data_shelxl _audit_creation_method SHELXL-97 _publ_section_references ; CrystalClear, Rigaku Corp., (1999) Altomare, A., M. Burla, M. Camalli, G. Cascarano, C. Giacovazzo A. Guagliardi, A. Moliterni, G. Polidori & R. Spagna. (1999) J. Appl. Cryst. 32, 115-119. Sheldrick, G.M. SHELXL97. Program for crystal structure refinement. University of Gottingen, Germany, 1997. ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H16 Cu I N2' _chemical_formula_weight 330.67 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C 2 2 21 ' _symmetry_Int_Tables_number 20 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, -z' '-x, y, -z+1/2' '-x, -y, z+1/2' 'x+1/2, y+1/2, 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' _cell_length_a 8.9975(15) _cell_length_b 12.9799(19) _cell_length_c 9.8043(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1145.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 143(1) _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.918 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 640 _exptl_absorpt_coefficient_mu 4.559 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details ; Shape and scale corrections using equivalent reflections. Shape function based on spherical harmonics. Highest even and odd order for spherical harmonics: 4 and 3 Laue group: mmm Friedel opposites are equivalent. ; _exptl_absorpt_correction_T_min 0.7013 _exptl_absorpt_correction_T_max 1.0000 _diffrn_ambient_temperature 143(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'CCD Area Detector' _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method 'phi and omega rotations' _diffrn_reflns_number 3284 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_sigmaI/netI 0.0258 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 25.00 _reflns_number_total 995 _reflns_number_gt 911 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku, 1999)' _computing_data_reduction 'CrystalClear (Rigaku, 1999)' _computing_structure_solution 'SIR97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0476P)^2^+0.2870P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _chemical_absolute_configuration rmad _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(7) _refine_ls_number_reflns 995 _refine_ls_number_parameters 57 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0331 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0786 _refine_ls_wR_factor_gt 0.0765 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.000 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.48481(8) 0.5000 0.5000 0.0526(3) Uani 1 2 d S . . I1 I 0.75222(4) 0.5000 0.5000 0.0476(2) Uani 1 2 d S . . N1 N 0.3121(6) 0.4555(3) 0.6310(4) 0.0461(11) Uani 1 1 d . . . H1 H 0.3303 0.4741 0.7190 0.061 Uiso 1 1 calc R . . C2 C 0.2960(10) 0.3428(4) 0.6159(6) 0.0618(18) Uani 1 1 d . . . H2A H 0.2033 0.3202 0.6567 0.082 Uiso 1 1 calc R . . H2B H 0.3772 0.3079 0.6618 0.082 Uiso 1 1 calc R . . C3 C 0.2976(9) 0.3165(3) 0.4634(5) 0.0633(16) Uani 1 1 d . . . H3A H 0.3942 0.3329 0.4252 0.084 Uiso 1 1 calc R . . H3B H 0.2803 0.2433 0.4513 0.084 Uiso 1 1 calc R . . C4 C 0.1785(8) 0.3769(4) 0.3893(6) 0.0610(17) Uani 1 1 d . . . H4A H 0.0820 0.3485 0.4123 0.081 Uiso 1 1 calc R . . H4B H 0.1926 0.3688 0.2918 0.081 Uiso 1 1 calc R . . C5 C 0.1792(6) 0.4929(6) 0.4241(5) 0.0448(11) Uani 1 1 d . . . H5 H 0.0901 0.5252 0.3858 0.060 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 0.0615(5) 0.0450(4) 0.0512(5) -0.0091(6) 0.000 0.000 I1 0.0634(3) 0.0515(3) 0.0278(3) 0.0028(3) 0.000 0.000 N1 0.074(3) 0.0387(19) 0.026(2) -0.0006(16) 0.000(2) 0.004(2) C2 0.102(5) 0.038(3) 0.045(3) 0.011(2) -0.004(4) 0.007(4) C3 0.106(4) 0.030(2) 0.054(4) -0.007(2) 0.006(4) -0.004(3) C4 0.098(5) 0.043(3) 0.042(3) -0.007(3) -0.003(3) -0.024(3) C5 0.061(3) 0.040(2) 0.034(2) 0.002(3) 0.000(2) -0.010(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 Cu1 N1 2.097(5) 2_566 ? Cu1 N1 2.097(5) . ? Cu1 I1 2.4060(9) . ? N1 C5 1.473(7) 2_566 ? N1 C2 1.478(6) . ? C2 C3 1.534(8) . ? C3 C4 1.513(9) . ? C4 C5 1.544(8) . ? C5 N1 1.473(7) 2_566 ? C5 C5 1.499(9) 2_566 ? 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 N1 Cu1 N1 84.4(2) 2_566 . ? N1 Cu1 I1 137.81(12) 2_566 . ? N1 Cu1 I1 137.81(12) . . ? C5 N1 C2 109.5(6) 2_566 . ? C5 N1 Cu1 104.6(3) 2_566 . ? C2 N1 Cu1 106.5(4) . . ? N1 C2 C3 108.5(4) . . ? C4 C3 C2 110.3(6) . . ? C3 C4 C5 113.3(5) . . ? N1 C5 C5 108.0(4) 2_566 2_566 ? N1 C5 C4 111.4(5) 2_566 . ? C5 C5 C4 109.8(7) 2_566 . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.438 _refine_diff_density_min -0.980 _refine_diff_density_rms 0.107