#------------------------------------------------------------------------------ #$Date: 2008-06-25 12:31:45 +0300 (Wed, 25 Jun 2008) $ #$Revision: 403 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/7101618.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_7101618 loop_ _publ_author_name 'Chen, Chun-Long' 'Beatty, Alicia M' _publ_section_title ; From crystal engineering to cluster engineering: How to transform cadmium chloride from 2-D to 0-D. ; _journal_issue 1 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 76 _journal_page_last 78 _journal_year 2007 _chemical_formula_sum 'C64 H88 Cl8 N8' _chemical_formula_weight 1253.02 _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _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 102.936(4) _cell_angle_gamma 90.00 _cell_formula_units_Z 1 _cell_length_a 12.648(3) _cell_length_b 16.387(3) _cell_length_c 8.3423(17) _cell_measurement_reflns_used 2797 _cell_measurement_temperature 300(2) _cell_measurement_theta_max 22.708 _cell_measurement_theta_min 2.797 _cell_volume 1685.2(6) _computing_cell_refinement SMART _computing_data_collection 'SMART (Bruker,1998)' _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_molecular_graphics 'SHELXTL (Bruker, 1998)' _computing_publication_material SHELXTL _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 300(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _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 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0294 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 12085 _diffrn_reflns_theta_full 25.01 _diffrn_reflns_theta_max 25.01 _diffrn_reflns_theta_min 2.07 _exptl_absorpt_coefficient_mu 0.378 _exptl_absorpt_correction_T_max 0.9490 _exptl_absorpt_correction_T_min 0.8453 _exptl_absorpt_correction_type none _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour 'pale yellow' _exptl_crystal_density_diffrn 1.235 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 664 _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.14 _refine_diff_density_max 0.472 _refine_diff_density_min -0.327 _refine_diff_density_rms 0.051 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_hydrogen_treatment none _refine_ls_matrix_type full _refine_ls_number_parameters 191 _refine_ls_number_reflns 2950 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.039 _refine_ls_R_factor_all 0.0662 _refine_ls_R_factor_gt 0.0449 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0643P)^2^+1.1239P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1216 _refine_ls_wR_factor_ref 0.1370 _reflns_number_gt 2179 _reflns_number_total 2950 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file b613761j.txt _[local]_cod_data_source_block diethylbenzidinehydrochloride _[local]_cod_cif_authors_sg_H-M P2(1)/c 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags Cl1 Cl -0.01311(5) 0.50272(4) 0.24705(8) 0.0469(2) Uani 1 1 d . Cl2 Cl -0.00259(6) 0.23109(4) 0.21175(10) 0.0520(2) Uani 1 1 d . N1 N -0.89158(17) 0.36766(14) -0.5301(3) 0.0488(6) Uani 1 1 d . H1A H -0.9274 0.3858 -0.4568 0.073 Uiso 1 1 d R H1B H -0.9057 0.3149 -0.5490 0.073 Uiso 1 1 d R H1C H -0.9125 0.3955 -0.6235 0.073 Uiso 1 1 d R N2 N -0.10191(16) 0.37746(14) -0.0292(3) 0.0441(6) Uani 1 1 d . H2A H -0.0650 0.3887 -0.1057 0.066 Uiso 1 1 d R H2B H -0.0874 0.3267 0.0068 0.066 Uiso 1 1 d R H2C H -0.0825 0.4121 0.0544 0.066 Uiso 1 1 d R C1 C -0.7740(2) 0.37894(17) -0.4653(4) 0.0438(7) Uani 1 1 d . C2 C -0.6996(2) 0.3553(2) -0.5563(4) 0.0540(8) Uani 1 1 d . C3 C -0.5907(2) 0.36540(19) -0.4810(4) 0.0522(8) Uani 1 1 d . H3A H -0.5389 0.3506 -0.5391 0.063 Uiso 1 1 d R C4 C -0.5555(2) 0.39644(18) -0.3241(3) 0.0455(7) Uani 1 1 d . C5 C -0.4371(2) 0.39787(17) -0.2448(3) 0.0435(7) Uani 1 1 d . C6 C -0.3601(2) 0.41530(19) -0.3345(3) 0.0486(7) Uani 1 1 d . H6A H -0.3819 0.4316 -0.4438 0.058 Uiso 1 1 d R C7 C -0.2511(2) 0.40840(18) -0.2625(3) 0.0478(7) Uani 1 1 d . H7A H -0.1995 0.4192 -0.3234 0.057 Uiso 1 1 d R C8 C -0.2190(2) 0.38555(16) -0.1002(3) 0.0411(6) Uani 1 1 d . C9 C -0.2928(2) 0.37084(19) -0.0039(3) 0.0493(7) Uani 1 1 d . C10 C -0.4018(2) 0.37732(18) -0.0807(4) 0.0504(7) Uani 1 1 d . H10A H -0.4533 0.3673 -0.0191 0.060 Uiso 1 1 d R C11 C -0.6330(2) 0.4210(2) -0.2404(4) 0.0529(8) Uani 1 1 d . H11A H -0.6116 0.4433 -0.1356 0.063 Uiso 1 1 d R C12 C -0.7417(2) 0.41213(19) -0.3112(4) 0.0531(8) Uani 1 1 d . H12A H -0.7934 0.4287 -0.2543 0.064 Uiso 1 1 d R C13 C -0.7319(3) 0.3184(3) -0.7267(4) 0.0883(14) Uani 1 1 d . H13A H -0.7903 0.2808 -0.7273 0.106 Uiso 1 1 d R H13B H -0.6712 0.2873 -0.7445 0.106 Uiso 1 1 d R C14 C -0.7647(6) 0.3715(4) -0.8616(8) 0.0786(19) Uani 0.60 1 d P H14A H -0.7828 0.3414 -0.9628 0.118 Uiso 0.60 1 d PR H14B H -0.8269 0.4019 -0.8476 0.118 Uiso 0.60 1 d PR H14C H -0.7063 0.4085 -0.8649 0.118 Uiso 0.60 1 d PR C14' C -0.6745(13) 0.3526(9) -0.8443(15) 0.126(5) Uani 0.40 1 d P H14D H -0.6965 0.3261 -0.9492 0.189 Uiso 0.40 1 d PR H14E H -0.6937 0.4093 -0.8554 0.189 Uiso 0.40 1 d PR H14F H -0.5974 0.3474 -0.8056 0.189 Uiso 0.40 1 d PR C15 C -0.2559(3) 0.3471(3) 0.1749(4) 0.0780(11) Uani 1 1 d . H15A H -0.2100 0.2993 0.1806 0.094 Uiso 1 1 d R H15B H -0.2111 0.3909 0.2318 0.094 Uiso 1 1 d R C16 C -0.3389(4) 0.3296(3) 0.2648(5) 0.0956(14) Uani 1 1 d . H16A H -0.3054 0.3156 0.3763 0.143 Uiso 1 1 d R H16B H -0.3823 0.2846 0.2135 0.143 Uiso 1 1 d R H16C H -0.3840 0.3767 0.2637 0.143 Uiso 1 1 d R 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 Cl1 0.0414(4) 0.0467(4) 0.0527(4) 0.0017(3) 0.0109(3) 0.0023(3) Cl2 0.0489(4) 0.0480(4) 0.0609(5) 0.0028(3) 0.0163(3) 0.0019(3) N1 0.0318(12) 0.0597(15) 0.0517(15) 0.0123(11) 0.0024(10) -0.0021(10) N2 0.0299(12) 0.0569(15) 0.0442(13) -0.0013(11) 0.0054(10) 0.0013(10) C1 0.0275(13) 0.0502(16) 0.0493(17) 0.0105(13) -0.0004(12) 0.0008(11) C2 0.0385(16) 0.078(2) 0.0445(17) 0.0021(15) 0.0069(13) -0.0099(15) C3 0.0338(15) 0.078(2) 0.0451(17) -0.0032(15) 0.0104(13) -0.0055(14) C4 0.0323(14) 0.0544(17) 0.0478(17) 0.0029(13) 0.0045(12) 0.0016(12) C5 0.0305(14) 0.0517(17) 0.0463(16) -0.0037(13) 0.0046(12) 0.0021(12) C6 0.0360(15) 0.0653(19) 0.0421(16) 0.0056(14) 0.0036(12) -0.0020(13) C7 0.0335(14) 0.0646(19) 0.0455(16) 0.0012(14) 0.0089(12) -0.0060(13) C8 0.0275(13) 0.0493(16) 0.0447(16) -0.0045(12) 0.0041(11) -0.0006(11) C9 0.0345(15) 0.072(2) 0.0417(16) 0.0036(14) 0.0085(12) 0.0054(13) C10 0.0311(14) 0.075(2) 0.0460(17) 0.0036(14) 0.0112(12) 0.0018(13) C11 0.0367(16) 0.069(2) 0.0498(17) -0.0099(15) 0.0039(13) 0.0089(14) C12 0.0303(15) 0.067(2) 0.061(2) -0.0064(16) 0.0085(13) 0.0089(13) C13 0.056(2) 0.151(4) 0.058(2) -0.023(3) 0.0128(18) -0.037(2) C14 0.079(5) 0.091(5) 0.063(4) 0.000(3) 0.011(4) -0.003(4) C14' 0.144(13) 0.178(14) 0.072(8) -0.043(8) 0.057(9) -0.063(11) C15 0.0429(19) 0.138(3) 0.053(2) 0.022(2) 0.0105(15) 0.009(2) C16 0.101(3) 0.124(4) 0.066(3) 0.022(2) 0.028(2) 0.000(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance N1 C1 1.476(3) N1 H1A 0.8901 N1 H1B 0.8900 N1 H1C 0.8900 N2 C8 1.472(3) N2 H2A 0.8901 N2 H2B 0.8900 N2 H2C 0.8900 C1 C12 1.371(4) C1 C2 1.389(4) C2 C3 1.390(4) C2 C13 1.515(5) C3 C4 1.382(4) C3 H3A 0.9300 C4 C11 1.384(4) C4 C5 1.495(4) C5 C10 1.383(4) C5 C6 1.385(4) C6 C7 1.379(4) C6 H6A 0.9300 C7 C8 1.376(4) C7 H7A 0.9300 C8 C9 1.382(4) C9 C10 1.389(4) C9 C15 1.510(4) C10 H10A 0.9302 C11 C12 1.378(4) C11 H11A 0.9300 C12 H12A 0.9299 C13 C14 1.410(7) C13 C14' 1.457(12) C13 H13A 0.9601 C13 H13B 0.9600 C14 C14' 1.160(15) C14 H14A 0.9600 C14 H14B 0.9602 C14 H14C 0.9600 C14 H14D 1.4530 C14 H14E 1.0826 C14' H13B 1.3504 C14' H14A 1.5103 C14' H14C 0.9997 C14' H14D 0.9599 C14' H14E 0.9601 C14' H14F 0.9600 C15 C16 1.449(5) C15 H15A 0.9699 C15 H15B 0.9700 C16 H16A 0.9600 C16 H16B 0.9600 C16 H16C 0.9600 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C1 N1 H1A 109.5 C1 N1 H1B 109.4 H1A N1 H1B 109.5 C1 N1 H1C 109.5 H1A N1 H1C 109.5 H1B N1 H1C 109.5 C8 N2 H2A 109.5 C8 N2 H2B 109.4 H2A N2 H2B 109.5 C8 N2 H2C 109.5 H2A N2 H2C 109.5 H2B N2 H2C 109.5 C12 C1 C2 121.8(2) C12 C1 N1 117.2(3) C2 C1 N1 121.0(3) C1 C2 C3 116.4(3) C1 C2 C13 123.4(3) C3 C2 C13 120.2(3) C4 C3 C2 123.2(3) C4 C3 H3A 118.4 C2 C3 H3A 118.4 C3 C4 C11 118.1(3) C3 C4 C5 120.2(3) C11 C4 C5 121.6(3) C10 C5 C6 118.4(2) C10 C5 C4 120.2(2) C6 C5 C4 121.3(2) C7 C6 C5 120.2(3) C7 C6 H6A 119.9 C5 C6 H6A 119.9 C8 C7 C6 119.9(3) C8 C7 H7A 120.0 C6 C7 H7A 120.1 C7 C8 C9 122.0(2) C7 C8 N2 118.0(2) C9 C8 N2 120.0(2) C8 C9 C10 116.6(3) C8 C9 C15 121.3(3) C10 C9 C15 122.1(3) C5 C10 C9 122.9(3) C5 C10 H10A 118.6 C9 C10 H10A 118.5 C12 C11 C4 120.3(3) C12 C11 H11A 119.8 C4 C11 H11A 119.9 C1 C12 C11 120.2(3) C1 C12 H12A 119.9 C11 C12 H12A 119.9 C14 C13 C14' 47.7(7) C14 C13 C2 118.1(5) C14' C13 C2 114.1(5) C14 C13 H13A 107.6 C14' C13 H13A 137.8 C2 C13 H13A 107.9 C14 C13 H13B 107.8 C14' C13 H13B 64.1 C2 C13 H13B 107.5 H13A C13 H13B 107.4 C14' C14 C13 68.3(8) C14' C14 H14A 90.4 C13 C14 H14A 110.7 C14' C14 H14B 159.0 C13 C14 H14B 109.0 H14A C14 H14B 109.5 C14' C14 H14C 55.3 C13 C14 H14C 108.7 H14A C14 H14C 109.5 H14B C14 H14C 109.5 C14' C14 H14D 41.2 C13 C14 H14D 89.1 H14A C14 H14D 49.2 H14B C14 H14D 157.1 H14C C14 H14D 76.2 C14' C14 H14E 50.6 C13 C14 H14E 102.8 H14A C14 H14E 111.6 H14B C14 H14E 113.0 H14C C14 H14E 6.0 H14D C14 H14E 74.8 C14 C14' C13 64.0(7) C14 C14' H13B 100.5 C13 C14' H13B 39.8 C14 C14' H14A 39.5 C13 C14' H14A 83.0 H13B C14' H14A 101.9 C14 C14' H14C 52.1 C13 C14' H14C 103.0 H13B C14' H14C 141.9 H14A C14' H14C 74.2 C14 C14' H14D 86.0 C13 C14' H14D 110.7 H13B C14' H14D 99.6 H14A C14' H14D 46.6 H14C C14' H14D 103.5 C14 C14' H14E 60.5 C13 C14' H14E 106.5 H13B C14' H14E 143.0 H14A C14' H14E 83.2 H14C C14' H14E 9.2 H14D C14' H14E 109.5 C14 C14' H14F 164.2 C13 C14' H14F 111.2 H13B C14' H14F 80.5 H14A C14' H14F 156.1 H14C C14' H14F 118.5 H14D C14' H14F 109.5 H14E C14' H14F 109.5 C16 C15 C9 117.5(3) C16 C15 H15A 108.0 C9 C15 H15A 107.8 C16 C15 H15B 107.8 C9 C15 H15B 108.1 H15A C15 H15B 107.2 C15 C16 H16A 109.6 C15 C16 H16B 109.3 H16A C16 H16B 109.5 C15 C16 H16C 109.5 H16A C16 H16C 109.5 H16B C16 H16C 109.5 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 _geom_hbond_site_symmetry_A N2 H2A Cl1 0.89 2.46 3.234(2) 145.5 3_565 N2 H2A Cl2 0.89 2.71 3.260(2) 121.3 4_565 N2 H2B Cl2 0.89 2.39 3.200(2) 151.7 . N2 H2C Cl1 0.89 2.22 3.103(2) 171.5 . N1 H1A Cl2 0.89 2.67 3.151(2) 114.7 4_465 N1 H1A Cl1 0.89 2.75 3.580(3) 156.0 3_465 N1 H1B Cl2 0.89 2.50 3.204(3) 135.8 1_454 N1 H1C Cl1 0.89 2.29 3.072(2) 146.0 1_454