#============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name 'Dr. simona Galli' _publ_contact_author_address ; Dipartimento di Scienze Chimiche e Ambientali Via Valleggio, 11 22100 Como - Italy ; _publ_contact_author_email simona.galli@uninsubria.it _publ_contact_author_fax +39-031-326230 _publ_contact_author_phone +39-031-326227 _publ_requested_journal 'Chemistry of Materials' _publ_requested_category ? _publ_contact_letter ;? ; #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_paper_category ? _iucr_compatibility_tag ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Sequential self-organization of silver(I) layered materials with strong SHG by J aggregation and intercalation of organic NLO-phores through mechanochemical synthesis ; # The loop structure below should contain the names and addresses of all # authors in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Elena Cariati' ; Dipartimento di Chimica Inorganica, Metallorganica e Analitica Università degli Studi di Milano Centro di Eccellenza CIMAINA UdR di Milano dell'INSTM and ISTM-CNR Via Venezian, 21 20133 Milano - Italy ; 'Roberto Macchi' ; Dipartimento di Chimica Inorganica, Metallorganica e Analitica Università degli Studi di Milano Centro di Eccellenza CIMAINA UdR di Milano dell'INSTM and ISTM-CNR Via Venezian, 21 20133 Milano - Italy ; 'Dominique Roberto' ; Dipartimento di Chimica Inorganica, Metallorganica e Analitica Università degli Studi di Milano Centro di Eccellenza CIMAINA UdR di Milano dell'INSTM and ISTM-CNR Via Venezian, 21 20133 Milano - Italy ; 'Renato Ugo' ; Dipartimento di Chimica Inorganica, Metallorganica e Analitica Università degli Studi di Milano Centro di Eccellenza CIMAINA UdR di Milano dell'INSTM and ISTM-CNR Via Venezian, 21 20133 Milano - Italy ; 'Simona Galli' ; Dipartimento di Scienze Chimiche e Ambientali Università dell'Insubria Via Valleggio, 11 22100 Como - Italy ; 'Norberto Masciocchi' ; Dipartimento di Scienze Chimiche e Ambientali Università dell'Insubria Via Valleggio, 11 22100 Como - Italy ; 'Angelo Sironi' ; Dipartimento di Chimica Strutturale e Stereochimica Inorganica Università degli Studi di Milano Centro di Eccellenza CIMAINA UdR di Milano dell'INSTM and ISTM-CNR Via Venezian, 21 20133 Milano - Italy ; #============================================================================== data_[DAMS+][Ag5I6-] _chemical_name_systematic ; catena-E-4-(4-dimethylaminostyryl)-1-methylpyridinium-esaidodide-pentasilver(i) ; _chemical_name_common ? _chemical_formula_moiety [C16 H19 N2]+, [Ag5 I6]- _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum C16 H19 Ag5 I6 N2 _chemical_formula_weight 1540.11 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C International Tables for Crystallography (Vol. IV) H H International Tables for Crystallography (Vol. IV) Ag Ag International Tables for Crystallography (Vol. IV) I I International Tables for Crystallography (Vol. IV) N N International Tables for Crystallography (Vol. IV) #============================================================================== # POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M 'R-3m' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz '-x, -x+y, -z' '-x, -y, -z' '-x+1/3, -x+y-1/3, -z-1/3' '-x+1/3, -y-1/3, -z-1/3' '-x-1/3, -x+y+1/3, -z+1/3' '-x-1/3, -y+1/3, -z+1/3' '-x+y, -x, z' '-x+y, y, z' '-x+y+1/3, -x-1/3, z-1/3' '-x+y+1/3, y-1/3, z-1/3' '-x+y-1/3, -x+1/3, z+1/3' '-x+y-1/3, y+1/3, z+1/3' '-y, -x, z' '-y, x-y, z' '-y+1/3, -x-1/3, z-1/3' '-y+1/3, x-y-1/3, z-1/3' '-y-1/3, -x+1/3, z+1/3' '-y-1/3, x-y+1/3, z+1/3' 'y, -x+y, -z' 'y, x, -z' 'y+1/3, -x+y-1/3, -z-1/3' 'y+1/3, x-1/3, -z-1/3' 'y-1/3, -x+y+1/3, -z+1/3' 'y-1/3, x+1/3, -z+1/3' 'x-y, -y, -z' 'x-y, x, -z' 'x-y+1/3, -y-1/3, -z-1/3' 'x-y+1/3, x-1/3, -z-1/3' 'x-y-1/3, -y+1/3, -z+1/3' 'x-y-1/3, x+1/3, -z+1/3' 'x, y, z' 'x, x-y, z' 'x+1/3, y-1/3, z-1/3' 'x+1/3, x-y-1/3, z-1/3' 'x-1/3, y+1/3, z+1/3' 'x-1/3, x-y+1/3, z+1/3' _cell_length_a 4.49906(84) _cell_length_b 4.49906(84) _cell_length_c 38.5395(48) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 675.58(27) _cell_formula_units_Z 6 _cell_measurement_temperature 298(2) _pd_calibration_special_details ; ? ; _cell_special_details ; ? ; _exptl_crystal_density_diffrn ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 4092 # The next three fields give the specimen dimensions in mm. # The equatorial plane contains the incident and diffracted beam. _pd_spec_size_axial 15 # perpendicular to # equatorial plane _pd_spec_size_equat 20 # parallel to # scattering vector # in transmission _pd_spec_size_thick 0.2 # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting ; packed powder pellet ; _pd_spec_mount_mode 'reflection' # options are reflection # or transmission _pd_spec_shape 'flat_sheet' # options are cylinder # flat_sheet or irregular _pd_char_particle_morphology ? _pd_char_colour brown # use ICDD colour descriptions # The next four fields are normally only needed for transmission experiments. _exptl_absorpt_coefficient_mu ? _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #============================================================================== # EXPERIMENTAL DATA _exptl_special_details ; ? ; # This following item is used to identify the equipment used to record the # powder pattern when the diffractogram was measured at a laboratory # other than the authors home institution e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_source 'sealed X-ray tube' _diffrn_source_target Cu _diffrn_source_type ? _diffrn_measurement_device_type 'Bruker AXS D8 Advance' _diffrn_detector ? _diffrn_detector_type 'scintillator' _pd_meas_scan_method step # options are step or cont # tof or fixed or # disp (= dispersive) _pd_meas_special_details ; ? ; loop_ _diffrn_radiation_type _diffrn_radiation_wavelength CuK\a~1~ 1.54056 CuK\a~2~ 1.54439 _diffrn_radiation_monochromator 'HOPG Graphite' # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 5001 _pd_meas_2theta_range_min 5 _pd_meas_2theta_range_max 105 _pd_meas_2theta_range_inc 0.02 # The following three items are used for time-of-flight measurements only. _pd_instr_dist_src/spec ? _pd_instr_dist_spec/detc ? _pd_meas_2theta_fixed ? # The following fields are used to identify the programs used. _computing_data_collection ? _computing_cell_refinement 'TOPAS-R' _computing_data_reduction ? _computing_structure_solution 'TOPAS-R' _computing_structure_refinement 'TOPAS-R' _computing_molecular_graphics ? _computing_publication_material 'TOPAS-R' # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; The effect of the translational disordered [DAMS+] cations, in the ab plane, has been modeled by a single N atom (in 0,0,1/3) with s.o.f. of 3 (corresponding to the total electron count of one [DAMS+] cation per cell) and a large B factor (100 Å^2). Such model implies a non zero scattering contribution only for low-angle 00l reflections. ; # The next three items are given as text _pd_proc_ls_profile_function 'fundamental parameters' _pd_proc_ls_background_function 'polynomial' _pd_proc_ls_pref_orient_corr 'March Dollase correction on [001]' _pd_proc_ls_prof_R_factor 0.119 _pd_proc_ls_prof_wR_factor 0.152 _pd_proc_ls_prof_wR_expected 0.080 _refine_special_details ; ? ; _refine_ls_structure_factor_coef Inet _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme '1/[Y~i~]' _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_parameters 19 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 # The following item is CHI squared _refine_ls_goodness_of_fit_all 1.901 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_shift/su_max .01 _refine_ls_shift/su_mean ? # The following four items apply to angular dispersive measurements. # 2theta minimum maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 5 _pd_proc_2theta_range_max 105 _pd_proc_2theta_range_inc 0.02 loop_ _pd_proc_wavelength 1.540562 1.544390 _pd_block_diffractogram_id ? # The id used for the block # containing the powder # pattern profile (section 11). # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_symmetry_multiplicity _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_B_iso_or_equiv I I 6 0 0 0.11375(14) 1 3.89(16) Ag Ag 6 0 0 0.18917(19) 5/6 3.89(16) N N 6 0 0 1/3 3 100.0(96) #============================================================================== data_[DAMS]2[Cu2I4] _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis-E-4-(4-dimethylaminostyryl)-1-methylpyridinium-tetrakisiodide-biscopper(i) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [C32 H38 N4]2+, [Cu2 I4]2- _chemical_formula_sum 'C32 H38 Cu2 I4 N4' _chemical_formula_weight 1113.39 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6460(10) _cell_length_b 9.443(2) _cell_length_c 11.988(2) _cell_angle_alpha 74.060(10) _cell_angle_beta 80.120(10) _cell_angle_gamma 76.590(10) _cell_volume 909.3(3) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 23 _cell_measurement_theta_min 10.59 _cell_measurement_theta_max 15.38 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.033 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 528 _exptl_absorpt_coefficient_mu 4.591 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius CAD4 automated diffractometer' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3184 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0141 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 24.95 _reflns_number_total 3184 _reflns_number_gt 2662 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'Sir97' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The carbon (and hydrogen) atoms of the ethylene bond (C7, C7') are disordered over two distinct sites. Each disordered carbon atom has been modeled by allowing its presence into the two sites (C7, C7A; C7', C7'A) with refinable s.o.f of x and (1-x), respectively. The hydrogen atoms have been introduced, with the proper s.o.f., using the riding model. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0259P)^2^+0.8337P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0075(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3184 _refine_ls_number_parameters 190 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0343 _refine_ls_R_factor_gt 0.0245 _refine_ls_wR_factor_ref 0.0583 _refine_ls_wR_factor_gt 0.0542 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.020 _refine_ls_shift/su_mean 0.002 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 Cu1 Cu -0.48459(6) 0.07926(6) -0.11267(4) 0.06248(15) Uani 1 1 d . . . I1 I -0.47439(3) 0.23666(3) -0.31785(2) 0.06442(11) Uani 1 1 d . . . I2 I -0.25067(3) 0.00708(3) 0.01248(2) 0.06544(11) Uani 1 1 d . . . N1 N -0.3799(4) 0.6102(3) -0.2391(3) 0.0537(8) Uani 1 1 d . . . C2 C -0.2663(5) 0.4871(5) -0.2194(4) 0.0597(10) Uani 1 1 d . . . H2 H -0.2281 0.4362 -0.2779 0.072 Uiso 1 1 calc R . . C3 C -0.2048(5) 0.4340(5) -0.1146(4) 0.0667(11) Uani 1 1 d . . . H3 H -0.1256 0.3477 -0.1023 0.080 Uiso 1 1 calc R . . C4 C -0.2615(6) 0.5100(6) -0.0263(3) 0.0703(13) Uani 1 1 d D . . C5 C -0.3796(6) 0.6371(6) -0.0513(4) 0.0761(13) Uani 1 1 d . . . H5 H -0.4209 0.6911 0.0050 0.091 Uiso 1 1 calc R . . C6 C -0.4351(6) 0.6834(5) -0.1552(4) 0.0684(12) Uani 1 1 d . . . H6 H -0.5146 0.7692 -0.1696 0.082 Uiso 1 1 calc R . . C7 C -0.2167(6) 0.4749(6) 0.0948(4) 0.0555(17) Uiso 0.747(11) 1 d PD . . H7 H -0.2660 0.5360 0.1450 0.067 Uiso 1 1 calc R . . C7' C -0.1059(6) 0.3554(6) 0.1290(4) 0.0533(16) Uiso 0.747(11) 1 d PD . . H7' H -0.0582 0.2958 0.0774 0.064 Uiso 1 1 calc R . . C7A C -0.1544(14) 0.4067(13) 0.0603(9) 0.054(5) Uiso 0.253(11) 1 d PD . . C7'A C -0.1624(13) 0.4251(11) 0.1664(8) 0.045(4) Uiso 0.253(11) 1 d PD . . C1' C 0.0660(4) 0.1971(4) 0.4696(3) 0.0497(9) Uani 1 1 d . . . C2' C -0.0556(5) 0.3257(4) 0.4495(4) 0.0606(10) Uani 1 1 d . . . H2' H -0.0977 0.3741 0.5091 0.073 Uiso 1 1 calc R . . C3' C -0.1140(5) 0.3816(5) 0.3410(5) 0.0710(13) Uani 1 1 d . . . H3' H -0.1946 0.4669 0.3299 0.085 Uiso 1 1 calc R . . C4' C -0.0552(6) 0.3133(6) 0.2489(4) 0.0711(13) Uani 1 1 d D . . C5' C 0.0656(5) 0.1887(5) 0.2702(4) 0.0670(11) Uani 1 1 d . . . H5' H 0.1083 0.1412 0.2101 0.080 Uiso 1 1 calc R . . C6' C 0.1251(5) 0.1319(5) 0.3742(3) 0.0575(10) Uani 1 1 d . . . H6' H 0.2071 0.0477 0.3829 0.069 Uiso 1 1 calc R . . C8 C -0.4430(6) 0.6650(5) -0.3532(4) 0.0776(13) Uani 1 1 d . . . H81 H -0.3896 0.5999 -0.4029 0.093 Uiso 1 1 calc R . . H82 H -0.4248 0.7649 -0.3887 0.093 Uiso 1 1 calc R . . H83 H -0.5558 0.6659 -0.3423 0.093 Uiso 1 1 calc R . . N2 N 0.1255(4) 0.1401(4) 0.5736(3) 0.0592(8) Uani 1 1 d . . . C9 C 0.0531(6) 0.1983(6) 0.6742(4) 0.0782(13) Uani 1 1 d . . . H91 H 0.1107 0.1447 0.7397 0.094 Uiso 1 1 calc R . . H92 H -0.0563 0.1859 0.6924 0.094 Uiso 1 1 calc R . . H93 H 0.0567 0.3031 0.6571 0.094 Uiso 1 1 calc R . . C10 C 0.2489(5) 0.0061(4) 0.5923(4) 0.0643(11) Uani 1 1 d . . . H101 H 0.2764 -0.0176 0.6705 0.077 Uiso 1 1 calc R . . H102 H 0.3419 0.0229 0.5377 0.077 Uiso 1 1 calc R . . H103 H 0.2104 -0.0760 0.5811 0.077 Uiso 1 1 calc 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 Cu1 0.0651(3) 0.0642(3) 0.0592(3) -0.0178(2) -0.0082(2) -0.0107(2) I1 0.06393(18) 0.0727(2) 0.05694(18) -0.01184(13) -0.01047(13) -0.01615(14) I2 0.05107(17) 0.0851(2) 0.06059(18) -0.01396(14) -0.00878(12) -0.01718(14) N1 0.0537(19) 0.0512(19) 0.0562(19) -0.0087(15) -0.0104(15) -0.0124(15) C2 0.058(2) 0.059(2) 0.065(3) -0.022(2) -0.011(2) -0.006(2) C3 0.061(3) 0.056(2) 0.081(3) -0.005(2) -0.023(2) -0.012(2) C4 0.086(3) 0.086(3) 0.050(2) -0.002(2) -0.011(2) -0.056(3) C5 0.093(4) 0.076(3) 0.069(3) -0.031(3) 0.006(3) -0.031(3) C6 0.071(3) 0.054(3) 0.079(3) -0.022(2) 0.001(2) -0.011(2) C1' 0.0424(19) 0.049(2) 0.057(2) -0.0107(17) -0.0058(17) -0.0121(16) C2' 0.053(2) 0.056(2) 0.073(3) -0.018(2) -0.006(2) -0.0082(19) C3' 0.048(2) 0.054(2) 0.101(4) 0.008(2) -0.024(2) -0.0117(19) C4' 0.069(3) 0.087(3) 0.058(3) 0.004(2) -0.010(2) -0.042(3) C5' 0.061(3) 0.087(3) 0.058(3) -0.015(2) -0.002(2) -0.031(2) C6' 0.050(2) 0.062(2) 0.063(3) -0.017(2) -0.0057(19) -0.0124(19) C8 0.083(3) 0.079(3) 0.071(3) -0.001(2) -0.030(3) -0.022(3) N2 0.057(2) 0.059(2) 0.060(2) -0.0192(16) -0.0138(16) 0.0022(16) C9 0.078(3) 0.086(3) 0.070(3) -0.029(3) -0.014(2) 0.000(3) C10 0.055(2) 0.057(2) 0.079(3) -0.010(2) -0.021(2) -0.0056(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Cu1 I1 2.4990(7) . ? Cu1 I2 2.5780(7) . ? Cu1 I2 2.5944(7) 2_455 ? Cu1 Cu1 2.7067(11) 2_455 ? I2 Cu1 2.5944(7) 2_455 ? N1 C2 1.331(5) . ? N1 C6 1.334(5) . ? N1 C8 1.474(5) . ? C2 C3 1.368(6) . ? C2 H2 0.9300 . ? C3 C4 1.397(6) . ? C3 H3 0.9300 . ? C4 C5 1.383(7) . ? C4 C7 1.496(4) . ? C4 C7A 1.497(4) . ? C5 C6 1.336(7) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C7' 1.319(6) . ? C7 H7 0.9300 . ? C7' C4' 1.496(4) . ? C7' H7' 0.9300 . ? C7A C7'A 1.319(6) . ? C7'A C4' 1.496(4) . ? C1' N2 1.354(5) . ? C1' C2' 1.404(5) . ? C1' C6' 1.411(5) . ? C2' C3' 1.396(6) . ? C2' H2' 0.9300 . ? C3' C4' 1.393(7) . ? C3' H3' 0.9300 . ? C4' C5' 1.377(7) . ? C5' C6' 1.353(6) . ? C5' H5' 0.9300 . ? C6' H6' 0.9300 . ? C8 H81 0.9600 . ? C8 H82 0.9600 . ? C8 H83 0.9600 . ? N2 C10 1.445(5) . ? N2 C9 1.447(5) . ? C9 H91 0.9600 . ? C9 H92 0.9600 . ? C9 H93 0.9600 . ? C10 H101 0.9600 . ? C10 H102 0.9600 . ? C10 H103 0.9600 . ? 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 I1 Cu1 I2 123.97(2) . . ? I1 Cu1 I2 119.05(2) . 2_455 ? I2 Cu1 I2 116.89(2) . 2_455 ? I1 Cu1 Cu1 176.06(3) . 2_455 ? I2 Cu1 Cu1 58.74(2) . 2_455 ? I2 Cu1 Cu1 58.15(2) 2_455 2_455 ? Cu1 I2 Cu1 63.11(2) . 2_455 ? C2 N1 C6 119.5(4) . . ? C2 N1 C8 119.9(4) . . ? C6 N1 C8 120.6(4) . . ? N1 C2 C3 121.2(4) . . ? N1 C2 H2 119.4 . . ? C3 C2 H2 119.4 . . ? C2 C3 C4 119.7(4) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 116.7(4) . . ? C5 C4 C7 113.0(4) . . ? C3 C4 C7 130.2(5) . . ? C5 C4 C7A 147.5(6) . . ? C3 C4 C7A 95.8(6) . . ? C7 C4 C7A 34.4(5) . . ? C6 C5 C4 120.8(4) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? N1 C6 C5 122.0(4) . . ? N1 C6 H6 119.0 . . ? C5 C6 H6 119.0 . . ? C7' C7 C4 118.6(4) . . ? C7' C7 H7 120.7 . . ? C4 C7 H7 120.7 . . ? C7 C7' C4' 121.5(4) . . ? C7 C7' H7' 119.2 . . ? C4' C7' H7' 119.2 . . ? C7'A C7A C4 121.8(6) . . ? C7A C7'A C4' 118.3(6) . . ? N2 C1' C2' 122.3(4) . . ? N2 C1' C6' 121.7(3) . . ? C2' C1' C6' 116.0(4) . . ? C3' C2' C1' 120.7(4) . . ? C3' C2' H2' 119.6 . . ? C1' C2' H2' 119.6 . . ? C4' C3' C2' 121.9(4) . . ? C4' C3' H3' 119.0 . . ? C2' C3' H3' 119.0 . . ? C5' C4' C3' 116.3(4) . . ? C5' C4' C7' 114.6(5) . . ? C3' C4' C7' 129.0(5) . . ? C5' C4' C7'A 149.6(6) . . ? C3' C4' C7'A 94.1(6) . . ? C7' C4' C7'A 35.0(5) . . ? C6' C5' C4' 123.2(4) . . ? C6' C5' H5' 118.4 . . ? C4' C5' H5' 118.4 . . ? C5' C6' C1' 121.8(4) . . ? C5' C6' H6' 119.1 . . ? C1' C6' H6' 119.1 . . ? N1 C8 H81 109.5 . . ? N1 C8 H82 109.5 . . ? H81 C8 H82 109.5 . . ? N1 C8 H83 109.5 . . ? H81 C8 H83 109.5 . . ? H82 C8 H83 109.5 . . ? C1' N2 C10 121.0(3) . . ? C1' N2 C9 121.0(3) . . ? C10 N2 C9 117.4(4) . . ? N2 C9 H91 109.5 . . ? N2 C9 H92 109.5 . . ? H91 C9 H92 109.5 . . ? N2 C9 H93 109.5 . . ? H91 C9 H93 109.5 . . ? H92 C9 H93 109.5 . . ? N2 C10 H101 109.5 . . ? N2 C10 H102 109.5 . . ? H101 C10 H102 109.5 . . ? N2 C10 H103 109.5 . . ? H101 C10 H103 109.5 . . ? H102 C10 H103 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.95 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.411 _refine_diff_density_min -0.390 _refine_diff_density_rms 0.061