Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_y924 _database_code_CSD 154232 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Shen, Liang' 'Xu, Yun-Zhi' _publ_contact_author_name 'Dr Liang Shen' _publ_contact_author_address ; Chemistry Hangzhou Teachers College wen yi road 96# Hangzhou Zhejiang 310012 CHINA ; _publ_contact_author_email 'SHENCHEM@SINA.COM' _publ_section_title ; Structure and magnetic properties of a novel two-dimensional thiocyanato-bridged heterometallic polymer {Cu(en)2[Ni(en)(SCN)3]2}n ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H32 Cu N14 Ni2 S6' _chemical_formula_weight 769.86 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' 'S' 'S' 0.1246 0.1234 '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' '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 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 7.472(2) _cell_length_b 21.770(7) _cell_length_c 9.297(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.01(1) _cell_angle_gamma 90.00 _cell_volume 1504.0(7) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 31 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 15.82 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.700 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 790 _exptl_absorpt_coefficient_mu 2.389 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4040 _exptl_absorpt_correction_T_max 0.4786 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.99 _diffrn_reflns_number 3036 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2613 _reflns_number_gt 2111 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0416P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2613 _refine_ls_number_parameters 187 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0365 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_ref 0.0680 _refine_ls_wR_factor_gt 0.0663 _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_restrained_S_all 0.979 _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 Cu Cu 0.0000 0.5000 0.0000 0.03264(14) Uani 1 2 d S . . Ni Ni 0.13043(4) 0.667385(15) 0.41231(4) 0.02998(11) Uani 1 1 d . . . S1 S 0.32515(12) 0.58344(4) -0.03083(9) 0.0495(2) Uani 1 1 d . A . S2 S -0.34021(11) 0.52250(4) 0.37132(11) 0.0520(2) Uani 1 1 d . A . S3 S -0.14378(10) 0.71657(4) 0.26510(9) 0.0454(2) Uani 1 1 d . A . N1 N 0.2886(3) 0.74553(10) 0.4050(3) 0.0416(6) Uani 0.50 1 d PD A 1 H1A H 0.3226 0.7501 0.3156 0.050 Uiso 0.50 1 calc PR A 1 H1B H 0.2244 0.7789 0.4251 0.050 Uiso 0.50 1 calc PR A 1 N2 N 0.3599(3) 0.63273(10) 0.5308(3) 0.0424(6) Uani 0.50 1 d PD A 1 H2A H 0.3445 0.6315 0.6255 0.051 Uiso 0.50 1 calc PR A 1 H2B H 0.3827 0.5944 0.5013 0.051 Uiso 0.50 1 calc PR A 1 N1' N 0.2886(3) 0.74553(10) 0.4050(3) 0.0416(6) Uani 0.50 1 d P A 2 H1A' H 0.2822 0.7597 0.3137 0.050 Uiso 0.50 1 calc PR A 2 H1B' H 0.2476 0.7751 0.4609 0.050 Uiso 0.50 1 calc PR A 2 N2' N 0.3599(3) 0.63273(10) 0.5308(3) 0.0424(6) Uani 0.50 1 d P A 2 H2A' H 0.3286 0.6154 0.6125 0.051 Uiso 0.50 1 calc PR A 2 H2B' H 0.4075 0.6031 0.4789 0.051 Uiso 0.50 1 calc PR A 2 N3 N 0.2242(3) 0.63669(12) 0.2213(3) 0.0460(6) Uani 1 1 d . A . N4 N -0.0271(3) 0.59120(11) 0.4233(3) 0.0436(6) Uani 1 1 d . A . N5 N 0.0342(4) 0.79713(13) 0.0972(3) 0.0494(7) Uani 1 1 d . . . N6 N 0.0826(3) 0.48032(10) 0.2085(2) 0.0359(5) Uani 1 1 d . . . H6A H 0.1192 0.5149 0.2560 0.043 Uiso 1 1 calc R . . H6B H -0.0089 0.4641 0.2516 0.043 Uiso 1 1 calc R . . N7 N 0.1530(3) 0.42729(10) -0.0430(2) 0.0334(5) Uani 1 1 d . . . H7A H 0.0937 0.4036 -0.1117 0.040 Uiso 1 1 calc R . . H7B H 0.2559 0.4403 -0.0755 0.040 Uiso 1 1 calc R . . C1 C 0.4495(8) 0.7405(4) 0.5110(7) 0.033(2) Uani 0.50 1 d PD A 1 H1C H 0.4200 0.7510 0.6071 0.039 Uiso 0.50 1 calc PR A 1 H1D H 0.5434 0.7679 0.4854 0.039 Uiso 0.50 1 calc PR A 1 C2 C 0.5110(9) 0.6741(3) 0.5064(10) 0.045(3) Uani 0.50 1 d PD A 1 H2C H 0.5524 0.6654 0.4130 0.054 Uiso 0.50 1 calc PR A 1 H2D H 0.6105 0.6673 0.5804 0.054 Uiso 0.50 1 calc PR A 1 C1' C 0.4770(7) 0.7309(5) 0.4568(10) 0.053(3) Uani 0.50 1 d PD A 2 H1'1 H 0.5349 0.7677 0.4978 0.064 Uiso 0.50 1 calc PR A 2 H1'2 H 0.5392 0.7188 0.3748 0.064 Uiso 0.50 1 calc PR A 2 C2' C 0.4981(14) 0.6802(4) 0.5692(9) 0.063(4) Uani 0.50 1 d PD A 2 H2'1 H 0.6172 0.6623 0.5721 0.076 Uiso 0.50 1 calc PR A 2 H2'2 H 0.4837 0.6969 0.6641 0.076 Uiso 0.50 1 calc PR A 2 C3 C 0.2697(4) 0.61513(12) 0.1185(3) 0.0350(7) Uani 1 1 d . . . C4 C -0.1580(4) 0.56277(11) 0.4035(3) 0.0309(6) Uani 1 1 d . . . C5 C -0.0398(4) 0.76397(13) 0.1655(3) 0.0357(6) Uani 1 1 d . . . C6 C 0.2326(5) 0.43599(15) 0.2132(3) 0.0504(8) Uani 1 1 d . . . H6C H 0.2443 0.4142 0.3047 0.061 Uiso 1 1 calc R . . H6D H 0.3446 0.4574 0.2036 0.061 Uiso 1 1 calc R . . C7 C 0.1937(4) 0.39166(13) 0.0913(3) 0.0448(8) Uani 1 1 d . . . H7C H 0.2970 0.3653 0.0837 0.054 Uiso 1 1 calc R . . H7D H 0.0917 0.3660 0.1082 0.054 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0410(3) 0.0263(2) 0.0297(3) -0.00381(19) -0.0005(2) 0.0081(2) Ni 0.02828(19) 0.02651(19) 0.0352(2) -0.00469(15) 0.00370(14) -0.00261(14) S1 0.0521(5) 0.0487(5) 0.0504(5) -0.0137(4) 0.0188(4) -0.0059(4) S2 0.0394(4) 0.0437(5) 0.0740(6) -0.0049(4) 0.0113(4) -0.0137(4) S3 0.0345(4) 0.0525(5) 0.0493(5) 0.0131(4) 0.0036(3) -0.0013(4) N1 0.0449(14) 0.0267(12) 0.0510(15) 0.0017(11) -0.0050(12) -0.0034(11) N2 0.0377(14) 0.0311(13) 0.0578(16) 0.0054(12) 0.0024(12) -0.0008(11) N1' 0.0449(14) 0.0267(12) 0.0510(15) 0.0017(11) -0.0050(12) -0.0034(11) N2' 0.0377(14) 0.0311(13) 0.0578(16) 0.0054(12) 0.0024(12) -0.0008(11) N3 0.0396(14) 0.0504(16) 0.0493(16) -0.0177(13) 0.0107(12) -0.0033(12) N4 0.0382(15) 0.0351(14) 0.0580(17) -0.0017(12) 0.0070(12) -0.0065(12) N5 0.0448(15) 0.0600(17) 0.0435(15) 0.0156(14) 0.0051(13) 0.0000(14) N6 0.0432(14) 0.0332(13) 0.0317(13) -0.0011(10) 0.0051(11) 0.0063(11) N7 0.0362(13) 0.0302(12) 0.0345(13) -0.0018(10) 0.0073(10) 0.0001(10) C1 0.019(3) 0.023(4) 0.059(5) 0.005(4) 0.014(3) -0.005(2) C2 0.029(4) 0.037(4) 0.061(7) 0.007(4) -0.029(4) -0.010(3) C1' 0.027(4) 0.055(6) 0.081(7) 0.013(6) 0.016(4) -0.004(3) C2' 0.079(7) 0.051(5) 0.053(7) 0.002(5) -0.027(5) -0.014(4) C3 0.0290(15) 0.0288(14) 0.0473(18) -0.0014(13) 0.0035(13) -0.0053(12) C4 0.0367(16) 0.0253(14) 0.0321(15) 0.0009(11) 0.0097(12) 0.0013(12) C5 0.0307(15) 0.0448(17) 0.0306(15) 0.0015(13) -0.0008(12) 0.0056(13) C6 0.056(2) 0.056(2) 0.0372(17) 0.0020(15) -0.0036(15) 0.0229(16) C7 0.0520(19) 0.0338(16) 0.0501(19) 0.0097(14) 0.0122(15) 0.0163(14) _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 Cu N7 2.017(2) 3_565 ? Cu N7 2.017(2) . ? Cu N6 2.018(2) 3_565 ? Cu N6 2.018(2) . ? Cu S1 3.0708(10) . ? Ni N4 2.043(2) . ? Ni N1 2.077(2) . ? Ni N5 2.080(3) 4_576 ? Ni N2 2.081(2) . ? Ni N3 2.086(3) . ? Ni S3 2.5750(10) . ? S1 C3 1.642(3) . ? S2 C4 1.620(3) . ? S3 C5 1.636(3) . ? N1 C1 1.476(4) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C2 1.481(4) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N3 C3 1.147(4) . ? N4 C4 1.156(3) . ? N5 C5 1.141(4) . ? N5 Ni 2.080(3) 4_575 ? N6 C6 1.477(4) . ? N6 H6A 0.9000 . ? N6 H6B 0.9000 . ? N7 C7 1.475(4) . ? N7 H7A 0.9000 . ? N7 H7B 0.9000 . ? C1 C2 1.518(4) . ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? C2 H2C 0.9700 . ? C2 H2D 0.9700 . ? C1' C2' 1.516(4) . ? C1' H1'1 0.9700 . ? C1' H1'2 0.9700 . ? C2' H2'1 0.9700 . ? C2' H2'2 0.9700 . ? C6 C7 1.493(4) . ? C6 H6C 0.9700 . ? C6 H6D 0.9700 . ? C7 H7C 0.9700 . ? C7 H7D 0.9700 . ? 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 N7 Cu N7 180.0 3_565 . ? N7 Cu N6 84.32(9) 3_565 3_565 ? N7 Cu N6 95.68(9) . 3_565 ? N7 Cu N6 95.68(9) 3_565 . ? N7 Cu N6 84.32(9) . . ? N6 Cu N6 180.00(12) 3_565 . ? N7 Cu S1 91.42(7) 3_565 . ? N7 Cu S1 88.58(7) . . ? N6 Cu S1 87.14(7) 3_565 . ? N6 Cu S1 92.86(7) . . ? N4 Ni N1 178.80(10) . . ? N4 Ni N5 90.52(11) . 4_576 ? N1 Ni N5 88.28(11) . 4_576 ? N4 Ni N2 97.26(9) . . ? N1 Ni N2 82.76(9) . . ? N5 Ni N2 91.96(11) 4_576 . ? N4 Ni N3 91.69(10) . . ? N1 Ni N3 89.51(10) . . ? N5 Ni N3 176.72(11) 4_576 . ? N2 Ni N3 90.17(10) . . ? N4 Ni S3 86.20(8) . . ? N1 Ni S3 93.78(7) . . ? N5 Ni S3 87.71(8) 4_576 . ? N2 Ni S3 176.53(6) . . ? N3 Ni S3 90.01(8) . . ? C3 S1 Cu 84.11(10) . . ? C5 S3 Ni 99.47(10) . . ? C1 N1 Ni 110.1(4) . . ? C1 N1 H1A 109.6 . . ? Ni N1 H1A 109.6 . . ? C1 N1 H1B 109.6 . . ? Ni N1 H1B 109.6 . . ? H1A N1 H1B 108.2 . . ? C2 N2 Ni 107.3(4) . . ? C2 N2 H2A 110.3 . . ? Ni N2 H2A 110.3 . . ? C2 N2 H2B 110.3 . . ? Ni N2 H2B 110.3 . . ? H2A N2 H2B 108.5 . . ? C3 N3 Ni 174.3(2) . . ? C4 N4 Ni 155.4(2) . . ? C5 N5 Ni 157.5(3) . 4_575 ? C6 N6 Cu 108.77(17) . . ? C6 N6 H6A 109.9 . . ? Cu N6 H6A 109.9 . . ? C6 N6 H6B 109.9 . . ? Cu N6 H6B 109.9 . . ? H6A N6 H6B 108.3 . . ? C7 N7 Cu 108.40(17) . . ? C7 N7 H7A 110.0 . . ? Cu N7 H7A 110.0 . . ? C7 N7 H7B 110.0 . . ? Cu N7 H7B 110.0 . . ? H7A N7 H7B 108.4 . . ? N1 C1 C2 106.3(6) . . ? N1 C1 H1C 110.5 . . ? C2 C1 H1C 110.5 . . ? N1 C1 H1D 110.5 . . ? C2 C1 H1D 110.5 . . ? H1C C1 H1D 108.7 . . ? N2 C2 C1 109.7(6) . . ? N2 C2 H2C 109.7 . . ? C1 C2 H2C 109.7 . . ? N2 C2 H2D 109.7 . . ? C1 C2 H2D 109.7 . . ? H2C C2 H2D 108.2 . . ? C2' C1' H1'1 108.7 . . ? C2' C1' H1'2 108.7 . . ? H1'1 C1' H1'2 107.6 . . ? C1' C2' H2'1 109.9 . . ? C1' C2' H2'2 109.9 . . ? H2'1 C2' H2'2 108.3 . . ? N3 C3 S1 177.4(3) . . ? N4 C4 S2 178.4(3) . . ? N5 C5 S3 179.2(3) . . ? N6 C6 C7 108.2(2) . . ? N6 C6 H6C 110.0 . . ? C7 C6 H6C 110.0 . . ? N6 C6 H6D 110.0 . . ? C7 C6 H6D 110.0 . . ? H6C C6 H6D 108.4 . . ? N7 C7 C6 108.0(2) . . ? N7 C7 H7C 110.1 . . ? C6 C7 H7C 110.1 . . ? N7 C7 H7D 110.1 . . ? C6 C7 H7D 110.1 . . ? H7C C7 H7D 108.4 . . ? 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 N7 Cu S1 C3 45.80(12) 3_565 . . . ? N7 Cu S1 C3 -134.20(12) . . . . ? N6 Cu S1 C3 130.04(12) 3_565 . . . ? N6 Cu S1 C3 -49.96(12) . . . . ? N4 Ni S3 C5 -151.11(13) . . . . ? N1 Ni S3 C5 30.09(13) . . . . ? N5 Ni S3 C5 118.21(13) 4_576 . . . ? N2 Ni S3 C5 33.6(13) . . . . ? N3 Ni S3 C5 -59.42(13) . . . . ? N4 Ni N1 C1 77(5) . . . . ? N5 Ni N1 C1 78.6(4) 4_576 . . . ? N2 Ni N1 C1 -13.6(3) . . . . ? N3 Ni N1 C1 -103.8(4) . . . . ? S3 Ni N1 C1 166.2(3) . . . . ? N4 Ni N2 C2 165.5(4) . . . . ? N1 Ni N2 C2 -15.7(4) . . . . ? N5 Ni N2 C2 -103.7(4) 4_576 . . . ? N3 Ni N2 C2 73.8(4) . . . . ? S3 Ni N2 C2 -19.2(15) . . . . ? N4 Ni N3 C3 -13(3) . . . . ? N1 Ni N3 C3 167(3) . . . . ? N5 Ni N3 C3 -145(2) 4_576 . . . ? N2 Ni N3 C3 84(3) . . . . ? S3 Ni N3 C3 -99(3) . . . . ? N1 Ni N4 C4 86(5) . . . . ? N5 Ni N4 C4 84.8(6) 4_576 . . . ? N2 Ni N4 C4 176.8(6) . . . . ? N3 Ni N4 C4 -92.8(6) . . . . ? S3 Ni N4 C4 -2.9(6) . . . . ? N7 Cu N6 C6 -167.5(2) 3_565 . . . ? N7 Cu N6 C6 12.5(2) . . . . ? N6 Cu N6 C6 149(48) 3_565 . . . ? S1 Cu N6 C6 -75.77(19) . . . . ? N7 Cu N7 C7 85(100) 3_565 . . . ? N6 Cu N7 C7 -164.37(19) 3_565 . . . ? N6 Cu N7 C7 15.63(19) . . . . ? S1 Cu N7 C7 108.65(19) . . . . ? Ni N1 C1 C2 39.1(6) . . . . ? Ni N2 C2 C1 42.2(7) . . . . ? N1 C1 C2 N2 -54.3(8) . . . . ? Ni N3 C3 S1 57(8) . . . . ? Cu S1 C3 N3 -30(6) . . . . ? Ni N4 C4 S2 82(10) . . . . ? Ni N5 C5 S3 145(22) 4_575 . . . ? Ni S3 C5 N5 -35(23) . . . . ? Cu N6 C6 C7 -38.1(3) . . . . ? Cu N7 C7 C6 -40.6(3) . . . . ? N6 C6 C7 N7 52.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.284 _refine_diff_density_min -0.249 _refine_diff_density_rms 0.059