#------------------------------------------------------------------------------ #$Date: 2010-01-30 14:59:17 +0100 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003298.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_2003298 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 484 _journal_page_last 487 _publ_section_title ; Struktur der Molekularverbindung von 3,5-Dinitroindazol und Piperidin ; _chemical_formula_moiety '2C7 H3 N4 O4 , 2C5 H12 N1' _chemical_formula_sum 'C24 H30 N10 O8' _chemical_formula_weight 586.56 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 'P n a 21' _cell_length_a 20.076(2) _cell_length_b 6.831(2) _cell_length_c 20.113(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2758.3(9) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.412 _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 0.820 _cell_measurement_temperature 293 _exptl_crystal_description 'Nadeln' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_size_rad ? _exptl_crystal_colour 'gelb' _chemical_compound_source ; Kristallisation (Propanol/Hexan) ; _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method '\w-2\q' _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 3275 _reflns_number_total 2784 _reflns_number_observed 2560 _reflns_observed_criterion I>1.96\s(I) _diffrn_reflns_av_R_equivalents 'nicht verf\"ugbar' _diffrn_reflns_theta_max 75 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_standards_number 2 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.035 _refine_ls_wR_factor_obs 0.034 _refine_ls_goodness_of_fit_obs 2.8675 _refine_ls_number_reflns 2560 _refine_ls_number_parameters 500 _refine_ls_hydrogen_treatment 'refall' _refine_ls_weighting_scheme '1/\s^2^(F)' _refine_ls_shift/esd_max 0.01 _refine_diff_density_max 0.18 _refine_diff_density_min -0.17 _refine_ls_extinction_method "F~c~' = F~c~(1-0.0001\cF~c~^2^/sin\q)" _refine_ls_extinction_coef '\c = 0.00269' _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) .4907(1) .1368(4) .4149(1) .050(1) N(2A) .4964(1) .1360(4) .4820(1) .048(1) C(3A) .5607(1) .1472(4) .4976(1) .043(1) C(4A) .6696(1) .1607(4) .4265(1) .042(1) C(5A) .6864(1) .1664(4) .3601(1) .045(1) C(6A) .6393(2) .1685(5) .3082(1) .051(2) C(7A) .5733(2) .1599(5) .3219(2) .053(2) C(8A) .5538(1) .1489(4) .3893(1) .044(1) C(9A) .6016(1) .1547(4) .4403(1) .039(1) N(10A) .5814(1) .1525(4) .5651(1) .050(1) O(11A) .5379(1) .1526(4) .6086(1) .072(2) O(12A) .6409(1) .1536(4) .5768(1) .062(1) N(13A) .7567(1) .1748(4) .3433(1) .055(1) O(14A) .7981(1) .1873(4) .3877(1) .063(1) O(15A) .7723(1) .1713(6) .2845(1) .085(2) N(16A) .3840(1) .1540(4) .5798(1) .044(1) C(17A) .3661(2) .3431(5) .5483(2) .060(2) C(18A) .3062(2) .4292(7) .5814(3) .085(3) C(19A) .3169(3) .4550(7) .6556(3) .093(3) C(20A) .3342(2) .2583(7) .6864(2) .075(3) C(21A) .3951(2) .1722(7) .6532(2) .065(2) N(1B) .2702(1) -.0717(4) .5390(1) .048(1) N(2B) .2642(1) -.0837(4) .4721(1) .045(1) C(3B) .2007(1) -.1228(4) .4576(1) .040(1) C(4B) .0940(1) -.1726(4) .5301(1) .041(1) C(5B) .0782(1) -.1752(4) .5970(1) .044(1) C(6B) .1252(2) -.1483(5) .6482(1) .051(2) C(7B) .1899(2) -.1144(5) .6332(1) .050(2) C(8B) .2083(1) -.1064(4) .5657(1) .042(1) C(9B) .1608(1) -.1389(4) .5150(1) .038(1) N(10B) .1808(1) -.1442(3) .3900(1) .047(1) O(11B) .2237(1) -.1311(4) .3463(1) .066(1) O(12B) .1217(1) -.1712(4) .3787(1) .061(1) N(13B) .0088(1) -.2108(4) .6151(1) .055(1) O(14B) -.0324(1) -.2426(4) .5709(1) .062(1) O(15B) -.0065(1) -.2081(1) .6740(1) .082(2) N(16B) .3772(1) -.0966(4) .3767(1) .046(1) C(17B) .3961(2) -.2780(5) .4124(2) .055(2) C(18B) .4592(2) -.3639(6) .3855(2) .074(2) C(19B) .4525(2) -.4058(7) .3117(2) .086(3) C(20B) .4332(2) -.2188(8) .2756(2) .075(3) C(21B) .3696(2) -.1307(7) .3034(2) .064(2) H(41A) .708(1) .162(4) .463(1) .046(8) H(61A) .664(2) .196(5) .263(2) .07(1) H(71A) .538(1) .181(5) .292(2) .06(1) H(161A) .346(2) .062(5) .570(2) .07(1) H(162A) .423(1) .101(4) .562(1) .052(8) H(171A) .408(2) .420(5) .555(2) .08(1) H(172A) .364(2) .304(5) .495(2) .08(1) H(181A) .259(2) .328(7) .576(2) .13(2) H(182A) .293(2) .528(7) .562(2) .10(2) H(191A) .351(2) .532(7) .663(3) .12(2) H(192A) .267(2) .510(7) .673(2) .14(2) H(201A) .294(2) .179(5) .678(2) .07(1) H(202A) .347(2) .259(6) .732(2) .08(1) H(211A) .406(2) .026(7) .667(2) .10(1) H(212A) .439(2) .267(6) .659(2) .09(1) H(41B) .063(1) -.191(4) .499(1) .037(7) H(61B) .110(1) -.152(5) .691(2) .057(9) H(71B) .221(2) -.107(6) .667(2) .08(1) H(161B) .407(2) -.016(5) .386(2) .06(1) H(162B) .331(2) -.056(6) .400(2) .09(1) H(171B) .407(2) -.236(5) .455(2) .06(1) H(172B) .359(2) -.361(6) .407(2) .09(1) H(181B) .504(2) -.266(6) .388(2) .10(1) H(182B) .470(2) -.488(6) .416(2) .10(1) H(191B) .408(2) -.500(5) .302(2) .07(1) H(192B) .496(2) -.466(7) .298(2) .11(2) H(201B) .427(2) -.236(7) .235(2) .10(1) H(202B) .465(2) -.094(7) .278(2) .10(1) H(211B) .329(2) -.234(5) .301(1) .06(1) H(212B) .356(2) -.015(5) .286(2) .06(1) _cod_database_code 2003298