#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/4000234.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_4000234 _journal_name_full 'Chemistry of Materials' _journal_year 2003 _chemical_formula_moiety 'C2 H11 F3 N2 O3 P1 V1' _chemical_formula_sum 'C2 H11 F3 N2 O3 P V' _chemical_formula_weight 250.04 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 12.809(2) _cell_length_b 9.5180(14) _cell_length_c 6.4403(13) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 785.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 9 _cell_measurement_theta_max 30 _cell_measurement_wavelength 0.71073 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 2.115 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 504 _exptl_absorpt_coefficient_mu 1.493 _exptl_absorpt_correction_type none _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_orient_matrix_type ; x-axis points to radiation source the matrix is specified in reciprocal space ; _diffrn_orient_matrix_ub_11 -0.069178 _diffrn_orient_matrix_ub_12 -0.048703 _diffrn_orient_matrix_ub_13 0.002288 _diffrn_orient_matrix_ub_21 0.036006 _diffrn_orient_matrix_ub_22 -0.091855 _diffrn_orient_matrix_ub_23 0.022427 _diffrn_orient_matrix_ub_31 -0.004304 _diffrn_orient_matrix_ub_32 0.014177 _diffrn_orient_matrix_ub_33 0.153658 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_standards_number 2 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_standards_decay_corr_max 1 _diffrn_standards_decay_corr_min 1 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 -3 0 2 0 3 _diffrn_reflns_av_unetI/netI 0.2362 _diffrn_reflns_number 1169 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 28.69 _diffrn_reflns_theta_full 28.69 _diffrn_measured_fraction_theta_full 0.976 _diffrn_measured_fraction_theta_max 0.976 _reflns_number_total 1169 _reflns_number_gt 531 _reflns_threshold_expression >2sigma(I) _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 1169 _refine_ls_number_parameters 113 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1695 _refine_ls_R_factor_gt 0.0603 _refine_ls_wR_factor_ref 0.1262 _refine_ls_wR_factor_gt 0.1064 _refine_ls_goodness_of_fit_ref 0.856 _refine_ls_restrained_S_all 0.856 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.21(15) _refine_diff_density_max 0.964 _refine_diff_density_min -0.989 _refine_diff_density_rms 0.181 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 V V 0.80597(15) 0.1783(2) 0.8370(5) 0.0133(4) Uani 1 1 d . . . P P 0.7441(2) 0.1620(3) 0.3373(6) 0.0189(6) Uani 1 1 d D . . H1 H 0.667(8) 0.246(12) 0.28(3) 0.11(2) Uiso 1 1 d D . . F1 F 0.6602(4) 0.1862(7) 0.8389(14) 0.0327(16) Uani 1 1 d . . . F2 F 0.8103(5) 0.3844(5) 0.8368(12) 0.0248(14) Uani 1 1 d . . . F3 F 0.9601(4) 0.1866(6) 0.8290(12) 0.0272(14) Uani 1 1 d . . . O1 O 0.8120(7) 0.1831(11) 0.5311(14) 0.024(2) Uani 1 1 d . . . O2 O 0.8199(6) -0.0299(7) 0.8344(15) 0.0288(19) Uani 1 1 d . . . O3 O 0.8106(6) 0.1849(10) 1.1484(19) 0.036(2) Uani 1 1 d . . . N1 N -0.0108(8) 0.9694(10) 0.5110(14) 0.027(2) Uani 1 1 d . . . H2 H -0.0208 1.0249 0.6205 0.11(2) Uiso 1 1 calc R . . H3 H 0.031 0.8987 0.5463 0.11(2) Uiso 1 1 calc R . . H4 H -0.0718 0.9355 0.4682 0.11(2) Uiso 1 1 calc R . . N2 N 0.1180(8) 1.0297(9) -0.0056(14) 0.025(2) Uani 1 1 d . . . H5 H 0.1269 0.9721 -0.1131 0.11(2) Uiso 1 1 calc R . . H6 H 0.1801 1.0548 0.0444 0.11(2) Uiso 1 1 calc R . . H7 H 0.0835 1.1059 -0.0468 0.11(2) Uiso 1 1 calc R . . C1 C 0.0381(9) 1.0515(11) 0.341(2) 0.029(3) Uani 1 1 d . . . H8 H 0.1037 1.0914 0.3879 0.11(2) Uiso 1 1 calc R . . H9 H -0.0076 1.1279 0.3 0.11(2) Uiso 1 1 calc R . . C2 C 0.0569(9) 0.9562(12) 0.160(2) 0.036(3) Uani 1 1 d . . . H10 H -0.0095 0.9254 0.1039 0.11(2) Uiso 1 1 calc R . . H11 H 0.095 0.8738 0.2063 0.11(2) Uiso 1 1 calc R . . 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 V 0.0193(9) 0.0136(8) 0.0069(7) 0.0017(14) 0.0030(12) -0.0048(10) P 0.0271(15) 0.0190(13) 0.0106(11) -0.0004(17) 0.0011(16) 0.0004(12) F1 0.028(4) 0.037(4) 0.034(4) 0.014(6) -0.008(4) -0.007(3) F2 0.023(3) 0.023(3) 0.028(3) 0.003(4) 0.011(6) -0.009(3) F3 0.020(3) 0.034(3) 0.027(3) -0.003(6) 0.004(4) -0.006(3) O1 0.026(4) 0.043(5) 0.003(4) -0.002(5) 0.004(4) -0.003(7) O2 0.032(5) 0.030(4) 0.024(4) 0.007(5) -0.004(7) -0.002(4) O3 0.033(4) 0.060(5) 0.015(4) -0.002(8) 0.005(6) -0.006(7) N1 0.028(6) 0.043(6) 0.011(4) 0.010(5) 0.007(5) -0.013(5) N2 0.035(6) 0.027(5) 0.013(5) -0.004(5) 0.016(6) -0.009(5) C1 0.028(6) 0.032(6) 0.028(6) -0.021(7) 0.008(8) 0.008(6) C2 0.026(6) 0.046(7) 0.036(7) 0.031(8) 0.014(9) -0.004(6) _cod_database_code 4000234