#Copyright The Royal Society of Chemistry, 1998 data_global #=============================================================================== # 1. SUBMISSION DETAILS #=============================================================================== _publ_contact_author ; Prof. G. De Munno Dipartimento di Chimica Universit\'a della Calabria I-87030 Arcavacata di Rende, Cosenza Italy ; _publ_contact_author_phone '39 984 492068' _publ_contact_author_fax '39 984 492044' _publ_contact_author_email demunno@unical.it _publ_contact_letter ; Dear Sir Compounds have been identified in the paper with number 1, 2 and 3. (in this cif file they have been called data_(1), data_(2) and data_(3)). The paper has been accepted in J. C. S., Dalton Transactions with this reference number 7/08477C. No melting point has been determined. Prof. De Munno told me to prepare this punch cif file and to send it back to you. He begs your pardon for the delay in sending the crystallographic data. I hope that everything it's okay. For further comunications or informations contact me at this E-mail address: a.crispini@unical.it Yours sincerely Alessandra Crispini ; #=============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) #=============================================================================== _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full 'Journal of the Chemical Society, Dalton Transactions' _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=============================================================================== # 3. TITLE AND AUTHOR LIST #=============================================================================== _publ_section_title ; Synthesis, crystal structures and magnetic properties of one-, two- and three-dimensional bipym-containing copper(II) complexes (bipym = 2,2'-bipyrimidine) ; loop_ _publ_author_name _publ_author_address 'Giovanni De Munno' ; Dipartimento di Chimica Universit\'a degli Studi della Calabria I-87030 Arcavacata di Rende, Cosenza Italy ; 'Teresa Poerio' ; Dipartimento di Chimica Universit\'a degli Studi della Calabria I-87030 Arcavacata di Rende, Cosenza Italy ; 'Miguel Julve' ; Departament de Quimica Inorganica Facultat de Quimica Dr. Moliner 50 E-46100 Burjassot, Valencia Spain ; 'Francesc Lloret' ; Departament de Quimica Inorganica Facultat de Quimica Dr. Moliner 50 E-46100 Burjassot, Valencia Spain ; 'Juan Faus' ; Departament de Quimica Inorganica Facultat de Quimica Dr. Moliner 50 E-46100 Burjassot, Valencia Spain ; 'Andrea Caneschi' ; Dipartimento di Chimica Universit\'a degli Studi di Firenze I-50144 Via Maragliano 77, Firenze Italy ; #=============================================================================== # 4. TEXT #=============================================================================== _publ_section_abstract ; ? ; _publ_section_experimental ; ? ; _publ_section_comment ; ? ; _publ_section_acknowledgements ; ? ; _publ_section_references ; ? ; _publ_section_figure_captions ; ? ; _publ_section_table_legends ; ? ; #=============================================================================== # 5. CHEMICAL DATA #=============================================================================== #=============================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, put the structure code in the "data_?" # line below, using a unique identifier. data_(1) #=============================================================================== _chemical_name_systematic ; ; _chemical_name_common ? _chemical_formula_moiety '[Cu(bipym)(H2O)2](NO3)2.H2O' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C8 H12 Cu N6 O9' _chemical_formula_weight 399.8 _chemical_melting_point ? _chemical_compound_source 'chemical synthesis' loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C Carbon 0 32 0.0020 0.0020 Internat_Tables_Vol_IV_Table_2.3.1 H Hydrogen 0 48 0.0000 0.0000 Internat_Tables_Vol_IV_Table_2.3.1 N Nitrogen 0 8 0.0040 0.0030 Internat_Tables_Vol_IV_Table_2.3.1 O Oxygen 0 36 0.0080 0.0060 Internat_Tables_Vol_IV_Table_2.3.1 Cu Copper 0 8 0.2630 1.2660 Internat_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA #=============================================================================== _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/m 1' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '1/2+x,1/2+y,z' 'x,-y,1/2+z' '1/2+x,1/2-y,1/2+z' _cell_length_a 10.073(2) _cell_length_b 16.372(3) _cell_length_c 9.746(2) _cell_length_alpha 90. _cell_length_beta 110.08(2) _cell_length_gamma 90. _cell_volume 1509.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 295 _cell_measurement_radiation 'Mo K\a' _cell_measurement_wavelength 0.710730 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; ? ; _exptl_crystal_colour blue-green _exptl_crystal_description parallelepiped _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_diffrn 1.759 _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 1.508 _exptl_absorpt_correction_type 'semi-empirical' _exptl_absorpt_correction_T_max 0.681 _exptl_absorpt_correction_T_min 0.620 #=============================================================================== # 7. EXPERIMENTAL DATA #=============================================================================== _exptl_special_details ; ? ; _diffrn_special_details ;? ; _diffrn_ambient_temperature 295 _diffrn_radiation_wavelength 0.710730 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus xray_tube' _diffrn_radiation_monochromator 'highly-oriented graphite crystal' _diffrn_measurement_device 'Siemens R3m/V diffractometer' _diffrn_measurement_method \w-2\q _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_av_R_equivalents 1.15 _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 27.0 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_number 1857 _reflns_number_total 1757 _reflns_number_observed 1340 _reflns_observed_criterion >3\s(I) _diffrn_reflns_reduction_process ? _computing_data_collection 'Siemens P3/V,(VMS vers 4.21/V, 1990)' _computing_cell_refinement 'Siemens P3/V' _computing_data_reduction 'Siemens SHELXTL-PLUS,(VMS vers 4.21/V , 1990)' _computing_structure_solution 'Siemens SHELXTL-PLUS' _computing_structure_refinement 'Siemens SHELXTL-PLUS' _computing_molecular_graphics 'Siemens XP' _computing_publication_material 'Siemens SHELXTL-PLUS and PARST' #=============================================================================== # 8. REFINEMENT DATA #=============================================================================== _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '1/(\s^2^(F)+ 0.0012*F^2^))' _refine_ls_hydrogen_treatment '"riding model" with fixed isotropic U' _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_number_reflns 1340 _refine_ls_number_parameters 193 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 5.24 _refine_ls_R_factor_obs 3.53 _refine_ls_wR_factor_all 5.09 _refine_ls_wR_factor_obs 4.42 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 0.95 _refine_ls_shift/esd_mean 0.000 _refine_ls_shift/esd_max 0.002 _refine_diff_density_min -0.45 _refine_diff_density_max 0.39 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS #=============================================================================== loop_ _atom_site_label _atom_site_occupancy _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_type_symbol _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_disorder_group # #label occ x/a y/b z/c Ueq the typ cal att dis # Cu1 1.00 0. 0.08709(4) 0. 0.0307(2) Uani Cu ? ? ? O1 1.00 -0.1656(6) 0.1767(3) -0.1444(5) 0.043(2) Uani O ? ? ? O2 1.00 0.1050(6) 0.1820(3) 0.1078(6) 0.038(2) Uani O ? ? ? N1 1.00 -0.1050(7) -0.0027(4) -0.1396(6) 0.030(2) Uani N ? ? ? C1 1.00 -0.2233(8) -0.0432(4) -0.1469(8) 0.036(2) Uiso C ? ? ? C2 1.00 -0.2851(8) -0.0982(4) -0.2559(8) 0.038(2) Uiso C ? ? ? C3 1.00 -0.2231(9) -0.1114(5) -0.3596(9) 0.040(2) Uiso C ? ? ? N2 1.00 -0.1047(7) -0.0697(4) -0.3554(7) 0.029(2) Uani N ? ? ? C4 1.00 -0.0500(7) -0.0195(4) -0.2445(7) 0.026(1) Uiso C ? ? ? C5 1.00 0.0836(8) 0.0238(4) -0.2308(7) 0.026(2) Uiso C ? ? ? N4 1.00 0.1464(7) 0.0066(4) -0.3235(7) 0.034(2) Uani N ? ? ? C6 1.00 0.2434(8) 0.1194(5) -0.1087(9) 0.037(2) Uiso C ? ? ? C7 1.00 0.318(1) 0.1049(5) -0.201(1) 0.042(2) Uiso C ? ? ? C8 1.00 0.2655(8) 0.0468(4) -0.3084(8) 0.035(2) Uiso C ? ? ? N3 1.00 0.1261(8) 0.0792(3) -0.1225(7) 0.032(2) Uani N ? ? ? N5 1.00 -0.0165(7) 0.2275(4) -0.4045(7) 0.045(2) Uani N ? ? ? O3 1.00 -0.0352(8) 0.2682(4) -0.3041(8) 0.080(3) Uani O ? ? ? O4 1.00 -0.0493(8) 0.1552(3) -0.4183(8) 0.075(3) Uani O ? ? ? O5 1.00 0.0383(7) 0.2604(4) -0.4857(9) 0.074(3) Uani O ? ? ? N6 1.00 0.0326(7) 0.3954(4) 0.0421(7) 0.043(3) Uani N ? ? ? O6 1.00 0.1567(8) 0.4064(5) 0.1135(9) 0.084(3) Uani O ? ? ? O7 1.00 -0.0287(9) 0.4482(5) -0.0442(9) 0.099(4) Uani O ? ? ? O8 1.00 -0.0310(6) 0.3326(3) 0.0546(8) 0.068(3) Uani O ? ? ? O9 1.00 0.1733(6) 0.1496(3) 0.3857(5) 0.049(2) Uani O ? ? ? H1w 1.00 -0.241(6) 0.147(4) -0.213(6) 0.06 Uiso H ? O1 ? H2w 1.00 -0.129(8) 0.209(4) -0.206(6) 0.06 Uiso H ? O1 ? H3w 1.00 0.060(8) 0.234(2) 0.095(8) 0.06 Uiso H ? O2 ? H4w 1.00 0.155(8) 0.180(5) 0.211(2) 0.06 Uiso H ? O2 ? H5w 1.00 0.140(7) 0.181(5) 0.450(7) 0.06 Uiso H ? O9 ? H6w 1.00 0.273(2) 0.151(5) 0.435(7) 0.06 Uiso H ? O9 ? H1 1.00 -0.2622(8) -0.0295(4) -0.0742(8) 0.06 Uiso H ? C1 ? H2 1.00 -0.3648(8) -0.1253(4) -0.2686(8) 0.06 Uiso H ? C2 ? H3 1.00 -0.2451(9) -0.1580(5) -0.4308(9) 0.06 Uiso H ? C3 ? H6 1.00 0.2719(8) 0.1545(5) -0.0313(9) 0.06 Uiso H ? C6 ? H7 1.00 0.402(1) 0.1482(5) -0.206(1) 0.06 Uiso H ? C7 ? H8 1.00 0.3117(8) 0.0302(4) -0.3772(8) 0.06 Uiso H ? C8 ? 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 _atom_site_aniso_type_symbol # #label U11 U22 U33 U23 U13 U12 typ # Cu1 0.0346(3) 0.0287(3) 0.0248(3) -0.0026(5) 0.0148(3) -0.0049(5) Cu O1 0.047(3) 0.039(3) 0.036(3) 0.008(2) 0.012(3) 0.005(3) O O2 0.044(3) 0.031(3) 0.032(3) -0.001(2) 0.011(2) -0.003(2) O N1 0.032(3) 0.026(3) 0.026(3) 0.003(2) 0.013(3) 0.000(3) N N2 0.028(3) 0.029(3) 0.024(3) 0.000(2) 0.007(3) -0.003(2) N N4 0.039(3) 0.030(3) 0.027(3) -0.001(2) 0.017(3) -0.000(3) N N3 0.035(4) 0.025(3) 0.032(4) -0.006(2) 0.014(3) -0.006(3) N N5 0.040(3) 0.037(3) 0.049(4) 0.004(3) 0.008(3) -0.003(3) N O3 0.089(5) 0.054(4) 0.088(5) -0.015(3) 0.055(4) -0.021(3) O O4 0.103(5) 0.034(3) 0.072(4) -0.002(3) 0.027(4) -0.013(3) O O5 0.078(6) 0.056(3) 0.079(5) -0.002(4) 0.041(5) -0.010(3) O N6 0.033(4) 0.042(3) 0.049(4) 0.006(3) 0.014(3) 0.006(3) N O6 0.055(4) 0.092(6) 0.086(5) 0.019(4) 0.004(4) -0.014(4) O O7 0.081(6) 0.080(5) 0.113(7) 0.051(5) 0.016(5) 0.009(5) O O8 0.056(4) 0.047(3) 0.088(5) 0.011(3) 0.023(3) 0.004(3) O O9 0.051(3) 0.050(3) 0.038(3) -0.005(2) 0.009(2) -0.004(3) O #=============================================================================== # 10. MOLECULAR GEOMETRY #=============================================================================== _geom_special_details ; The geometric calculation (and the starting release of this CIF file) has been made by a locally modified release of the program PARST of prof. M. Nardelli (we have already adviced prof. Nardelli about it). This release is interactive and has included into one body : I/O interface to other programs, no formated line, logical commands, better output listing and now we are developping a graphical interface PLUTO-like. All computational routines are the original ones. However this release is reserved for internal use of our laboratory only (it is neither public neither commercial release!). ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag # # Complete list of bond lengths for non-H atoms. # Cu1 O1 2.303(5) . . . Cu1 O2 1.969(5) . . . Cu1 N1 2.036(6) . . . Cu1 N3 2.024(9) . . . Cu1 N2 2.049(8) . 3_555 . Cu1 N4 2.397(6) . 3_555 . N1 C4 1.35(1) . . . N1 C1 1.34(1) . . . N2 C4 1.318(9) . . . N2 C3 1.36(1) . . . N4 C5 1.30(1) . . . N4 C8 1.33(1) . . . N3 C5 1.345(9) . . . N3 C6 1.32(1) . . . N5 O3 1.25(1) . . . N5 O4 1.224(8) . . . N5 O5 1.23(1) . . . N6 O6 1.217(9) . . . N6 O7 1.22(1) . . . N6 O8 1.240(9) . . . C5 C4 1.49(1) . . . C2 C1 1.37(1) . . . C2 C3 1.38(1) . . . C6 C7 1.38(1) . . . C7 C8 1.38(1) . . . 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag # # Complete list of bond angles for non-H atoms. # N1 Cu1 N3 81.2(2) . . . . O2 Cu1 N3 92.0(2) . . . . O2 Cu1 N1 171.0(2) . . . . O1 Cu1 N3 98.6(2) . . . . O1 Cu1 N1 87.2(2) . . . . O1 Cu1 O2 88.1(2) . . . . O1 Cu1 N2 94.2(2) . . 3_555 . N1 Cu1 N2 95.0(3) . . 3_555 . O2 Cu1 N2 93.0(3) . . 3_555 . N3 Cu1 N2 166.4(2) . . 3_555 . O1 Cu1 N4 169.9(3) . . 3_555 . O2 Cu1 N4 92.1(2) . . 3_555 . N1 Cu1 N4 93.9(2) . . 3_555 . N3 Cu1 N4 91.5(3) . . 3_555 . N2 Cu1 N4 75.7(3) 3_555 . 3_555 . Cu1 N1 C1 129.8(5) . . . . Cu1 N1 C4 113.5(4) . . . . C4 N1 C1 116.6(7) . . . . C4 N2 C3 116.9(7) . . . . C5 N4 C8 116.8(7) . . . . Cu1 N3 C6 129.0(6) . . . . Cu1 N3 C5 114.3(5) . . . . C5 N3 C6 116.7(7) . . . . O4 N5 O5 121.0(7) . . . . O3 N5 O5 119.4(7) . . . . O3 N5 O4 119.5(6) . . . . O7 N6 O8 120.0(7) . . . . O6 N6 O8 122.0(7) . . . . O6 N6 O7 118.0(8) . . . . N4 C5 N3 126.4(7) . . . . N3 C5 C4 115.2(6) . . . . N4 C5 C4 118.4(7) . . . . C1 C2 C3 118.3(7) . . . . N3 C6 C7 121.2(8) . . . . N2 C4 C5 118.8(6) . . . . N1 C4 C5 115.5(7) . . . . N1 C4 N2 125.7(6) . . . . C6 C7 C8 117.5(8) . . . . N1 C1 C2 121.6(7) . . . . N4 C8 C7 121.5(7) . . . . N2 C3 C2 120.8(8) . . . . #=============================================================================== #=============================================================================== data_(2) #=============================================================================== _chemical_name_systematic ; ; _chemical_name_common ? _chemical_formula_moiety [Cu(bipym)(Cr2O7)] _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C8 H6 Cr2 Cu N4 O7' _chemical_formula_weight 437.7 _chemical_melting_point ? _chemical_compound_source 'chemical synthesis' loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C Carbon 0 16 0.0020 0.0020 Internat_Tables_Vol_IV_Table_2.3.1 H Hydrogen 0 12 0.0000 0.0000 Internat_Tables_Vol_IV_Table_2.3.1 N Nitrogen 0 8 0.0040 0.0030 Internat_Tables_Vol_IV_Table_2.3.1 O Oxygen 0 14 0.0080 0.0060 Internat_Tables_Vol_IV_Table_2.3.1 Cr Chromium 0 4 0.2840 0.6240 Internat_Tables_Vol_IV_Table_2.3.1 Cu Copper 0 2 0.2630 1.2660 Internat_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA #=============================================================================== _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 8.199(2) _cell_length_b 8.633(3) _cell_length_c 10.049(2) _cell_length_alpha 114.47(2) _cell_length_beta 92.67(2) _cell_length_gamma 90.48(2) _cell_volume 646.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 295 _cell_measurement_radiation 'Mo K\a' _cell_measurement_wavelength 0.710730 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; ? ; _exptl_crystal_colour brown _exptl_crystal_description prismatic _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.35 _exptl_crystal_density_diffrn 2.249 _exptl_crystal_F_000 430 _exptl_absorpt_coefficient_mu 3.324 _exptl_absorpt_correction_type 'semi-empirical' _exptl_absorpt_correction_T_max 0.491 _exptl_absorpt_correction_T_min 0.455 #=============================================================================== # 7. EXPERIMENTAL DATA #=============================================================================== _exptl_special_details ; ? ; _diffrn_special_details ;? ; _diffrn_ambient_temperature 295 _diffrn_radiation_wavelength 0.710730 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus xray_tube' _diffrn_radiation_monochromator 'highly-oriented graphite crystal' _diffrn_measurement_device 'Siemens R3m/V diffractometer' _diffrn_measurement_method \w-2\q _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_av_R_equivalents 0.65 _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 27.0 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_number 3271 _reflns_number_total 2842 _reflns_number_observed 2563 _reflns_observed_criterion >3\s(I) _diffrn_reflns_reduction_process ? _computing_data_collection 'Siemens P3/V,(VMS vers 4.21/V, 1990)' _computing_cell_refinement 'Siemens P3/V' _computing_data_reduction 'Siemens SHELXTL-PLUS,(VMS vers 4.21/V , 1990)' _computing_structure_solution 'Siemens SHELXTL-PLUS' _computing_structure_refinement 'Siemens SHELXTL-PLUS' _computing_molecular_graphics 'Siemens XP' _computing_publication_material 'Siemens SHELXTL-PLUS and PARST' #=============================================================================== # 8. REFINEMENT DATA #=============================================================================== _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '1/(\s^2^(F)+ 0.0010*F^2^))' _refine_ls_hydrogen_treatment '"riding model" with fixed isotropic U' _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_number_reflns 2563 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 2.65 _refine_ls_R_factor_obs 2.33 _refine_ls_wR_factor_all 4.83 _refine_ls_wR_factor_obs 4.13 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.16 _refine_ls_shift/esd_mean 0.002 _refine_ls_shift/esd_max 0.006 _refine_diff_density_min -0.53 _refine_diff_density_max 0.47 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS #=============================================================================== loop_ _atom_site_label _atom_site_occupancy _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_type_symbol _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_disorder_group # #label occ x/a y/b z/c Ueq the typ cal att dis # Cu1 1.00 0.05249(3) 0.34966(3) 0.70653(2) 0.0197(1) Uani Cu ? ? ? N1 1.00 -0.1211(2) 0.3481(2) 0.8489(2) 0.0205(5) Uani N ? ? ? C1 1.00 -0.2658(3) 0.2651(3) 0.8252(3) 0.0258(7) Uani C ? ? ? C2 1.00 -0.3681(3) 0.2964(3) 0.9384(3) 0.0317(8) Uani C ? ? ? C3 1.00 -0.3180(3) 0.4139(3) 1.0773(3) 0.0267(7) Uani C ? ? ? N2 1.00 -0.1703(2) 0.4928(2) 1.1017(2) 0.0206(5) Uani N ? ? ? C4 1.00 -0.0812(2) 0.4565(3) 0.9863(2) 0.0196(6) Uani C ? ? ? N3 1.00 -0.0688(2) 0.2050(2) 0.5153(2) 0.0197(5) Uani N ? ? ? C5 1.00 -0.1570(3) 0.2685(3) 0.4348(3) 0.0255(8) Uani C ? ? ? C6 1.00 -0.2200(3) 0.1645(3) 0.2966(3) 0.0317(9) Uani C ? ? ? C7 1.00 -0.1904(3) -0.0068(3) 0.2425(3) 0.0278(7) Uani C ? ? ? N4 1.00 -0.1049(2) -0.0716(2) 0.3234(2) 0.0218(6) Uani N ? ? ? C8 1.00 -0.0476(2) 0.0360(3) 0.4551(2) 0.0192(6) Uani C ? ? ? O6 1.00 0.2321(2) 0.3867(2) 0.6040(2) 0.0273(5) Uani O ? ? ? Cr1 1.00 0.37848(4) 0.26805(4) 0.50217(4) 0.0217(1) Uani Cr ? ? ? O5 1.00 0.5505(2) 0.3199(3) 0.5925(2) 0.0431(7) Uani O ? ? ? O4 1.00 0.3360(3) 0.0715(2) 0.4581(2) 0.0404(7) Uani O ? ? ? O7 1.00 0.3917(2) 0.3012(3) 0.3417(2) 0.0350(6) Uani O ? ? ? Cr2 1.00 0.22588(4) 0.26893(5) 0.20772(4) 0.0249(1) Uani Cr ? ? ? O1 1.00 0.2967(2) 0.3056(3) 0.0759(2) 0.0407(7) Uani O ? ? ? O2 1.00 0.0813(2) 0.3988(2) 0.2825(2) 0.0349(6) Uani O ? ? ? O3 1.00 0.1581(3) 0.0761(3) 0.1486(3) 0.0512(8) Uani O ? ? ? H1 1.00 -0.2984(3) 0.1827(3) 0.7285(3) 0.06 Uiso H ? C1 ? H2 1.00 -0.4726(3) 0.2384(3) 0.9210(3) 0.06 Uiso H ? C2 ? H3 1.00 -0.3879(3) 0.4386(3) 1.1572(3) 0.06 Uiso H ? C3 ? H5 1.00 -0.1758(3) 0.3885(3) 0.4746(3) 0.06 Uiso H ? C5 ? H6 1.00 -0.2839(3) 0.2099(3) 0.2393(3) 0.06 Uiso H ? C6 ? H7 1.00 -0.2304(3) -0.0808(3) 0.1452(3) 0.06 Uiso H ? C7 ? 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 _atom_site_aniso_type_symbol # #label U11 U22 U33 U23 U13 U12 typ # Cu1 0.0214(2) 0.0195(2) 0.0126(2) 0.0033(1) 0.0028(1) -0.0002(1) Cu N1 0.0211(9) 0.0194(8) 0.0158(8) 0.0051(7) 0.0010(7) 0.0016(7) N C1 0.024(1) 0.025(1) 0.022(1) 0.0076(9) -0.0039(8) -0.0011(8) C C2 0.022(1) 0.035(1) 0.028(1) 0.010(1) -0.0031(9) -0.008(1) C C3 0.022(1) 0.029(1) 0.023(1) 0.0114(9) 0.0036(8) 0.0016(8) C N2 0.0199(9) 0.0220(8) 0.0143(8) 0.0052(7) 0.0004(7) 0.0003(7) N C4 0.020(1) 0.0192(9) 0.0151(9) 0.0068(8) 0.0026(7) 0.0032(8) C N3 0.0213(9) 0.0187(8) 0.0143(8) 0.0050(7) 0.0020(6) 0.0015(7) N C5 0.025(1) 0.022(1) 0.024(1) 0.0107(9) 0.0007(8) 0.0046(8) C C6 0.031(1) 0.031(1) 0.027(1) 0.015(1) -0.0050(9) 0.0023(9) C C7 0.029(1) 0.029(1) 0.020(1) 0.0092(9) -0.0037(9) -0.0007(9) C N4 0.0250(9) 0.0193(9) 0.0154(8) 0.0041(7) -0.0003(7) -0.0007(7) N C8 0.0187(9) 0.0166(9) 0.0176(9) 0.0066(8) 0.0024(7) 0.0009(7) C O6 0.0278(8) 0.0265(8) 0.0215(8) 0.0090(7) 0.0084(6) 0.0038(6) O Cr1 0.0189(2) 0.0228(2) 0.0181(2) 0.0078(2) 0.0029(1) 0.0026(1) Cr O5 0.0261(9) 0.053(1) 0.040(1) 0.0233(9) -0.0062(8) -0.0006(8) O O4 0.047(1) 0.0228(8) 0.041(1) 0.0085(8) 0.0106(9) 0.0037(8) O O7 0.0256(8) 0.047(1) 0.0258(9) 0.0199(8) 0.0051(7) 0.0044(7) O Cr2 0.0252(2) 0.0245(2) 0.0193(2) 0.0083(2) 0.0034(1) 0.0042(1) Cr O1 0.040(1) 0.050(1) 0.0241(9) 0.0165(8) 0.0074(7) 0.0052(9) O O2 0.0295(9) 0.0355(9) 0.0317(9) 0.0151(8) 0.0064(7) 0.0086(7) O O3 0.053(1) 0.028(1) 0.059(1) 0.0152(9) -0.006(1) -0.0032(9) O #=============================================================================== # 10. MOLECULAR GEOMETRY #=============================================================================== _geom_special_details ; The geometric calculation (and the starting release of this CIF file) has been made by a locally modified release of the program PARST of prof. M. Nardelli (we have already adviced prof. Nardelli about it). This release is interactive and has included into one body : I/O interface to other programs, no formated line, logical commands, better output listing and now we are developping a graphical interface PLUTO-like. All computational routines are the original ones. However this release is reserved for internal use of our laboratory only (it is neither public neither commercial release!). ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag # # Complete list of bond lengths for non-H atoms. # Cu1 N1 2.069(2) . . . Cu1 N3 2.014(2) . . . Cu1 O6 1.933(2) . . . Cu1 N2 2.032(2) . 2_567 . Cu1 N4 2.339(2) . 2_556 . Cu1 O2 2.405(2) . 2_566 . N1 C1 1.340(3) . . . N1 C4 1.331(2) . . . C1 C2 1.382(4) . . . C2 C3 1.383(3) . . . C3 N2 1.345(3) . . . N2 C4 1.326(3) . . . N3 C5 1.341(3) . . . N3 C8 1.345(3) . . . C5 C6 1.376(3) . . . C6 C7 1.376(4) . . . C7 N4 1.340(4) . . . N4 C8 1.323(2) . . . O6 Cr1 1.675(2) . . . Cr1 O5 1.596(2) . . . Cr1 O4 1.597(2) . . . Cr1 O7 1.759(2) . . . O7 Cr2 1.803(2) . . . Cr2 O1 1.615(2) . . . Cr2 O2 1.623(2) . . . Cr2 O3 1.603(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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag # # Complete list of bond angles for non-H atoms. # N3 Cu1 O6 90.89(7) . . . . N1 Cu1 O6 169.48(7) . . . . N1 Cu1 N3 99.16(7) . . . . N1 Cu1 N2 81.1(1) . . 2_567 . N3 Cu1 N2 176.8(1) . . 2_567 . O6 Cu1 N2 88.7(1) . . 2_567 . N1 Cu1 N4 86.0(1) . . 2_556 . N3 Cu1 N4 76.6(1) . . 2_556 . O6 Cu1 N4 99.4(1) . . 2_556 . N2 Cu1 N4 106.6(1) 2_567 . 2_556 . N1 Cu1 O2 84.1(1) . . 2_566 . N3 Cu1 O2 91.6(1) . . 2_566 . O6 Cu1 O2 92.6(1) . . 2_566 . N2 Cu1 O2 85.3(1) 2_567 . 2_566 . N4 Cu1 O2 163.2(1) 2_556 . 2_566 . Cu1 N1 C4 112.0(1) . . . . Cu1 N1 C1 131.5(2) . . . . C1 N1 C4 116.5(2) . . . . N1 C1 C2 120.7(2) . . . . C1 C2 C3 118.8(2) . . . . C2 C3 N2 120.3(2) . . . . C3 N2 C4 116.7(2) . . . . N1 C4 N2 126.9(2) . . . . Cu1 N3 C8 119.0(1) . . . . Cu1 N3 C5 123.8(2) . . . . C5 N3 C8 116.8(2) . . . . N3 C5 C6 121.0(2) . . . . C5 C6 C7 118.5(2) . . . . C6 C7 N4 120.9(2) . . . . C7 N4 C8 117.4(2) . . . . N3 C8 N4 125.5(2) . . . . Cu1 O6 Cr1 136.0(1) . . . . O6 Cr1 O7 110.24(8) . . . . O6 Cr1 O4 109.4(1) . . . . O6 Cr1 O5 109.80(9) . . . . O4 Cr1 O7 109.0(1) . . . . O5 Cr1 O7 108.6(1) . . . . O5 Cr1 O4 109.9(1) . . . . Cr1 O7 Cr2 125.1(1) . . . . O7 Cr2 O3 108.8(1) . . . . O7 Cr2 O2 109.64(9) . . . . O7 Cr2 O1 107.71(9) . . . . O2 Cr2 O3 109.9(1) . . . . O1 Cr2 O3 110.5(1) . . . . O1 Cr2 O2 110.3(1) . . . . #=============================================================================== #=============================================================================== data_(3) #=============================================================================== _chemical_name_systematic ; ; _chemical_name_common ? _chemical_formula_moiety '[Cu(bipym)(SO4)].H2O' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C8 H8 Cu N4 O5 S' _chemical_formula_weight 335.8 _chemical_melting_point ? _chemical_compound_source 'chemical synthesis' loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C Carbon 0 32 0.0020 0.0020 Internat_Tables_Vol_IV_Table_2.3.1 H Hydrogen 0 32 0.0000 0.0000 Internat_Tables_Vol_IV_Table_2.3.1 N Nitrogen 0 16 0.0040 0.0030 Internat_Tables_Vol_IV_Table_2.3.1 O Oxygen 0 20 0.0080 0.0060 Internat_Tables_Vol_IV_Table_2.3.1 O Sulphur 0 4 0.1100 0.1240 Internat_Tables_Vol_IV_Table_2.3.1 Cu Copper 0 4 0.2630 1.2660 Internat_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA #=============================================================================== _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 2/m 1' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '1/2+x,-y,1/2+z' _cell_length_a 8.868(2) _cell_length_b 13.752(3) _cell_length_c 9.848(2) _cell_length_alpha 90. _cell_length_beta 116.35(1) _cell_length_gamma 90. _cell_volume 1076.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 295 _cell_measurement_radiation 'Mo K\a' _cell_measurement_wavelength 0.710730 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; ? ; _exptl_crystal_colour green _exptl_crystal_description prismatic _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.23 _exptl_crystal_density_diffrn 2.072 _exptl_crystal_F_000 676 _exptl_absorpt_coefficient_mu 2.249 _exptl_absorpt_correction_type 'semi-empirical' _exptl_absorpt_correction_T_max 0.592 _exptl_absorpt_correction_T_min 0.520 #=============================================================================== # 7. EXPERIMENTAL DATA #=============================================================================== _exptl_special_details ; ? ; _diffrn_special_details ;? ; _diffrn_ambient_temperature 295 _diffrn_radiation_wavelength 0.710730 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus xray_tube' _diffrn_radiation_monochromator 'highly-oriented graphite crystal' _diffrn_measurement_device 'Siemens R3m/V diffractometer' _diffrn_measurement_method \w-2\q _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_av_R_equivalents 0.64 _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 27.0 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_number 2694 _reflns_number_total 2530 _reflns_number_observed 2278 _reflns_observed_criterion >3\s(I) _diffrn_reflns_reduction_process ? _computing_data_collection 'Siemens P3/V,(VMS vers 4.21/V, 1990)' _computing_cell_refinement 'Siemens P3/V' _computing_data_reduction 'Siemens SHELXTL-PLUS,(VMS vers 4.21/V , 1990)' _computing_structure_solution 'Siemens SHELXTL-PLUS' _computing_structure_refinement 'Siemens SHELXTL-PLUS' _computing_molecular_graphics 'Siemens XP' _computing_publication_material 'Siemens SHELXTL-PLUS and PARST' #=============================================================================== # 8. REFINEMENT DATA #=============================================================================== _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '1/(\s^2^(F)+ 0.0004*F^2^))' _refine_ls_hydrogen_treatment '"riding model" with fixed isotropic U' _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_number_reflns 2278 _refine_ls_number_parameters 273 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 3.21 _refine_ls_R_factor_obs 2.72 _refine_ls_wR_factor_all 3.69 _refine_ls_wR_factor_obs 3.57 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.34 _refine_ls_shift/esd_mean 0.000 _refine_ls_shift/esd_max 0.002 _refine_diff_density_min -0.49 _refine_diff_density_max 0.39 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS #=============================================================================== loop_ _atom_site_label _atom_site_occupancy _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_type_symbol _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_disorder_group # #label occ x/a y/b z/c Ueq the typ cal att dis # Cu1 1.00 0. 0.15103(4) 0. 0.0173(2) Uani Cu ? ? ? Cu2 1.00 0.08198(8) 0.35163(4) 0.52887(7) 0.0171(2) Uani Cu ? ? ? N1 1.00 -0.1213(6) 0.1665(3) 0.1247(6) 0.020(2) Uani N ? ? ? N2 1.00 -0.0976(6) 0.2332(3) 0.3561(6) 0.022(2) Uani N ? ? ? N3 1.00 0.1661(6) 0.2431(3) 0.1684(6) 0.018(1) Uani N ? ? ? N4 1.00 0.2014(6) 0.3156(3) 0.3969(5) 0.015(1) Uani N ? ? ? N5 1.00 0.1339(6) 0.1556(3) -0.1270(6) 0.018(2) Uani N ? ? ? N6 1.00 0.1769(6) 0.2349(3) -0.3204(5) 0.018(1) Uani N ? ? ? N7 1.00 -0.0997(6) 0.2965(3) -0.1571(6) 0.022(2) Uani N ? ? ? N8 1.00 -0.0538(7) 0.3668(3) -0.3553(6) 0.020(2) Uani N ? ? ? S1 1.00 -0.2280(2) -0.0208(1) -0.2015(2) 0.0191(4) Uani S ? ? ? O1 1.00 -0.1872(5) 0.0852(3) -0.1644(5) 0.023(1) Uani O ? ? ? O2 1.00 -0.3459(6) -0.0237(3) -0.3620(5) 0.027(1) Uani O ? ? ? O3 1.00 -0.3054(7) -0.0584(3) -0.1086(6) 0.038(2) Uani O ? ? ? O4 1.00 -0.0743(6) -0.0725(3) -0.1728(6) 0.039(2) Uani O ? ? ? S2 1.00 -0.1524(2) 0.4698(1) 0.2441(2) 0.0177(4) Uani S ? ? ? O5 1.00 -0.0137(5) 0.4662(3) 0.4056(4) 0.021(1) Uani O ? ? ? O6 1.00 -0.1795(6) 0.5743(3) 0.2060(5) 0.027(1) Uani O ? ? ? O7 1.00 -0.0945(6) 0.4222(3) 0.1445(5) 0.030(1) Uani O ? ? ? O8 1.00 -0.3029(6) 0.4252(3) 0.2393(6) 0.037(2) Uani O ? ? ? O9 1.00 -0.0090(7) 0.6876(3) 0.4732(6) 0.038(2) Uani O ? ? ? O10 1.00 0.0929(7) -0.1954(3) 0.0787(6) 0.038(2) Uani O ? ? ? C4 1.00 -0.0443(7) 0.2178(3) 0.2516(6) 0.015(1) Uiso C ? ? ? C10 1.00 0.3316(7) 0.0926(4) -0.2090(6) 0.024(1) Uiso C ? ? ? C5 1.00 0.1174(6) 0.2613(3) 0.2745(6) 0.013(1) Uiso C ? ? ? C11 1.00 0.2919(7) 0.1684(4) -0.3108(6) 0.019(1) Uiso C ? ? ? C8 1.00 0.3481(8) 0.3544(4) 0.4162(7) 0.022(1) Uiso C ? ? ? C3 1.00 -0.2448(7) 0.1919(4) 0.3299(6) 0.022(1) Uiso C ? ? ? C12 1.00 0.1019(6) 0.2258(3) -0.2299(6) 0.015(1) Uiso C ? ? ? C13 1.00 -0.0253(6) 0.3004(4) -0.2480(6) 0.015(1) Uiso C ? ? ? C6 1.00 0.3102(7) 0.2837(4) 0.1847(6) 0.019(1) Uiso C ? ? ? C14 1.00 -0.2184(7) 0.3629(4) -0.1819(6) 0.023(1) Uiso C ? ? ? C9 1.00 0.2481(7) 0.0880(4) -0.1166(6) 0.022(1) Uiso C ? ? ? C15 1.00 -0.2566(7) 0.4337(4) -0.2925(6) 0.024(1) Uiso C ? ? ? C7 1.00 0.4052(8) 0.3408(4) 0.3063(6) 0.023(1) Uiso C ? ? ? C16 1.00 -0.1699(7) 0.4346(4) -0.3757(6) 0.025(1) Uiso C ? ? ? C2 1.00 -0.3340(8) 0.1375(4) 0.2029(7) 0.026(1) Uiso C ? ? ? C1 1.00 -0.2676(8) 0.1248(4) 0.1022(6) 0.023(1) Uiso C ? ? ? H1W 1.00 0.093(5) 0.652(5) 0.530(6) 0.06 Uiso H ? O9 ? H2W 1.00 -0.047(8) 0.658(5) 0.376(3) 0.06 Uiso H ? O9 ? H3W 1.00 0.184(6) -0.154(4) 0.144(6) 0.06 Uiso H ? O10 ? H4W 1.00 0.049(9) -0.156(4) -0.011(5) 0.06 Uiso H ? O10 ? H1 1.00 -0.3266(8) 0.0861(4) 0.0129(6) 0.06 Uiso H ? C1 ? H2 1.00 -0.4390(8) 0.1081(4) 0.1863(7) 0.06 Uiso H ? C2 ? H3 1.00 -0.2885(7) 0.2013(4) 0.4023(6) 0.06 Uiso H ? C3 ? H6 1.00 0.3477(7) 0.2724(4) 0.1083(6) 0.06 Uiso H ? C6 ? H7 1.00 0.5080(8) 0.3704(4) 0.3171(6) 0.06 Uiso H ? C7 ? H8 1.00 0.4128(8) 0.3923(4) 0.5051(7) 0.06 Uiso H ? C8 ? H9 1.00 0.2714(7) 0.0352(4) -0.0462(6) 0.06 Uiso H ? C9 ? H10 1.00 0.4147(7) 0.0450(4) -0.2001(6) 0.06 Uiso H ? C10 ? H11 1.00 0.3280(7) 0.1881(4) -0.3852(6) 0.06 Uiso H ? C11 ? H14 1.00 -0.2768(7) 0.3622(4) -0.1199(6) 0.06 Uiso H ? C14 ? H15 1.00 -0.3425(7) 0.4810(4) -0.3085(6) 0.06 Uiso H ? C15 ? H16 1.00 -0.1702(7) 0.4742(4) -0.4561(6) 0.06 Uiso H ? C16 ? 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 _atom_site_aniso_type_symbol # #label U11 U22 U33 U23 U13 U12 typ # Cu1 0.0179(3) 0.0181(3) 0.0125(3) -0.0029(3) 0.0085(3) -0.0037(3) Cu Cu2 0.0203(3) 0.0153(3) 0.0127(3) 0.0024(3) 0.0103(3) 0.0020(3) Cu N1 0.019(2) 0.019(2) 0.016(2) -0.003(2) 0.006(2) -0.002(2) N N2 0.025(2) 0.020(2) 0.018(2) -0.002(2) 0.014(2) -0.005(2) N N3 0.016(2) 0.016(2) 0.018(2) 0.000(2) 0.010(2) 0.002(2) N N4 0.017(2) 0.015(2) 0.011(2) -0.001(2) 0.007(2) 0.001(2) N N5 0.017(2) 0.015(2) 0.019(3) -0.001(2) 0.010(2) 0.002(2) N N6 0.019(2) 0.016(2) 0.015(2) -0.002(2) 0.011(2) 0.000(2) N N7 0.021(2) 0.021(2) 0.020(2) -0.003(2) 0.013(2) -0.001(2) N N8 0.024(2) 0.019(2) 0.014(2) 0.003(2) 0.010(2) 0.001(2) N S1 0.0204(6) 0.0179(6) 0.0143(6) -0.0026(5) 0.0076(5) -0.0011(5) S O1 0.026(2) 0.017(2) 0.019(2) -0.001(1) 0.007(2) -0.003(2) O O2 0.035(2) 0.020(2) 0.013(2) -0.004(1) -0.001(2) -0.007(2) O O3 0.045(3) 0.031(2) 0.032(2) -0.003(2) 0.026(2) -0.006(2) O O4 0.028(2) 0.042(3) 0.036(2) -0.008(2) 0.011(2) 0.012(2) O S2 0.0176(6) 0.0157(6) 0.0150(6) 0.0029(5) 0.0063(5) -0.0004(5) S O5 0.024(2) 0.018(2) 0.014(2) 0.005(1) 0.003(2) 0.003(2) O O6 0.031(2) 0.022(2) 0.021(2) 0.006(2) 0.008(2) 0.003(2) O O7 0.036(2) 0.030(2) 0.016(2) 0.000(2) 0.010(2) 0.007(2) O O8 0.025(2) 0.040(2) 0.037(3) 0.010(2) 0.014(2) -0.006(2) O O9 0.045(3) 0.032(2) 0.027(2) -0.001(2) 0.016(2) 0.009(2) O O10 0.044(3) 0.030(2) 0.027(2) -0.005(2) 0.012(2) -0.004(2) O #=============================================================================== # 10. MOLECULAR GEOMETRY #=============================================================================== _geom_special_details ; The geometric calculation (and the starting release of this CIF file) has been made by a locally modified release of the program PARST of prof. M. Nardelli (we have already adviced prof. Nardelli about it). This release is interactive and has included into one body : I/O interface to other programs, no formated line, logical commands, better output listing and now we are developping a graphical interface PLUTO-like. All computational routines are the original ones. However this release is reserved for internal use of our laboratory only (it is neither public neither commercial release!). ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag # # Complete list of bond lengths for non-H atoms. # Cu1 N1 1.971(7) . . . Cu1 N3 2.087(4) . . . Cu1 N5 2.073(7) . . . Cu1 N7 2.442(5) . . . Cu1 O1 1.952(4) . . . Cu1 O2 2.266(4) . 2_555 . Cu2 N2 2.383(4) . . . Cu2 N4 2.068(6) . . . Cu2 O5 1.940(4) . . . Cu2 N6 2.093(4) . 1_556 . Cu2 N8 2.003(7) . 1_556 . Cu2 O6 2.298(4) . 2_565 . N1 C4 1.330(7) . . . N1 C1 1.344(9) . . . N2 C4 1.327(9) . . . N2 C3 1.339(8) . . . N3 C5 1.320(9) . . . N3 C6 1.338(8) . . . N4 C5 1.330(6) . . . N4 C8 1.339(8) . . . N5 C12 1.336(7) . . . N5 C9 1.345(8) . . . N6 C11 1.342(8) . . . N6 C12 1.333(9) . . . N7 C13 1.33(1) . . . N7 C14 1.332(8) . . . N8 C13 1.334(7) . . . N8 C16 1.337(8) . . . S1 O1 1.507(4) . . . S1 O2 1.458(4) . . . S1 O3 1.461(7) . . . S1 O4 1.450(6) . . . S2 O5 1.519(4) . . . S2 O6 1.478(4) . . . S2 O7 1.449(6) . . . S2 O8 1.451(6) . . . C4 C5 1.475(8) . . . C10 C11 1.379(8) . . . C10 C9 1.41(1) . . . C8 C7 1.40(1) . . . C3 C2 1.368(8) . . . C12 C13 1.476(8) . . . C6 C7 1.366(7) . . . C14 C15 1.386(8) . . . C15 C16 1.35(1) . . . C2 C1 1.37(1) . . . 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag # # Complete list of bond angles for non-H atoms. # N7 Cu1 O1 85.3(2) . . . . N5 Cu1 O1 91.0(2) . . . . N5 Cu1 N7 74.7(2) . . . . N3 Cu1 O1 168.8(2) . . . . N3 Cu1 N7 86.3(2) . . . . N3 Cu1 N5 94.0(2) . . . . N1 Cu1 O1 93.9(2) . . . . N1 Cu1 N7 99.4(2) . . . . N1 Cu1 N5 172.0(2) . . . . N1 Cu1 N3 80.1(2) . . . . N3 Cu1 O2 91.8(2) . . 2_555 . N1 Cu1 O2 93.5(2) . . 2_555 . N3 Cu1 O2 88.1(1) . . 2_555 . N5 Cu1 O2 91.8(2) . . 2_555 . N7 Cu1 O2 164.9(2) . . 2_555 . N4 Cu2 O5 90.3(2) . . . . N2 Cu2 O5 98.1(2) . . . . N2 Cu2 N4 75.8(2) . . . . N2 Cu2 N6 85.0(1) . . 1_556 . N4 Cu2 N6 96.0(2) . . 1_556 . O5 Cu2 N6 173.5(2) . . 1_556 . N2 Cu2 N8 95.6(2) . . 1_556 . N4 Cu2 N8 170.9(2) . . 1_556 . O5 Cu2 N8 93.7(2) . . 1_556 . N6 Cu2 N8 80.2(2) 1_556 . 1_556 . N2 Cu2 O6 95.6(2) . . 2_565 . N4 Cu2 O6 91.6(2) . . 2_565 . O5 Cu2 O6 96.6(1) . . 2_565 . N6 Cu2 O6 81.8(2) . . 2_565 . N8 Cu2 O6 96.0(2) 1_556 . 2_565 . Cu1 N1 C1 127.2(5) . . . . Cu1 N1 C4 116.6(4) . . . . C4 N1 C1 115.9(5) . . . . Cu2 N2 C3 135.5(4) . . . . Cu2 N2 C4 107.9(3) . . . . C4 N2 C3 115.8(6) . . . . Cu1 N3 C6 130.4(4) . . . . Cu1 N3 C5 112.4(4) . . . . C5 N3 C6 117.2(5) . . . . Cu2 N4 C8 123.5(5) . . . . Cu2 N4 C5 117.8(4) . . . . C5 N4 C8 118.1(5) . . . . Cu1 N5 C9 123.1(4) . . . . Cu1 N5 C12 119.6(4) . . . . C12 N5 C9 117.2(5) . . . . C11 N6 C12 118.6(5) . . . . Cu1 N7 C14 135.4(4) . . . . Cu1 N7 C13 108.2(3) . . . . C13 N7 C14 115.9(6) . . . . C13 N8 C16 117.3(5) . . . . O3 S1 O4 111.5(4) . . . . O2 S1 O4 110.9(3) . . . . O2 S1 O3 111.1(3) . . . . O1 S1 O4 108.9(3) . . . . O1 S1 O3 108.7(3) . . . . O1 S1 O2 105.6(2) . . . . Cu1 O1 S1 132.3(3) . . . . O7 S2 O8 112.6(3) . . . . O6 S2 O8 111.1(3) . . . . O6 S2 O7 109.5(3) . . . . O5 S2 O8 109.0(3) . . . . O5 S2 O7 109.2(3) . . . . O5 S2 O6 105.2(2) . . . . Cu2 O5 S2 127.4(2) . . . . N1 C4 N2 127.0(5) . . . . N2 C4 C5 118.3(5) . . . . N1 C4 C5 114.7(5) . . . . C11 C10 C9 117.8(5) . . . . N4 C5 C4 118.8(5) . . . . N3 C5 C4 116.1(5) . . . . N3 C5 N4 125.1(5) . . . . N6 C11 C10 120.5(5) . . . . N4 C8 C7 120.0(6) . . . . N2 C3 C2 121.8(6) . . . . N5 C12 N6 125.0(5) . . . . N6 C12 C13 115.8(5) . . . . N5 C12 C13 119.2(4) . . . . N8 C13 C12 115.9(4) . . . . N7 C13 C12 118.2(5) . . . . N7 C13 N8 125.9(5) . . . . N3 C6 C7 122.0(5) . . . . N7 C14 C15 121.6(5) . . . . N5 C9 C10 120.9(6) . . . . C14 C15 C16 118.5(5) . . . . C8 C7 C6 117.5(5) . . . . N8 C16 C15 120.7(6) . . . . C3 C2 C1 118.1(6) . . . . N1 C1 C2 121.3(7) . . . . #===============================================================================