#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/7101734.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7101734 loop_ _publ_author_name 'Steed, Jonathan W' 'Goeta, Andr\'es E' 'Lipkowski, Janusz' 'Swierczynski, Dariusz' 'Panteleon, Vicky' 'Handa, Sheetal' _publ_section_title ; Templated crystal nucleation: mixed crystals of very different copper(II) N,N',N''-trimethyltriazacyclononane complexes. ; _journal_issue 8 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 813 _journal_page_last 815 _journal_year 2007 _chemical_formula_sum 'C9.5 H22 Cl3 Cu N3' _[local]_cod_chemical_formula_sum_orig 'C9.50 H22 Cl3 Cu N3' _chemical_formula_weight 348.19 _chemical_name_systematic ; ? ; _space_group_IT_number 60 _symmetry_cell_setting ORTHORHOMBIC _symmetry_space_group_name_Hall '-P 2n 2ab' _symmetry_space_group_name_H-M 'P b c n' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 13.7910(3) _cell_length_b 14.5310(2) _cell_length_c 15.0530(4) _cell_measurement_temperature 293(2) _cell_volume 3016.58(11) _computing_molecular_graphics 'RES2INS (Barbour, 1995)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.933 _diffrn_measured_fraction_theta_max 0.933 _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi scans 2o frames DX=25mm' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71070 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0244 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 33372 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 4.17 _exptl_absorpt_coefficient_mu 1.961 _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.533 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1440 _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.531 _refine_diff_density_min -0.391 _refine_diff_density_rms 0.061 _refine_ls_extinction_coef 0.0053(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 151 _refine_ls_number_reflns 2580 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.031 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0371 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0554P)^2^+3.8144P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_gt 0.1008 _refine_ls_wR_factor_ref 0.1039 _reflns_number_gt 2397 _reflns_number_total 2580 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file b614043b.txt _[local]_cod_data_source_block tacncu _[local]_cod_cif_authors_sg_H-M Pbcn 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' Cu Cu 0.3201 1.2651 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z' 'x, -y, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z' '-x, y, -z-1/2' 'x-1/2, y-1/2, -z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags Cu1 Cu 0.04249(2) 0.16340(2) 0.49108(2) 0.03320(18) Uani 1 d . Cl1 Cl -0.06294(6) 0.21605(6) 0.59848(5) 0.0521(3) Uani 1 d . Cl2 Cl -0.08229(6) 0.12998(8) 0.39971(6) 0.0688(3) Uani 1 d . Cl3 Cl 0.60305(9) 0.02822(9) 0.27327(9) 0.0865(4) Uani 1 d . N1 N 0.16105(18) 0.16990(18) 0.57837(17) 0.0420(6) Uani 1 d . N2 N 0.14702(18) 0.10893(17) 0.40316(16) 0.0411(6) Uani 1 d . N3 N 0.10074(18) 0.29775(17) 0.44339(19) 0.0476(6) Uani 1 d . C1 C 0.2450(3) 0.1239(4) 0.5371(3) 0.0756(12) Uani 1 d . H1A H 0.2915 0.1704 0.5190 0.091 Uiso 1 calc R H1B H 0.2762 0.0852 0.5811 0.091 Uiso 1 calc R C2 C 0.2209(3) 0.0691(3) 0.4621(3) 0.0741(12) Uani 1 d . H2A H 0.1979 0.0098 0.4829 0.089 Uiso 1 calc R H2B H 0.2794 0.0584 0.4278 0.089 Uiso 1 calc R C3 C 0.1877(3) 0.1859(3) 0.3503(3) 0.0705(11) Uani 1 d . H3A H 0.2544 0.1954 0.3687 0.085 Uiso 1 calc R H3B H 0.1888 0.1675 0.2884 0.085 Uiso 1 calc R C4 C 0.1372(4) 0.2732(3) 0.3567(3) 0.0798(13) Uani 1 d . H4A H 0.1809 0.3214 0.3371 0.096 Uiso 1 calc R H4B H 0.0830 0.2720 0.3157 0.096 Uiso 1 calc R C5 C 0.1765(4) 0.3237(3) 0.5075(3) 0.0745(13) Uani 1 d . H5A H 0.2391 0.3184 0.4784 0.089 Uiso 1 calc R H5B H 0.1676 0.3879 0.5232 0.089 Uiso 1 calc R C6 C 0.1790(4) 0.2698(3) 0.5886(3) 0.0755(12) Uani 1 d . H6A H 0.1309 0.2945 0.6292 0.091 Uiso 1 calc R H6B H 0.2420 0.2780 0.6161 0.091 Uiso 1 calc R C7 C 0.1418(3) 0.1295(3) 0.6663(2) 0.0688(11) Uani 1 d . H7A H 0.0881 0.1608 0.6935 0.083 Uiso 1 calc R H7B H 0.1982 0.1359 0.7031 0.083 Uiso 1 calc R H7C H 0.1264 0.0654 0.6597 0.083 Uiso 1 calc R C8 C 0.1134(3) 0.0342(3) 0.3442(3) 0.0762(12) Uani 1 d . H8A H 0.0711 0.0591 0.2996 0.091 Uiso 1 calc R H8B H 0.0790 -0.0109 0.3785 0.091 Uiso 1 calc R H8C H 0.1683 0.0058 0.3161 0.091 Uiso 1 calc R C9 C 0.0257(3) 0.3688(3) 0.4360(4) 0.0853(15) Uani 1 d . H9A H 0.0545 0.4252 0.4159 0.102 Uiso 1 calc R H9B H -0.0038 0.3783 0.4930 0.102 Uiso 1 calc R H9C H -0.0227 0.3493 0.3942 0.102 Uiso 1 calc R C1S C 0.5000 0.0950(4) 0.2500 0.0761(16) Uani 1 d S H1S1 H 0.4864 0.1344 0.3005 0.091 Uiso 0.50 calc PR H1S2 H 0.5136 0.1344 0.1995 0.091 Uiso 0.50 calc PR 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 Cu1 0.0271(2) 0.0372(3) 0.0353(2) 0.00144(13) 0.00019(12) -0.00205(12) Cl1 0.0374(4) 0.0680(5) 0.0509(5) -0.0081(4) 0.0082(3) 0.0020(3) Cl2 0.0373(4) 0.1090(8) 0.0600(6) -0.0225(5) -0.0081(4) -0.0051(4) Cl3 0.0812(8) 0.0792(8) 0.0989(9) -0.0046(6) -0.0057(6) 0.0060(5) N1 0.0348(12) 0.0547(16) 0.0365(13) 0.0016(10) -0.0030(10) -0.0027(10) N2 0.0391(13) 0.0452(14) 0.0390(13) -0.0039(10) 0.0020(10) -0.0001(10) N3 0.0400(13) 0.0401(14) 0.0629(17) 0.0145(12) 0.0086(12) 0.0035(11) C1 0.050(2) 0.120(4) 0.058(2) -0.003(2) -0.0106(18) 0.036(2) C2 0.061(2) 0.091(3) 0.070(2) -0.013(2) -0.007(2) 0.040(2) C3 0.080(3) 0.072(2) 0.060(2) 0.0103(19) 0.033(2) 0.002(2) C4 0.098(3) 0.071(3) 0.071(3) 0.032(2) 0.030(2) 0.010(2) C5 0.074(3) 0.042(2) 0.107(4) -0.0024(19) -0.011(2) -0.0164(18) C6 0.081(3) 0.075(3) 0.070(3) -0.006(2) -0.019(2) -0.032(2) C7 0.059(2) 0.104(3) 0.0431(19) 0.017(2) -0.0087(16) -0.003(2) C8 0.067(2) 0.081(3) 0.081(3) -0.042(2) 0.011(2) -0.010(2) C9 0.066(3) 0.056(2) 0.134(4) 0.039(3) 0.021(3) 0.0179(19) C1S 0.087(4) 0.054(3) 0.087(4) 0.000 -0.013(3) 0.000 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Cu1 N1 2.100(2) . Cu1 N2 2.111(2) . Cu1 N3 2.230(2) . Cu1 Cl2 2.2558(9) . Cu1 Cl1 2.3050(8) . Cl3 C1S 1.756(4) . N1 C7 1.472(4) . N1 C1 1.475(4) . N1 C6 1.481(5) . N2 C2 1.470(4) . N2 C8 1.478(4) . N2 C3 1.483(4) . N3 C4 1.443(5) . N3 C9 1.466(4) . N3 C5 1.471(5) . C1 C2 1.420(6) . C3 C4 1.450(6) . C5 C6 1.451(6) . C1S Cl3 1.756(4) 7_656 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 N1 Cu1 N2 82.96(10) . N1 Cu1 N3 83.20(10) . N2 Cu1 N3 83.13(10) . N1 Cu1 Cl2 170.15(8) . N2 Cu1 Cl2 93.32(7) . N3 Cu1 Cl2 105.49(8) . N1 Cu1 Cl1 92.14(7) . N2 Cu1 Cl1 174.24(7) . N3 Cu1 Cl1 99.35(7) . Cl2 Cu1 Cl1 91.03(3) . C7 N1 C1 109.9(3) . C7 N1 C6 109.1(3) . C1 N1 C6 110.9(3) . C7 N1 Cu1 113.8(2) . C1 N1 Cu1 109.1(2) . C6 N1 Cu1 103.9(2) . C2 N2 C8 106.9(3) . C2 N2 C3 111.0(3) . C8 N2 C3 110.5(3) . C2 N2 Cu1 104.0(2) . C8 N2 Cu1 116.0(2) . C3 N2 Cu1 108.2(2) . C4 N3 C9 110.6(3) . C4 N3 C5 114.1(3) . C9 N3 C5 111.8(4) . C4 N3 Cu1 101.5(2) . C9 N3 Cu1 112.7(2) . C5 N3 Cu1 105.6(2) . C2 C1 N1 113.9(3) . C1 C2 N2 114.9(3) . C4 C3 N2 116.2(3) . N3 C4 C3 116.4(3) . C6 C5 N3 115.5(3) . C5 C6 N1 115.9(3) . Cl3 C1S Cl3 112.9(3) 7_656 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 N2 Cu1 N1 C7 -130.3(3) N3 Cu1 N1 C7 145.8(3) Cl2 Cu1 N1 C7 -62.0(5) Cl1 Cu1 N1 C7 46.7(3) N2 Cu1 N1 C1 -7.2(3) N3 Cu1 N1 C1 -91.0(3) Cl2 Cu1 N1 C1 61.2(5) Cl1 Cu1 N1 C1 169.8(3) N2 Cu1 N1 C6 111.2(2) N3 Cu1 N1 C6 27.3(2) Cl2 Cu1 N1 C6 179.5(4) Cl1 Cu1 N1 C6 -71.9(2) N1 Cu1 N2 C2 25.4(3) N3 Cu1 N2 C2 109.3(3) Cl2 Cu1 N2 C2 -145.5(2) Cl1 Cu1 N2 C2 -6.5(9) N1 Cu1 N2 C8 142.4(3) N3 Cu1 N2 C8 -133.6(3) Cl2 Cu1 N2 C8 -28.4(3) Cl1 Cu1 N2 C8 110.6(7) N1 Cu1 N2 C3 -92.7(2) N3 Cu1 N2 C3 -8.8(2) Cl2 Cu1 N2 C3 96.4(2) Cl1 Cu1 N2 C3 -124.6(7) N1 Cu1 N3 C4 109.8(3) N2 Cu1 N3 C4 26.1(2) Cl2 Cu1 N3 C4 -65.5(2) Cl1 Cu1 N3 C4 -159.2(2) N1 Cu1 N3 C9 -131.9(3) N2 Cu1 N3 C9 144.4(3) Cl2 Cu1 N3 C9 52.9(3) Cl1 Cu1 N3 C9 -40.8(3) N1 Cu1 N3 C5 -9.5(3) N2 Cu1 N3 C5 -93.2(3) Cl2 Cu1 N3 C5 175.2(2) Cl1 Cu1 N3 C5 81.5(2) C7 N1 C1 C2 111.2(4) C6 N1 C1 C2 -128.1(4) Cu1 N1 C1 C2 -14.3(5) N1 C1 C2 N2 39.6(6) C8 N2 C2 C1 -165.6(4) C3 N2 C2 C1 73.8(5) Cu1 N2 C2 C1 -42.4(5) C2 N2 C3 C4 -124.9(4) C8 N2 C3 C4 116.7(4) Cu1 N2 C3 C4 -11.3(5) C9 N3 C4 C3 -161.2(4) C5 N3 C4 C3 71.8(5) Cu1 N3 C4 C3 -41.3(5) N2 C3 C4 N3 38.8(6) C4 N3 C5 C6 -122.6(4) C9 N3 C5 C6 111.0(4) Cu1 N3 C5 C6 -12.0(5) N3 C5 C6 N1 39.5(6) C7 N1 C6 C5 -166.0(4) C1 N1 C6 C5 72.8(5) Cu1 N1 C6 C5 -44.3(5) _cod_database_code 7101734