#------------------------------------------------------------------------------ #$Date: 2012-02-03 17:16:24 +0000 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/29/2012965.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_2012965 loop_ _publ_author_name 'Poto\N,N^1^)(dicyanamido-\kN')copper(II) perchlorate and \m-dicyanamido-\k^2^N^1^:N^5^-bis[bis(2,2'-bipyridine-\k^2^N,N')copper(II)] triperchlorate ethanol hemisolvate, complexes with unusual dicyanamide coordination ; _journal_issue 10 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m523 _journal_page_last m528 _journal_volume 58 _journal_year 2002 _chemical_formula_iupac '[Cu (C10 H8 N2)2 (C2 N3)] Cl O4' _chemical_formula_moiety 'C22 H16 N7 Cu + , Cl O4 -' _chemical_formula_sum 'C22 H16 Cl Cu N7 O4' _chemical_formula_weight 541.41 _chemical_name_systematic ; Bis(2,2'-bipyridine-\k^2^N,N')(dicyanamido-\kN')copper(II) perchlorate ; _space_group_IT_number 61 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_space_group_name_H-M 'P b c a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL97 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 8.7343(4) _cell_length_b 17.9450(9) _cell_length_c 28.7230(17) _cell_measurement_reflns_used 8000 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.95 _cell_measurement_theta_min 14.3 _cell_volume 4502.0(4) _computing_cell_refinement 'CELL in IPDS' _computing_data_collection 'EXPOSE in IPDS (Stoe & Cie, 1999)' _computing_data_reduction 'INTEGRATE in IPDS' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.971 _diffrn_measured_fraction_theta_max 0.971 _diffrn_measurement_device_type 'Stoe IPDS image-plate' _diffrn_measurement_method 'D = 60mm, \f 0-200\%, \D\f 1.2\%, 1 min/rec' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.062 _diffrn_reflns_av_sigmaI/netI 0.042 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_number 40361 _diffrn_reflns_theta_full 28.06 _diffrn_reflns_theta_max 28.06 _diffrn_reflns_theta_min 2.27 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu 1.135 _exptl_absorpt_correction_T_max 0.792 _exptl_absorpt_correction_T_min 0.627 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'indexed faces' _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.598 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'hexagonal plate' _exptl_crystal_F_000 2200 _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.22 _refine_diff_density_max 0.53 _refine_diff_density_min -0.43 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 316 _refine_ls_number_reflns 5308 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.969 _refine_ls_R_factor_all 0.064 _refine_ls_R_factor_gt 0.036 _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^)+(0.050P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.084 _refine_ls_wR_factor_ref 0.091 _reflns_number_gt 3430 _reflns_number_total 5308 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bm1508.cif _[local]_cod_data_source_block I _cod_database_code 2012965 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' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' 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_type_symbol Cl1 0.30387(8) 0.27579(3) 0.15764(2) 0.0438(2) Uani . . 1.000 Cl O1 0.2975(3) 0.30780(14) 0.11289(9) 0.0894(10) Uani . . 1.000 O O2 0.1895(3) 0.30149(13) 0.18853(11) 0.0958(11) Uani . . 1.000 O O3 0.2929(3) 0.19614(10) 0.15371(7) 0.0668(8) Uani . . 1.000 O O4 0.4494(3) 0.29272(14) 0.17746(8) 0.0736(9) Uani . . 1.000 O Cu1 0.52177(3) 0.059620(10) 0.127510(10) 0.03120(10) Uani . . 1.000 Cu N1 0.0416(3) 0.06184(14) 0.10884(9) 0.0530(9) Uani . . 1.000 N N2 0.3086(3) 0.02478(12) 0.11532(7) 0.0407(8) Uani . . 1.000 N N3 -0.0563(3) 0.15526(14) 0.05380(9) 0.0582(9) Uani . . 1.000 N N10 0.5332(2) 0.10238(10) 0.06321(6) 0.0318(6) Uani . . 1.000 N N20 0.6778(2) -0.01626(10) 0.09462(6) 0.0318(6) Uani . . 1.000 N N30 0.5200(2) 0.01971(10) 0.19221(6) 0.0338(6) Uani . . 1.000 N N40 0.6580(2) 0.13695(10) 0.15901(6) 0.0313(6) Uani . . 1.000 N C2 0.1849(3) 0.04457(13) 0.11080(8) 0.0357(9) Uani . . 1.000 C C3 -0.0047(3) 0.11266(15) 0.07858(9) 0.0421(9) Uani . . 1.000 C C11 0.6236(3) 0.06758(12) 0.03207(7) 0.0309(7) Uani . . 1.000 C C12 0.4526(3) 0.16228(13) 0.05013(8) 0.0410(8) Uani . . 1.000 C C13 0.4626(3) 0.19159(14) 0.00596(8) 0.0450(9) Uani . . 1.000 C C14 0.5552(3) 0.15686(15) -0.02596(8) 0.0463(9) Uani . . 1.000 C C15 0.6357(3) 0.09453(15) -0.01310(8) 0.0421(9) Uani . . 1.000 C C21 0.7072(3) 0.00161(12) 0.05000(8) 0.0323(7) Uani . . 1.000 C C22 0.7511(3) -0.07424(13) 0.11352(9) 0.0395(8) Uani . . 1.000 C C23 0.8558(3) -0.11649(14) 0.08952(10) 0.0495(10) Uani . . 1.000 C C24 0.8854(4) -0.09851(16) 0.04377(11) 0.0557(11) Uani . . 1.000 C C25 0.8111(3) -0.03933(14) 0.02369(10) 0.0465(9) Uani . . 1.000 C C31 0.5937(3) 0.06138(12) 0.22422(7) 0.0318(7) Uani . . 1.000 C C32 0.4489(3) -0.04304(13) 0.20536(8) 0.0404(8) Uani . . 1.000 C C33 0.4501(3) -0.06746(14) 0.25087(8) 0.0451(9) Uani . . 1.000 C C34 0.5212(4) -0.02376(15) 0.28399(8) 0.0495(9) Uani . . 1.000 C C35 0.5930(4) 0.04114(14) 0.27077(8) 0.0442(9) Uani . . 1.000 C C41 0.6758(3) 0.12655(12) 0.20532(7) 0.0337(7) Uani . . 1.000 C C42 0.7350(3) 0.19240(13) 0.13865(8) 0.0383(8) Uani . . 1.000 C C43 0.8338(3) 0.23801(14) 0.16282(10) 0.0471(10) Uani . . 1.000 C C44 0.8512(4) 0.22814(15) 0.20980(10) 0.0532(10) Uani . . 1.000 C C45 0.7697(4) 0.17169(14) 0.23156(9) 0.0459(9) Uani . . 1.000 C H12 0.38770 0.18480 0.07160 0.0490 Uiso calc R 1.000 H H13 0.40770 0.23410 -0.00210 0.0540 Uiso calc R 1.000 H H14 0.56330 0.17540 -0.05610 0.0550 Uiso calc R 1.000 H H15 0.69810 0.07040 -0.03460 0.0510 Uiso calc R 1.000 H H22 0.73030 -0.08650 0.14430 0.0470 Uiso calc R 1.000 H H23 0.90540 -0.15620 0.10380 0.0590 Uiso calc R 1.000 H H24 0.95530 -0.12630 0.02660 0.0670 Uiso calc R 1.000 H H25 0.83000 -0.02670 -0.00720 0.0560 Uiso calc R 1.000 H H32 0.39720 -0.07100 0.18310 0.0480 Uiso calc R 1.000 H H33 0.40400 -0.11230 0.25910 0.0540 Uiso calc R 1.000 H H34 0.52070 -0.03810 0.31510 0.0590 Uiso calc R 1.000 H H35 0.64060 0.07110 0.29290 0.0530 Uiso calc R 1.000 H H42 0.72130 0.20050 0.10690 0.0460 Uiso calc R 1.000 H H43 0.88810 0.27510 0.14740 0.0560 Uiso calc R 1.000 H H44 0.91650 0.25870 0.22680 0.0640 Uiso calc R 1.000 H H45 0.77830 0.16440 0.26350 0.0550 Uiso calc R 1.000 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 Cl1 0.0446(4) 0.0412(3) 0.0456(3) -0.0036(3) 0.0073(3) -0.0040(3) O1 0.107(2) 0.0838(17) 0.0773(16) -0.0198(16) -0.0390(15) 0.0317(13) O2 0.083(2) 0.0655(15) 0.139(2) 0.0185(13) 0.0615(18) -0.0061(15) O3 0.103(2) 0.0405(10) 0.0570(12) -0.0114(11) 0.0199(12) -0.0117(9) O4 0.0645(17) 0.0839(16) 0.0724(15) -0.0103(13) -0.0150(12) -0.0070(12) Cu1 0.0402(2) 0.03260(10) 0.02090(10) 0.00110(10) -0.00020(10) 0.00220(10) N1 0.0380(16) 0.0646(15) 0.0564(14) -0.0041(12) -0.0005(11) 0.0239(12) N2 0.0441(16) 0.0448(12) 0.0332(11) -0.0011(10) -0.0023(10) 0.0052(8) N3 0.0612(19) 0.0603(15) 0.0532(14) 0.0083(13) 0.0057(12) 0.0173(12) N10 0.0401(12) 0.0311(9) 0.0241(8) 0.0026(8) 0.0000(8) 0.0021(7) N20 0.0330(12) 0.0316(9) 0.0309(9) 0.0027(8) -0.0008(8) 0.0005(8) N30 0.0425(13) 0.0348(10) 0.0241(9) 0.0003(9) -0.0019(8) 0.0000(7) N40 0.0361(13) 0.0312(9) 0.0266(9) 0.0043(8) 0.0026(8) -0.0007(7) C2 0.0437(19) 0.0399(13) 0.0236(11) -0.0047(12) -0.0004(10) 0.0038(9) C3 0.0357(17) 0.0491(14) 0.0414(13) 0.0010(11) 0.0041(11) 0.0062(11) C11 0.0329(14) 0.0346(12) 0.0252(10) -0.0040(10) 0.0010(9) -0.0020(9) C12 0.0515(18) 0.0372(12) 0.0342(12) 0.0085(11) 0.0003(11) 0.0040(10) C13 0.0548(19) 0.0401(13) 0.0402(13) -0.0006(12) -0.0050(12) 0.0113(11) C14 0.054(2) 0.0546(15) 0.0302(12) -0.0076(13) -0.0035(11) 0.0152(11) C15 0.0460(18) 0.0542(15) 0.0262(11) -0.0063(12) 0.0058(10) 0.0002(11) C21 0.0313(14) 0.0335(11) 0.0320(11) -0.0048(10) 0.0028(10) -0.0032(9) C22 0.0406(16) 0.0339(13) 0.0439(13) 0.0049(10) -0.0045(11) 0.0035(10) C23 0.0452(18) 0.0371(13) 0.0661(18) 0.0107(12) -0.0027(14) 0.0022(13) C24 0.047(2) 0.0480(16) 0.072(2) 0.0110(13) 0.0160(15) -0.0070(14) C25 0.0475(19) 0.0466(14) 0.0454(14) 0.0018(12) 0.0128(13) -0.0059(11) C31 0.0355(14) 0.0340(11) 0.0258(10) 0.0048(10) -0.0014(9) -0.0016(9) C32 0.0540(18) 0.0367(12) 0.0305(12) -0.0045(11) -0.0035(11) 0.0044(9) C33 0.058(2) 0.0444(13) 0.0329(12) -0.0040(13) -0.0005(11) 0.0100(10) C34 0.068(2) 0.0566(16) 0.0238(11) -0.0026(14) -0.0026(12) 0.0086(11) C35 0.0581(19) 0.0480(14) 0.0266(12) -0.0012(12) -0.0055(11) -0.0003(10) C41 0.0393(16) 0.0327(11) 0.0290(11) 0.0036(10) -0.0008(10) -0.0023(9) C42 0.0400(16) 0.0364(12) 0.0384(13) 0.0021(11) 0.0043(11) 0.0033(10) C43 0.0476(19) 0.0405(14) 0.0531(16) -0.0070(12) 0.0026(13) 0.0037(12) C44 0.057(2) 0.0456(15) 0.0569(18) -0.0120(14) -0.0086(14) -0.0059(13) C45 0.056(2) 0.0437(14) 0.0379(13) -0.0030(12) -0.0083(12) -0.0035(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cu1 N30 . . 1.9916(18) yes Cu1 N40 . . 2.0396(18) yes Cu1 N10 . . 2.0025(18) yes Cu1 N20 . . 2.1457(18) yes Cu1 N2 . . 1.995(3) yes Cl1 O3 . . 1.4370(19) yes Cl1 O4 . . 1.426(3) yes Cl1 O1 . . 1.409(3) yes Cl1 O2 . . 1.413(3) yes N1 C2 . . 1.291(4) yes N1 C3 . . 1.323(4) yes N2 C2 . . 1.145(4) yes N3 C3 . . 1.138(4) yes N10 C11 . . 1.347(3) yes N10 C12 . . 1.339(3) yes N20 C21 . . 1.346(3) yes N20 C22 . . 1.337(3) yes N30 C31 . . 1.349(3) yes N30 C32 . . 1.340(3) yes N40 C41 . . 1.352(3) yes N40 C42 . . 1.336(3) yes C11 C15 . . 1.389(3) no C11 C21 . . 1.483(3) no C12 C13 . . 1.376(3) no C13 C14 . . 1.372(4) no C14 C15 . . 1.372(4) no C21 C25 . . 1.391(4) no C22 C23 . . 1.373(4) no C23 C24 . . 1.378(4) no C24 C25 . . 1.372(4) no C31 C35 . . 1.386(3) no C31 C41 . . 1.475(3) no C32 C33 . . 1.379(3) no C33 C34 . . 1.380(4) no C34 C35 . . 1.376(4) no C41 C45 . . 1.377(4) no C42 C43 . . 1.377(4) no C43 C44 . . 1.369(4) no C44 C45 . . 1.387(4) no C12 H12 . . 0.9300 no C13 H13 . . 0.9303 no C14 H14 . . 0.9301 no C15 H15 . . 0.9305 no C22 H22 . . 0.9290 no C23 H23 . . 0.9294 no C24 H24 . . 0.9299 no C25 H25 . . 0.9305 no C32 H32 . . 0.9298 no C33 H33 . . 0.9303 no C34 H34 . . 0.9299 no C35 H35 . . 0.9306 no C42 H42 . . 0.9312 no C43 H43 . . 0.9296 no C44 H44 . . 0.9298 no C45 H45 . . 0.9297 no 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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 _geom_angle_publ_flag N30 Cu1 N40 80.52(7) yes N2 Cu1 N30 92.51(8) yes N2 Cu1 N40 146.67(8) yes N10 Cu1 N20 78.78(7) yes N10 Cu1 N30 177.17(7) yes N10 Cu1 N40 96.85(7) yes N2 Cu1 N10 90.27(8) yes N2 Cu1 N20 108.46(8) yes N20 Cu1 N40 104.87(7) yes N20 Cu1 N30 100.81(7) yes O1 Cl1 O4 108.22(15) yes O1 Cl1 O3 109.34(14) yes O3 Cl1 O4 107.63(15) yes O2 Cl1 O3 109.07(14) yes O2 Cl1 O4 108.06(15) yes O1 Cl1 O2 114.31(16) yes C2 N1 C3 119.4(2) yes Cu1 N2 C2 143.5(2) yes Cu1 N10 C11 117.65(14) yes Cu1 N10 C12 122.71(15) yes C11 N10 C12 119.62(19) yes Cu1 N20 C21 112.91(14) yes Cu1 N20 C22 128.26(16) yes C21 N20 C22 118.7(2) yes Cu1 N30 C31 115.66(14) yes Cu1 N30 C32 124.66(15) yes C31 N30 C32 119.66(19) yes Cu1 N40 C41 114.17(14) yes Cu1 N40 C42 127.33(15) yes C41 N40 C42 118.40(19) yes N1 C2 N2 174.1(3) yes N1 C3 N3 174.4(3) yes N10 C11 C15 120.2(2) yes N10 C11 C21 115.35(18) yes C15 C11 C21 124.4(2) no N10 C12 C13 122.2(2) yes C12 C13 C14 118.7(2) no C13 C14 C15 119.5(2) no C11 C15 C14 119.8(2) no N20 C21 C11 115.3(2) yes N20 C21 C25 121.1(2) yes C11 C21 C25 123.7(2) no N20 C22 C23 123.0(2) yes C22 C23 C24 118.3(3) no C23 C24 C25 119.6(3) no C21 C25 C24 119.3(3) no N30 C31 C35 120.7(2) yes N30 C31 C41 114.88(18) yes C35 C31 C41 124.4(2) no N30 C32 C33 122.1(2) yes C32 C33 C34 118.4(2) no C33 C34 C35 119.7(2) no C31 C35 C34 119.3(2) no N40 C41 C31 114.55(19) yes N40 C41 C45 121.7(2) yes C31 C41 C45 123.7(2) no N40 C42 C43 122.5(2) yes C42 C43 C44 119.3(2) no C43 C44 C45 118.8(3) no C41 C45 C44 119.2(2) no N10 C12 H12 118.90 no C13 C12 H12 118.94 no C12 C13 H13 120.67 no C14 C13 H13 120.66 no C13 C14 H14 120.28 no C15 C14 H14 120.22 no C11 C15 H15 120.17 no C14 C15 H15 120.06 no N20 C22 H22 118.50 no C23 C22 H22 118.50 no C22 C23 H23 120.81 no C24 C23 H23 120.87 no C23 C24 H24 120.23 no C25 C24 H24 120.19 no C21 C25 H25 120.34 no C24 C25 H25 120.37 no N30 C32 H32 118.99 no C33 C32 H32 118.96 no C32 C33 H33 120.83 no C34 C33 H33 120.73 no C33 C34 H34 120.19 no C35 C34 H34 120.10 no C31 C35 H35 120.38 no C34 C35 H35 120.27 no N40 C42 H42 118.71 no C43 C42 H42 118.78 no C42 C43 H43 120.34 no C44 C43 H43 120.36 no C43 C44 H44 120.62 no C45 C44 H44 120.60 no C41 C45 H45 120.35 no C44 C45 H45 120.40 no