#------------------------------------------------------------------------------ #$Date: 2016-03-26 17:22:32 +0200 (Sat, 26 Mar 2016) $ #$Revision: 180390 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/20/59/7205945.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_7205945 loop_ _publ_author_name 'Song, Jiao' 'Hou, Yajie' 'Zhang, Lifang' 'Fu, Yunlong' _publ_section_title ; Synthesis and photoluminescent properties of two 2D and 3D iodocuprates modified by a protonated ligand ; _journal_issue 11 _journal_name_full CrystEngComm _journal_page_first 3750 _journal_paper_doi 10.1039/c1ce05020f _journal_volume 13 _journal_year 2011 _chemical_formula_sum 'C8 H16 Cu4 I5 N3' _chemical_formula_weight 1042.90 _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 94.213(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 8.7682(10) _cell_length_b 16.8580(19) _cell_length_c 13.7225(15) _cell_measurement_temperature 298(2) _cell_volume 2022.9(4) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _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 0.0209 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 11263 _diffrn_reflns_theta_full 26.00 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_min 1.92 _exptl_absorpt_coefficient_mu 11.771 _exptl_absorpt_correction_T_max 0.4527 _exptl_absorpt_correction_T_min 0.2895 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 3.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1864 _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.515 _refine_diff_density_min -0.781 _refine_diff_density_rms 0.130 _refine_ls_extinction_coef 0.00124(5) _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 1.010 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 187 _refine_ls_number_reflns 3974 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.009 _refine_ls_R_factor_all 0.0268 _refine_ls_R_factor_gt 0.0223 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0258P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.0504 _reflns_number_gt 3524 _reflns_number_total 3974 _reflns_threshold_expression >2sigma(I) _cod_data_source_file c1ce05020f.txt _cod_data_source_block aa _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius ; _cod_original_sg_symbol_H-M 'P2(1)/c ' _cod_database_code 7205945 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 _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.97942(3) 0.183125(17) 0.58200(2) 0.03311(8) Uani 1 1 d . . . I2 I 0.46007(3) 0.209543(16) 0.54926(2) 0.03233(8) Uani 1 1 d . . . I3 I 0.74823(4) 0.415454(17) 0.55613(2) 0.03768(9) Uani 1 1 d . . . I4 I 0.71603(3) 0.241199(17) 0.808249(19) 0.03468(9) Uani 1 1 d . . . I5 I 0.28789(3) -0.014454(16) 0.58823(2) 0.03250(8) Uani 1 1 d . . . Cu1 Cu 0.71420(7) 0.16475(3) 0.46212(4) 0.04234(15) Uani 1 1 d . . . Cu2 Cu 0.73107(7) 0.26494(3) 0.61453(4) 0.03977(15) Uani 1 1 d . . . Cu3 Cu 0.45093(7) 0.07038(3) 0.46250(4) 0.03728(14) Uani 1 1 d . . . Cu4 Cu 0.89879(7) 0.30289(4) 0.46174(5) 0.04870(17) Uani 1 1 d . . . N1 N 0.3024(4) 0.07061(19) 0.3322(2) 0.0256(7) Uani 1 1 d . . . N2 N 0.1147(4) 0.0695(2) 0.1835(3) 0.0385(9) Uani 1 1 d D . . N3 N 1.0910(5) 0.3437(3) 0.4124(3) 0.0482(10) Uani 1 1 d . . . C1 C 0.2673(6) -0.0105(3) 0.3009(3) 0.0461(13) Uani 1 1 d . . . H1A H 0.2358 -0.0408 0.3560 0.055 Uiso 1 1 calc R . . H1B H 0.3587 -0.0350 0.2788 0.055 Uiso 1 1 calc R . . C2 C 0.1413(6) -0.0131(3) 0.2188(3) 0.0488(13) Uani 1 1 d . . . H2A H 0.1717 -0.0465 0.1660 0.059 Uiso 1 1 calc R . . H2B H 0.0484 -0.0346 0.2426 0.059 Uiso 1 1 calc R . . C3 C 0.1594(6) 0.1095(4) 0.3540(4) 0.0539(15) Uani 1 1 d . . . H3A H 0.1819 0.1614 0.3821 0.065 Uiso 1 1 calc R . . H3B H 0.1094 0.0783 0.4019 0.065 Uiso 1 1 calc R . . C4 C 0.0512(6) 0.1186(3) 0.2613(3) 0.0516(14) Uani 1 1 d . . . H4A H -0.0507 0.1006 0.2734 0.062 Uiso 1 1 calc R . . H4B H 0.0453 0.1738 0.2414 0.062 Uiso 1 1 calc R . . C5 C 0.3650(6) 0.1128(3) 0.2506(3) 0.0515(14) Uani 1 1 d . . . H5A H 0.4653 0.0916 0.2400 0.062 Uiso 1 1 calc R . . H5B H 0.3769 0.1685 0.2671 0.062 Uiso 1 1 calc R . . C6 C 0.2616(6) 0.1048(3) 0.1567(3) 0.0508(14) Uani 1 1 d . . . H6A H 0.2435 0.1564 0.1268 0.061 Uiso 1 1 calc R . . H6B H 0.3091 0.0709 0.1105 0.061 Uiso 1 1 calc R . . C7 C 1.2007(6) 0.3579(3) 0.3776(4) 0.0449(12) Uani 1 1 d . . . C8 C 1.3418(6) 0.3763(4) 0.3329(5) 0.0691(17) Uani 1 1 d . . . H8A H 1.3511 0.4328 0.3262 0.104 Uiso 1 1 calc R . . H8B H 1.3403 0.3519 0.2697 0.104 Uiso 1 1 calc R . . H8C H 1.4273 0.3565 0.3735 0.104 Uiso 1 1 calc R . . H1 H 0.043(5) 0.068(3) 0.134(3) 0.063(17) Uiso 1 1 d D . . 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 I1 0.03004(17) 0.03659(17) 0.03280(15) -0.00074(12) 0.00296(12) 0.00442(12) I2 0.02709(16) 0.03386(16) 0.03632(16) -0.00912(12) 0.00418(12) -0.00308(12) I3 0.0443(2) 0.02952(16) 0.03813(16) -0.00032(12) -0.00463(13) 0.00036(12) I4 0.04230(19) 0.03927(18) 0.02262(14) -0.00076(11) 0.00333(12) 0.00106(13) I5 0.03480(18) 0.02881(16) 0.03447(16) 0.00005(12) 0.00645(12) 0.00084(12) Cu1 0.0499(4) 0.0360(3) 0.0415(3) -0.0018(3) 0.0063(3) -0.0027(3) Cu2 0.0379(3) 0.0442(3) 0.0375(3) -0.0029(3) 0.0050(2) -0.0015(3) Cu3 0.0361(3) 0.0394(3) 0.0353(3) -0.0025(2) -0.0047(2) 0.0018(2) Cu4 0.0421(4) 0.0557(4) 0.0484(4) 0.0080(3) 0.0036(3) -0.0059(3) N1 0.0274(19) 0.0263(18) 0.0227(16) -0.0024(13) -0.0010(14) 0.0023(14) N2 0.036(2) 0.052(3) 0.0259(19) -0.0007(17) -0.0079(16) -0.0046(18) N3 0.040(3) 0.052(3) 0.053(3) 0.013(2) 0.003(2) -0.004(2) C1 0.061(4) 0.031(3) 0.044(3) -0.001(2) -0.015(2) -0.003(2) C2 0.066(4) 0.038(3) 0.040(3) -0.002(2) -0.015(2) -0.012(2) C3 0.046(3) 0.074(4) 0.040(3) -0.015(3) -0.011(2) 0.027(3) C4 0.039(3) 0.070(4) 0.045(3) -0.003(3) -0.003(2) 0.021(3) C5 0.042(3) 0.072(4) 0.039(3) 0.016(3) -0.005(2) -0.018(3) C6 0.045(3) 0.074(4) 0.033(3) 0.014(2) -0.002(2) -0.016(3) C7 0.048(3) 0.036(3) 0.051(3) 0.007(2) 0.005(3) -0.001(2) C8 0.053(4) 0.075(4) 0.083(4) 0.013(3) 0.034(3) 0.008(3) 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' I I -0.4742 1.8119 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cu2 I1 Cu4 61.69(2) . . ? Cu2 I1 Cu1 59.449(19) . . ? Cu4 I1 Cu1 62.88(2) . . ? Cu3 I2 Cu2 117.69(2) . . ? Cu3 I2 Cu1 63.300(19) . . ? Cu2 I2 Cu1 60.084(19) . . ? Cu2 I3 Cu4 61.02(2) . . ? Cu1 I4 Cu4 64.72(2) 4_566 4_566 ? Cu1 I4 Cu2 134.54(2) 4_566 . ? Cu4 I4 Cu2 138.71(2) 4_566 . ? Cu3 I5 Cu1 64.649(19) 3_656 3_656 ? Cu3 I5 Cu3 60.71(2) 3_656 . ? Cu1 I5 Cu3 109.49(2) 3_656 . ? I5 Cu1 I4 111.66(2) 3_656 4_565 ? I5 Cu1 Cu2 144.21(3) 3_656 . ? I4 Cu1 Cu2 104.00(3) 4_565 . ? I5 Cu1 I2 113.24(2) 3_656 . ? I4 Cu1 I2 103.81(2) 4_565 . ? Cu2 Cu1 I2 58.755(19) . . ? I5 Cu1 I1 104.71(2) 3_656 . ? I4 Cu1 I1 110.74(2) 4_565 . ? Cu2 Cu1 I1 58.007(18) . . ? I2 Cu1 I1 112.88(2) . . ? I5 Cu1 Cu3 57.532(18) 3_656 . ? I4 Cu1 Cu3 113.29(2) 4_565 . ? Cu2 Cu1 Cu3 110.72(3) . . ? I2 Cu1 Cu3 56.906(19) . . ? I1 Cu1 Cu3 135.96(3) . . ? I5 Cu1 Cu4 141.70(3) 3_656 . ? I4 Cu1 Cu4 57.910(19) 4_565 . ? Cu2 Cu1 Cu4 59.06(2) . . ? I2 Cu1 Cu4 105.05(3) . . ? I1 Cu1 Cu4 56.912(18) . . ? Cu3 Cu1 Cu4 159.38(3) . . ? I1 Cu2 I2 119.27(2) . . ? I1 Cu2 I3 112.34(2) . . ? I2 Cu2 I3 107.63(2) . . ? I1 Cu2 Cu1 62.54(2) . . ? I2 Cu2 Cu1 61.161(19) . . ? I3 Cu2 Cu1 111.44(3) . . ? I1 Cu2 I4 100.91(2) . . ? I2 Cu2 I4 99.97(2) . . ? I3 Cu2 I4 116.38(2) . . ? Cu1 Cu2 I4 132.05(3) . . ? I1 Cu2 Cu4 59.64(2) . . ? I2 Cu2 Cu4 110.14(2) . . ? I3 Cu2 Cu4 60.00(2) . . ? Cu1 Cu2 Cu4 63.26(2) . . ? I4 Cu2 Cu4 149.37(3) . . ? N1 Cu3 I5 105.66(9) . 3_656 ? N1 Cu3 I2 111.98(9) . . ? I5 Cu3 I2 116.34(2) 3_656 . ? N1 Cu3 Cu3 118.59(9) . 3_656 ? I5 Cu3 Cu3 61.62(2) 3_656 3_656 ? I2 Cu3 Cu3 127.80(3) . 3_656 ? N1 Cu3 I5 102.43(9) . . ? I5 Cu3 I5 119.29(2) 3_656 . ? I2 Cu3 I5 100.46(2) . . ? Cu3 Cu3 I5 57.67(2) 3_656 . ? N1 Cu3 Cu1 116.71(9) . . ? I5 Cu3 Cu1 57.82(2) 3_656 . ? I2 Cu3 Cu1 59.794(18) . . ? Cu3 Cu3 Cu1 105.06(3) 3_656 . ? I5 Cu3 Cu1 140.27(2) . . ? N3 Cu4 I4 107.70(12) . 4_565 ? N3 Cu4 I1 106.25(12) . . ? I4 Cu4 I1 113.28(3) 4_565 . ? N3 Cu4 I3 112.22(13) . . ? I4 Cu4 I3 106.83(2) 4_565 . ? I1 Cu4 I3 110.61(2) . . ? N3 Cu4 Cu2 149.76(12) . . ? I4 Cu4 Cu2 102.48(3) 4_565 . ? I1 Cu4 Cu2 58.674(19) . . ? I3 Cu4 Cu2 58.98(2) . . ? N3 Cu4 Cu1 141.62(13) . . ? I4 Cu4 Cu1 57.369(19) 4_565 . ? I1 Cu4 Cu1 60.21(2) . . ? I3 Cu4 Cu1 106.10(3) . . ? Cu2 Cu4 Cu1 57.68(2) . . ? C1 N1 C3 108.3(4) . . ? C1 N1 C5 108.2(4) . . ? C3 N1 C5 108.3(4) . . ? C1 N1 Cu3 110.3(2) . . ? C3 N1 Cu3 107.9(2) . . ? C5 N1 Cu3 113.6(3) . . ? C2 N2 C6 109.7(4) . . ? C2 N2 C4 110.2(4) . . ? C6 N2 C4 109.3(4) . . ? C2 N2 H1 108(3) . . ? C6 N2 H1 113(3) . . ? C4 N2 H1 107(3) . . ? C7 N3 Cu4 171.0(5) . . ? N1 C1 C2 111.8(4) . . ? N1 C1 H1A 109.3 . . ? C2 C1 H1A 109.3 . . ? N1 C1 H1B 109.3 . . ? C2 C1 H1B 109.3 . . ? H1A C1 H1B 107.9 . . ? N2 C2 C1 107.6(4) . . ? N2 C2 H2A 110.2 . . ? C1 C2 H2A 110.2 . . ? N2 C2 H2B 110.2 . . ? C1 C2 H2B 110.2 . . ? H2A C2 H2B 108.5 . . ? N1 C3 C4 111.1(4) . . ? N1 C3 H3A 109.4 . . ? C4 C3 H3A 109.4 . . ? N1 C3 H3B 109.4 . . ? C4 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? N2 C4 C3 107.3(4) . . ? N2 C4 H4A 110.3 . . ? C3 C4 H4A 110.3 . . ? N2 C4 H4B 110.3 . . ? C3 C4 H4B 110.3 . . ? H4A C4 H4B 108.5 . . ? N1 C5 C6 111.6(4) . . ? N1 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? N1 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? N2 C6 C5 107.3(4) . . ? N2 C6 H6A 110.3 . . ? C5 C6 H6A 110.3 . . ? N2 C6 H6B 110.3 . . ? C5 C6 H6B 110.3 . . ? H6A C6 H6B 108.5 . . ? N3 C7 C8 179.8(7) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Cu2 2.6431(7) . ? I1 Cu4 2.6698(7) . ? I1 Cu1 2.7654(7) . ? I2 Cu3 2.6294(6) . ? I2 Cu2 2.6473(7) . ? I2 Cu1 2.7124(7) . ? I3 Cu2 2.6685(7) . ? I3 Cu4 2.6968(8) . ? I4 Cu1 2.6415(7) 4_566 ? I4 Cu4 2.6573(7) 4_566 ? I4 Cu2 2.7011(7) . ? I5 Cu3 2.6177(7) 3_656 ? I5 Cu1 2.6260(7) 3_656 ? I5 Cu3 2.7255(7) . ? Cu1 I5 2.6260(7) 3_656 ? Cu1 I4 2.6415(7) 4_565 ? Cu1 Cu2 2.6838(8) . ? Cu1 Cu3 2.8038(9) . ? Cu1 Cu4 2.8361(9) . ? Cu2 Cu4 2.7240(9) . ? Cu3 N1 2.134(3) . ? Cu3 I5 2.6177(7) 3_656 ? Cu3 Cu3 2.7019(11) 3_656 ? Cu4 N3 1.985(4) . ? Cu4 I4 2.6573(7) 4_565 ? N1 C1 1.459(5) . ? N1 C3 1.465(6) . ? N1 C5 1.467(6) . ? N2 C2 1.487(6) . ? N2 C6 1.489(6) . ? N2 C4 1.491(6) . ? N2 H1 0.893(19) . ? N3 C7 1.130(6) . ? C1 C2 1.519(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.538(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.527(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.455(7) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? 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 H1 I3 0.893(19) 2.74(3) 3.553(4) 152(4) 4_465