data_mpepi _audit_creation_method SHELXL-2012 loop_ _publ_author_name 'G. Vijaya Prakash,Mark E Light,K. Nageswara Rao and D Kumar' _publ_contact_author_address ; Nanophotonics Lab Department of physics Indian Institute of Technology Hauz Khas, New Delhi 110016 India ; _publ_contact_author_email 'prakash@physics.iitd.ac.in' _publ_contact_author_fax '+91-11-26591326' _publ_contact_author_phone '+91-11-26591326' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'I4 Pb, 2(C9 H14 N)' _chemical_formula_sum 'C18 H28 I4 N2 Pb' _chemical_formula_weight 987.22 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' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pb' 'Pb' -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 36 _space_group_name_H-M_alt 'C m c 21' _space_group_name_Hall 'C 2c -2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y, z+1/2' '-x, y, z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z' _cell_length_a 32.544(7) _cell_length_b 9.316(2) _cell_length_c 8.6028(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2608.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2200 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description 'needle' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776.0 _exptl_absorpt_coefficient_mu 11.208 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.339 _exptl_absorpt_correction_T_max 0.456 _exptl_absorpt_process_details 'SADABS v2.03, Sheldrick, G.M., (2001)' _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 'Bruker Apex CCD' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11467 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2331 _reflns_number_gt 2201 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX 2' _computing_cell_refinement 'SAINT V6.28A' _computing_data_reduction 'SAINT V6.28A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-2012 (Sheldrick, 2012)' _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. ; _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^)+(0.0227P)^2^+0.0000P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.054(6) _refine_ls_number_reflns 2331 _refine_ls_number_parameters 121 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0267 _refine_ls_R_factor_gt 0.0251 _refine_ls_wR_factor_ref 0.0549 _refine_ls_wR_factor_gt 0.0544 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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 N1 N 0.91625(18) 0.3600(7) 0.2268(7) 0.0447(16) Uani 1 1 d . . . H1A1 H 0.9114 0.3197 0.3187 0.067 Uiso 1 1 calc R . . H1B1 H 0.9127 0.4545 0.2338 0.067 Uiso 1 1 calc R . . H1C1 H 0.9420 0.3415 0.1981 0.067 Uiso 1 1 calc R . . C1 C 0.7133(3) 0.3666(10) 0.2673(14) 0.084(3) Uani 1 1 d . . . H1A H 0.6988 0.2916 0.2140 0.126 Uiso 1 1 calc R . . H1B H 0.7033 0.4582 0.2329 0.126 Uiso 1 1 calc R . . H1C H 0.7090 0.3574 0.3773 0.126 Uiso 1 1 calc R . . C2 C 0.7595(2) 0.3549(10) 0.2318(10) 0.057(2) Uani 1 1 d . . . C3 C 0.7774(2) 0.4376(8) 0.1183(12) 0.060(2) Uani 1 1 d . . . H3 H 0.7616 0.5054 0.0661 0.072 Uiso 1 1 calc R . . C4 C 0.8190(2) 0.4218(8) 0.0797(11) 0.056(2) Uani 1 1 d . . . H4 H 0.8304 0.4783 0.0018 0.067 Uiso 1 1 calc R . . C5 C 0.8426(2) 0.3243(7) 0.1554(9) 0.0413(16) Uani 1 1 d . . . C6 C 0.8247(3) 0.2458(8) 0.2756(11) 0.055(2) Uani 1 1 d . . . H6 H 0.8406 0.1817 0.3325 0.066 Uiso 1 1 calc R . . C7 C 0.7836(3) 0.2621(9) 0.3113(13) 0.062(2) Uani 1 1 d . . . H7 H 0.7723 0.2082 0.3916 0.074 Uiso 1 1 calc R . . C8 C 0.8867(2) 0.2988(8) 0.1065(9) 0.0427(18) Uani 1 1 d . . . H8 H 0.8912 0.3510 0.0091 0.051 Uiso 1 1 calc R . . C9 C 0.8969(3) 0.1424(9) 0.0769(12) 0.064(3) Uani 1 1 d . . . H9A H 0.8957 0.0901 0.1730 0.096 Uiso 1 1 calc R . . H9B H 0.9241 0.1352 0.0342 0.096 Uiso 1 1 calc R . . H9C H 0.8775 0.1028 0.0048 0.096 Uiso 1 1 calc R . . I1 I 1.0000 0.92816(7) -0.17017(11) 0.0459(2) Uani 1 2 d S . . I2 I 0.902436(12) 0.72994(5) 0.13792(8) 0.04235(14) Uani 1 1 d . . . I3 I 1.0000 0.45258(7) -0.04212(10) 0.03679(17) Uani 1 2 d S . . Pb1 Pb 1.0000 0.76324(4) 0.15072(6) 0.03346(11) Uani 1 2 d S . . 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 N1 0.036(3) 0.048(4) 0.050(4) 0.006(3) 0.001(3) -0.007(3) C1 0.040(5) 0.079(7) 0.132(10) -0.014(7) -0.004(5) -0.010(5) C2 0.036(4) 0.066(6) 0.069(6) -0.017(5) -0.005(4) -0.011(4) C3 0.045(5) 0.051(5) 0.084(7) 0.003(5) -0.022(5) 0.007(4) C4 0.050(5) 0.053(6) 0.065(6) 0.008(4) -0.006(4) -0.004(4) C5 0.041(4) 0.034(4) 0.049(4) 0.004(4) -0.006(4) -0.005(3) C6 0.044(5) 0.056(6) 0.064(6) 0.014(4) -0.001(4) -0.004(4) C7 0.049(5) 0.070(7) 0.067(6) 0.011(5) 0.005(5) -0.008(4) C8 0.039(4) 0.052(5) 0.038(4) 0.004(3) 0.002(3) -0.001(3) C9 0.067(6) 0.056(6) 0.069(7) -0.018(5) -0.003(5) 0.005(4) I1 0.0526(4) 0.0426(4) 0.0424(4) 0.0135(3) 0.000 0.000 I2 0.0335(2) 0.0455(3) 0.0481(3) -0.0020(3) 0.0010(3) 0.00165(19) I3 0.0380(3) 0.0386(4) 0.0338(4) -0.0062(3) 0.000 0.000 Pb1 0.03164(17) 0.0342(2) 0.03458(19) 0.0009(2) 0.000 0.000 _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 N1 C8 1.523(9) . ? N1 H1A1 0.8900 . ? N1 H1B1 0.8900 . ? N1 H1C1 0.8900 . ? C1 C2 1.536(11) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C7 1.354(12) . ? C2 C3 1.374(12) . ? C3 C4 1.400(11) . ? C3 H3 0.9300 . ? C4 C5 1.357(10) . ? C4 H4 0.9300 . ? C5 C6 1.394(11) . ? C5 C8 1.515(9) . ? C6 C7 1.380(12) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.516(11) . ? C8 H8 0.9800 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? I1 Pb1 3.1593(13) . ? I1 Pb1 3.2616(10) 2_774 ? I2 Pb1 3.1922(8) . ? I3 Pb1 3.3203(12) 2_764 ? I3 Pb1 3.3358(10) . ? Pb1 I2 3.1922(8) 4_755 ? Pb1 I1 3.2616(10) 2_775 ? Pb1 I3 3.3203(12) 2_765 ? 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 C8 N1 H1A1 109.5 . . ? C8 N1 H1B1 109.5 . . ? H1A1 N1 H1B1 109.5 . . ? C8 N1 H1C1 109.5 . . ? H1A1 N1 H1C1 109.5 . . ? H1B1 N1 H1C1 109.5 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C7 C2 C3 118.0(8) . . ? C7 C2 C1 120.8(9) . . ? C3 C2 C1 121.1(9) . . ? C2 C3 C4 121.3(8) . . ? C2 C3 H3 119.3 . . ? C4 C3 H3 119.3 . . ? C5 C4 C3 120.3(8) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 118.1(8) . . ? C4 C5 C8 120.6(7) . . ? C6 C5 C8 121.3(7) . . ? C7 C6 C5 120.8(9) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C2 C7 C6 121.4(10) . . ? C2 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? C5 C8 C9 113.9(6) . . ? C5 C8 N1 110.6(6) . . ? C9 C8 N1 109.6(6) . . ? C5 C8 H8 107.5 . . ? C9 C8 H8 107.5 . . ? N1 C8 H8 107.5 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Pb1 I1 Pb1 147.29(4) . 2_774 ? Pb1 I3 Pb1 157.09(3) 2_764 . ? I1 Pb1 I2 90.980(13) . . ? I1 Pb1 I2 90.980(13) . 4_755 ? I2 Pb1 I2 168.16(2) . 4_755 ? I1 Pb1 I1 89.09(2) . 2_775 ? I2 Pb1 I1 95.853(11) . 2_775 ? I2 Pb1 I1 95.852(11) 4_755 2_775 ? I1 Pb1 I3 171.83(3) . 2_765 ? I2 Pb1 I3 88.202(13) . 2_765 ? I2 Pb1 I3 88.202(13) 4_755 2_765 ? I1 Pb1 I3 99.08(4) 2_775 2_765 ? I1 Pb1 I3 89.27(3) . . ? I2 Pb1 I3 84.175(11) . . ? I2 Pb1 I3 84.175(11) 4_755 . ? I1 Pb1 I3 178.37(4) 2_775 . ? I3 Pb1 I3 82.557(19) 2_765 . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 C2 C3 C4 3.3(13) . . . . ? C1 C2 C3 C4 -176.5(8) . . . . ? C2 C3 C4 C5 -0.6(13) . . . . ? C3 C4 C5 C6 -2.6(12) . . . . ? C3 C4 C5 C8 175.5(7) . . . . ? C4 C5 C6 C7 3.1(12) . . . . ? C8 C5 C6 C7 -175.0(8) . . . . ? C3 C2 C7 C6 -2.8(14) . . . . ? C1 C2 C7 C6 177.0(9) . . . . ? C5 C6 C7 C2 -0.4(14) . . . . ? C4 C5 C8 C9 -127.7(8) . . . . ? C6 C5 C8 C9 50.4(10) . . . . ? C4 C5 C8 N1 108.4(8) . . . . ? C6 C5 C8 N1 -73.5(9) . . . . ? Pb1 I1 Pb1 I2 95.839(11) 2_774 . . . ? Pb1 I1 Pb1 I2 -95.839(11) 2_774 . . 4_755 ? Pb1 I1 Pb1 I1 0.0 2_774 . . 2_775 ? Pb1 I1 Pb1 I3 180.0 2_774 . . . ? Pb1 I3 Pb1 I2 91.059(13) 2_764 . . . ? Pb1 I3 Pb1 I2 -91.059(13) 2_764 . . 4_755 ? Pb1 I3 Pb1 I3 180.0 2_764 . . 2_765 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.143 _refine_diff_density_min -0.619 _refine_diff_density_rms 0.127