#------------------------------------------------------------------------------ #$Date: 2009-11-14 13:09:05 +0000 (Sat, 14 Nov 2009) $ #$Revision: 846 $ #$URL: svn://www.crystallography.net/cod/cif/2/2002967.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_2002967 _journal_name_full 'Acta Crystallographica, Section B' _journal_volume 55 _journal_year 1999 _journal_page_first 70 _journal_page_last 77 _publ_section_title ; LOW-TEMPERATURE CRYSTALLIZATION AND STRUCTURE DETERMINATION OF N-TRIFLUOROMETHYL FORMAMIDE, C~2~H~2~F~3~NO, N-2,2,2-TRIFLUOROETHYL FORMAMIDE, C~3~H~4~F~3~NO, AND 2,2,2-TRIFLUOROETHYL ISOCYANIDE, C~3~H~2~F~3~N ; loop_ _publ_author_name 'Perpetuo, Genivaldo' 'Buschmann, J\"urgen' 'Luger, Peter' 'Lentz, Dieter' 'Dreissig, D.' _chemical_formula_sum 'C3 H4 F3 N O' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_weight 127.07 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 4.8070(10) _cell_length_b 16.707(3) _cell_length_c 6.7080(10) _cell_angle_alpha 90.00 _cell_angle_beta 109.900(10) _cell_angle_gamma 90.00 _cell_volume 506.6(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 141.0(10) _exptl_crystal_description ; cylinder with diameter 0.5 mm ; _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_diffrn 1.666 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method ? _exptl_crystal_F_000 256 _exptl_absorpt_coefficient_mu 0.192 _exptl_absorpt_correction_type 'no' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_ambient_temperature 141.0(10) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71068 _diffrn_radiation_source 'fine-focus x-ray tube' _diffrn_radiation_monochromator none _diffrn_measurement_device ; Siemens four circle diffractometer, N2 gas stream cooled ; _diffrn_measurement_method '\w/2\q' _diffrn_reflns_number 2983 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_sigmaI/netI 0.0229 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 30.08 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 90 _diffrn_standards_decay_% 4 _reflns_number_total 1484 _reflns_number_observed 1018 _reflns_observed_criterion >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0783 _refine_ls_R_factor_obs 0.0508 _refine_ls_wR_factor_all 0.1402 _refine_ls_wR_factor_obs 0.1619 _refine_ls_goodness_of_fit_all 1.085 _refine_ls_goodness_of_fit_obs 1.085 _refine_ls_restrained_S_all 1.085 _refine_ls_restrained_S_obs 1.085 _refine_ls_number_reflns 1484 _refine_ls_number_parameters 89 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment ? _refine_ls_weighting_scheme ; calc w=1/[\s^2^(Fo^2^) + (0.0587P)^2^+0.2157P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_shift/esd_max 0.043 _refine_ls_shift/esd_mean 0.007 _refine_diff_density_max 0.295 _refine_diff_density_min -0.292 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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' 'F' 'F' 0.0171 0.0103 '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' _computing_data_collection ; Siemens software ; _computing_data_reduction ; Siemens software ; 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 O1 1.0908(3) 0.21170(10) 0.3539(2) 0.0270(10) Uani d . 1 . O C1 0.9939(4) 0.24450(10) 0.4805(3) 0.0210(10) Uani d . 1 . C H1 1.016(6) 0.298(2) 0.509(4) 0.027(6) Uiso d . 1 . H N2 0.8317(3) 0.20820(10) 0.5793(2) 0.0220(10) Uani d . 1 . N H2 0.766(5) 0.2350(10) 0.666(4) 0.013(5) Uiso d . 1 . H C3 0.7452(4) 0.12560(10) 0.5396(3) 0.0230(10) Uani d . 1 . C H31 0.780(7) 0.108(2) 0.411(5) 0.034(7) Uiso d . 1 . H H32 0.550(7) 0.121(2) 0.524(5) 0.041(8) Uiso d . 1 . H C4 0.9133(4) 0.07370(10) 0.7229(3) 0.0260(10) Uani d . 1 . C F1 1.2041(3) 0.07440(10) 0.7593(2) 0.0400(10) Uani d . 1 . F F2 0.8787(4) 0.09670(10) 0.9037(2) 0.0410(10) Uani d . 1 . F F3 0.8245(4) -0.00200(10) 0.6893(3) 0.0420(10) Uani d . 1 . F 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 O1 0.0278(6) 0.0326(7) 0.0256(6) 0.0004(5) 0.0153(5) 0.0029(5) C1 0.0194(7) 0.0233(8) 0.0202(7) 0.0009(6) 0.0053(5) 0.0032(6) N2 0.0247(7) 0.0225(7) 0.0214(6) 0.0007(6) 0.0120(5) -0.0006(5) C3 0.0216(8) 0.0245(8) 0.0241(7) -0.0016(6) 0.0086(6) 0.0011(6) C4 0.0263(8) 0.0245(9) 0.0285(8) -0.0001(7) 0.0107(6) 0.0015(7) F1 0.0251(6) 0.0457(8) 0.0466(7) 0.0078(5) 0.0088(5) 0.0054(6) F2 0.0547(8) 0.0449(8) 0.0266(6) 0.0094(6) 0.0193(5) 0.0080(5) F3 0.0517(8) 0.0250(6) 0.0480(8) -0.0037(6) 0.0130(6) 0.0068(5)