#------------------------------------------------------------------------------ #$Date: 2015-04-02 12:22:18 +0100 (Thu, 02 Apr 2015) $ #$Revision: 134621 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/85/2008541.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_2008541 loop_ _publ_author_name 'Alcock, Nathaniel W.' 'Zhang, Delong' 'Busch, Daryle H.' _publ_section_title ; Tris(2-pyridylmethyl)triazacyclododecane complexes of Fe^II^ and Cu^II^ ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 886 _journal_page_last 889 _journal_paper_doi 10.1107/S0108270198018381 _journal_volume 55 _journal_year 1999 _chemical_formula_iupac '[Fe (C27 H36 N6)] [Fe Cl4]' _chemical_formula_sum 'C27 H36 Cl4 Fe2 N6' _chemical_formula_weight 698.12 _chemical_name_systematic ? _space_group_IT_number 205 _symmetry_cell_setting cubic _symmetry_space_group_name_Hall '-P 2ac 2ab 3' _symmetry_space_group_name_H-M 'P a -3' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 18.793(2) _cell_length_b 18.793(2) _cell_length_c 18.793(2) _cell_measurement_reflns_used 15 _cell_measurement_temperature 200(2) _cell_measurement_theta_max 11 _cell_measurement_theta_min 10 _cell_volume 6637.3(12) _computing_cell_refinement R3M _computing_data_collection 'R3M (Siemens, 1986)' _computing_data_reduction R3M _computing_molecular_graphics 'XP (Siemens, 1995)' _computing_publication_material 'XCIF (Siemens, 1995)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXTL-Plus (Sheldrick, 1990a)' _diffrn_ambient_temperature 200(2) _diffrn_measurement_device 'Siemens R3m' _diffrn_measurement_method \w-2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'Normal focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.127 _diffrn_reflns_av_sigmaI/netI 0.0973 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min 1 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 2262 _diffrn_reflns_theta_max 22.54 _diffrn_reflns_theta_min 1.88 _diffrn_standards_decay_% 22 _diffrn_standards_interval_count 200 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.223 _exptl_absorpt_correction_T_max 0.946 _exptl_absorpt_correction_T_min 0.845 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details '(SHELXTL-Plus; Sheldrick, 1990a)' _exptl_crystal_colour 'light brown' _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 2880 _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.37 _refine_diff_density_max 0.758 _refine_diff_density_min -0.377 _refine_ls_extinction_coef 0.0012(4) _refine_ls_extinction_method 'SHELXL97 (Sheldrick, 1997)' _refine_ls_goodness_of_fit_all 1.094 _refine_ls_goodness_of_fit_obs 1.165 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 129 _refine_ls_number_reflns 1461 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.092 _refine_ls_restrained_S_obs 1.161 _refine_ls_R_factor_all 0.088 _refine_ls_R_factor_obs .063 _refine_ls_shift/esd_max <0.001 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0720P)^2^+17.7800P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.173 _refine_ls_wR_factor_obs .157 _reflns_number_observed 1098 _reflns_number_total 1461 _reflns_observed_criterion I>2\s(I) _[local]_cod_data_source_file cf1275.cif _[local]_cod_data_source_block delcub _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Cubic' changed to 'cubic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_geom_bond_publ_flag' value 'Y' changed to 'y' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (2 times). Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_exptl_absorpt_correction_type' value 'Gaussian' changed to 'gaussian' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_geom_bond_publ_flag' value 'Y' changed to 'y' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (2 times). '_geom_angle_publ_flag' value 'Y' changed to 'y' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (5 times). Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(Fo^2^)+(0.0720P)^2^+17.7800P] where P = (Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/[\s^2^(Fo^2^)+(0.0720P)^2^+17.7800P] where P = (Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 6637.3(13) _cod_database_code 2008541 _cod_database_fobs_code 2008541 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-1/2' 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 .0270(5) .0270(5) .0270(5) .0004(4) .0004(4) .0004(4) Fe2 .0337(6) .0337(6) .0337(6) .0037(5) .0037(5) .0037(5) Cl1 .0388(8) .0388(8) .0388(8) .0026(8) .0026(8) .0026(8) Cl2 .0723(15) .0367(12) .0567(13) -.0089(10) -.0066(11) .0132(9) N1 .032(3) .028(3) .034(3) .000(3) .008(3) -.002(3) N2 .029(3) .028(3) .038(3) -.001(3) .001(3) -.002(3) C1 .028(4) .061(5) .050(5) -.008(4) .004(4) .004(4) C2A .038(7) .067(10) .049(8) -.010(6) -.013(5) .008(7) C2B .021(12) .058(18) .035(14) .002(11) -.016(10) .007(12) C3 .030(4) .046(4) .053(5) .001(3) -.012(4) .005(4) C4 .044(4) .037(4) .039(4) -.001(4) .010(4) .000(3) C5 .034(4) .033(4) .031(4) -.004(3) .002(3) .001(3) C6 .045(4) .037(4) .045(4) -.002(4) .012(4) -.009(4) C7 .056(5) .032(4) .051(5) .004(4) .010(4) -.013(4) C8 .050(5) .028(4) .040(4) .004(4) -.001(4) .001(3) C9 .041(4) .033(4) .044(5) -.001(3) .007(4) .007(4) 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_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol Fe1 .63084(5) .63084(5) .63084(5) .0270(5) Uani d S 1 . Fe Fe2 .16689(5) .16689(5) .16689(5) .0337(6) Uani d S 1 . Fe Cl1 .09424(10) .09424(10) .09424(10) .0388(8) Uani d S 1 . Cl Cl2 .17626(12) .27680(10) .11202(11) .0553(7) Uani d . 1 . Cl N1 .7405(3) .6632(3) .5942(3) .0312(14) Uani d . 1 . N N2 .6671(3) .5365(3) .5690(3) .0317(14) Uani d . 1 . N C1 .8001(4) .6358(4) .6409(4) .046(2) Uani d . 1 . C H1A .8091 .5857 .6276 .056 Uiso calc PR .687(17) 1 H H1B .8436 .6631 .6290 .056 Uiso calc PR .687(17) 1 H H1C .8180 .6760 .6699 .056 Uiso calc PR .313(17) 2 H H1D .8396 .6204 .6096 .056 Uiso calc PR .313(17) 2 H C2A .7907(6) .6387(7) .7181(6) .051(4) Uani d P .687(17) 1 C H2AA .7723 .6864 .7307 .062 Uiso calc PR .687(17) 1 H H2AB .8381 .6336 .7407 .062 Uiso calc PR .687(17) 1 H C2B .7819(11) .5732(14) .6921(12) .038(8) Uani d PU .313(17) 2 C H2BA .7585 .5360 .6630 .046 Uiso calc PR .313(17) 2 H H2BB .8277 .5530 .7085 .046 Uiso calc PR .313(17) 2 H C3 .7409(4) .5828(4) .7508(4) .0430(19) Uani d . 1 . C H3A .7534 .5359 .7305 .052 Uiso calc PR .687(17) 1 H H3B .7504 .5806 .8025 .052 Uiso calc PR .687(17) 1 H H3C .7599 .6243 .7771 .052 Uiso calc PR .313(17) 2 H H3D .7470 .5407 .7818 .052 Uiso calc PR .313(17) 2 H C4 .7478(4) .6272(3) .5229(4) .0402(18) Uani d . 1 . C H4A .7984 .6278 .5082 .048 Uiso calc R 1 . H H4B .7202 .6541 .4870 .048 Uiso calc R 1 . H C5 .7218(3) .5511(4) .5246(3) .0325(17) Uani d . 1 . C C6 .7508(4) .4997(4) .4796(4) .0421(18) Uani d . 1 . C H6A .7903 .5106 .4499 .051 Uiso calc R 1 . H C7 .7209(4) .4324(4) .4791(4) .046(2) Uani d . 1 . C H7A .7391 .3966 .4484 .055 Uiso calc R 1 . H C8 .6643(4) .4176(4) .5236(4) .0396(18) Uani d . 1 . C H8A .6434 .3716 .5241 .047 Uiso calc R 1 . H C9 .6390(4) .4699(4) .5668(4) .0393(18) Uani d . 1 . C H9A .5998 .4594 .5969 .047 Uiso calc R 1 . H 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' Cl Cl 0.1484 0.1585 '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' 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 _geom_angle_publ_flag N2 Fe1 N2 9 5 89.3(2) ? N2 Fe1 N2 9 . 89.3(2) y N2 Fe1 N2 5 . 89.3(2) ? N2 Fe1 N1 9 . 164.0(2) y N2 Fe1 N1 5 . 98.7(2) ? N2 Fe1 N1 . . 77.04(19) y N2 Fe1 N1 9 9 77.04(19) ? N2 Fe1 N1 5 9 164.0(2) ? N2 Fe1 N1 . 9 98.7(2) y N1 Fe1 N1 . 9 96.57(18) y N2 Fe1 N1 9 5 98.7(2) ? N2 Fe1 N1 5 5 77.04(19) ? N2 Fe1 N1 . 5 164.0(2) ? N1 Fe1 N1 . 5 96.57(18) ? N1 Fe1 N1 9 5 96.57(18) ? Cl2 Fe2 Cl2 . 9 111.31(6) ? Cl2 Fe2 Cl2 . 5 111.31(6) ? Cl2 Fe2 Cl2 9 5 111.31(6) ? Cl2 Fe2 Cl1 . . 107.57(6) ? Cl2 Fe2 Cl1 9 . 107.57(6) ? Cl2 Fe2 Cl1 5 . 107.57(6) ? C3 N1 C4 5 . 107.5(5) ? C3 N1 C1 5 . 108.7(5) ? C4 N1 C1 . . 107.2(5) ? C3 N1 Fe1 5 . 115.3(4) ? C4 N1 Fe1 . . 103.5(4) ? C1 N1 Fe1 . . 114.1(4) ? C5 N2 C9 . . 117.5(6) ? C5 N2 Fe1 . . 113.2(4) ? C9 N2 Fe1 . . 129.1(5) ? C2A C1 N1 . . 118.2(7) ? N1 C1 C2B . . 116.8(9) ? C1 C2A C3 . . 116.4(9) ? C3 C2B C1 . . 121.7(18) ? C2B C3 N1 . 9 118.1(10) ? N1 C3 C2A 9 . 116.6(7) ? N1 C4 C5 . . 112.1(6) ? N2 C5 C6 . . 122.1(6) ? N2 C5 C4 . . 116.8(6) ? C6 C5 C4 . . 121.0(6) ? C7 C6 C5 . . 118.6(7) ? C8 C7 C6 . . 119.5(7) ? C9 C8 C7 . . 119.0(7) ? N2 C9 C8 . . 123.3(7) ? 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 N2 9 2.226(5) ? Fe1 N2 5 2.226(5) ? Fe1 N2 . 2.226(5) y Fe1 N1 . 2.257(5) y Fe1 N1 9 2.257(5) ? Fe1 N1 5 2.257(5) ? Fe2 Cl2 . 2.3154(19) ? Fe2 Cl2 9 2.3155(19) ? Fe2 Cl2 5 2.3155(19) ? Fe2 Cl1 . 2.365(4) ? N1 C3 5 1.488(8) ? N1 C4 . 1.509(9) ? N1 C1 . 1.512(9) ? N2 C5 . 1.352(8) ? N2 C9 . 1.359(9) ? C1 C2A . 1.464(14) ? C1 C2B . 1.56(2) ? C2A C3 . 1.535(13) ? C2B C3 . 1.36(2) ? C3 N1 9 1.488(8) ? C4 C5 . 1.511(9) ? C5 C6 . 1.395(10) ? C6 C7 . 1.384(10) ? C7 C8 . 1.381(10) ? C8 C9 . 1.361(10) ?