#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003507.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_2003507 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 963 _journal_page_last 967 _publ_section_title ; Azoles. 38.* Struktur der Molekularverbindung von 3,5-Dinitroindazol, 5-Nitro-3-piperazinoindazol und Methanol ; _chemical_formula_sum 'C19 H21 N9 O7' _chemical_formula_weight 487.43 loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' 'x,-y,1/2+z' '1/2+x,1/2+y,z' '1/2+x,1/2-y,1/2+z' _symmetry_space_group_name_H-M 'C c' _cell_length_a 10.197(7) _cell_length_b 10.623(1) _cell_length_c 20.080(3) _cell_angle_alpha 90 _cell_angle_beta 101.53(2) _cell_angle_gamma 90 _cell_volume 2131.2(9) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_meas ? _diffrn_radiation_type 'CuK\a' _diffrn_radiation_wavelength 1.54178 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 25 _exptl_absorpt_coefficient_mu 0.907 _cell_measurement_temperature 293(2) _exptl_crystal_description 'tafeln' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_crystal_size_rad ? _exptl_crystal_colour 'dunkelgelb' _chemical_compound_source 'Synthese, Kristallisation aus CH~3~OH' _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method '\w-2\q' _exptl_absorpt_correction_type 'Experimentell' _exptl_absorpt_correction_T_min 0.5111 _exptl_absorpt_correction_T_max 0.9828 _diffrn_reflns_number 2429 _reflns_number_total 1863 _reflns_number_observed 1583 _reflns_observed_criterion F>=2\s(F) _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_theta_max 75 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_standards_number 2 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <6 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.0889 _refine_ls_wR_factor_obs 0.0947 _refine_ls_goodness_of_fit_obs 1.8529 _refine_ls_number_reflns 1583 _refine_ls_number_parameters 315 _refine_ls_hydrogen_treatment 'noref (4 H Atome vernachl\"assigt)' _refine_ls_weighting_scheme '1/[\s^2^(F~o~)+0.001F~o~^2^]' _refine_ls_shift/esd_max 0.02 _refine_diff_density_max 0.40 _refine_diff_density_min -0.36 _refine_ls_extinction_method "F~c~' = F~c~(1 - 0.0001\cF~c~^2^/sin \q)" _refine_ls_extinction_coef '\c = 0.0055(11)' _atom_type_scat_source 'SHELX76 (Sheldrick, 1976)' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv N(1A) 0.5114(12) 1.0786(6) 0.4591(5) 0.062(2) N(2A) 0.4621(13) 0.9600(6) 0.4619(5) 0.065(2) C(3A) 0.4794(14) 0.9275(7) 0.5274(5) 0.060(3) C(4A) 0.5816(13) 1.0440(8) 0.6423(5) 0.056(3) C(5A) 0.6344(15) 1.1607(10) 0.6601(6) 0.078(4) C(6A) 0.6531(15) 1.2544(9) 0.6132(7) 0.081(4) C(7A) 0.6169(15) 1.2353(8) 0.5483(7) 0.072(3) C(8A) 0.5582(14) 1.1173(7) 0.5249(5) 0.056(3) C(9A) 0.5402(14) 1.0250(7) 0.5725(5) 0.055(3) N(10A) 0.4465(13) 0.8051(6) 0.5458(5) 0.067(3) O(11A) 0.3944(12) 0.7304(6) 0.5015(5) 0.093(3) O(12A) 0.4693 0.7776(5) 0.6065 0.082(2) N(13A) 0.6808(18) 1.1836(11) 0.7331(6) 0.120(5) O(14A) 0.6588(16) 1.1052(10) 0.7737(5) 0.123(4) O(15A) 0.739(2) 1.2808(10) 0.7510(7) 0.218(5) N(1B) 0.3929(13) 0.5020(6) 0.1028(5) 0.067(5) N(2B) 0.4003(14) 0.5412(6) 0.1687(5) 0.080(3) C(3B) 0.3487(14) 0.6586(7) 0.1630(5) 0.058(3) C(4B) 0.2551(15) 0.8023(8) 0.0575(5) 0.063(3) C(5B) 0.2344(13) 0.7957(7) -0.0109(5) 0.051(3) C(6B) 0.2634(15) 0.6904(8) -0.0488(5) 0.066(3) C(7B) 0.3177(4) 0.5861(8) -0.0136(5) 0.067(3) C(8B) 0.3394(14) 0.5879(7) 0.0562(6) 0.056(3) C(9B) 0.3103(4) 0.6958(7) 0.0940(5) 0.053(2) N(10B) 0.3529(13) 0.7259(6) 0.2230(5) 0.069(2) C(11B) 0.2489(19) 0.8224(10) 0.2212(6) 0.096(3) C(12B) 0.2830(19) 0.9092(9) 0.2815(6) 0.104(3) N(13B) 0.3019(4) 0.8347(8) 0.3457(5) 0.079(3) C(14B) 0.4104(18) 0.7367(12) 0.3450(7) 0.100(5) C(15B) 0.3805(17) 0.6556(10) 0.2845(6) 0.086(3) N(16B) 0.1801(14) 0.9086(7) -0.0512(5) 0.080(3) O(17B) 0.1456(14) 0.9955(7) -0.0182(5) 0.114(3) O(18B) 0.1731(14) 0.9102(7) -0.1115(5) 0.096(3) O(19) 0.5612(6) 1.2143(10) 0.3492(6) 0.129(4) C(20) 0.486(6) 1.302(10) 0.286(7) 0.74(6) H(41A) 0.573 0.972 0.679 0.068 H(61A) 0.698 1.343 0.631 0.089 H(71A) 0.631 1.308 0.513 0.085 H(11B) 0.427 0.411 0.090 0.066 H(41B) 0.230 0.886 0.083 0.066 H(61B) 0.243 0.692 -0.104 0.071 H(71B) 0.343 0.504 -0.040 0.073 H(111B) 0.241 0.877 0.175 0.104 H(112B) 0.154 0.777 0.222 0.104 H(121B) 0.203 0.976 0.280 0.110 H(122B) 0.374 0.959 0.279 0.110 H(131B) 0.209 0.788 0.349 0.080 H(132B) 0.332 0.897 0.389 0.080 H(141B) 0.419 0.679 0.390 0.112 H(142B) 0.504 0.784 0.346 0.112 H(151B) 0.294 0.598 0.287 0.095 H(152B) 0.466 0.595 0.284 0.095