#------------------------------------------------------------------------------ #$Date: 2016-02-20 03:06:23 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176774 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/22/2202211.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2202211 loop_ _publ_author_name 'Chen, Bao-Hua' 'Li, Yi-Zhi' 'Ma, Yong-Xiang' 'Wu, Xiao-Li' 'Li, Ping-Ren' _publ_section_title Bis[dicarbonyl(\h^5^-cyclopentadienyl)ferrio](N,N-diisobutyldithiocarbamato)tin(II) _journal_issue 5 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m223 _journal_page_last m224 _journal_paper_doi 10.1107/S160053680300713X _journal_volume 59 _journal_year 2003 _chemical_formula_iupac '[Sn Fe2 (C5 H5)2 (C9 H18 N1 S2)2 (C1 O1)4]' _chemical_formula_moiety 'C32 H46 Fe2 N2 O4 S4 Sn' _chemical_formula_sum 'C32 H46 Fe2 N2 O4 S4 Sn' _chemical_formula_weight 881.34 _chemical_name_systematic ; Bis[dicarbonyl(\h^5^-cyclopentadienyl)ferrio](N,N- diisobutyldithiocarbamato)tin(II) ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 112.17(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 21.800(4) _cell_length_b 11.587(2) _cell_length_c 16.886(3) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 17.54 _cell_measurement_theta_min 2.01 _cell_volume 3950.0(15) _computing_cell_refinement XSCANS _computing_data_collection 'XSCANS (Bruker, 2000)' _computing_data_reduction 'SHELXTL (Bruker, 2000)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement SHELXTL _computing_structure_solution SHELXTL _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0630 _diffrn_reflns_av_sigmaI/netI 0.0836 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 6972 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 2.02 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time 25 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.598 _exptl_absorpt_correction_T_max 0.72 _exptl_absorpt_correction_T_min 0.69 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 2000)' _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Block _exptl_crystal_F_000 1800 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.778 _refine_diff_density_min -0.959 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 208 _refine_ls_number_reflns 3488 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.052 _refine_ls_R_factor_all 0.0986 _refine_ls_R_factor_gt 0.0537 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.07P)^2^+1.66P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1428 _refine_ls_wR_factor_ref 0.1533 _reflns_number_gt 2132 _reflns_number_total 3488 _reflns_threshold_expression I>2\s(I) _cod_data_source_file wn6146.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 2202211 _cod_database_fobs_code 2202211 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Fe1 1.08704(6) 0.90777(10) 0.38100(7) 0.0750(4) Uani d . 1 . . Fe Sn1 1.0000 0.81279(5) 0.2500 0.0539(2) Uani d S 1 . . Sn O1 0.9917(3) 1.0797(6) 0.3832(5) 0.114(2) Uani d . 1 . . O O2 1.1365(3) 1.0538(6) 0.2773(5) 0.114(2) Uani d . 1 . . O S1 0.94815(11) 0.63240(17) 0.28891(14) 0.0788(6) Uani d . 1 . . S S2 0.90183(11) 0.83421(17) 0.35645(15) 0.0815(6) Uani d . 1 . . S N1 0.8743(3) 0.6162(5) 0.3812(4) 0.0780(18) Uani d . 1 . . N C1 0.9042(4) 0.6900(6) 0.3467(5) 0.075(2) Uani d . 1 . . C C2 0.8688(4) 0.4901(7) 0.3653(5) 0.080(2) Uani d . 1 . . C H2A 0.8795 0.4507 0.4196 0.097 Uiso calc R 1 . . H H2B 0.9015 0.4674 0.3421 0.097 Uiso calc R 1 . . H C3 0.8018(5) 0.4504(7) 0.3052(6) 0.093(2) Uani d . 1 . . C H3 0.7700 0.4677 0.3318 0.111 Uiso calc R 1 . . H C4 0.7775(5) 0.5069(8) 0.2190(6) 0.111(3) Uani d . 1 . . C H4A 0.7668 0.5861 0.2244 0.166 Uiso calc R 1 . . H H4B 0.7387 0.4674 0.1815 0.166 Uiso calc R 1 . . H H4C 0.8114 0.5032 0.1957 0.166 Uiso calc R 1 . . H C5 0.8032(5) 0.3190(7) 0.2946(6) 0.110(3) Uani d . 1 . . C H5A 0.8409 0.2981 0.2814 0.165 Uiso calc R 1 . . H H5B 0.7634 0.2947 0.2489 0.165 Uiso calc R 1 . . H H5C 0.8062 0.2820 0.3468 0.165 Uiso calc R 1 . . H C6 0.8400(5) 0.6578(8) 0.4359(6) 0.093(3) Uani d . 1 . . C H6A 0.8191 0.7309 0.4131 0.111 Uiso calc R 1 . . H H6B 0.8050 0.6035 0.4314 0.111 Uiso calc R 1 . . H C7 0.8805(6) 0.6742(10) 0.5272(6) 0.118(3) Uani d . 1 . . C H7 0.9012 0.7473 0.5218 0.142 Uiso calc R 1 . . H C8 0.9436(7) 0.6057(11) 0.5692(7) 0.147(5) Uani d . 1 . . C H8A 0.9345 0.5382 0.5959 0.221 Uiso calc R 1 . . H H8B 0.9759 0.6525 0.6116 0.221 Uiso calc R 1 . . H H8C 0.9606 0.5828 0.5267 0.221 Uiso calc R 1 . . H C9 0.8445(7) 0.7171(12) 0.5780(7) 0.144(4) Uani d . 1 . . C H9A 0.8057 0.6707 0.5675 0.216 Uiso calc R 1 . . H H9B 0.8316 0.7958 0.5626 0.216 Uiso calc R 1 . . H H9C 0.8724 0.7133 0.6376 0.216 Uiso calc R 1 . . H C10 1.0295(5) 1.0095(8) 0.3828(6) 0.090(2) Uani d . 1 . . C C11 1.1164(5) 0.9924(8) 0.3169(6) 0.093(3) Uani d . 1 . . C C12 1.1104(5) 0.7408(10) 0.4330(6) 0.102(3) Uani d . 1 . . C H12 1.0890 0.6698 0.4041 0.122 Uiso calc R 1 . . H C13 1.0873(5) 0.8087(9) 0.4826(6) 0.103(3) Uani d . 1 . . C H13 1.0495 0.7925 0.4988 0.124 Uiso calc R 1 . . H C14 1.1347(6) 0.9011(9) 0.5142(6) 0.108(3) Uani d . 1 . . C H14 1.1339 0.9614 0.5544 0.130 Uiso calc R 1 . . H C15 1.1801(5) 0.8911(10) 0.4773(6) 0.109(3) Uani d . 1 . . C H15 1.2175 0.9434 0.4867 0.131 Uiso calc R 1 . . H C16 1.1660(5) 0.7910(10) 0.4250(6) 0.105(3) Uani d . 1 . . C H16 1.1917 0.7606 0.3930 0.126 Uiso calc R 1 . . H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe1 0.0740(7) 0.0808(7) 0.0635(7) 0.0008(6) 0.0182(5) -0.0096(5) Sn1 0.0591(4) 0.0496(4) 0.0551(4) 0.000 0.0240(3) 0.000 O1 0.108(5) 0.089(4) 0.133(5) 0.011(4) 0.031(4) -0.037(4) O2 0.111(5) 0.109(5) 0.125(5) -0.028(4) 0.046(4) 0.003(4) S1 0.0949(15) 0.0627(11) 0.1008(15) -0.0050(11) 0.0621(13) 0.0000(10) S2 0.0973(15) 0.0621(12) 0.0999(15) 0.0016(10) 0.0539(13) 0.0053(10) N1 0.096(5) 0.071(4) 0.087(4) -0.007(4) 0.056(4) 0.003(3) C1 0.092(5) 0.064(4) 0.085(5) -0.004(4) 0.052(4) 0.002(4) C2 0.097(6) 0.072(5) 0.086(5) -0.011(5) 0.050(5) 0.002(4) C3 0.106(7) 0.079(5) 0.095(6) -0.014(5) 0.040(5) 0.003(5) C4 0.120(8) 0.092(6) 0.105(7) -0.006(6) 0.026(6) 0.012(5) C5 0.126(8) 0.079(6) 0.105(7) -0.016(6) 0.021(6) 0.002(5) C6 0.112(7) 0.095(6) 0.093(6) -0.003(5) 0.064(6) -0.003(5) C7 0.139(9) 0.129(9) 0.099(7) 0.005(8) 0.059(7) -0.010(7) C8 0.166(12) 0.141(10) 0.119(9) 0.025(10) 0.034(9) -0.006(8) C9 0.174(12) 0.171(11) 0.106(8) 0.002(10) 0.074(8) -0.030(8) C10 0.092(6) 0.080(6) 0.087(6) 0.004(5) 0.022(5) -0.023(4) C11 0.087(6) 0.092(6) 0.093(6) -0.025(5) 0.025(5) -0.005(5) C12 0.098(7) 0.107(7) 0.077(6) 0.015(6) 0.005(5) 0.016(5) C13 0.101(7) 0.122(8) 0.069(5) 0.008(7) 0.011(5) 0.015(6) C14 0.101(7) 0.128(9) 0.072(6) 0.007(7) 0.006(6) -0.001(6) C15 0.089(7) 0.127(9) 0.085(7) 0.006(6) 0.003(6) 0.000(6) C16 0.087(7) 0.120(8) 0.086(6) 0.019(6) 0.007(5) 0.005(6) 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle C10 Fe1 C11 . . 93.7(5) C10 Fe1 C13 . . 98.0(4) C11 Fe1 C13 . . 159.9(4) C10 Fe1 C15 . . 123.4(4) C11 Fe1 C15 . . 93.4(4) C13 Fe1 C15 . . 66.5(4) C10 Fe1 C16 . . 159.9(4) C11 Fe1 C16 . . 97.9(5) C13 Fe1 C16 . . 66.5(4) C15 Fe1 C16 . . 39.8(4) C10 Fe1 C14 . . 94.4(4) C11 Fe1 C14 . . 122.4(4) C13 Fe1 C14 . . 40.6(4) C15 Fe1 C14 . . 38.0(4) C16 Fe1 C14 . . 65.5(4) C10 Fe1 C12 . . 133.0(5) C11 Fe1 C12 . . 133.2(5) C13 Fe1 C12 . . 38.5(4) C15 Fe1 C12 . . 65.0(4) C16 Fe1 C12 . . 38.8(4) C14 Fe1 C12 . . 64.8(4) C10 Fe1 Sn1 . . 90.1(3) C11 Fe1 Sn1 . . 91.8(3) C13 Fe1 Sn1 . . 104.4(3) C15 Fe1 Sn1 . . 145.6(3) C16 Fe1 Sn1 . . 105.7(3) C14 Fe1 Sn1 . . 145.0(3) C12 Fe1 Sn1 . . 87.1(3) Fe1 Sn1 Fe1 . 2_755 129.01(6) Fe1 Sn1 S1 . . 112.48(6) Fe1 Sn1 S1 2_755 . 108.43(6) Fe1 Sn1 S1 . 2_755 108.43(6) Fe1 Sn1 S1 2_755 2_755 112.48(6) S1 Sn1 S1 . 2_755 71.57(9) C1 S1 Sn1 . . 102.7(3) C1 N1 C6 . . 120.8(6) C1 N1 C2 . . 124.9(6) C6 N1 C2 . . 114.3(6) N1 C1 S2 . . 123.8(6) N1 C1 S1 . . 117.5(5) S2 C1 S1 . . 118.7(4) N1 C2 C3 . . 114.5(7) N1 C2 H2A . . 108.6 C3 C2 H2A . . 108.6 N1 C2 H2B . . 108.6 C3 C2 H2B . . 108.6 H2A C2 H2B . . 107.6 C4 C3 C2 . . 114.8(7) C4 C3 C5 . . 109.5(8) C2 C3 C5 . . 109.1(8) C4 C3 H3 . . 107.7 C2 C3 H3 . . 107.7 C5 C3 H3 . . 107.7 C3 C4 H4A . . 109.5 C3 C4 H4B . . 109.5 H4A C4 H4B . . 109.5 C3 C4 H4C . . 109.5 H4A C4 H4C . . 109.5 H4B C4 H4C . . 109.5 C3 C5 H5A . . 109.5 C3 C5 H5B . . 109.5 H5A C5 H5B . . 109.5 C3 C5 H5C . . 109.5 H5A C5 H5C . . 109.5 H5B C5 H5C . . 109.5 C7 C6 N1 . . 117.0(8) C7 C6 H6A . . 108.0 N1 C6 H6A . . 108.0 C7 C6 H6B . . 108.0 N1 C6 H6B . . 108.0 H6A C6 H6B . . 107.3 C9 C7 C6 . . 114.7(10) C9 C7 C8 . . 120.1(10) C6 C7 C8 . . 120.2(9) C9 C7 H7 . . 97.4 C6 C7 H7 . . 97.4 C8 C7 H7 . . 97.4 C7 C8 H8A . . 109.5 C7 C8 H8B . . 109.5 H8A C8 H8B . . 109.5 C7 C8 H8C . . 109.5 H8A C8 H8C . . 109.5 H8B C8 H8C . . 109.5 C7 C9 H9A . . 109.5 C7 C9 H9B . . 109.5 H9A C9 H9B . . 109.5 C7 C9 H9C . . 109.5 H9A C9 H9C . . 109.5 H9B C9 H9C . . 109.5 O1 C10 Fe1 . . 178.3(9) O2 C11 Fe1 . . 176.3(8) C13 C12 C16 . . 110.6(10) C13 C12 Fe1 . . 69.0(6) C16 C12 Fe1 . . 70.0(6) C13 C12 H12 . . 124.7 C16 C12 H12 . . 124.7 Fe1 C12 H12 . . 124.7 C12 C13 C14 . . 105.8(10) C12 C13 Fe1 . . 72.4(6) C14 C13 Fe1 . . 70.8(6) C12 C13 H13 . . 126.9 C14 C13 H13 . . 126.9 Fe1 C13 H13 . . 126.9 C15 C14 C13 . . 108.2(10) C15 C14 Fe1 . . 70.3(6) C13 C14 Fe1 . . 68.6(5) C15 C14 H14 . . 125.9 C13 C14 H14 . . 125.9 Fe1 C14 H14 . . 125.9 C14 C15 C16 . . 109.3(11) C14 C15 Fe1 . . 71.7(6) C16 C15 Fe1 . . 70.8(5) C14 C15 H15 . . 125.3 C16 C15 H15 . . 125.3 Fe1 C15 H15 . . 125.3 C12 C16 C15 . . 105.8(10) C12 C16 Fe1 . . 71.1(6) C15 C16 Fe1 . . 69.4(6) C12 C16 H16 . . 127.0 C15 C16 H16 . . 127.0 Fe1 C16 H16 . . 127.0 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 C10 . 1.729(10) ? Fe1 C11 . 1.751(10) ? Fe1 C13 . 2.063(9) ? Fe1 C15 . 2.075(9) ? Fe1 C16 . 2.093(10) ? Fe1 C14 . 2.093(9) ? Fe1 C12 . 2.106(10) ? Fe1 Sn1 . 2.5568(14) ? Sn1 Fe1 2_755 2.5568(14) ? Sn1 S1 . 2.577(2) ? Sn1 S1 2_755 2.577(2) ? O1 C10 . 1.161(10) ? O2 C11 . 1.170(10) ? S1 C1 . 1.738(7) ? S2 C1 . 1.682(7) ? N1 C1 . 1.335(9) ? N1 C6 . 1.471(9) ? N1 C2 . 1.482(10) ? C2 C3 . 1.502(12) ? C2 H2A . 0.9700 ? C2 H2B . 0.9700 ? C3 C4 . 1.499(11) ? C3 C5 . 1.535(11) ? C3 H3 . 0.9800 ? C4 H4A . 0.9600 ? C4 H4B . 0.9600 ? C4 H4C . 0.9600 ? C5 H5A . 0.9600 ? C5 H5B . 0.9600 ? C5 H5C . 0.9600 ? C6 C7 . 1.471(13) ? C6 H6A . 0.9700 ? C6 H6B . 0.9700 ? C7 C9 . 1.453(13) ? C7 C8 . 1.513(15) ? C7 H7 . 0.9800 ? C8 H8A . 0.9600 ? C8 H8B . 0.9600 ? C8 H8C . 0.9600 ? C9 H9A . 0.9600 ? C9 H9B . 0.9600 ? C9 H9C . 0.9600 ? C12 C13 . 1.376(13) ? C12 C16 . 1.396(14) ? C12 H12 . 0.9800 ? C13 C14 . 1.444(13) ? C13 H13 . 0.9800 ? C14 C15 . 1.357(14) ? C14 H14 . 0.9800 ? C15 C16 . 1.419(14) ? C15 H15 . 0.9800 ? C16 H16 . 0.9800 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA C2 H2B S1 0.97 2.49 3.009(8) 114 C6 H6A S2 0.97 2.63 3.026(9) 105 C8 H8C N1 0.96 2.50 2.960(13) 109