2) 0.002(2) C11 0.023(3) 0.021(3) 0.026(3) -0.003(2) 0.003(2) 0.002(2) C12 0.026(3) 0.017(3) 0.026(3) 0.000(2) -0.003(2) -0.004(2) C13 0.035(3) 0.013(3) 0.024(3) -0.004(2) 0.000(2) -0.002(2) C14 0.030(3) 0.023(3) 0.022(3) 0.000(2) 0.006(2) 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 Cu1 N1 2.024(4) . ? Cu1 N2 2.088(3) . ? Cu1 Cl2 2.2425(13) . ? Cu1 Cl1 2.3043(12) . ? Cu1 Cl1 2.5600(13) 4_565 ? Cu2 N4 2.024(4) . ? Cu2 N3 2.049(3) . ? Cu2 Cl3 2.2394(13) . ? Cu2 Cl4 2.2708(12) . ? Cu2 Cl4 2.7726(13) 3_654 ? Cl1 Cu1 2.5600(13) 4_566 ? N1 C1 1.343(5) . ? N1 C5 1.351(5) . ? N2 C7 1.335(5) . ? N2 C6 1.352(5) . ? N3 C8 1.332(5) . ? N3 C9 1.351(5) . ? N4 C14 1.338(6) . ? N4 C10 1.354(5) . ? C1 C2 1.373(6) . ? C1 H1 0.95 . ? C2 C3 1.379(6) . ? C2 H2 0.95 . ? C3 C4 1.382(6) . ? C3 H3 0.95 . ? C4 C5 1.374(6) . ? C4 H4 0.95 . ? C5 C6 1.465(6) . ? C6 C9 1.418(6) . ? C7 C8 1.380(6) . ? C7 H7 0.95 . ? C8 H8 0.95 . ? C9 C10 1.474(6) . ? C10 C11 1.390(6) . ? C11 C12 1.381(6) . ? C11 H11 0.95 . ? C12 C13 1.361(6) . ? C12 H12 0.95 . ? C13 C14 1.395(6) . ? C13 H13 0.95 . ? C14 H14 0.95 . ? 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 Cu1 N2 79.31(14) . . ? N1 Cu1 Cl2 170.74(10) . . ? N2 Cu1 Cl2 91.67(11) . . ? N1 Cu1 Cl1 93.25(10) . . ? N2 Cu1 Cl1 154.59(11) . . ? Cl2 Cu1 Cl1 94.08(5) . . ? N1 Cu1 Cl1 92.18(11) . 4_565 ? N2 Cu1 Cl1 107.83(10) . 4_565 ? Cl2 Cu1 Cl1 92.58(4) . 4_565 ? Cl1 Cu1 Cl1 96.63(4) . 4_565 ? N4 Cu2 N3 79.53(14) . . ? N4 Cu2 Cl3 164.42(11) . . ? N3 Cu2 Cl3 91.08(11) . . ? N4 Cu2 Cl4 95.43(11) . . ? N3 Cu2 Cl4 173.76(11) . . ? Cl3 Cu2 Cl4 93.01(5) . . ? N4 Cu2 Cl4 91.53(11) . 3_654 ? N3 Cu2 Cl4 92.47(10) . 3_654 ? Cl3 Cu2 Cl4 101.35(5) . 3_654 ? Cl4 Cu2 Cl4 91.34(4) . 3_654 ? Cu1 Cl1 Cu1 98.46(4) . 4_566 ? C1 N1 C5 117.9(4) . . ? C1 N1 Cu1 125.5(3) . . ? C5 N1 Cu1 115.2(3) . . ? C7 N2 C6 118.7(4) . . ? C7 N2 Cu1 127.4(3) . . ? C6 N2 Cu1 112.2(3) . . ? C8 N3 C9 119.4(4) . . ? C8 N3 Cu2 126.7(3) . . ? C9 N3 Cu2 113.9(3) . . ? C14 N4 C10 118.8(4) . . ? C14 N4 Cu2 125.3(3) . . ? C10 N4 Cu2 115.5(3) . . ? N1 C1 C2 123.1(4) . . ? N1 C1 H1 118.4(3) . . ? C2 C1 H1 118.4(3) . . ? C1 C2 C3 118.2(4) . . ? C1 C2 H2 120.9(3) . . ? C3 C2 H2 120.9(3) . . ? C2 C3 C4 119.2(5) . . ? C2 C3 H3 120.4(3) . . ? C4 C3 H3 120.4(3) . . ? C5 C4 C3 119.1(4) . . ? C5 C4 H4 120.4(3) . . ? C3 C4 H4 120.4(3) . . ? N1 C5 C4 121.7(4) . . ? N1 C5 C6 113.7(4) . . ? C4 C5 C6 124.5(4) . . ? N2 C6 C9 119.4(4) . . ? N2 C6 C5 114.1(4) . . ? C9 C6 C5 126.4(4) . . ? N2 C7 C8 120.8(4) . . ? N2 C7 H7 119.6(3) . . ? C8 C7 H7 119.6(3) . . ? N3 C8 C7 120.7(4) . . ? N3 C8 H8 119.7(2) . . ? C7 C8 H8 119.7(3) . . ? N3 C9 C6 118.6(4) . . ? N3 C9 C10 114.0(4) . . ? C6 C9 C10 127.1(4) . . ? N4 C10 C11 121.3(4) . . ? N4 C10 C9 114.2(4) . . ? C11 C10 C9 124.2(4) . . ? C12 C11 C10 118.7(4) . . ? C12 C11 H11 120.6(3) . . ? C10 C11 H11 120.6(3) . . ? C13 C12 C11 120.2(4) . . ? C13 C12 H12 119.9(3) . . ? C11 C12 H12 119.9(3) . . ? C12 C13 C14 118.5(4) . . ? C12 C13 H13 120.8(3) . . ? C14 C13 H13 120.8(3) . . ? N4 C14 C13 122.3(4) . . ? N4 C14 H14 118.9(3) . . ? C13 C14 H14 118.9(3) . . ? _refine_diff_density_max 0.580 _refine_diff_density_min -0.524 _refine_diff_density_rms 0.128 "#===END"