# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1403 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 I am sending the cif file of the paper 8/00569B: "Novel sheetlike manganese (II) networks. Synthesis and structure of [Mn(bpe)(NCS)2(CH3OH)2} and [Mn(bpe)(NCS)2(CH3OH)2]bpe [bpe = 1,2-trans-(4-pyridyl)ethene]" The compounds have been identified in the paper with number 1 and 2. (in this cif file they have been called data_(1) and data_(2)). For further comunications or informations contact me at this E-mail address: demunno@unical.it Yours sincerely Giovanni De Munno ; #======================================================================= # 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 '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 ; Novel sheetlike manganese (II) networks. Synthesis and structure of [Mn(bpe)(NCS)2(CH3OH)2} and [Mn(bpe)(NCS)2(CH3OH)2]bpe [bpe = 1,2-trans-(4-pyridyl)ethene] ; 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 ; 'Donatella Armentano' ; 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 ; 'Jose' Antonio Real' ; Departament de Quimica Inorganica Facultat de Quimica Dr. Moliner 50 E-46100 Burjassot, Valencia Spain ; #======================================================================= # 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 '[Mn(bpe)(NCS)2(CH3OH)2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C16 H18 Mn N4 O2 S2' _chemical_formula_weight 417.4 _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 18 0.0000 0.0000 Internat_Tables_Vol_IV_Table_2.3.1 N Nitrogen 0 4 0.0040 0.0030 Internat_Tables_Vol_IV_Table_2.3.1 O Oxygen 0 2 0.0080 0.0060 Internat_Tables_Vol_IV_Table_2.3.1 S Sulfur 0 2 0.1100 0.1240 Internat_Tables_Vol_IV_Table_2.3.1 Mn Manganese 0 1 0.2950 0.7290 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' '-x,1/2+y,1/2-z' '-x,-y,-z' 'x,1/2-y,1/2+z' _cell_length_a 10.382(4) _cell_length_b 13.482(7) _cell_length_c 14.038(4) _cell_length_alpha 90. _cell_length_beta 91.71(3) _cell_length_gamma 90. _cell_volume 1964.0(14) _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 'pale yellow' _exptl_crystal_description parallelepiped _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.26 _exptl_crystal_density_diffrn 1.412 _exptl_crystal_F_000 860 _exptl_absorpt_coefficient_mu 9.0073 _exptl_absorpt_correction_type ? #======================================================================= # 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 ? _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 25.0 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_number 7714 _reflns_number_total 3479 _reflns_number_observed 954 _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)+ 0.0007*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 954 _refine_ls_number_parameters 156 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_R_factor_all 24.80 _refine_ls_R_factor_obs 8.61 _refine_ls_wR_factor_all 17.57 _refine_ls_wR_factor_obs 10.33 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.04 _refine_ls_shift/esd_mean 0.000 _refine_ls_shift/esd_max 0.002 _refine_diff_density_min -0.43 _refine_diff_density_max 0.68 #======================================================================= # 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 # Mn1 1.00 0.0125(4) 0.2341(1) 0.9175(1) 0.054(1) Uani Mn ? ? ? N1 1.00 0.017(2) 0.2414(8) 0.7521(6) 0.062(7) Uani N ? ? ? N2 1.00 0.013(2) 0.2218(8) 0.0806(6) 0.064(9) Uani N ? ? ? C13 1.00 0.189(3) 0.436(1) 0.9206(7) 0.09(1) Uani C ? ? ? S1 1.00 0.2763(9) 0.5376(3) 0.9101(3) 0.093(4) Uani S ? ? ? C14 1.00 -0.204(3) 0.054(1) 0.9038(8) 0.06(1) Uani C ? ? ? S2 1.00 -0.3237(9) -0.0261(3) 0.9016(3) 0.076(3) Uani S ? ? ? O1 1.00 -0.158(2) 0.3410(7) 0.9208(6) 0.073(7) Uani O ? ? ? C15 1.00 -0.180(2) 0.410(1) 0.8487(9) 0.08(1) Uani C ? ? ? O2 1.00 0.186(2) 0.1331(8) 0.9219(7) 0.081(9) Uani O ? ? ? C16 1.00 0.255(3) 0.096(1) 0.849(1) 0.12(2) Uani C ? ? ? C6 1.00 0.041(2) 0.262(1) 0.4463(8) 0.047(4) Uiso C ? ? ? N3 1.00 0.148(3) 0.362(1) 0.9284(8) 0.064(4) Uiso N ? ? ? C7 1.00 -0.008(2) 0.199(1) 0.385(1) 0.061(4) Uiso C ? ? ? C4 1.00 0.113(2) 0.308(1) 0.6105(9) 0.058(4) Uiso C ? ? ? C8 1.00 0.000(2) 0.210(1) 0.2804(8) 0.049(4) Uiso C ? ? ? C9 1.00 -0.025(2) 0.130(1) 0.2233(9) 0.055(4) Uiso C ? ? ? C2 1.00 -0.066(2) 0.191(1) 0.5975(9) 0.059(4) Uiso C ? ? ? C10 1.00 -0.025(2) 0.138(1) 0.1255(9) 0.055(4) Uiso C ? ? ? N4 1.00 -0.124(2) 0.1100(9) 0.9085(8) 0.054(4) Uiso N ? ? ? C1 1.00 -0.065(2) 0.1871(9) 0.6956(9) 0.048(4) Uiso C ? ? ? C11 1.00 0.043(2) 0.298(1) 0.1383(9) 0.052(4) Uiso C ? ? ? C5 1.00 0.099(3) 0.300(1) 0.708(1) 0.063(4) Uiso C ? ? ? C12 1.00 0.045(2) 0.2935(9) 0.2359(8) 0.048(4) Uiso C ? ? ? C3 1.00 0.028(2) 0.2503(9) 0.5532(8) 0.038(3) Uiso C ? ? ? H6 1.00 0.076(2) 0.322(1) 0.4227(8) 0.06 Uiso H ? C6 ? H7 1.00 -0.041(2) 0.138(1) 0.409(1) 0.06 Uiso H ? C7 ? H9 1.00 -0.042(2) 0.067(1) 0.2512(9) 0.06 Uiso H ? C9 ? H10 1.00 -0.053(2) 0.083(1) 0.0870(9) 0.06 Uiso H ? C10 ? H11 1.00 0.068(2) 0.359(1) 0.1083(9) 0.06 Uiso H ? C11 ? H12 1.00 0.075(2) 0.3486(9) 0.2737(8) 0.06 Uiso H ? C12 ? H1 1.00 -0.126(2) 0.1446(9) 0.7254(9) 0.06 Uiso H ? C1 ? H2 1.00 -0.123(2) 0.150(1) 0.5591(9) 0.06 Uiso H ? C2 ? H1O 1.00 -0.149(2) 0.3739(7) 0.9721(6) 0.06 Uiso H ? O1 ? H4 1.00 0.180(2) 0.348(1) 0.5841(9) 0.06 Uiso H ? C4 ? H15A 1.00 -0.255(2) 0.449(1) 0.8622(9) 0.06 Uiso H ? C15 ? H15B 1.00 -0.106(2) 0.453(1) 0.8458(9) 0.06 Uiso H ? C15 ? H15C 1.00 -0.193(2) 0.377(1) 0.7888(9) 0.06 Uiso H ? C15 ? H2O 1.00 0.162(2) 0.0824(8) 0.9526(7) 0.06 Uiso H ? O2 ? H5 1.00 0.145(3) 0.347(1) 0.748(1) 0.06 Uiso H ? C5 ? H16A 1.00 0.324(3) 0.054(1) 0.874(1) 0.06 Uiso H ? C16 ? H16B 1.00 0.198(3) 0.057(1) 0.809(1) 0.06 Uiso H ? C16 ? H16C 1.00 0.291(3) 0.149(1) 0.814(1) 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 # Mn1 0.089(4) 0.051(1) 0.0214(8) 0.0008(8) 0.006(1) -0.009(3) Mn N1 0.11(2) 0.049(6) 0.028(4) -0.002(4) 0.016(8) -0.01(1) N N2 0.12(3) 0.050(6) 0.023(4) -0.003(4) 0.010(8) 0.02(1) N C13 0.17(4) 0.071(9) 0.015(5) 0.003(5) 0.00(1) 0.01(2) C S1 0.15(1) 0.054(2) 0.075(3) -0.008(2) 0.040(4) -0.021(5) S C14 0.11(3) 0.042(8) 0.035(6) -0.009(6) -0.02(1) 0.02(2) C S2 0.106(8) 0.057(3) 0.066(2) 0.005(2) -0.015(4) -0.010(5) S O1 0.11(2) 0.057(6) 0.054(5) -0.007(4) -0.004(8) 0.01(1) O C15 0.07(2) 0.10(1) 0.062(8) 0.012(8) -0.01(1) 0.06(2) C O2 0.10(2) 0.078(7) 0.062(6) 0.011(5) 0.021(9) 0.02(1) O C16 0.20(4) 0.09(1) 0.059(9) -0.014(8) 0.03(2) 0.02(2) C #======================================================================= # 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. # Mn1 N1 2.326(9) . . . Mn1 O1 2.28(2) . . . Mn1 O2 2.26(2) . . . Mn1 N3 2.23(2) . . . Mn1 N4 2.20(2) . . . Mn1 N2 2.30(1) . 3_555 . N1 C1 1.36(2) . . . N2 C5 1.33(3) . . . N2 C10 1.36(2) . . . N2 C11 1.34(2) . . . C13 S1 1.65(2) . . . C13 N3 1.09(3) . . . C14 S2 1.65(2) . . . C14 N4 1.11(3) . . . O1 C15 1.39(2) . . . O2 C16 1.36(2) . . . C6 C7 1.29(2) . . . C6 C3 1.52(2) . . . C7 C8 1.49(2) . . . C4 C5 1.39(2) . . . C4 C3 1.41(2) . . . C8 C9 1.36(2) . . . C8 C12 1.37(2) . . . C9 C10 1.38(2) . . . C2 C1 1.38(2) . . . C2 C3 1.43(3) . . . C11 C12 1.37(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 Mn1 N4 178.7(6) . . . . O2 Mn1 N4 93.3(6) . . . . O2 Mn1 N3 87.9(6) . . . . O1 Mn1 N4 89.0(5) . . . . O1 Mn1 N3 89.9(6) . . . . O1 Mn1 O2 176.6(5) . . . . N1 Mn1 N4 90.4(4) . . . . N1 Mn1 N3 90.2(4) . . . . N1 Mn1 O2 90.7(4) . . . . N1 Mn1 O1 91.9(4) . . . . N1 Mn1 N2 177.8(5) . . 3_555 . N3 Mn1 N2 90.2(5) . . 3_555 . N4 Mn1 N2 89.1(5) . . 3_555 . O1 Mn1 N2 90.3(5) . . 3_555 . O2 Mn1 N2 87.1(5) . . 3_555 . Mn1 N1 C5 121.5(8) . . . . Mn1 N1 C1 121.9(7) . . . . C1 N1 C5 117(1) . . . . C10 N2 C11 115(1) . . . . C10 N2 Mn1 122.8(8) . . 3_555 . C11 N2 Mn1 122.7(8) . . 3_555 . S1 C13 N3 170(2) . . . . S2 C14 N4 177(2) . . . . Mn1 O1 C15 121.4(9) . . . . Mn1 O2 C16 130(1) . . . . C7 C6 C3 123(1) . . . . Mn1 N3 C13 161(2) . . . . C6 C7 C8 124(1) . . . . C5 C4 C3 116(1) . . . . C7 C8 C12 124(1) . . . . C7 C8 C9 119(1) . . . . C9 C8 C12 116(1) . . . . C8 C9 C10 121(1) . . . . C1 C2 C3 118(1) . . . . N2 C10 C9 122(1) . . . . Mn1 N4 C14 173(1) . . . . N1 C1 C2 124(1) . . . . N2 C11 C12 124(1) . . . . N1 C5 C4 126(1) . . . . C8 C12 C11 120(1) . . . . C4 C3 C2 119(1) . . . . C6 C3 C2 125(1) . . . . C6 C3 C4 116(1) . . . . #======================================================================= #======================================================================= data_(2) _chemical_name_systematic ; ; _chemical_name_common ? _chemical_formula_moiety '[Mn(bpe)(NCS)2(CH3OH)2.bpe' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C28 H28 Mn N6 O2 S2' _chemical_formula_weight 599.6 _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 28 0.0020 0.0020 Internat_Tables_Vol_IV_Table_2.3.1 H Hydrogen 0 28 0.0000 0.0000 Internat_Tables_Vol_IV_Table_2.3.1 N Nitrogen 0 6 0.0040 0.0030 Internat_Tables_Vol_IV_Table_2.3.1 O Oxygen 0 2 0.0080 0.0060 Internat_Tables_Vol_IV_Table_2.3.1 S Sulfur 0 2 0.1100 0.1240 Internat_Tables_Vol_IV_Table_2.3.1 Mn Manganese 0 1 0.2950 0.7290 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' '-x,1/2+y,1/2-z' '-x,-y,-z' 'x,1/2-y,1/2+z' _cell_length_a 7.356(4) _cell_length_b 17.096(6) _cell_length_c 12.310(5) _cell_length_alpha 90. _cell_length_beta 93.66(4) _cell_length_gamma 90. _cell_volume 1544.9(12) _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 yellow _exptl_crystal_description parallelepiped _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.22 _exptl_crystal_density_diffrn 1.289 _exptl_crystal_F_000 622 _exptl_absorpt_coefficient_mu 5.9600 _exptl_absorpt_correction_type ? #======================================================================= # 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 ? _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 25.0 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_number 3360 _reflns_number_total 2742 _reflns_number_observed 1498 _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)+ 0.0050*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 1498 _refine_ls_number_parameters 178 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_R_factor_all 12.09 _refine_ls_R_factor_obs 7.01 _refine_ls_wR_factor_all 13.09 _refine_ls_wR_factor_obs 9.91 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.19 _refine_ls_shift/esd_mean 0.000 _refine_ls_shift/esd_max 0.001 _refine_diff_density_min -1.25 _refine_diff_density_max 0.46 #======================================================================= # 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 # Mn1 1.00 0. 0. 0. 0.0451(5) Uani Mn ? ? ? S1 1.00 -0.3630(3) 0.2305(1) 0.0897(3) 0.114(1) Uani S ? ? ? O1 1.00 -0.1671(6) -0.0835(3) 0.0852(4) 0.060(2) Uani O ? ? ? C6 1.00 -0.4960(8) -0.0268(4) -0.4609(5) 0.048(2) Uani C ? ? ? C5 1.00 -0.283(1) -0.0720(4) -0.1838(6) 0.056(2) Uani C ? ? ? N3 1.00 -0.1495(8) 0.1004(4) 0.0551(5) 0.062(2) Uani N ? ? ? N1 1.00 -0.1984(8) -0.0061(3) -0.1517(4) 0.054(2) Uani N ? ? ? C2 1.00 -0.3153(8) 0.0529(4) -0.3179(5) 0.050(2) Uani C ? ? ? C3 1.00 -0.3999(8) -0.0175(4) -0.3531(5) 0.044(2) Uani C ? ? ? C4 1.00 -0.3859(9) -0.0794(4) -0.2823(6) 0.052(2) Uani C ? ? ? C13 1.00 -0.2390(9) 0.1541(4) 0.0678(6) 0.057(3) Uani C ? ? ? C1 1.00 -0.2187(9) 0.0557(4) -0.2192(5) 0.052(2) Uani C ? ? ? C12 1.00 0.027(1) -0.4777(4) 0.0417(6) 0.065(3) Uani C ? ? ? N2 1.00 -0.086(1) -0.2364(4) 0.0878(7) 0.087(3) Uani N ? ? ? C7 1.00 0.014(1) -0.2778(5) 0.1589(9) 0.090(4) Uani C ? ? ? C9 1.00 -0.0098(9) -0.3936(5) 0.0532(7) 0.065(3) Uani C ? ? ? C10 1.00 -0.116(1) -0.3517(5) -0.0229(8) 0.084(4) Uani C ? ? ? C11 1.00 -0.148(1) -0.2741(5) -0.002(1) 0.096(4) Uani C ? ? ? C8 1.00 0.057(1) -0.3551(5) 0.1456(8) 0.078(3) Uani C ? ? ? C14 1.00 -0.340(1) -0.0738(5) 0.1269(9) 0.100(4) Uani C ? ? ? H1O 1.00 -0.1734(6) -0.1262(3) 0.0497(4) 0.06 Uiso H ? O1 ? H4 1.00 -0.4478(9) -0.1275(4) -0.3009(6) 0.06 Uiso H ? C4 ? H7 1.00 0.059(1) -0.2516(5) 0.2241(9) 0.06 Uiso H ? C7 ? H5 1.00 -0.271(1) -0.1164(4) -0.1363(6) 0.06 Uiso H ? C5 ? H2 1.00 -0.3269(8) 0.0985(4) -0.3633(5) 0.06 Uiso H ? C2 ? H10 1.00 -0.163(1) -0.3770(5) -0.0882(8) 0.06 Uiso H ? C10 ? H1 1.00 -0.1618(9) 0.1040(4) -0.1962(5) 0.06 Uiso H ? C1 ? H11 1.00 -0.224(1) -0.2449(5) -0.054(1) 0.06 Uiso H ? C11 ? H6 1.00 -0.5596(8) -0.0751(4) -0.4749(5) 0.06 Uiso H ? C6 ? H8 1.00 0.135(1) -0.3825(5) 0.1987(8) 0.06 Uiso H ? C8 ? H12 1.00 0.098(1) -0.5021(4) 0.1006(6) 0.06 Uiso H ? C12 ? H14C 1.00 -0.378(1) -0.1216(5) 0.1597(9) 0.06 Uiso H ? C14 ? H14A 1.00 -0.333(1) -0.0330(5) 0.1805(9) 0.06 Uiso H ? C14 ? H14B 1.00 -0.426(1) -0.0597(5) 0.0684(9) 0.06 Uiso H ? C14 ? 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 # Mn1 0.0554(8) 0.0443(9) 0.0353(7) -0.0063(6) -0.0085(5) 0.0103(6) Mn S1 0.089(2) 0.056(1) 0.196(3) -0.015(2) 0.029(2) 0.022(1) S O1 0.064(3) 0.054(3) 0.062(3) -0.003(2) 0.007(2) 0.009(2) O C6 0.048(3) 0.058(4) 0.038(3) -0.000(3) -0.005(3) 0.001(3) C C5 0.073(4) 0.047(4) 0.047(4) 0.005(3) -0.010(3) -0.001(4) C N3 0.067(4) 0.061(4) 0.058(4) -0.016(3) -0.004(3) 0.015(3) N N1 0.068(3) 0.051(3) 0.042(3) -0.002(3) -0.006(2) 0.007(3) N C2 0.057(4) 0.053(4) 0.040(3) 0.011(3) -0.006(3) 0.009(3) C C3 0.042(3) 0.054(4) 0.036(3) -0.001(3) -0.002(3) 0.003(3) C C4 0.061(4) 0.050(4) 0.045(4) -0.002(3) -0.004(3) -0.003(3) C C13 0.054(4) 0.050(4) 0.067(5) -0.007(3) 0.000(3) -0.005(3) C C1 0.057(4) 0.048(4) 0.052(4) -0.003(3) -0.013(3) 0.000(3) C C12 0.065(4) 0.054(5) 0.076(5) 0.015(4) 0.008(4) 0.001(4) C N2 0.083(5) 0.052(4) 0.125(7) 0.005(5) 0.018(5) 0.002(4) N C7 0.104(7) 0.063(6) 0.104(8) -0.006(5) 0.013(6) -0.002(5) C C9 0.050(4) 0.054(5) 0.091(6) 0.013(4) 0.018(4) 0.003(3) C C10 0.084(6) 0.061(5) 0.105(7) 0.006(5) -0.009(5) 0.003(5) C C11 0.088(6) 0.062(6) 0.14(1) 0.032(6) -0.005(6) 0.014(5) C C8 0.080(5) 0.064(5) 0.088(6) 0.012(5) 0.006(5) 0.007(4) C C14 0.102(7) 0.080(7) 0.119(8) -0.016(6) 0.037(6) 0.008(5) C #======================================================================= # 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. # Mn1 O1 2.194(5) . . . Mn1 N3 2.170(6) . . . Mn1 N1 2.298(5) . . . S1 C13 1.625(8) . . . O1 C14 1.41(1) . . . C6 C3 1.472(8) . . . C6 C6 1.33(1) . 3_454 . C5 N1 1.336(9) . . . C5 C4 1.392(9) . . . N3 C13 1.146(9) . . . N1 C1 1.345(9) . . . C2 C3 1.411(9) . . . C2 C1 1.368(9) . . . C3 C4 1.371(9) . . . C12 C9 1.47(1) . . . C12 C12 1.32(1) . 3_545 . N2 C7 1.31(1) . . . N2 C11 1.33(1) . . . C7 C8 1.37(1) . . . C9 C10 1.38(1) . . . C9 C8 1.38(1) . . . C10 C11 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. # N3 Mn1 N1 88.9(2) . . . . O1 Mn1 N1 90.7(2) . . . . O1 Mn1 N3 93.1(2) . . . . O1 Mn1 N3 86.9(2) 3_555 . . . O1 Mn1 N1 89.3(2) 3_555 . . . O1 Mn1 N3 91.1(2) . . 3_555 . Mn1 O1 C14 130.0(5) . . . . Mn1 N3 C13 169.4(6) . . . . Mn1 N1 C5 122.6(4) . . . . C3 C6 C6 125.2(8) . . 3_454 . C5 N1 C1 116.6(6) . . . . Mn1 N1 C1 120.4(4) . . . . C3 C2 C1 119.7(6) . . . . C6 C3 C2 123.1(6) . . . . C2 C3 C4 116.7(6) . . . . C6 C3 C4 120.2(6) . . . . C5 C4 C3 119.8(6) . . . . S1 C13 N3 178.2(7) . . . . C9 C12 C12 126.3(9) . . 3_545 . N1 C1 C2 123.5(6) . . . . C7 N2 C11 116.0(9) . . . . N2 C7 C8 124.3(8) . . . . C12 C9 C8 119.2(7) . . . . C12 C9 C10 122.8(7) . . . . C10 C9 C8 117.9(8) . . . . C9 C10 C11 118.1(8) . . . . N2 C1 C10 124.6(9) . . . . C7 C8 C9 119.0(8) . . . . #=======================================================================