#------------------------------------------------------------------------------ #$Date: 2016-02-19 14:29:56 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176759 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/62/2006222.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2006222 loop_ _publ_author_name 'Jones, Peter G.' 'Ahrens, Birte' 'H\"opfner, Thomas' 'Hopf, Henning' _publ_section_title ; 2,4,6-Tris(diazo)cyclohexane-1,3,5-trione ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 783 _journal_page_last 786 _journal_paper_doi 10.1107/S0108270197002114 _journal_volume 53 _journal_year 1997 _chemical_formula_sum 'C6 N6 O3' _chemical_formula_weight 204.12 _chemical_name_systematic ; 2,4,6-Tris(diazo)-cyclohexane-1,3,5-trione ; _space_group_IT_number 176 _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall '-P 6c' _symmetry_space_group_name_H-M 'P 63/m' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 2 _cell_length_a 9.1599(13) _cell_length_b 9.1599(13) _cell_length_c 5.445(3) _cell_measurement_reflns_used 60 _cell_measurement_temperature 143(2) _cell_measurement_theta_max 11.5 _cell_measurement_theta_min 10 _cell_volume 395.6(2) _computing_cell_refinement DIF4 _computing_data_collection 'DIF4 (Stoe & Cie, 1991a)' _computing_data_reduction 'REDU4 (Stoe & Cie, 1991b)' _computing_molecular_graphics 'XP (Siemens, 1994)' _computing_publication_material SHELXL-93 _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _diffrn_ambient_temperature 143(2) _diffrn_measurement_device 'Stoe STADI-4' _diffrn_measurement_method '\w/2\q 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 0.0516 _diffrn_reflns_av_sigmaI/netI 0.0244 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_number 2386 _diffrn_reflns_theta_max 29.45 _diffrn_reflns_theta_min 4.45 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.144 _exptl_absorpt_correction_type none _exptl_crystal_colour 'pale yellow' _exptl_crystal_density_diffrn 1.713 _exptl_crystal_density_meas ? _exptl_crystal_description prism _exptl_crystal_F_000 204 _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.40 _refine_diff_density_max 0.410 _refine_diff_density_min -0.187 _refine_ls_extinction_coef 0.70(6) _refine_ls_extinction_method 'SHELXL93 (Sheldrick, 1993)' _refine_ls_goodness_of_fit_all 1.184 _refine_ls_goodness_of_fit_obs 1.196 _refine_ls_hydrogen_treatment none _refine_ls_matrix_type full _refine_ls_number_parameters 32 _refine_ls_number_reflns 407 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.225 _refine_ls_restrained_S_obs 1.196 _refine_ls_R_factor_all 0.0306 _refine_ls_R_factor_obs .0291 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0534P)^2^+0.0293P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.0933 _refine_ls_wR_factor_obs .0885 _reflns_number_observed 385 _reflns_number_total 408 _reflns_observed_criterion >2sigma(I) _cod_data_source_file fg1274.cif _cod_data_source_block vowel _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(Fo^2^)+(0.0534P)^2^+0.0293P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/[\s^2^(Fo^2^)+(0.0534P)^2^+0.0293P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_sg_symbol_H-M P6~3~/m _cod_database_code 2006222 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O .0235(4) .0200(4) .0272(4) .0079(3) .000 .000 N1 .0223(4) .0234(4) .0231(5) .0121(3) .000 .000 N2 .0245(5) .0372(6) .0396(6) .0170(4) .000 .000 C1 .0205(5) .0210(5) .0170(5) .0102(4) .000 .000 C2 .0185(5) .0210(5) .0228(5) .0100(3) .000 .000 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol O .41446(9) .00385(9) .2500 .0249(3) Uani d S 1 . O N1 .33774(11) .25478(10) .2500 .0226(3) Uani d S 1 . N N2 .20295(12) .21895(13) .2500 .0331(3) Uani d S 1 . N C1 .52808(12) .15168(12) .2500 .0196(3) Uani d S 1 . C C2 .49860(11) .29383(12) .2500 .0207(3) Uani d S 1 . C 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N2 N1 C2 . . 178.59(10) y O C1 C2 . 2_655 124.11(8) y O C1 C2 . . 123.52(8) y C2 C1 C2 2_655 . 112.37(9) y N1 C2 C1 . 3_665 116.58(8) y N1 C2 C1 . . 115.79(9) y C1 C2 C1 3_665 . 127.63(9) y loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O C1 . 1.2278(11) y N1 N2 . 1.1077(12) y N1 C2 . 1.3311(12) y C1 C2 2_655 1.4506(12) y C1 C2 . 1.4560(12) y C2 C1 3_665 1.4506(12) ? 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_site_symmetry_1 _geom_torsion_site_symmetry_4 _geom_torsion N2 N1 C2 C1 . 3_665 180.0 N2 N1 C2 C1 . . 0.0 O C1 C2 N1 . . 0.0 C2 C1 C2 N1 2_655 . 180.0 O C1 C2 C1 . 3_665 180.0 C2 C1 C2 C1 2_655 3_665 0.0