#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2008810.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_2008810 loop_ _publ_author_name 'Kitamura, Y.' 'Azuma, N.' 'Matsuda, T.' 'Tanabe, Y.' _publ_section_title ; Tetrakis(methylamine-N)(oxalato-O^1^,O^2^)cobalt(III) perchlorate and tetrakis(ethylamine-N)(oxalato-O^1^,O^2^)cobalt(III) perchlorate monohydrate ; _journal_issue 8 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1267 _journal_page_last 1270 _journal_volume 55 _journal_year 1999 _chemical_formula_analytical 'C6 H20 Cl1 Co1 N4 O8 ' _chemical_formula_moiety '[Co (C2 O4)(C H5 N)4] Cl O4 ' _chemical_formula_structural 'C6 H20 Cl1 Co1 N4 O8 ' _chemical_formula_sum 'C6 H20 Cl Co N4 O8' _chemical_formula_weight 370.63 _chemical_name_common Tetrakis(methylamine)oxalatocobalt(III) _space_group_IT_number 29 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2c -2ac' _symmetry_space_group_name_H-M 'P c a 21' _audit_creation_method 'from TEXRAY.INF file' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.780(3) _cell_length_b 11.004(3) _cell_length_c 12.108(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 298.2 _cell_measurement_theta_max 12.8 _cell_measurement_theta_min 12.1 _cell_volume 1436.3(6) _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_collection 'MSC/AFC Diffractometer Control (Molecular Structure Corporation, 1988)' _computing_data_reduction 'TEXSAN (Molecular Structure Corporation, 1989)' _computing_molecular_graphics TEXSAN _computing_publication_material TEXSAN _computing_structure_refinement TEXSAN _computing_structure_solution TEXSAN _diffrn_ambient_temperature 298.2 _diffrn_measurement_device_type 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI 0.000 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 2393 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_min 2.35 _diffrn_standards_decay_% 0.17 _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.418 _exptl_absorpt_correction_T_max 0.932 _exptl_absorpt_correction_T_min 0.748 _exptl_absorpt_correction_type \y-scans _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.714 _exptl_crystal_density_meas 'not measured' _exptl_crystal_description prismatic _exptl_crystal_F_000 768.00 _exptl_crystal_size_max 0.330 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.050 _refine_diff_density_max 0.62 _refine_diff_density_min -0.59 _refine_ls_abs_structure_details ; ? ; _refine_ls_extinction_coef 0.00000 _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_goodness_of_fit_ref 1.287 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 180 _refine_ls_number_reflns 2182 _refine_ls_number_restraints 0 _refine_ls_R_factor_gt 0.064 _refine_ls_shift/su_max 0.0022 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/\s^2^(Fo^2^)' _refine_ls_weighting_scheme sigma _refine_ls_wR_factor_ref 0.048 _reflns_number_gt 2182 _reflns_number_total 2393 _reflns_observed_criterion I>0 _[local]_cod_data_source_file oa1068.cif _[local]_cod_data_source_block 1 _[local]_cod_cif_authors_sg_H-M 'P c a 21 ' _[local]_cod_chemical_formula_sum_orig 'C6 H20 Cl1 Co1 N4 O8 ' _cod_original_cell_volume 1436.0(10) _cod_database_code 2008810 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y,1/2+z' '1/2-x, +y,1/2+z' '1/2+x, -y, +z' 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 Co 0.0288(3) 0.0288(3) 0.0208(3) 0.0022(3) -0.0024(4) -0.0010(4) Cl 0.0790(10) 0.0440(10) 0.0500(10) 0.0080(10) -0.0100(10) 0.0016(9) O1 0.0240(10) 0.036(2) 0.0230(10) -0.0020(10) 0.0030(10) -0.0030(10) O2 0.039(2) 0.050(2) 0.036(2) -0.016(2) -0.0020(10) -0.009(2) O3 0.0300(10) 0.031(2) 0.0260(10) -0.0050(10) 0.0000(10) 0.0040(10) O4 0.043(2) 0.061(2) 0.0220(10) -0.007(2) 0.0060(10) -0.002(2) O5 0.225(9) 0.041(3) 0.083(5) 0.019(4) 0.011(5) 0.003(3) O6 0.153(7) 0.210(10) 0.113(7) 0.117(7) 0.055(6) 0.056(6) O7 0.139(7) 0.105(5) 0.092(5) 0.014(4) -0.018(4) 0.051(4) O8 0.185(8) 0.240(10) 0.099(6) -0.120(8) -0.053(6) -0.012(7) N1 0.040(2) 0.052(3) 0.024(2) 0.011(2) 0.001(2) -0.001(2) N2 0.034(2) 0.033(2) 0.025(2) 0.0010(10) 0.001(2) 0.000(2) N3 0.042(2) 0.037(2) 0.030(2) -0.003(2) -0.009(2) -0.001(2) N4 0.044(2) 0.036(2) 0.037(3) 0.007(2) -0.006(2) 0.000(2) C1 0.035(3) 0.031(3) 0.025(2) 0.003(2) 0.002(2) 0.001(2) C2 0.027(2) 0.026(2) 0.025(2) 0.005(2) 0.001(2) 0.002(2) C3 0.051(3) 0.052(4) 0.034(3) 0.004(3) 0.006(3) 0.003(3) C4 0.046(3) 0.033(3) 0.063(5) -0.005(2) 0.009(3) 0.006(3) C5 0.037(3) 0.061(4) 0.048(3) -0.016(3) -0.003(2) 0.005(3) C6 0.094(6) 0.043(4) 0.048(4) 0.014(4) -0.001(4) 0.006(3) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy Co 0.12990(10) 0.19060(10) 0.00000 0.0262(3) Uani 1.000 Cl 0.6636(2) 0.4249(2) 0.1926(2) 0.0580(10) Uani 1.000 O1 -0.0208(3) 0.1082(3) -0.0365(3) 0.0280(10) Uani 1.000 O2 -0.1110(4) 0.0219(4) -0.1815(4) 0.042(2) Uani 1.000 O3 0.1650(4) 0.1858(4) -0.1518(3) 0.029(2) Uani 1.000 O4 0.0943(4) 0.0994(4) -0.3069(3) 0.042(2) Uani 1.000 O5 0.6448(9) 0.5469(5) 0.2105(6) 0.116(5) Uani 1.000 O6 0.7571(9) 0.4150(9) 0.1156(7) 0.160(8) Uani 1.000 O7 0.6908(7) 0.3706(6) 0.2941(6) 0.112(5) Uani 1.000 O8 0.5559(9) 0.3762(9) 0.1516(8) 0.175(8) Uani 1.000 N1 0.0835(5) 0.1831(5) 0.1610(4) 0.039(2) Uani 1.000 N2 0.2232(4) 0.0357(4) 0.0170(4) 0.031(2) Uani 1.000 N3 0.2845(5) 0.2747(4) 0.0421(4) 0.037(2) Uani 1.000 N4 0.0414(5) 0.3473(4) -0.0181(4) 0.039(2) Uani 1.000 C1 -0.0268(5) 0.0795(5) -0.1394(4) 0.031(2) Uani 1.000 C2 0.0866(5) 0.1236(5) -0.2079(4) 0.026(2) Uani 1.000 C3 -0.0407(6) 0.2093(6) 0.1961(5) 0.046(3) Uani 1.000 C4 0.1598(6) -0.0837(5) 0.0226(7) 0.047(4) Uani 1.000 C5 0.3824(6) 0.2842(7) -0.0432(5) 0.049(3) Uani 1.000 C6 0.0961(8) 0.4383(6) -0.0940(6) 0.062(5) Uani 1.000 H1 0.10148 0.10283 0.18520 0.04632 Uiso 1.000 H2 0.13608 0.23890 0.19836 0.04632 Uiso 1.000 H3 -0.06195 0.28983 0.17506 0.05502 Uiso 1.000 H4 -0.09643 0.15368 0.16227 0.05502 Uiso 1.000 H5 -0.04610 0.20172 0.27408 0.05502 Uiso 1.000 H6 0.27842 0.03131 -0.04408 0.03697 Uiso 1.000 H7 0.26959 0.04309 0.08335 0.03697 Uiso 1.000 H8 0.10434 -0.08444 0.08357 0.05690 Uiso 1.000 H9 0.11465 -0.09696 -0.04372 0.05690 Uiso 1.000 H10 0.21971 -0.14625 0.03151 0.05690 Uiso 1.000 H11 0.26302 0.35498 0.06374 0.04406 Uiso 1.000 H12 0.31884 0.23256 0.10332 0.04406 Uiso 1.000 H13 0.40745 0.20502 -0.06519 0.05822 Uiso 1.000 H14 0.35095 0.32689 -0.10542 0.05822 Uiso 1.000 H15 0.45162 0.32673 -0.01386 0.05822 Uiso 1.000 H16 -0.03957 0.32936 -0.04432 0.04679 Uiso 1.000 H17 0.03598 0.38388 0.05282 0.04679 Uiso 1.000 H18 0.17694 0.45928 -0.06918 0.07381 Uiso 1.000 H19 0.10109 0.40500 -0.16625 0.07381 Uiso 1.000 H20 0.04543 0.50887 -0.09519 0.07381 Uiso 1.000 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.002 0.002 'International Tables Vol IV Table 2.2A' H 0.000 0.000 'International Tables Vol IV Table 2.2A' Cl 0.132 0.159 'International Tables Vol IV Table 2.2A' Co 0.299 0.973 'International Tables Vol IV Table 2.2A' N 0.004 0.003 'International Tables Vol IV Table 2.2A' O 0.008 0.006 'International Tables Vol IV Table 2.2A' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 -1 -2 -2 -1 -2 -1 1 -2 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O1 Co O3 86.1(2) yes O1 Co N1 89.6(2) no O1 Co N2 92.7(2) no O1 Co N3 178.4(2) no O1 Co N4 88.7(2) no O3 Co N1 175.2(2) no O3 Co N2 88.6(2) no O3 Co N3 95.5(2) yes O3 Co N4 90.8(2) no N1 Co N2 89.4(2) no N1 Co N3 88.8(2) no N1 Co N4 91.3(2) no N2 Co N3 87.0(2) no N2 Co N4 178.4(2) no N3 Co N4 91.5(2) no O5 Cl O6 107.0(5) no O5 Cl O7 108.0(5) no O5 Cl O8 108.3(6) no O6 Cl O7 114.0(5) no O6 Cl O8 110.1(6) no O7 Cl O8 109.2(6) no Co O1 C1 112.5(4) no Co O3 C2 113.6(3) no Co N1 C3 120.6(4) yes Co N2 C4 122.0(3) yes Co N3 C5 117.1(4) yes Co N4 C6 117.7(4) yes O1 C1 O2 124.8(5) no O1 C1 C2 113.6(5) no O2 C1 C2 121.6(5) no O3 C2 O4 125.9(5) no O3 C2 C1 113.7(5) no O4 C2 C1 120.4(5) no Co N1 H1 106.61 no Co N1 H2 106.61 no C3 N1 H1 106.62 no C3 N1 H2 106.62 no H1 N1 H2 109.46 no Co N2 H6 106.24 no Co N2 H7 106.24 no C4 N2 H6 106.26 no C4 N2 H7 106.25 no H6 N2 H7 109.46 no Co N3 H11 107.54 no Co N3 H12 107.54 no C5 N3 H11 107.54 no C5 N3 H12 107.54 no H11 N3 H12 109.46 no Co N4 H16 107.38 no Co N4 H17 107.38 no C6 N4 H16 107.38 no C6 N4 H17 107.38 no H16 N4 H17 109.46 no N1 C3 H3 109.47 no N1 C3 H4 109.47 no N1 C3 H5 109.47 no H3 C3 H4 109.47 no H3 C3 H5 109.47 no H4 C3 H5 109.47 no N2 C4 H8 109.48 no N2 C4 H9 109.48 no N2 C4 H10 109.47 no H8 C4 H9 109.48 no H8 C4 H10 109.47 no H9 C4 H10 109.46 no N3 C5 H13 109.47 no N3 C5 H14 109.47 no N3 C5 H15 109.47 no H13 C5 H14 109.47 no H13 C5 H15 109.47 no H14 C5 H15 109.47 no N4 C6 H18 109.47 no N4 C6 H19 109.46 no N4 C6 H20 109.47 no H18 C6 H19 109.47 no H18 C6 H20 109.48 no H19 C6 H20 109.48 no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Co O1 1.912(4) yes Co O3 1.877(4) yes Co N1 2.015(5) yes Co N2 1.990(4) yes Co N3 1.973(5) yes Co N4 1.983(5) yes Cl O5 1.375(6) no Cl O6 1.377(8) no Cl O7 1.399(7) no Cl O8 1.371(8) no O1 C1 1.287(6) yes O2 C1 1.220(7) yes O3 C2 1.282(6) yes O4 C2 1.230(7) yes N1 C3 1.435(8) yes N2 C4 1.483(7) yes N3 C5 1.480(8) yes N4 C6 1.481(9) yes C1 C2 1.555(7) yes N1 H1 0.950 no N1 H2 0.950 no N2 H6 0.950 no N2 H7 0.950 no N3 H11 0.950 no N3 H12 0.950 no N4 H16 0.950 no N4 H17 0.950 no C3 H3 0.950 no C3 H4 0.950 no C3 H5 0.950 no C4 H8 0.950 no C4 H9 0.950 no C4 H10 0.950 no C5 H13 0.950 no C5 H14 0.950 no C5 H15 0.950 no C6 H18 0.950 no C6 H19 0.950 no C6 H20 0.950 no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_2 _geom_contact_publ_flag O1 N2 3.247(6) 4_455 no O1 C4 3.528(7) 4_455 no O2 N1 2.968(7) 2_554 no O2 N2 3.061(6) 4_455 no O2 O3 3.344(6) 4_455 no O2 C3 3.368(8) 2_554 no O2 C4 3.560(8) 4_455 no O3 N1 3.534(7) 3_554 no O4 N3 2.962(6) 3_554 no O4 N2 2.985(6) 3_554 no O4 C4 3.435(8) 2_554 no O4 C3 3.446(8) 2_554 no O4 O8 3.490(10) 3_554 no O4 C5 3.520(8) 3_554 no O5 N1 3.102(8) 4_565 no O5 N4 3.202(9) 4_565 no O5 N3 3.206(9) 4_565 no O5 C3 3.350(10) 4_565 no O5 C5 3.526(9) 2_665 no O6 C3 3.290(10) 1_655 no O6 C6 3.470(10) 4_565 no O6 N3 3.540(10) 4_565 no O6 N4 3.550(10) 1_655 no O7 N4 3.392(9) 3_555 no O7 C6 3.400(10) 3_665 no O7 C6 3.460(10) 3_555 no O7 C3 3.600(10) 1_655 no O8 C5 3.180(10) 1_555 no O8 N3 3.401(9) 1_555 no O8 C6 3.560(10) 3_555 no N2 C1 3.529(7) 4_555 no Cl H17 3.030 4_565 no Cl H11 3.074 4_565 no Cl H3 3.318 1_655 no Cl H19 3.333 3_555 no Cl H18 3.419 4_565 no Cl H20 3.540 3_555 no Cl H15 3.555 1_555 no Cl H19 3.586 2_665 no Cl H18 3.592 2_665 no O1 H6 2.656 4_455 no O1 H10 2.946 4_455 no O1 H7 3.160 4_455 no O1 H13 3.550 4_455 no O2 H1 2.121 2_554 no O2 H6 2.129 4_455 no O2 H13 2.874 4_455 no O2 H8 2.927 2_554 no O2 H5 3.036 2_554 no O2 H2 3.229 2_554 no O2 H7 3.397 2_554 no O2 H10 3.443 4_455 no O2 H9 3.494 4_455 no O2 H4 3.509 2_554 no O2 H7 3.529 4_455 no O3 H2 2.869 3_554 no O3 H12 3.014 3_554 no O6 H11 2.609 4_565 no O6 H18 2.769 4_565 no O6 H16 3.073 1_655 no O6 H17 3.120 1_655 no O6 H10 3.154 4_555 no O6 H4 3.329 1_655 no O6 H17 3.341 4_565 no O6 H20 3.525 4_565 no O7 H16 2.587 3_555 no O7 H18 2.877 2_665 no O7 H3 3.158 1_655 no O7 H19 3.206 3_555 no O7 H20 3.256 3_555 no O7 H19 3.371 2_665 no O7 H5 3.399 1_655 no O7 H20 3.412 2_665 no O7 H14 3.573 2_665 no O8 H15 2.361 1_555 no O8 H19 2.798 3_555 no O8 H17 2.906 4_565 no O8 H12 3.061 1_555 no O8 H20 3.246 4_565 no O8 H11 3.340 1_555 no O8 H8 3.355 4_555 no O8 H10 3.411 4_555 no O8 H18 3.482 4_565 no C5 H2 3.174 3_554 no C5 H9 3.242 4_555 no C5 H8 3.593 4_555 no C6 H15 3.171 4_465 no H1 H13 3.226 3_555 no H1 H14 3.573 3_555 no H2 H14 2.569 3_555 no H2 H13 2.925 3_555 no H3 H10 3.325 4_455 no H3 H14 3.522 3_555 no H3 H20 3.561 2_565 no H4 H10 2.538 4_455 no H4 H7 2.773 4_455 no H4 H8 3.449 4_455 no H4 H6 3.494 4_455 no H5 H13 2.454 3_555 no H5 H9 2.596 2_555 no H5 H14 2.907 3_555 no H5 H15 3.086 3_555 no H5 H20 3.556 2_565 no H8 H13 3.084 4_455 no H8 H15 3.348 4_455 no H8 H12 3.491 4_455 no H9 H13 2.544 4_455 no H9 H15 3.100 4_455 no H10 H16 3.411 4_555 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H1 O2 2_554 2_554 1_555 0.950 2.121 2.968(7) 147.7 yes N3 H12 O4 3_554 3_554 1_555 0.950 2.051 2.962(6) 160.2 yes N2 H7 O4 3_554 3_554 1_555 0.950 2.074 2.985(6) 160.0 yes N2 H6 O2 4_455 4_455 1_555 0.950 2.129 3.061(6) 166.5 no N1 H2 O5 4_565 4_565 1_555 0.950 2.363 3.102(8) 134.3 no N4 H17 O5 4_565 4_565 1_555 0.950 2.366 3.202(9) 146.6 no N3 H11 O5 4_565 4_565 1_555 0.950 2.438 3.206(9) 137.8 no 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_publ_flag Co O1 C1 O2 176.6(5) no Co O1 C1 C2 -2.4(6) no Co O3 C2 O4 -174.3(5) no Co O3 C2 C1 6.7(6) no O1 Co O3 C2 -6.6(4) no O1 Co N1 C3 -43.3(5) no O1 Co N2 C4 -12.6(5) no O1 Co N3 C5 158(6) no O1 Co N4 C6 -126.4(5) no O1 C1 C2 O3 -2.9(7) no O1 C1 C2 O4 178.0(5) no O2 C1 C2 O3 178.1(5) no O2 C1 C2 O4 -1.0(9) no O3 Co O1 C1 4.8(4) no O3 Co N1 C3 -70(3) no O3 Co N2 C4 -98.6(5) no O3 Co N3 C5 -11.6(5) no O3 Co N4 C6 -40.4(5) no N1 Co O1 C1 -173.0(4) no N1 Co O3 C2 20(3) no N1 Co N2 C4 77.0(5) no N1 Co N3 C5 166.2(5) no N1 Co N4 C6 144.0(5) no N2 Co O1 C1 -83.6(4) no N2 Co O3 C2 86.3(4) no N2 Co N1 C3 -136.0(5) no N2 Co N3 C5 76.7(5) no N2 Co N4 C6 26(8) no N3 Co O1 C1 -164(6) no N3 Co O3 C2 173.1(4) no N3 Co N1 C3 137.0(5) no N3 Co N2 C4 165.9(5) no N3 Co N4 C6 55.2(5) no N4 Co O1 C1 95.6(4) no N4 Co O3 C2 -95.2(4) no N4 Co N1 C3 45.4(5) no N4 Co N2 C4 -165(8) no N4 Co N3 C5 -102.5(5) no