#------------------------------------------------------------------------------ #$Date: 2016-03-23 03:29:40 +0200 (Wed, 23 Mar 2016) $ #$Revision: 179248 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/31/68/4316860.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_4316860 loop_ _publ_author_name 'Xiaoqing Zeng' 'Michael Gerken' 'Helmut Beckers' 'Helge Willner' _publ_section_title ; Synthesis and Characterization of Carbonyl Diazide, OC(N3)2 ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 9694 _journal_page_last 9699 _journal_paper_doi 10.1021/ic1015143 _journal_volume 49 _journal_year 2010 _chemical_formula_sum 'C N6 O' _chemical_formula_weight 112.07 _chemical_name_common 'carbonyl diazide' _chemical_name_systematic ; ? ; _space_group_IT_number 62 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_space_group_name_H-M 'P n m a' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 5.431(2) _cell_length_b 5.797(2) _cell_length_c 13.800(4) _cell_measurement_reflns_used 266 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 60.7815 _cell_measurement_theta_min 3.1997 _cell_volume 434.5(3) _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 150(2) _diffrn_detector_area_resol_mean 16.2705 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_radiation_monochromator mirror _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0248 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 625 _diffrn_reflns_theta_full 60.87 _diffrn_reflns_theta_max 60.87 _diffrn_reflns_theta_min 6.41 _exptl_absorpt_coefficient_mu 1.318 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.47308 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.713 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 224 _exptl_crystal_size_max 0.116 _exptl_crystal_size_mid 0.058 _exptl_crystal_size_min 0.028 _refine_diff_density_max 0.311 _refine_diff_density_min -0.344 _refine_diff_density_rms 0.088 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.222 _refine_ls_matrix_type full _refine_ls_number_parameters 49 _refine_ls_number_reflns 361 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.222 _refine_ls_R_factor_all 0.0732 _refine_ls_R_factor_gt 0.0588 _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^)+(0.1478P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2180 _refine_ls_wR_factor_ref 0.2240 _reflns_number_gt 282 _reflns_number_total 361 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic1015143_si_002.cif _cod_data_source_block mg_28d _cod_database_code 4316860 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, 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 O1 O 0.4415(7) 0.7500 1.0574(3) 0.0396(14) Uani 1 2 d S . . C1 C 0.2674(9) 0.7500 1.0038(4) 0.0336(15) Uani 1 2 d S . . N1 N 0.2711(9) 0.7500 0.9019(3) 0.0371(14) Uani 1 2 d S . . N2 N 0.4907(9) 0.7500 0.8693(3) 0.0354(14) Uani 1 2 d S . . N3 N 0.6704(10) 0.7500 0.8308(3) 0.0449(16) Uani 1 2 d S . . N4 N 0.0160(8) 0.7500 1.0298(3) 0.0375(14) Uani 1 2 d S . . N5 N -0.0125(8) 0.7500 1.1208(3) 0.0364(15) Uani 1 2 d S . . N6 N -0.0637(9) 0.7500 1.1988(4) 0.0488(15) 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 O1 0.023(2) 0.052(2) 0.044(2) 0.000 -0.0047(17) 0.000 C1 0.028(3) 0.028(3) 0.044(3) 0.000 -0.001(3) 0.000 N1 0.022(3) 0.047(2) 0.042(3) 0.000 0.001(2) 0.000 N2 0.032(3) 0.040(2) 0.035(3) 0.000 -0.001(2) 0.000 N3 0.031(3) 0.059(3) 0.044(3) 0.000 0.005(2) 0.000 N4 0.024(3) 0.047(2) 0.042(3) 0.000 -0.003(2) 0.000 N5 0.021(3) 0.040(2) 0.048(3) 0.000 0.001(2) 0.000 N6 0.032(3) 0.064(3) 0.050(3) 0.000 0.007(3) 0.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 O1 C1 N1 127.2(5) . . ? O1 C1 N4 127.2(5) . . ? N1 C1 N4 105.5(4) . . ? N2 N1 C1 111.5(4) . . ? N3 N2 N1 172.1(5) . . ? N5 N4 C1 111.8(4) . . ? N6 N5 N4 172.6(6) . . ? 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 O1 C1 1.200(6) . ? C1 N1 1.407(8) . ? C1 N4 1.412(7) . ? N1 N2 1.274(7) . ? N2 N3 1.111(7) . ? N4 N5 1.265(7) . ? N5 N6 1.111(6) . ?